# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Philip Lightfoot' 'Yang Li.' 'Thushitha Mahenthirarajah' _publ_contact_author_name 'Philip Lightfoot' _publ_contact_author_email PL@ST-ANDREWS.AC.UK _publ_section_title ; Organic-inorganic hybrid chains and layers constructed from copper-amine cations and early transition metal (Nb, Mo) oxyfluoride anions. ; # Attachment 'Mahenthirarajah.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 715741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Cu F4 Mo N8 O3' _chemical_formula_sum 'C4 H10 Cu F4 Mo N8 O3' _chemical_formula_weight 453.69 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.1627(18) _cell_length_b 11.810(3) _cell_length_c 14.438(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.992(9) _cell_angle_gamma 90.00 _cell_volume 1220.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8275 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 2.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8275 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2495 _reflns_number_gt 2151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0437P)^2^+2.9196P] 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 2495 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 Mo1 Mo -0.26651(5) 0.25681(3) 0.14647(3) 0.01971(15) Uani 1 1 d . . . Cu2 Cu 0.5000 0.0000 0.0000 0.01149(19) Uani 1 2 d S . . Cu1 Cu 0.0000 0.0000 0.0000 0.01117(19) Uani 1 2 d S . . F1 F -0.2756(4) 0.3398(2) 0.03657(19) 0.0275(6) Uani 1 1 d . . . F2 F -0.2018(5) 0.1454(2) 0.24205(19) 0.0412(8) Uani 1 1 d . . . F3 F 0.0128(4) 0.2607(2) 0.1354(2) 0.0290(6) Uani 1 1 d . . . F4 F -0.2438(3) 0.11604(19) 0.06128(16) 0.0181(5) Uani 1 1 d . . . O1 O -0.2586(4) 0.3714(3) 0.2209(2) 0.0230(7) Uani 1 1 d . . . O2 O -0.5058(4) 0.2264(3) 0.1518(2) 0.0256(7) Uani 1 1 d . . . O3 O 0.2328(5) 0.2227(3) 0.2994(3) 0.0245(8) Uani 1 1 d . . . H3A H 0.136(9) 0.220(5) 0.272(4) 0.037 Uiso 1 1 d . . . H3B H 0.308(9) 0.230(5) 0.280(5) 0.037 Uiso 1 1 d . . . N1 N 0.1611(4) -0.0130(3) 0.1156(2) 0.0125(7) Uani 1 1 d . . . N2 N 0.3541(4) -0.0114(3) 0.1145(2) 0.0122(7) Uani 1 1 d . . . N3 N 0.2704(5) -0.0234(3) 0.2570(2) 0.0136(7) Uani 1 1 d . . . N4 N 0.2737(5) -0.0306(3) 0.3546(2) 0.0233(8) Uani 1 1 d . . . H4A H 0.1707 -0.0331 0.3834 0.028 Uiso 1 1 calc R . . H4B H 0.3788 -0.0326 0.3853 0.028 Uiso 1 1 calc R . . N5 N 0.1490(4) 0.1310(3) -0.0393(2) 0.0122(7) Uani 1 1 d . . . N6 N 0.3418(4) 0.1328(3) -0.0422(2) 0.0113(7) Uani 1 1 d . . . N7 N 0.2354(4) 0.3023(3) -0.0657(2) 0.0139(7) Uani 1 1 d . . . N8 N 0.2178(5) 0.4199(3) -0.0813(3) 0.0277(9) Uani 1 1 d . . . H8A H 0.1091 0.4509 -0.0836 0.033 Uiso 1 1 calc R . . H8B H 0.3158 0.4606 -0.0885 0.033 Uiso 1 1 calc R . . C1 C 0.4163(6) -0.0165(3) 0.2002(3) 0.0153(8) Uani 1 1 d . . . H11 H 0.5416 -0.0157 0.2194 0.018 Uiso 1 1 calc R . . C2 C 0.1150(5) -0.0197(3) 0.2017(3) 0.0129(8) Uani 1 1 d . . . H21 H -0.0067 -0.0218 0.2220 0.016 Uiso 1 1 calc R . . C3 C 0.3904(5) 0.2374(3) -0.0589(3) 0.0129(8) Uani 1 1 d . . . H31 H 0.5121 0.2630 -0.0650 0.016 Uiso 1 1 calc R . . C4 C 0.0885(6) 0.2334(3) -0.0539(3) 0.0152(8) Uani 1 1 d . . . H41 H -0.0362 0.2556 -0.0558 0.018 Uiso 1 1 calc R . . 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 Mo1 0.0225(2) 0.0174(2) 0.0190(3) -0.00432(15) -0.00412(16) 0.00469(13) Cu2 0.0088(3) 0.0138(4) 0.0120(4) 0.0029(3) 0.0020(3) 0.0023(2) Cu1 0.0085(3) 0.0120(4) 0.0130(4) 0.0028(3) -0.0012(3) -0.0025(2) F1 0.0285(14) 0.0233(14) 0.0304(15) 0.0032(12) -0.0035(11) -0.0013(10) F2 0.072(2) 0.0332(17) 0.0183(15) 0.0068(13) -0.0008(14) 0.0195(15) F3 0.0182(14) 0.0352(16) 0.0333(16) -0.0121(12) -0.0025(11) 0.0028(10) F4 0.0211(13) 0.0140(12) 0.0195(13) -0.0038(10) 0.0020(9) -0.0026(9) O1 0.0154(15) 0.0251(16) 0.0284(18) -0.0119(14) 0.0000(12) 0.0018(12) O2 0.0205(16) 0.0250(17) 0.032(2) -0.0110(15) 0.0107(13) -0.0066(12) O3 0.0242(19) 0.0233(17) 0.026(2) -0.0026(15) -0.0005(14) -0.0002(15) N1 0.0091(16) 0.0112(16) 0.0171(19) 0.0009(14) 0.0007(13) -0.0008(11) N2 0.0075(15) 0.0119(16) 0.0172(19) 0.0011(13) 0.0001(12) 0.0002(11) N3 0.0177(17) 0.0148(16) 0.0083(17) -0.0006(14) 0.0005(13) -0.0014(13) N4 0.025(2) 0.033(2) 0.0117(19) 0.0028(16) 0.0016(15) -0.0049(16) N5 0.0076(15) 0.0130(16) 0.0161(17) 0.0012(14) -0.0002(12) -0.0002(12) N6 0.0069(15) 0.0161(17) 0.0110(17) 0.0018(14) 0.0019(11) -0.0004(12) N7 0.0174(17) 0.0071(16) 0.0173(18) 0.0029(14) 0.0017(13) -0.0016(12) N8 0.024(2) 0.0094(17) 0.050(3) 0.0088(18) 0.0099(17) 0.0034(14) C1 0.016(2) 0.015(2) 0.014(2) -0.0022(16) -0.0017(15) -0.0028(15) C2 0.014(2) 0.0146(19) 0.010(2) 0.0001(16) 0.0036(15) 0.0009(15) C3 0.0115(19) 0.016(2) 0.012(2) 0.0009(16) 0.0015(14) -0.0043(14) C4 0.015(2) 0.014(2) 0.017(2) 0.0030(16) 0.0039(16) 0.0027(15) _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 Mo1 O1 1.728(3) . ? Mo1 O2 1.755(3) . ? Mo1 F1 1.864(3) . ? Mo1 F2 1.951(3) . ? Mo1 F3 2.013(3) . ? Mo1 F4 2.078(2) . ? Cu2 N2 1.991(3) . ? Cu2 N2 1.991(3) 3_655 ? Cu2 N6 2.016(3) 3_655 ? Cu2 N6 2.016(3) . ? Cu1 N5 1.974(3) 3 ? Cu1 N5 1.974(3) . ? Cu1 N1 2.001(3) . ? Cu1 N1 2.001(3) 3 ? Cu1 F4 2.412(2) 3 ? Cu1 F4 2.412(2) . ? O3 H3A 0.79(6) . ? O3 H3B 0.62(7) . ? N1 C2 1.300(5) . ? N1 N2 1.383(4) . ? N2 C1 1.302(5) . ? N3 C2 1.348(5) . ? N3 C1 1.354(5) . ? N3 N4 1.410(5) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C4 1.300(5) . ? N5 N6 1.384(4) . ? N6 C3 1.309(5) . ? N7 C4 1.345(5) . ? N7 C3 1.349(5) . ? N7 N8 1.413(5) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? C1 H11 0.9300 . ? C2 H21 0.9300 . ? C3 H31 0.9300 . ? C4 H41 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 Mo1 O2 98.28(14) . . ? O1 Mo1 F1 96.70(13) . . ? O2 Mo1 F1 98.02(14) . . ? O1 Mo1 F2 94.97(14) . . ? O2 Mo1 F2 92.27(15) . . ? F1 Mo1 F2 163.15(12) . . ? O1 Mo1 F3 91.13(12) . . ? O2 Mo1 F3 169.35(12) . . ? F1 Mo1 F3 85.75(12) . . ? F2 Mo1 F3 81.90(13) . . ? O1 Mo1 F4 173.39(11) . . ? O2 Mo1 F4 87.65(12) . . ? F1 Mo1 F4 85.30(11) . . ? F2 Mo1 F4 81.81(11) . . ? F3 Mo1 F4 82.71(10) . . ? N2 Cu2 N2 180.00(18) . 3_655 ? N2 Cu2 N6 90.12(13) . 3_655 ? N2 Cu2 N6 89.88(13) 3_655 3_655 ? N2 Cu2 N6 89.88(13) . . ? N2 Cu2 N6 90.12(13) 3_655 . ? N6 Cu2 N6 180.0(2) 3_655 . ? N5 Cu1 N5 180.0(2) 3 . ? N5 Cu1 N1 90.13(13) 3 . ? N5 Cu1 N1 89.87(13) . . ? N5 Cu1 N1 89.87(13) 3 3 ? N5 Cu1 N1 90.13(13) . 3 ? N1 Cu1 N1 180.0(2) . 3 ? N5 Cu1 F4 93.76(11) 3 3 ? N5 Cu1 F4 86.24(11) . 3 ? N1 Cu1 F4 81.87(11) . 3 ? N1 Cu1 F4 98.13(11) 3 3 ? N5 Cu1 F4 86.24(11) 3 . ? N5 Cu1 F4 93.76(11) . . ? N1 Cu1 F4 98.13(11) . . ? N1 Cu1 F4 81.87(11) 3 . ? F4 Cu1 F4 180.00(10) 3 . ? Mo1 F4 Cu1 138.10(11) . . ? H3A O3 H3B 123(8) . . ? C2 N1 N2 107.4(3) . . ? C2 N1 Cu1 130.1(3) . . ? N2 N1 Cu1 122.5(3) . . ? C1 N2 N1 107.4(3) . . ? C1 N2 Cu2 128.3(3) . . ? N1 N2 Cu2 124.3(2) . . ? C2 N3 C1 106.1(3) . . ? C2 N3 N4 125.4(3) . . ? C1 N3 N4 128.5(3) . . ? N3 N4 H4A 120.0 . . ? N3 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C4 N5 N6 108.0(3) . . ? C4 N5 Cu1 126.6(3) . . ? N6 N5 Cu1 124.8(2) . . ? C3 N6 N5 107.0(3) . . ? C3 N6 Cu2 129.8(3) . . ? N5 N6 Cu2 122.0(2) . . ? C4 N7 C3 107.0(3) . . ? C4 N7 N8 123.3(3) . . ? C3 N7 N8 129.7(3) . . ? N7 N8 H8A 120.0 . . ? N7 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? N2 C1 N3 109.4(4) . . ? N2 C1 H11 125.3 . . ? N3 C1 H11 125.3 . . ? N1 C2 N3 109.7(3) . . ? N1 C2 H21 125.1 . . ? N3 C2 H21 125.1 . . ? N6 C3 N7 109.0(3) . . ? N6 C3 H31 125.5 . . ? N7 C3 H31 125.5 . . ? N5 C4 N7 109.0(3) . . ? N5 C4 H41 125.5 . . ? N7 C4 H41 125.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3B O2 0.62(7) 2.32(7) 2.885(5) 153(8) 1_655 N8 H8B F1 0.86 2.49 2.936(4) 112.8 3_565 O3 H3A F3 0.79(6) 2.18(6) 2.833(5) 140(6) . O3 H3A F2 0.79(6) 2.60(6) 3.321(5) 154(5) . _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.798 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.155 #===end data_2 _database_code_depnum_ccdc_archive 'CCDC 715742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Cu F5 N8 Nb O2' _chemical_formula_sum 'C4 H10 Cu F5 N8 Nb O2' _chemical_formula_weight 453.66 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.1511(18) _cell_length_b 11.869(3) _cell_length_c 14.671(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.051(9) _cell_angle_gamma 90.00 _cell_volume 1245.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8504 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 2.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8504 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2593 _reflns_number_gt 1838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0528P)^2^+3.3043P] 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 SHELXL _refine_ls_extinction_coef 0.0016(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2593 _refine_ls_number_parameters 197 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.027 _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 Nb1 Nb -0.24805(7) -0.25231(4) 1.14127(3) 0.0313(2) Uani 1 1 d . . . Cu2 Cu 0.5000 0.0000 1.0000 0.0229(3) Uani 1 2 d S . . Cu1 Cu 0.0000 0.0000 1.0000 0.0213(3) Uani 1 2 d S . . F1 F -0.2791(5) -0.3461(3) 1.0343(2) 0.0471(9) Uani 1 1 d . . . F5 F -0.2534(5) -0.3848(3) 1.2166(2) 0.0395(9) Uani 0.50 1 d P . . O5 O -0.2534(5) -0.3848(3) 1.2166(2) 0.0395(9) Uani 0.50 1 d P . . F3 F -0.1900(7) -0.1609(3) 1.2461(3) 0.0778(15) Uani 1 1 d . . . F4 F -0.5107(5) -0.2369(3) 1.1573(4) 0.0637(13) Uani 1 1 d . . . F2 F 0.0199(5) -0.2697(3) 1.1304(3) 0.0542(11) Uani 1 1 d . . . F6 F -0.2487(5) -0.1199(3) 1.0651(2) 0.0354(8) Uani 0.50 1 d P . . O6 O -0.2487(5) -0.1199(3) 1.0651(2) 0.0354(8) Uani 0.50 1 d P . . O1 O 0.2405(7) -0.2275(3) 1.3029(3) 0.0443(11) Uani 1 1 d D . . H10A H 0.140(7) -0.223(6) 1.266(5) 0.066 Uiso 1 1 d D . . H10B H 0.322(9) -0.226(6) 1.258(4) 0.066 Uiso 1 1 d D . . N1 N 0.1581(6) 0.0118(3) 1.1139(3) 0.0217(9) Uani 1 1 d . . . N2 N 0.3514(6) 0.0109(3) 1.1140(3) 0.0215(9) Uani 1 1 d . . . N3 N 0.2614(6) 0.0194(3) 1.2538(3) 0.0228(10) Uani 1 1 d . . . N4 N 0.2588(7) 0.0231(4) 1.3492(3) 0.0366(12) Uani 1 1 d . . . H4A H 0.1539 0.0242 1.3768 0.044 Uiso 1 1 calc R . . H4B H 0.3622 0.0244 1.3800 0.044 Uiso 1 1 calc R . . N5 N 0.1497(6) -0.1298(3) 0.9591(3) 0.0227(9) Uani 1 1 d . . . N6 N 0.3431(6) -0.1336(3) 0.9604(3) 0.0242(10) Uani 1 1 d . . . N7 N 0.2351(7) -0.3014(3) 0.9342(3) 0.0278(11) Uani 1 1 d . . . N8 N 0.2160(8) -0.4183(3) 0.9190(4) 0.0488(15) Uani 1 1 d . . . H8A H 0.3138 -0.4600 0.9150 0.059 Uiso 1 1 calc R . . H8B H 0.1065 -0.4478 0.9138 0.059 Uiso 1 1 calc R . . C1 C 0.1091(8) 0.0172(4) 1.1988(4) 0.0266(12) Uani 1 1 d . . . H11 H -0.0137 0.0193 1.2185 0.032 Uiso 1 1 calc R . . C2 C 0.4105(5) 0.0154(3) 1.1982(3) 0.0259(12) Uani 1 1 d . . . H21 H 0.5352 0.0157 1.2173 0.031 Uiso 1 1 calc R . . C3 C 0.0883(5) -0.2317(3) 0.9431(3) 0.0261(12) Uani 1 1 d R . . H31 H -0.0368 -0.2527 0.9385 0.031 Uiso 1 1 calc R . . C4 C 0.3902(8) -0.2388(4) 0.9442(4) 0.0254(12) Uani 1 1 d . . . H41 H 0.5120 -0.2655 0.9402 0.030 Uiso 1 1 calc R . . 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 Nb1 0.0288(4) 0.0337(3) 0.0314(4) -0.0045(2) 0.0011(2) 0.0014(2) Cu2 0.0193(5) 0.0261(5) 0.0235(5) -0.0058(4) 0.0045(4) -0.0043(3) Cu1 0.0184(5) 0.0209(4) 0.0244(5) -0.0043(3) -0.0025(4) 0.0045(3) F1 0.064(3) 0.0329(18) 0.044(2) -0.0045(16) -0.0085(18) 0.0075(16) F5 0.035(2) 0.0378(19) 0.046(2) 0.0202(17) 0.0000(18) -0.0014(16) O5 0.035(2) 0.0378(19) 0.046(2) 0.0202(17) 0.0000(18) -0.0014(16) F3 0.141(5) 0.056(2) 0.036(2) -0.008(2) 0.005(3) -0.028(3) F4 0.034(2) 0.055(2) 0.104(4) 0.026(2) 0.025(2) 0.0111(17) F2 0.027(2) 0.067(2) 0.068(3) 0.028(2) 0.0004(18) 0.0033(17) F6 0.039(2) 0.0284(17) 0.039(2) 0.0059(16) 0.0033(17) 0.0016(15) O6 0.039(2) 0.0284(17) 0.039(2) 0.0059(16) 0.0033(17) 0.0016(15) O1 0.058(3) 0.035(2) 0.040(3) 0.003(2) -0.001(2) -0.002(2) N1 0.019(2) 0.025(2) 0.022(2) -0.0042(18) 0.0020(19) 0.0002(17) N2 0.018(2) 0.023(2) 0.024(2) 0.0007(18) 0.0008(19) -0.0011(16) N3 0.024(3) 0.024(2) 0.020(2) 0.0000(18) 0.000(2) 0.0015(17) N4 0.045(3) 0.049(3) 0.016(2) -0.002(2) -0.002(2) -0.001(2) N5 0.014(2) 0.025(2) 0.029(2) -0.0001(19) -0.0018(18) 0.0011(17) N6 0.018(2) 0.025(2) 0.030(2) -0.0052(19) 0.0013(19) 0.0025(17) N7 0.038(3) 0.0133(19) 0.032(3) 0.0027(19) 0.006(2) 0.0026(18) N8 0.055(4) 0.014(2) 0.078(4) -0.009(2) 0.023(3) -0.006(2) C1 0.028(3) 0.025(3) 0.027(3) 0.000(2) 0.005(2) 0.002(2) C2 0.023(3) 0.025(2) 0.030(3) 0.000(2) 0.000(2) 0.000(2) C3 0.024(3) 0.024(2) 0.030(3) -0.006(2) 0.006(2) -0.006(2) C4 0.023(3) 0.026(3) 0.027(3) -0.003(2) 0.001(2) 0.011(2) _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 Nb1 F4 1.906(4) . ? Nb1 F3 1.921(4) . ? Nb1 F5 1.923(3) . ? Nb1 F6 1.928(3) . ? Nb1 F1 1.934(4) . ? Nb1 F2 1.937(4) . ? Cu2 N2 2.002(4) . ? Cu2 N2 2.002(4) 3_657 ? Cu2 N6 2.022(4) 3_657 ? Cu2 N6 2.022(4) . ? Cu1 N5 1.975(4) 3_557 ? Cu1 N5 1.975(4) . ? Cu1 N1 2.005(4) 3_557 ? Cu1 N1 2.005(4) . ? O1 H10A 0.89(2) . ? O1 H10B 0.89(2) . ? N1 C1 1.302(7) . ? N1 N2 1.382(6) . ? N2 C2 1.300(6) . ? N3 C1 1.344(7) . ? N3 C2 1.354(5) . ? N3 N4 1.400(6) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C3 1.307(5) . ? N5 N6 1.384(6) . ? N6 C4 1.315(6) . ? N7 C4 1.341(7) . ? N7 C3 1.344(6) . ? N7 N8 1.411(6) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? C1 H11 0.9300 . ? C2 H21 0.9300 . ? C3 H31 0.9300 . ? C4 H41 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 F4 Nb1 F3 92.6(2) . . ? F4 Nb1 F5 88.72(16) . . ? F3 Nb1 F5 90.44(17) . . ? F4 Nb1 F6 90.06(15) . . ? F3 Nb1 F6 90.10(16) . . ? F5 Nb1 F6 178.69(15) . . ? F4 Nb1 F1 93.3(2) . . ? F3 Nb1 F1 174.12(19) . . ? F5 Nb1 F1 89.57(15) . . ? F6 Nb1 F1 90.01(14) . . ? F4 Nb1 F2 177.56(18) . . ? F3 Nb1 F2 85.8(2) . . ? F5 Nb1 F2 89.43(15) . . ? F6 Nb1 F2 91.80(15) . . ? F1 Nb1 F2 88.32(18) . . ? N2 Cu2 N2 180.000(1) . 3_657 ? N2 Cu2 N6 90.55(16) . 3_657 ? N2 Cu2 N6 89.45(16) 3_657 3_657 ? N2 Cu2 N6 89.45(16) . . ? N2 Cu2 N6 90.55(16) 3_657 . ? N6 Cu2 N6 180.0 3_657 . ? N5 Cu1 N5 180.0(2) 3_557 . ? N5 Cu1 N1 90.41(16) 3_557 3_557 ? N5 Cu1 N1 89.59(17) . 3_557 ? N5 Cu1 N1 89.59(17) 3_557 . ? N5 Cu1 N1 90.41(16) . . ? N1 Cu1 N1 180.000(1) 3_557 . ? H10A O1 H10B 94(7) . . ? C1 N1 N2 106.6(4) . . ? C1 N1 Cu1 130.0(4) . . ? N2 N1 Cu1 123.3(3) . . ? C2 N2 N1 107.9(4) . . ? C2 N2 Cu2 129.0(3) . . ? N1 N2 Cu2 123.1(3) . . ? C1 N3 C2 106.0(4) . . ? C1 N3 N4 125.1(4) . . ? C2 N3 N4 128.8(4) . . ? N3 N4 H4A 120.0 . . ? N3 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C3 N5 N6 107.7(4) . . ? C3 N5 Cu1 126.5(3) . . ? N6 N5 Cu1 124.7(3) . . ? C4 N6 N5 106.7(4) . . ? C4 N6 Cu2 130.8(4) . . ? N5 N6 Cu2 121.8(3) . . ? C4 N7 C3 107.1(4) . . ? C4 N7 N8 129.8(5) . . ? C3 N7 N8 123.1(4) . . ? N7 N8 H8A 120.0 . . ? N7 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? N1 C1 N3 110.2(5) . . ? N1 C1 H11 124.9 . . ? N3 C1 H11 124.9 . . ? N2 C2 N3 109.2(4) . . ? N2 C2 H21 125.4 . . ? N3 C2 H21 125.4 . . ? N5 C3 N7 109.1(4) . . ? N5 C3 H31 125.5 . . ? N7 C3 H31 125.5 . . ? N6 C4 N7 109.4(4) . . ? N6 C4 H41 125.3 . . ? N7 C4 H41 125.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H10A F3 0.89(2) 2.49(5) 3.272(7) 148(7) . O1 H10A F2 0.89(2) 2.23(5) 3.000(7) 145(7) . O1 H10B F4 0.89(2) 1.92(2) 2.807(6) 174(7) 1_655 N8 H8A F1 0.86 2.43 2.912(5) 115.8 3_547 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.823 _refine_diff_density_min -0.870 _refine_diff_density_rms 0.161 #===end data_3 _database_code_depnum_ccdc_archive 'CCDC 715743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Cu3 F12 Mo3 N24 O6' _chemical_formula_sum 'C36 H48 Cu3 F12 Mo3 N24 O6' _chemical_formula_weight 1619.45 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' Cu Cu 0.3201 1.2651 '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' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 31.427(7) _cell_length_b 12.608(2) _cell_length_c 16.951(4) _cell_angle_alpha 90.00 _cell_angle_beta 120.476(4) _cell_angle_gamma 90.00 _cell_volume 5788(2) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 18046 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25.3 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3204 _exptl_absorpt_coefficient_mu 1.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18046 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5203 _reflns_number_gt 4593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1137P)^2^+0.6046P] 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 0.00017(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5203 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Mo1 Mo 0.059055(14) 0.26778(3) 0.45086(3) 0.01753(18) Uani 1 1 d . . . Mo2 Mo 0.2500 0.7500 0.5000 0.0235(2) Uani 1 2 d S . . Cu1 Cu 0.157410(19) 0.50261(4) 0.48443(4) 0.0192(2) Uani 1 1 d . . . Cu2 Cu 0.0000 0.0000 0.5000 0.0253(2) Uani 1 2 d S . . F1 F 0.03681(10) 0.3498(3) 0.51786(19) 0.0499(9) Uani 1 1 d . . . F2 F 0.11775(10) 0.2302(2) 0.5841(2) 0.0306(7) Uani 1 1 d . . . F3 F 0.09477(14) 0.1786(3) 0.4135(3) 0.0698(11) Uani 1 1 d . . . F4 F 0.10306(10) 0.3782(2) 0.46486(19) 0.0321(7) Uani 0.50 1 d P . . O4 O 0.10306(10) 0.3782(2) 0.46486(19) 0.0321(7) Uani 0.50 1 d P . . F5 F 0.03165(10) 0.1454(2) 0.4726(2) 0.0343(8) Uani 0.50 1 d P . . O5 O 0.03165(10) 0.1454(2) 0.4726(2) 0.0343(8) Uani 0.50 1 d P . . F6 F 0.20296(12) 0.7731(2) 0.3760(2) 0.0358(8) Uani 0.75 1 d P . . O6 O 0.20296(12) 0.7731(2) 0.3760(2) 0.0358(8) Uani 0.25 1 d P . . F7 F 0.28476(11) 0.6574(3) 0.4647(2) 0.0446(9) Uani 0.75 1 d P . . O7 O 0.28476(11) 0.6574(3) 0.4647(2) 0.0446(9) Uani 0.25 1 d P . . F8 F 0.21103(10) 0.6346(2) 0.49945(19) 0.0295(7) Uani 0.50 1 d P . . O8 O 0.21103(10) 0.6346(2) 0.49945(19) 0.0295(7) Uani 0.50 1 d P . . O1 O 0.01170(13) 0.2997(3) 0.3470(2) 0.0418(9) Uani 1 1 d . . . N1 N 0.19095(13) 0.4085(3) 0.4370(2) 0.0219(8) Uani 1 1 d . . . N1A N 0.17843(15) 0.3102(3) 0.4062(3) 0.0351(10) Uani 1 1 d . . . H1A1 H 0.1542 0.2763 0.4041 0.042 Uiso 1 1 d R . . N2 N 0.12794(12) 0.6020(3) 0.5372(2) 0.0191(7) Uani 1 1 d . . . N2A N 0.14438(14) 0.6978(3) 0.5696(3) 0.0312(9) Uani 1 1 d . . . H2A1 H 0.1658 0.7318 0.5625 0.037 Uiso 1 1 d R . . N3 N 0.11111(12) 0.5507(3) 0.3546(2) 0.0212(8) Uani 1 1 d . . . N3A N 0.12281(12) 0.6254(3) 0.3120(2) 0.0235(8) Uani 1 1 d . . . H3A1 H 0.1486 0.6646 0.3388 0.028 Uiso 1 1 d R . . N4 N 0.20328(13) 0.4513(3) 0.6135(3) 0.0233(8) Uani 1 1 d . . . N4A N 0.19468(12) 0.3698(3) 0.6539(2) 0.0233(8) Uani 1 1 d . . . H4A1 H 0.1701 0.3273 0.6265 0.028 Uiso 1 1 d R . . N5 N -0.06110(14) 0.0119(3) 0.3744(3) 0.0248(9) Uani 1 1 d . . . N5A N -0.09835(12) -0.0578(3) 0.3405(3) 0.0280(9) Uani 1 1 d . . . H5A1 H -0.1014 -0.1072 0.3722 0.034 Uiso 1 1 d R . . N6 N 0.02986(12) -0.0910(3) 0.4434(3) 0.0249(8) Uani 1 1 d . . . N6A N 0.02023(13) -0.1932(3) 0.4220(3) 0.0270(9) Uani 1 1 d . . . H6A1 H 0.0031 -0.2329 0.4365 0.032 Uiso 1 1 d R . . C1 C 0.2094(2) 0.2697(4) 0.3784(4) 0.0442(15) Uani 1 1 d . . . H11 H 0.2079 0.2029 0.3539 0.053 Uiso 1 1 calc R . . C2 C 0.2419(2) 0.3457(5) 0.3938(4) 0.0463(15) Uani 1 1 d . . . H21 H 0.2676 0.3422 0.3817 0.056 Uiso 1 1 calc R . . C3 C 0.23071(15) 0.4306(4) 0.4308(3) 0.0253(10) Uani 1 1 d . . . H31 H 0.2482 0.4941 0.4489 0.030 Uiso 1 1 calc R . . C4 C 0.12341(18) 0.7358(4) 0.6187(4) 0.0354(13) Uani 1 1 d . . . H41 H 0.1291 0.8011 0.6480 0.043 Uiso 1 1 calc R . . C5 C 0.09280(10) 0.6578(3) 0.6153(2) 0.0361(13) Uani 1 1 d . . . H51 H 0.0734 0.6590 0.6423 0.043 Uiso 1 1 calc R . . C6 C 0.09590(10) 0.5764(3) 0.5638(2) 0.0205(9) Uani 1 1 d R . . H61 H 0.0783 0.5131 0.5499 0.025 Uiso 1 1 calc R . . C7 C 0.08935(15) 0.6327(4) 0.2238(3) 0.0254(10) Uani 1 1 d . . . H71 H 0.0900 0.6791 0.1817 0.030 Uiso 1 1 calc R . . C8 C 0.05321(16) 0.5583(4) 0.2061(3) 0.0266(10) Uani 1 1 d . . . H81 H 0.0249 0.5442 0.1503 0.032 Uiso 1 1 calc R . . C9 C 0.06846(17) 0.5089(4) 0.2899(3) 0.0252(10) Uani 1 1 d . . . H91 H 0.0514 0.4548 0.2994 0.030 Uiso 1 1 calc R . . C10 C 0.22932(15) 0.3611(4) 0.7420(3) 0.0272(10) Uani 1 1 d . . . H101 H 0.2306 0.3101 0.7829 0.033 Uiso 1 1 calc R . . C11 C 0.26221(17) 0.4403(4) 0.7608(3) 0.0316(11) Uani 1 1 d . . . H111 H 0.2907 0.4541 0.8164 0.038 Uiso 1 1 calc R . . C12 C 0.24429(17) 0.4974(4) 0.6783(3) 0.0271(11) Uani 1 1 d . . . H121 H 0.2588 0.5577 0.6706 0.032 Uiso 1 1 calc R . . C13 C -0.06934(17) 0.0739(4) 0.3049(3) 0.0268(10) Uani 1 1 d . . . H131 H -0.0489 0.1292 0.3083 0.032 Uiso 1 1 calc R . . C14 C -0.11363(17) 0.0439(4) 0.2248(3) 0.0332(11) Uani 1 1 d . . . H141 H -0.1283 0.0750 0.1671 0.040 Uiso 1 1 calc R . . C15 C -0.12977(16) -0.0423(4) 0.2527(3) 0.0321(11) Uani 1 1 d . . . H151 H -0.1579 -0.0824 0.2160 0.039 Uiso 1 1 calc R . . C16 C 0.04211(18) -0.2283(4) 0.3748(4) 0.0324(12) Uani 1 1 d . . . H161 H 0.0408 -0.2964 0.3525 0.039 Uiso 1 1 calc R . . C17 C 0.0660(2) -0.1440(5) 0.3671(4) 0.0465(15) Uani 1 1 d . . . H171 H 0.0847 -0.1424 0.3388 0.056 Uiso 1 1 calc R . . C18 C 0.05727(17) -0.0602(4) 0.4096(4) 0.0335(12) Uani 1 1 d . . . H181 H 0.0692 0.0083 0.4136 0.040 Uiso 1 1 calc R . . 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 Mo1 0.0242(3) 0.0137(3) 0.0195(3) -0.00336(14) 0.0147(2) -0.00713(13) Mo2 0.0259(4) 0.0208(3) 0.0309(4) -0.0081(2) 0.0197(3) -0.0122(2) Cu1 0.0263(4) 0.0189(3) 0.0147(4) 0.0039(2) 0.0122(3) 0.0087(2) Cu2 0.0310(5) 0.0237(5) 0.0212(5) -0.0062(3) 0.0133(4) 0.0043(3) F1 0.0493(17) 0.069(2) 0.0261(16) -0.0088(15) 0.0152(14) 0.0340(16) F2 0.0291(15) 0.0291(16) 0.0299(17) 0.0085(12) 0.0123(13) 0.0046(11) F3 0.082(2) 0.081(3) 0.057(2) -0.016(2) 0.043(2) 0.030(2) F4 0.0476(18) 0.0298(17) 0.0259(17) 0.0100(14) 0.0237(14) 0.0106(14) O4 0.0476(18) 0.0298(17) 0.0259(17) 0.0100(14) 0.0237(14) 0.0106(14) F5 0.0309(16) 0.0370(19) 0.0337(18) -0.0134(15) 0.0154(14) -0.0015(13) O5 0.0309(16) 0.0370(19) 0.0337(18) -0.0134(15) 0.0154(14) -0.0015(13) F6 0.0446(18) 0.0403(19) 0.0200(16) 0.0042(13) 0.0146(14) 0.0162(13) O6 0.0446(18) 0.0403(19) 0.0200(16) 0.0042(13) 0.0146(14) 0.0162(13) F7 0.0503(18) 0.056(2) 0.0258(16) 0.0014(14) 0.0177(14) 0.0342(16) O7 0.0503(18) 0.056(2) 0.0258(16) 0.0014(14) 0.0177(14) 0.0342(16) F8 0.0396(16) 0.0300(18) 0.0231(15) 0.0083(13) 0.0189(13) 0.0146(13) O8 0.0396(16) 0.0300(18) 0.0231(15) 0.0083(13) 0.0189(13) 0.0146(13) O1 0.046(2) 0.053(2) 0.0196(18) -0.0009(17) 0.0122(16) 0.0034(18) N1 0.0311(19) 0.0143(19) 0.027(2) 0.0049(15) 0.0194(16) 0.0069(15) N1A 0.041(2) 0.025(2) 0.044(3) -0.003(2) 0.024(2) -0.0026(18) N2 0.0205(17) 0.0197(19) 0.0182(18) 0.0014(15) 0.0107(15) 0.0016(14) N2A 0.036(2) 0.024(2) 0.041(3) -0.0019(19) 0.0244(19) -0.0032(17) N3 0.0248(19) 0.021(2) 0.018(2) -0.0001(16) 0.0109(16) 0.0085(15) N3A 0.0243(19) 0.024(2) 0.023(2) 0.0037(16) 0.0125(16) 0.0020(15) N4 0.0236(19) 0.023(2) 0.025(2) 0.0071(17) 0.0136(17) 0.0086(15) N4A 0.0252(18) 0.028(2) 0.0189(19) 0.0064(16) 0.0130(16) 0.0055(15) N5 0.025(2) 0.019(2) 0.027(2) -0.0027(16) 0.0110(18) 0.0052(15) N5A 0.028(2) 0.026(2) 0.031(2) 0.0037(17) 0.0155(17) 0.0025(16) N6 0.0313(19) 0.021(2) 0.026(2) -0.0053(16) 0.0171(17) -0.0038(15) N6A 0.029(2) 0.023(2) 0.031(2) -0.0011(18) 0.0167(17) -0.0044(16) C1 0.070(4) 0.026(3) 0.047(4) -0.004(2) 0.037(3) 0.009(3) C2 0.053(3) 0.052(4) 0.061(4) 0.022(3) 0.049(3) 0.029(3) C3 0.025(2) 0.024(2) 0.035(3) 0.000(2) 0.022(2) -0.0078(18) C4 0.032(3) 0.032(3) 0.035(3) -0.015(2) 0.012(2) 0.003(2) C5 0.036(3) 0.052(3) 0.036(3) 0.013(3) 0.029(2) 0.018(2) C6 0.018(2) 0.020(2) 0.027(2) 0.0067(18) 0.0133(18) -0.0026(16) C7 0.030(2) 0.029(3) 0.019(2) 0.0052(19) 0.014(2) 0.0093(19) C8 0.025(2) 0.030(3) 0.017(2) 0.003(2) 0.0058(19) 0.0069(19) C9 0.028(3) 0.027(3) 0.023(3) 0.0005(19) 0.015(2) -0.0019(18) C10 0.031(2) 0.033(3) 0.021(2) 0.010(2) 0.016(2) 0.007(2) C11 0.035(3) 0.035(3) 0.017(2) 0.005(2) 0.008(2) 0.007(2) C12 0.028(3) 0.027(3) 0.021(3) 0.0086(19) 0.009(2) 0.0040(18) C13 0.040(3) 0.017(2) 0.025(2) -0.0064(19) 0.017(2) -0.0011(19) C14 0.040(3) 0.032(3) 0.028(3) 0.004(2) 0.017(2) 0.003(2) C15 0.027(2) 0.033(3) 0.026(3) 0.002(2) 0.006(2) -0.001(2) C16 0.039(3) 0.025(3) 0.034(3) -0.011(2) 0.019(2) 0.003(2) C17 0.056(3) 0.051(4) 0.060(4) 0.003(3) 0.049(3) 0.006(3) C18 0.047(3) 0.018(2) 0.050(3) -0.001(2) 0.036(3) -0.012(2) _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 Mo1 O1 1.679(3) . ? Mo1 F4 1.891(3) . ? Mo1 F5 1.892(3) . ? Mo1 F3 1.910(3) . ? Mo1 F1 1.911(3) . ? Mo1 F2 2.122(3) . ? Mo2 F6 1.880(3) . ? Mo2 O6 1.880(3) 7_566 ? Mo2 F6 1.880(3) 7_566 ? Mo2 F7 1.891(3) . ? Mo2 O7 1.891(3) 7_566 ? Mo2 F7 1.891(3) 7_566 ? Mo2 O8 1.899(3) 7_566 ? Mo2 F8 1.899(3) 7_566 ? Mo2 F8 1.899(3) . ? Cu1 N1 2.007(3) . ? Cu1 N2 2.017(3) . ? Cu1 N4 2.020(4) . ? Cu1 N3 2.020(4) . ? Cu1 F4 2.216(3) . ? Cu1 F8 2.289(3) . ? Cu2 N6 2.008(4) . ? Cu2 N6 2.008(4) 5_556 ? Cu2 N5 2.023(4) . ? Cu2 N5 2.023(4) 5_556 ? Cu2 O5 2.244(3) 5_556 ? Cu2 F5 2.244(3) 5_556 ? Cu2 F5 2.244(3) 5_556 ? Cu2 F5 2.244(3) . ? N1 N1A 1.324(5) . ? N1 C3 1.335(5) . ? N1A C1 1.378(7) . ? N1A H1A1 0.8580 . ? N2 N2A 1.319(5) . ? N2 C6 1.335(4) . ? N2A C4 1.383(6) . ? N2A H2A1 0.8578 . ? N3 C9 1.336(6) . ? N3 N3A 1.346(5) . ? N3A C7 1.326(6) . ? N3A H3A1 0.8576 . ? N4 C12 1.331(6) . ? N4 N4A 1.337(5) . ? N4A C10 1.334(6) . ? N4A H4A1 0.8576 . ? N5 C13 1.325(6) . ? N5 N5A 1.339(5) . ? N5A C15 1.318(6) . ? N5A H5A1 0.8577 . ? N6 C18 1.313(6) . ? N6 N6A 1.330(5) . ? N6A C16 1.367(6) . ? N6A H6A1 0.8577 . ? C1 C2 1.325(8) . ? C1 H11 0.9300 . ? C2 C3 1.374(7) . ? C2 H21 0.9300 . ? C3 H31 0.9300 . ? C4 C5 1.356(6) . ? C4 H41 0.9300 . ? C5 C6 1.3828 . ? C5 H51 0.9300 . ? C6 H61 0.9300 . ? C7 C8 1.384(6) . ? C7 H71 0.9300 . ? C8 C9 1.395(6) . ? C8 H81 0.9300 . ? C9 H91 0.9300 . ? C10 C11 1.354(7) . ? C10 H101 0.9300 . ? C11 C12 1.411(7) . ? C11 H111 0.9300 . ? C12 H121 0.9300 . ? C13 C14 1.417(7) . ? C13 H131 0.9300 . ? C14 C15 1.380(7) . ? C14 H141 0.9300 . ? C15 H151 0.9300 . ? C16 C17 1.344(7) . ? C16 H161 0.9300 . ? C17 C18 1.381(7) . ? C17 H171 0.9300 . ? C18 H181 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 Mo1 F4 99.10(16) . . ? O1 Mo1 F5 98.67(16) . . ? F4 Mo1 F5 162.23(12) . . ? O1 Mo1 F3 98.68(17) . . ? F4 Mo1 F3 87.69(16) . . ? F5 Mo1 F3 89.26(16) . . ? O1 Mo1 F1 95.53(15) . . ? F4 Mo1 F1 89.52(14) . . ? F5 Mo1 F1 89.16(14) . . ? F3 Mo1 F1 165.78(15) . . ? O1 Mo1 F2 178.10(15) . . ? F4 Mo1 F2 81.10(11) . . ? F5 Mo1 F2 81.16(12) . . ? F3 Mo1 F2 83.21(14) . . ? F1 Mo1 F2 82.58(12) . . ? F6 Mo2 O6 180.000(1) . 7_566 ? F6 Mo2 F6 180.000(1) . 7_566 ? O6 Mo2 F6 0.0(2) 7_566 7_566 ? F6 Mo2 F7 89.70(12) . . ? O6 Mo2 F7 90.30(12) 7_566 . ? F6 Mo2 F7 90.30(12) 7_566 . ? F6 Mo2 O7 90.30(12) . 7_566 ? O6 Mo2 O7 89.70(12) 7_566 7_566 ? F6 Mo2 O7 89.70(12) 7_566 7_566 ? F7 Mo2 O7 180.00(16) . 7_566 ? F6 Mo2 F7 90.30(12) . 7_566 ? O6 Mo2 F7 89.70(12) 7_566 7_566 ? F6 Mo2 F7 89.70(12) 7_566 7_566 ? F7 Mo2 F7 180.00(16) . 7_566 ? O7 Mo2 F7 0.00(16) 7_566 7_566 ? F6 Mo2 O8 91.52(13) . 7_566 ? O6 Mo2 O8 88.48(13) 7_566 7_566 ? F6 Mo2 O8 88.48(13) 7_566 7_566 ? F7 Mo2 O8 89.99(15) . 7_566 ? O7 Mo2 O8 90.01(15) 7_566 7_566 ? F7 Mo2 O8 90.01(15) 7_566 7_566 ? F6 Mo2 F8 91.52(13) . 7_566 ? O6 Mo2 F8 88.48(13) 7_566 7_566 ? F6 Mo2 F8 88.48(13) 7_566 7_566 ? F7 Mo2 F8 89.99(15) . 7_566 ? O7 Mo2 F8 90.01(15) 7_566 7_566 ? F7 Mo2 F8 90.01(15) 7_566 7_566 ? O8 Mo2 F8 0.0(2) 7_566 7_566 ? F6 Mo2 F8 88.48(13) . . ? O6 Mo2 F8 91.52(13) 7_566 . ? F6 Mo2 F8 91.52(13) 7_566 . ? F7 Mo2 F8 90.01(15) . . ? O7 Mo2 F8 89.99(15) 7_566 . ? F7 Mo2 F8 89.99(15) 7_566 . ? O8 Mo2 F8 180.00(15) 7_566 . ? F8 Mo2 F8 180.00(15) 7_566 . ? N1 Cu1 N2 176.27(13) . . ? N1 Cu1 N4 90.75(14) . . ? N2 Cu1 N4 87.39(14) . . ? N1 Cu1 N3 88.58(14) . . ? N2 Cu1 N3 93.33(14) . . ? N4 Cu1 N3 178.78(14) . . ? N1 Cu1 F4 92.47(12) . . ? N2 Cu1 F4 90.78(12) . . ? N4 Cu1 F4 90.47(13) . . ? N3 Cu1 F4 88.54(13) . . ? N1 Cu1 F8 88.17(13) . . ? N2 Cu1 F8 88.66(12) . . ? N4 Cu1 F8 91.81(13) . . ? N3 Cu1 F8 89.19(13) . . ? F4 Cu1 F8 177.63(10) . . ? N6 Cu2 N6 180.00(16) . 5_556 ? N6 Cu2 N5 87.94(15) . . ? N6 Cu2 N5 92.06(15) 5_556 . ? N6 Cu2 N5 92.06(15) . 5_556 ? N6 Cu2 N5 87.94(15) 5_556 5_556 ? N5 Cu2 N5 180.0(2) . 5_556 ? N6 Cu2 O5 89.75(13) . 5_556 ? N6 Cu2 O5 90.25(13) 5_556 5_556 ? N5 Cu2 O5 89.69(13) . 5_556 ? N5 Cu2 O5 90.31(13) 5_556 5_556 ? N6 Cu2 F5 89.75(13) . 5_556 ? N6 Cu2 F5 90.25(13) 5_556 5_556 ? N5 Cu2 F5 89.69(13) . 5_556 ? N5 Cu2 F5 90.31(13) 5_556 5_556 ? O5 Cu2 F5 0.00(16) 5_556 5_556 ? N6 Cu2 F5 89.75(13) . 5_556 ? N6 Cu2 F5 90.25(13) 5_556 5_556 ? N5 Cu2 F5 89.69(13) . 5_556 ? N5 Cu2 F5 90.31(13) 5_556 5_556 ? O5 Cu2 F5 0.00(16) 5_556 5_556 ? F5 Cu2 F5 0.00(16) 5_556 5_556 ? N6 Cu2 F5 90.25(13) . . ? N6 Cu2 F5 89.75(13) 5_556 . ? N5 Cu2 F5 90.31(13) . . ? N5 Cu2 F5 89.69(13) 5_556 . ? O5 Cu2 F5 180.00(13) 5_556 . ? F5 Cu2 F5 180.00(13) 5_556 . ? F5 Cu2 F5 180.00(13) 5_556 . ? Mo1 F4 Cu1 177.43(15) . . ? Mo1 F5 Cu2 179.32(19) . . ? Mo2 F8 Cu1 173.91(15) . . ? N1A N1 C3 105.5(4) . . ? N1A N1 Cu1 126.9(3) . . ? C3 N1 Cu1 127.6(3) . . ? N1 N1A C1 111.2(4) . . ? N1 N1A H1A1 124.2 . . ? C1 N1A H1A1 124.6 . . ? N2A N2 C6 106.5(3) . . ? N2A N2 Cu1 125.6(3) . . ? C6 N2 Cu1 126.4(3) . . ? N2 N2A C4 111.3(4) . . ? N2 N2A H2A1 124.7 . . ? C4 N2A H2A1 124.1 . . ? C9 N3 N3A 105.6(4) . . ? C9 N3 Cu1 130.1(3) . . ? N3A N3 Cu1 123.5(3) . . ? C7 N3A N3 112.2(4) . . ? C7 N3A H3A1 123.6 . . ? N3 N3A H3A1 124.2 . . ? C12 N4 N4A 106.0(4) . . ? C12 N4 Cu1 128.0(3) . . ? N4A N4 Cu1 125.6(3) . . ? C10 N4A N4 112.0(4) . . ? C10 N4A H4A1 123.6 . . ? N4 N4A H4A1 124.3 . . ? C13 N5 N5A 105.7(4) . . ? C13 N5 Cu2 129.2(3) . . ? N5A N5 Cu2 124.0(3) . . ? C15 N5A N5 112.2(4) . . ? C15 N5A H5A1 123.8 . . ? N5 N5A H5A1 123.9 . . ? C18 N6 N6A 106.1(4) . . ? C18 N6 Cu2 127.5(3) . . ? N6A N6 Cu2 125.9(3) . . ? N6 N6A C16 111.1(4) . . ? N6 N6A H6A1 125.2 . . ? C16 N6A H6A1 123.7 . . ? C2 C1 N1A 105.8(4) . . ? C2 C1 H11 127.1 . . ? N1A C1 H11 127.1 . . ? C1 C2 C3 107.7(4) . . ? C1 C2 H21 126.1 . . ? C3 C2 H21 126.1 . . ? N1 C3 C2 109.8(4) . . ? N1 C3 H31 125.1 . . ? C2 C3 H31 125.1 . . ? C5 C4 N2A 105.5(4) . . ? C5 C4 H41 127.3 . . ? N2A C4 H41 127.3 . . ? C4 C5 C6 106.9(3) . . ? C4 C5 H51 126.6 . . ? C6 C5 H51 126.6 . . ? N2 C6 C5 109.9(2) . . ? N2 C6 H61 125.1 . . ? C5 C6 H61 125.1 . . ? N3A C7 C8 106.9(4) . . ? N3A C7 H71 126.5 . . ? C8 C7 H71 126.5 . . ? C7 C8 C9 105.2(4) . . ? C7 C8 H81 127.4 . . ? C9 C8 H81 127.4 . . ? N3 C9 C8 110.1(4) . . ? N3 C9 H91 125.0 . . ? C8 C9 H91 125.0 . . ? N4A C10 C11 107.1(4) . . ? N4A C10 H101 126.4 . . ? C11 C10 H101 126.4 . . ? C10 C11 C12 105.7(4) . . ? C10 C11 H111 127.2 . . ? C12 C11 H111 127.2 . . ? N4 C12 C11 109.2(4) . . ? N4 C12 H121 125.4 . . ? C11 C12 H121 125.4 . . ? N5 C13 C14 110.4(4) . . ? N5 C13 H131 124.8 . . ? C14 C13 H131 124.8 . . ? C15 C14 C13 103.6(4) . . ? C15 C14 H141 128.2 . . ? C13 C14 H141 128.2 . . ? N5A C15 C14 108.0(4) . . ? N5A C15 H151 126.0 . . ? C14 C15 H151 126.0 . . ? C17 C16 N6A 105.7(4) . . ? C17 C16 H161 127.1 . . ? N6A C16 H161 127.1 . . ? C16 C17 C18 106.7(4) . . ? C16 C17 H171 126.7 . . ? C18 C17 H171 126.7 . . ? N6 C18 C17 110.4(4) . . ? N6 C18 H181 124.8 . . ? C17 C18 H181 124.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A1 F3 0.86 2.31 3.163(6) 174.0 . N1A H1A1 F4 0.86 2.64 3.118(5) 116.4 . N3A H3A1 F6 0.86 2.02 2.866(5) 167.8 . N3A H3A1 F8 0.86 2.45 2.976(5) 120.6 . N4A H4A1 F2 0.86 1.88 2.727(5) 171.5 . N4A H4A1 F4 0.86 2.55 3.035(5) 116.8 . N5A H5A1 F2 0.86 1.90 2.742(5) 167.0 5_556 N5A H5A1 F5 0.86 2.47 2.985(5) 119.2 5_556 N6A H6A1 F1 0.86 2.31 3.163(5) 174.8 5_556 N6A H6A1 F5 0.86 2.55 3.027(5) 116.4 5_556 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.065 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.106 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 715744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 Cu F5 N8 Nb O' _chemical_formula_sum 'C12 H16 Cu F5 N8 Nb O' _chemical_formula_weight 539.79 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 10.310(2) _cell_length_b 12.941(3) _cell_length_c 15.038(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.793(7) _cell_angle_gamma 90.00 _cell_volume 1987.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 6756 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6756 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.39 _reflns_number_total 1967 _reflns_number_gt 1551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0388P)^2^+5.6166P] 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 1967 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 Nb1 Nb 0.0000 0.5000 0.0000 0.0417(2) Uani 1 2 d S . . Cu1 Cu -0.2500 0.7500 0.0000 0.0424(3) Uani 1 2 d S . . F1 F -0.1131(3) 0.6185(2) -0.00351(18) 0.0522(8) Uani 0.50 1 d P . . O1 O -0.1131(3) 0.6185(2) -0.00351(18) 0.0522(8) Uani 0.50 1 d P . . F2 F -0.0217(3) 0.4811(2) 0.12431(18) 0.0615(8) Uani 1 1 d . . . F3 F 0.1515(3) 0.5850(3) 0.0360(2) 0.0765(10) Uani 1 1 d . . . N1 N -0.2728(4) 0.7134(3) 0.1280(2) 0.0423(9) Uani 1 1 d . . . N2 N -0.2018(4) 0.6383(3) 0.1737(2) 0.0509(10) Uani 1 1 d . . . H2A H -0.1480 0.5992 0.1504 0.061 Uiso 1 1 calc R . . N3 N -0.0970(4) 0.8425(3) 0.0493(2) 0.0398(9) Uani 1 1 d . . . N4 N -0.1075(4) 0.9385(3) 0.0797(3) 0.0534(10) Uani 1 1 d . . . H4A H -0.1797 0.9726 0.0756 0.064 Uiso 1 1 calc R . . C1 C -0.2232(6) 0.6310(5) 0.2579(3) 0.0641(15) Uani 1 1 d . . . H11 H -0.1849 0.5840 0.3004 0.077 Uiso 1 1 calc R . . C2 C -0.3120(6) 0.7054(5) 0.2705(3) 0.0647(16) Uani 1 1 d . . . H21 H -0.3471 0.7195 0.3230 0.078 Uiso 1 1 calc R . . C3 C -0.3402(5) 0.7572(4) 0.1866(3) 0.0562(13) Uani 1 1 d . . . H31 H -0.3969 0.8129 0.1748 0.067 Uiso 1 1 calc R . . C4 C 0.0093(4) 0.9751(3) 0.1176(3) 0.0593(15) Uani 1 1 d . . . H41 H 0.0263 1.0397 0.1436 0.071 Uiso 1 1 calc R . . C5 C 0.0965(4) 0.8991(3) 0.1101(3) 0.0747(18) Uani 1 1 d R . . H51 H 0.1859 0.9009 0.1299 0.090 Uiso 1 1 calc R . . C6 C 0.0271(5) 0.8186(4) 0.0675(3) 0.0504(12) Uani 1 1 d . . . H61 H 0.0633 0.7557 0.0536 0.060 Uiso 1 1 calc R . . 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 Nb1 0.0419(3) 0.0380(4) 0.0422(4) -0.0091(2) -0.0048(2) 0.0046(3) Cu1 0.0580(5) 0.0399(5) 0.0272(4) -0.0005(3) -0.0010(3) -0.0183(4) F1 0.0605(19) 0.0476(19) 0.0468(17) -0.0050(14) 0.0007(14) -0.0054(15) O1 0.0605(19) 0.0476(19) 0.0468(17) -0.0050(14) 0.0007(14) -0.0054(15) F2 0.074(2) 0.073(2) 0.0372(16) -0.0048(13) 0.0057(13) -0.0043(16) F3 0.077(2) 0.091(2) 0.0604(19) -0.0249(17) 0.0068(15) -0.0383(19) N1 0.053(2) 0.043(2) 0.031(2) 0.0007(17) 0.0040(17) -0.0121(19) N2 0.058(3) 0.056(3) 0.037(2) 0.0052(18) 0.0003(18) -0.013(2) N3 0.050(2) 0.032(2) 0.037(2) -0.0024(15) 0.0025(16) -0.0050(18) N4 0.050(2) 0.044(3) 0.065(3) -0.007(2) 0.002(2) 0.003(2) C1 0.068(4) 0.079(4) 0.043(3) 0.007(3) -0.003(2) -0.017(3) C2 0.077(4) 0.087(4) 0.033(3) -0.005(3) 0.019(3) -0.030(4) C3 0.060(3) 0.062(3) 0.048(3) -0.009(3) 0.012(2) -0.015(3) C4 0.073(4) 0.043(3) 0.057(3) -0.012(2) -0.009(3) -0.026(3) C5 0.042(3) 0.078(4) 0.098(5) 0.023(4) -0.013(3) -0.005(3) C6 0.045(3) 0.030(3) 0.077(3) -0.001(2) 0.009(2) 0.005(2) _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 Nb1 F1 1.923(3) . ? Nb1 O1 1.923(3) 5_565 ? Nb1 F1 1.923(3) 5_565 ? Nb1 F3 1.927(3) . ? Nb1 F3 1.927(3) 5_565 ? Nb1 F2 1.928(3) 5_565 ? Nb1 F2 1.928(3) . ? Cu1 N1 2.027(4) 7_465 ? Cu1 N1 2.027(4) . ? Cu1 N3 2.038(3) . ? Cu1 N3 2.038(3) 7_465 ? Cu1 O1 2.216(3) 7_465 ? Cu1 F1 2.216(3) 7_465 ? Cu1 F1 2.216(3) . ? N1 C3 1.321(6) . ? N1 N2 1.348(5) . ? N2 C1 1.317(6) . ? N2 H2A 0.8600 . ? N3 C6 1.309(6) . ? N3 N4 1.334(5) . ? N4 C4 1.347(5) . ? N4 H4A 0.8600 . ? C1 C2 1.360(8) . ? C1 H11 0.9300 . ? C2 C3 1.424(7) . ? C2 H21 0.9300 . ? C3 H31 0.9300 . ? C4 C5 1.3466 . ? C4 H41 0.9300 . ? C5 C6 1.373(6) . ? C5 H51 0.9300 . ? C6 H61 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 F1 Nb1 O1 180.0 . 5_565 ? F1 Nb1 F1 180.0 . 5_565 ? O1 Nb1 F1 0.00(10) 5_565 5_565 ? F1 Nb1 F3 91.02(14) . . ? O1 Nb1 F3 88.98(14) 5_565 . ? F1 Nb1 F3 88.98(14) 5_565 . ? F1 Nb1 F3 88.98(14) . 5_565 ? O1 Nb1 F3 91.02(14) 5_565 5_565 ? F1 Nb1 F3 91.02(14) 5_565 5_565 ? F3 Nb1 F3 180.0 . 5_565 ? F1 Nb1 F2 91.27(12) . 5_565 ? O1 Nb1 F2 88.73(12) 5_565 5_565 ? F1 Nb1 F2 88.73(12) 5_565 5_565 ? F3 Nb1 F2 90.19(13) . 5_565 ? F3 Nb1 F2 89.81(13) 5_565 5_565 ? F1 Nb1 F2 88.73(12) . . ? O1 Nb1 F2 91.27(12) 5_565 . ? F1 Nb1 F2 91.27(12) 5_565 . ? F3 Nb1 F2 89.81(13) . . ? F3 Nb1 F2 90.19(13) 5_565 . ? F2 Nb1 F2 180.0 5_565 . ? N1 Cu1 N1 180.000(1) 7_465 . ? N1 Cu1 N3 91.38(14) 7_465 . ? N1 Cu1 N3 88.62(14) . . ? N1 Cu1 N3 88.62(14) 7_465 7_465 ? N1 Cu1 N3 91.38(14) . 7_465 ? N3 Cu1 N3 180.0 . 7_465 ? N1 Cu1 O1 89.95(13) 7_465 7_465 ? N1 Cu1 O1 90.05(13) . 7_465 ? N3 Cu1 O1 90.26(13) . 7_465 ? N3 Cu1 O1 89.74(13) 7_465 7_465 ? N1 Cu1 F1 89.96(13) 7_465 7_465 ? N1 Cu1 F1 90.04(13) . 7_465 ? N3 Cu1 F1 90.26(13) . 7_465 ? N3 Cu1 F1 89.74(13) 7_465 7_465 ? O1 Cu1 F1 0.00(11) 7_465 7_465 ? N1 Cu1 F1 90.04(13) 7_465 . ? N1 Cu1 F1 89.96(13) . . ? N3 Cu1 F1 89.74(13) . . ? N3 Cu1 F1 90.26(13) 7_465 . ? O1 Cu1 F1 180.0 7_465 . ? F1 Cu1 F1 180.0 7_465 . ? Nb1 F1 Cu1 176.01(15) . . ? C3 N1 N2 105.5(4) . . ? C3 N1 Cu1 132.2(4) . . ? N2 N1 Cu1 121.9(3) . . ? C1 N2 N1 113.1(5) . . ? C1 N2 H2A 123.5 . . ? N1 N2 H2A 123.5 . . ? C6 N3 N4 105.7(4) . . ? C6 N3 Cu1 128.6(3) . . ? N4 N3 Cu1 125.2(3) . . ? N3 N4 C4 111.3(4) . . ? N3 N4 H4A 124.4 . . ? C4 N4 H4A 124.4 . . ? N2 C1 C2 106.7(5) . . ? N2 C1 H11 126.7 . . ? C2 C1 H11 126.7 . . ? C1 C2 C3 105.7(5) . . ? C1 C2 H21 127.2 . . ? C3 C2 H21 127.2 . . ? N1 C3 C2 109.1(5) . . ? N1 C3 H31 125.5 . . ? C2 C3 H31 125.5 . . ? N4 C4 C5 106.1(3) . . ? N4 C4 H41 127.0 . . ? C5 C4 H41 127.0 . . ? C4 C5 C6 106.4(3) . . ? C4 C5 H51 126.8 . . ? C6 C5 H51 126.8 . . ? N3 C6 C5 110.6(4) . . ? N3 C6 H61 124.7 . . ? C5 C6 H61 124.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A F2 0.86 2.08 2.917(6) 164.7 . N2 H2A F1 0.86 2.40 2.944(5) 121.4 . N4 H4A F3 0.86 2.29 3.124(6) 165.1 3_455 N4 H4A F1 0.86 2.55 3.042(5) 117.3 7_465 _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.406 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.097 #===end data_5 _database_code_depnum_ccdc_archive 'CCDC 715745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Cu2 F6 Mo N6 O2' _chemical_formula_sum 'C20 H18 Cu2 F6 Mo N6 O2' _chemical_formula_weight 711.44 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m ' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.399(4) _cell_length_b 17.160(6) _cell_length_c 7.441(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.708(8) _cell_angle_gamma 90.00 _cell_volume 1098.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3487 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.3 _exptl_crystal_description Platelet _exptl_crystal_colour Green _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 2.565 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3487 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.32 _reflns_number_total 1044 _reflns_number_gt 930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0586P)^2^+13.4738P] 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 SHELXL _refine_ls_extinction_coef 0.0013(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1044 _refine_ls_number_parameters 96 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.072 _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 Mo1 Mo 0.5000 0.0000 0.0000 0.0374(4) Uani 1 4 d S . . Cu1 Cu 0.32670(9) 0.0000 0.41145(12) 0.0160(3) Uani 1 2 d S . . F1 F 0.6556(5) 0.0000 0.2595(6) 0.0222(10) Uani 0.50 2 d SP . . F2 F 0.3438(5) 0.0000 0.0968(6) 0.0212(10) Uani 0.50 2 d SP . . F3 F 0.5000 0.1105(3) 0.0000 0.0328(11) Uani 1 2 d S . . F4 F 0.5000 0.0717(2) 0.5000 0.0203(9) Uani 1 2 d S . . O1 O 0.6556(5) 0.0000 0.2595(6) 0.0222(10) Uani 0.50 2 d SP . . O2 O 0.3438(5) 0.0000 0.0968(6) 0.0212(10) Uani 0.50 2 d SP . . N1 N 0.1668(5) 0.0837(2) 0.3260(6) 0.0158(9) Uani 1 1 d . . . N2 N -0.0462(10) 0.0000 0.240(3) 0.101(6) Uani 1 2 d SD . . H2A H -0.13(2) 0.0000 0.18(3) 0.122 Uiso 1 2 d SD . . C1 C 0.2173(6) 0.1578(3) 0.3315(9) 0.0260(12) Uani 1 1 d . . . H11 H 0.3237 0.1664 0.3772 0.031 Uiso 1 1 calc R . . C2 C 0.1208(6) 0.2206(3) 0.2738(8) 0.0271(13) Uani 1 1 d . . . H21 H 0.1607 0.2706 0.2800 0.033 Uiso 1 1 calc R . . C3 C -0.0378(6) 0.2086(3) 0.2059(8) 0.0227(11) Uani 1 1 d . . . H31 H -0.1066 0.2503 0.1649 0.027 Uiso 1 1 calc R . . C4 C -0.0910(6) 0.1346(4) 0.2004(11) 0.0449(19) Uani 1 1 d . . . H41 H -0.1969 0.1250 0.1582 0.054 Uiso 1 1 calc R . . C5 C 0.0137(7) 0.0743(3) 0.2579(11) 0.0355(15) 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 Mo1 0.0111(5) 0.0166(5) 0.0635(8) 0.000 -0.0070(5) 0.000 Cu1 0.0070(5) 0.0178(5) 0.0204(5) 0.000 0.0026(4) 0.000 F1 0.014(2) 0.036(3) 0.014(2) 0.000 0.0035(18) 0.000 F2 0.017(2) 0.033(3) 0.014(2) 0.000 0.0067(18) 0.000 F3 0.025(2) 0.019(2) 0.050(3) 0.000 0.011(2) 0.000 F4 0.014(2) 0.021(2) 0.024(2) 0.000 0.0058(17) 0.000 O1 0.014(2) 0.036(3) 0.014(2) 0.000 0.0035(18) 0.000 O2 0.017(2) 0.033(3) 0.014(2) 0.000 0.0067(18) 0.000 N1 0.011(2) 0.019(2) 0.019(2) 0.0020(17) 0.0074(16) -0.0003(17) N2 0.010(4) 0.020(4) 0.254(18) 0.000 0.031(7) 0.000 C1 0.014(3) 0.023(3) 0.039(3) 0.004(2) 0.009(2) -0.002(2) C2 0.022(3) 0.018(3) 0.039(3) -0.001(2) 0.011(3) 0.001(2) C3 0.018(3) 0.018(3) 0.028(3) -0.003(2) 0.006(2) 0.006(2) C4 0.006(3) 0.032(4) 0.085(5) -0.003(3) 0.006(3) 0.003(2) C5 0.013(3) 0.019(3) 0.068(4) -0.005(3) 0.010(3) -0.004(2) _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 Mo1 F2 1.877(4) . ? Mo1 O2 1.877(4) 5_655 ? Mo1 F2 1.877(4) 5_655 ? Mo1 O1 1.897(4) 5_655 ? Mo1 F1 1.897(4) 5_655 ? Mo1 F1 1.897(4) . ? Mo1 F3 1.896(4) 5_655 ? Mo1 F3 1.896(4) . ? Cu1 F4 1.934(3) . ? Cu1 F4 1.934(3) 5_656 ? Cu1 N1 1.989(4) 6 ? Cu1 N1 1.989(4) . ? Cu1 O1 2.386(5) 5_656 ? Cu1 F1 2.386(5) 5_656 ? Cu1 F2 2.410(4) . ? Cu1 Cu1 2.983(2) 5_656 ? F1 Cu1 2.386(5) 5_656 ? F4 Cu1 1.934(3) 5_656 ? N1 C5 1.330(7) . ? N1 C1 1.353(7) . ? N2 C5 1.379(6) . ? N2 C5 1.379(6) 6 ? N2 H2A 0.73(18) . ? C1 C2 1.361(8) . ? C1 H11 0.9300 . ? C2 C3 1.384(8) . ? C2 H21 0.9300 . ? C3 C4 1.359(9) . ? C3 H31 0.9300 . ? C4 C5 1.372(9) . ? C4 H41 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 F2 Mo1 O2 180.00(19) . 5_655 ? F2 Mo1 F2 180.00(19) . 5_655 ? O2 Mo1 F2 0.00(19) 5_655 5_655 ? F2 Mo1 O1 89.36(19) . 5_655 ? O2 Mo1 O1 90.64(19) 5_655 5_655 ? F2 Mo1 O1 90.64(19) 5_655 5_655 ? F2 Mo1 F1 89.36(19) . 5_655 ? O2 Mo1 F1 90.64(19) 5_655 5_655 ? F2 Mo1 F1 90.64(19) 5_655 5_655 ? O1 Mo1 F1 0.0(2) 5_655 5_655 ? F2 Mo1 F1 90.64(19) . . ? O2 Mo1 F1 89.36(19) 5_655 . ? F2 Mo1 F1 89.36(19) 5_655 . ? O1 Mo1 F1 180.0 5_655 . ? F1 Mo1 F1 180.0 5_655 . ? F2 Mo1 F3 90.0 . 5_655 ? O2 Mo1 F3 90.0 5_655 5_655 ? F2 Mo1 F3 90.0 5_655 5_655 ? O1 Mo1 F3 90.0 5_655 5_655 ? F1 Mo1 F3 90.0 5_655 5_655 ? F1 Mo1 F3 90.0 . 5_655 ? F2 Mo1 F3 90.0 . . ? O2 Mo1 F3 90.0 5_655 . ? F2 Mo1 F3 90.0 5_655 . ? O1 Mo1 F3 90.0 5_655 . ? F1 Mo1 F3 90.0 5_655 . ? F1 Mo1 F3 90.0 . . ? F3 Mo1 F3 180.0 5_655 . ? F4 Cu1 F4 79.07(19) . 5_656 ? F4 Cu1 N1 173.25(15) . 6 ? F4 Cu1 N1 94.23(16) 5_656 6 ? F4 Cu1 N1 94.23(16) . . ? F4 Cu1 N1 173.25(15) 5_656 . ? N1 Cu1 N1 92.4(2) 6 . ? F4 Cu1 O1 87.06(9) . 5_656 ? F4 Cu1 O1 87.06(9) 5_656 5_656 ? N1 Cu1 O1 93.46(14) 6 5_656 ? N1 Cu1 O1 93.46(14) . 5_656 ? F4 Cu1 F1 87.06(9) . 5_656 ? F4 Cu1 F1 87.06(9) 5_656 5_656 ? N1 Cu1 F1 93.46(14) 6 5_656 ? N1 Cu1 F1 93.46(14) . 5_656 ? O1 Cu1 F1 0.0(2) 5_656 5_656 ? F4 Cu1 F2 87.41(9) . . ? F4 Cu1 F2 87.41(9) 5_656 . ? N1 Cu1 F2 91.50(14) 6 . ? N1 Cu1 F2 91.50(14) . . ? O1 Cu1 F2 172.83(15) 5_656 . ? F1 Cu1 F2 172.83(15) 5_656 . ? F4 Cu1 Cu1 39.53(9) . 5_656 ? F4 Cu1 Cu1 39.53(9) 5_656 5_656 ? N1 Cu1 Cu1 133.76(12) 6 5_656 ? N1 Cu1 Cu1 133.76(12) . 5_656 ? O1 Cu1 Cu1 86.19(11) 5_656 5_656 ? F1 Cu1 Cu1 86.19(11) 5_656 5_656 ? F2 Cu1 Cu1 86.64(11) . 5_656 ? Mo1 F1 Cu1 138.7(2) . 5_656 ? Mo1 F2 Cu1 137.8(2) . . ? Cu1 F4 Cu1 100.93(19) . 5_656 ? C5 N1 C1 116.0(4) . . ? C5 N1 Cu1 126.7(4) . . ? C1 N1 Cu1 117.3(3) . . ? C5 N2 C5 135.3(8) . 6 ? C5 N2 H2A 111(2) . . ? C5 N2 H2A 111(2) 6 . ? N1 C1 C2 123.6(5) . . ? N1 C1 H11 118.2 . . ? C2 C1 H11 118.2 . . ? C1 C2 C3 118.8(5) . . ? C1 C2 H21 120.6 . . ? C3 C2 H21 120.6 . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H31 120.7 . . ? C2 C3 H31 120.7 . . ? C3 C4 C5 119.0(5) . . ? C3 C4 H41 120.5 . . ? C5 C4 H41 120.5 . . ? N1 C5 C4 124.0(5) . . ? N1 C5 N2 119.1(6) . . ? C4 C5 N2 117.0(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A F2 0.73(18) 2.22(18) 2.910(14) 157(19) 5 N2 H2A F1 0.73(18) 2.33(18) 2.864(11) 131(18) 1_455 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.119 _refine_diff_density_min -2.196 _refine_diff_density_rms 0.165 #===end data_6 _database_code_depnum_ccdc_archive 'CCDC 715746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Cu2 F7 N6 Nb O ' _chemical_formula_sum 'C20 H18 Cu2 F7 N6 Nb O ' _chemical_formula_weight 711.41 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m ' _symmetry_space_group_name_Hall '-C 2y ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.469(6) _cell_length_b 17.173(10) _cell_length_c 7.419(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.57(2) _cell_angle_gamma 90.00 _cell_volume 1114.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3853 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 2.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3853 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.38 _reflns_number_total 1184 _reflns_number_gt 974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1144P)^2^+2.4201P] 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 SHELXL _refine_ls_extinction_coef 0.014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1184 _refine_ls_number_parameters 96 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.162 _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 Nb1 Nb 0.0000 0.0000 0.5000 0.0245(4) Uani 1 4 d S . . Cu1 Cu -0.17213(9) 0.0000 -0.07811(12) 0.0177(4) Uani 1 2 d S . . F2 F -0.1613(5) 0.0000 0.2414(6) 0.0263(11) Uani 0.75 2 d SP . . O2 O -0.1613(5) 0.0000 0.2414(6) 0.0263(11) Uani 0.25 2 d SP . . F3 F 0.1591(5) 0.0000 0.3983(6) 0.0292(12) Uani 0.75 2 d SP . . O3 O 0.1591(5) 0.0000 0.3983(6) 0.0292(12) Uani 0.25 2 d SP . . F1 F 0.0000 0.1119(3) 0.5000 0.0410(13) Uani 1 2 d S . . F4 F 0.0000 0.0719(3) 0.0000 0.0235(10) Uani 1 2 d S . . N1 N -0.3296(5) 0.0837(3) -0.1679(6) 0.0185(10) Uani 1 1 d . . . N2 N -0.5416(9) 0.0000 -0.2322(14) 0.042(2) Uani 1 2 d SD . . H2A H -0.632(6) 0.0000 -0.320(13) 0.063 Uiso 1 2 d SD . . C4 C -0.5839(5) 0.1364(4) -0.2906(8) 0.0267(15) Uani 1 1 d . . . H41 H -0.6885 0.1276 -0.3319 0.032 Uiso 1 1 calc R . . C1 C -0.2797(6) 0.1580(3) -0.1680(8) 0.0256(13) Uani 1 1 d . . . H11 H -0.1748 0.1663 -0.1249 0.031 Uiso 1 1 calc R . . C5 C -0.4818(6) 0.0732(3) -0.2289(8) 0.0224(12) Uani 1 1 d . . . C3 C -0.5315(6) 0.2095(3) -0.2905(8) 0.0261(12) Uani 1 1 d . . . H31 H -0.5989 0.2512 -0.3317 0.031 Uiso 1 1 calc R . . C2 C -0.3738(6) 0.2211(3) -0.2271(8) 0.0265(12) Uani 1 1 d . . . H21 H -0.3339 0.2707 -0.2253 0.032 Uiso 1 1 calc R . . 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 Nb1 0.0196(6) 0.0215(7) 0.0365(7) 0.000 0.0155(5) 0.000 Cu1 0.0099(6) 0.0225(6) 0.0183(6) 0.000 0.0028(4) 0.000 F2 0.014(2) 0.045(3) 0.022(2) 0.000 0.0089(18) 0.000 O2 0.014(2) 0.045(3) 0.022(2) 0.000 0.0089(18) 0.000 F3 0.018(2) 0.050(3) 0.018(2) 0.000 0.0047(18) 0.000 O3 0.018(2) 0.050(3) 0.018(2) 0.000 0.0047(18) 0.000 F1 0.037(3) 0.021(3) 0.056(3) 0.000 0.009(3) 0.000 F4 0.017(2) 0.024(2) 0.026(2) 0.000 0.0047(18) 0.000 N1 0.012(2) 0.024(2) 0.018(2) 0.0003(17) 0.0034(17) 0.0020(17) N2 0.020(4) 0.031(4) 0.063(5) 0.000 0.004(4) 0.000 C4 0.010(3) 0.030(4) 0.039(4) -0.001(2) 0.008(3) 0.003(2) C1 0.013(2) 0.027(3) 0.033(3) 0.004(2) 0.005(2) -0.002(2) C5 0.013(3) 0.024(3) 0.030(3) 0.000(2) 0.007(2) 0.000(2) C3 0.025(3) 0.024(3) 0.028(3) 0.000(2) 0.008(2) 0.005(2) C2 0.018(3) 0.024(3) 0.037(3) 0.001(2) 0.010(2) -0.001(2) _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 Nb1 F1 1.921(5) . ? Nb1 F1 1.921(5) 5_556 ? Nb1 F3 1.926(4) . ? Nb1 O3 1.926(4) 5_556 ? Nb1 F3 1.926(4) 5_556 ? Nb1 F2 1.940(4) 5_556 ? Nb1 O2 1.940(4) 5_556 ? Nb1 F2 1.940(4) . ? Cu1 F4 1.948(3) . ? Cu1 F4 1.948(3) 5 ? Cu1 N1 1.992(5) 6 ? Cu1 N1 1.992(5) . ? Cu1 F2 2.333(5) . ? Cu1 O3 2.426(5) 5 ? Cu1 Cu1 3.011(2) 5 ? F4 Cu1 1.948(3) 5 ? N1 C5 1.347(7) . ? N1 C1 1.362(7) . ? N2 C5 1.375(7) . ? N2 C5 1.375(7) 6 ? N2 H2A 0.86(2) . ? C4 C3 1.350(9) . ? C4 C5 1.406(8) . ? C4 H41 0.9300 . ? C1 C2 1.363(8) . ? C1 H11 0.9300 . ? C3 C2 1.397(7) . ? C3 H31 0.9300 . ? C2 H21 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 F1 Nb1 F1 180.0 . 5_556 ? F1 Nb1 F3 90.000(1) . . ? F1 Nb1 F3 90.0 5_556 . ? F1 Nb1 O3 90.0 . 5_556 ? F1 Nb1 O3 90.000(1) 5_556 5_556 ? F3 Nb1 O3 180.0 . 5_556 ? F1 Nb1 F3 90.0 . 5_556 ? F1 Nb1 F3 90.000(1) 5_556 5_556 ? F3 Nb1 F3 180.0 . 5_556 ? O3 Nb1 F3 0.00(10) 5_556 5_556 ? F1 Nb1 F2 90.000(1) . 5_556 ? F1 Nb1 F2 90.0 5_556 5_556 ? F3 Nb1 F2 87.14(18) . 5_556 ? O3 Nb1 F2 92.86(18) 5_556 5_556 ? F3 Nb1 F2 92.86(18) 5_556 5_556 ? F1 Nb1 O2 90.000(1) . 5_556 ? F1 Nb1 O2 90.0 5_556 5_556 ? F3 Nb1 O2 87.14(18) . 5_556 ? O3 Nb1 O2 92.86(18) 5_556 5_556 ? F3 Nb1 O2 92.86(18) 5_556 5_556 ? F2 Nb1 O2 0.0(2) 5_556 5_556 ? F1 Nb1 F2 90.0 . . ? F1 Nb1 F2 90.000(1) 5_556 . ? F3 Nb1 F2 92.86(18) . . ? O3 Nb1 F2 87.14(18) 5_556 . ? F3 Nb1 F2 87.14(18) 5_556 . ? F2 Nb1 F2 180.0 5_556 . ? O2 Nb1 F2 180.0 5_556 . ? F4 Cu1 F4 78.7(2) . 5 ? F4 Cu1 N1 172.06(16) . 6 ? F4 Cu1 N1 94.34(17) 5 6 ? F4 Cu1 N1 94.34(17) . . ? F4 Cu1 N1 172.06(16) 5 . ? N1 Cu1 N1 92.3(3) 6 . ? F4 Cu1 F2 89.56(9) . . ? F4 Cu1 F2 89.56(9) 5 . ? N1 Cu1 F2 94.31(14) 6 . ? N1 Cu1 F2 94.31(14) . . ? F4 Cu1 O3 86.57(8) . 5 ? F4 Cu1 O3 86.57(8) 5 5 ? N1 Cu1 O3 89.16(14) 6 5 ? N1 Cu1 O3 89.16(14) . 5 ? F2 Cu1 O3 174.98(15) . 5 ? F4 Cu1 Cu1 39.36(10) . 5 ? F4 Cu1 Cu1 39.36(10) 5 5 ? N1 Cu1 Cu1 133.59(13) 6 5 ? N1 Cu1 Cu1 133.59(13) . 5 ? F2 Cu1 Cu1 89.42(11) . 5 ? O3 Cu1 Cu1 85.56(11) 5 5 ? Nb1 F2 Cu1 135.7(2) . . ? Cu1 F4 Cu1 101.3(2) . 5 ? C5 N1 C1 116.8(4) . . ? C5 N1 Cu1 125.7(3) . . ? C1 N1 Cu1 117.4(3) . . ? C5 N2 C5 132.3(8) . 6 ? C5 N2 H2A 107(3) . . ? C5 N2 H2A 107(3) 6 . ? C3 C4 C5 120.7(5) . . ? C3 C4 H41 119.6 . . ? C5 C4 H41 119.6 . . ? N1 C1 C2 124.1(5) . . ? N1 C1 H11 117.9 . . ? C2 C1 H11 117.9 . . ? N1 C5 N2 120.5(5) . . ? N1 C5 C4 121.3(5) . . ? N2 C5 C4 118.2(6) . . ? C4 C3 C2 118.5(5) . . ? C4 C3 H31 120.7 . . ? C2 C3 H31 120.7 . . ? C1 C2 C3 118.5(5) . . ? C1 C2 H21 120.7 . . ? C3 C2 H21 120.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A F2 0.86(2) 2.24(11) 2.788(9) 122(10) 5_455 N2 H2A F3 0.86(2) 2.26(4) 3.096(10) 166(12) 1_454 _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.271 _refine_diff_density_min -1.966 _refine_diff_density_rms 0.627 #===end data_7 _database_code_depnum_ccdc_archive 'CCDC 715747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Cu N4 O2, F4 Mo O2' _chemical_formula_sum 'C20 H20 Cu F4 Mo N4 O4' _chemical_formula_weight 615.89 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' _symmetry_space_group_name_Hall '-P 4a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 11.243(3) _cell_length_b 11.243(3) _cell_length_c 15.773(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1993.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11179 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.4 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.0500 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.773 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11179 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.35 _reflns_number_total 926 _reflns_number_gt 904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1928P)^2^+32.6079P] 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 SHELXL _refine_ls_extinction_coef 0.0022(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 926 _refine_ls_number_parameters 85 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2664 _refine_ls_wR_factor_gt 0.2624 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.922 _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 Mo1 Mo 0.2500 0.2500 0.18479(11) 0.0333(7) Uani 1 4 d S . . Cu1 Cu 0.7500 0.2500 0.2500 0.0189(7) Uani 1 4 d S . . F1 F 0.3480(5) 0.1150(5) 0.1901(4) 0.0384(14) Uani 0.75 1 d P . . O1 O 0.3480(5) 0.1150(5) 0.1901(4) 0.0384(14) Uani 0.25 1 d P . . F2 F 0.2500 0.2500 0.0617(7) 0.037(3) Uani 0.50 4 d SP . . O2 O 0.2500 0.2500 0.0617(7) 0.037(3) Uani 0.50 4 d SP . . F3 F 0.2500 0.2500 0.3070(8) 0.033(3) Uani 0.50 4 d SP . . O3 O 0.2500 0.2500 0.3070(8) 0.033(3) Uani 0.50 4 d SP . . O4 O 0.8967(5) 0.1033(5) 0.2500 0.0259(18) Uani 1 2 d SD . . H4A H 0.963(5) 0.104(9) 0.224(6) 0.039 Uiso 1 1 d D . . N1 N 0.6590(5) 0.1573(6) 0.1586(4) 0.0193(14) Uani 1 1 d . . . C1 C 0.6575(7) 0.0384(7) 0.1581(5) 0.0247(17) Uani 1 1 d . . . H11 H 0.6980 -0.0023 0.2006 0.030 Uiso 1 1 calc R . . C2 C 0.5980(7) -0.0266(7) 0.0967(5) 0.0233(17) Uani 1 1 d . . . H21 H 0.6013 -0.1093 0.0971 0.028 Uiso 1 1 calc R . . C3 C 0.5325(7) 0.0330(7) 0.0337(5) 0.0226(17) Uani 1 1 d . . . C4 C 0.5331(7) 0.1550(7) 0.0365(5) 0.0256(18) Uani 1 1 d . . . H41 H 0.4904 0.1977 -0.0038 0.031 Uiso 1 1 calc R . . C5 C 0.5966(8) 0.2156(8) 0.0985(5) 0.0284(18) Uani 1 1 d . . . H51 H 0.5960 0.2983 0.0986 0.034 Uiso 1 1 calc R . . 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 Mo1 0.0322(8) 0.0322(8) 0.0357(11) 0.000 0.000 0.000 Cu1 0.0212(9) 0.0212(9) 0.0141(11) 0.000 0.000 -0.0051(7) F1 0.031(3) 0.034(3) 0.050(3) -0.005(3) -0.004(2) -0.001(2) O1 0.031(3) 0.034(3) 0.050(3) -0.005(3) -0.004(2) -0.001(2) F2 0.045(5) 0.045(5) 0.020(5) 0.000 0.000 0.000 O2 0.045(5) 0.045(5) 0.020(5) 0.000 0.000 0.000 F3 0.033(4) 0.033(4) 0.034(6) 0.000 0.000 0.000 O3 0.033(4) 0.033(4) 0.034(6) 0.000 0.000 0.000 O4 0.024(3) 0.024(3) 0.030(4) 0.005(2) 0.005(2) 0.002(3) N1 0.018(3) 0.024(3) 0.017(3) 0.000(2) -0.001(2) -0.003(2) C1 0.021(4) 0.032(4) 0.022(4) 0.001(3) 0.002(3) -0.001(3) C2 0.032(4) 0.015(4) 0.022(4) -0.001(3) -0.004(3) -0.002(3) C3 0.016(3) 0.028(4) 0.023(4) -0.005(3) 0.001(3) -0.005(3) C4 0.028(4) 0.026(4) 0.022(4) -0.003(3) 0.000(3) -0.002(3) C5 0.027(4) 0.025(4) 0.033(4) -0.005(3) 0.003(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 Mo1 O1 1.877(6) 3 ? Mo1 F1 1.877(6) 3 ? Mo1 O1 1.877(6) 4 ? Mo1 F1 1.877(6) 4 ? Mo1 F1 1.877(6) . ? Mo1 O1 1.877(6) 2 ? Mo1 F1 1.877(6) 2 ? Mo1 F3 1.927(12) . ? Mo1 F2 1.942(11) . ? Cu1 N1 2.052(6) 8_665 ? Cu1 N1 2.052(6) . ? Cu1 N1 2.052(6) 7_545 ? Cu1 N1 2.052(6) 2_655 ? Cu1 O4 2.333(8) . ? Cu1 O4 2.333(8) 2_655 ? O4 H4A 0.85(2) . ? N1 C1 1.337(11) . ? N1 C5 1.349(11) . ? C1 C2 1.386(11) . ? C1 H11 0.9300 . ? C2 C3 1.407(11) . ? C2 H21 0.9300 . ? C3 C4 1.372(12) . ? C3 C3 1.489(15) 9_655 ? C4 C5 1.390(11) . ? C4 H41 0.9300 . ? C5 H51 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 Mo1 F1 0.0(5) 3 3 ? O1 Mo1 O1 174.9(4) 3 4 ? F1 Mo1 O1 174.9(4) 3 4 ? O1 Mo1 F1 174.9(4) 3 4 ? F1 Mo1 F1 174.9(4) 3 4 ? O1 Mo1 F1 0.0(5) 4 4 ? O1 Mo1 F1 89.887(17) 3 . ? F1 Mo1 F1 89.887(17) 3 . ? O1 Mo1 F1 89.887(17) 4 . ? F1 Mo1 F1 89.887(17) 4 . ? O1 Mo1 O1 89.887(17) 3 2 ? F1 Mo1 O1 89.887(17) 3 2 ? O1 Mo1 O1 89.887(17) 4 2 ? F1 Mo1 O1 89.887(17) 4 2 ? F1 Mo1 O1 174.9(4) . 2 ? O1 Mo1 F1 89.887(17) 3 2 ? F1 Mo1 F1 89.887(17) 3 2 ? O1 Mo1 F1 89.887(17) 4 2 ? F1 Mo1 F1 89.887(17) 4 2 ? F1 Mo1 F1 174.9(4) . 2 ? O1 Mo1 F1 0.0(4) 2 2 ? O1 Mo1 F3 87.46(18) 3 . ? F1 Mo1 F3 87.46(18) 3 . ? O1 Mo1 F3 87.46(18) 4 . ? F1 Mo1 F3 87.46(18) 4 . ? F1 Mo1 F3 87.46(18) . . ? O1 Mo1 F3 87.46(18) 2 . ? F1 Mo1 F3 87.46(18) 2 . ? O1 Mo1 F2 92.54(18) 3 . ? F1 Mo1 F2 92.54(18) 3 . ? O1 Mo1 F2 92.54(18) 4 . ? F1 Mo1 F2 92.54(18) 4 . ? F1 Mo1 F2 92.54(18) . . ? O1 Mo1 F2 92.54(18) 2 . ? F1 Mo1 F2 92.54(18) 2 . ? F3 Mo1 F2 180.000(1) . . ? N1 Cu1 N1 179.2(4) 8_665 . ? N1 Cu1 N1 90.7(3) 8_665 7_545 ? N1 Cu1 N1 89.3(3) . 7_545 ? N1 Cu1 N1 89.3(3) 8_665 2_655 ? N1 Cu1 N1 90.7(3) . 2_655 ? N1 Cu1 N1 179.2(4) 7_545 2_655 ? N1 Cu1 O4 89.62(17) 8_665 . ? N1 Cu1 O4 89.62(17) . . ? N1 Cu1 O4 90.38(17) 7_545 . ? N1 Cu1 O4 90.38(17) 2_655 . ? N1 Cu1 O4 90.38(17) 8_665 2_655 ? N1 Cu1 O4 90.38(17) . 2_655 ? N1 Cu1 O4 89.62(17) 7_545 2_655 ? N1 Cu1 O4 89.62(17) 2_655 2_655 ? O4 Cu1 O4 180.0 . 2_655 ? Cu1 O4 H4A 128(7) . . ? C1 N1 C5 118.4(7) . . ? C1 N1 Cu1 121.2(5) . . ? C5 N1 Cu1 120.4(5) . . ? N1 C1 C2 122.5(7) . . ? N1 C1 H11 118.8 . . ? C2 C1 H11 118.8 . . ? C1 C2 C3 119.7(7) . . ? C1 C2 H21 120.2 . . ? C3 C2 H21 120.2 . . ? C4 C3 C2 116.8(7) . . ? C4 C3 C3 121.5(9) . 9_655 ? C2 C3 C3 121.6(9) . 9_655 ? C3 C4 C5 121.0(8) . . ? C3 C4 H41 119.5 . . ? C5 C4 H41 119.5 . . ? N1 C5 C4 121.6(8) . . ? N1 C5 H51 119.2 . . ? C4 C5 H51 119.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A F1 0.85(2) 1.87(4) 2.686(7) 160(10) 4_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.273 _refine_diff_density_min -1.823 _refine_diff_density_rms 0.160 #===end data_8 _database_code_depnum_ccdc_archive 'CCDC 715748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Cu N4 O2, F5 Nb O' _chemical_formula_sum 'C20 H20 Cu F5 N4 Nb O3' _chemical_formula_weight 615.86 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' _symmetry_space_group_name_Hall '-P 4a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z+1/2' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' '-y, -x, -z+1/2' '-x, -y, -z' '-x-1/2, y, z-1/2' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' 'y, x, z-1/2' _cell_length_a 11.340(4) _cell_length_b 11.340(4) _cell_length_c 15.657(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2013.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 12515 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.7 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12515 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.68 _reflns_number_total 1178 _reflns_number_gt 925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1920P)^2^+13.6782P] 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 SHELXL _refine_ls_extinction_coef 0.0048(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1178 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 0.589 _refine_ls_restrained_S_all 0.589 _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 Nb1 Nb 0.2500 0.2500 0.18766(5) 0.0249(3) Uani 1 4 d S . . Cu1 Cu 0.7500 0.2500 0.2500 0.0158(4) Uani 1 4 d S . . F1 F 0.3477(2) 0.1105(2) 0.19154(15) 0.0344(6) Uani 0.81 1 d P . . O1 O 0.3477(2) 0.1105(2) 0.19154(15) 0.0344(6) Uani 0.19 1 d P . . F2 F 0.2500 0.2500 0.3128(3) 0.0250(12) Uani 0.88 4 d SP . . O2 O 0.2500 0.2500 0.3128(3) 0.0250(12) Uani 0.12 4 d SP . . F3 F 0.2500 0.2500 0.0659(3) 0.0380(14) Uani 0.88 4 d SP . . O3 O 0.2500 0.2500 0.0659(3) 0.0380(14) Uani 0.12 4 d SP . . O4 O 0.8960(2) 0.1040(2) 0.2500 0.0257(8) Uani 1 2 d S . . H4A H 0.881(4) 0.037(4) 0.270(3) 0.039 Uiso 1 1 d . . . N1 N 0.6583(2) 0.1592(2) 0.34150(17) 0.0200(6) Uani 1 1 d . . . C1 C 0.7139(3) 0.0964(3) 0.4014(2) 0.0237(7) Uani 1 1 d . . . H11 H 0.7959 0.0963 0.4015 0.028 Uiso 1 1 calc R . . C2 C 0.6557(3) 0.0316(3) 0.4630(2) 0.0252(8) Uani 1 1 d . . . H21 H 0.6984 -0.0127 0.5022 0.030 Uiso 1 1 calc R . . C3 C 0.5331(3) 0.0329(3) 0.46630(18) 0.0196(7) Uani 1 1 d . . . C4 C 0.4748(2) 0.0973(2) 0.40322(16) 0.0233(7) Uani 1 1 d . . . H41 H 0.3928 0.0995 0.4019 0.028 Uiso 1 1 calc R . . C5 C 0.5400(2) 0.1582(2) 0.34234(16) 0.0232(7) Uani 1 1 d R . . H51 H 0.4999 0.2002 0.3004 0.028 Uiso 1 1 calc R . . 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 Nb1 0.0267(4) 0.0267(4) 0.0214(5) 0.000 0.000 0.000 Cu1 0.0183(4) 0.0183(4) 0.0110(6) 0.000 0.000 -0.0051(3) F1 0.0318(13) 0.0266(12) 0.0446(14) 0.0032(10) 0.0007(10) 0.0048(9) O1 0.0318(13) 0.0266(12) 0.0446(14) 0.0032(10) 0.0007(10) 0.0048(9) F2 0.0328(18) 0.0328(18) 0.010(2) 0.000 0.000 0.000 O2 0.0328(18) 0.0328(18) 0.010(2) 0.000 0.000 0.000 F3 0.042(2) 0.042(2) 0.030(3) 0.000 0.000 0.000 O3 0.042(2) 0.042(2) 0.030(3) 0.000 0.000 0.000 O4 0.0226(11) 0.0226(11) 0.0319(19) 0.0054(10) 0.0054(10) -0.0008(14) N1 0.0225(14) 0.0224(14) 0.0151(12) 0.0001(11) -0.0001(11) -0.0027(11) C1 0.0210(16) 0.0277(18) 0.0223(15) 0.0013(14) 0.0002(14) -0.0026(14) C2 0.0276(18) 0.0265(17) 0.0216(16) 0.0030(13) -0.0004(13) 0.0017(14) C3 0.0247(16) 0.0200(15) 0.0140(15) -0.0032(12) -0.0005(12) -0.0001(15) C4 0.0221(15) 0.0247(17) 0.0231(16) 0.0031(13) -0.0019(13) -0.0030(13) C5 0.0254(17) 0.0234(17) 0.0208(15) 0.0026(13) -0.0030(13) -0.0014(12) _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 Nb1 F3 1.907(6) . ? Nb1 O1 1.932(2) 6 ? Nb1 F1 1.932(2) 6 ? Nb1 O1 1.932(2) 7 ? Nb1 F1 1.932(2) 7 ? Nb1 F1 1.932(2) . ? Nb1 F1 1.932(2) 3 ? Nb1 O1 1.932(2) 3 ? Nb1 F2 1.960(4) . ? Cu1 N1 2.048(3) 5_545 ? Cu1 N1 2.048(3) 3_655 ? Cu1 N1 2.048(3) . ? Cu1 N1 2.048(3) 8_665 ? Cu1 O4 2.341(4) . ? Cu1 O4 2.341(4) 3_655 ? O4 H4A 0.83(5) . ? N1 C1 1.335(5) . ? N1 C5 1.341(4) . ? C1 C2 1.381(5) . ? C1 H11 0.9300 . ? C2 C3 1.391(5) . ? C2 H21 0.9300 . ? C3 C4 1.395(4) . ? C3 C3 1.495(7) 9_656 ? C4 C5 1.3906 . ? C4 H41 0.9300 . ? C5 H51 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 F3 Nb1 O1 91.80(7) . 6 ? F3 Nb1 F1 91.80(7) . 6 ? O1 Nb1 F1 0.0(2) 6 6 ? F3 Nb1 O1 91.80(7) . 7 ? O1 Nb1 O1 176.39(15) 6 7 ? F1 Nb1 O1 176.39(15) 6 7 ? F3 Nb1 F1 91.80(7) . 7 ? O1 Nb1 F1 176.39(15) 6 7 ? F1 Nb1 F1 176.39(15) 6 7 ? O1 Nb1 F1 0.0(2) 7 7 ? F3 Nb1 F1 91.80(7) . . ? O1 Nb1 F1 89.943(5) 6 . ? F1 Nb1 F1 89.943(5) 6 . ? O1 Nb1 F1 89.943(5) 7 . ? F1 Nb1 F1 89.943(5) 7 . ? F3 Nb1 F1 91.80(7) . 3 ? O1 Nb1 F1 89.943(5) 6 3 ? F1 Nb1 F1 89.943(5) 6 3 ? O1 Nb1 F1 89.943(5) 7 3 ? F1 Nb1 F1 89.943(5) 7 3 ? F1 Nb1 F1 176.39(15) . 3 ? F3 Nb1 O1 91.80(7) . 3 ? O1 Nb1 O1 89.943(5) 6 3 ? F1 Nb1 O1 89.943(5) 6 3 ? O1 Nb1 O1 89.943(5) 7 3 ? F1 Nb1 O1 89.943(5) 7 3 ? F1 Nb1 O1 176.39(15) . 3 ? F1 Nb1 O1 0.00(19) 3 3 ? F3 Nb1 F2 180.0 . . ? O1 Nb1 F2 88.20(7) 6 . ? F1 Nb1 F2 88.20(7) 6 . ? O1 Nb1 F2 88.20(7) 7 . ? F1 Nb1 F2 88.20(7) 7 . ? F1 Nb1 F2 88.20(7) . . ? F1 Nb1 F2 88.20(7) 3 . ? O1 Nb1 F2 88.20(7) 3 . ? N1 Cu1 N1 179.60(16) 5_545 3_655 ? N1 Cu1 N1 88.80(15) 5_545 . ? N1 Cu1 N1 91.21(15) 3_655 . ? N1 Cu1 N1 91.21(15) 5_545 8_665 ? N1 Cu1 N1 88.80(15) 3_655 8_665 ? N1 Cu1 N1 179.60(16) . 8_665 ? N1 Cu1 O4 89.80(8) 5_545 . ? N1 Cu1 O4 89.80(8) 3_655 . ? N1 Cu1 O4 90.20(8) . . ? N1 Cu1 O4 90.20(8) 8_665 . ? N1 Cu1 O4 90.20(8) 5_545 3_655 ? N1 Cu1 O4 90.20(8) 3_655 3_655 ? N1 Cu1 O4 89.80(8) . 3_655 ? N1 Cu1 O4 89.80(8) 8_665 3_655 ? O4 Cu1 O4 180.0 . 3_655 ? Cu1 O4 H4A 120(3) . . ? C1 N1 C5 117.5(3) . . ? C1 N1 Cu1 121.3(2) . . ? C5 N1 Cu1 121.24(19) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H11 118.4 . . ? C2 C1 H11 118.4 . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H21 120.1 . . ? C3 C2 H21 120.1 . . ? C2 C3 C4 116.9(3) . . ? C2 C3 C3 121.6(4) . 9_656 ? C4 C3 C3 121.5(4) . 9_656 ? C5 C4 C3 119.53(18) . . ? C5 C4 H41 120.2 . . ? C3 C4 H41 120.2 . . ? N1 C5 C4 122.89(15) . . ? N1 C5 H51 118.6 . . ? C4 C5 H51 118.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A F1 0.83(5) 1.82(5) 2.656(3) 178(5) 2 _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.542 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.152 #===end