data_1 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Abdessadek Lachgar' _publ_contact_author_address ; Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 ; _publ_contact_author_email 'lachgar@wfu.edu' _publ_contact_author_fax '(336) 758-4656' _publ_contact_author_phone '(336) 758-4676' _publ_requested_journal ; Chemistry of Materials ; _publ_section_title ; Assembly of Hybrid Inorganic-Organic Materials from Octahedral Nb6 Clusters and Metal Complexes ; loop_ _publ_author_name _publ_author_address 'Huajun Zhou' ; Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 ; 'Cynthia S. Day ' ; Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 ; 'Abdessadek Lachgar' ; Department of Chemistry, Wake Forest University, Winston-Salem, NC 27109 ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 Cl12 N10 Nb6 O2' _chemical_formula_weight 1499.65 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 14.086(3) _cell_length_b 20.057(4) _cell_length_c 20.938(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5915(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3966 _cell_measurement_theta_min 3.893 _cell_measurement_theta_max 22.705 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ; Data were corrected for absorption effects using the multiscan technique (SADABS). The ratio of minimum to maximum apparent transmission was 0.79. ; _exptl_special_details ; ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method "phi and omega scans" _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25560 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3521 _reflns_number_gt 2647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL Vers 6.12' _computing_structure_refinement 'Bruker SHELXTL Vers 6.12' _computing_molecular_graphics 'Bruker SHELXTL Vers 6.12' _computing_publication_material 'Bruker SHELXTL Vers 6.12' _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^)+(0.0640P)^2^+7.7140P] 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 3521 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.0000 0.05760(3) 0.41787(3) 0.04018(17) Uani 1 2 d S . . Nb2 Nb 0.10399(3) 0.06036(2) 0.539108(19) 0.03939(15) Uani 1 1 d . . . Cl1 Cl 0.12381(9) 0.13859(6) 0.44897(6) 0.0509(3) Uani 1 1 d . . . Cl2 Cl 0.12184(9) -0.00346(7) 0.35770(5) 0.0528(3) Uani 1 1 d . . . Cl3 Cl 0.24476(12) 0.0000 0.5000 0.0480(4) Uani 1 2 d S . . Cl4 Cl 0.0000 0.14213(9) 0.59267(9) 0.0524(4) Uani 1 2 d S . . C1 C 0.0000 0.1197(4) 0.3265(4) 0.0559(19) Uani 1 2 d S . . C2 C 0.2178(4) 0.1278(3) 0.5821(3) 0.0596(14) Uani 1 1 d . . . C3 C 0.5000 0.0905(4) 0.5102(5) 0.089(3) Uani 1 2 d S . . H3A H 0.5000 0.0675 0.4689 0.133 Uiso 1 2 calc SR . . H3B H 0.4432 0.0778 0.5343 0.133 Uiso 0.50 1 calc PR . . H3C H 0.5568 0.0778 0.5343 0.133 Uiso 0.50 1 calc PR . . C4 C 0.5000 0.1995(5) 0.5626(5) 0.080(3) Uani 1 2 d S . . H4A H 0.5573 0.1877 0.5866 0.119 Uiso 0.50 1 calc PR . . H4B H 0.4437 0.1867 0.5872 0.119 Uiso 0.50 1 calc PR . . H4C H 0.4990 0.2477 0.5551 0.119 Uiso 1 2 calc SR . . C5 C 0.4127(5) 0.1829(4) 0.4632(3) 0.087(2) Uani 1 1 d . . . H5A H 0.4122 0.1599 0.4218 0.130 Uiso 1 1 calc R . . H5B H 0.4127 0.2312 0.4562 0.130 Uiso 1 1 calc R . . H5C H 0.3562 0.1702 0.4876 0.130 Uiso 1 1 calc R . . C6 C 0.2526(5) 0.3050(3) 0.6921(3) 0.0761(18) Uani 1 1 d . . . H6A H 0.3091 0.3335 0.6932 0.114 Uiso 1 1 calc R . . H6B H 0.1956 0.3329 0.6905 0.114 Uiso 1 1 calc R . . H6C H 0.2550 0.2765 0.6540 0.114 Uiso 1 1 calc R . . C7 C 0.1632(4) 0.2193(3) 0.7478(3) 0.0665(15) Uani 1 1 d . . . H7A H 0.1610 0.1912 0.7860 0.100 Uiso 1 1 calc R . . H7B H 0.1656 0.1910 0.7097 0.100 Uiso 1 1 calc R . . H7C H 0.1063 0.2474 0.7462 0.100 Uiso 1 1 calc R . . O1 O 0.4347(12) 0.0944(9) 0.3384(8) 0.170(6) Uiso 0.50 1 d P . . N1 N 0.0000 0.1487(4) 0.2800(3) 0.072(2) Uani 1 2 d S . . N2 N 0.2749(4) 0.1601(3) 0.6037(3) 0.0839(17) Uani 1 1 d . . . N3 N 0.5000 0.1634(3) 0.4996(3) 0.0627(17) Uani 1 2 d S . . N4 N 0.2500 0.2628(3) 0.7500 0.0560(15) Uani 1 2 d S . . C8 C 0.3712(15) 0.0128(10) 0.3237(11) 0.126(6) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0437(3) 0.0433(3) 0.0336(3) 0.0044(2) 0.000 0.000 Nb2 0.0417(3) 0.0416(2) 0.0349(2) -0.00350(17) -0.00087(16) -0.00302(17) Cl1 0.0538(7) 0.0461(7) 0.0526(7) 0.0066(5) 0.0017(6) -0.0093(5) Cl2 0.0521(7) 0.0716(8) 0.0346(6) 0.0018(5) 0.0071(5) 0.0055(6) Cl3 0.0403(8) 0.0584(10) 0.0454(9) -0.0049(7) 0.000 0.000 Cl4 0.0581(10) 0.0473(9) 0.0519(10) -0.0153(8) 0.000 0.000 C1 0.050(4) 0.068(5) 0.050(4) 0.020(4) 0.000 0.000 C2 0.057(3) 0.067(3) 0.054(3) -0.017(3) 0.005(3) -0.013(3) C3 0.124(9) 0.046(5) 0.095(7) 0.009(5) 0.000 0.000 C4 0.064(5) 0.074(6) 0.101(7) -0.024(5) 0.000 0.000 C5 0.075(5) 0.099(6) 0.087(5) 0.016(4) -0.016(4) -0.005(4) C6 0.092(5) 0.076(4) 0.060(4) 0.010(3) -0.004(3) -0.005(4) C7 0.059(4) 0.081(4) 0.059(3) -0.007(3) 0.006(3) -0.008(3) N1 0.069(5) 0.086(5) 0.062(4) 0.029(4) 0.000 0.000 N2 0.076(4) 0.101(4) 0.074(3) -0.035(3) 0.007(3) -0.039(3) N3 0.062(4) 0.050(4) 0.077(5) 0.012(3) 0.000 0.000 N4 0.058(4) 0.063(4) 0.047(3) 0.000 0.001(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 C1 2.282(7) . ? Nb1 Cl2 2.4560(13) 12 ? Nb1 Cl2 2.4560(13) . ? Nb1 Cl1 2.4707(13) . ? Nb1 Cl1 2.4707(13) 12 ? Nb1 Nb2 2.9248(8) 9_556 ? Nb1 Nb2 2.9248(8) 4_556 ? Nb1 Nb2 2.9314(8) . ? Nb1 Nb2 2.9314(8) 12 ? Nb2 C2 2.283(5) . ? Nb2 Cl2 2.4564(13) 4_556 ? Nb2 Cl3 2.4633(14) . ? Nb2 Cl4 2.4685(14) . ? Nb2 Cl1 2.4703(13) . ? Nb2 Nb2 2.9230(9) 4_556 ? Nb2 Nb1 2.9248(8) 9_556 ? Nb2 Nb2 2.9297(10) 12 ? Cl2 Nb2 2.4564(13) 4_556 ? Cl3 Nb2 2.4633(14) 4_556 ? Cl4 Nb2 2.4685(14) 12 ? C1 N1 1.134(9) . ? C2 N2 1.126(6) . ? C3 N3 1.479(11) . ? C4 N3 1.505(12) . ? C5 N3 1.498(7) . ? C6 N4 1.480(6) . ? C7 N4 1.503(7) . ? O1 C8 1.89(3) . ? N3 C5 1.498(7) 12_655 ? N4 C6 1.480(6) 7_546 ? N4 C7 1.503(7) 7_546 ? 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 C1 Nb1 Cl2 80.93(15) . 12 ? C1 Nb1 Cl2 80.93(15) . . ? Cl2 Nb1 Cl2 88.66(7) 12 . ? C1 Nb1 Cl1 82.07(15) . . ? Cl2 Nb1 Cl1 162.99(5) 12 . ? Cl2 Nb1 Cl1 88.27(5) . . ? C1 Nb1 Cl1 82.07(15) . 12 ? Cl2 Nb1 Cl1 88.27(5) 12 12 ? Cl2 Nb1 Cl1 162.99(5) . 12 ? Cl1 Nb1 Cl1 89.80(7) . 12 ? C1 Nb1 Nb2 134.39(15) . 9_556 ? Cl2 Nb1 Nb2 53.47(3) 12 9_556 ? Cl2 Nb1 Nb2 96.01(4) . 9_556 ? Cl1 Nb1 Nb2 143.53(4) . 9_556 ? Cl1 Nb1 Nb2 95.57(4) 12 9_556 ? C1 Nb1 Nb2 134.39(15) . 4_556 ? Cl2 Nb1 Nb2 96.01(4) 12 4_556 ? Cl2 Nb1 Nb2 53.47(3) . 4_556 ? Cl1 Nb1 Nb2 95.57(4) . 4_556 ? Cl1 Nb1 Nb2 143.53(4) 12 4_556 ? Nb2 Nb1 Nb2 60.11(2) 9_556 4_556 ? C1 Nb1 Nb2 135.67(15) . . ? Cl2 Nb1 Nb2 143.40(4) 12 . ? Cl2 Nb1 Nb2 95.99(3) . . ? Cl1 Nb1 Nb2 53.60(3) . . ? Cl1 Nb1 Nb2 96.44(4) 12 . ? Nb2 Nb1 Nb2 89.93(2) 9_556 . ? Nb2 Nb1 Nb2 59.885(18) 4_556 . ? C1 Nb1 Nb2 135.67(15) . 12 ? Cl2 Nb1 Nb2 95.99(3) 12 12 ? Cl2 Nb1 Nb2 143.40(4) . 12 ? Cl1 Nb1 Nb2 96.44(4) . 12 ? Cl1 Nb1 Nb2 53.60(3) 12 12 ? Nb2 Nb1 Nb2 59.885(18) 9_556 12 ? Nb2 Nb1 Nb2 89.93(2) 4_556 12 ? Nb2 Nb1 Nb2 59.96(2) . 12 ? C2 Nb2 Cl2 81.78(15) . 4_556 ? C2 Nb2 Cl3 81.79(14) . . ? Cl2 Nb2 Cl3 88.95(4) 4_556 . ? C2 Nb2 Cl4 81.01(14) . . ? Cl2 Nb2 Cl4 88.27(6) 4_556 . ? Cl3 Nb2 Cl4 162.79(4) . . ? C2 Nb2 Cl1 81.08(15) . . ? Cl2 Nb2 Cl1 162.86(5) 4_556 . ? Cl3 Nb2 Cl1 88.12(4) . . ? Cl4 Nb2 Cl1 89.55(6) . . ? C2 Nb2 Nb2 135.39(14) . 4_556 ? Cl2 Nb2 Nb2 96.20(4) 4_556 4_556 ? Cl3 Nb2 Nb2 53.61(3) . 4_556 ? Cl4 Nb2 Nb2 143.60(3) . 4_556 ? Cl1 Nb2 Nb2 95.63(4) . 4_556 ? C2 Nb2 Nb1 135.24(15) . 9_556 ? Cl2 Nb2 Nb1 53.45(3) 4_556 9_556 ? Cl3 Nb2 Nb1 96.20(3) . 9_556 ? Cl4 Nb2 Nb1 95.76(4) . 9_556 ? Cl1 Nb2 Nb1 143.68(3) . 9_556 ? Nb2 Nb2 Nb1 60.17(2) 4_556 9_556 ? C2 Nb2 Nb2 134.60(14) . 12 ? Cl2 Nb2 Nb2 95.87(3) 4_556 12 ? Cl3 Nb2 Nb2 143.61(3) . 12 ? Cl4 Nb2 Nb2 53.60(3) . 12 ? Cl1 Nb2 Nb2 96.49(3) . 12 ? Nb2 Nb2 Nb2 90.0 4_556 12 ? Nb1 Nb2 Nb2 59.944(12) 9_556 12 ? C2 Nb2 Nb1 134.69(15) . . ? Cl2 Nb2 Nb1 143.52(4) 4_556 . ? Cl3 Nb2 Nb1 96.03(2) . . ? Cl4 Nb2 Nb1 96.28(4) . . ? Cl1 Nb2 Nb1 53.62(3) . . ? Nb2 Nb2 Nb1 59.945(18) 4_556 . ? Nb1 Nb2 Nb1 90.07(2) 9_556 . ? Nb2 Nb2 Nb1 60.019(12) 12 . ? Nb2 Cl1 Nb1 72.78(4) . . ? Nb1 Cl2 Nb2 73.08(4) . 4_556 ? Nb2 Cl3 Nb2 72.78(5) 4_556 . ? Nb2 Cl4 Nb2 72.80(5) 12 . ? N1 C1 Nb1 177.8(7) . . ? N2 C2 Nb2 178.6(6) . . ? C3 N3 C5 109.5(5) . 12_655 ? C3 N3 C5 109.5(5) . . ? C5 N3 C5 110.2(7) 12_655 . ? C3 N3 C4 110.2(7) . . ? C5 N3 C4 108.7(5) 12_655 . ? C5 N3 C4 108.7(5) . . ? C6 N4 C6 110.2(6) 7_546 . ? C6 N4 C7 109.7(3) 7_546 . ? C6 N4 C7 109.1(3) . . ? C6 N4 C7 109.1(3) 7_546 7_546 ? C6 N4 C7 109.7(3) . 7_546 ? C7 N4 C7 109.1(6) . 7_546 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.674 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.113 data_2 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Cl12 Mn2 N12 Nb6 O4' _chemical_formula_weight 1929.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.1512(13) _cell_length_b 13.0142(7) _cell_length_c 23.2007(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6990.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8598 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.53 _exptl_crystal_description 'triangular-shaped' _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 1.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ; Data were corrected for absorption effects using the multiscan technique (SADABS). The ratio of minimum to maximum apparent transmission was 0.72. ; _exptl_special_details ; ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method "phi and omega scans" _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81015 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5028 _reflns_number_gt 4192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL Vers 6.12' _computing_structure_refinement 'Bruker SHELXTL Vers. 6.12' _computing_molecular_graphics 'Bruker SHELXTL Vers. 6.12' _computing_publication_material 'Bruker SHELXTL Vers. 6.12' _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^)+(0.0442P)^2^+1.9409P] 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 5028 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.047087(13) 0.36594(2) 0.488445(13) 0.03099(10) Uani 1 1 d . . . Nb2 Nb -0.050580(13) 0.46393(2) 0.429288(13) 0.02969(10) Uani 1 1 d . . . Nb3 Nb 0.056503(13) 0.57816(2) 0.447115(13) 0.03106(10) Uani 1 1 d . . . Cl1 Cl 0.12118(4) 0.43526(7) 0.42322(4) 0.0423(2) Uani 1 1 d . . . Cl2 Cl -0.00381(4) 0.30052(7) 0.40261(4) 0.0428(2) Uani 1 1 d . . . Cl3 Cl 0.11430(4) 0.38506(7) 0.57008(4) 0.0412(2) Uani 1 1 d . . . Cl4 Cl -0.01286(4) 0.25096(7) 0.54666(4) 0.0436(2) Uani 1 1 d . . . Cl5 Cl -0.12714(4) 0.36690(7) 0.47925(4) 0.0393(2) Uani 1 1 d . . . Cl6 Cl 0.00713(4) 0.54878(8) 0.35426(4) 0.0440(2) Uani 1 1 d . . . N1 N 0.13155(17) 0.1536(3) 0.4740(2) 0.0773(12) Uani 1 1 d . . . N2 N -0.13109(14) 0.3936(3) 0.31251(14) 0.0546(9) Uani 1 1 d . A . N3 N 0.14542(14) 0.7074(3) 0.35494(15) 0.0576(9) Uani 1 1 d . . . C1 C 0.10157(17) 0.2220(3) 0.47735(17) 0.0465(10) Uani 1 1 d . . . C2 C -0.10624(16) 0.4212(3) 0.35149(17) 0.0417(9) Uani 1 1 d . . . C3 C 0.11796(16) 0.6634(3) 0.38721(17) 0.0444(9) Uani 1 1 d . . . Mn1 Mn -0.14238(2) 0.30923(4) 0.22945(2) 0.03886(15) Uani 1 1 d . . . O1 O -0.21929(10) 0.35171(18) 0.21941(10) 0.0416(6) Uani 1 1 d . A . O2 O -0.10977(11) 0.4166(2) 0.18642(11) 0.0486(7) Uani 1 1 d . A . N4 N -0.1687(8) 0.1927(13) 0.2784(5) 0.044(3) Uani 0.546(10) 1 d P A 1 N4' N -0.1664(9) 0.1714(15) 0.2570(7) 0.047(4) Uani 0.454(10) 1 d P A 2 N5 N -0.06544(14) 0.2460(2) 0.24332(13) 0.0454(8) Uani 1 1 d . A . C4 C -0.05673(17) 0.4266(3) 0.16618(17) 0.0458(10) Uani 1 1 d . . . C5 C -0.01068(17) 0.3626(3) 0.18315(18) 0.0510(10) Uani 1 1 d . A . C6 C -0.01756(18) 0.2771(3) 0.22149(18) 0.0513(11) Uani 1 1 d . . . H6 H 0.0156 0.2410 0.2315 0.062 Uiso 1 1 calc R A . C7 C -0.0667(2) 0.1541(3) 0.27870(19) 0.0606(12) Uani 1 1 d . . . H7A H -0.0340 0.1547 0.3049 0.073 Uiso 0.546(10) 1 calc PR A 1 H7B H -0.0633 0.0940 0.2542 0.073 Uiso 0.546(10) 1 calc PR A 1 H7C H -0.0331 0.1121 0.2706 0.073 Uiso 0.454(10) 1 calc PR A 2 H7D H -0.0659 0.1729 0.3191 0.073 Uiso 0.454(10) 1 calc PR A 2 C8 C -0.1218(3) 0.1475(6) 0.3128(3) 0.055(3) Uani 0.546(10) 1 d P A 1 H8A H -0.1305 0.0763 0.3216 0.066 Uiso 0.546(10) 1 calc PR A 1 H8B H -0.1176 0.1846 0.3489 0.066 Uiso 0.546(10) 1 calc PR A 1 C8' C -0.1176(4) 0.0980(7) 0.2666(5) 0.061(4) Uani 0.454(10) 1 d P A 2 H8'A H -0.1266 0.0529 0.2987 0.074 Uiso 0.454(10) 1 calc PR A 2 H8'B H -0.1120 0.0560 0.2326 0.074 Uiso 0.454(10) 1 calc PR A 2 C9 C -0.2188(2) 0.1465(4) 0.2683(3) 0.0819(16) Uani 1 1 d . . . H9 H -0.2216 0.0773 0.2779 0.098 Uiso 1 1 calc R A 1 C10 C -0.26788(18) 0.1934(3) 0.24440(19) 0.0538(11) Uani 1 1 d . A . C11 C -0.26668(16) 0.2949(3) 0.22237(15) 0.0438(9) Uani 1 1 d . . . C12 C -0.04593(18) 0.5034(3) 0.12548(18) 0.0557(11) Uani 1 1 d . A . H12 H -0.0756 0.5475 0.1146 0.067 Uiso 1 1 calc R . . C13 C 0.0080(2) 0.5149(4) 0.1012(2) 0.0684(13) Uani 1 1 d . . . H13 H 0.0141 0.5660 0.0739 0.082 Uiso 1 1 calc R A . C14 C 0.0529(2) 0.4516(4) 0.1170(2) 0.0733(15) Uani 1 1 d . A . H14 H 0.0891 0.4597 0.1000 0.088 Uiso 1 1 calc R . . C15 C 0.04445(18) 0.3764(4) 0.1577(2) 0.0640(13) Uani 1 1 d . . . H15 H 0.0750 0.3344 0.1687 0.077 Uiso 1 1 calc R A . C16 C -0.31794(18) 0.3365(4) 0.20316(19) 0.0628(12) Uani 1 1 d . A . H16 H -0.3189 0.4042 0.1905 0.075 Uiso 1 1 calc R . . C17 C -0.3680(2) 0.2781(5) 0.2026(2) 0.0851(17) Uani 1 1 d . . . H17 H -0.4018 0.3069 0.1882 0.102 Uiso 1 1 calc R A . C18 C -0.3690(2) 0.1799(5) 0.2225(2) 0.0850(17) Uani 1 1 d . A . H18 H -0.4031 0.1422 0.2220 0.102 Uiso 1 1 calc R . . C19 C -0.3201(2) 0.1380(4) 0.2429(2) 0.0784(15) Uani 1 1 d . . . H19 H -0.3207 0.0707 0.2563 0.094 Uiso 1 1 calc R A . N6 N -0.21012(14) 0.4161(2) 0.03364(17) 0.0538(9) Uani 1 1 d . . . C20 C -0.14730(18) 0.3989(4) 0.0254(2) 0.0771(15) Uani 1 1 d . . . H20A H -0.1275 0.4638 0.0258 0.116 Uiso 1 1 calc R . . H20B H -0.1409 0.3655 -0.0110 0.116 Uiso 1 1 calc R . . H20C H -0.1328 0.3564 0.0559 0.116 Uiso 1 1 calc R . . C21 C -0.2191(2) 0.4776(4) 0.0872(2) 0.0794(15) Uani 1 1 d . . . H21A H -0.1989 0.5418 0.0840 0.119 Uiso 1 1 calc R . . H21B H -0.2046 0.4401 0.1198 0.119 Uiso 1 1 calc R . . H21C H -0.2596 0.4906 0.0924 0.119 Uiso 1 1 calc R . . C22 C -0.2338(2) 0.4719(4) -0.0156(2) 0.0820(16) Uani 1 1 d . . . H22A H -0.2129 0.5349 -0.0208 0.123 Uiso 1 1 calc R . . H22B H -0.2738 0.4871 -0.0086 0.123 Uiso 1 1 calc R . . H22C H -0.2304 0.4305 -0.0496 0.123 Uiso 1 1 calc R . . C23 C -0.24045(19) 0.3153(3) 0.0406(3) 0.0934(19) Uani 1 1 d . . . H23A H -0.2228 0.2771 0.0713 0.140 Uiso 1 1 calc R . . H23B H -0.2377 0.2769 0.0053 0.140 Uiso 1 1 calc R . . H23C H -0.2804 0.3272 0.0495 0.140 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 0.03190(19) 0.02448(17) 0.0366(2) -0.00231(13) -0.00270(14) 0.00303(13) Nb2 0.03113(19) 0.02784(18) 0.03011(18) -0.00152(13) -0.00351(13) 0.00023(13) Nb3 0.03197(19) 0.02863(19) 0.03259(18) 0.00246(13) -0.00135(14) -0.00158(14) Cl1 0.0354(5) 0.0454(5) 0.0463(5) -0.0033(4) 0.0068(4) 0.0050(4) Cl2 0.0450(5) 0.0357(5) 0.0478(5) -0.0141(4) -0.0072(4) 0.0045(4) Cl3 0.0397(5) 0.0368(5) 0.0471(5) -0.0002(4) -0.0111(4) 0.0073(4) Cl4 0.0461(5) 0.0276(5) 0.0572(6) 0.0095(4) -0.0027(5) -0.0004(4) Cl5 0.0361(5) 0.0379(5) 0.0438(5) 0.0017(4) -0.0058(4) -0.0083(4) Cl6 0.0449(5) 0.0553(6) 0.0318(5) 0.0058(4) -0.0022(4) -0.0070(4) N1 0.072(3) 0.046(2) 0.114(3) -0.017(2) -0.007(2) 0.025(2) N2 0.054(2) 0.069(2) 0.0412(19) -0.0138(18) -0.0135(17) 0.0051(18) N3 0.048(2) 0.069(2) 0.056(2) 0.0198(19) -0.0024(18) -0.0151(19) C1 0.049(2) 0.033(2) 0.058(3) -0.0057(19) -0.005(2) 0.005(2) C2 0.042(2) 0.039(2) 0.044(2) -0.0002(18) -0.0013(19) 0.0042(18) C3 0.042(2) 0.047(2) 0.044(2) 0.0062(19) -0.0075(19) -0.0055(19) Mn1 0.0393(3) 0.0398(3) 0.0375(3) -0.0007(3) -0.0063(2) 0.0032(3) O1 0.0380(15) 0.0409(15) 0.0460(15) 0.0001(12) -0.0049(11) 0.0003(12) O2 0.0435(16) 0.0484(16) 0.0539(16) 0.0068(13) -0.0021(13) -0.0004(13) N4 0.047(5) 0.050(7) 0.036(7) 0.004(5) 0.004(6) 0.008(5) N4' 0.048(6) 0.047(8) 0.046(10) 0.004(7) -0.004(8) 0.007(5) N5 0.042(2) 0.050(2) 0.0444(19) -0.0026(16) -0.0068(16) 0.0056(16) C4 0.046(2) 0.044(2) 0.047(2) -0.0103(19) -0.0059(19) -0.0071(19) C5 0.046(2) 0.051(3) 0.056(3) -0.013(2) -0.002(2) -0.007(2) C6 0.037(2) 0.061(3) 0.056(3) -0.013(2) -0.014(2) 0.011(2) C7 0.061(3) 0.062(3) 0.058(3) 0.009(2) -0.004(2) 0.018(2) C8 0.062(5) 0.058(5) 0.045(5) 0.018(4) -0.006(4) 0.021(4) C8' 0.087(8) 0.040(6) 0.057(7) 0.001(5) -0.009(6) 0.016(5) C9 0.063(3) 0.052(3) 0.130(5) 0.031(3) 0.003(3) 0.000(3) C10 0.047(2) 0.048(3) 0.066(3) 0.001(2) 0.000(2) -0.005(2) C11 0.041(2) 0.058(3) 0.032(2) -0.0042(19) 0.0001(17) -0.002(2) C12 0.059(3) 0.051(3) 0.057(3) -0.007(2) -0.002(2) -0.013(2) C13 0.077(4) 0.061(3) 0.067(3) -0.010(3) 0.002(3) -0.026(3) C14 0.065(3) 0.078(4) 0.077(4) -0.026(3) 0.017(3) -0.031(3) C15 0.048(3) 0.065(3) 0.079(3) -0.023(3) -0.005(2) -0.006(2) C16 0.043(3) 0.080(3) 0.065(3) 0.023(2) -0.007(2) 0.000(2) C17 0.046(3) 0.130(5) 0.080(4) 0.027(4) -0.011(3) -0.003(3) C18 0.049(3) 0.101(4) 0.105(4) 0.007(4) -0.006(3) -0.023(3) C19 0.063(3) 0.061(3) 0.111(4) -0.002(3) 0.008(3) -0.013(3) N6 0.0394(19) 0.0357(18) 0.086(3) 0.0038(18) -0.0063(18) 0.0021(15) C20 0.039(3) 0.055(3) 0.137(5) 0.000(3) 0.003(3) 0.000(2) C21 0.067(3) 0.089(4) 0.083(4) 0.006(3) 0.006(3) -0.016(3) C22 0.074(4) 0.088(4) 0.084(4) 0.014(3) -0.028(3) -0.004(3) C23 0.047(3) 0.047(3) 0.186(6) 0.009(3) -0.003(3) -0.007(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 C1 2.273(4) . ? Nb1 Cl4 2.4473(9) . ? Nb1 Cl1 2.4589(9) . ? Nb1 Cl3 2.4638(9) . ? Nb1 Cl2 2.4656(9) . ? Nb1 Nb3 2.9182(4) 5_566 ? Nb1 Nb2 2.9244(4) 5_566 ? Nb1 Nb3 2.9317(5) . ? Nb1 Nb2 2.9364(4) . ? Nb2 C2 2.286(4) . ? Nb2 Cl6 2.4564(9) . ? Nb2 Cl3 2.4574(9) 5_566 ? Nb2 Cl2 2.4654(9) . ? Nb2 Cl5 2.4657(9) . ? Nb2 Nb3 2.9201(4) . ? Nb2 Nb3 2.9226(4) 5_566 ? Nb2 Nb1 2.9244(4) 5_566 ? Nb3 C3 2.277(4) . ? Nb3 Cl4 2.4470(9) 5_566 ? Nb3 Cl1 2.4511(9) . ? Nb3 Cl6 2.4686(9) . ? Nb3 Cl5 2.4708(9) 5_566 ? Nb3 Nb1 2.9182(4) 5_566 ? Nb3 Nb2 2.9226(4) 5_566 ? Cl3 Nb2 2.4574(9) 5_566 ? Cl4 Nb3 2.4470(9) 5_566 ? Cl5 Nb3 2.4708(9) 5_566 ? N1 C1 1.131(5) . ? N2 C2 1.131(4) . ? N2 Mn1 2.233(3) . ? N3 C3 1.137(4) . ? N3 Mn1 2.365(3) 3 ? Mn1 O2 1.876(3) . ? Mn1 O1 1.879(2) . ? Mn1 N4' 1.98(2) . ? Mn1 N5 1.988(3) . ? Mn1 N4 1.990(17) . ? Mn1 N3 2.365(3) 3_545 ? O1 C11 1.325(4) . ? O2 C4 1.321(4) . ? N4 C9 1.327(18) . ? N4 C8 1.471(18) . ? N4' C9 1.28(2) . ? N4' C8' 1.50(2) . ? N5 C6 1.284(5) . ? N5 C7 1.451(5) . ? C4 C12 1.398(6) . ? C4 C5 1.409(6) . ? C5 C15 1.417(6) . ? C5 C6 1.433(6) . ? C7 C8' 1.415(11) . ? C7 C8 1.503(9) . ? C9 C10 1.404(6) . ? C10 C19 1.407(6) . ? C10 C11 1.417(6) . ? C11 C16 1.378(5) . ? C12 C13 1.377(6) . ? C13 C14 1.376(7) . ? C14 C15 1.375(7) . ? C16 C17 1.386(6) . ? C17 C18 1.359(7) . ? C18 C19 1.344(7) . ? N6 C22 1.461(6) . ? N6 C20 1.484(5) . ? N6 C21 1.493(6) . ? N6 C23 1.496(5) . ? 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 C1 Nb1 Cl4 82.72(10) . . ? C1 Nb1 Cl1 81.12(10) . . ? Cl4 Nb1 Cl1 163.65(3) . . ? C1 Nb1 Cl3 79.62(10) . . ? Cl4 Nb1 Cl3 89.75(3) . . ? Cl1 Nb1 Cl3 89.74(3) . . ? C1 Nb1 Cl2 83.63(10) . . ? Cl4 Nb1 Cl2 87.92(3) . . ? Cl1 Nb1 Cl2 87.88(3) . . ? Cl3 Nb1 Cl2 163.25(3) . . ? C1 Nb1 Nb3 136.02(10) . 5_566 ? Cl4 Nb1 Nb3 53.39(2) . 5_566 ? Cl1 Nb1 Nb3 142.86(2) . 5_566 ? Cl3 Nb1 Nb3 95.74(2) . 5_566 ? Cl2 Nb1 Nb3 96.15(2) . 5_566 ? C1 Nb1 Nb2 133.04(10) . 5_566 ? Cl4 Nb1 Nb2 96.80(3) . 5_566 ? Cl1 Nb1 Nb2 96.00(2) . 5_566 ? Cl3 Nb1 Nb2 53.44(2) . 5_566 ? Cl2 Nb1 Nb2 143.30(2) . 5_566 ? Nb3 Nb1 Nb2 59.973(10) 5_566 5_566 ? C1 Nb1 Nb3 134.28(10) . . ? Cl4 Nb1 Nb3 143.01(2) . . ? Cl1 Nb1 Nb3 53.22(2) . . ? Cl3 Nb1 Nb3 96.27(2) . . ? Cl2 Nb1 Nb3 95.55(2) . . ? Nb3 Nb1 Nb3 89.646(12) 5_566 . ? Nb2 Nb1 Nb3 59.877(11) 5_566 . ? C1 Nb1 Nb2 137.08(10) . . ? Cl4 Nb1 Nb2 94.98(2) . . ? Cl1 Nb1 Nb2 95.17(2) . . ? Cl3 Nb1 Nb2 143.30(2) . . ? Cl2 Nb1 Nb2 53.45(2) . . ? Nb3 Nb1 Nb2 59.892(11) 5_566 . ? Nb2 Nb1 Nb2 89.859(12) 5_566 . ? Nb3 Nb1 Nb2 59.685(10) . . ? C2 Nb2 Cl6 81.75(9) . . ? C2 Nb2 Cl3 82.01(9) . 5_566 ? Cl6 Nb2 Cl3 88.35(3) . 5_566 ? C2 Nb2 Cl2 80.76(9) . . ? Cl6 Nb2 Cl2 88.34(3) . . ? Cl3 Nb2 Cl2 162.75(3) 5_566 . ? C2 Nb2 Cl5 80.87(9) . . ? Cl6 Nb2 Cl5 162.61(3) . . ? Cl3 Nb2 Cl5 88.58(3) 5_566 . ? Cl2 Nb2 Cl5 89.54(3) . . ? C2 Nb2 Nb3 135.57(9) . . ? Cl6 Nb2 Nb3 53.83(2) . . ? Cl3 Nb2 Nb3 95.84(2) 5_566 . ? Cl2 Nb2 Nb3 95.84(2) . . ? Cl5 Nb2 Nb3 143.56(2) . . ? C2 Nb2 Nb3 134.63(9) . 5_566 ? Cl6 Nb2 Nb3 143.61(2) . 5_566 ? Cl3 Nb2 Nb3 96.65(2) 5_566 5_566 ? Cl2 Nb2 Nb3 96.04(2) . 5_566 ? Cl5 Nb2 Nb3 53.78(2) . 5_566 ? Nb3 Nb2 Nb3 89.787(12) . 5_566 ? C2 Nb2 Nb1 135.65(9) . 5_566 ? Cl6 Nb2 Nb1 96.15(3) . 5_566 ? Cl3 Nb2 Nb1 53.64(2) 5_566 5_566 ? Cl2 Nb2 Nb1 143.59(2) . 5_566 ? Cl5 Nb2 Nb1 95.79(2) . 5_566 ? Nb3 Nb2 Nb1 59.909(10) . 5_566 ? Nb3 Nb2 Nb1 60.186(11) 5_566 5_566 ? C2 Nb2 Nb1 134.21(9) . . ? Cl6 Nb2 Nb1 96.18(2) . . ? Cl3 Nb2 Nb1 143.78(2) 5_566 . ? Cl2 Nb2 Nb1 53.45(2) . . ? Cl5 Nb2 Nb1 96.40(2) . . ? Nb3 Nb2 Nb1 60.077(11) . . ? Nb3 Nb2 Nb1 59.745(10) 5_566 . ? Nb1 Nb2 Nb1 90.141(12) 5_566 . ? C3 Nb3 Cl4 81.45(10) . 5_566 ? C3 Nb3 Cl1 81.36(10) . . ? Cl4 Nb3 Cl1 162.78(3) 5_566 . ? C3 Nb3 Cl6 80.34(9) . . ? Cl4 Nb3 Cl6 90.06(3) 5_566 . ? Cl1 Nb3 Cl6 88.16(3) . . ? C3 Nb3 Cl5 82.39(9) . 5_566 ? Cl4 Nb3 Cl5 88.25(3) 5_566 5_566 ? Cl1 Nb3 Cl5 88.38(3) . 5_566 ? Cl6 Nb3 Cl5 162.70(3) . 5_566 ? C3 Nb3 Nb1 134.80(10) . 5_566 ? Cl4 Nb3 Nb1 53.40(2) 5_566 5_566 ? Cl1 Nb3 Nb1 143.81(3) . 5_566 ? Cl6 Nb3 Nb1 96.03(2) . 5_566 ? Cl5 Nb3 Nb1 96.75(2) 5_566 5_566 ? C3 Nb3 Nb2 133.78(9) . . ? Cl4 Nb3 Nb2 96.92(2) 5_566 . ? Cl1 Nb3 Nb2 95.76(2) . . ? Cl6 Nb3 Nb2 53.44(2) . . ? Cl5 Nb3 Nb2 143.82(2) 5_566 . ? Nb1 Nb3 Nb2 60.118(11) 5_566 . ? C3 Nb3 Nb2 136.01(9) . 5_566 ? Cl4 Nb3 Nb2 95.34(3) 5_566 5_566 ? Cl1 Nb3 Nb2 96.22(2) . 5_566 ? Cl6 Nb3 Nb2 143.66(2) . 5_566 ? Cl5 Nb3 Nb2 53.62(2) 5_566 5_566 ? Nb1 Nb3 Nb2 60.363(10) 5_566 5_566 ? Nb2 Nb3 Nb2 90.213(12) . 5_566 ? C3 Nb3 Nb1 134.82(10) . . ? Cl4 Nb3 Nb1 143.73(3) 5_566 . ? Cl1 Nb3 Nb1 53.46(2) . . ? Cl6 Nb3 Nb1 96.03(3) . . ? Cl5 Nb3 Nb1 95.49(2) 5_566 . ? Nb1 Nb3 Nb1 90.354(12) 5_566 . ? Nb2 Nb3 Nb1 60.237(10) . . ? Nb2 Nb3 Nb1 59.937(10) 5_566 . ? Nb3 Cl1 Nb1 73.32(3) . . ? Nb2 Cl2 Nb1 73.10(3) . . ? Nb2 Cl3 Nb1 72.92(3) 5_566 . ? Nb3 Cl4 Nb1 73.20(3) 5_566 . ? Nb2 Cl5 Nb3 72.60(3) . 5_566 ? Nb2 Cl6 Nb3 72.73(3) . . ? C2 N2 Mn1 155.0(3) . . ? C3 N3 Mn1 144.2(3) . 3 ? N1 C1 Nb1 175.3(4) . . ? N2 C2 Nb2 174.7(3) . . ? N3 C3 Nb3 175.2(3) . . ? O2 Mn1 O1 95.52(11) . . ? O2 Mn1 N4' 163.3(4) . . ? O1 Mn1 N4' 92.3(6) . . ? O2 Mn1 N5 91.94(13) . . ? O1 Mn1 N5 172.21(13) . . ? N4' Mn1 N5 79.9(6) . . ? O2 Mn1 N4 174.0(5) . . ? O1 Mn1 N4 90.3(5) . . ? N4' Mn1 N4 16.5(4) . . ? N5 Mn1 N4 82.3(5) . . ? O2 Mn1 N2 92.63(12) . . ? O1 Mn1 N2 94.20(11) . . ? N4' Mn1 N2 101.5(4) . . ? N5 Mn1 N2 87.64(12) . . ? N4 Mn1 N2 85.3(3) . . ? O2 Mn1 N3 89.36(12) . 3_545 ? O1 Mn1 N3 91.95(11) . 3_545 ? N4' Mn1 N3 75.6(4) . 3_545 ? N5 Mn1 N3 85.92(12) . 3_545 ? N4 Mn1 N3 92.1(3) . 3_545 ? N2 Mn1 N3 173.33(12) . 3_545 ? C11 O1 Mn1 127.9(2) . . ? C4 O2 Mn1 129.5(2) . . ? C9 N4 C8 124.1(13) . . ? C9 N4 Mn1 120.8(10) . . ? C8 N4 Mn1 112.9(11) . . ? C9 N4' C8' 121.4(16) . . ? C9 N4' Mn1 124.0(13) . . ? C8' N4' Mn1 114.5(13) . . ? C6 N5 C7 120.0(4) . . ? C6 N5 Mn1 125.4(3) . . ? C7 N5 Mn1 114.5(3) . . ? O2 C4 C12 118.5(4) . . ? O2 C4 C5 123.1(4) . . ? C12 C4 C5 118.4(4) . . ? C4 C5 C15 119.3(4) . . ? C4 C5 C6 123.2(4) . . ? C15 C5 C6 117.2(4) . . ? N5 C6 C5 125.8(4) . . ? C8' C7 N5 109.3(5) . . ? C8' C7 C8 50.8(5) . . ? N5 C7 C8 111.3(4) . . ? N4 C8 C7 108.4(7) . . ? C7 C8' N4' 109.1(10) . . ? N4 C9 N4' 25.2(6) . . ? N4 C9 C10 125.5(8) . . ? N4' C9 C10 125.1(10) . . ? C9 C10 C19 118.9(4) . . ? C9 C10 C11 122.1(4) . . ? C19 C10 C11 119.0(4) . . ? O1 C11 C16 118.5(4) . . ? O1 C11 C10 123.7(3) . . ? C16 C11 C10 117.8(4) . . ? C13 C12 C4 121.0(4) . . ? C14 C13 C12 120.8(5) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C5 120.3(5) . . ? C11 C16 C17 120.5(5) . . ? C18 C17 C16 121.8(5) . . ? C19 C18 C17 119.1(5) . . ? C18 C19 C10 121.7(5) . . ? C22 N6 C20 110.0(4) . . ? C22 N6 C21 109.3(4) . . ? C20 N6 C21 108.9(4) . . ? C22 N6 C23 110.1(4) . . ? C20 N6 C23 110.0(3) . . ? C21 N6 C23 108.4(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.875 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.078 data_3 _audit_creation_method SHELXTL-PC _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H84 Cl12 Mn2 N12 Nb6 O8' _chemical_formula_weight 2170.11 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2271(11) _cell_length_b 21.8002(18) _cell_length_c 13.7809(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.648(6) _cell_angle_gamma 90.00 _cell_volume 3965.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 12.51 _exptl_crystal_description 'blcok shape' _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4576 _exptl_absorpt_correction_T_max 0.6412 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12795 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 29.35 _reflns_number_total 10883 _reflns_number_gt 8327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL-PC' _computing_structure_solution 'Bruker SHELXTL-PC' _computing_structure_refinement 'Bruker SHELXTL-PC' _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^)+(0.0352P)^2^+4.5592P] 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 SHELXTL-PC _refine_ls_extinction_coef 0.00049(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10883 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.008 _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 0.10072(2) 0.057072(13) 0.43539(2) 0.01779(7) Uani 1 1 d . . . Nb2 Nb -0.11146(2) 0.066819(13) 0.48260(2) 0.01739(7) Uani 1 1 d . . . Nb3 Nb 0.04592(2) 0.036376(13) 0.63544(2) 0.01764(7) Uani 1 1 d . . . Cl1 Cl 0.17268(7) 0.10996(4) 0.58227(6) 0.02623(18) Uani 1 1 d . . . Cl2 Cl -0.18099(7) 0.03733(4) 0.32049(6) 0.02573(17) Uani 1 1 d . . . Cl3 Cl -0.01181(7) 0.14665(4) 0.40529(6) 0.02416(17) Uani 1 1 d . . . Cl4 Cl 0.25052(6) -0.01079(4) 0.44648(7) 0.02558(17) Uani 1 1 d . . . Cl5 Cl 0.06681(7) 0.02373(4) 0.26515(6) 0.02432(17) Uani 1 1 d . . . Cl6 Cl -0.07911(7) 0.12040(4) 0.63932(6) 0.02459(17) Uani 1 1 d . . . N1 N 0.2596(3) 0.15333(18) 0.3225(3) 0.0411(9) Uani 1 1 d . . . N2 N -0.3010(2) 0.17416(15) 0.4460(2) 0.0302(7) Uani 1 1 d . . . N3 N 0.1355(3) 0.09341(19) 0.8562(3) 0.0439(9) Uani 1 1 d . . . C1 C 0.2087(3) 0.12036(18) 0.3614(3) 0.0274(8) Uani 1 1 d . . . C2 C -0.2370(3) 0.13952(16) 0.4606(3) 0.0241(7) Uani 1 1 d . . . C3 C 0.1020(3) 0.07523(18) 0.7830(3) 0.0282(8) Uani 1 1 d . . . Mn1 Mn -0.44642(4) 0.21438(2) 0.37168(4) 0.02233(11) Uani 1 1 d . . . O1 O -0.3836(2) 0.28025(12) 0.3110(2) 0.0293(6) Uani 1 1 d . . . O2 O -0.4358(2) 0.15888(12) 0.26834(19) 0.0296(6) Uani 1 1 d . . . N4 N -0.4718(2) 0.26614(14) 0.4867(2) 0.0254(6) Uani 1 1 d . . . N5 N -0.5253(2) 0.15402(14) 0.4447(2) 0.0253(6) Uani 1 1 d . . . C4 C -0.3765(3) 0.33842(17) 0.3361(3) 0.0276(8) Uani 1 1 d . . . C5 C -0.3255(3) 0.37931(19) 0.2771(3) 0.0369(9) Uani 1 1 d . . . H5 H -0.2992 0.3647 0.2197 0.044 Uiso 1 1 calc R . . C6 C -0.3134(4) 0.4400(2) 0.3014(4) 0.0450(11) Uani 1 1 d . . . H6 H -0.2771 0.4658 0.2615 0.054 Uiso 1 1 calc R . . C7 C -0.3540(4) 0.4641(2) 0.3844(4) 0.0499(13) Uani 1 1 d . . . H7 H -0.3459 0.5058 0.4002 0.060 Uiso 1 1 calc R . . C8 C -0.4054(4) 0.42614(19) 0.4417(3) 0.0397(10) Uani 1 1 d . . . H8 H -0.4346 0.4425 0.4966 0.048 Uiso 1 1 calc R . . C9 C -0.4166(3) 0.36268(17) 0.4218(3) 0.0288(8) Uani 1 1 d . . . C10 C -0.4614(3) 0.32465(18) 0.4922(3) 0.0301(8) Uani 1 1 d . . . H10 H -0.4851 0.3442 0.5471 0.036 Uiso 1 1 calc R . . C11 C -0.5105(3) 0.23136(19) 0.5685(3) 0.0337(9) Uani 1 1 d . . . H11A H -0.5487 0.2585 0.6096 0.040 Uiso 1 1 calc R . . H11B H -0.4543 0.2133 0.6084 0.040 Uiso 1 1 calc R . . C12 C -0.5785(3) 0.18170(19) 0.5248(3) 0.0337(9) Uani 1 1 d . . . H12A H -0.5916 0.1507 0.5739 0.040 Uiso 1 1 calc R . . H12B H -0.6434 0.1991 0.5001 0.040 Uiso 1 1 calc R . . C13 C -0.5331(3) 0.09672(18) 0.4253(3) 0.0308(8) Uani 1 1 d . . . H13 H -0.5729 0.0729 0.4651 0.037 Uiso 1 1 calc R . . C14 C -0.4866(3) 0.06599(18) 0.3482(3) 0.0314(8) Uani 1 1 d . . . C15 C -0.4893(4) 0.00140(19) 0.3460(4) 0.0408(10) Uani 1 1 d . . . H15 H -0.5227 -0.0198 0.3940 0.049 Uiso 1 1 calc R . . C16 C -0.4442(4) -0.0312(2) 0.2754(4) 0.0468(12) Uani 1 1 d . . . H16 H -0.4444 -0.0743 0.2764 0.056 Uiso 1 1 calc R . . C17 C -0.3985(3) 0.0001(2) 0.2029(3) 0.0413(11) Uani 1 1 d . . . H17 H -0.3684 -0.0220 0.1537 0.050 Uiso 1 1 calc R . . C18 C -0.3964(3) 0.0631(2) 0.2016(3) 0.0351(9) Uani 1 1 d . . . H18 H -0.3652 0.0832 0.1511 0.042 Uiso 1 1 calc R . . C19 C -0.4395(3) 0.09822(18) 0.2739(3) 0.0288(8) Uani 1 1 d . . . O3 O -0.6016(2) 0.24313(13) 0.2976(2) 0.0325(6) Uani 1 1 d . . . H3O H -0.635(4) 0.217(2) 0.298(4) 0.039 Uiso 1 1 d . . . C20 C -0.6570(4) 0.2988(2) 0.2983(4) 0.0513(13) Uani 1 1 d . . . H20A H -0.6878 0.3067 0.2337 0.077 Uiso 1 1 calc R . . H20B H -0.6117 0.3322 0.3175 0.077 Uiso 1 1 calc R . . H20C H -0.7095 0.2955 0.3440 0.077 Uiso 1 1 calc R . . N6 N -0.0862(3) 0.16969(14) 0.0596(2) 0.0289(7) Uani 1 1 d . . . C21 C -0.1601(4) 0.2209(2) 0.0768(4) 0.0428(14) Uani 0.836(6) 1 d P . . C22 C -0.2142(4) 0.2160(3) 0.1709(5) 0.0682(18) Uani 1 1 d . . . C23 C -0.1443(4) 0.1095(2) 0.0473(4) 0.0416(13) Uani 0.836(6) 1 d P . . C24 C -0.0843(5) 0.0549(2) 0.0162(5) 0.0625(16) Uani 1 1 d . . . C25 C -0.0058(4) 0.1635(3) 0.1449(4) 0.0428(14) Uani 0.836(6) 1 d P . . C26 C 0.0531(4) 0.2219(2) 0.1707(4) 0.0506(12) Uani 1 1 d . . . C27 C -0.0297(4) 0.1860(3) -0.0303(4) 0.0394(13) Uani 0.836(6) 1 d P . . C28 C -0.0973(5) 0.1867(3) -0.1239(3) 0.0591(15) Uani 1 1 d . . . C21' C -0.160(2) 0.1692(14) 0.148(2) 0.044(7) Uiso 0.164(6) 1 d P . . C23' C -0.040(2) 0.1038(15) 0.048(2) 0.048(8) Uiso 0.164(6) 1 d P . . C25' C -0.0085(19) 0.2220(11) 0.0697(18) 0.031(5) Uiso 0.164(6) 1 d P . . C27' C -0.161(2) 0.1845(12) -0.0341(19) 0.036(6) Uiso 0.164(6) 1 d P . . O4 O 0.3102(4) 0.3971(2) 0.4935(3) 0.0640(17) Uani 0.850(9) 1 d P A 1 C29 C 0.2808(5) 0.3696(3) 0.5757(5) 0.083(2) Uani 1 1 d . . . H29A H 0.2131 0.3832 0.5885 0.125 Uiso 0.850(9) 1 calc PR A 1 H29B H 0.3274 0.3806 0.6301 0.125 Uiso 1 1 calc R A 1 H29C H 0.2808 0.3255 0.5671 0.125 Uiso 1 1 calc R A 1 O4' O 0.212(2) 0.4047(13) 0.550(2) 0.068(10) Uiso 0.150(9) 1 d P A 2 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 0.01646(13) 0.01819(13) 0.01866(14) 0.00124(11) 0.00066(10) -0.00130(11) Nb2 0.01596(13) 0.01760(13) 0.01844(14) 0.00037(11) -0.00023(10) 0.00182(11) Nb3 0.01737(14) 0.01857(13) 0.01672(13) -0.00070(11) -0.00103(10) 0.00001(11) Cl1 0.0258(4) 0.0265(4) 0.0260(4) -0.0025(3) -0.0011(3) -0.0083(3) Cl2 0.0234(4) 0.0291(4) 0.0236(4) -0.0011(3) -0.0069(3) 0.0052(3) Cl3 0.0266(4) 0.0192(4) 0.0268(4) 0.0046(3) 0.0024(3) 0.0011(3) Cl4 0.0170(4) 0.0282(4) 0.0319(4) 0.0028(3) 0.0044(3) 0.0011(3) Cl5 0.0268(4) 0.0278(4) 0.0185(4) 0.0018(3) 0.0027(3) -0.0016(3) Cl6 0.0284(4) 0.0222(4) 0.0230(4) -0.0044(3) -0.0002(3) 0.0053(3) N1 0.0345(19) 0.048(2) 0.040(2) 0.0108(17) -0.0004(16) -0.0137(17) N2 0.0246(16) 0.0282(16) 0.0375(18) -0.0004(14) -0.0013(14) 0.0040(13) N3 0.048(2) 0.050(2) 0.0327(19) -0.0104(17) -0.0033(17) -0.0040(19) C1 0.0220(17) 0.0323(19) 0.0277(18) 0.0056(15) -0.0003(14) -0.0033(15) C2 0.0230(17) 0.0239(16) 0.0254(17) -0.0025(14) 0.0006(14) -0.0002(14) C3 0.0267(18) 0.0304(18) 0.0275(19) -0.0026(15) 0.0025(15) -0.0006(15) Mn1 0.0210(3) 0.0228(3) 0.0235(3) 0.0014(2) 0.0039(2) 0.0010(2) O1 0.0306(14) 0.0257(13) 0.0328(14) 0.0026(11) 0.0105(12) -0.0003(11) O2 0.0351(15) 0.0276(13) 0.0265(13) -0.0024(11) 0.0046(11) 0.0003(11) N4 0.0218(15) 0.0306(16) 0.0240(15) 0.0011(12) 0.0036(12) 0.0010(12) N5 0.0235(15) 0.0266(15) 0.0261(15) 0.0055(12) 0.0033(12) -0.0001(12) C4 0.0202(17) 0.0284(18) 0.034(2) 0.0024(15) -0.0012(15) 0.0009(14) C5 0.034(2) 0.035(2) 0.043(2) 0.0065(18) 0.0057(18) -0.0057(17) C6 0.049(3) 0.038(2) 0.047(3) 0.015(2) -0.003(2) -0.015(2) C7 0.071(4) 0.027(2) 0.050(3) 0.005(2) -0.012(3) -0.010(2) C8 0.052(3) 0.029(2) 0.037(2) -0.0029(18) -0.006(2) -0.0002(19) C9 0.031(2) 0.0254(17) 0.0296(19) 0.0007(15) -0.0014(16) -0.0013(15) C10 0.0283(19) 0.034(2) 0.0279(19) -0.0055(16) 0.0025(15) 0.0017(16) C11 0.039(2) 0.036(2) 0.0264(19) 0.0027(16) 0.0094(17) -0.0026(18) C12 0.032(2) 0.038(2) 0.032(2) 0.0040(17) 0.0091(17) -0.0051(17) C13 0.029(2) 0.0314(19) 0.031(2) 0.0067(16) -0.0026(16) -0.0044(16) C14 0.0277(19) 0.0293(19) 0.036(2) 0.0006(16) -0.0082(16) -0.0025(15) C15 0.045(3) 0.027(2) 0.049(3) 0.0028(19) -0.007(2) -0.0050(18) C16 0.053(3) 0.031(2) 0.055(3) -0.009(2) -0.011(2) 0.003(2) C17 0.037(2) 0.037(2) 0.049(3) -0.018(2) -0.011(2) 0.0076(18) C18 0.028(2) 0.041(2) 0.035(2) -0.0084(18) -0.0036(16) 0.0031(17) C19 0.0237(18) 0.0291(18) 0.032(2) -0.0021(15) -0.0089(15) 0.0012(15) O3 0.0241(14) 0.0284(14) 0.0447(17) 0.0073(13) -0.0001(12) -0.0037(11) C20 0.051(3) 0.036(2) 0.064(3) 0.005(2) -0.013(3) 0.011(2) N6 0.0357(18) 0.0275(15) 0.0240(15) 0.0022(13) 0.0044(13) 0.0062(14) C21 0.040(3) 0.032(3) 0.056(4) -0.012(2) -0.001(3) 0.012(2) C22 0.050(3) 0.087(4) 0.071(4) -0.035(3) 0.027(3) -0.003(3) C23 0.045(3) 0.028(2) 0.052(3) -0.001(2) 0.012(3) -0.005(2) C24 0.082(4) 0.033(2) 0.071(4) -0.008(2) -0.006(3) 0.012(3) C25 0.048(3) 0.051(3) 0.028(3) 0.006(2) -0.007(2) 0.010(3) C26 0.046(3) 0.057(3) 0.046(3) -0.008(2) -0.014(2) 0.001(2) C27 0.046(3) 0.045(3) 0.027(2) 0.006(2) 0.007(2) -0.005(2) C28 0.079(4) 0.075(4) 0.022(2) 0.002(2) -0.006(2) -0.007(3) O4 0.056(3) 0.090(4) 0.046(3) -0.007(2) 0.005(2) -0.013(3) C29 0.067(4) 0.096(5) 0.086(5) 0.035(4) 0.005(4) 0.003(4) _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 C1 2.274(4) . ? Nb1 Cl1 2.4672(9) . ? Nb1 Cl4 2.4696(9) . ? Nb1 Cl5 2.4698(9) . ? Nb1 Cl3 2.4745(9) . ? Nb1 Nb2 2.9277(5) 3_556 ? Nb1 Nb2 2.9287(5) . ? Nb1 Nb3 2.9297(5) . ? Nb1 Nb3 2.9368(4) 3_556 ? Nb2 C2 2.302(4) . ? Nb2 Cl2 2.4473(9) . ? Nb2 Cl4 2.4616(9) 3_556 ? Nb2 Cl3 2.4658(9) . ? Nb2 Cl6 2.4686(9) . ? Nb2 Nb1 2.9277(5) 3_556 ? Nb2 Nb3 2.9391(4) 3_556 ? Nb2 Nb3 2.9415(5) . ? Nb3 C3 2.283(4) . ? Nb3 Cl2 2.4504(9) 3_556 ? Nb3 Cl5 2.4652(9) 3_556 ? Nb3 Cl1 2.4653(9) . ? Nb3 Cl6 2.4707(9) . ? Nb3 Nb1 2.9368(4) 3_556 ? Nb3 Nb2 2.9391(4) 3_556 ? Cl2 Nb3 2.4504(9) 3_556 ? Cl4 Nb2 2.4616(9) 3_556 ? Cl5 Nb3 2.4652(9) 3_556 ? N1 C1 1.141(5) . ? N2 C2 1.143(5) . ? N2 Mn1 2.295(3) . ? N3 C3 1.146(5) . ? Mn1 O2 1.881(3) . ? Mn1 O1 1.881(3) . ? Mn1 N4 1.992(3) . ? Mn1 N5 1.992(3) . ? Mn1 O3 2.320(3) . ? O1 C4 1.316(4) . ? O2 C19 1.326(4) . ? N4 C10 1.285(5) . ? N4 C11 1.477(5) . ? N5 C13 1.281(5) . ? N5 C12 1.476(5) . ? C4 C5 1.408(5) . ? C4 C9 1.427(5) . ? C5 C6 1.372(6) . ? C6 C7 1.396(7) . ? C7 C8 1.356(7) . ? C8 C9 1.416(5) . ? C9 C10 1.432(5) . ? C11 C12 1.508(6) . ? C13 C14 1.428(6) . ? C14 C15 1.409(5) . ? C14 C19 1.419(6) . ? C15 C16 1.372(7) . ? C16 C17 1.381(7) . ? C17 C18 1.374(6) . ? C18 C19 1.405(6) . ? O3 C20 1.418(5) . ? N6 C21 1.513(6) . ? N6 C23 1.524(6) . ? N6 C27 1.529(6) . ? N6 C25' 1.54(2) . ? N6 C25 1.540(6) . ? N6 C23' 1.58(3) . ? N6 C21' 1.60(3) . ? N6 C27' 1.61(3) . ? C21 C21' 1.49(3) . ? C21 C22 1.524(8) . ? C21 C27' 1.72(3) . ? C21 C25' 2.01(3) . ? C22 C21' 1.30(3) . ? C23 C23' 1.39(3) . ? C23 C24 1.509(7) . ? C23 C21' 1.92(3) . ? C23 C27' 1.99(3) . ? C24 C23' 1.28(3) . ? C25 C26 1.524(8) . ? C25 C25' 1.64(2) . ? C25 C23' 1.90(3) . ? C25 C21' 2.04(3) . ? C26 C25' 1.57(3) . ? C27 C28 1.521(7) . ? C27 C25' 1.60(2) . ? C27 C27' 1.73(3) . ? C28 C27' 1.54(3) . ? O4 C29 1.359(7) . ? C29 O4' 1.22(3) . ? 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 C1 Nb1 Cl1 82.18(10) . . ? C1 Nb1 Cl4 82.34(10) . . ? Cl1 Nb1 Cl4 87.89(3) . . ? C1 Nb1 Cl5 80.43(10) . . ? Cl1 Nb1 Cl5 162.58(3) . . ? Cl4 Nb1 Cl5 88.80(3) . . ? C1 Nb1 Cl3 80.46(10) . . ? Cl1 Nb1 Cl3 88.01(3) . . ? Cl4 Nb1 Cl3 162.71(3) . . ? Cl5 Nb1 Cl3 90.11(3) . . ? C1 Nb1 Nb2 135.77(10) . 3_556 ? Cl1 Nb1 Nb2 96.19(2) . 3_556 ? Cl4 Nb1 Nb2 53.45(2) . 3_556 ? Cl5 Nb1 Nb2 95.54(2) . 3_556 ? Cl3 Nb1 Nb2 143.77(2) . 3_556 ? C1 Nb1 Nb2 133.94(10) . . ? Cl1 Nb1 Nb2 96.25(2) . . ? Cl4 Nb1 Nb2 143.72(2) . . ? Cl5 Nb1 Nb2 96.53(2) . . ? Cl3 Nb1 Nb2 53.51(2) . . ? Nb2 Nb1 Nb2 90.276(12) 3_556 . ? C1 Nb1 Nb3 135.70(10) . . ? Cl1 Nb1 Nb3 53.53(2) . . ? Cl4 Nb1 Nb3 95.46(2) . . ? Cl5 Nb1 Nb3 143.87(2) . . ? Cl3 Nb1 Nb3 95.57(2) . . ? Nb2 Nb1 Nb3 60.234(10) 3_556 . ? Nb2 Nb1 Nb3 60.276(11) . . ? C1 Nb1 Nb3 133.81(10) . 3_556 ? Cl1 Nb1 Nb3 144.00(2) . 3_556 ? Cl4 Nb1 Nb3 96.62(2) . 3_556 ? Cl5 Nb1 Nb3 53.41(2) . 3_556 ? Cl3 Nb1 Nb3 96.56(2) . 3_556 ? Nb2 Nb1 Nb3 60.208(11) 3_556 3_556 ? Nb2 Nb1 Nb3 60.143(11) . 3_556 ? Nb3 Nb1 Nb3 90.471(12) . 3_556 ? C2 Nb2 Cl2 80.49(9) . . ? C2 Nb2 Cl4 80.96(9) . 3_556 ? Cl2 Nb2 Cl4 89.15(3) . 3_556 ? C2 Nb2 Cl3 81.85(9) . . ? Cl2 Nb2 Cl3 88.35(3) . . ? Cl4 Nb2 Cl3 162.80(3) 3_556 . ? C2 Nb2 Cl6 82.69(9) . . ? Cl2 Nb2 Cl6 163.16(3) . . ? Cl4 Nb2 Cl6 88.84(3) 3_556 . ? Cl3 Nb2 Cl6 88.65(3) . . ? C2 Nb2 Nb1 134.66(9) . 3_556 ? Cl2 Nb2 Nb1 96.67(2) . 3_556 ? Cl4 Nb2 Nb1 53.71(2) 3_556 3_556 ? Cl3 Nb2 Nb1 143.49(2) . 3_556 ? Cl6 Nb2 Nb1 95.59(2) . 3_556 ? C2 Nb2 Nb1 135.59(9) . . ? Cl2 Nb2 Nb1 95.04(2) . . ? Cl4 Nb2 Nb1 143.42(2) 3_556 . ? Cl3 Nb2 Nb1 53.78(2) . . ? Cl6 Nb2 Nb1 96.52(2) . . ? Nb1 Nb2 Nb1 89.724(12) 3_556 . ? C2 Nb2 Nb3 133.63(9) . 3_556 ? Cl2 Nb2 Nb3 53.17(2) . 3_556 ? Cl4 Nb2 Nb3 95.40(2) 3_556 3_556 ? Cl3 Nb2 Nb3 96.69(2) . 3_556 ? Cl6 Nb2 Nb3 143.67(2) . 3_556 ? Nb1 Nb2 Nb3 59.917(11) 3_556 3_556 ? Nb1 Nb2 Nb3 60.064(10) . 3_556 ? C2 Nb2 Nb3 136.17(9) . . ? Cl2 Nb2 Nb3 143.34(2) . . ? Cl4 Nb2 Nb3 96.68(2) 3_556 . ? Cl3 Nb2 Nb3 95.47(2) . . ? Cl6 Nb2 Nb3 53.48(2) . . ? Nb1 Nb2 Nb3 60.049(10) 3_556 . ? Nb1 Nb2 Nb3 59.878(11) . . ? Nb3 Nb2 Nb3 90.195(12) 3_556 . ? C3 Nb3 Cl2 80.32(10) . 3_556 ? C3 Nb3 Cl5 82.88(10) . 3_556 ? Cl2 Nb3 Cl5 88.34(3) 3_556 3_556 ? C3 Nb3 Cl1 80.48(10) . . ? Cl2 Nb3 Cl1 90.08(3) 3_556 . ? Cl5 Nb3 Cl1 163.31(3) 3_556 . ? C3 Nb3 Cl6 83.44(10) . . ? Cl2 Nb3 Cl6 163.59(3) 3_556 . ? Cl5 Nb3 Cl6 87.29(3) 3_556 . ? Cl1 Nb3 Cl6 89.59(3) . . ? C3 Nb3 Nb1 134.04(10) . . ? Cl2 Nb3 Nb1 96.55(2) 3_556 . ? Cl5 Nb3 Nb1 143.07(2) 3_556 . ? Cl1 Nb3 Nb1 53.59(2) . . ? Cl6 Nb3 Nb1 96.44(2) . . ? C3 Nb3 Nb1 136.38(10) . 3_556 ? Cl2 Nb3 Nb1 94.78(2) 3_556 3_556 ? Cl5 Nb3 Nb1 53.55(2) 3_556 3_556 ? Cl1 Nb3 Nb1 143.12(2) . 3_556 ? Cl6 Nb3 Nb1 95.31(2) . 3_556 ? Nb1 Nb3 Nb1 89.529(12) . 3_556 ? C3 Nb3 Nb2 133.35(10) . 3_556 ? Cl2 Nb3 Nb2 53.07(2) 3_556 3_556 ? Cl5 Nb3 Nb2 96.36(2) 3_556 3_556 ? Cl1 Nb3 Nb2 95.94(2) . 3_556 ? Cl6 Nb3 Nb2 143.21(2) . 3_556 ? Nb1 Nb3 Nb2 59.849(11) . 3_556 ? Nb1 Nb3 Nb2 59.793(11) 3_556 3_556 ? C3 Nb3 Nb2 136.83(10) . . ? Cl2 Nb3 Nb2 142.85(2) 3_556 . ? Cl5 Nb3 Nb2 95.30(2) 3_556 . ? Cl1 Nb3 Nb2 95.97(2) . . ? Cl6 Nb3 Nb2 53.42(2) . . ? Nb1 Nb3 Nb2 59.845(11) . . ? Nb1 Nb3 Nb2 59.743(11) 3_556 . ? Nb2 Nb3 Nb2 89.805(12) 3_556 . ? Nb3 Cl1 Nb1 72.88(3) . . ? Nb2 Cl2 Nb3 73.75(2) . 3_556 ? Nb2 Cl3 Nb1 72.72(2) . . ? Nb2 Cl4 Nb1 72.84(3) 3_556 . ? Nb3 Cl5 Nb1 73.04(2) 3_556 . ? Nb2 Cl6 Nb3 73.10(2) . . ? C2 N2 Mn1 157.2(3) . . ? N1 C1 Nb1 177.2(4) . . ? N2 C2 Nb2 176.8(3) . . ? N3 C3 Nb3 176.1(4) . . ? O2 Mn1 O1 95.65(12) . . ? O2 Mn1 N4 172.58(13) . . ? O1 Mn1 N4 91.31(12) . . ? O2 Mn1 N5 91.39(12) . . ? O1 Mn1 N5 171.58(12) . . ? N4 Mn1 N5 81.47(13) . . ? O2 Mn1 N2 89.51(12) . . ? O1 Mn1 N2 96.23(12) . . ? N4 Mn1 N2 92.31(12) . . ? N5 Mn1 N2 88.44(12) . . ? O2 Mn1 O3 86.96(12) . . ? O1 Mn1 O3 90.11(11) . . ? N4 Mn1 O3 90.45(12) . . ? N5 Mn1 O3 85.64(11) . . ? N2 Mn1 O3 173.03(11) . . ? C4 O1 Mn1 130.1(3) . . ? C19 O2 Mn1 126.4(3) . . ? C10 N4 C11 120.4(3) . . ? C10 N4 Mn1 125.9(3) . . ? C11 N4 Mn1 113.6(2) . . ? C13 N5 C12 121.3(3) . . ? C13 N5 Mn1 125.2(3) . . ? C12 N5 Mn1 113.5(2) . . ? O1 C4 C5 119.1(4) . . ? O1 C4 C9 123.4(3) . . ? C5 C4 C9 117.4(4) . . ? C6 C5 C4 121.5(4) . . ? C5 C6 C7 121.1(4) . . ? C8 C7 C6 118.8(4) . . ? C7 C8 C9 122.2(4) . . ? C8 C9 C4 118.9(4) . . ? C8 C9 C10 118.5(4) . . ? C4 C9 C10 122.5(3) . . ? N4 C10 C9 125.6(4) . . ? N4 C11 C12 106.9(3) . . ? N5 C12 C11 106.9(3) . . ? N5 C13 C14 125.5(4) . . ? C15 C14 C19 119.4(4) . . ? C15 C14 C13 118.3(4) . . ? C19 C14 C13 122.3(4) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C17 119.2(4) . . ? C18 C17 C16 120.9(4) . . ? C17 C18 C19 121.7(4) . . ? O2 C19 C18 119.0(4) . . ? O2 C19 C14 123.7(4) . . ? C18 C19 C14 117.3(4) . . ? C20 O3 Mn1 132.2(3) . . ? C21 N6 C23 109.1(4) . . ? C21 N6 C27 108.0(4) . . ? C23 N6 C27 112.2(4) . . ? C21 N6 C25' 82.6(9) . . ? C23 N6 C25' 168.3(10) . . ? C27 N6 C25' 62.8(9) . . ? C21 N6 C25 111.5(4) . . ? C23 N6 C25 109.2(4) . . ? C27 N6 C25 106.8(4) . . ? C25' N6 C25 64.6(10) . . ? C21 N6 C23' 161.8(12) . . ? C23 N6 C23' 53.3(12) . . ? C27 N6 C23' 85.2(12) . . ? C25' N6 C23' 115.0(15) . . ? C25 N6 C23' 74.9(12) . . ? C21 N6 C21' 57.1(11) . . ? C23 N6 C21' 75.7(11) . . ? C27 N6 C21' 165.2(11) . . ? C25' N6 C21' 111.8(14) . . ? C25 N6 C21' 81.0(11) . . ? C23' N6 C21' 109.2(16) . . ? C21 N6 C27' 66.9(10) . . ? C23 N6 C27' 78.7(10) . . ? C27 N6 C27' 67.0(10) . . ? C25' N6 C27' 107.3(13) . . ? C25 N6 C27' 171.8(10) . . ? C23' N6 C27' 109.1(15) . . ? C21' N6 C27' 103.8(15) . . ? C21' C21 N6 64.4(12) . . ? C21' C21 C22 51.2(12) . . ? N6 C21 C22 115.1(5) . . ? C21' C21 C27' 103.3(15) . . ? N6 C21 C27' 59.2(9) . . ? C22 C21 C27' 138.2(10) . . ? C21' C21 C25' 94.4(14) . . ? N6 C21 C25' 49.2(7) . . ? C22 C21 C25' 124.4(8) . . ? C27' C21 C25' 85.0(12) . . ? C21' C22 C21 63.1(13) . . ? C23' C23 C24 52.4(13) . . ? C23' C23 N6 65.3(13) . . ? C24 C23 N6 116.2(5) . . ? C23' C23 C21' 101.8(16) . . ? C24 C23 C21' 145.3(10) . . ? N6 C23 C21' 54.0(9) . . ? C23' C23 C27' 98.9(16) . . ? C24 C23 C27' 122.1(9) . . ? N6 C23 C27' 52.6(8) . . ? C21' C23 C27' 80.6(12) . . ? C23' C24 C23 59.0(14) . . ? C26 C25 N6 115.0(4) . . ? C26 C25 C25' 59.2(9) . . ? N6 C25 C25' 57.6(9) . . ? C26 C25 C23' 146.4(10) . . ? N6 C25 C23' 53.4(10) . . ? C25' C25 C23' 95.5(13) . . ? C26 C25 C21' 116.1(9) . . ? N6 C25 C21' 50.8(9) . . ? C25' C25 C21' 89.0(12) . . ? C23' C25 C21' 82.2(13) . . ? C25 C26 C25' 64.2(9) . . ? C28 C27 N6 113.5(4) . . ? C28 C27 C25' 142.0(10) . . ? N6 C27 C25' 58.8(9) . . ? C28 C27 C27' 56.0(9) . . ? N6 C27 C27' 58.7(9) . . ? C25' C27 C27' 99.0(13) . . ? C27 C28 C27' 68.9(10) . . ? C22 C21' C21 65.7(14) . . ? C22 C21' N6 124(2) . . ? C21 C21' N6 58.5(11) . . ? C22 C21' C23 143(2) . . ? C21 C21' C23 92.2(15) . . ? N6 C21' C23 50.4(9) . . ? C22 C21' C25 128(2) . . ? C21 C21' C25 89.9(15) . . ? N6 C21' C25 48.2(8) . . ? C23 C21' C25 78.2(11) . . ? C24 C23' C23 68.6(16) . . ? C24 C23' N6 128(2) . . ? C23 C23' N6 61.5(13) . . ? C24 C23' C25 154(2) . . ? C23 C23' C25 97.7(18) . . ? N6 C23' C25 51.7(10) . . ? N6 C25' C26 112.8(15) . . ? N6 C25' C27 58.4(9) . . ? C26 C25' C27 145.0(17) . . ? N6 C25' C25 57.8(9) . . ? C26 C25' C25 56.6(9) . . ? C27 C25' C25 99.0(13) . . ? N6 C25' C21 48.2(7) . . ? C26 C25' C21 114.8(14) . . ? C27 C25' C21 85.1(11) . . ? C25 C25' C21 86.7(11) . . ? C28 C27' N6 108.2(16) . . ? C28 C27' C21 136.5(18) . . ? N6 C27' C21 53.9(9) . . ? C28 C27' C27 55.0(9) . . ? N6 C27' C27 54.3(9) . . ? C21 C27' C27 90.9(13) . . ? C28 C27' C23 115.7(15) . . ? N6 C27' C23 48.8(8) . . ? C21 C27' C23 83.3(11) . . ? C27 C27' C23 85.6(12) . . ? O4' C29 O4 74.5(14) . . ? 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 H3O N1 0.72(5) 2.01(5) 2.720(4) 169(5) 1_455 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.685 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.123