data_4000020 _journal_name_full 'Chemistry of Materials' _journal_year 2000 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a c d ' _symmetry_Int_Tables_number 142 _cell_length_a 24.691(1) _cell_length_b 24.691(1) _cell_length_c 14.556(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8873.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 153.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2+z' ' -x, +y,1/2+z' '1/4+y,1/4+x,1/4+z' '1/4+y,1/4+x,1/4+z' '3/4-y,1/4+x,3/4+z' '3/4-y,1/4+x,3/4+z' ' +x,1/2-y,1/2+z' ' +x,1/2-y,1/2+z' ' -x,1/2-y, +z' ' -x,1/2-y, +z' '1/4+y,1/4-x,3/4+z' '1/4+y,1/4-x,3/4+z' '3/4-y,1/4-x,1/4+z' '3/4-y,1/4-x,1/4+z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2-z' ' +x, -y,1/2-z' '1/4-y,1/4-x,1/4-z' '1/4-y,1/4-x,1/4-z' '3/4+y,1/4-x,3/4-z' '3/4+y,1/4-x,3/4-z' ' -x,1/2+y,1/2-z' ' -x,1/2+y,1/2-z' ' +x,1/2+y, -z' ' +x,1/2+y, -z' '1/4-y,1/4+x,3/4-z' '1/4-y,1/4+x,3/4-z' '3/4+y,1/4+x,1/4-z' '3/4+y,1/4+x,1/4-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, +z' '1/2-x,1/2+y, +z' '3/4+y,3/4+x,3/4+z' '3/4+y,3/4+x,3/4+z' '1/4-y,3/4+x,1/4+z' '1/4-y,3/4+x,1/4+z' '1/2+x, -y, +z' '1/2+x, -y, +z' '1/2-x, -y,1/2+z' '1/2-x, -y,1/2+z' '3/4+y,3/4-x,1/4+z' '3/4+y,3/4-x,1/4+z' '1/4-y,3/4-x,3/4+z' '1/4-y,3/4-x,3/4+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, -z' '1/2+x,1/2-y, -z' '3/4-y,3/4-x,3/4-z' '3/4-y,3/4-x,3/4-z' '1/4+y,3/4-x,1/4-z' '1/4+y,3/4-x,1/4-z' '1/2-x, +y, -z' '1/2-x, +y, -z' '1/2+x, +y,1/2-z' '1/2+x, +y,1/2-z' '3/4-y,3/4+x,1/4-z' '3/4-y,3/4+x,1/4-z' '1/4+y,3/4+x,3/4-z' '1/4+y,3/4+x,3/4-z' _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1039.82 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H43 Cu2 F8 N8 Nb O2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _diffrn_ambient_temperature 153.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku CCD' _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 40126 _reflns_number_total 3060 _reflns_number_gt 806 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.16071 _diffrn_reflns_av_sigmaI/netI 0.303 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Nb(0) 0.0000 0.2500 0.1250 0.0249(3) 0.250 ST Uani d ? Cu(0) 0.12012(5) 0.1299 0.1250 0.0258(3) 0.500 ST Uani d ? F(1) -0.0545(3) 0.3045 0.1250 0.017(2) 0.250 S Uiso d ? F(2) 0.0000 0.2500 0.2576(4) 0.021(3) 0.500 ST Uani d ? F(3) 0.0554(2) 0.3054 0.1250 0.022(1) 0.500 ST Uani d ? F(4) 0.1968(3) 0.0532 0.1250 0.047(2) 0.500 ST Uani d ? F(5) -0.1818(3) 0.4318 -0.3750 0.081(2) 0.500 ST Uani d ? O(1) -0.0545 0.3045 0.1250 0.017 0.250 S Uiso d ? O(2) 0.2574(5) -0.0069(6) 0.1745(8) 0.026(5) 0.500 S Uani d ? N(1) 0.1189(5) 0.1251(6) -0.0148(5) 0.021(2) 1.000 . Uiso d ? N(2) 0.1800(3) 0.1877(3) 0.1224(9) 0.020(2) 1.000 . Uiso d ? C(1) 0.0863(7) 0.1576(6) -0.0638(7) 0.027(3) 1.000 . Uiso d ? C(2) 0.0835(6) 0.1566(6) -0.1600(7) 0.027(3) 1.000 . Uiso d ? C(3) 0.1170(6) 0.1198(5) -0.2064(7) 0.028(3) 1.000 . Uiso d ? C(4) 0.1513(5) 0.0849(5) -0.1577(7) 0.030(3) 1.000 . Uiso d ? C(5) 0.1503(5) 0.0893(5) -0.0610(7) 0.025(3) 1.000 . Uiso d ? C(6) 0.1678(3) 0.2411(4) 0.134(1) 0.027(3) 1.000 . Uiso d ? C(7) 0.2073(4) 0.2800(4) 0.129(1) 0.035(3) 1.000 . Uiso d ? C(8) 0.2618(4) 0.2637(4) 0.123(2) 0.034(3) 1.000 . Uiso d ? C(9) 0.2735(4) 0.2095(4) 0.117(1) 0.035(3) 1.000 . Uiso d ? C(10) 0.2319(4) 0.1714(4) 0.118(1) 0.031(3) 1.000 . Uiso d ? H(1) 0.0635 0.1819 -0.0316 0.029 1.000 . Uiso c ? H(2) 0.0596 0.1799 -0.1922 0.032 1.000 . Uiso c ? H(3) 0.1161 0.1183 -0.2714 0.031 1.000 . Uiso c ? H(4) 0.1739 0.0596 -0.1881 0.037 1.000 . Uiso c ? H(5) 0.1729 0.0659 -0.0263 0.030 1.000 . Uiso c ? H(6) 0.1316 0.2520 0.1428 0.034 1.000 . Uiso c ? H(7) 0.1985 0.3169 0.1337 0.041 1.000 . Uiso c ? H(8) 0.2900 0.2899 0.1223 0.035 1.000 . Uiso c ? H(9) 0.3103 0.1985 0.1129 0.041 1.000 . Uiso c ? H(10) 0.2408 0.1339 0.1170 0.036 1.000 . Uiso c ?