data_UP9177 # Crystallographer: Brian C. Manor _audit_creation_date 2015-11-02 _audit_creation_method ; Olex2 1.2-dev (compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_formula_moiety 'C40 H63 N Nb O P2, C5 H12' _chemical_formula_sum 'C45 H75 N Nb O P2' _chemical_formula_weight 800.91 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' 'Nb' 'Nb' -2.0727 0.6215 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3046(12) _cell_length_b 12.9264(13) _cell_length_c 15.7965(15) _cell_angle_alpha 112.094(5) _cell_angle_beta 104.837(5) _cell_angle_gamma 90.285(5) _cell_volume 2235.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9810 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.52 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS v2014/4' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.190 _exptl_crystal_description prism _exptl_crystal_F_000 862 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_unetI/netI 0.0664 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 56350 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.587 _diffrn_reflns_theta_min 1.449 _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device 'CCD Area Detector' _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _reflns_number_gt 7650 _reflns_number_total 10243 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker APEX2 v2014.11-0' _computing_data_reduction 'Bruker SAINT v8.34A' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS-1997 (Sheldrick, 2008)' _refine_diff_density_max 1.173 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 469 _refine_ls_number_reflns 10243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0436 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.2441P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1091 _atom_sites_solution_hydrogens geom 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.28375(2) 0.19422(2) 0.26476(2) 0.01750(8) Uani 1 1 d . . . . . P1 P 0.23561(5) 0.30019(5) 0.42631(4) 0.01835(14) Uani 1 1 d . . . . . P2 P 0.22945(5) -0.02635(5) 0.13426(4) 0.01751(14) Uani 1 1 d . . . . . O1 O 0.40024(13) 0.18293(13) 0.19868(11) 0.0201(4) Uani 1 1 d . . . . . N1 N 0.30045(16) 0.08508(16) 0.33889(14) 0.0195(4) Uani 1 1 d . . . . . C1 C 0.2564(2) 0.0880(2) 0.41417(16) 0.0190(5) Uani 1 1 d . . . . . C2 C 0.2423(2) -0.0049(2) 0.43676(17) 0.0215(5) Uani 1 1 d . . . . . H2 H 0.2679 -0.0737 0.4033 0.029 Uiso 1 1 calc R . . . . C3 C 0.1916(2) 0.0017(2) 0.50711(17) 0.0230(5) Uani 1 1 d . . . . . H3 H 0.1822 -0.0633 0.5201 0.031 Uiso 1 1 calc R . . . . C4 C 0.1540(2) 0.1002(2) 0.55925(17) 0.0236(6) Uani 1 1 d . . . . . C5 C 0.1682(2) 0.1929(2) 0.53710(17) 0.0234(6) Uani 1 1 d . . . . . H5 H 0.1437 0.2617 0.5718 0.031 Uiso 1 1 calc R . . . . C6 C 0.2172(2) 0.1878(2) 0.46540(17) 0.0208(5) Uani 1 1 d . . . . . C7 C 0.1007(2) 0.1057(2) 0.63702(19) 0.0309(6) Uani 1 1 d . . . . . H7a H 0.0571 0.0334 0.6191 0.046 Uiso 1 1 calc GR . . . . H7b H 0.0503 0.1650 0.6457 0.046 Uiso 1 1 calc GR . . . . H7c H 0.1602 0.1224 0.6966 0.046 Uiso 1 1 calc GR . . . . C8 C 0.1097(2) 0.3759(2) 0.43912(17) 0.0236(6) Uani 1 1 d . . . . . H8 H 0.1100 0.4019 0.5073 0.031 Uiso 1 1 calc R . . . . C9 C -0.0002(2) 0.2991(2) 0.37971(19) 0.0310(6) Uani 1 1 d . . . . . H9a H -0.0647 0.3402 0.3927 0.046 Uiso 1 1 calc GR . . . . H9b H -0.0015 0.2333 0.3963 0.046 Uiso 1 1 calc GR . . . . H9c H -0.0049 0.2745 0.3120 0.046 Uiso 1 1 calc GR . . . . C10 C 0.1143(2) 0.4804(2) 0.41625(19) 0.0284(6) Uani 1 1 d . . . . . H10a H 0.1118 0.4578 0.3491 0.043 Uiso 1 1 calc GR . . . . H10b H 0.1847 0.5291 0.4563 0.043 Uiso 1 1 calc GR . . . . H10c H 0.0495 0.5213 0.4286 0.043 Uiso 1 1 calc GR . . . . C11 C 0.3551(2) 0.3974(2) 0.52233(17) 0.0206(5) Uani 1 1 d . . . . . H11 H 0.3717 0.4591 0.5023 0.027 Uiso 1 1 calc R . . . . C12 C 0.4605(2) 0.3354(2) 0.53033(18) 0.0264(6) Uani 1 1 d . . . . . H12a H 0.5259 0.3887 0.5754 0.040 Uiso 1 1 calc GR . . . . H12b H 0.4746 0.3015 0.4678 0.040 Uiso 1 1 calc GR . . . . H12c H 0.4487 0.2765 0.5529 0.040 Uiso 1 1 calc GR . . . . C13 C 0.3321(2) 0.4524(2) 0.61915(17) 0.0258(6) Uani 1 1 d . . . . . H13a H 0.3103 0.3940 0.6391 0.039 Uiso 1 1 calc GR . . . . H13b H 0.2706 0.4996 0.6145 0.039 Uiso 1 1 calc GR . . . . H13c H 0.4006 0.4988 0.6660 0.039 Uiso 1 1 calc GR . . . . C14 C 0.3612(2) -0.0096(2) 0.30547(16) 0.0189(5) Uani 1 1 d . . . . . C15 C 0.4536(2) -0.0302(2) 0.36730(17) 0.0220(5) Uani 1 1 d . . . . . H15 H 0.4785 0.0204 0.4321 0.029 Uiso 1 1 calc R . . . . C16 C 0.5092(2) -0.1238(2) 0.33495(18) 0.0231(5) Uani 1 1 d . . . . . H16 H 0.5717 -0.1366 0.3781 0.031 Uiso 1 1 calc R . . . . C17 C 0.4753(2) -0.1997(2) 0.24013(18) 0.0219(5) Uani 1 1 d . . . . . C18 C 0.3867(2) -0.1754(2) 0.17813(17) 0.0201(5) Uani 1 1 d . . . . . H18 H 0.3639 -0.2246 0.1129 0.027 Uiso 1 1 calc R . . . . C19 C 0.33034(19) -0.0807(2) 0.20929(16) 0.0183(5) Uani 1 1 d . . . . . C20 C 0.5339(2) -0.3037(2) 0.2076(2) 0.0300(6) Uani 1 1 d . . . . . H20a H 0.5077 -0.3410 0.1381 0.045 Uiso 1 1 calc GR . . . . H20b H 0.5162 -0.3550 0.2359 0.045 Uiso 1 1 calc GR . . . . H20c H 0.6158 -0.2827 0.2275 0.045 Uiso 1 1 calc GR . . . . C21 C 0.0881(2) -0.1021(2) 0.10816(17) 0.0225(5) Uani 1 1 d . . . . . H21 H 0.0333 -0.0757 0.0639 0.030 Uiso 1 1 calc R . . . . C22 C 0.0811(2) -0.2296(2) 0.0584(2) 0.0307(6) Uani 1 1 d . . . . . H22a H 0.1359 -0.2585 0.0986 0.046 Uiso 1 1 calc GR . . . . H22b H 0.0983 -0.2487 -0.0026 0.046 Uiso 1 1 calc GR . . . . H22c H 0.0046 -0.2633 0.0473 0.046 Uiso 1 1 calc GR . . . . C23 C 0.0496(2) -0.0699(2) 0.19833(18) 0.0267(6) Uani 1 1 d . . . . . H23a H -0.0277 -0.1051 0.1822 0.040 Uiso 1 1 calc GR . . . . H23b H 0.0513 0.0120 0.2275 0.040 Uiso 1 1 calc GR . . . . H23c H 0.1003 -0.0958 0.2432 0.040 Uiso 1 1 calc GR . . . . C24 C 0.2619(2) -0.0825(2) 0.01823(16) 0.0200(5) Uani 1 1 d . . . . . H24 H 0.2497 -0.1664 -0.0070 0.027 Uiso 1 1 calc R . . . . C25 C 0.1784(2) -0.0439(2) -0.05096(18) 0.0270(6) Uani 1 1 d . . . . . H25a H 0.1840 0.0384 -0.0247 0.041 Uiso 1 1 calc GR . . . . H25b H 0.1013 -0.0746 -0.0604 0.041 Uiso 1 1 calc GR . . . . H25c H 0.1964 -0.0707 -0.1121 0.041 Uiso 1 1 calc GR . . . . C26 C 0.3835(2) -0.0483(2) 0.02531(17) 0.0220(5) Uani 1 1 d . . . . . H26a H 0.3962 -0.0814 -0.0378 0.033 Uiso 1 1 calc GR . . . . H26b H 0.4354 -0.0753 0.0689 0.033 Uiso 1 1 calc GR . . . . H26c H 0.3972 0.0337 0.0494 0.033 Uiso 1 1 calc GR . . . . C27 C 0.4902(2) 0.23240(19) 0.18807(16) 0.0185(5) Uani 1 1 d . . . . . C28 C 0.4738(2) 0.2848(2) 0.12244(17) 0.0226(5) Uani 1 1 d . . . . . C29 C 0.5705(2) 0.3305(2) 0.11192(18) 0.0251(6) Uani 1 1 d . . . . . H29 H 0.5617 0.3671 0.0689 0.033 Uiso 1 1 calc R . . . . C30 C 0.6782(2) 0.3240(2) 0.16201(18) 0.0246(6) Uani 1 1 d . . . . . H30 H 0.7424 0.3556 0.1535 0.033 Uiso 1 1 calc R . . . . C31 C 0.6911(2) 0.2709(2) 0.22473(17) 0.0235(5) Uani 1 1 d . . . . . H31 H 0.7653 0.2656 0.2588 0.031 Uiso 1 1 calc R . . . . C32 C 0.5988(2) 0.22495(19) 0.23941(16) 0.0207(5) Uani 1 1 d . . . . . C33 C 0.3576(2) 0.2879(2) 0.06221(18) 0.0251(6) Uani 1 1 d . . . . . H33 H 0.3005 0.2595 0.0857 0.033 Uiso 1 1 calc R . . . . C34 C 0.3399(2) 0.2110(2) -0.04270(18) 0.0299(6) Uani 1 1 d . . . . . H34a H 0.3946 0.2373 -0.0677 0.045 Uiso 1 1 calc GR . . . . H34b H 0.2629 0.2126 -0.0793 0.045 Uiso 1 1 calc GR . . . . H34c H 0.3508 0.1340 -0.0481 0.045 Uiso 1 1 calc GR . . . . C35 C 0.3352(3) 0.4074(2) 0.0705(2) 0.0348(7) Uani 1 1 d . . . . . H35a H 0.3497 0.4570 0.1378 0.052 Uiso 1 1 calc GR . . . . H35b H 0.2562 0.4069 0.0369 0.052 Uiso 1 1 calc GR . . . . H35c H 0.3853 0.4346 0.0423 0.052 Uiso 1 1 calc GR . . . . C36 C 0.6163(2) 0.1653(2) 0.30751(17) 0.0238(6) Uani 1 1 d . . . . . H36 H 0.5400 0.1441 0.3114 0.032 Uiso 1 1 calc R . . . . C37 C 0.6701(3) 0.0569(2) 0.27040(19) 0.0338(7) Uani 1 1 d . . . . . H37a H 0.6237 0.0088 0.2065 0.051 Uiso 1 1 calc GR . . . . H37b H 0.6750 0.0174 0.3132 0.051 Uiso 1 1 calc GR . . . . H37c H 0.7463 0.0751 0.2677 0.051 Uiso 1 1 calc GR . . . . C38 C 0.6855(2) 0.2410(2) 0.40783(18) 0.0295(6) Uani 1 1 d . . . . . H38a H 0.7643 0.2540 0.4083 0.044 Uiso 1 1 calc GR . . . . H38b H 0.6827 0.2046 0.4517 0.044 Uiso 1 1 calc GR . . . . H38c H 0.6541 0.3130 0.4279 0.044 Uiso 1 1 calc GR . . . . C39 C 0.1203(2) 0.2221(2) 0.18483(18) 0.0242(6) Uani 1 1 d . . . . . H39a H 0.1062 0.3002 0.2155 0.036 Uiso 1 1 calc GR . . . . H39b H 0.0599 0.1714 0.1837 0.036 Uiso 1 1 calc GR . . . . H39c H 0.1217 0.2071 0.1195 0.036 Uiso 1 1 calc GR . . . . C40 C 0.3497(2) 0.3775(2) 0.31297(18) 0.0242(6) Uani 1 1 d . . . . . H40a H 0.4291 0.3906 0.3506 0.036 Uiso 1 1 calc GR . . . . H40b H 0.3047 0.4253 0.3519 0.036 Uiso 1 1 calc GR . . . . H40c H 0.3440 0.3956 0.2572 0.036 Uiso 1 1 calc GR . . . . C41 C 0.2457(2) 0.6546(2) 0.2849(2) 0.0397(7) Uani 1 1 d . . . . . H41a H 0.2451 0.7281 0.2803 0.060 Uiso 1 1 calc GR . . . . H41b H 0.3156 0.6230 0.2740 0.060 Uiso 1 1 calc GR . . . . H41c H 0.2420 0.6633 0.3484 0.060 Uiso 1 1 calc GR . . . . C42 C 0.1442(2) 0.5760(2) 0.2104(2) 0.0339(7) Uani 1 1 d . . . . . H42a H 0.1476 0.5693 0.1466 0.045 Uiso 1 1 calc R . . . . H42b H 0.1487 0.5004 0.2123 0.045 Uiso 1 1 calc R . . . . C43 C 0.0322(2) 0.6148(2) 0.2244(2) 0.0325(6) Uani 1 1 d . . . . . H43a H 0.0282 0.6904 0.2226 0.043 Uiso 1 1 calc R . . . . H43b H 0.0296 0.6219 0.2885 0.043 Uiso 1 1 calc R . . . . C44 C -0.0713(3) 0.5381(2) 0.1515(2) 0.0388(7) Uani 1 1 d . . . . . H44a H -0.0694 0.5308 0.0872 0.052 Uiso 1 1 calc R . . . . H44b H -0.0683 0.4625 0.1533 0.052 Uiso 1 1 calc R . . . . C45 C -0.1818(3) 0.5806(3) 0.1681(2) 0.0440(8) Uani 1 1 d . . . . . H45a H -0.1860 0.5845 0.2304 0.066 Uiso 1 1 calc GR . . . . H45b H -0.2453 0.5291 0.1182 0.066 Uiso 1 1 calc GR . . . . H45c H -0.1853 0.6556 0.1665 0.066 Uiso 1 1 calc GR . . . . 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 0.02170(13) 0.01878(13) 0.01303(11) 0.00575(9) 0.00720(9) 0.00326(9) P1 0.0208(3) 0.0189(3) 0.0149(3) 0.0047(2) 0.0070(3) 0.0018(3) P2 0.0207(3) 0.0182(3) 0.0141(3) 0.0057(2) 0.0064(3) 0.0027(3) O1 0.0226(9) 0.0187(9) 0.0191(8) 0.0060(7) 0.0083(7) 0.0017(7) N1 0.0234(11) 0.0196(11) 0.0175(10) 0.0077(8) 0.0085(9) 0.0033(9) C1 0.0213(12) 0.0221(13) 0.0127(11) 0.0050(10) 0.0056(10) 0.0002(10) C2 0.0270(13) 0.0193(13) 0.0164(12) 0.0045(10) 0.0069(11) 0.0019(10) C3 0.0277(14) 0.0237(13) 0.0178(12) 0.0091(10) 0.0049(11) -0.0019(11) C4 0.0236(13) 0.0304(14) 0.0187(12) 0.0100(11) 0.0083(11) 0.0006(11) C5 0.0266(14) 0.0233(13) 0.0175(12) 0.0028(10) 0.0097(11) 0.0017(11) C6 0.0204(12) 0.0226(13) 0.0173(12) 0.0045(10) 0.0068(10) -0.0006(10) C7 0.0399(16) 0.0359(16) 0.0247(14) 0.0145(12) 0.0178(13) 0.0033(13) C8 0.0224(13) 0.0291(14) 0.0186(12) 0.0056(11) 0.0102(11) 0.0058(11) C9 0.0239(14) 0.0401(16) 0.0273(14) 0.0093(12) 0.0102(12) 0.0031(12) C10 0.0281(14) 0.0294(15) 0.0281(14) 0.0093(12) 0.0115(12) 0.0111(12) C11 0.0245(13) 0.0177(12) 0.0177(12) 0.0048(10) 0.0058(10) 0.0011(10) C12 0.0245(14) 0.0254(14) 0.0235(13) 0.0054(11) 0.0035(11) 0.0005(11) C13 0.0312(14) 0.0258(14) 0.0160(12) 0.0030(10) 0.0072(11) -0.0008(11) C14 0.0226(13) 0.0197(13) 0.0162(12) 0.0079(10) 0.0069(10) 0.0013(10) C15 0.0265(13) 0.0243(13) 0.0157(12) 0.0084(10) 0.0060(11) 0.0015(11) C16 0.0210(13) 0.0299(14) 0.0239(13) 0.0166(11) 0.0059(11) 0.0046(11) C17 0.0241(13) 0.0239(13) 0.0244(13) 0.0136(11) 0.0118(11) 0.0051(11) C18 0.0231(13) 0.0198(13) 0.0169(12) 0.0058(10) 0.0070(10) 0.0004(10) C19 0.0187(12) 0.0203(12) 0.0164(12) 0.0071(10) 0.0060(10) 0.0016(10) C20 0.0360(16) 0.0303(15) 0.0322(15) 0.0165(12) 0.0169(13) 0.0131(12) C21 0.0227(13) 0.0245(13) 0.0202(12) 0.0095(11) 0.0048(11) 0.0023(11) C22 0.0328(15) 0.0268(15) 0.0291(15) 0.0066(12) 0.0098(12) -0.0045(12) C23 0.0236(14) 0.0307(15) 0.0270(14) 0.0110(12) 0.0095(11) -0.0012(11) C24 0.0251(13) 0.0193(12) 0.0146(11) 0.0047(10) 0.0066(10) 0.0020(10) C25 0.0256(14) 0.0380(16) 0.0181(13) 0.0115(12) 0.0063(11) 0.0022(12) C26 0.0264(13) 0.0239(13) 0.0179(12) 0.0082(10) 0.0099(11) 0.0058(11) C27 0.0222(13) 0.0151(12) 0.0166(12) 0.0016(9) 0.0100(10) -0.0002(10) C28 0.0285(14) 0.0192(13) 0.0197(12) 0.0047(10) 0.0105(11) 0.0040(11) C29 0.0372(16) 0.0195(13) 0.0213(13) 0.0053(10) 0.0168(12) 0.0038(11) C30 0.0279(14) 0.0207(13) 0.0251(13) 0.0029(11) 0.0167(12) -0.0014(11) C31 0.0225(13) 0.0237(13) 0.0197(12) 0.0025(10) 0.0074(11) 0.0025(11) C32 0.0266(13) 0.0174(12) 0.0151(12) 0.0021(10) 0.0077(10) 0.0009(10) C33 0.0310(14) 0.0273(14) 0.0228(13) 0.0131(11) 0.0117(12) 0.0069(12) C34 0.0364(16) 0.0317(15) 0.0236(14) 0.0120(12) 0.0103(12) 0.0029(12) C35 0.0440(17) 0.0310(16) 0.0302(15) 0.0117(12) 0.0119(13) 0.0134(13) C36 0.0240(13) 0.0271(14) 0.0208(13) 0.0090(11) 0.0077(11) 0.0010(11) C37 0.0479(18) 0.0292(15) 0.0208(14) 0.0075(12) 0.0071(13) 0.0062(13) C38 0.0310(15) 0.0358(16) 0.0192(13) 0.0072(12) 0.0084(12) 0.0042(12) C39 0.0272(14) 0.0227(13) 0.0210(13) 0.0052(11) 0.0087(11) 0.0036(11) C40 0.0316(14) 0.0221(13) 0.0218(13) 0.0074(11) 0.0140(11) 0.0014(11) C41 0.0389(17) 0.0365(17) 0.0434(18) 0.0138(14) 0.0139(15) 0.0065(14) C42 0.0438(17) 0.0277(15) 0.0370(16) 0.0153(13) 0.0184(14) 0.0088(13) C43 0.0417(17) 0.0252(15) 0.0356(16) 0.0143(12) 0.0155(14) 0.0065(13) C44 0.0457(18) 0.0322(16) 0.0412(17) 0.0159(14) 0.0140(15) 0.0038(14) C45 0.0440(18) 0.0436(19) 0.052(2) 0.0273(16) 0.0137(16) 0.0081(15) 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 P1 2.6253(7) . ? Nb1 P2 2.7713(7) . ? Nb1 O1 1.9542(16) . ? Nb1 N1 2.1275(19) . ? Nb1 C39 2.195(2) . ? Nb1 C40 2.271(2) . ? P1 C6 1.813(3) . ? P1 C8 1.850(2) . ? P1 C11 1.856(2) . ? P2 C19 1.822(2) . ? P2 C21 1.862(2) . ? P2 C24 1.850(2) . ? O1 C27 1.353(3) . ? N1 C1 1.416(3) . ? N1 C14 1.436(3) . ? C1 C2 1.398(3) . ? C1 C6 1.403(3) . ? C2 C3 1.384(3) . ? C3 C4 1.387(4) . ? C4 C5 1.391(4) . ? C4 C7 1.514(3) . ? C5 C6 1.395(3) . ? C8 C9 1.527(4) . ? C8 C10 1.528(4) . ? C11 C12 1.531(3) . ? C11 C13 1.526(3) . ? C14 C15 1.395(3) . ? C14 C19 1.395(3) . ? C15 C16 1.384(3) . ? C16 C17 1.397(3) . ? C17 C18 1.390(3) . ? C17 C20 1.507(3) . ? C18 C19 1.398(3) . ? C21 C22 1.526(4) . ? C21 C23 1.526(3) . ? C24 C25 1.530(3) . ? C24 C26 1.522(3) . ? C27 C28 1.413(3) . ? C27 C32 1.399(3) . ? C28 C29 1.400(4) . ? C28 C33 1.512(4) . ? C29 C30 1.379(4) . ? C30 C31 1.382(4) . ? C31 C32 1.389(3) . ? C32 C36 1.518(3) . ? C33 C34 1.535(4) . ? C33 C35 1.532(4) . ? C36 C37 1.528(4) . ? C36 C38 1.526(3) . ? C41 C42 1.521(4) . ? C42 C43 1.510(4) . ? C43 C44 1.520(4) . ? C44 C45 1.516(4) . ? 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 P1 Nb1 P2 131.82(2) . . ? O1 Nb1 P1 143.80(5) . . ? O1 Nb1 P2 79.62(5) . . ? O1 Nb1 N1 112.28(7) . . ? O1 Nb1 C39 112.25(8) . . ? O1 Nb1 C40 78.09(8) . . ? N1 Nb1 P1 72.03(5) . . ? N1 Nb1 P2 70.79(5) . . ? N1 Nb1 C39 123.44(9) . . ? N1 Nb1 C40 131.52(8) . . ? C39 Nb1 P1 90.94(7) . . ? C39 Nb1 P2 84.91(7) . . ? C39 Nb1 C40 90.49(9) . . ? C40 Nb1 P1 74.16(6) . . ? C40 Nb1 P2 153.55(6) . . ? C6 P1 Nb1 102.55(8) . . ? C6 P1 C8 104.09(11) . . ? C6 P1 C11 104.04(11) . . ? C8 P1 Nb1 125.01(8) . . ? C8 P1 C11 104.61(11) . . ? C11 P1 Nb1 114.19(8) . . ? C19 P2 Nb1 93.73(8) . . ? C19 P2 C21 106.69(11) . . ? C19 P2 C24 104.78(11) . . ? C21 P2 Nb1 120.08(8) . . ? C24 P2 Nb1 125.16(8) . . ? C24 P2 C21 103.34(11) . . ? C27 O1 Nb1 148.87(15) . . ? C1 N1 Nb1 130.01(15) . . ? C1 N1 C14 114.08(19) . . ? C14 N1 Nb1 115.83(14) . . ? C2 C1 N1 123.9(2) . . ? C2 C1 C6 117.5(2) . . ? C6 C1 N1 118.5(2) . . ? C3 C2 C1 121.0(2) . . ? C2 C3 C4 122.1(2) . . ? C3 C4 C5 117.0(2) . . ? C3 C4 C7 121.1(2) . . ? C5 C4 C7 121.9(2) . . ? C4 C5 C6 121.9(2) . . ? C1 C6 P1 113.16(17) . . ? C5 C6 P1 126.37(19) . . ? C5 C6 C1 120.5(2) . . ? C9 C8 P1 111.86(17) . . ? C9 C8 C10 111.1(2) . . ? C10 C8 P1 111.89(17) . . ? C12 C11 P1 109.24(16) . . ? C13 C11 P1 115.06(17) . . ? C13 C11 C12 110.6(2) . . ? C15 C14 N1 121.0(2) . . ? C15 C14 C19 119.0(2) . . ? C19 C14 N1 120.0(2) . . ? C16 C15 C14 120.5(2) . . ? C15 C16 C17 121.4(2) . . ? C16 C17 C20 120.4(2) . . ? C18 C17 C16 117.7(2) . . ? C18 C17 C20 121.9(2) . . ? C17 C18 C19 121.7(2) . . ? C14 C19 P2 113.58(17) . . ? C14 C19 C18 119.5(2) . . ? C18 C19 P2 126.35(18) . . ? C22 C21 P2 114.28(18) . . ? C22 C21 C23 110.8(2) . . ? C23 C21 P2 110.71(17) . . ? C25 C24 P2 108.56(16) . . ? C26 C24 P2 113.05(17) . . ? C26 C24 C25 110.9(2) . . ? O1 C27 C28 120.1(2) . . ? O1 C27 C32 118.5(2) . . ? C32 C27 C28 121.3(2) . . ? C27 C28 C33 122.1(2) . . ? C29 C28 C27 117.4(2) . . ? C29 C28 C33 120.5(2) . . ? C30 C29 C28 122.1(2) . . ? C29 C30 C31 119.0(2) . . ? C30 C31 C32 121.8(2) . . ? C27 C32 C36 121.2(2) . . ? C31 C32 C27 118.4(2) . . ? C31 C32 C36 120.4(2) . . ? C28 C33 C34 111.5(2) . . ? C28 C33 C35 112.2(2) . . ? C35 C33 C34 109.7(2) . . ? C32 C36 C37 111.3(2) . . ? C32 C36 C38 112.3(2) . . ? C38 C36 C37 110.7(2) . . ? C43 C42 C41 113.4(2) . . ? C42 C43 C44 114.9(2) . . ? C45 C44 C43 113.0(3) . . ?