# ic001110+.cif data_sg261a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 N8 Nb2 O2' _chemical_formula_weight 798.55 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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.079(3) _cell_length_b 9.551(3) _cell_length_c 10.571(4) _cell_angle_alpha 83.476(6) _cell_angle_beta 89.613(6) _cell_angle_gamma 69.641(5) _cell_volume 853.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 406 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.561012 _exptl_absorpt_correction_T_max 0.928074 _exptl_absorpt_process_details 'Blessing,R., Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 6608 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.1531 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.68 _reflns_number_total 3830 _reflns_number_gt 2287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two peaks in the final diff map > 1 are located 0.9 Angstrom from the Nb atom position. ; _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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3830 _refine_ls_number_parameters 221 _refine_ls_number_restraints 225 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 0.984 _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 Nb Nb 0.47634(7) 0.10899(7) 0.43547(6) 0.0276(2) Uani 1 1 d U . . N1 N 0.7442(6) -0.0915(6) 0.6511(5) 0.0331(12) Uani 1 1 d U . . N2 N 0.6919(6) 0.1341(5) 0.5053(5) 0.0343(12) Uani 1 1 d U . . C1 C 0.8435(7) -0.1810(7) 0.7436(6) 0.0379(16) Uani 1 1 d U . . H1A H 0.8253 -0.2668 0.7821 0.045 Uiso 1 1 calc R . . C2 C 0.9717(8) -0.1504(8) 0.7839(7) 0.0465(18) Uani 1 1 d U . . H2A H 1.0395 -0.2182 0.8478 0.056 Uiso 1 1 calc R . . C3 C 1.0053(8) -0.0277(9) 0.7363(8) 0.0525(19) Uani 1 1 d U . . H3A H 1.0917 -0.0081 0.7682 0.063 Uiso 1 1 calc R . . C4 C 0.9091(8) 0.0664(8) 0.6405(7) 0.0423(16) Uani 1 1 d U . . C5 C 0.7797(7) 0.0305(7) 0.6012(6) 0.0317(14) Uani 1 1 d U . . C6 C 0.8965(8) 0.2047(8) 0.5600(7) 0.0456(17) Uani 1 1 d U . . H6A H 0.9648 0.2594 0.5603 0.055 Uiso 1 1 calc R . . C7 C 0.7657(8) 0.2379(7) 0.4847(7) 0.0427(17) Uani 1 1 d U . . H7A H 0.7290 0.3236 0.4242 0.051 Uiso 1 1 calc R . . N3 N 0.5964(6) -0.0165(6) 0.2753(5) 0.0341(12) Uani 1 1 d U . . N4 N 0.6768(6) -0.2380(5) 0.4247(5) 0.0339(12) Uani 1 1 d U . . C8 C 0.6118(8) 0.0298(8) 0.1498(7) 0.0400(15) Uani 1 1 d U . . H8A H 0.5587 0.1308 0.1175 0.048 Uiso 1 1 calc R . . C9 C 0.7026(9) -0.0672(11) 0.0700(8) 0.060(2) Uani 1 1 d U . . H9A H 0.7080 -0.0282 -0.0149 0.072 Uiso 1 1 calc R . . C10 C 0.7802(12) -0.2067(13) 0.1026(11) 0.060(3) Uani 0.80(2) 1 d PU . . H10A H 0.8411 -0.2685 0.0444 0.072 Uiso 1 1 calc R . . C10' C 0.862(5) -0.377(6) 0.209(5) 0.060(3) Uani 0.20 1 d PU . . C11 C 0.7709(9) -0.2578(10) 0.2185(8) 0.0539(18) Uani 1 1 d U . . C12 C 0.6792(7) -0.1655(7) 0.3064(7) 0.0340(14) Uani 1 1 d U . . C13 C 0.8417(9) -0.4199(9) 0.3071(10) 0.064(2) Uani 1 1 d U . . H13A H 0.9106 -0.5121 0.2848 0.077 Uiso 1 1 calc R . . C14 C 0.7748(8) -0.3875(7) 0.4233(8) 0.0445(17) Uani 1 1 d U . . H14A H 0.7936 -0.4600 0.4950 0.053 Uiso 1 1 calc R . . O1 O 0.3639(12) 0.4363(9) 0.1702(11) 0.148(4) Uani 1 1 d U . . C15 C 0.2463(14) 0.5448(14) 0.1021(15) 0.132(5) Uani 1 1 d U . . H15A H 0.1466 0.5539 0.1429 0.158 Uiso 1 1 calc R . . H15B H 0.2401 0.5163 0.0166 0.158 Uiso 1 1 calc R . . C16 C 0.2670(13) 0.6829(11) 0.0917(11) 0.093(3) Uani 1 1 d U . . H16A H 0.1735 0.7598 0.1198 0.111 Uiso 1 1 calc R . . H16B H 0.2846 0.7140 0.0031 0.111 Uiso 1 1 calc R . . C17 C 0.4049(11) 0.6645(12) 0.1733(10) 0.088(3) Uani 1 1 d U . . H17A H 0.3767 0.7328 0.2392 0.106 Uiso 1 1 calc R . . H17B H 0.4885 0.6834 0.1229 0.106 Uiso 1 1 calc R . . C18 C 0.4546(14) 0.5043(15) 0.2309(12) 0.114(4) Uani 1 1 d U . . H18A H 0.5667 0.4526 0.2181 0.137 Uiso 1 1 calc R . . H18B H 0.4371 0.4987 0.3226 0.137 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 Nb 0.0290(3) 0.0293(3) 0.0254(3) -0.0098(2) 0.0014(2) -0.00934(19) N1 0.029(3) 0.035(3) 0.032(3) -0.006(2) -0.002(2) -0.007(2) N2 0.038(3) 0.033(3) 0.034(3) -0.005(2) 0.001(2) -0.015(2) C1 0.043(4) 0.040(4) 0.028(4) -0.003(3) -0.001(3) -0.012(3) C2 0.040(4) 0.057(4) 0.039(5) -0.006(3) -0.007(3) -0.011(3) C3 0.045(4) 0.064(4) 0.053(5) -0.020(4) 0.002(3) -0.020(3) C4 0.040(4) 0.050(4) 0.040(4) -0.020(3) 0.000(3) -0.015(3) C5 0.031(3) 0.034(3) 0.032(4) -0.012(3) 0.004(3) -0.011(3) C6 0.041(4) 0.051(4) 0.057(5) -0.017(3) 0.008(3) -0.027(3) C7 0.047(4) 0.035(3) 0.049(5) -0.001(3) 0.002(3) -0.020(3) N3 0.035(3) 0.049(3) 0.021(3) -0.007(2) 0.004(2) -0.017(2) N4 0.035(3) 0.030(3) 0.038(3) -0.010(2) 0.007(2) -0.010(2) C8 0.039(4) 0.055(4) 0.030(4) -0.010(3) 0.008(3) -0.020(3) C9 0.053(5) 0.093(5) 0.041(5) -0.031(4) 0.012(4) -0.025(4) C10 0.056(6) 0.081(6) 0.053(5) -0.032(5) 0.009(5) -0.029(4) C10' 0.056(6) 0.081(6) 0.053(5) -0.032(5) 0.009(5) -0.029(4) C11 0.044(4) 0.083(5) 0.046(4) -0.036(3) 0.017(4) -0.028(4) C12 0.027(3) 0.042(3) 0.037(4) -0.015(3) 0.005(3) -0.014(3) C13 0.062(5) 0.058(4) 0.086(6) -0.045(4) 0.030(5) -0.026(4) C14 0.045(4) 0.035(3) 0.054(5) -0.013(3) 0.007(3) -0.011(3) O1 0.145(8) 0.083(5) 0.209(11) 0.028(6) -0.040(7) -0.042(5) C15 0.102(8) 0.097(7) 0.206(14) 0.003(8) -0.047(8) -0.053(7) C16 0.108(8) 0.073(5) 0.095(8) 0.006(5) -0.030(6) -0.034(5) C17 0.082(6) 0.095(6) 0.092(8) -0.031(6) -0.003(6) -0.030(5) C18 0.099(8) 0.136(9) 0.085(9) 0.026(7) -0.020(6) -0.023(7) _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 Nb N2 2.195(5) . ? Nb N4 2.198(5) 2_656 ? Nb N3 2.240(5) . ? Nb Nb 2.2628(14) 2_656 ? Nb N1 2.273(5) 2_656 ? N1 C1 1.336(7) . ? N1 C5 1.364(8) . ? N1 Nb 2.273(5) 2_656 ? N2 C5 1.370(8) . ? N2 C7 1.375(8) . ? C1 C2 1.376(9) . ? C2 C3 1.354(10) . ? C3 C4 1.362(10) . ? C4 C5 1.411(8) . ? C4 C6 1.457(10) . ? C6 C7 1.356(9) . ? N3 C12 1.361(8) . ? N3 C8 1.372(8) . ? N4 C12 1.362(8) . ? N4 C14 1.397(8) . ? N4 Nb 2.198(5) 2_656 ? C8 C9 1.373(10) . ? C9 C10 1.279(13) . ? C10 C11 1.279(13) . ? C11 C12 1.415(10) . ? C11 C13 1.635(13) . ? C13 C14 1.386(11) . ? O1 C15 1.343(13) . ? O1 C18 1.409(13) . ? C15 C16 1.388(14) . ? C16 C17 1.473(12) . ? C17 C18 1.493(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Nb N4 95.42(19) . 2_656 ? N2 Nb N3 93.40(19) . . ? N4 Nb N3 170.76(17) 2_656 . ? N2 Nb Nb 91.73(14) . 2_656 ? N4 Nb Nb 91.41(14) 2_656 2_656 ? N3 Nb Nb 91.08(14) . 2_656 ? N2 Nb N1 175.8(2) . 2_656 ? N4 Nb N1 86.77(18) 2_656 2_656 ? N3 Nb N1 84.26(18) . 2_656 ? Nb Nb N1 91.85(14) 2_656 2_656 ? C1 N1 C5 115.1(5) . . ? C1 N1 Nb 130.3(4) . 2_656 ? C5 N1 Nb 114.7(4) . 2_656 ? C5 N2 C7 104.8(5) . . ? C5 N2 Nb 118.3(4) . . ? C7 N2 Nb 136.7(4) . . ? N1 C1 C2 121.6(6) . . ? C3 C2 C1 123.4(7) . . ? C2 C3 C4 117.4(7) . . ? C3 C4 C5 117.4(7) . . ? C3 C4 C6 138.1(7) . . ? C5 C4 C6 104.5(6) . . ? N1 C5 N2 123.3(5) . . ? N1 C5 C4 125.0(6) . . ? N2 C5 C4 111.6(6) . . ? C7 C6 C4 105.6(6) . . ? C6 C7 N2 113.5(6) . . ? C12 N3 C8 111.7(6) . . ? C12 N3 Nb 116.0(4) . . ? C8 N3 Nb 132.1(5) . . ? C12 N4 C14 106.9(6) . . ? C12 N4 Nb 117.8(4) . 2_656 ? C14 N4 Nb 135.2(5) . 2_656 ? N3 C8 C9 121.9(7) . . ? C10 C9 C8 124.9(10) . . ? C11 C10 C9 116.6(11) . . ? C10 C11 C12 122.0(10) . . ? C10 C11 C13 136.7(9) . . ? C12 C11 C13 101.3(7) . . ? N3 C12 N4 122.2(6) . . ? N3 C12 C11 122.9(7) . . ? N4 C12 C11 114.8(7) . . ? C14 C13 C11 102.6(6) . . ? C13 C14 N4 114.3(7) . . ? C15 O1 C18 108.5(9) . . ? O1 C15 C16 112.1(10) . . ? C15 C16 C17 107.2(10) . . ? C16 C17 C18 103.4(9) . . ? O1 C18 C17 107.4(8) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 1.859 _refine_diff_density_min -2.173 _refine_diff_density_rms 0.193 #===END