Supplementary Material (ESI) for J. Mater. Chem. This journal is (C) The Royal Society of Chemistry 2002 data_global _publ_contact_author_email dyzhao@fudan.edu.cn _publ_contact_author_name 'Prof Dongyuan Zhao' _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Zhao Dongyuan' 'Chen Zhenxia' 'Liu Zhicheng' 'Weng Linhong' ; Zhou Yaming ; data_FDZG-1 _database_code_CSD 193906 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 F2 Ge4 N2 O10 Zr' _chemical_formula_weight 667.74 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.725(5) _cell_length_b 10.149(3) _cell_length_c 9.547(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.720(2) _cell_angle_gamma 90.00 _cell_volume 1476.4(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 8.808 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5392 _exptl_absorpt_correction_T_max 0.6671 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3590 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.14 _reflns_number_total 1619 _reflns_number_gt 1550 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+11.3650P] 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 1619 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.003 _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 Zr1 Zr 0.5000 0.21839(5) 0.7500 0.01185(14) Uani 1 2 d S . . Ge1 Ge 0.30962(3) 0.06827(4) 0.45105(5) 0.01148(13) Uani 1 1 d . . . Ge2 Ge 0.20327(3) 0.31668(4) 0.26084(5) 0.01162(13) Uani 1 1 d . . . O1 O 0.2680(2) 0.1779(3) 0.2876(4) 0.0175(6) Uani 1 1 d . . . O2 O 0.25443(19) 0.0961(3) 0.5561(4) 0.0173(6) Uani 1 1 d . . . O3 O 0.2797(2) -0.0912(3) 0.3754(4) 0.0166(6) Uani 1 1 d . . . O4 O 0.4215(2) 0.0815(3) 0.5756(4) 0.0213(6) Uani 1 1 d . . . O5 O 0.40519(19) 0.2236(3) 0.8191(4) 0.0187(6) Uani 1 1 d . . . F1 F 0.4472(2) 0.3621(4) 0.5837(7) 0.0730(16) Uani 1 1 d . . . C1 C 0.4244(3) 0.2248(5) 0.2241(6) 0.0281(10) Uani 1 1 d . . . C2 C 0.4168(6) 0.3642(10) 0.1694(12) 0.0226(19) Uani 0.50 1 d P . . C3 C 0.5683(6) 0.3747(10) 0.2249(13) 0.0235(19) Uani 0.50 1 d P . . N1 N 0.5243(5) 0.1915(8) 0.3431(9) 0.0213(16) Uani 0.50 1 d P . . N2 N 0.4719(5) 0.3982(7) 0.1001(9) 0.0203(15) Uani 0.50 1 d P . . 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 Zr1 0.0099(2) 0.0109(3) 0.0148(3) 0.000 0.0063(2) 0.000 Ge1 0.0118(2) 0.0113(2) 0.0121(2) -0.00099(14) 0.00663(17) 0.00050(14) Ge2 0.0138(2) 0.0109(2) 0.0130(2) 0.00090(14) 0.00894(17) 0.00101(14) O1 0.0241(16) 0.0155(14) 0.0179(14) 0.0037(11) 0.0144(13) 0.0063(11) O2 0.0149(14) 0.0235(15) 0.0165(13) -0.0064(12) 0.0102(12) -0.0024(12) O3 0.0253(15) 0.0119(13) 0.0189(14) -0.0039(11) 0.0158(12) -0.0018(12) O4 0.0119(14) 0.0301(17) 0.0194(15) -0.0049(13) 0.0062(12) -0.0022(12) O5 0.0119(13) 0.0271(17) 0.0179(14) -0.0035(12) 0.0083(11) -0.0026(12) F1 0.042(2) 0.062(3) 0.131(4) 0.076(3) 0.055(3) 0.0339(19) C1 0.024(2) 0.030(3) 0.025(2) -0.0015(19) 0.0090(19) -0.010(2) C2 0.012(4) 0.037(5) 0.020(5) 0.005(4) 0.009(3) 0.007(4) C3 0.014(4) 0.032(5) 0.026(5) 0.009(4) 0.011(4) 0.004(4) N1 0.027(4) 0.024(4) 0.015(4) 0.001(3) 0.012(3) 0.002(3) N2 0.024(4) 0.017(4) 0.023(4) 0.002(3) 0.014(3) 0.004(3) _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 Zr1 F1 2.001(3) 2_656 ? Zr1 F1 2.001(3) . ? Zr1 O4 2.067(3) . ? Zr1 O4 2.067(3) 2_656 ? Zr1 O5 2.097(3) 2_656 ? Zr1 O5 2.097(3) . ? Ge1 O4 1.719(3) . ? Ge1 O3 1.741(3) . ? Ge1 O1 1.744(3) . ? Ge1 O2 1.745(3) . ? Ge2 O5 1.716(3) 7_556 ? Ge2 O3 1.749(3) 4 ? Ge2 O2 1.749(3) 7_556 ? Ge2 O1 1.751(3) . ? O2 Ge2 1.749(3) 7_556 ? O3 Ge2 1.749(3) 4_545 ? O5 Ge2 1.716(3) 7_556 ? C1 N1 1.396(9) 2_655 ? C1 C2 1.490(11) . ? C1 N1 1.576(9) . ? C1 C3 1.582(11) 2_655 ? C2 C3 0.909(13) 2_655 ? C2 N2 1.474(11) . ? C3 C2 0.909(13) 2_655 ? C3 N2 1.522(11) . ? C3 C1 1.582(11) 2_655 ? N1 C1 1.396(9) 2_655 ? N1 N1 1.530(14) 2_655 ? 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 F1 Zr1 F1 86.4(4) 2_656 . ? F1 Zr1 O4 168.11(13) 2_656 . ? F1 Zr1 O4 90.06(19) . . ? F1 Zr1 O4 90.06(19) 2_656 2_656 ? F1 Zr1 O4 168.11(13) . 2_656 ? O4 Zr1 O4 95.55(19) . 2_656 ? F1 Zr1 O5 96.08(14) 2_656 2_656 ? F1 Zr1 O5 81.80(14) . 2_656 ? O4 Zr1 O5 94.65(12) . 2_656 ? O4 Zr1 O5 87.29(12) 2_656 2_656 ? F1 Zr1 O5 81.80(14) 2_656 . ? F1 Zr1 O5 96.08(14) . . ? O4 Zr1 O5 87.29(12) . . ? O4 Zr1 O5 94.65(12) 2_656 . ? O5 Zr1 O5 177.12(18) 2_656 . ? O4 Ge1 O3 111.03(15) . . ? O4 Ge1 O1 112.36(15) . . ? O3 Ge1 O1 108.77(14) . . ? O4 Ge1 O2 112.16(15) . . ? O3 Ge1 O2 104.34(14) . . ? O1 Ge1 O2 107.80(15) . . ? O5 Ge2 O3 112.08(15) 7_556 4 ? O5 Ge2 O2 112.08(14) 7_556 7_556 ? O3 Ge2 O2 108.89(15) 4 7_556 ? O5 Ge2 O1 112.00(15) 7_556 . ? O3 Ge2 O1 100.93(14) 4 . ? O2 Ge2 O1 110.29(14) 7_556 . ? Ge1 O1 Ge2 126.16(17) . . ? Ge1 O2 Ge2 125.17(17) . 7_556 ? Ge1 O3 Ge2 132.36(17) . 4_545 ? Ge1 O4 Zr1 132.36(18) . . ? Ge2 O5 Zr1 138.56(17) 7_556 . ? N1 C1 C2 91.9(6) 2_655 . ? N1 C1 N1 61.6(5) 2_655 . ? C2 C1 N1 108.9(5) . . ? N1 C1 C3 113.9(6) 2_655 2_655 ? C2 C1 C3 34.3(5) . 2_655 ? N1 C1 C3 95.7(5) . 2_655 ? C3 C2 N2 126.0(11) 2_655 . ? C3 C2 C1 78.4(9) 2_655 . ? N2 C2 C1 114.6(7) . . ? C2 C3 N2 117.4(10) 2_655 . ? C2 C3 C1 67.3(9) 2_655 2_655 ? N2 C3 C1 105.9(7) . 2_655 ? C1 N1 N1 65.0(5) 2_655 2_655 ? C1 N1 C1 111.8(5) 2_655 . ? N1 N1 C1 53.4(5) 2_655 . ? C2 N2 C3 110.4(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.234 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.216