# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Christine Thomas' _publ_contact_author_email thomasc@brandeis.edu loop_ _publ_author_name D.Evers A.Bluestein B.Foxman C.Thomas data_1Nb _database_code_depnum_ccdc_archive 'CCDC 862673' #TrackingRef '- combined_22Feb.cif' _audit_creation_date 11-03-21 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'DE1_5_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.5194(7) _cell_length_b 12.7582(8) _cell_length_c 16.2521(10) _cell_angle_alpha 85.882(3) _cell_angle_beta 84.414(3) _cell_angle_gamma 76.135(3) _cell_volume 2305.0(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C49 H60 N4 Nb1 P3 # Dc = 1.28 Fooo = 936.00 Mu = 4.03 M = 890.87 # Found Formula = C49 H60 N4 Nb1 P3 # Dc = 1.28 FOOO = 936.00 Mu = 4.03 M = 890.87 _chemical_formula_sum 'C49 H60 N4 Nb1 P3' _chemical_formula_moiety 'C49 H60 N4 Nb1 P3' _chemical_compound_source ? _chemical_formula_weight 890.87 _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'prism fragment' _exptl_crystal_colour colorless _exptl_crystal_size_min 0.150 _exptl_crystal_size_mid 0.217 _exptl_crystal_size_max 0.443 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.403 # Sheldrick geometric approximatio 0.92 0.94 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.94 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 54137 _reflns_number_total 13461 _diffrn_reflns_av_R_equivalents 0.037 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 13461 # Theoretical number of reflections is about 27133 _diffrn_reflns_theta_min 1.827 _diffrn_reflns_theta_max 30.098 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.496 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 1.27 _oxford_diffrn_Wilson_scale 20.72 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.77 _refine_diff_density_max 1.34 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 13461 _refine_ls_number_restraints 0 _refine_ls_number_parameters 514 _oxford_refine_ls_R_factor_ref 0.0437 _refine_ls_wR_factor_ref 0.0733 _refine_ls_goodness_of_fit_ref 0.9839 _refine_ls_shift/su_max 0.0016842 _refine_ls_shift/su_mean 0.0000687 # The values computed from all data _oxford_reflns_number_all 13461 _refine_ls_R_factor_all 0.0437 _refine_ls_wR_factor_all 0.0733 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10666 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_gt 0.0683 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 2.27P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Nb1 Nb 0.824151(12) 0.305142(11) 0.330268(9) 0.0122 1.0000 Uani . . . . . . P1 P 0.83654(4) 0.47123(3) 0.19647(3) 0.0173 1.0000 Uani . . . . . . P2 P 0.72052(4) 0.16128(3) 0.27906(3) 0.0142 1.0000 Uani . . . . . . P3 P 1.00205(3) 0.17505(3) 0.21164(3) 0.0148 1.0000 Uani . . . . . . N1 N 0.83028(12) 0.46303(10) 0.30099(9) 0.0163 1.0000 Uani . . . . . . N2 N 0.66149(11) 0.29151(11) 0.28853(8) 0.0153 1.0000 Uani . . . . . . N3 N 0.99843(11) 0.21275(10) 0.30945(8) 0.0146 1.0000 Uani . . . . . . N4 N 0.79608(12) 0.29995(10) 0.43908(8) 0.0153 1.0000 Uani . . . . . . C1 C 0.96508(15) 0.52853(13) 0.16122(11) 0.0192 1.0000 Uani . . . . . . C2 C 1.06712(16) 0.50280(14) 0.20490(13) 0.0273 1.0000 Uani . . . . . . C3 C 1.17116(17) 0.53277(16) 0.17283(15) 0.0333 1.0000 Uani . . . . . . C4 C 1.17592(17) 0.58548(16) 0.09568(15) 0.0332 1.0000 Uani . . . . . . C5 C 1.07575(19) 0.61101(16) 0.05122(12) 0.0302 1.0000 Uani . . . . . . C6 C 0.97058(16) 0.58368(14) 0.08415(11) 0.0238 1.0000 Uani . . . . . . C7 C 0.71051(15) 0.57931(14) 0.16375(11) 0.0217 1.0000 Uani . . . . . . C8 C 0.68610(17) 0.68653(15) 0.18584(13) 0.0288 1.0000 Uani . . . . . . C9 C 0.58154(19) 0.75914(17) 0.16443(15) 0.0374 1.0000 Uani . . . . . . C10 C 0.50217(18) 0.7265(2) 0.11902(15) 0.0409 1.0000 Uani . . . . . . C11 C 0.52797(18) 0.6223(2) 0.09341(14) 0.0381 1.0000 Uani . . . . . . C12 C 0.63103(17) 0.54894(16) 0.11635(12) 0.0287 1.0000 Uani . . . . . . C13 C 0.82889(16) 0.55665(13) 0.35072(11) 0.0207 1.0000 Uani . . . . . . C14 C 0.92166(18) 0.52676(15) 0.41429(12) 0.0283 1.0000 Uani . . . . . . C15 C 0.70511(18) 0.60053(15) 0.39295(13) 0.0298 1.0000 Uani . . . . . . C16 C 0.63496(14) 0.07305(13) 0.33748(10) 0.0169 1.0000 Uani . . . . . . C17 C 0.69464(15) -0.00562(14) 0.39224(11) 0.0215 1.0000 Uani . . . . . . C18 C 0.63911(18) -0.08354(15) 0.43094(13) 0.0293 1.0000 Uani . . . . . . C19 C 0.52292(18) -0.08232(16) 0.41628(13) 0.0314 1.0000 Uani . . . . . . C20 C 0.46133(17) -0.00328(16) 0.36350(13) 0.0283 1.0000 Uani . . . . . . C21 C 0.51700(15) 0.07354(14) 0.32387(11) 0.0223 1.0000 Uani . . . . . . C22 C 0.71751(13) 0.12374(13) 0.17346(10) 0.0158 1.0000 Uani . . . . . . C23 C 0.70540(15) 0.02175(14) 0.15528(11) 0.0218 1.0000 Uani . . . . . . C24 C 0.71287(16) -0.00644(15) 0.07366(12) 0.0264 1.0000 Uani . . . . . . C25 C 0.73390(17) 0.06555(17) 0.00990(12) 0.0287 1.0000 Uani . . . . . . C26 C 0.74787(17) 0.16650(16) 0.02721(11) 0.0251 1.0000 Uani . . . . . . C27 C 0.74056(15) 0.19541(14) 0.10851(11) 0.0199 1.0000 Uani . . . . . . C28 C 0.53158(15) 0.34057(15) 0.29519(12) 0.0258 1.0000 Uani . . . . . . C29 C 0.47569(16) 0.33510(15) 0.21437(13) 0.0275 1.0000 Uani . . . . . . C30 C 0.50674(18) 0.45503(16) 0.32145(14) 0.0322 1.0000 Uani . . . . . . C31 C 1.00840(14) 0.03000(13) 0.21613(11) 0.0178 1.0000 Uani . . . . . . C32 C 1.01592(16) -0.01876(14) 0.14080(11) 0.0228 1.0000 Uani . . . . . . C33 C 1.00854(17) -0.12504(15) 0.13853(13) 0.0284 1.0000 Uani . . . . . . C34 C 0.99330(17) -0.18493(14) 0.21177(14) 0.0306 1.0000 Uani . . . . . . C35 C 0.98424(18) -0.13746(15) 0.28658(13) 0.0288 1.0000 Uani . . . . . . C36 C 0.99188(15) -0.03038(14) 0.28892(11) 0.0223 1.0000 Uani . . . . . . C37 C 1.15342(14) 0.17249(13) 0.16180(10) 0.0171 1.0000 Uani . . . . . . C38 C 1.16891(15) 0.25932(14) 0.10833(11) 0.0214 1.0000 Uani . . . . . . C39 C 1.28058(17) 0.26138(16) 0.06815(12) 0.0268 1.0000 Uani . . . . . . C40 C 1.37840(16) 0.17676(16) 0.08089(11) 0.0258 1.0000 Uani . . . . . . C41 C 1.36467(15) 0.08980(15) 0.13355(11) 0.0232 1.0000 Uani . . . . . . C42 C 1.25306(15) 0.08734(14) 0.17369(11) 0.0198 1.0000 Uani . . . . . . C43 C 1.10260(14) 0.17254(13) 0.35923(10) 0.0178 1.0000 Uani . . . . . . C44 C 1.06585(15) 0.14558(15) 0.44901(11) 0.0235 1.0000 Uani . . . . . . C45 C 1.18093(16) 0.25473(15) 0.35417(12) 0.0245 1.0000 Uani . . . . . . C46 C 0.74538(15) 0.28920(13) 0.52452(10) 0.0183 1.0000 Uani . . . . . . C47 C 0.77217(16) 0.16959(14) 0.55353(11) 0.0230 1.0000 Uani . . . . . . C48 C 0.60932(16) 0.33370(15) 0.52761(12) 0.0259 1.0000 Uani . . . . . . C49 C 0.79956(17) 0.35217(15) 0.58120(11) 0.0249 1.0000 Uani . . . . . . H21 H 1.0656 0.4645 0.2557 0.0325 1.0000 Uiso . . . . . . H31 H 1.2388 0.5161 0.2024 0.0398 1.0000 Uiso . . . . . . H41 H 1.2477 0.6030 0.0730 0.0398 1.0000 Uiso . . . . . . H51 H 1.0783 0.6467 -0.0004 0.0359 1.0000 Uiso . . . . . . H61 H 0.9024 0.6025 0.0532 0.0292 1.0000 Uiso . . . . . . H81 H 0.7413 0.7104 0.2163 0.0345 1.0000 Uiso . . . . . . H91 H 0.5657 0.8301 0.1810 0.0450 1.0000 Uiso . . . . . . H101 H 0.4316 0.7754 0.1052 0.0489 1.0000 Uiso . . . . . . H111 H 0.4757 0.5998 0.0604 0.0466 1.0000 Uiso . . . . . . H121 H 0.6478 0.4771 0.1006 0.0344 1.0000 Uiso . . . . . . H131 H 0.8518 0.6125 0.3129 0.0239 1.0000 Uiso . . . . . . H141 H 0.9100 0.4641 0.4478 0.0415 1.0000 Uiso . . . . . . H142 H 1.0019 0.5099 0.3882 0.0421 1.0000 Uiso . . . . . . H143 H 0.9129 0.5865 0.4503 0.0424 1.0000 Uiso . . . . . . H151 H 0.7039 0.6638 0.4222 0.0452 1.0000 Uiso . . . . . . H152 H 0.6456 0.6200 0.3528 0.0440 1.0000 Uiso . . . . . . H153 H 0.6828 0.5466 0.4324 0.0440 1.0000 Uiso . . . . . . H171 H 0.7744 -0.0066 0.4011 0.0260 1.0000 Uiso . . . . . . H181 H 0.6809 -0.1372 0.4669 0.0355 1.0000 Uiso . . . . . . H191 H 0.4853 -0.1354 0.4430 0.0383 1.0000 Uiso . . . . . . H201 H 0.3821 -0.0017 0.3537 0.0343 1.0000 Uiso . . . . . . H211 H 0.4740 0.1260 0.2876 0.0268 1.0000 Uiso . . . . . . H231 H 0.6927 -0.0284 0.1981 0.0256 1.0000 Uiso . . . . . . H241 H 0.7036 -0.0749 0.0621 0.0327 1.0000 Uiso . . . . . . H251 H 0.7396 0.0467 -0.0453 0.0338 1.0000 Uiso . . . . . . H261 H 0.7634 0.2145 -0.0161 0.0302 1.0000 Uiso . . . . . . H271 H 0.7503 0.2637 0.1204 0.0243 1.0000 Uiso . . . . . . H281 H 0.4887 0.3025 0.3431 0.0315 1.0000 Uiso . . . . . . H291 H 0.5038 0.3790 0.1728 0.0388 1.0000 Uiso . . . . . . H292 H 0.4942 0.2621 0.1965 0.0398 1.0000 Uiso . . . . . . H293 H 0.3889 0.3588 0.2218 0.0409 1.0000 Uiso . . . . . . H301 H 0.5443 0.4992 0.2760 0.0486 1.0000 Uiso . . . . . . H302 H 0.5399 0.4592 0.3768 0.0479 1.0000 Uiso . . . . . . H303 H 0.4164 0.4810 0.3291 0.0482 1.0000 Uiso . . . . . . H321 H 1.0232 0.0224 0.0911 0.0278 1.0000 Uiso . . . . . . H331 H 1.0141 -0.1567 0.0880 0.0341 1.0000 Uiso . . . . . . H341 H 0.9869 -0.2575 0.2113 0.0369 1.0000 Uiso . . . . . . H351 H 0.9733 -0.1769 0.3368 0.0349 1.0000 Uiso . . . . . . H361 H 0.9854 0.0018 0.3401 0.0269 1.0000 Uiso . . . . . . H381 H 1.1024 0.3172 0.0993 0.0255 1.0000 Uiso . . . . . . H391 H 1.2891 0.3196 0.0317 0.0322 1.0000 Uiso . . . . . . H401 H 1.4539 0.1773 0.0540 0.0320 1.0000 Uiso . . . . . . H411 H 1.4300 0.0318 0.1432 0.0280 1.0000 Uiso . . . . . . H421 H 1.2451 0.0282 0.2088 0.0236 1.0000 Uiso . . . . . . H431 H 1.1510 0.1056 0.3344 0.0201 1.0000 Uiso . . . . . . H441 H 1.1351 0.1141 0.4783 0.0350 1.0000 Uiso . . . . . . H442 H 1.0153 0.0946 0.4523 0.0348 1.0000 Uiso . . . . . . H443 H 1.0214 0.2093 0.4763 0.0343 1.0000 Uiso . . . . . . H451 H 1.2515 0.2267 0.3837 0.0366 1.0000 Uiso . . . . . . H452 H 1.2058 0.2729 0.2967 0.0361 1.0000 Uiso . . . . . . H453 H 1.1365 0.3204 0.3794 0.0367 1.0000 Uiso . . . . . . H471 H 0.7337 0.1628 0.6090 0.0347 1.0000 Uiso . . . . . . H472 H 0.8581 0.1410 0.5556 0.0339 1.0000 Uiso . . . . . . H473 H 0.7417 0.1276 0.5169 0.0342 1.0000 Uiso . . . . . . H481 H 0.5761 0.3220 0.5836 0.0390 1.0000 Uiso . . . . . . H482 H 0.5914 0.4101 0.5119 0.0374 1.0000 Uiso . . . . . . H483 H 0.5742 0.2961 0.4903 0.0379 1.0000 Uiso . . . . . . H491 H 0.7704 0.3399 0.6368 0.0366 1.0000 Uiso . . . . . . H492 H 0.8855 0.3297 0.5760 0.0362 1.0000 Uiso . . . . . . H493 H 0.7764 0.4285 0.5664 0.0355 1.0000 Uiso . . . . . . 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 0.01181(6) 0.01069(6) 0.01432(7) -0.00028(5) -0.00178(5) -0.00312(4) P1 0.01844(19) 0.01316(18) 0.0208(2) 0.00158(15) -0.00361(16) -0.00468(15) P2 0.01353(17) 0.01424(18) 0.01621(19) -0.00032(15) -0.00178(14) -0.00564(14) P3 0.01258(17) 0.01361(18) 0.01796(19) -0.00095(15) -0.00123(14) -0.00231(14) N1 0.0173(6) 0.0121(6) 0.0201(7) 0.0011(5) -0.0038(5) -0.0045(5) N2 0.0122(6) 0.0155(6) 0.0187(6) -0.0039(5) -0.0024(5) -0.0030(5) N3 0.0108(6) 0.0145(6) 0.0182(6) -0.0010(5) -0.0013(5) -0.0022(5) N4 0.0149(6) 0.0139(6) 0.0176(6) -0.0009(5) -0.0022(5) -0.0043(5) C1 0.0195(8) 0.0123(7) 0.0250(8) -0.0019(6) 0.0008(6) -0.0028(6) C2 0.0205(8) 0.0198(8) 0.0394(11) 0.0053(8) -0.0044(7) -0.0013(6) C3 0.0182(8) 0.0225(9) 0.0571(14) 0.0034(9) -0.0051(8) -0.0015(7) C4 0.0214(9) 0.0234(9) 0.0536(13) -0.0052(9) 0.0096(9) -0.0072(7) C5 0.0357(10) 0.0268(9) 0.0297(10) -0.0038(8) 0.0086(8) -0.0142(8) C6 0.0267(9) 0.0234(8) 0.0229(8) -0.0022(7) 0.0013(7) -0.0100(7) C7 0.0193(8) 0.0223(8) 0.0235(8) 0.0077(7) -0.0040(6) -0.0064(6) C8 0.0276(9) 0.0206(8) 0.0363(11) 0.0065(8) -0.0080(8) -0.0022(7) C9 0.0305(10) 0.0265(10) 0.0485(13) 0.0122(9) -0.0044(9) 0.0030(8) C10 0.0210(9) 0.0470(13) 0.0481(13) 0.0230(11) -0.0069(9) -0.0007(9) C11 0.0237(9) 0.0516(13) 0.0410(12) 0.0164(10) -0.0138(9) -0.0140(9) C12 0.0236(9) 0.0334(10) 0.0313(10) 0.0081(8) -0.0070(7) -0.0120(8) C13 0.0247(8) 0.0137(7) 0.0256(8) -0.0011(6) -0.0040(7) -0.0071(6) C14 0.0342(10) 0.0257(9) 0.0306(10) -0.0026(8) -0.0105(8) -0.0144(8) C15 0.0313(10) 0.0220(9) 0.0347(10) -0.0070(8) 0.0021(8) -0.0038(7) C16 0.0178(7) 0.0180(7) 0.0166(7) -0.0005(6) -0.0001(6) -0.0080(6) C17 0.0208(8) 0.0206(8) 0.0245(8) 0.0021(7) -0.0046(7) -0.0078(6) C18 0.0313(10) 0.0245(9) 0.0341(10) 0.0103(8) -0.0083(8) -0.0118(7) C19 0.0323(10) 0.0294(10) 0.0367(11) 0.0088(8) -0.0024(8) -0.0188(8) C20 0.0224(9) 0.0318(10) 0.0355(10) 0.0035(8) -0.0044(8) -0.0162(7) C21 0.0195(8) 0.0243(8) 0.0255(9) 0.0033(7) -0.0039(7) -0.0100(6) C22 0.0122(7) 0.0169(7) 0.0186(7) -0.0030(6) -0.0011(6) -0.0035(5) C23 0.0216(8) 0.0194(8) 0.0255(9) -0.0044(7) -0.0001(7) -0.0070(6) C24 0.0247(9) 0.0259(9) 0.0311(10) -0.0134(7) 0.0011(7) -0.0090(7) C25 0.0265(9) 0.0400(11) 0.0219(9) -0.0128(8) 0.0020(7) -0.0108(8) C26 0.0262(9) 0.0318(9) 0.0192(8) -0.0010(7) -0.0009(7) -0.0109(7) C27 0.0196(8) 0.0204(8) 0.0203(8) -0.0023(6) -0.0003(6) -0.0062(6) C28 0.0159(8) 0.0281(9) 0.0321(10) -0.0076(8) -0.0036(7) -0.0002(7) C29 0.0206(8) 0.0251(9) 0.0366(10) -0.0058(8) -0.0128(7) 0.0004(7) C30 0.0261(9) 0.0277(10) 0.0410(12) -0.0087(8) -0.0033(8) -0.0008(7) C31 0.0131(7) 0.0151(7) 0.0250(8) -0.0027(6) -0.0016(6) -0.0021(5) C32 0.0207(8) 0.0215(8) 0.0260(9) -0.0053(7) 0.0019(7) -0.0049(6) C33 0.0256(9) 0.0228(9) 0.0374(11) -0.0142(8) 0.0044(8) -0.0060(7) C34 0.0260(9) 0.0163(8) 0.0496(12) -0.0077(8) 0.0003(8) -0.0046(7) C35 0.0312(10) 0.0174(8) 0.0372(11) 0.0036(7) -0.0037(8) -0.0055(7) C36 0.0214(8) 0.0178(8) 0.0274(9) -0.0008(7) -0.0036(7) -0.0037(6) C37 0.0150(7) 0.0193(7) 0.0177(7) -0.0035(6) -0.0008(6) -0.0050(6) C38 0.0215(8) 0.0217(8) 0.0208(8) -0.0013(6) 0.0005(6) -0.0057(6) C39 0.0278(9) 0.0309(9) 0.0234(9) 0.0014(7) 0.0037(7) -0.0132(8) C40 0.0201(8) 0.0374(10) 0.0233(9) -0.0088(8) 0.0034(7) -0.0135(7) C41 0.0154(7) 0.0285(9) 0.0258(9) -0.0082(7) -0.0020(6) -0.0032(6) C42 0.0171(7) 0.0208(8) 0.0211(8) -0.0025(6) -0.0020(6) -0.0033(6) C43 0.0146(7) 0.0179(7) 0.0201(8) 0.0001(6) -0.0041(6) -0.0015(6) C44 0.0201(8) 0.0274(9) 0.0225(8) 0.0037(7) -0.0059(7) -0.0043(7) C45 0.0190(8) 0.0284(9) 0.0282(9) 0.0000(7) -0.0062(7) -0.0087(7) C46 0.0189(7) 0.0190(7) 0.0174(7) -0.0016(6) 0.0014(6) -0.0062(6) C47 0.0268(9) 0.0226(8) 0.0203(8) 0.0020(7) 0.0008(7) -0.0093(7) C48 0.0204(8) 0.0287(9) 0.0270(9) -0.0010(7) 0.0037(7) -0.0051(7) C49 0.0314(9) 0.0264(9) 0.0194(8) -0.0044(7) -0.0003(7) -0.0113(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.13260(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 . P1 . 2.9431(5) yes Nb1 . P2 . 2.6362(4) yes Nb1 . P3 . 2.9550(4) yes Nb1 . N1 . 2.0526(13) yes Nb1 . N2 . 2.1028(13) yes Nb1 . N3 . 2.0797(13) yes Nb1 . N4 . 1.7659(14) yes P1 . N1 . 1.6900(15) yes P1 . C1 . 1.8300(17) yes P1 . C7 . 1.8377(17) yes P2 . N2 . 1.6498(14) yes P2 . C16 . 1.8264(16) yes P2 . C22 . 1.8202(16) yes P3 . N3 . 1.6874(14) yes P3 . C31 . 1.8308(16) yes P3 . C37 . 1.8436(16) yes N1 . C13 . 1.486(2) yes N2 . C28 . 1.474(2) yes N3 . C43 . 1.481(2) yes N4 . C46 . 1.463(2) yes C1 . C2 . 1.392(2) yes C1 . C6 . 1.395(2) yes C2 . C3 . 1.387(3) yes C2 . H21 . 0.929 no C3 . C4 . 1.382(3) yes C3 . H31 . 0.929 no C4 . C5 . 1.381(3) yes C4 . H41 . 0.941 no C5 . C6 . 1.388(3) yes C5 . H51 . 0.926 no C6 . H61 . 0.947 no C7 . C8 . 1.395(3) yes C7 . C12 . 1.390(2) yes C8 . C9 . 1.389(3) yes C8 . H81 . 0.958 no C9 . C10 . 1.383(3) yes C9 . H91 . 0.933 no C10 . C11 . 1.376(4) yes C10 . H101 . 0.934 no C11 . C12 . 1.389(3) yes C11 . H111 . 0.949 no C12 . H121 . 0.939 no C13 . C14 . 1.522(3) yes C13 . C15 . 1.516(3) yes C13 . H131 . 0.975 no C14 . H141 . 0.963 no C14 . H142 . 0.960 no C14 . H143 . 0.974 no C15 . H151 . 0.962 no C15 . H152 . 0.969 no C15 . H153 . 0.970 no C16 . C17 . 1.390(2) yes C16 . C21 . 1.396(2) yes C17 . C18 . 1.389(2) yes C17 . H171 . 0.941 no C18 . C19 . 1.378(3) yes C18 . H181 . 0.939 no C19 . C20 . 1.381(3) yes C19 . H191 . 0.947 no C20 . C21 . 1.384(2) yes C20 . H201 . 0.937 no C21 . H211 . 0.939 no C22 . C23 . 1.397(2) yes C22 . C27 . 1.394(2) yes C23 . C24 . 1.389(2) yes C23 . H231 . 0.936 no C24 . C25 . 1.377(3) yes C24 . H241 . 0.939 no C25 . C26 . 1.387(3) yes C25 . H251 . 0.938 no C26 . C27 . 1.387(2) yes C26 . H261 . 0.932 no C27 . H271 . 0.941 no C28 . C29 . 1.531(3) yes C28 . C30 . 1.504(3) yes C28 . H281 . 1.035 no C29 . H291 . 0.930 no C29 . H292 . 0.964 no C29 . H293 . 0.971 no C30 . H301 . 1.022 no C30 . H302 . 1.021 no C30 . H303 . 1.012 no C31 . C32 . 1.399(2) yes C31 . C36 . 1.387(2) yes C32 . C33 . 1.382(2) yes C32 . H321 . 0.940 no C33 . C34 . 1.387(3) yes C33 . H331 . 0.932 no C34 . C35 . 1.381(3) yes C34 . H341 . 0.947 no C35 . C36 . 1.393(2) yes C35 . H351 . 0.942 no C36 . H361 . 0.942 no C37 . C38 . 1.393(2) yes C37 . C42 . 1.397(2) yes C38 . C39 . 1.390(2) yes C38 . H381 . 0.943 no C39 . C40 . 1.381(3) yes C39 . H391 . 0.934 no C40 . C41 . 1.382(3) yes C40 . H401 . 0.936 no C41 . C42 . 1.390(2) yes C41 . H411 . 0.937 no C42 . H421 . 0.930 no C43 . C44 . 1.518(2) yes C43 . C45 . 1.532(2) yes C43 . H431 . 0.990 no C44 . H441 . 0.958 no C44 . H442 . 0.968 no C44 . H443 . 0.963 no C45 . H451 . 0.964 no C45 . H452 . 0.978 no C45 . H453 . 0.968 no C46 . C47 . 1.531(2) yes C46 . C48 . 1.531(2) yes C46 . C49 . 1.530(2) yes C47 . H471 . 0.973 no C47 . H472 . 0.973 no C47 . H473 . 0.970 no C48 . H481 . 0.968 no C48 . H482 . 0.968 no C48 . H483 . 0.972 no C49 . H491 . 0.948 no C49 . H492 . 0.959 no C49 . H493 . 0.965 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Nb1 . P2 . 108.936(14) yes P1 . Nb1 . P3 . 80.355(13) yes P2 . Nb1 . P3 . 73.677(13) yes P2 . Nb1 . N1 . 137.68(4) yes P3 . Nb1 . N1 . 105.79(4) yes P1 . Nb1 . N2 . 88.22(4) yes P3 . Nb1 . N2 . 101.72(4) yes N1 . Nb1 . N2 . 104.46(5) yes P1 . Nb1 . N3 . 97.45(4) yes P2 . Nb1 . N3 . 95.29(4) yes N1 . Nb1 . N3 . 106.70(5) yes N2 . Nb1 . N3 . 131.38(5) yes P1 . Nb1 . N4 . 137.41(4) yes P2 . Nb1 . N4 . 105.08(4) yes P3 . Nb1 . N4 . 134.45(4) yes N1 . Nb1 . N4 . 103.88(6) yes N2 . Nb1 . N4 . 103.37(6) yes N3 . Nb1 . N4 . 104.22(6) yes Nb1 . P1 . C1 . 127.25(6) yes N1 . P1 . C1 . 106.22(7) yes Nb1 . P1 . C7 . 126.07(6) yes N1 . P1 . C7 . 108.67(8) yes C1 . P1 . C7 . 101.71(8) yes Nb1 . P2 . C16 . 130.38(5) yes N2 . P2 . C16 . 114.29(7) yes Nb1 . P2 . C22 . 128.05(5) yes N2 . P2 . C22 . 110.86(7) yes C16 . P2 . C22 . 101.56(7) yes Nb1 . P3 . C31 . 116.23(5) yes N3 . P3 . C31 . 107.87(7) yes Nb1 . P3 . C37 . 138.68(5) yes N3 . P3 . C37 . 107.45(7) yes C31 . P3 . C37 . 99.05(7) yes P1 . N1 . Nb1 . 103.27(7) yes P1 . N1 . C13 . 122.80(11) yes Nb1 . N1 . C13 . 133.92(11) yes Nb1 . N2 . P2 . 88.40(6) yes Nb1 . N2 . C28 . 142.25(11) yes P2 . N2 . C28 . 124.20(11) yes P3 . N3 . Nb1 . 102.84(6) yes P3 . N3 . C43 . 120.94(10) yes Nb1 . N3 . C43 . 136.05(10) yes Nb1 . N4 . C46 . 165.81(11) yes P1 . C1 . C2 . 119.93(13) yes P1 . C1 . C6 . 120.80(13) yes C2 . C1 . C6 . 118.48(16) yes C1 . C2 . C3 . 120.55(18) yes C1 . C2 . H21 . 119.5 no C3 . C2 . H21 . 119.9 no C2 . C3 . C4 . 120.26(19) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 119.4 no C3 . C4 . C5 . 119.94(17) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 119.90(18) yes C4 . C5 . H51 . 120.3 no C6 . C5 . H51 . 119.8 no C1 . C6 . C5 . 120.84(18) yes C1 . C6 . H61 . 120.3 no C5 . C6 . H61 . 118.9 no P1 . C7 . C8 . 125.32(14) yes P1 . C7 . C12 . 116.29(14) yes C8 . C7 . C12 . 118.32(17) yes C7 . C8 . C9 . 120.41(19) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 119.6 no C8 . C9 . C10 . 120.3(2) yes C8 . C9 . H91 . 119.2 no C10 . C9 . H91 . 120.6 no C9 . C10 . C11 . 119.92(18) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 119.9(2) yes C10 . C11 . H111 . 120.7 no C12 . C11 . H111 . 119.4 no C7 . C12 . C11 . 121.09(19) yes C7 . C12 . H121 . 118.6 no C11 . C12 . H121 . 120.3 no N1 . C13 . C14 . 111.22(14) yes N1 . C13 . C15 . 111.18(14) yes C14 . C13 . C15 . 110.38(16) yes N1 . C13 . H131 . 107.4 no C14 . C13 . H131 . 107.0 no C15 . C13 . H131 . 109.5 no C13 . C14 . H141 . 109.9 no C13 . C14 . H142 . 111.6 no H141 . C14 . H142 . 107.8 no C13 . C14 . H143 . 109.7 no H141 . C14 . H143 . 108.6 no H142 . C14 . H143 . 109.1 no C13 . C15 . H151 . 110.6 no C13 . C15 . H152 . 110.8 no H151 . C15 . H152 . 108.4 no C13 . C15 . H153 . 110.2 no H151 . C15 . H153 . 108.3 no H152 . C15 . H153 . 108.5 no P2 . C16 . C17 . 117.87(12) yes P2 . C16 . C21 . 123.32(13) yes C17 . C16 . C21 . 118.48(15) yes C16 . C17 . C18 . 120.70(16) yes C16 . C17 . H171 . 118.7 no C18 . C17 . H171 . 120.6 no C17 . C18 . C19 . 120.02(17) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 120.05(17) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 120.2 no C19 . C20 . C21 . 120.08(17) yes C19 . C20 . H201 . 120.4 no C21 . C20 . H201 . 119.5 no C16 . C21 . C20 . 120.64(16) yes C16 . C21 . H211 . 120.5 no C20 . C21 . H211 . 118.8 no P2 . C22 . C23 . 122.26(13) yes P2 . C22 . C27 . 118.46(12) yes C23 . C22 . C27 . 118.95(15) yes C22 . C23 . C24 . 120.36(16) yes C22 . C23 . H231 . 120.2 no C24 . C23 . H231 . 119.4 no C23 . C24 . C25 . 120.22(16) yes C23 . C24 . H241 . 119.7 no C25 . C24 . H241 . 120.1 no C24 . C25 . C26 . 119.94(17) yes C24 . C25 . H251 . 120.5 no C26 . C25 . H251 . 119.5 no C25 . C26 . C27 . 120.28(17) yes C25 . C26 . H261 . 119.7 no C27 . C26 . H261 . 120.1 no C22 . C27 . C26 . 120.23(16) yes C22 . C27 . H271 . 119.3 no C26 . C27 . H271 . 120.4 no N2 . C28 . C29 . 111.61(15) yes N2 . C28 . C30 . 110.80(15) yes C29 . C28 . C30 . 111.09(16) yes N2 . C28 . H281 . 110.4 no C29 . C28 . H281 . 109.6 no C30 . C28 . H281 . 103.0 no C28 . C29 . H291 . 110.5 no C28 . C29 . H292 . 111.0 no H291 . C29 . H292 . 108.9 no C28 . C29 . H293 . 110.7 no H291 . C29 . H293 . 108.6 no H292 . C29 . H293 . 107.1 no C28 . C30 . H301 . 108.0 no C28 . C30 . H302 . 111.7 no H301 . C30 . H302 . 110.6 no C28 . C30 . H303 . 106.2 no H301 . C30 . H303 . 112.4 no H302 . C30 . H303 . 107.8 no P3 . C31 . C32 . 117.18(13) yes P3 . C31 . C36 . 123.85(13) yes C32 . C31 . C36 . 118.49(15) yes C31 . C32 . C33 . 121.03(17) yes C31 . C32 . H321 . 119.3 no C33 . C32 . H321 . 119.7 no C32 . C33 . C34 . 119.93(17) yes C32 . C33 . H331 . 120.2 no C34 . C33 . H331 . 119.9 no C33 . C34 . C35 . 119.68(17) yes C33 . C34 . H341 . 121.0 no C35 . C34 . H341 . 119.3 no C34 . C35 . C36 . 120.42(18) yes C34 . C35 . H351 . 120.7 no C36 . C35 . H351 . 118.9 no C35 . C36 . C31 . 120.44(17) yes C35 . C36 . H361 . 120.2 no C31 . C36 . H361 . 119.4 no P3 . C37 . C38 . 118.27(12) yes P3 . C37 . C42 . 123.54(13) yes C38 . C37 . C42 . 118.18(15) yes C37 . C38 . C39 . 120.93(16) yes C37 . C38 . H381 . 119.2 no C39 . C38 . H381 . 119.8 no C38 . C39 . C40 . 120.19(17) yes C38 . C39 . H391 . 119.8 no C40 . C39 . H391 . 120.0 no C39 . C40 . C41 . 119.70(16) yes C39 . C40 . H401 . 120.8 no C41 . C40 . H401 . 119.5 no C40 . C41 . C42 . 120.28(16) yes C40 . C41 . H411 . 121.0 no C42 . C41 . H411 . 118.7 no C37 . C42 . C41 . 120.73(16) yes C37 . C42 . H421 . 119.9 no C41 . C42 . H421 . 119.4 no N3 . C43 . C44 . 112.65(13) yes N3 . C43 . C45 . 110.50(13) yes C44 . C43 . C45 . 110.12(14) yes N3 . C43 . H431 . 107.0 no C44 . C43 . H431 . 108.3 no C45 . C43 . H431 . 108.0 no C43 . C44 . H441 . 110.5 no C43 . C44 . H442 . 110.2 no H441 . C44 . H442 . 108.4 no C43 . C44 . H443 . 111.1 no H441 . C44 . H443 . 108.6 no H442 . C44 . H443 . 107.9 no C43 . C45 . H451 . 110.6 no C43 . C45 . H452 . 111.3 no H451 . C45 . H452 . 108.9 no C43 . C45 . H453 . 109.8 no H451 . C45 . H453 . 107.8 no H452 . C45 . H453 . 108.3 no N4 . C46 . C47 . 109.42(13) yes N4 . C46 . C48 . 108.77(14) yes C47 . C46 . C48 . 109.12(14) yes N4 . C46 . C49 . 110.23(13) yes C47 . C46 . C49 . 109.57(14) yes C48 . C46 . C49 . 109.70(14) yes C46 . C47 . H471 . 108.8 no C46 . C47 . H472 . 110.4 no H471 . C47 . H472 . 108.3 no C46 . C47 . H473 . 110.9 no H471 . C47 . H473 . 109.0 no H472 . C47 . H473 . 109.4 no C46 . C48 . H481 . 108.1 no C46 . C48 . H482 . 109.8 no H481 . C48 . H482 . 110.1 no C46 . C48 . H483 . 110.5 no H481 . C48 . H483 . 109.0 no H482 . C48 . H483 . 109.4 no C46 . C49 . H491 . 109.1 no C46 . C49 . H492 . 110.6 no H491 . C49 . H492 . 109.7 no C46 . C49 . H493 . 109.7 no H491 . C49 . H493 . 109.0 no H492 . C49 . H493 . 108.6 no _iucr_refine_instruction_details_constraints ; # # Punched on 21/03/11 at 17:11:47 # #LIST 12 BLOCK SCALE X'S, U'S END ; _iucr_refine_instruction_details_restraints ; # # Punched on 21/03/11 at 17:11:47 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END data_2Nb _database_code_depnum_ccdc_archive 'CCDC 862674' #TrackingRef '- combined_22Feb.cif' _audit_creation_date 11-07-10 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'de1_17_0m in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.1155(4) _cell_length_b 18.2831(6) _cell_length_c 25.2678(8) _cell_angle_alpha 90 _cell_angle_beta 95.274(2) _cell_angle_gamma 90 _cell_volume 6033.4(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C63 H76 Co1 I1 N4 Nb1 P3 # Dc = 1.39 Fooo = 2592.00 Mu = 10.97 M = 1260.99 # Found Formula = C63 H76 Co1 I1 N4 Nb1 P3 # Dc = 1.39 FOOO = 2592.00 Mu = 10.97 M = 1260.99 _chemical_formula_sum 'C63 H76 Co1 I1 N4 Nb1 P3' _chemical_formula_moiety 'C49 H60 Co I N4 Nb P3,2(C7 H8)' _chemical_compound_source ? _chemical_formula_weight 1260.99 _cell_measurement_reflns_used 9824 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 329.96 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_min 0.130 _exptl_crystal_size_mid 0.342 _exptl_crystal_size_max 0.439 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.097 # Sheldrick geometric approximatio 0.69 0.87 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 71799 _reflns_number_total 17598 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 17598 # Theoretical number of reflections is about 35361 _diffrn_reflns_theta_min 1.619 _diffrn_reflns_theta_max 30.051 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.450 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 1.69 _oxford_diffrn_Wilson_scale 406.42 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.22 _refine_diff_density_max 1.38 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 17598 _refine_ls_number_restraints 90 _refine_ls_number_parameters 658 _oxford_refine_ls_R_factor_ref 0.0568 _refine_ls_wR_factor_ref 0.0992 _refine_ls_goodness_of_fit_ref 1.0078 _refine_ls_shift/su_max 0.0046685 _refine_ls_shift/su_mean 0.0001712 # The values computed from all data _oxford_reflns_number_all 17598 _refine_ls_R_factor_all 0.0568 _refine_ls_wR_factor_all 0.0992 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 13273 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_gt 0.0893 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +13.12P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Nb1 Nb 0.103586(17) 0.447047(12) 0.675169(9) 0.0144 1.0000 Uani . . . . . . I1 I 0.498888(15) 0.455958(11) 0.775294(8) 0.0279 1.0000 Uani . . . . . . Co1 Co 0.31627(3) 0.448595(19) 0.733396(13) 0.0148 1.0000 Uani . . . . . . P1 P 0.27737(5) 0.55187(4) 0.68783(3) 0.0153 1.0000 Uani . . . . . . P2 P 0.29145(5) 0.35605(4) 0.67479(3) 0.0148 1.0000 Uani . . . . . . P3 P 0.19153(5) 0.43356(4) 0.78800(3) 0.0176 1.0000 Uani . . . . . . N1 N 0.15471(17) 0.55083(12) 0.66199(8) 0.0167 1.0000 Uani . . . . . . N2 N 0.17911(17) 0.36652(12) 0.63784(9) 0.0175 1.0000 Uani . . . . . . N3 N 0.07690(18) 0.42571(12) 0.75246(9) 0.0192 1.0000 Uani . . . . . . N4 N -0.02063(17) 0.44583(13) 0.64075(9) 0.0194 1.0000 Uani . . . . . . C1 C 0.3049(2) 0.63712(15) 0.72401(11) 0.0205 1.0000 Uani . . . . . . C2 C 0.3228(2) 0.63582(17) 0.77921(11) 0.0249 1.0000 Uani . . . . . . C3 C 0.3444(3) 0.70007(19) 0.80792(13) 0.0323 1.0000 Uani . . . . . . C4 C 0.3492(2) 0.76602(18) 0.78184(14) 0.0320 1.0000 Uani . . . . . . C5 C 0.3341(2) 0.76851(16) 0.72697(14) 0.0301 1.0000 Uani . . . . . . C6 C 0.3118(2) 0.70482(15) 0.69804(12) 0.0241 1.0000 Uani . . . . . . C7 C 0.3539(2) 0.56475(14) 0.63155(10) 0.0174 1.0000 Uani . . . . . . C8 C 0.3183(2) 0.54176(16) 0.58075(11) 0.0223 1.0000 Uani . . . . . . C9 C 0.3814(3) 0.54546(18) 0.53949(12) 0.0299 1.0000 Uani . . . . . . C10 C 0.4813(3) 0.57078(17) 0.54847(12) 0.0289 1.0000 Uani . . . . . . C11 C 0.5175(2) 0.59193(16) 0.59931(13) 0.0268 1.0000 Uani . . . . . . C12 C 0.4551(2) 0.58960(15) 0.64040(12) 0.0235 1.0000 Uani . . . . . . C13 C 0.1046(2) 0.61753(15) 0.63797(11) 0.0228 1.0000 Uani . . . . . . C14 C 0.0268(3) 0.64539(18) 0.67428(13) 0.0352 1.0000 Uani . . . . . . C15 C 0.0557(2) 0.60356(18) 0.58222(11) 0.0273 1.0000 Uani . . . . . . C16 C 0.3926(2) 0.34222(14) 0.62988(10) 0.0175 1.0000 Uani . . . . . . C17 C 0.4643(2) 0.39733(15) 0.62586(11) 0.0198 1.0000 Uani . . . . . . C18 C 0.5432(2) 0.38926(17) 0.59353(12) 0.0253 1.0000 Uani . . . . . . C19 C 0.5515(2) 0.32581(18) 0.56427(12) 0.0285 1.0000 Uani . . . . . . C20 C 0.4811(2) 0.27007(17) 0.56780(12) 0.0268 1.0000 Uani . . . . . . C21 C 0.4027(2) 0.27780(16) 0.60078(11) 0.0218 1.0000 Uani . . . . . . C22 C 0.2873(2) 0.26487(14) 0.70444(10) 0.0172 1.0000 Uani . . . . . . C23 C 0.3770(2) 0.22453(16) 0.71604(11) 0.0220 1.0000 Uani . . . . . . C24 C 0.3741(3) 0.15682(17) 0.73983(12) 0.0292 1.0000 Uani . . . . . . C25 C 0.2824(3) 0.12829(18) 0.75321(13) 0.0369 1.0000 Uani . . . . . . C26 C 0.1934(3) 0.16843(18) 0.74329(14) 0.0352 1.0000 Uani . . . . . . C27 C 0.1951(2) 0.23640(16) 0.71880(12) 0.0257 1.0000 Uani . . . . . . C28 C 0.1552(2) 0.32031(17) 0.58976(12) 0.0259 1.0000 Uani . . . . . . C29 C 0.0564(3) 0.27811(18) 0.59229(15) 0.0349 1.0000 Uani . . . . . . C30 C 0.1570(3) 0.3674(2) 0.54012(12) 0.0375 1.0000 Uani . . . . . . C31 C 0.1732(2) 0.50812(16) 0.83471(11) 0.0237 1.0000 Uani . . . . . . C32 C 0.1099(3) 0.56673(17) 0.81836(13) 0.0303 1.0000 Uani . . . . . . C33 C 0.1006(3) 0.6266(2) 0.85102(16) 0.0431 1.0000 Uani . . . . . . C34 C 0.1541(3) 0.6289(2) 0.90040(16) 0.0507 1.0000 Uani . . . . . . C35 C 0.2177(4) 0.5721(2) 0.91708(15) 0.0498 1.0000 Uani . . . . . . C36 C 0.2281(3) 0.5115(2) 0.88434(12) 0.0349 1.0000 Uani . . . . . . C37 C 0.2159(2) 0.35590(16) 0.83393(11) 0.0228 1.0000 Uani . . . . . . C38 C 0.1526(3) 0.3374(2) 0.87363(13) 0.0363 1.0000 Uani . . . . . . C39 C 0.1774(3) 0.2791(2) 0.90774(14) 0.0420 1.0000 Uani . . . . . . C40 C 0.2672(3) 0.2403(2) 0.90401(14) 0.0426 1.0000 Uani . . . . . . C41 C 0.3313(3) 0.25901(19) 0.86577(13) 0.0386 1.0000 Uani . . . . . . C42 C 0.3052(3) 0.31625(17) 0.83102(12) 0.0279 1.0000 Uani . . . . . . C43 C -0.0162(2) 0.40950(17) 0.78013(12) 0.0266 1.0000 Uani . . . . . . C44 C -0.0475(3) 0.33007(19) 0.77039(16) 0.0395 1.0000 Uani . . . . . . C45 C -0.1037(2) 0.4617(2) 0.76442(14) 0.0344 1.0000 Uani . . . . . . C46 C -0.1237(2) 0.44193(17) 0.61204(12) 0.0260 1.0000 Uani . . . . . . C47 C -0.1812(2) 0.37573(19) 0.63250(16) 0.0368 1.0000 Uani . . . . . . C48 C -0.1840(2) 0.51212(19) 0.62127(14) 0.0325 1.0000 Uani . . . . . . C49 C -0.1150(3) 0.4338(2) 0.55231(13) 0.0360 1.0000 Uani . . . . . . C50 C 0.5152(7) 0.5628(3) 0.9258(3) 0.1102 1.0000 Uani . U . . . . C51 C 0.6280(7) 0.5753(3) 0.9320(2) 0.1093 1.0000 Uani D U . . . . C52 C 0.6753(7) 0.5862(4) 0.9830(2) 0.1095 1.0000 Uani D U . . . . C53 C 0.7813(7) 0.5900(4) 0.9842(3) 0.1255 1.0000 Uani D U . . . . C54 C 0.8362(7) 0.5944(4) 0.9383(2) 0.1212 1.0000 Uani D U . . . . C55 C 0.7802(6) 0.5902(3) 0.8924(2) 0.1025 1.0000 Uani D U . . . . C56 C 0.6711(6) 0.5775(3) 0.8874(2) 0.1120 1.0000 Uani D U . . . . C57 C 0.0880(6) 0.8941(4) 0.5527(3) 0.1134 1.0000 Uani . U . . . . C58 C 0.1787(5) 0.8520(3) 0.5572(2) 0.0856 1.0000 Uani D U . . . . C59 C 0.2708(5) 0.8810(3) 0.5797(2) 0.0724 1.0000 Uani D U . . . . C60 C 0.3606(6) 0.8393(4) 0.5795(3) 0.0994 1.0000 Uani D U . . . . C61 C 0.3620(6) 0.7708(3) 0.5618(2) 0.0962 1.0000 Uani D U . . . . C62 C 0.2678(5) 0.7445(3) 0.5426(2) 0.0835 1.0000 Uani D U . . . . C63 C 0.1764(5) 0.7791(3) 0.53828(18) 0.0748 1.0000 Uani D . . . . . H411 H 0.3930 0.2329 0.8636 0.0452 1.0000 Uiso R . . . . . H351 H 0.2549 0.5742 0.9506 0.0602 1.0000 Uiso R . . . . . H251 H 0.2805 0.0818 0.7686 0.0441 1.0000 Uiso R . . . . . H321 H 0.0742 0.5659 0.7843 0.0361 1.0000 Uiso R . . . . . H401 H 0.2842 0.2017 0.9275 0.0506 1.0000 Uiso R . . . . . H181 H 0.5913 0.4268 0.5919 0.0306 1.0000 Uiso R . . . . . H281 H 0.2084 0.2829 0.5888 0.0301 1.0000 Uiso R . . . . . H302 H 0.1414 0.3378 0.5089 0.0558 1.0000 Uiso R . . . . . H303 H 0.1071 0.4051 0.5409 0.0553 1.0000 Uiso R . . . . . H301 H 0.2232 0.3884 0.5391 0.0561 1.0000 Uiso R . . . . . H171 H 0.4607 0.4403 0.6454 0.0233 1.0000 Uiso R . . . . . H271 H 0.1348 0.2633 0.7117 0.0305 1.0000 Uiso R . . . . . H231 H 0.4390 0.2439 0.7076 0.0263 1.0000 Uiso R . . . . . H241 H 0.4339 0.1291 0.7470 0.0344 1.0000 Uiso R . . . . . H152 H 0.0181 0.6472 0.5691 0.0405 1.0000 Uiso R . . . . . H151 H 0.0085 0.5637 0.5821 0.0409 1.0000 Uiso R . . . . . H153 H 0.1076 0.5927 0.5587 0.0415 1.0000 Uiso R . . . . . H131 H 0.1576 0.6548 0.6360 0.0272 1.0000 Uiso R . . . . . H141 H -0.0095 0.6867 0.6583 0.0531 1.0000 Uiso R . . . . . H142 H 0.0615 0.6597 0.7077 0.0527 1.0000 Uiso R . . . . . H143 H -0.0220 0.6065 0.6801 0.0521 1.0000 Uiso R . . . . . H121 H 0.4800 0.6052 0.6748 0.0280 1.0000 Uiso R . . . . . H111 H 0.5841 0.6071 0.6058 0.0328 1.0000 Uiso R . . . . . H101 H 0.5234 0.5722 0.5205 0.0356 1.0000 Uiso R . . . . . H91 H 0.3565 0.5299 0.5051 0.0361 1.0000 Uiso R . . . . . H81 H 0.2514 0.5234 0.5746 0.0271 1.0000 Uiso R . . . . . H21 H 0.3198 0.5910 0.7965 0.0296 1.0000 Uiso R . . . . . H61 H 0.3029 0.7064 0.6609 0.0287 1.0000 Uiso R . . . . . H201 H 0.4864 0.2275 0.5480 0.0326 1.0000 Uiso R . . . . . H31 H 0.3556 0.6981 0.8451 0.0387 1.0000 Uiso R . . . . . H191 H 0.6038 0.3201 0.5422 0.0338 1.0000 Uiso R . . . . . H431 H 0.0037 0.4157 0.8187 0.0310 1.0000 Uiso R . . . . . H441 H -0.1046 0.3175 0.7903 0.0589 1.0000 Uiso R . . . . . H443 H 0.0098 0.2975 0.7812 0.0585 1.0000 Uiso R . . . . . H442 H -0.0667 0.3228 0.7331 0.0586 1.0000 Uiso R . . . . . H41 H 0.3637 0.8090 0.8012 0.0382 1.0000 Uiso R . . . . . H481 H -0.2523 0.5084 0.6035 0.0486 1.0000 Uiso R . . . . . H483 H -0.1893 0.5193 0.6587 0.0483 1.0000 Uiso R . . . . . H482 H -0.1518 0.5547 0.6067 0.0483 1.0000 Uiso R . . . . . H471 H -0.2438 0.3693 0.6114 0.0548 1.0000 Uiso R . . . . . H472 H -0.1957 0.3838 0.6685 0.0547 1.0000 Uiso R . . . . . H473 H -0.1404 0.3324 0.6292 0.0544 1.0000 Uiso R . . . . . H492 H -0.1831 0.4320 0.5340 0.0539 1.0000 Uiso R . . . . . H493 H -0.0782 0.4741 0.5391 0.0533 1.0000 Uiso R . . . . . H491 H -0.0799 0.3886 0.5448 0.0532 1.0000 Uiso R . . . . . H421 H 0.3496 0.3287 0.8055 0.0341 1.0000 Uiso R . . . . . H211 H 0.3562 0.2396 0.6030 0.0256 1.0000 Uiso R . . . . . H51 H 0.3388 0.8123 0.7087 0.0356 1.0000 Uiso R . . . . . H361 H 0.2717 0.4739 0.8957 0.0416 1.0000 Uiso R . . . . . H293 H 0.0385 0.2521 0.5587 0.0519 1.0000 Uiso R . . . . . H292 H 0.0628 0.2430 0.6206 0.0518 1.0000 Uiso R . . . . . H291 H 0.0012 0.3108 0.5983 0.0521 1.0000 Uiso R . . . . . H261 H 0.1311 0.1498 0.7526 0.0425 1.0000 Uiso R . . . . . H451 H -0.1639 0.4469 0.7816 0.0508 1.0000 Uiso R . . . . . H452 H -0.0841 0.5102 0.7754 0.0510 1.0000 Uiso R . . . . . H453 H -0.1182 0.4601 0.7268 0.0509 1.0000 Uiso R . . . . . H381 H 0.0931 0.3652 0.8776 0.0436 1.0000 Uiso R . . . . . H391 H 0.1331 0.2659 0.9336 0.0501 1.0000 Uiso R . . . . . H331 H 0.0586 0.6664 0.8394 0.0513 1.0000 Uiso R . . . . . H341 H 0.1467 0.6690 0.9224 0.0609 1.0000 Uiso R . . . . . H591 H 0.2726 0.9268 0.5945 0.0875 1.0000 Uiso R . . . . . H631 H 0.1159 0.7565 0.5253 0.0901 1.0000 Uiso R . . . . . H621 H 0.2656 0.6963 0.5309 0.1006 1.0000 Uiso R . . . . . H611 H 0.4252 0.7434 0.5640 0.1167 1.0000 Uiso R . . . . . H601 H 0.4260 0.8585 0.5922 0.1195 1.0000 Uiso R . . . . . H521 H 0.6321 0.5911 1.0127 0.1289 1.0000 Uiso R . . . . . H551 H 0.8140 0.5961 0.8624 0.1224 1.0000 Uiso R . . . . . H531 H 0.8208 0.5905 1.0181 0.1510 1.0000 Uiso R . . . . . H541 H 0.9093 0.6001 0.9396 0.1457 1.0000 Uiso R . . . . . H561 H 0.6318 0.5716 0.8546 0.1339 1.0000 Uiso R . . . . . H571 H 0.0883 0.9232 0.5854 0.1702 1.0000 Uiso R . . . . . H572 H 0.0332 0.8557 0.5495 0.1701 1.0000 Uiso R . . . . . H573 H 0.0831 0.9249 0.5200 0.1703 1.0000 Uiso R . . . . . H501 H 0.4899 0.5619 0.9598 0.1313 1.0000 Uiso R . . . . . H502 H 0.4830 0.6012 0.9052 0.1313 1.0000 Uiso R . . . . . H503 H 0.5010 0.5174 0.9084 0.1313 1.0000 Uiso 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 0.01336(10) 0.01315(10) 0.01647(10) -0.00035(8) 0.00080(8) 0.00048(8) I1 0.02153(9) 0.02466(10) 0.03536(10) -0.00037(8) -0.00977(7) -0.00015(7) Co1 0.01548(16) 0.01360(16) 0.01505(15) -0.00042(13) 0.00057(12) 0.00028(13) P1 0.0175(3) 0.0131(3) 0.0151(3) -0.0011(2) 0.0006(2) -0.0012(2) P2 0.0142(3) 0.0126(3) 0.0177(3) -0.0007(2) 0.0022(2) -0.0001(2) P3 0.0203(3) 0.0173(3) 0.0153(3) 0.0017(2) 0.0029(2) 0.0023(2) N1 0.0173(10) 0.0136(10) 0.0191(10) 0.0003(8) 0.0003(8) -0.0009(8) N2 0.0169(11) 0.0152(10) 0.0199(10) -0.0038(8) -0.0006(8) 0.0007(8) N3 0.0184(11) 0.0175(10) 0.0222(11) 0.0033(9) 0.0049(9) 0.0004(9) N4 0.0147(10) 0.0194(11) 0.0237(11) -0.0008(9) -0.0004(8) 0.0007(9) C1 0.0178(13) 0.0198(13) 0.0239(13) -0.0074(11) 0.0014(10) -0.0004(10) C2 0.0239(14) 0.0269(14) 0.0241(13) -0.0063(11) 0.0024(11) -0.0051(12) C3 0.0302(17) 0.0393(18) 0.0282(15) -0.0171(14) 0.0074(13) -0.0079(14) C4 0.0241(15) 0.0261(15) 0.0462(19) -0.0221(14) 0.0055(13) -0.0050(12) C5 0.0247(15) 0.0161(13) 0.0498(19) -0.0088(13) 0.0043(14) -0.0014(11) C6 0.0259(15) 0.0175(13) 0.0287(14) -0.0017(11) 0.0010(12) -0.0004(11) C7 0.0209(13) 0.0126(11) 0.0188(12) 0.0008(9) 0.0020(10) 0.0002(9) C8 0.0225(13) 0.0254(14) 0.0187(12) -0.0019(11) 0.0013(10) 0.0046(11) C9 0.0346(17) 0.0366(17) 0.0188(12) 0.0003(12) 0.0044(12) 0.0123(14) C10 0.0343(17) 0.0272(15) 0.0274(14) 0.0048(12) 0.0157(13) 0.0070(13) C11 0.0259(15) 0.0178(13) 0.0381(16) -0.0020(12) 0.0111(13) -0.0035(11) C12 0.0254(15) 0.0185(13) 0.0269(14) -0.0047(11) 0.0044(11) -0.0052(11) C13 0.0256(14) 0.0146(12) 0.0269(14) 0.0048(10) -0.0037(11) 0.0026(10) C14 0.041(2) 0.0287(16) 0.0343(17) -0.0070(13) -0.0035(14) 0.0182(14) C15 0.0286(16) 0.0313(16) 0.0211(13) 0.0053(12) -0.0024(11) 0.0062(12) C16 0.0165(12) 0.0176(12) 0.0184(11) 0.0015(10) 0.0021(9) 0.0017(10) C17 0.0166(13) 0.0162(12) 0.0267(13) 0.0023(10) 0.0025(10) 0.0015(10) C18 0.0177(13) 0.0257(14) 0.0335(15) 0.0080(12) 0.0069(11) 0.0003(11) C19 0.0217(14) 0.0371(17) 0.0282(15) 0.0048(13) 0.0108(12) 0.0046(12) C20 0.0285(16) 0.0287(15) 0.0239(14) -0.0043(12) 0.0065(12) 0.0050(12) C21 0.0209(14) 0.0212(13) 0.0238(13) -0.0033(11) 0.0041(11) 0.0006(10) C22 0.0199(13) 0.0113(11) 0.0209(12) -0.0010(9) 0.0042(10) 0.0008(9) C23 0.0227(14) 0.0232(13) 0.0200(12) 0.0023(10) 0.0024(10) 0.0024(11) C24 0.0376(18) 0.0233(14) 0.0263(14) 0.0033(12) 0.0010(13) 0.0095(13) C25 0.061(2) 0.0208(15) 0.0302(16) 0.0093(13) 0.0092(16) -0.0002(15) C26 0.0402(19) 0.0255(15) 0.0428(19) 0.0051(14) 0.0183(15) -0.0081(14) C27 0.0242(15) 0.0220(14) 0.0321(15) 0.0024(12) 0.0093(12) -0.0020(11) C28 0.0224(14) 0.0258(14) 0.0285(14) -0.0118(12) -0.0032(11) 0.0007(11) C29 0.0271(16) 0.0258(15) 0.050(2) -0.0102(14) -0.0076(14) -0.0051(13) C30 0.0392(19) 0.049(2) 0.0234(15) -0.0093(14) -0.0026(13) -0.0066(16) C31 0.0294(15) 0.0237(14) 0.0188(12) -0.0028(11) 0.0070(11) 0.0018(12) C32 0.0351(17) 0.0246(15) 0.0319(16) -0.0033(12) 0.0071(13) 0.0077(13) C33 0.048(2) 0.0313(18) 0.051(2) -0.0099(16) 0.0121(18) 0.0109(16) C34 0.061(3) 0.048(2) 0.046(2) -0.0254(19) 0.0167(19) 0.005(2) C35 0.061(3) 0.058(3) 0.0294(17) -0.0174(17) 0.0016(17) 0.003(2) C36 0.043(2) 0.0361(18) 0.0246(15) -0.0046(13) -0.0003(14) 0.0032(15) C37 0.0278(15) 0.0223(13) 0.0183(12) 0.0048(10) 0.0021(11) 0.0017(11) C38 0.0346(18) 0.044(2) 0.0313(16) 0.0154(15) 0.0092(14) 0.0057(15) C39 0.051(2) 0.044(2) 0.0325(17) 0.0199(16) 0.0110(16) 0.0044(17) C40 0.066(3) 0.0317(18) 0.0304(17) 0.0135(14) 0.0049(17) 0.0112(17) C41 0.058(2) 0.0292(17) 0.0299(16) 0.0088(14) 0.0105(16) 0.0200(16) C42 0.0384(18) 0.0240(14) 0.0218(13) 0.0034(11) 0.0063(12) 0.0056(13) C43 0.0222(14) 0.0311(15) 0.0283(14) 0.0078(12) 0.0112(12) 0.0012(12) C44 0.0266(17) 0.0334(18) 0.060(2) 0.0134(17) 0.0091(16) -0.0046(14) C45 0.0243(16) 0.0394(18) 0.0408(18) 0.0058(15) 0.0104(13) 0.0084(14) C46 0.0151(13) 0.0274(15) 0.0342(15) -0.0052(12) -0.0051(11) 0.0008(11) C47 0.0190(15) 0.0335(17) 0.057(2) -0.0014(16) -0.0041(14) -0.0052(13) C48 0.0201(15) 0.0341(17) 0.0421(18) -0.0036(14) -0.0031(13) 0.0093(13) C49 0.0290(17) 0.046(2) 0.0306(16) -0.0084(14) -0.0129(13) 0.0063(15) C50 0.186(6) 0.044(3) 0.089(3) -0.004(3) -0.050(4) 0.016(4) C51 0.201(5) 0.043(2) 0.076(3) 0.003(2) -0.031(4) 0.019(3) C52 0.170(6) 0.091(4) 0.057(3) 0.011(3) -0.045(4) -0.018(4) C53 0.210(7) 0.112(5) 0.052(3) 0.004(3) -0.002(4) -0.047(5) C54 0.210(7) 0.083(4) 0.073(4) 0.002(3) 0.023(4) -0.049(4) C55 0.211(6) 0.048(3) 0.048(3) 0.010(2) 0.009(4) -0.030(4) C56 0.238(7) 0.038(2) 0.049(3) 0.001(2) -0.046(4) -0.005(4) C57 0.140(5) 0.107(4) 0.100(4) 0.013(3) 0.052(4) 0.006(4) C58 0.109(4) 0.071(3) 0.082(3) 0.025(3) 0.035(3) 0.008(3) C59 0.108(4) 0.036(2) 0.075(3) -0.017(2) 0.015(3) -0.011(2) C60 0.142(5) 0.082(4) 0.075(3) 0.007(3) 0.017(4) 0.005(4) C61 0.139(5) 0.080(4) 0.073(3) 0.029(3) 0.028(4) 0.025(4) C62 0.128(4) 0.068(3) 0.057(3) 0.021(2) 0.028(3) 0.002(3) C63 0.127(5) 0.059(3) 0.041(2) 0.007(2) 0.019(3) -0.030(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.050160(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 . Co1 . 3.0319(4) yes Nb1 . P1 . 2.9727(7) yes Nb1 . P2 . 2.9738(7) yes Nb1 . P3 . 2.9859(7) yes Nb1 . N1 . 2.050(2) yes Nb1 . N2 . 2.052(2) yes Nb1 . N3 . 2.053(2) yes Nb1 . N4 . 1.775(2) yes I1 . Co1 . 2.5316(4) yes Co1 . P1 . 2.2458(7) yes Co1 . P2 . 2.2524(7) yes Co1 . P3 . 2.2519(8) yes P1 . N1 . 1.680(2) yes P1 . C1 . 1.826(3) yes P1 . C7 . 1.830(3) yes P2 . N2 . 1.681(2) yes P2 . C16 . 1.841(3) yes P2 . C22 . 1.831(3) yes P3 . N3 . 1.685(2) yes P3 . C31 . 1.833(3) yes P3 . C37 . 1.843(3) yes N1 . C13 . 1.488(3) yes N2 . C28 . 1.489(3) yes N3 . C43 . 1.492(4) yes N4 . C46 . 1.476(3) yes C1 . C2 . 1.393(4) yes C1 . C6 . 1.408(4) yes C2 . C3 . 1.396(4) yes C2 . H21 . 0.932 no C3 . C4 . 1.378(5) yes C3 . H31 . 0.938 no C4 . C5 . 1.383(5) yes C4 . H41 . 0.937 no C5 . C6 . 1.391(4) yes C5 . H51 . 0.929 no C6 . H61 . 0.935 no C7 . C8 . 1.390(4) yes C7 . C12 . 1.400(4) yes C8 . C9 . 1.391(4) yes C8 . H81 . 0.938 no C9 . C10 . 1.388(5) yes C9 . H91 . 0.945 no C10 . C11 . 1.383(4) yes C10 . H101 . 0.936 no C11 . C12 . 1.381(4) yes C11 . H111 . 0.916 no C12 . H121 . 0.943 no C13 . C14 . 1.521(4) yes C13 . C15 . 1.515(4) yes C13 . H131 . 0.977 no C14 . H141 . 0.963 no C14 . H142 . 0.957 no C14 . H143 . 0.977 no C15 . H152 . 0.979 no C15 . H151 . 0.957 no C15 . H153 . 0.965 no C16 . C17 . 1.388(4) yes C16 . C21 . 1.401(4) yes C17 . C18 . 1.384(4) yes C17 . H171 . 0.931 no C18 . C19 . 1.385(4) yes C18 . H181 . 0.936 no C19 . C20 . 1.384(4) yes C19 . H191 . 0.930 no C20 . C21 . 1.389(4) yes C20 . H201 . 0.931 no C21 . H211 . 0.932 no C22 . C23 . 1.396(4) yes C22 . C27 . 1.395(4) yes C23 . C24 . 1.378(4) yes C23 . H231 . 0.931 no C24 . C25 . 1.381(5) yes C24 . H241 . 0.938 no C25 . C26 . 1.382(5) yes C25 . H251 . 0.935 no C26 . C27 . 1.389(4) yes C26 . H261 . 0.934 no C27 . H271 . 0.934 no C28 . C29 . 1.515(4) yes C28 . C30 . 1.523(5) yes C28 . H281 . 0.978 no C29 . H293 . 0.982 no C29 . H292 . 0.960 no C29 . H291 . 0.962 no C30 . H302 . 0.964 no C30 . H303 . 0.953 no C30 . H301 . 0.951 no C31 . C32 . 1.394(4) yes C31 . C36 . 1.389(4) yes C32 . C33 . 1.382(5) yes C32 . H321 . 0.941 no C33 . C34 . 1.374(6) yes C33 . H331 . 0.944 no C34 . C35 . 1.374(6) yes C34 . H341 . 0.931 no C35 . C36 . 1.397(5) yes C35 . H351 . 0.938 no C36 . H361 . 0.922 no C37 . C38 . 1.402(4) yes C37 . C42 . 1.384(4) yes C38 . C39 . 1.389(5) yes C38 . H381 . 0.945 no C39 . C40 . 1.386(5) yes C39 . H391 . 0.946 no C40 . C41 . 1.381(5) yes C40 . H401 . 0.937 no C41 . C42 . 1.389(4) yes C41 . H411 . 0.945 no C42 . H421 . 0.936 no C43 . C44 . 1.523(5) yes C43 . C45 . 1.517(4) yes C43 . H431 . 0.992 no C44 . H441 . 0.968 no C44 . H443 . 0.978 no C44 . H442 . 0.962 no C45 . H451 . 0.974 no C45 . H452 . 0.958 no C45 . H453 . 0.952 no C46 . C47 . 1.540(5) yes C46 . C48 . 1.536(4) yes C46 . C49 . 1.531(4) yes C47 . H471 . 0.944 no C47 . H472 . 0.958 no C47 . H473 . 0.963 no C48 . H481 . 0.967 no C48 . H483 . 0.963 no C48 . H482 . 0.975 no C49 . H492 . 0.968 no C49 . H493 . 0.957 no C49 . H491 . 0.974 no C50 . C51 . 1.491(10) yes C50 . H501 . 0.950 no C50 . H502 . 0.950 no C50 . H503 . 0.950 no C51 . C52 . 1.391(6) yes C51 . C56 . 1.308(7) yes C52 . C53 . 1.390(8) yes C52 . H521 . 0.985 no C53 . C54 . 1.424(7) yes C53 . H531 . 0.958 no C54 . C55 . 1.316(7) yes C54 . H541 . 0.962 no C55 . C56 . 1.444(7) yes C55 . H551 . 0.920 no C56 . H561 . 0.940 no C57 . C58 . 1.411(9) yes C57 . H571 . 0.983 no C57 . H572 . 1.002 no C57 . H573 . 0.996 no C58 . C59 . 1.392(6) yes C58 . C63 . 1.417(6) yes C59 . C60 . 1.404(7) yes C59 . H591 . 0.915 no C60 . C61 . 1.330(7) yes C60 . H601 . 0.954 no C61 . C62 . 1.372(7) yes C61 . H611 . 0.967 no C62 . C63 . 1.351(6) yes C62 . H621 . 0.930 no C63 . H631 . 0.927 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Co1 . Nb1 . P1 . 43.913(15) yes Co1 . Nb1 . P2 . 44.042(14) yes P1 . Nb1 . P2 . 74.557(19) yes Co1 . Nb1 . P3 . 43.943(15) yes P1 . Nb1 . P3 . 74.063(19) yes P2 . Nb1 . P3 . 73.108(19) yes Co1 . Nb1 . N1 . 76.71(6) yes P1 . Nb1 . N1 . 33.04(6) yes P2 . Nb1 . N1 . 103.53(6) yes P3 . Nb1 . N1 . 97.36(6) yes Co1 . Nb1 . N2 . 76.60(6) yes P1 . Nb1 . N2 . 96.56(6) yes P2 . Nb1 . N2 . 33.06(6) yes P3 . Nb1 . N2 . 102.66(6) yes N1 . Nb1 . N2 . 114.25(9) yes Co1 . Nb1 . N3 . 76.69(7) yes P1 . Nb1 . N3 . 102.49(7) yes P2 . Nb1 . N3 . 96.35(7) yes P3 . Nb1 . N3 . 32.92(7) yes N1 . Nb1 . N3 . 114.66(9) yes Co1 . Nb1 . N4 . 179.64(7) yes P1 . Nb1 . N4 . 136.13(8) yes P2 . Nb1 . N4 . 135.63(8) yes P3 . Nb1 . N4 . 136.34(8) yes N1 . Nb1 . N4 . 103.37(10) yes N2 . Nb1 . N3 . 115.63(9) yes N2 . Nb1 . N4 . 103.06(10) yes N3 . Nb1 . N4 . 103.58(10) yes Nb1 . Co1 . I1 . 175.062(15) yes Nb1 . Co1 . P1 . 66.642(19) yes I1 . Co1 . P1 . 109.35(2) yes Nb1 . Co1 . P2 . 66.609(19) yes I1 . Co1 . P2 . 112.89(2) yes P1 . Co1 . P2 . 106.39(3) yes Nb1 . Co1 . P3 . 66.94(2) yes I1 . Co1 . P3 . 117.58(2) yes P1 . Co1 . P3 . 105.85(3) yes P2 . Co1 . P3 . 104.00(3) yes Nb1 . P1 . Co1 . 69.45(2) yes Co1 . P1 . N1 . 110.74(8) yes Nb1 . P1 . C1 . 135.94(9) yes Co1 . P1 . C1 . 115.84(10) yes N1 . P1 . C1 . 110.04(12) yes Nb1 . P1 . C7 . 117.99(9) yes Co1 . P1 . C7 . 113.05(9) yes N1 . P1 . C7 . 105.89(12) yes C1 . P1 . C7 . 100.47(12) yes Nb1 . P2 . Co1 . 69.35(2) yes Co1 . P2 . N2 . 110.24(8) yes Nb1 . P2 . C16 . 136.32(9) yes Co1 . P2 . C16 . 116.08(9) yes N2 . P2 . C16 . 108.54(12) yes Nb1 . P2 . C22 . 116.90(9) yes Co1 . P2 . C22 . 115.01(9) yes N2 . P2 . C22 . 105.88(12) yes C16 . P2 . C22 . 100.22(12) yes Nb1 . P3 . Co1 . 69.11(2) yes Co1 . P3 . N3 . 110.28(8) yes Nb1 . P3 . C31 . 119.41(10) yes Co1 . P3 . C31 . 116.71(10) yes N3 . P3 . C31 . 104.05(13) yes Nb1 . P3 . C37 . 133.97(10) yes Co1 . P3 . C37 . 112.71(10) yes N3 . P3 . C37 . 111.39(13) yes C31 . P3 . C37 . 101.13(13) yes P1 . N1 . Nb1 . 105.26(11) yes P1 . N1 . C13 . 121.37(18) yes Nb1 . N1 . C13 . 133.32(18) yes P2 . N2 . Nb1 . 105.19(11) yes P2 . N2 . C28 . 119.75(18) yes Nb1 . N2 . C28 . 135.06(18) yes P3 . N3 . Nb1 . 105.61(11) yes P3 . N3 . C43 . 119.73(19) yes Nb1 . N3 . C43 . 134.60(19) yes Nb1 . N4 . C46 . 177.9(2) yes P1 . C1 . C2 . 119.6(2) yes P1 . C1 . C6 . 122.4(2) yes C2 . C1 . C6 . 118.0(3) yes C1 . C2 . C3 . 120.9(3) yes C1 . C2 . H21 . 118.3 no C3 . C2 . H21 . 120.9 no C2 . C3 . C4 . 120.2(3) yes C2 . C3 . H31 . 119.6 no C4 . C3 . H31 . 120.1 no C3 . C4 . C5 . 120.0(3) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 120.2(3) yes C4 . C5 . H51 . 121.1 no C6 . C5 . H51 . 118.7 no C1 . C6 . C5 . 120.7(3) yes C1 . C6 . H61 . 119.1 no C5 . C6 . H61 . 120.2 no P1 . C7 . C8 . 121.1(2) yes P1 . C7 . C12 . 119.8(2) yes C8 . C7 . C12 . 118.6(3) yes C7 . C8 . C9 . 120.3(3) yes C7 . C8 . H81 . 119.4 no C9 . C8 . H81 . 120.4 no C8 . C9 . C10 . 120.7(3) yes C8 . C9 . H91 . 119.7 no C10 . C9 . H91 . 119.5 no C9 . C10 . C11 . 118.9(3) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 121.1 no C10 . C11 . C12 . 120.8(3) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 119.7 no C7 . C12 . C11 . 120.6(3) yes C7 . C12 . H121 . 119.2 no C11 . C12 . H121 . 120.3 no N1 . C13 . C14 . 108.9(2) yes N1 . C13 . C15 . 112.0(2) yes C14 . C13 . C15 . 111.6(3) yes N1 . C13 . H131 . 107.6 no C14 . C13 . H131 . 108.5 no C15 . C13 . H131 . 108.1 no C13 . C14 . H141 . 110.0 no C13 . C14 . H142 . 109.4 no H141 . C14 . H142 . 109.4 no C13 . C14 . H143 . 109.4 no H141 . C14 . H143 . 109.2 no H142 . C14 . H143 . 109.4 no C13 . C15 . H152 . 109.5 no C13 . C15 . H151 . 110.5 no H152 . C15 . H151 . 108.3 no C13 . C15 . H153 . 110.3 no H152 . C15 . H153 . 108.8 no H151 . C15 . H153 . 109.5 no P2 . C16 . C17 . 118.5(2) yes P2 . C16 . C21 . 123.2(2) yes C17 . C16 . C21 . 118.3(2) yes C16 . C17 . C18 . 120.9(3) yes C16 . C17 . H171 . 120.4 no C18 . C17 . H171 . 118.7 no C17 . C18 . C19 . 120.2(3) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 120.3 no C18 . C19 . C20 . 119.8(3) yes C18 . C19 . H191 . 120.9 no C20 . C19 . H191 . 119.3 no C19 . C20 . C21 . 119.9(3) yes C19 . C20 . H201 . 119.8 no C21 . C20 . H201 . 120.2 no C16 . C21 . C20 . 120.8(3) yes C16 . C21 . H211 . 120.3 no C20 . C21 . H211 . 118.9 no P2 . C22 . C23 . 120.7(2) yes P2 . C22 . C27 . 120.3(2) yes C23 . C22 . C27 . 118.8(3) yes C22 . C23 . C24 . 120.7(3) yes C22 . C23 . H231 . 119.2 no C24 . C23 . H231 . 120.1 no C23 . C24 . C25 . 120.3(3) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 118.8 no C24 . C25 . C26 . 119.7(3) yes C24 . C25 . H251 . 120.1 no C26 . C25 . H251 . 120.3 no C25 . C26 . C27 . 120.5(3) yes C25 . C26 . H261 . 120.3 no C27 . C26 . H261 . 119.2 no C22 . C27 . C26 . 120.0(3) yes C22 . C27 . H271 . 119.5 no C26 . C27 . H271 . 120.5 no N2 . C28 . C29 . 111.8(3) yes N2 . C28 . C30 . 109.5(2) yes C29 . C28 . C30 . 113.6(3) yes N2 . C28 . H281 . 108.6 no C29 . C28 . H281 . 105.0 no C30 . C28 . H281 . 108.1 no C28 . C29 . H293 . 110.3 no C28 . C29 . H292 . 110.9 no H293 . C29 . H292 . 108.5 no C28 . C29 . H291 . 110.4 no H293 . C29 . H291 . 108.4 no H292 . C29 . H291 . 108.3 no C28 . C30 . H302 . 109.8 no C28 . C30 . H303 . 109.2 no H302 . C30 . H303 . 109.3 no C28 . C30 . H301 . 109.4 no H302 . C30 . H301 . 109.2 no H303 . C30 . H301 . 109.9 no P3 . C31 . C32 . 119.4(2) yes P3 . C31 . C36 . 121.7(2) yes C32 . C31 . C36 . 118.6(3) yes C31 . C32 . C33 . 120.9(3) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 119.6 no C32 . C33 . C34 . 120.1(4) yes C32 . C33 . H331 . 120.3 no C34 . C33 . H331 . 119.6 no C33 . C34 . C35 . 120.0(3) yes C33 . C34 . H341 . 119.6 no C35 . C34 . H341 . 120.4 no C34 . C35 . C36 . 120.5(4) yes C34 . C35 . H351 . 119.8 no C36 . C35 . H351 . 119.7 no C35 . C36 . C31 . 119.9(3) yes C35 . C36 . H361 . 119.8 no C31 . C36 . H361 . 120.3 no P3 . C37 . C38 . 123.9(2) yes P3 . C37 . C42 . 118.0(2) yes C38 . C37 . C42 . 118.1(3) yes C37 . C38 . C39 . 120.6(3) yes C37 . C38 . H381 . 119.7 no C39 . C38 . H381 . 119.7 no C38 . C39 . C40 . 120.2(3) yes C38 . C39 . H391 . 120.0 no C40 . C39 . H391 . 119.8 no C39 . C40 . C41 . 119.8(3) yes C39 . C40 . H401 . 119.8 no C41 . C40 . H401 . 120.4 no C40 . C41 . C42 . 119.9(3) yes C40 . C41 . H411 . 119.7 no C42 . C41 . H411 . 120.4 no C41 . C42 . C37 . 121.5(3) yes C41 . C42 . H421 . 119.1 no C37 . C42 . H421 . 119.5 no N3 . C43 . C44 . 109.5(3) yes N3 . C43 . C45 . 112.6(2) yes C44 . C43 . C45 . 111.8(3) yes N3 . C43 . H431 . 106.5 no C44 . C43 . H431 . 108.1 no C45 . C43 . H431 . 108.0 no C43 . C44 . H441 . 110.6 no C43 . C44 . H443 . 110.4 no H441 . C44 . H443 . 108.8 no C43 . C44 . H442 . 109.4 no H441 . C44 . H442 . 109.2 no H443 . C44 . H442 . 108.4 no C43 . C45 . H451 . 109.5 no C43 . C45 . H452 . 109.3 no H451 . C45 . H452 . 109.5 no C43 . C45 . H453 . 108.6 no H451 . C45 . H453 . 109.9 no H452 . C45 . H453 . 110.0 no N4 . C46 . C47 . 109.1(2) yes N4 . C46 . C48 . 110.2(2) yes C47 . C46 . C48 . 109.3(3) yes N4 . C46 . C49 . 109.9(2) yes C47 . C46 . C49 . 109.8(3) yes C48 . C46 . C49 . 108.4(3) yes C46 . C47 . H471 . 109.6 no C46 . C47 . H472 . 110.1 no H471 . C47 . H472 . 108.5 no C46 . C47 . H473 . 108.9 no H471 . C47 . H473 . 108.0 no H472 . C47 . H473 . 111.7 no C46 . C48 . H481 . 109.9 no C46 . C48 . H483 . 110.3 no H481 . C48 . H483 . 108.4 no C46 . C48 . H482 . 111.3 no H481 . C48 . H482 . 107.2 no H483 . C48 . H482 . 109.6 no C46 . C49 . H492 . 109.1 no C46 . C49 . H493 . 110.9 no H492 . C49 . H493 . 109.4 no C46 . C49 . H491 . 110.7 no H492 . C49 . H491 . 107.9 no H493 . C49 . H491 . 108.9 no C51 . C50 . H501 . 109.5 no C51 . C50 . H502 . 109.4 no H501 . C50 . H502 . 109.5 no C51 . C50 . H503 . 109.5 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no C50 . C51 . C52 . 118.3(7) yes C50 . C51 . C56 . 114.6(6) yes C52 . C51 . C56 . 127.1(8) yes C51 . C52 . C53 . 112.9(8) yes C51 . C52 . H521 . 118.7 no C53 . C52 . H521 . 128.4 no C52 . C53 . C54 . 124.3(7) yes C52 . C53 . H531 . 118.6 no C54 . C53 . H531 . 117.1 no C53 . C54 . C55 . 115.6(8) yes C53 . C54 . H541 . 123.6 no C55 . C54 . H541 . 120.8 no C54 . C55 . C56 . 123.7(6) yes C54 . C55 . H551 . 116.6 no C56 . C55 . H551 . 119.7 no C55 . C56 . C51 . 115.6(6) yes C55 . C56 . H561 . 123.7 no C51 . C56 . H561 . 120.7 no C58 . C57 . H571 . 106.8 no C58 . C57 . H572 . 102.6 no H571 . C57 . H572 . 113.2 no C58 . C57 . H573 . 111.5 no H571 . C57 . H573 . 112.6 no H572 . C57 . H573 . 109.8 no C57 . C58 . C59 . 121.3(6) yes C57 . C58 . C63 . 119.6(7) yes C59 . C58 . C63 . 119.2(6) yes C58 . C59 . C60 . 119.3(5) yes C58 . C59 . H591 . 120.2 no C60 . C59 . H591 . 120.5 no C59 . C60 . C61 . 123.3(7) yes C59 . C60 . H601 . 121.8 no C61 . C60 . H601 . 114.9 no C60 . C61 . C62 . 114.2(7) yes C60 . C61 . H611 . 120.5 no C62 . C61 . H611 . 125.3 no C61 . C62 . C63 . 128.9(6) yes C61 . C62 . H621 . 116.4 no C63 . C62 . H621 . 114.7 no C58 . C63 . C62 . 115.0(6) yes C58 . C63 . H631 . 122.0 no C62 . C63 . H631 . 122.9 no _iucr_refine_instruction_details_constraints ; # # Punched on 10/07/11 at 10:12:36 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 293,X'S) H ( 292,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 302,X'S) H ( 303,X'S) H ( 301,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 443,X'S) H ( 442,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) H ( 473,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 483,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 492,X'S) H ( 493,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) H ( 503,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) H ( 573,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 60,X'S) H ( 601,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 63,X'S) H ( 631,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 10/07/11 at 10:12:36 # #LIST 16 NO DISTANCE 1.390000 , 0.010000 = C(51) TO C(56) DISTANCE 1.390000 , 0.010000 = C(51) TO C(52) DISTANCE 1.390000 , 0.010000 = C(52) TO C(53) DISTANCE 1.390000 , 0.010000 = C(53) TO C(54) DISTANCE 1.390000 , 0.010000 = C(54) TO C(55) DISTANCE 1.390000 , 0.010000 = C(55) TO C(56) U(IJ)'S 0.0, 0.010000 = C(51) TO C(56) U(IJ)'S 0.0, 0.010000 = C(51) TO C(52) U(IJ)'S 0.0, 0.010000 = C(52) TO C(53) U(IJ)'S 0.0, 0.010000 = C(53) TO C(54) U(IJ)'S 0.0, 0.010000 = C(54) TO C(55) U(IJ)'S 0.0, 0.010000 = C(55) TO C(56) U(IJ)'S 0.0, 0.005000 = C(50) TO C(51) DISTANCE 1.390000 , 0.010000 = C(58) TO C(63) DISTANCE 1.390000 , 0.010000 = C(58) TO C(59) DISTANCE 1.390000 , 0.010000 = C(59) TO C(60) DISTANCE 1.390000 , 0.010000 = C(60) TO C(61) DISTANCE 1.390000 , 0.010000 = C(61) TO C(62) DISTANCE 1.390000 , 0.010000 = C(62) TO C(63) U(IJ)'S 0.0, 0.010000 = C(57) TO C(58) U(IJ)'S 0.0, 0.010000 = C(58) TO C(59) U(IJ)'S 0.0, 0.010000 = C(59) TO C(60) U(IJ)'S 0.0, 0.010000 = C(60) TO C(61) U(IJ)'S 0.0, 0.010000 = C(61) TO C(62) U(IJ)'S 0.0, 0.010000 = C(62) TO C(62) U(IJ)'S 0.0, 0.005000 = C(57) TO C(62) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END data_2Ta _database_code_depnum_ccdc_archive 'CCDC 862675' #TrackingRef '- combined_22Feb.cif' _audit_creation_date 10-11-20 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title 'AB20_0m in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.1400(6) _cell_length_b 18.2564(7) _cell_length_c 25.2782(11) _cell_angle_alpha 90 _cell_angle_beta 95.270(2) _cell_angle_gamma 90 _cell_volume 6038.3(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ta -0.7052 6.5227 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C63 H76 Co1 I1 N4 P3 Ta1 # Dc = 1.48 Fooo = 2720.00 Mu = 27.17 M = 1349.03 # Found Formula = C63 H76 Co1 I1 N4 P3 Ta1 # Dc = 1.48 FOOO = 2720.00 Mu = 27.17 M = 1349.03 _chemical_formula_sum 'C63 H76 Co1 I1 N4 P3 Ta1' _chemical_formula_moiety 'C49 H60 Co I N4 P3 Ta,2(C7 H8)' _chemical_compound_source ? _chemical_formula_weight 1349.03 _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_min 0.314 _exptl_crystal_size_mid 0.548 _exptl_crystal_size_max 0.619 _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 2.717 # Sheldrick geometric approximatio 0.23 0.43 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 0.43 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 43911 _reflns_number_total 17465 _diffrn_reflns_av_R_equivalents 0.020 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 17465 # Theoretical number of reflections is about 35409 _diffrn_reflns_theta_min 1.378 _diffrn_reflns_theta_max 30.057 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 29.456 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 1.29 _oxford_diffrn_Wilson_scale 237.55 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.01 _refine_diff_density_max 1.50 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 17465 _refine_ls_number_restraints 90 _refine_ls_number_parameters 658 _oxford_refine_ls_R_factor_ref 0.0316 _refine_ls_wR_factor_ref 0.0635 _refine_ls_goodness_of_fit_ref 1.0001 _refine_ls_shift/su_max 0.0085188 _refine_ls_shift/su_mean 0.0002436 # The values computed from all data _oxford_reflns_number_all 17465 _refine_ls_R_factor_all 0.0316 _refine_ls_wR_factor_all 0.0635 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 14745 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_gt 0.0558 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +10.11P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ta1 Ta 0.103643(7) 0.447131(5) 0.674974(4) 0.0147 1.0000 Uani . . . . . . I1 I 0.498357(13) 0.455672(9) 0.775622(7) 0.0288 1.0000 Uani . . . . . . Co1 Co 0.31627(2) 0.448493(16) 0.733472(12) 0.0152 1.0000 Uani . . . . . . P1 P 0.27781(4) 0.55189(3) 0.68792(2) 0.0158 1.0000 Uani . . . . . . P2 P 0.29184(4) 0.35586(3) 0.67495(2) 0.0156 1.0000 Uani . . . . . . P3 P 0.19196(5) 0.43359(3) 0.78797(2) 0.0179 1.0000 Uani . . . . . . N1 N 0.15503(15) 0.55052(10) 0.66213(8) 0.0170 1.0000 Uani . . . . . . N2 N 0.17921(15) 0.36675(10) 0.63814(8) 0.0180 1.0000 Uani . . . . . . N3 N 0.07767(15) 0.42595(11) 0.75201(8) 0.0196 1.0000 Uani . . . . . . N4 N -0.02116(15) 0.44604(11) 0.64022(8) 0.0193 1.0000 Uani . . . . . . C1 C 0.30526(18) 0.63735(13) 0.72408(10) 0.0204 1.0000 Uani . . . . . . C2 C 0.3228(2) 0.63604(15) 0.77941(10) 0.0255 1.0000 Uani . . . . . . C3 C 0.3443(2) 0.70044(17) 0.80816(12) 0.0330 1.0000 Uani . . . . . . C4 C 0.3492(2) 0.76644(15) 0.78177(13) 0.0338 1.0000 Uani . . . . . . C5 C 0.3341(2) 0.76896(14) 0.72692(13) 0.0308 1.0000 Uani . . . . . . C6 C 0.3118(2) 0.70514(13) 0.69824(11) 0.0251 1.0000 Uani . . . . . . C7 C 0.35403(18) 0.56488(12) 0.63167(9) 0.0181 1.0000 Uani . . . . . . C8 C 0.3182(2) 0.54190(13) 0.58085(10) 0.0223 1.0000 Uani . . . . . . C9 C 0.3812(2) 0.54540(16) 0.53944(11) 0.0293 1.0000 Uani . . . . . . C10 C 0.4806(2) 0.57059(15) 0.54852(11) 0.0287 1.0000 Uani . . . . . . C11 C 0.5174(2) 0.59202(14) 0.59952(12) 0.0280 1.0000 Uani . . . . . . C12 C 0.4545(2) 0.58988(13) 0.64055(10) 0.0234 1.0000 Uani . . . . . . C13 C 0.1051(2) 0.61719(13) 0.63821(10) 0.0232 1.0000 Uani . . . . . . C14 C 0.0270(2) 0.64520(16) 0.67448(12) 0.0354 1.0000 Uani . . . . . . C15 C 0.0565(2) 0.60375(15) 0.58235(10) 0.0278 1.0000 Uani . . . . . . C16 C 0.39216(17) 0.34223(12) 0.62998(9) 0.0172 1.0000 Uani . . . . . . C17 C 0.46415(18) 0.39729(13) 0.62614(10) 0.0208 1.0000 Uani . . . . . . C18 C 0.5427(2) 0.38931(14) 0.59353(11) 0.0267 1.0000 Uani . . . . . . C19 C 0.5512(2) 0.32601(15) 0.56443(11) 0.0290 1.0000 Uani . . . . . . C20 C 0.4806(2) 0.27016(15) 0.56771(11) 0.0274 1.0000 Uani . . . . . . C21 C 0.4017(2) 0.27785(13) 0.60047(10) 0.0227 1.0000 Uani . . . . . . C22 C 0.28744(18) 0.26468(12) 0.70442(10) 0.0191 1.0000 Uani . . . . . . C23 C 0.3767(2) 0.22443(13) 0.71595(10) 0.0232 1.0000 Uani . . . . . . C24 C 0.3735(2) 0.15595(15) 0.73973(11) 0.0304 1.0000 Uani . . . . . . C25 C 0.2817(3) 0.12755(15) 0.75327(12) 0.0368 1.0000 Uani . . . . . . C26 C 0.1935(3) 0.16779(15) 0.74331(13) 0.0354 1.0000 Uani . . . . . . C27 C 0.1951(2) 0.23613(14) 0.71888(11) 0.0264 1.0000 Uani . . . . . . C28 C 0.1546(2) 0.32057(14) 0.59024(11) 0.0260 1.0000 Uani . . . . . . C29 C 0.0557(2) 0.27830(16) 0.59248(14) 0.0350 1.0000 Uani . . . . . . C30 C 0.1562(3) 0.36744(19) 0.54051(12) 0.0386 1.0000 Uani . . . . . . C31 C 0.1736(2) 0.50808(14) 0.83470(10) 0.0247 1.0000 Uani . . . . . . C32 C 0.1103(2) 0.56685(15) 0.81804(12) 0.0318 1.0000 Uani . . . . . . C33 C 0.1009(3) 0.62694(18) 0.85096(15) 0.0438 1.0000 Uani . . . . . . C34 C 0.1543(3) 0.6290(2) 0.90028(15) 0.0503 1.0000 Uani . . . . . . C35 C 0.2178(3) 0.5719(2) 0.91727(14) 0.0498 1.0000 Uani . . . . . . C36 C 0.2282(3) 0.51121(18) 0.88441(12) 0.0364 1.0000 Uani . . . . . . C37 C 0.2152(2) 0.35565(14) 0.83393(10) 0.0237 1.0000 Uani . . . . . . C38 C 0.1525(2) 0.33684(18) 0.87343(12) 0.0367 1.0000 Uani . . . . . . C39 C 0.1772(3) 0.27877(19) 0.90752(13) 0.0440 1.0000 Uani . . . . . . C40 C 0.2661(3) 0.23960(18) 0.90383(13) 0.0432 1.0000 Uani . . . . . . C41 C 0.3304(3) 0.25844(17) 0.86594(12) 0.0403 1.0000 Uani . . . . . . C42 C 0.3047(2) 0.31606(14) 0.83090(11) 0.0298 1.0000 Uani . . . . . . C43 C -0.0156(2) 0.40898(15) 0.77919(11) 0.0264 1.0000 Uani . . . . . . C44 C -0.0469(2) 0.33011(16) 0.76898(15) 0.0386 1.0000 Uani . . . . . . C45 C -0.1027(2) 0.46201(17) 0.76412(13) 0.0333 1.0000 Uani . . . . . . C46 C -0.12273(18) 0.44243(14) 0.61196(11) 0.0243 1.0000 Uani . . . . . . C47 C -0.1818(2) 0.37659(17) 0.63182(15) 0.0388 1.0000 Uani . . . . . . C48 C -0.1839(2) 0.51292(16) 0.62055(13) 0.0336 1.0000 Uani . . . . . . C49 C -0.1153(2) 0.43384(17) 0.55191(12) 0.0342 1.0000 Uani . . . . . . C50 C 0.5141(6) 0.5623(3) 0.9256(3) 0.1097 1.0000 Uani . U . . . . C51 C 0.6276(7) 0.5750(3) 0.9318(2) 0.1105 1.0000 Uani D U . . . . C52 C 0.6774(6) 0.5871(4) 0.9829(2) 0.1091 1.0000 Uani D U . . . . C53 C 0.7824(7) 0.5911(4) 0.9848(2) 0.1242 1.0000 Uani D U . . . . C54 C 0.8371(7) 0.5947(4) 0.9387(2) 0.1202 1.0000 Uani D U . . . . C55 C 0.7803(6) 0.5905(3) 0.8925(2) 0.1040 1.0000 Uani D U . . . . C56 C 0.6720(6) 0.5771(3) 0.8874(2) 0.1149 1.0000 Uani D U . . . . C57 C 0.0871(7) 0.8938(4) 0.5533(3) 0.1208 1.0000 Uani . U . . . . C58 C 0.1800(5) 0.8514(3) 0.5574(2) 0.0890 1.0000 Uani D U . . . . C59 C 0.2723(4) 0.8806(2) 0.5800(2) 0.0768 1.0000 Uani D U . . . . C60 C 0.3592(6) 0.8383(3) 0.5794(2) 0.1005 1.0000 Uani D U . . . . C61 C 0.3619(6) 0.7708(3) 0.5614(2) 0.1026 1.0000 Uani D U . . . . C62 C 0.2679(6) 0.7441(3) 0.5423(2) 0.0883 1.0000 Uani D U . . . . C63 C 0.1775(5) 0.7792(3) 0.53862(18) 0.0807 1.0000 Uani D . . . . . H21 H 0.3204 0.5917 0.7969 0.0306 1.0000 Uiso R . . . . . H31 H 0.3553 0.6985 0.8455 0.0393 1.0000 Uiso R . . . . . H41 H 0.3650 0.8102 0.8010 0.0409 1.0000 Uiso R . . . . . H51 H 0.3390 0.8136 0.7096 0.0365 1.0000 Uiso R . . . . . H61 H 0.3002 0.7068 0.6616 0.0292 1.0000 Uiso R . . . . . H81 H 0.2518 0.5232 0.5750 0.0272 1.0000 Uiso R . . . . . H91 H 0.3557 0.5314 0.5047 0.0353 1.0000 Uiso R . . . . . H101 H 0.5215 0.5736 0.5205 0.0344 1.0000 Uiso R . . . . . H111 H 0.5840 0.6088 0.6063 0.0339 1.0000 Uiso R . . . . . H121 H 0.4797 0.6055 0.6736 0.0280 1.0000 Uiso R . . . . . H131 H 0.1584 0.6538 0.6369 0.0281 1.0000 Uiso R . . . . . H141 H -0.0081 0.6872 0.6589 0.0530 1.0000 Uiso R . . . . . H142 H 0.0596 0.6576 0.7089 0.0529 1.0000 Uiso R . . . . . H143 H -0.0234 0.6069 0.6793 0.0523 1.0000 Uiso R . . . . . H151 H 0.0086 0.5648 0.5810 0.0416 1.0000 Uiso R . . . . . H152 H 0.0198 0.6464 0.5689 0.0411 1.0000 Uiso R . . . . . H153 H 0.1068 0.5933 0.5587 0.0420 1.0000 Uiso R . . . . . H171 H 0.4600 0.4401 0.6456 0.0250 1.0000 Uiso R . . . . . H181 H 0.5910 0.4264 0.5924 0.0320 1.0000 Uiso R . . . . . H191 H 0.6035 0.3219 0.5421 0.0353 1.0000 Uiso R . . . . . H201 H 0.4857 0.2267 0.5477 0.0330 1.0000 Uiso R . . . . . H211 H 0.3544 0.2400 0.6029 0.0267 1.0000 Uiso R . . . . . H231 H 0.4396 0.2434 0.7074 0.0281 1.0000 Uiso R . . . . . H241 H 0.4341 0.1277 0.7456 0.0359 1.0000 Uiso R . . . . . H251 H 0.2795 0.0820 0.7684 0.0442 1.0000 Uiso R . . . . . H261 H 0.1325 0.1489 0.7524 0.0424 1.0000 Uiso R . . . . . H271 H 0.1350 0.2629 0.7114 0.0316 1.0000 Uiso R . . . . . H281 H 0.2088 0.2836 0.5907 0.0311 1.0000 Uiso R . . . . . H291 H -0.0005 0.3105 0.5990 0.0528 1.0000 Uiso R . . . . . H292 H 0.0622 0.2422 0.6201 0.0531 1.0000 Uiso R . . . . . H293 H 0.0390 0.2523 0.5595 0.0528 1.0000 Uiso R . . . . . H301 H 0.2221 0.3894 0.5389 0.0573 1.0000 Uiso R . . . . . H302 H 0.1394 0.3394 0.5086 0.0576 1.0000 Uiso R . . . . . H303 H 0.1052 0.4063 0.5413 0.0572 1.0000 Uiso R . . . . . H321 H 0.0737 0.5658 0.7840 0.0384 1.0000 Uiso R . . . . . H331 H 0.0569 0.6659 0.8396 0.0529 1.0000 Uiso R . . . . . H341 H 0.1479 0.6688 0.9220 0.0597 1.0000 Uiso R . . . . . H351 H 0.2563 0.5744 0.9509 0.0602 1.0000 Uiso R . . . . . H361 H 0.2735 0.4725 0.8954 0.0440 1.0000 Uiso R . . . . . H381 H 0.0939 0.3649 0.8775 0.0442 1.0000 Uiso R . . . . . H391 H 0.1336 0.2677 0.9338 0.0530 1.0000 Uiso R . . . . . H401 H 0.2838 0.2004 0.9274 0.0518 1.0000 Uiso R . . . . . H411 H 0.3916 0.2330 0.8636 0.0479 1.0000 Uiso R . . . . . H421 H 0.3484 0.3282 0.8048 0.0353 1.0000 Uiso R . . . . . H431 H 0.0030 0.4150 0.8167 0.0312 1.0000 Uiso R . . . . . H441 H -0.1045 0.3186 0.7882 0.0578 1.0000 Uiso R . . . . . H442 H -0.0655 0.3226 0.7321 0.0569 1.0000 Uiso R . . . . . H443 H 0.0089 0.2984 0.7813 0.0572 1.0000 Uiso R . . . . . H451 H -0.1626 0.4459 0.7798 0.0501 1.0000 Uiso R . . . . . H452 H -0.0837 0.5109 0.7766 0.0497 1.0000 Uiso R . . . . . H453 H -0.1179 0.4616 0.7260 0.0497 1.0000 Uiso R . . . . . H471 H -0.2457 0.3717 0.6095 0.0581 1.0000 Uiso R . . . . . H472 H -0.1959 0.3841 0.6685 0.0570 1.0000 Uiso R . . . . . H473 H -0.1405 0.3336 0.6285 0.0576 1.0000 Uiso R . . . . . H481 H -0.2520 0.5096 0.6032 0.0500 1.0000 Uiso R . . . . . H482 H -0.1508 0.5549 0.6063 0.0492 1.0000 Uiso R . . . . . H483 H -0.1889 0.5208 0.6581 0.0498 1.0000 Uiso R . . . . . H491 H -0.0816 0.3893 0.5451 0.0505 1.0000 Uiso R . . . . . H492 H -0.1832 0.4321 0.5345 0.0507 1.0000 Uiso R . . . . . H493 H -0.0787 0.4732 0.5380 0.0506 1.0000 Uiso R . . . . . H501 H 0.4989 0.5157 0.9101 0.1207 1.0000 Uiso R . . . . . H502 H 0.4912 0.5639 0.9602 0.1207 1.0000 Uiso R . . . . . H503 H 0.4805 0.5994 0.9041 0.1207 1.0000 Uiso R . . . . . H521 H 0.6336 0.5916 1.0128 0.1258 1.0000 Uiso R . . . . . H531 H 0.8202 0.5936 1.0183 0.1680 1.0000 Uiso R . . . . . H541 H 0.9093 0.6005 0.9413 0.1471 1.0000 Uiso R . . . . . H551 H 0.8126 0.5948 0.8614 0.1244 1.0000 Uiso R . . . . . H561 H 0.6325 0.5718 0.8552 0.1797 1.0000 Uiso R . . . . . H571 H 0.0868 0.9292 0.5250 0.2820 1.0000 Uiso R . . . . . H572 H 0.0796 0.9170 0.5866 0.2820 1.0000 Uiso R . . . . . H573 H 0.0330 0.8583 0.5458 0.2820 1.0000 Uiso R . . . . . H591 H 0.2770 0.9265 0.5947 0.0913 1.0000 Uiso R . . . . . H601 H 0.4240 0.8559 0.5929 0.1282 1.0000 Uiso R . . . . . H611 H 0.4223 0.7441 0.5624 0.1356 1.0000 Uiso R . . . . . H621 H 0.2652 0.6944 0.5307 0.0946 1.0000 Uiso R . . . . . H631 H 0.1172 0.7585 0.5255 0.0945 1.0000 Uiso 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 Ta1 0.01391(4) 0.01364(4) 0.01655(4) -0.00033(3) 0.00085(3) 0.00061(3) I1 0.02234(8) 0.02563(8) 0.03594(9) -0.00045(7) -0.01027(7) -0.00020(6) Co1 0.01626(14) 0.01421(12) 0.01499(13) -0.00038(11) 0.00067(11) 0.00008(10) P1 0.0179(3) 0.0134(2) 0.0158(2) -0.0006(2) 0.0007(2) -0.0009(2) P2 0.0149(3) 0.0137(2) 0.0182(3) -0.0007(2) 0.0024(2) 0.00012(19) P3 0.0204(3) 0.0181(3) 0.0153(3) 0.0016(2) 0.0031(2) 0.0025(2) N1 0.0186(9) 0.0143(8) 0.0179(9) 0.0006(7) 0.0000(7) -0.0002(7) N2 0.0164(9) 0.0161(8) 0.0212(9) -0.0043(7) -0.0002(7) -0.0003(7) N3 0.0171(9) 0.0187(9) 0.0233(10) 0.0024(7) 0.0032(8) 0.0014(7) N4 0.0154(9) 0.0200(9) 0.0221(9) -0.0009(8) 0.0004(7) 0.0013(7) C1 0.0194(11) 0.0181(10) 0.0236(11) -0.0062(9) 0.0014(9) -0.0011(8) C2 0.0260(12) 0.0289(12) 0.0217(12) -0.0064(10) 0.0031(10) -0.0042(10) C3 0.0311(14) 0.0402(15) 0.0279(14) -0.0160(12) 0.0043(11) -0.0059(12) C4 0.0232(13) 0.0287(13) 0.0498(18) -0.0237(13) 0.0050(12) -0.0031(10) C5 0.0255(13) 0.0172(11) 0.0498(17) -0.0072(11) 0.0037(12) -0.0009(9) C6 0.0270(13) 0.0183(10) 0.0300(13) -0.0040(9) 0.0016(10) -0.0018(9) C7 0.0214(11) 0.0147(9) 0.0184(10) -0.0003(8) 0.0030(8) 0.0002(8) C8 0.0226(11) 0.0243(11) 0.0199(11) -0.0010(9) 0.0017(9) 0.0028(9) C9 0.0328(14) 0.0367(14) 0.0185(11) 0.0005(10) 0.0029(10) 0.0102(11) C10 0.0327(14) 0.0283(12) 0.0270(13) 0.0027(10) 0.0130(11) 0.0054(10) C11 0.0272(13) 0.0194(11) 0.0389(15) -0.0026(10) 0.0110(11) -0.0030(9) C12 0.0240(12) 0.0212(11) 0.0251(12) -0.0048(9) 0.0033(10) -0.0046(9) C13 0.0240(12) 0.0162(10) 0.0282(12) 0.0059(9) -0.0032(10) 0.0020(9) C14 0.0419(17) 0.0291(13) 0.0336(15) -0.0076(11) -0.0044(12) 0.0175(12) C15 0.0285(13) 0.0325(13) 0.0216(12) 0.0058(10) -0.0018(10) 0.0063(10) C16 0.0167(10) 0.0172(9) 0.0178(10) 0.0008(8) 0.0024(8) 0.0018(8) C17 0.0189(11) 0.0172(10) 0.0262(12) 0.0030(9) 0.0018(9) 0.0001(8) C18 0.0201(12) 0.0245(11) 0.0365(14) 0.0067(10) 0.0078(10) -0.0001(9) C19 0.0248(13) 0.0351(14) 0.0288(13) 0.0055(11) 0.0115(11) 0.0049(10) C20 0.0288(13) 0.0282(12) 0.0260(13) -0.0041(10) 0.0067(10) 0.0051(10) C21 0.0231(12) 0.0216(11) 0.0235(12) -0.0044(9) 0.0036(9) -0.0016(9) C22 0.0214(11) 0.0158(9) 0.0204(11) -0.0015(8) 0.0041(9) 0.0011(8) C23 0.0249(12) 0.0225(11) 0.0222(12) 0.0016(9) 0.0025(9) 0.0025(9) C24 0.0405(16) 0.0236(12) 0.0265(13) 0.0027(10) 0.0009(11) 0.0096(11) C25 0.056(2) 0.0212(12) 0.0346(15) 0.0097(11) 0.0120(14) 0.0007(12) C26 0.0402(16) 0.0267(13) 0.0422(17) 0.0049(12) 0.0185(13) -0.0067(11) C27 0.0252(13) 0.0226(11) 0.0326(14) 0.0015(10) 0.0090(10) -0.0006(9) C28 0.0246(12) 0.0239(11) 0.0284(13) -0.0119(10) -0.0028(10) 0.0002(9) C29 0.0270(14) 0.0269(13) 0.0492(18) -0.0113(12) -0.0071(13) -0.0052(10) C30 0.0423(17) 0.0490(18) 0.0236(13) -0.0095(12) -0.0020(12) -0.0049(14) C31 0.0294(13) 0.0241(11) 0.0218(12) -0.0028(9) 0.0085(10) 0.0003(10) C32 0.0369(15) 0.0272(13) 0.0320(14) -0.0051(11) 0.0069(12) 0.0057(11) C33 0.0479(19) 0.0351(16) 0.050(2) -0.0129(14) 0.0118(16) 0.0118(14) C34 0.060(2) 0.0468(19) 0.046(2) -0.0260(16) 0.0158(17) 0.0047(17) C35 0.064(2) 0.055(2) 0.0305(16) -0.0176(15) 0.0009(16) 0.0019(18) C36 0.0448(18) 0.0387(15) 0.0254(14) -0.0072(12) 0.0013(12) 0.0048(13) C37 0.0290(13) 0.0230(11) 0.0194(11) 0.0025(9) 0.0029(9) 0.0012(9) C38 0.0362(16) 0.0427(16) 0.0322(15) 0.0153(13) 0.0092(12) 0.0074(13) C39 0.052(2) 0.0478(18) 0.0328(16) 0.0209(14) 0.0104(14) 0.0015(15) C40 0.065(2) 0.0332(15) 0.0313(15) 0.0144(12) 0.0062(15) 0.0117(15) C41 0.059(2) 0.0308(14) 0.0316(15) 0.0091(12) 0.0079(14) 0.0190(14) C42 0.0434(16) 0.0237(12) 0.0231(12) 0.0040(10) 0.0074(11) 0.0096(11) C43 0.0225(12) 0.0305(13) 0.0274(13) 0.0082(10) 0.0088(10) 0.0017(10) C44 0.0255(14) 0.0314(14) 0.060(2) 0.0128(14) 0.0101(14) -0.0045(11) C45 0.0246(13) 0.0404(15) 0.0362(15) 0.0046(12) 0.0097(11) 0.0080(11) C46 0.0140(10) 0.0279(12) 0.0302(13) -0.0030(10) -0.0022(9) 0.0008(9) C47 0.0213(13) 0.0340(14) 0.059(2) -0.0014(14) -0.0049(13) -0.0045(11) C48 0.0210(13) 0.0356(14) 0.0431(17) -0.0031(12) -0.0026(12) 0.0079(11) C49 0.0277(14) 0.0405(15) 0.0317(14) -0.0075(12) -0.0123(11) 0.0064(12) C50 0.181(5) 0.049(2) 0.089(3) 0.000(2) -0.046(4) 0.013(3) C51 0.198(5) 0.048(2) 0.078(3) 0.006(2) -0.027(4) 0.017(3) C52 0.162(5) 0.098(4) 0.058(3) 0.013(3) -0.041(3) -0.018(4) C53 0.196(6) 0.123(4) 0.049(3) 0.002(3) -0.008(4) -0.051(5) C54 0.200(6) 0.089(4) 0.073(3) 0.006(3) 0.019(4) -0.050(4) C55 0.201(6) 0.054(3) 0.057(3) 0.012(2) 0.016(4) -0.028(3) C56 0.233(6) 0.045(2) 0.056(3) 0.003(2) -0.047(4) -0.002(4) C57 0.142(5) 0.119(4) 0.108(4) 0.015(3) 0.051(4) 0.007(4) C58 0.114(4) 0.075(3) 0.083(3) 0.021(3) 0.036(3) 0.011(3) C59 0.115(4) 0.0370(19) 0.081(3) -0.016(2) 0.023(3) -0.013(2) C60 0.148(5) 0.087(4) 0.068(3) 0.004(3) 0.017(3) 0.008(4) C61 0.148(5) 0.091(4) 0.072(3) 0.029(3) 0.027(4) 0.035(4) C62 0.133(4) 0.078(3) 0.058(3) 0.022(2) 0.030(3) 0.003(3) C63 0.132(5) 0.070(3) 0.043(2) 0.007(2) 0.021(3) -0.032(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.045826(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ta1 . Co1 . 3.0388(3) yes Ta1 . P1 . 2.9774(6) yes Ta1 . P2 . 2.9820(6) yes Ta1 . P3 . 2.9929(6) yes Ta1 . N1 . 2.0406(18) yes Ta1 . N2 . 2.0436(19) yes Ta1 . N3 . 2.045(2) yes Ta1 . N4 . 1.788(2) yes I1 . Co1 . 2.5315(4) yes Co1 . P1 . 2.2445(6) yes Co1 . P2 . 2.2505(6) yes Co1 . P3 . 2.2480(7) yes P1 . N1 . 1.684(2) yes P1 . C1 . 1.827(2) yes P1 . C7 . 1.828(2) yes P2 . N2 . 1.686(2) yes P2 . C16 . 1.835(2) yes P2 . C22 . 1.827(2) yes P3 . N3 . 1.688(2) yes P3 . C31 . 1.832(3) yes P3 . C37 . 1.845(3) yes N1 . C13 . 1.485(3) yes N2 . C28 . 1.486(3) yes N3 . C43 . 1.492(3) yes N4 . C46 . 1.456(3) yes C1 . C2 . 1.397(4) yes C1 . C6 . 1.406(3) yes C2 . C3 . 1.397(4) yes C2 . H21 . 0.924 no C3 . C4 . 1.382(4) yes C3 . H31 . 0.942 no C4 . C5 . 1.383(5) yes C4 . H41 . 0.947 no C5 . C6 . 1.389(3) yes C5 . H51 . 0.930 no C6 . H61 . 0.926 no C7 . C8 . 1.392(3) yes C7 . C12 . 1.395(3) yes C8 . C9 . 1.395(4) yes C8 . H81 . 0.935 no C9 . C10 . 1.383(4) yes C9 . H91 . 0.946 no C10 . C11 . 1.391(4) yes C10 . H101 . 0.930 no C11 . C12 . 1.385(4) yes C11 . H111 . 0.928 no C12 . H121 . 0.916 no C13 . C14 . 1.526(4) yes C13 . C15 . 1.516(4) yes C13 . H131 . 0.970 no C14 . H141 . 0.961 no C14 . H142 . 0.962 no C14 . H143 . 0.978 no C15 . H151 . 0.948 no C15 . H152 . 0.961 no C15 . H153 . 0.950 no C16 . C17 . 1.390(3) yes C16 . C21 . 1.404(3) yes C17 . C18 . 1.387(3) yes C17 . H171 . 0.928 no C18 . C19 . 1.380(4) yes C18 . H181 . 0.930 no C19 . C20 . 1.386(4) yes C19 . H191 . 0.932 no C20 . C21 . 1.392(4) yes C20 . H201 . 0.947 no C21 . H211 . 0.935 no C22 . C23 . 1.392(3) yes C22 . C27 . 1.399(3) yes C23 . C24 . 1.390(3) yes C23 . H231 . 0.938 no C24 . C25 . 1.385(4) yes C24 . H241 . 0.948 no C25 . C26 . 1.375(5) yes C25 . H251 . 0.917 no C26 . C27 . 1.393(4) yes C26 . H261 . 0.921 no C27 . H271 . 0.933 no C28 . C29 . 1.517(4) yes C28 . C30 . 1.522(4) yes C28 . H281 . 0.980 no C29 . H291 . 0.970 no C29 . H292 . 0.959 no C29 . H293 . 0.967 no C30 . H301 . 0.959 no C30 . H302 . 0.963 no C30 . H303 . 0.976 no C31 . C32 . 1.399(4) yes C31 . C36 . 1.390(4) yes C32 . C33 . 1.389(4) yes C32 . H321 . 0.947 no C33 . C34 . 1.374(5) yes C33 . H331 . 0.945 no C34 . C35 . 1.379(6) yes C34 . H341 . 0.919 no C35 . C36 . 1.399(4) yes C35 . H351 . 0.949 no C36 . H361 . 0.949 no C37 . C38 . 1.395(4) yes C37 . C42 . 1.389(4) yes C38 . C39 . 1.386(4) yes C38 . H381 . 0.938 no C39 . C40 . 1.380(5) yes C39 . H391 . 0.939 no C40 . C41 . 1.378(5) yes C40 . H401 . 0.946 no C41 . C42 . 1.396(4) yes C41 . H411 . 0.936 no C42 . H421 . 0.940 no C43 . C44 . 1.513(4) yes C43 . C45 . 1.520(4) yes C43 . H431 . 0.963 no C44 . H441 . 0.958 no C44 . H442 . 0.951 no C44 . H443 . 0.963 no C45 . H451 . 0.960 no C45 . H452 . 0.972 no C45 . H453 . 0.967 no C46 . C47 . 1.540(4) yes C46 . C48 . 1.543(4) yes C46 . C49 . 1.538(4) yes C47 . H471 . 0.971 no C47 . H472 . 0.972 no C47 . H473 . 0.962 no C48 . H481 . 0.962 no C48 . H482 . 0.966 no C48 . H483 . 0.967 no C49 . H491 . 0.950 no C49 . H492 . 0.959 no C49 . H493 . 0.950 no C50 . C51 . 1.503(11) yes C50 . H501 . 0.950 no C50 . H502 . 0.950 no C50 . H503 . 0.950 no C51 . C52 . 1.411(7) yes C51 . C56 . 1.312(7) yes C52 . C53 . 1.378(8) yes C52 . H521 . 0.995 no C53 . C54 . 1.425(7) yes C53 . H531 . 0.944 no C54 . C55 . 1.330(7) yes C54 . H541 . 0.951 no C55 . C56 . 1.438(7) yes C55 . H551 . 0.931 no C56 . H561 . 0.930 no C57 . C58 . 1.442(10) yes C57 . H571 . 0.962 no C57 . H572 . 0.956 no C57 . H573 . 0.967 no C58 . C59 . 1.398(7) yes C58 . C63 . 1.399(6) yes C59 . C60 . 1.379(7) yes C59 . H591 . 0.916 no C60 . C61 . 1.316(6) yes C60 . H601 . 0.943 no C61 . C62 . 1.374(7) yes C61 . H611 . 0.931 no C62 . C63 . 1.346(7) yes C62 . H621 . 0.953 no C63 . H631 . 0.912 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Ta1 . P2 . 74.330(16) yes P1 . Ta1 . P3 . 73.823(16) yes P2 . Ta1 . P3 . 72.855(16) yes Co1 . Ta1 . N1 . 76.53(5) yes P2 . Ta1 . N1 . 103.31(6) yes P3 . Ta1 . N1 . 97.08(6) yes Co1 . Ta1 . N2 . 76.35(6) yes P1 . Ta1 . N2 . 96.35(6) yes P3 . Ta1 . N2 . 102.32(6) yes N1 . Ta1 . N2 . 114.20(8) yes Co1 . Ta1 . N3 . 76.38(6) yes P1 . Ta1 . N3 . 102.16(6) yes P2 . Ta1 . N3 . 96.06(6) yes N1 . Ta1 . N3 . 114.40(8) yes Co1 . Ta1 . N4 . 179.65(6) yes P1 . Ta1 . N4 . 136.24(6) yes P2 . Ta1 . N4 . 135.80(6) yes P3 . Ta1 . N4 . 136.53(7) yes N1 . Ta1 . N4 . 103.53(8) yes N2 . Ta1 . N3 . 115.39(8) yes N2 . Ta1 . N4 . 103.32(8) yes N3 . Ta1 . N4 . 103.89(9) yes Ta1 . Co1 . I1 . 175.141(13) yes Ta1 . Co1 . P1 . 66.648(17) yes I1 . Co1 . P1 . 109.386(19) yes Ta1 . Co1 . P2 . 66.715(17) yes I1 . Co1 . P2 . 112.820(19) yes P1 . Co1 . P2 . 106.44(2) yes Ta1 . Co1 . P3 . 67.036(18) yes I1 . Co1 . P3 . 117.40(2) yes P1 . Co1 . P3 . 105.91(2) yes P2 . Co1 . P3 . 104.13(2) yes Co1 . P1 . Ta1 . 69.557(17) yes Co1 . P1 . N1 . 110.41(7) yes Co1 . P1 . C1 . 115.89(8) yes Ta1 . P1 . C1 . 135.88(8) yes N1 . P1 . C1 . 110.15(10) yes Co1 . P1 . C7 . 113.23(7) yes Ta1 . P1 . C7 . 117.92(8) yes N1 . P1 . C7 . 105.93(10) yes C1 . P1 . C7 . 100.44(11) yes Co1 . P2 . Ta1 . 69.400(16) yes Co1 . P2 . N2 . 109.82(7) yes Co1 . P2 . C16 . 116.22(8) yes Ta1 . P2 . C16 . 135.96(7) yes N2 . P2 . C16 . 108.56(10) yes Co1 . P2 . C22 . 115.13(8) yes Ta1 . P2 . C22 . 116.86(8) yes N2 . P2 . C22 . 105.87(10) yes C16 . P2 . C22 . 100.40(10) yes Co1 . P3 . Ta1 . 69.208(18) yes Co1 . P3 . N3 . 109.91(8) yes Co1 . P3 . C31 . 116.83(9) yes Ta1 . P3 . C31 . 119.46(9) yes N3 . P3 . C31 . 104.21(11) yes Co1 . P3 . C37 . 113.06(9) yes Ta1 . P3 . C37 . 133.80(8) yes N3 . P3 . C37 . 111.29(11) yes C31 . P3 . C37 . 100.98(12) yes P1 . N1 . Ta1 . 105.75(9) yes P1 . N1 . C13 . 121.13(15) yes Ta1 . N1 . C13 . 133.07(15) yes P2 . N2 . Ta1 . 105.78(10) yes P2 . N2 . C28 . 119.77(16) yes Ta1 . N2 . C28 . 134.44(16) yes P3 . N3 . Ta1 . 106.21(10) yes P3 . N3 . C43 . 119.82(17) yes Ta1 . N3 . C43 . 133.94(17) yes Ta1 . N4 . C46 . 178.04(17) yes P1 . C1 . C2 . 119.55(19) yes P1 . C1 . C6 . 122.47(19) yes C2 . C1 . C6 . 118.0(2) yes C1 . C2 . C3 . 120.9(3) yes C1 . C2 . H21 . 119.0 no C3 . C2 . H21 . 120.2 no C2 . C3 . C4 . 119.9(3) yes C2 . C3 . H31 . 119.6 no C4 . C3 . H31 . 120.5 no C3 . C4 . C5 . 120.3(2) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 119.3 no C4 . C5 . C6 . 119.9(3) yes C4 . C5 . H51 . 119.5 no C6 . C5 . H51 . 120.6 no C1 . C6 . C5 . 121.0(3) yes C1 . C6 . H61 . 118.9 no C5 . C6 . H61 . 120.1 no P1 . C7 . C8 . 121.03(18) yes P1 . C7 . C12 . 119.67(18) yes C8 . C7 . C12 . 118.8(2) yes C7 . C8 . C9 . 120.3(2) yes C7 . C8 . H81 . 119.2 no C9 . C8 . H81 . 120.4 no C8 . C9 . C10 . 120.5(3) yes C8 . C9 . H91 . 120.1 no C10 . C9 . H91 . 119.4 no C9 . C10 . C11 . 119.3(2) yes C9 . C10 . H101 . 119.7 no C11 . C10 . H101 . 120.9 no C10 . C11 . C12 . 120.3(3) yes C10 . C11 . H111 . 120.4 no C12 . C11 . H111 . 119.3 no C7 . C12 . C11 . 120.7(2) yes C7 . C12 . H121 . 120.5 no C11 . C12 . H121 . 118.9 no N1 . C13 . C14 . 109.1(2) yes N1 . C13 . C15 . 112.3(2) yes C14 . C13 . C15 . 111.4(2) yes N1 . C13 . H131 . 106.6 no C14 . C13 . H131 . 108.5 no C15 . C13 . H131 . 108.8 no C13 . C14 . H141 . 110.2 no C13 . C14 . H142 . 110.8 no H141 . C14 . H142 . 109.9 no C13 . C14 . H143 . 109.6 no H141 . C14 . H143 . 108.5 no H142 . C14 . H143 . 107.8 no C13 . C15 . H151 . 112.1 no C13 . C15 . H152 . 110.7 no H151 . C15 . H152 . 106.5 no C13 . C15 . H153 . 111.1 no H151 . C15 . H153 . 109.0 no H152 . C15 . H153 . 107.1 no P2 . C16 . C17 . 118.52(17) yes P2 . C16 . C21 . 123.16(18) yes C17 . C16 . C21 . 118.3(2) yes C16 . C17 . C18 . 120.9(2) yes C16 . C17 . H171 . 119.9 no C18 . C17 . H171 . 119.2 no C17 . C18 . C19 . 120.4(2) yes C17 . C18 . H181 . 119.3 no C19 . C18 . H181 . 120.3 no C18 . C19 . C20 . 119.8(2) yes C18 . C19 . H191 . 119.5 no C20 . C19 . H191 . 120.7 no C19 . C20 . C21 . 120.0(2) yes C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 119.7 no C16 . C21 . C20 . 120.5(2) yes C16 . C21 . H211 . 119.4 no C20 . C21 . H211 . 120.1 no P2 . C22 . C23 . 120.57(18) yes P2 . C22 . C27 . 120.44(18) yes C23 . C22 . C27 . 118.9(2) yes C22 . C23 . C24 . 120.5(2) yes C22 . C23 . H231 . 120.0 no C24 . C23 . H231 . 119.5 no C23 . C24 . C25 . 120.4(3) yes C23 . C24 . H241 . 119.9 no C25 . C24 . H241 . 119.7 no C24 . C25 . C26 . 119.5(2) yes C24 . C25 . H251 . 120.2 no C26 . C25 . H251 . 120.2 no C25 . C26 . C27 . 120.9(3) yes C25 . C26 . H261 . 119.5 no C27 . C26 . H261 . 119.6 no C22 . C27 . C26 . 119.9(3) yes C22 . C27 . H271 . 119.4 no C26 . C27 . H271 . 120.7 no N2 . C28 . C29 . 112.4(2) yes N2 . C28 . C30 . 109.6(2) yes C29 . C28 . C30 . 113.1(2) yes N2 . C28 . H281 . 106.1 no C29 . C28 . H281 . 105.8 no C30 . C28 . H281 . 109.5 no C28 . C29 . H291 . 111.5 no C28 . C29 . H292 . 111.0 no H291 . C29 . H292 . 108.1 no C28 . C29 . H293 . 110.2 no H291 . C29 . H293 . 109.1 no H292 . C29 . H293 . 106.9 no C28 . C30 . H301 . 110.5 no C28 . C30 . H302 . 111.9 no H301 . C30 . H302 . 109.0 no C28 . C30 . H303 . 109.3 no H301 . C30 . H303 . 108.7 no H302 . C30 . H303 . 107.3 no P3 . C31 . C32 . 119.0(2) yes P3 . C31 . C36 . 121.7(2) yes C32 . C31 . C36 . 119.0(2) yes C31 . C32 . C33 . 120.5(3) yes C31 . C32 . H321 . 119.8 no C33 . C32 . H321 . 119.7 no C32 . C33 . C34 . 120.0(3) yes C32 . C33 . H331 . 119.8 no C34 . C33 . H331 . 120.2 no C33 . C34 . C35 . 120.4(3) yes C33 . C34 . H341 . 119.8 no C35 . C34 . H341 . 119.8 no C34 . C35 . C36 . 120.2(3) yes C34 . C35 . H351 . 120.1 no C36 . C35 . H351 . 119.7 no C35 . C36 . C31 . 119.9(3) yes C35 . C36 . H361 . 120.6 no C31 . C36 . H361 . 119.4 no P3 . C37 . C38 . 124.5(2) yes P3 . C37 . C42 . 117.31(19) yes C38 . C37 . C42 . 118.1(2) yes C37 . C38 . C39 . 120.9(3) yes C37 . C38 . H381 . 119.2 no C39 . C38 . H381 . 119.9 no C38 . C39 . C40 . 120.4(3) yes C38 . C39 . H391 . 118.8 no C40 . C39 . H391 . 120.8 no C39 . C40 . C41 . 119.6(3) yes C39 . C40 . H401 . 120.7 no C41 . C40 . H401 . 119.6 no C40 . C41 . C42 . 120.1(3) yes C40 . C41 . H411 . 120.4 no C42 . C41 . H411 . 119.6 no C41 . C42 . C37 . 120.9(3) yes C41 . C42 . H421 . 119.7 no C37 . C42 . H421 . 119.4 no N3 . C43 . C44 . 109.9(2) yes N3 . C43 . C45 . 112.6(2) yes C44 . C43 . C45 . 112.1(2) yes N3 . C43 . H431 . 106.5 no C44 . C43 . H431 . 108.5 no C45 . C43 . H431 . 106.9 no C43 . C44 . H441 . 109.7 no C43 . C44 . H442 . 110.2 no H441 . C44 . H442 . 108.7 no C43 . C44 . H443 . 109.2 no H441 . C44 . H443 . 108.5 no H442 . C44 . H443 . 110.6 no C43 . C45 . H451 . 109.2 no C43 . C45 . H452 . 109.8 no H451 . C45 . H452 . 110.0 no C43 . C45 . H453 . 109.1 no H451 . C45 . H453 . 108.0 no H452 . C45 . H453 . 110.8 no N4 . C46 . C47 . 110.0(2) yes N4 . C46 . C48 . 111.0(2) yes C47 . C46 . C48 . 108.7(2) yes N4 . C46 . C49 . 110.5(2) yes C47 . C46 . C49 . 108.8(2) yes C48 . C46 . C49 . 107.8(2) yes C46 . C47 . H471 . 108.5 no C46 . C47 . H472 . 110.3 no H471 . C47 . H472 . 109.7 no C46 . C47 . H473 . 107.6 no H471 . C47 . H473 . 109.7 no H472 . C47 . H473 . 111.0 no C46 . C48 . H481 . 111.0 no C46 . C48 . H482 . 110.5 no H481 . C48 . H482 . 108.2 no C46 . C48 . H483 . 110.2 no H481 . C48 . H483 . 108.2 no H482 . C48 . H483 . 108.7 no C46 . C49 . H491 . 109.9 no C46 . C49 . H492 . 108.4 no H491 . C49 . H492 . 108.5 no C46 . C49 . H493 . 111.6 no H491 . C49 . H493 . 108.7 no H492 . C49 . H493 . 109.6 no C51 . C50 . H501 . 110.5 no C51 . C50 . H502 . 107.1 no H501 . C50 . H502 . 109.5 no C51 . C50 . H503 . 110.7 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no C50 . C51 . C52 . 119.5(7) yes C50 . C51 . C56 . 115.5(6) yes C52 . C51 . C56 . 124.9(8) yes C51 . C52 . C53 . 114.8(7) yes C51 . C52 . H521 . 117.1 no C53 . C52 . H521 . 128.1 no C52 . C53 . C54 . 123.5(7) yes C52 . C53 . H531 . 118.4 no C54 . C53 . H531 . 118.0 no C53 . C54 . C55 . 115.6(7) yes C53 . C54 . H541 . 121.5 no C55 . C54 . H541 . 122.9 no C54 . C55 . C56 . 124.0(6) yes C54 . C55 . H551 . 118.4 no C56 . C55 . H551 . 117.6 no C55 . C56 . C51 . 116.3(6) yes C55 . C56 . H561 . 124.3 no C51 . C56 . H561 . 119.4 no C58 . C57 . H571 . 111.1 no C58 . C57 . H572 . 109.2 no H571 . C57 . H572 . 111.2 no C58 . C57 . H573 . 104.8 no H571 . C57 . H573 . 110.6 no H572 . C57 . H573 . 109.6 no C57 . C58 . C59 . 121.5(6) yes C57 . C58 . C63 . 119.2(7) yes C59 . C58 . C63 . 119.3(5) yes C58 . C59 . C60 . 118.1(5) yes C58 . C59 . H591 . 122.5 no C60 . C59 . H591 . 119.4 no C59 . C60 . C61 . 125.2(7) yes C59 . C60 . H601 . 121.9 no C61 . C60 . H601 . 113.0 no C60 . C61 . C62 . 113.7(7) yes C60 . C61 . H611 . 122.2 no C62 . C61 . H611 . 124.1 no C61 . C62 . C63 . 127.9(6) yes C61 . C62 . H621 . 117.0 no C63 . C62 . H621 . 115.1 no C58 . C63 . C62 . 115.6(6) yes C58 . C63 . H631 . 120.4 no C62 . C63 . H631 . 124.0 no _iucr_refine_instruction_details_constraints ; # # Punched on 20/11/10 at 15:49:39 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) H ( 473,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) H ( 483,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) H ( 493,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) H ( 503,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) H ( 573,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 60,X'S) H ( 601,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 63,X'S) H ( 631,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 20/11/10 at 15:49:39 # #LIST 16 NO DISTANCE 1.390000 , 0.010000 = C(51) TO C(56) DISTANCE 1.390000 , 0.010000 = C(51) TO C(52) DISTANCE 1.390000 , 0.010000 = C(52) TO C(53) DISTANCE 1.390000 , 0.010000 = C(53) TO C(54) DISTANCE 1.390000 , 0.010000 = C(54) TO C(55) DISTANCE 1.390000 , 0.010000 = C(55) TO C(56) U(IJ)'S 0.0, 0.010000 = C(51) TO C(56) U(IJ)'S 0.0, 0.010000 = C(51) TO C(52) U(IJ)'S 0.0, 0.010000 = C(52) TO C(53) U(IJ)'S 0.0, 0.010000 = C(53) TO C(54) U(IJ)'S 0.0, 0.010000 = C(54) TO C(55) U(IJ)'S 0.0, 0.010000 = C(55) TO C(56) U(IJ)'S 0.0, 0.005000 = C(50) TO C(51) DISTANCE 1.390000 , 0.010000 = C(58) TO C(63) DISTANCE 1.390000 , 0.010000 = C(58) TO C(59) DISTANCE 1.390000 , 0.010000 = C(59) TO C(60) DISTANCE 1.390000 , 0.010000 = C(60) TO C(61) DISTANCE 1.390000 , 0.010000 = C(61) TO C(62) DISTANCE 1.390000 , 0.010000 = C(62) TO C(63) U(IJ)'S 0.0, 0.010000 = C(57) TO C(58) U(IJ)'S 0.0, 0.010000 = C(58) TO C(59) U(IJ)'S 0.0, 0.010000 = C(59) TO C(60) U(IJ)'S 0.0, 0.010000 = C(60) TO C(61) U(IJ)'S 0.0, 0.010000 = C(61) TO C(62) U(IJ)'S 0.0, 0.010000 = C(62) TO C(62) U(IJ)'S 0.0, 0.005000 = C(57) TO C(62) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END data_3Nb _database_code_depnum_ccdc_archive 'CCDC 862676' #TrackingRef '- combined_22Feb.cif' _audit_creation_date 11-07-14 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'DE1_24_0m in P1' _vrf_PLAT220_3Nb ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.8 Ratio RESPONSE: The warning is appropriate, but can be ignored owing to remaining unresolved disorder in the weakly coordinated THF molecules as well as the phenyl ring atoms c(16) - C(21). The THF molecules should not be defined as 'non-solvent' molecules on this case. ; _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.8515(4) _cell_length_b 12.9728(5) _cell_length_c 13.2306(4) _cell_angle_alpha 91.900(2) _cell_angle_beta 117.275(2) _cell_angle_gamma 112.938(2) _cell_volume 1744.07(12) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C34.50 H50 Co0.50 N3 Na0.50 Nb0.50 O2.50 P1.50 # Dc = 1.30 Fooo = 720.00 Mu = 5.29 M = 1361.34 # Found Formula = C34.50 H50 Co0.50 N3 Na0.50 Nb0.50 O2.50 P1.50 # Dc = 1.30 FOOO = 720.00 Mu = 5.29 M = 1361.34 _chemical_formula_sum 'C69 H100 Co1 N6 Na1 Nb1 O5 P3' _chemical_formula_moiety 'C69 H100 Co1 N6 Na1 Nb1 O5 P3' _chemical_compound_source ? _chemical_formula_weight 1361.34 _cell_measurement_reflns_used 8993 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'plate fragment' _exptl_crystal_colour red _exptl_crystal_size_min 0.095 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_max 0.396 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.529 # Sheldrick geometric approximatio 0.95 0.95 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 35556 _reflns_number_total 13788 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections without Friedels Law is 13788 # Number of reflections with Friedels Law is 10163 # Theoretical number of reflections is about 10243 _diffrn_reflns_theta_min 1.884 _diffrn_reflns_theta_max 30.074 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.074 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min -17 _reflns_limit_k_max 18 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.64 _oxford_diffrn_Wilson_scale 1.22 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.64 _refine_diff_density_max 0.73 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 13788 _refine_ls_number_restraints 3 _refine_ls_number_parameters 764 _oxford_refine_ls_R_factor_ref 0.0416 _refine_ls_wR_factor_ref 0.0884 _refine_ls_goodness_of_fit_ref 0.9935 _refine_ls_shift/su_max 0.0155579 _refine_ls_shift/su_mean 0.0006315 # The values computed from all data _oxford_reflns_number_all 13788 _refine_ls_R_factor_all 0.0416 _refine_ls_wR_factor_all 0.0884 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12445 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_gt 0.0804 _refine_ls_abs_structure_Flack -0.015(11) _refine_ls_abs_structure_details 'Flack (1983), 3625 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.31P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Nb1 Nb 0.00270(7) -0.00230(6) -0.00079(6) 0.0175 1.0000 Uani . . . . . . Co1 Co 0.27359(7) 0.15969(6) 0.10703(6) 0.0147 1.0000 Uani . . . . . . P1 P 0.25534(9) -0.00204(8) 0.14522(8) 0.0163 1.0000 Uani . . . . . . P2 P 0.17603(10) 0.22921(8) 0.15958(8) 0.0181 1.0000 Uani . . . . . . P3 P 0.18390(9) 0.12895(8) -0.07976(8) 0.0158 1.0000 Uani . . . . . . Na1 Na 0.78460(15) 0.46563(13) 0.36442(15) 0.0388 1.0000 Uani . . . . . . O1 O 0.7428(3) 0.6307(3) 0.3816(3) 0.0537 1.0000 Uani . . . . . . O2 O 0.7526(3) 0.4689(3) 0.1706(3) 0.0552 1.0000 Uani . . . . . . O3 O 0.8195(3) 0.2961(2) 0.3710(3) 0.0455 1.0000 Uani . . . . . . O4 O 0.7939(3) 0.4570(3) 0.5469(3) 0.0574 1.0000 Uani . . . . . . O5 O 1.0099(3) 0.5870(3) 0.4413(3) 0.0548 1.0000 Uani . . . . . . N1 N 0.0957(2) -0.0906(2) 0.0999(2) 0.0195 1.0000 Uani . . . . . . N2 N 0.0134(3) 0.1377(2) 0.0886(2) 0.0238 1.0000 Uani . . . . . . N3 N 0.0263(2) 0.0240(2) -0.1430(2) 0.0202 1.0000 Uani . . . . . . N4 N 0.4407(3) 0.2640(3) 0.1902(3) 0.0217 1.0000 Uani . . . . . . N5 N 0.5446(3) 0.3315(3) 0.2478(3) 0.0325 1.0000 Uani . . . . . . N6 N -0.1692(3) -0.1058(3) -0.0691(3) 0.0247 1.0000 Uani . . . . . . C1 C 0.3510(3) -0.0071(3) 0.2996(3) 0.0205 1.0000 Uani . . . . . . C2 C 0.3928(3) 0.0855(3) 0.3881(3) 0.0260 1.0000 Uani . . . . . . C3 C 0.4622(4) 0.0882(4) 0.5065(3) 0.0334 1.0000 Uani . . . . . . C4 C 0.4933(4) -0.0010(4) 0.5374(3) 0.0382 1.0000 Uani . . . . . . C5 C 0.4531(4) -0.0946(3) 0.4509(3) 0.0330 1.0000 Uani . . . . . . C6 C 0.3821(3) -0.0978(3) 0.3333(3) 0.0247 1.0000 Uani . . . . . . C7 C 0.2956(3) -0.0910(2) 0.0710(3) 0.0186 1.0000 Uani . . . . . . C8 C 0.4219(3) -0.0809(3) 0.1177(3) 0.0215 1.0000 Uani . . . . . . C9 C 0.4525(3) -0.1397(3) 0.0541(3) 0.0274 1.0000 Uani . . . . . . C10 C 0.3565(4) -0.2104(3) -0.0586(3) 0.0307 1.0000 Uani . . . . . . C11 C 0.2313(3) -0.2192(3) -0.1077(3) 0.0296 1.0000 Uani . . . . . . C12 C 0.2018(3) -0.1597(3) -0.0435(3) 0.0240 1.0000 Uani . . . . . . C13 C 0.0556(3) -0.2006(3) 0.1327(3) 0.0300 1.0000 Uani . . . . . . C14 C 0.0095(4) -0.1888(4) 0.2186(4) 0.0479 1.0000 Uani . . . . . . C15 C -0.0435(3) -0.3031(3) 0.0282(4) 0.0427 1.0000 Uani . . . . . . C16 C 0.2229(4) 0.2589(3) 0.3157(3) 0.0284 1.0000 Uani . . . . . . C17 C 0.1616(4) 0.1705(5) 0.3576(4) 0.0459 1.0000 Uani . . . . . . C18 C 0.2039(7) 0.1887(7) 0.4765(5) 0.0782 1.0000 Uani . . . . . . C19 C 0.3083(8) 0.2932(8) 0.5557(5) 0.0892 1.0000 Uani . . . . . . C20 C 0.3673(7) 0.3772(6) 0.5152(4) 0.0757 1.0000 Uani . . . . . . C21 C 0.3247(5) 0.3614(4) 0.3960(3) 0.0478 1.0000 Uani . . . . . . C22 C 0.1985(3) 0.3756(3) 0.1400(3) 0.0217 1.0000 Uani . . . . . . C23 C 0.1477(4) 0.4394(3) 0.1730(3) 0.0315 1.0000 Uani . . . . . . C24 C 0.1680(4) 0.5483(3) 0.1544(4) 0.0384 1.0000 Uani . . . . . . C25 C 0.2426(4) 0.5983(3) 0.1041(3) 0.0330 1.0000 Uani . . . . . . C26 C 0.2981(4) 0.5387(3) 0.0740(3) 0.0309 1.0000 Uani . . . . . . C27 C 0.2768(3) 0.4293(3) 0.0931(3) 0.0251 1.0000 Uani . . . . . . C28 C -0.0850(3) 0.1654(3) 0.0950(3) 0.0335 1.0000 Uani . . . . . . C29 C -0.1716(4) 0.0707(4) 0.1268(4) 0.0422 1.0000 Uani . . . . . . C30 C -0.1654(4) 0.1885(4) -0.0207(4) 0.0409 1.0000 Uani . . . . . . C31 C 0.1596(3) 0.2422(3) -0.1537(3) 0.0211 1.0000 Uani . . . . . . C32 C 0.2449(4) 0.3126(3) -0.1883(3) 0.0315 1.0000 Uani . . . . . . C33 C 0.2323(5) 0.4072(3) -0.2305(4) 0.0462 1.0000 Uani . . . . . . C34 C 0.1355(5) 0.4330(4) -0.2386(4) 0.0456 1.0000 Uani . . . . . . C35 C 0.0504(4) 0.3646(3) -0.2050(4) 0.0406 1.0000 Uani . . . . . . C36 C 0.0614(3) 0.2698(3) -0.1635(3) 0.0298 1.0000 Uani . . . . . . C37 C 0.2670(3) 0.0884(3) -0.1460(3) 0.0196 1.0000 Uani . . . . . . C38 C 0.2232(3) 0.0579(3) -0.2652(3) 0.0282 1.0000 Uani . . . . . . C39 C 0.2953(4) 0.0297(3) -0.3037(3) 0.0343 1.0000 Uani . . . . . . C40 C 0.4139(4) 0.0338(3) -0.2243(3) 0.0318 1.0000 Uani . . . . . . C41 C 0.4598(3) 0.0660(3) -0.1052(3) 0.0274 1.0000 Uani . . . . . . C42 C 0.3883(3) 0.0936(3) -0.0671(3) 0.0209 1.0000 Uani . . . . . . C43 C -0.0607(3) -0.0206(3) -0.2715(3) 0.0261 1.0000 Uani . . . . . . C44 C -0.1905(3) -0.0170(3) -0.3148(3) 0.0352 1.0000 Uani . . . . . . C45 C -0.0824(4) -0.1444(3) -0.3092(3) 0.0382 1.0000 Uani . . . . . . C46 C -0.3085(3) -0.1901(3) -0.1228(4) 0.0334 1.0000 Uani . . . . . . C47 C -0.3967(3) -0.1304(4) -0.1711(4) 0.0394 1.0000 Uani . . . . . . C48 C -0.3466(4) -0.2831(3) -0.2245(4) 0.0416 1.0000 Uani . . . . . . C49 C -0.3329(4) -0.2472(4) -0.0318(4) 0.0430 1.0000 Uani . . . . . . C57 C 0.7494(5) 0.3802(4) 0.1025(4) 0.0525 1.0000 Uani . . . . . . C58 C 0.7126(4) 0.1814(3) 0.3267(4) 0.0440 1.0000 Uani . . . . . . C59 C 0.7586(5) 0.1087(5) 0.4011(5) 0.0739 1.0000 Uani . . . . . . C60 C 0.8984(5) 0.1791(5) 0.4828(5) 0.0676 1.0000 Uani . . . . . . C61 C 0.9360(4) 0.2873(5) 0.4406(5) 0.0608 1.0000 Uani . . . . . . C62 C 0.7039(6) 0.3576(5) 0.5591(5) 0.0720 1.0000 Uani . . . . . . C63 C 0.7156(6) 0.3896(5) 0.6742(5) 0.0667 1.0000 Uani . . . . . . C65 C 0.8547(6) 0.5500(5) 0.6440(5) 0.0812 1.0000 Uani . . . . . . C69 C 1.0799(5) 0.5680(4) 0.3902(4) 0.0541 1.0000 Uani . . . . . . C500 C 0.7734(13) 0.7279(11) 0.3371(11) 0.065(3) 0.5000 Uiso . . . 1 1 . C501 C 0.8289(10) 0.7442(9) 0.3734(9) 0.047(2) 0.5000 Uiso . . . 1 2 . C510 C 0.6570(14) 0.7535(12) 0.3010(13) 0.076(3) 0.5000 Uiso . . . 1 1 . C511 C 0.7170(12) 0.7786(10) 0.2946(10) 0.062(3) 0.5000 Uiso . . . 1 2 . C520 C 0.5917(12) 0.6987(11) 0.3654(11) 0.069(3) 0.5000 Uiso . . . 1 1 . C521 C 0.6271(8) 0.7441(7) 0.3420(7) 0.0348(16) 0.5000 Uiso . . . 1 2 . C530 C 0.6096(13) 0.5924(11) 0.3722(11) 0.066(3) 0.5000 Uiso . . . 1 1 . C531 C 0.6347(10) 0.6364(9) 0.3740(9) 0.044(2) 0.5000 Uiso . . . 1 2 . C540 C 0.6695(8) 0.5131(7) 0.1177(7) 0.0340(15) 0.5000 Uiso . . . 1 2 . C541 C 0.6210(11) 0.4667(10) 0.0614(10) 0.055(2) 0.5000 Uiso . . . 1 1 . C550 C 0.5775(9) 0.4262(8) 0.0023(8) 0.0417(18) 0.5000 Uiso . . . 1 2 . C551 C 0.6247(8) 0.4515(7) -0.0472(7) 0.0418(18) 0.5000 Uiso . . . 1 1 . C560 C 0.6638(9) 0.3876(8) -0.0138(7) 0.0390(19) 0.5000 Uiso . . . 1 2 . C561 C 0.6960(9) 0.3795(8) -0.0304(8) 0.043(2) 0.5000 Uiso . . . 1 1 . C640 C 0.7669(12) 0.5211(10) 0.6907(11) 0.064(3) 0.5000 Uiso . . . 1 1 . C641 C 0.8236(13) 0.5146(11) 0.7338(12) 0.073(3) 0.5000 Uiso . . . 1 2 . C660 C 1.1059(11) 0.6688(10) 0.5531(10) 0.056(3) 0.5000 Uiso . . . 1 1 . C661 C 1.0957(9) 0.7012(9) 0.5223(9) 0.047(2) 0.5000 Uiso . . . 1 2 . C670 C 1.2333(11) 0.6923(10) 0.5826(10) 0.063(3) 0.5000 Uiso . . . 1 1 . C671 C 1.2223(14) 0.7356(13) 0.5430(13) 0.088(4) 0.5000 Uiso . . . 1 2 . C680 C 1.2213(11) 0.6147(10) 0.5053(10) 0.056(3) 0.5000 Uiso . . . 1 1 . C681 C 1.2158(14) 0.6383(14) 0.4615(14) 0.087(4) 0.5000 Uiso . . . 1 2 . H21 H 0.3756 0.1473 0.3687 0.0306 1.0000 Uiso R . . . . . H31 H 0.4890 0.1520 0.5629 0.0403 1.0000 Uiso R . . . . . H41 H 0.5406 0.0006 0.6160 0.0457 1.0000 Uiso R . . . . . H51 H 0.4736 -0.1545 0.4726 0.0401 1.0000 Uiso R . . . . . H61 H 0.3543 -0.1617 0.2753 0.0300 1.0000 Uiso R . . . . . H81 H 0.4882 -0.0326 0.1946 0.0261 1.0000 Uiso R . . . . . H91 H 0.5408 -0.1298 0.0899 0.0332 1.0000 Uiso R . . . . . H101 H 0.3746 -0.2515 -0.1021 0.0374 1.0000 Uiso R . . . . . H111 H 0.1658 -0.2649 -0.1848 0.0356 1.0000 Uiso R . . . . . H121 H 0.1179 -0.1656 -0.0758 0.0294 1.0000 Uiso R . . . . . H131 H 0.1336 -0.2130 0.1743 0.0353 1.0000 Uiso R . . . . . H141 H -0.0625 -0.1701 0.1824 0.0715 1.0000 Uiso R . . . . . H142 H -0.0167 -0.2593 0.2396 0.0716 1.0000 Uiso R . . . . . H143 H 0.0778 -0.1278 0.2892 0.0716 1.0000 Uiso R . . . . . H151 H -0.0761 -0.3692 0.0539 0.0631 1.0000 Uiso R . . . . . H152 H -0.0031 -0.3169 -0.0127 0.0623 1.0000 Uiso R . . . . . H153 H -0.1132 -0.2864 -0.0234 0.0620 1.0000 Uiso R . . . . . H171 H 0.0919 0.0983 0.3050 0.0555 1.0000 Uiso R . . . . . H181 H 0.1622 0.1294 0.5038 0.0931 1.0000 Uiso R . . . . . H191 H 0.3378 0.3064 0.6361 0.1073 1.0000 Uiso R . . . . . H201 H 0.4369 0.4466 0.5680 0.0902 1.0000 Uiso R . . . . . H211 H 0.3656 0.4204 0.3704 0.0571 1.0000 Uiso R . . . . . H231 H 0.0993 0.4063 0.2111 0.0383 1.0000 Uiso R . . . . . H241 H 0.1316 0.5882 0.1755 0.0455 1.0000 Uiso R . . . . . H251 H 0.2554 0.6714 0.0918 0.0407 1.0000 Uiso R . . . . . H261 H 0.3500 0.5718 0.0413 0.0363 1.0000 Uiso R . . . . . H271 H 0.3148 0.3901 0.0731 0.0298 1.0000 Uiso R . . . . . H281 H -0.0379 0.2376 0.1578 0.0398 1.0000 Uiso R . . . . . H291 H -0.2435 0.0848 0.1199 0.0630 1.0000 Uiso R . . . . . H292 H -0.1221 0.0663 0.2059 0.0624 1.0000 Uiso R . . . . . H293 H -0.2098 -0.0024 0.0730 0.0626 1.0000 Uiso R . . . . . H301 H -0.2332 0.2026 -0.0202 0.0613 1.0000 Uiso R . . . . . H302 H -0.2059 0.1230 -0.0854 0.0619 1.0000 Uiso R . . . . . H303 H -0.1075 0.2564 -0.0324 0.0618 1.0000 Uiso R . . . . . H321 H 0.3114 0.2983 -0.1830 0.0382 1.0000 Uiso R . . . . . H331 H 0.2892 0.4529 -0.2541 0.0559 1.0000 Uiso R . . . . . H341 H 0.1295 0.4974 -0.2645 0.0551 1.0000 Uiso R . . . . . H351 H -0.0167 0.3804 -0.2112 0.0496 1.0000 Uiso R . . . . . H361 H 0.0038 0.2241 -0.1404 0.0356 1.0000 Uiso R . . . . . H381 H 0.1447 0.0577 -0.3195 0.0343 1.0000 Uiso R . . . . . H391 H 0.2638 0.0072 -0.3840 0.0409 1.0000 Uiso R . . . . . H401 H 0.4602 0.0128 -0.2517 0.0372 1.0000 Uiso R . . . . . H411 H 0.5386 0.0666 -0.0513 0.0326 1.0000 Uiso R . . . . . H421 H 0.4216 0.1149 0.0138 0.0248 1.0000 Uiso R . . . . . H431 H -0.0167 0.0302 -0.3096 0.0305 1.0000 Uiso R . . . . . H441 H -0.2337 -0.0598 -0.2761 0.0529 1.0000 Uiso R . . . . . H442 H -0.1712 0.0647 -0.2980 0.0529 1.0000 Uiso R . . . . . H443 H -0.2464 -0.0505 -0.3996 0.0529 1.0000 Uiso R . . . . . H451 H 0.0004 -0.1436 -0.2881 0.0562 1.0000 Uiso R . . . . . H452 H -0.1413 -0.1763 -0.3943 0.0564 1.0000 Uiso R . . . . . H453 H -0.1204 -0.1967 -0.2698 0.0568 1.0000 Uiso R . . . . . H471 H -0.4852 -0.1858 -0.2113 0.0587 1.0000 Uiso R . . . . . H472 H -0.3816 -0.0778 -0.1079 0.0584 1.0000 Uiso R . . . . . H473 H -0.3798 -0.0898 -0.2245 0.0584 1.0000 Uiso R . . . . . H481 H -0.2864 -0.3161 -0.1948 0.0616 1.0000 Uiso R . . . . . H482 H -0.3398 -0.2478 -0.2858 0.0618 1.0000 Uiso R . . . . . H483 H -0.4342 -0.3409 -0.2538 0.0617 1.0000 Uiso R . . . . . H491 H -0.2848 -0.2924 -0.0073 0.0636 1.0000 Uiso R . . . . . H492 H -0.2977 -0.1839 0.0354 0.0642 1.0000 Uiso R . . . . . H493 H -0.4243 -0.2934 -0.0642 0.0629 1.0000 Uiso R . . . . . H571 H 0.8385 0.3898 0.1370 0.0632 0.5000 Uiso R . . 1 1 . H572 H 0.6945 0.3071 0.1078 0.0633 0.5000 Uiso R . . 1 1 . H573 H 0.8365 0.3997 0.1156 0.0632 0.5000 Uiso R . . 1 2 . H574 H 0.7147 0.3064 0.1186 0.0631 0.5000 Uiso R . . 1 2 . H581 H 0.6360 0.1829 0.3255 0.0531 1.0000 Uiso R . . . . . H582 H 0.6845 0.1505 0.2454 0.0538 1.0000 Uiso R . . . . . H591 H 0.7136 0.0879 0.4443 0.0892 1.0000 Uiso R . . . . . H592 H 0.7439 0.0402 0.3536 0.0896 1.0000 Uiso R . . . . . H601 H 0.9457 0.1361 0.4838 0.0820 1.0000 Uiso R . . . . . H602 H 0.9113 0.1972 0.5590 0.0814 1.0000 Uiso R . . . . . H611 H 0.9947 0.3541 0.5050 0.0730 1.0000 Uiso R . . . . . H612 H 0.9764 0.2855 0.3946 0.0733 1.0000 Uiso R . . . . . H621 H 0.6145 0.3343 0.4946 0.0870 1.0000 Uiso R . . . . . H622 H 0.7271 0.2938 0.5566 0.0875 1.0000 Uiso R . . . . . H631 H 0.6296 0.3657 0.6660 0.0799 1.0000 Uiso R . . . . . H632 H 0.7610 0.3537 0.7297 0.0802 1.0000 Uiso R . . . . . H651 H 0.9468 0.5684 0.6924 0.0974 1.0000 Uiso R . . . . . H652 H 0.8504 0.6180 0.6198 0.0971 1.0000 Uiso R . . . . . H691 H 1.0825 0.6122 0.3324 0.0651 0.5000 Uiso R . . 1 1 . H692 H 1.0426 0.4863 0.3541 0.0651 0.5000 Uiso R . . 1 1 . H693 H 1.0504 0.5839 0.3130 0.0649 0.5000 Uiso R . . 1 2 . H694 H 1.0626 0.4872 0.3821 0.0651 0.5000 Uiso R . . 1 2 . H5001 H 0.8429 0.7885 0.4058 0.0602 0.5000 Uiso R . . 1 1 . H5002 H 0.8009 0.7248 0.2820 0.0602 0.5000 Uiso R . . 1 1 . H5011 H 0.9012 0.7988 0.4453 0.0602 0.5000 Uiso R . . 1 2 . H5012 H 0.8602 0.7264 0.3259 0.0602 0.5000 Uiso R . . 1 2 . H5101 H 0.6791 0.8354 0.3101 0.0864 0.5000 Uiso R . . 1 1 . H5102 H 0.6007 0.7118 0.2182 0.0861 0.5000 Uiso R . . 1 1 . H5111 H 0.7673 0.8631 0.3146 0.0862 0.5000 Uiso R . . 1 2 . H5112 H 0.6721 0.7461 0.2109 0.0861 0.5000 Uiso R . . 1 2 . H5201 H 0.6336 0.7485 0.4437 0.0783 0.5000 Uiso R . . 1 1 . H5202 H 0.4985 0.6799 0.3230 0.0781 0.5000 Uiso R . . 1 1 . H5211 H 0.6577 0.8032 0.4096 0.0416 0.5000 Uiso R . . 1 2 . H5212 H 0.5394 0.7275 0.2813 0.0407 0.5000 Uiso R . . 1 2 . H5301 H 0.6134 0.5716 0.4437 0.0801 0.5000 Uiso R . . 1 1 . H5302 H 0.5398 0.5287 0.3036 0.0798 0.5000 Uiso R . . 1 1 . H5311 H 0.6374 0.6341 0.4493 0.0528 0.5000 Uiso R . . 1 2 . H5312 H 0.5571 0.5694 0.3118 0.0529 0.5000 Uiso R . . 1 2 . H5401 H 0.7138 0.5886 0.1102 0.0408 0.5000 Uiso R . . 1 2 . H5402 H 0.6238 0.5163 0.1580 0.0406 0.5000 Uiso R . . 1 2 . H5411 H 0.6201 0.5392 0.0782 0.0663 0.5000 Uiso R . . 1 1 . H5412 H 0.5432 0.4046 0.0529 0.0656 0.5000 Uiso R . . 1 1 . H5501 H 0.5394 0.4608 -0.0590 0.0503 0.5000 Uiso R . . 1 2 . H5502 H 0.5087 0.3631 0.0054 0.0500 0.5000 Uiso R . . 1 2 . H5511 H 0.6726 0.5260 -0.0566 0.0501 0.5000 Uiso R . . 1 1 . H5512 H 0.5371 0.4111 -0.1169 0.0500 0.5000 Uiso R . . 1 1 . H5601 H 0.7152 0.4428 -0.0408 0.0472 0.5000 Uiso R . . 1 2 . H5602 H 0.6123 0.3126 -0.0713 0.0469 0.5000 Uiso R . . 1 2 . H5611 H 0.7673 0.4142 -0.0450 0.0527 0.5000 Uiso R . . 1 1 . H5612 H 0.6370 0.3014 -0.0815 0.0529 0.5000 Uiso R . . 1 1 . H6401 H 0.8147 0.5622 0.7741 0.0774 0.5000 Uiso R . . 1 1 . H6402 H 0.6959 0.5406 0.6456 0.0768 0.5000 Uiso R . . 1 1 . H6411 H 0.9012 0.5193 0.8030 0.0873 0.5000 Uiso R . . 1 2 . H6412 H 0.7929 0.5638 0.7566 0.0875 0.5000 Uiso R . . 1 2 . H6601 H 1.0946 0.7394 0.5487 0.0660 0.5000 Uiso R . . 1 1 . H6602 H 1.0891 0.6362 0.6125 0.0661 0.5000 Uiso R . . 1 1 . H6611 H 1.0920 0.6973 0.5938 0.0569 0.5000 Uiso R . . 1 2 . H6612 H 1.0666 0.7571 0.4878 0.0567 0.5000 Uiso R . . 1 2 . H6701 H 1.2827 0.7714 0.5818 0.0778 0.5000 Uiso R . . 1 1 . H6702 H 1.2782 0.6812 0.6592 0.0773 0.5000 Uiso R . . 1 1 . H6711 H 1.2499 0.8089 0.5211 0.1080 0.5000 Uiso R . . 1 2 . H6712 H 1.2807 0.7463 0.6258 0.1081 0.5000 Uiso R . . 1 2 . H6801 H 1.2904 0.6497 0.4858 0.0686 0.5000 Uiso R . . 1 1 . H6802 H 1.2280 0.5503 0.5377 0.0682 0.5000 Uiso R . . 1 1 . H6811 H 1.2559 0.6709 0.4152 0.1031 0.5000 Uiso R . . 1 2 . H6812 H 1.2561 0.5938 0.5063 0.1032 0.5000 Uiso R . . 1 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 0.01502(12) 0.01903(13) 0.02452(13) 0.01150(10) 0.01170(10) 0.01081(10) Co1 0.01612(19) 0.01569(19) 0.01746(18) 0.00729(15) 0.01010(16) 0.00974(16) P1 0.0157(3) 0.0175(3) 0.0195(3) 0.0090(3) 0.0091(3) 0.0106(3) P2 0.0223(4) 0.0209(4) 0.0218(3) 0.0105(3) 0.0149(3) 0.0147(3) P3 0.0165(3) 0.0182(3) 0.0182(3) 0.0080(3) 0.0103(3) 0.0109(3) Na1 0.0272(7) 0.0252(7) 0.0581(9) 0.0022(7) 0.0212(7) 0.0079(6) O1 0.064(2) 0.0476(18) 0.080(2) 0.0320(16) 0.0506(18) 0.0362(16) O2 0.0577(19) 0.0425(17) 0.084(2) 0.0220(16) 0.0482(18) 0.0249(15) O3 0.0325(14) 0.0302(14) 0.0518(16) 0.0015(12) 0.0062(12) 0.0140(12) O4 0.063(2) 0.0368(16) 0.074(2) 0.0075(15) 0.0447(18) 0.0130(15) O5 0.0302(14) 0.0493(18) 0.0642(19) -0.0153(15) 0.0253(14) 0.0004(13) N1 0.0153(11) 0.0205(12) 0.0255(12) 0.0116(10) 0.0103(10) 0.0103(10) N2 0.0231(12) 0.0242(13) 0.0352(14) 0.0108(11) 0.0201(11) 0.0144(11) N3 0.0182(11) 0.0224(12) 0.0195(11) 0.0078(10) 0.0079(9) 0.0105(10) N4 0.0247(14) 0.0240(14) 0.0250(13) 0.0115(11) 0.0146(12) 0.0161(12) N5 0.0229(14) 0.0286(16) 0.0414(16) 0.0138(13) 0.0134(13) 0.0110(13) N6 0.0186(13) 0.0244(14) 0.0377(15) 0.0171(12) 0.0162(12) 0.0130(12) C1 0.0185(13) 0.0257(15) 0.0238(14) 0.0122(12) 0.0120(11) 0.0143(12) C2 0.0297(16) 0.0339(17) 0.0243(14) 0.0127(13) 0.0148(13) 0.0219(15) C3 0.0369(19) 0.051(2) 0.0231(15) 0.0117(15) 0.0166(14) 0.0284(18) C4 0.043(2) 0.070(3) 0.0254(16) 0.0273(17) 0.0207(15) 0.042(2) C5 0.0397(19) 0.046(2) 0.0365(18) 0.0267(16) 0.0253(16) 0.0321(17) C6 0.0239(15) 0.0287(16) 0.0302(15) 0.0173(13) 0.0143(12) 0.0186(13) C7 0.0211(13) 0.0158(13) 0.0246(14) 0.0110(11) 0.0129(11) 0.0117(11) C8 0.0178(13) 0.0233(15) 0.0254(14) 0.0105(12) 0.0110(11) 0.0110(12) C9 0.0301(16) 0.0304(17) 0.0384(17) 0.0181(14) 0.0241(14) 0.0201(14) C10 0.0429(19) 0.0294(17) 0.0387(18) 0.0132(14) 0.0293(16) 0.0228(16) C11 0.0330(17) 0.0247(16) 0.0284(16) 0.0020(13) 0.0145(14) 0.0127(14) C12 0.0231(14) 0.0233(15) 0.0255(14) 0.0079(12) 0.0109(12) 0.0122(12) C13 0.0208(14) 0.0257(16) 0.0469(19) 0.0252(15) 0.0154(14) 0.0147(13) C14 0.043(2) 0.051(2) 0.067(3) 0.045(2) 0.038(2) 0.022(2) C15 0.0225(17) 0.0218(17) 0.072(3) 0.0195(18) 0.0167(18) 0.0078(14) C16 0.0447(19) 0.0409(19) 0.0277(15) 0.0182(14) 0.0253(15) 0.0358(17) C17 0.056(2) 0.082(3) 0.047(2) 0.045(2) 0.041(2) 0.054(3) C18 0.107(5) 0.166(7) 0.069(3) 0.093(4) 0.079(4) 0.115(5) C19 0.148(6) 0.168(7) 0.035(2) 0.051(4) 0.057(4) 0.133(6) C20 0.123(5) 0.094(4) 0.028(2) 0.010(2) 0.023(3) 0.085(4) C21 0.074(3) 0.054(3) 0.0259(17) 0.0104(17) 0.0202(19) 0.046(2) C22 0.0262(15) 0.0213(14) 0.0230(14) 0.0087(12) 0.0132(12) 0.0147(12) C23 0.0424(19) 0.0281(17) 0.046(2) 0.0169(15) 0.0315(17) 0.0249(16) C24 0.055(2) 0.0340(19) 0.052(2) 0.0199(17) 0.0333(19) 0.0346(19) C25 0.043(2) 0.0217(16) 0.0401(19) 0.0146(14) 0.0211(16) 0.0196(15) C26 0.0418(19) 0.0224(16) 0.0335(17) 0.0112(13) 0.0237(15) 0.0133(15) C27 0.0337(17) 0.0198(15) 0.0294(15) 0.0091(12) 0.0191(14) 0.0152(14) C28 0.0292(17) 0.0383(19) 0.051(2) 0.0153(17) 0.0281(16) 0.0224(16) C29 0.034(2) 0.053(3) 0.058(2) 0.021(2) 0.0358(19) 0.0223(19) C30 0.0317(19) 0.043(2) 0.066(3) 0.026(2) 0.0297(19) 0.0261(18) C31 0.0242(14) 0.0233(15) 0.0221(13) 0.0096(11) 0.0125(12) 0.0155(13) C32 0.0431(19) 0.0320(18) 0.0411(19) 0.0203(15) 0.0315(16) 0.0239(16) C33 0.070(3) 0.034(2) 0.064(3) 0.035(2) 0.049(2) 0.031(2) C34 0.072(3) 0.041(2) 0.049(2) 0.0306(19) 0.037(2) 0.040(2) C35 0.050(2) 0.042(2) 0.052(2) 0.0243(18) 0.0281(19) 0.0377(19) C36 0.0318(17) 0.0350(18) 0.0372(17) 0.0199(15) 0.0194(15) 0.0254(15) C37 0.0234(14) 0.0189(13) 0.0252(14) 0.0102(11) 0.0159(12) 0.0130(12) C38 0.0339(17) 0.0387(19) 0.0236(14) 0.0110(13) 0.0159(13) 0.0253(15) C39 0.048(2) 0.047(2) 0.0304(17) 0.0174(16) 0.0266(16) 0.0338(19) C40 0.0425(19) 0.041(2) 0.0407(18) 0.0198(16) 0.0323(16) 0.0303(17) C41 0.0292(16) 0.0316(17) 0.0402(18) 0.0192(14) 0.0252(15) 0.0209(14) C42 0.0222(14) 0.0208(14) 0.0258(14) 0.0100(12) 0.0158(12) 0.0109(12) C43 0.0214(14) 0.0315(17) 0.0214(14) 0.0075(13) 0.0066(12) 0.0137(13) C44 0.0228(16) 0.043(2) 0.0312(17) 0.0147(16) 0.0062(13) 0.0156(16) C45 0.0332(19) 0.0302(19) 0.0306(17) -0.0023(15) 0.0057(15) 0.0095(16) C46 0.0183(16) 0.0294(19) 0.053(2) 0.0204(17) 0.0174(16) 0.0114(14) C47 0.0232(16) 0.044(2) 0.062(2) 0.0329(19) 0.0227(17) 0.0224(16) C48 0.0215(16) 0.0308(19) 0.056(2) 0.0063(17) 0.0112(16) 0.0075(15) C49 0.0278(18) 0.043(2) 0.073(3) 0.038(2) 0.0310(19) 0.0217(17) C57 0.053(3) 0.054(3) 0.053(3) 0.013(2) 0.024(2) 0.030(2) C58 0.039(2) 0.035(2) 0.047(2) 0.0055(17) 0.0149(18) 0.0157(18) C59 0.059(3) 0.050(3) 0.084(4) 0.028(3) 0.014(3) 0.025(3) C60 0.050(3) 0.069(3) 0.065(3) 0.038(3) 0.016(2) 0.026(3) C61 0.037(2) 0.065(3) 0.064(3) 0.033(3) 0.013(2) 0.023(2) C62 0.098(4) 0.050(3) 0.072(3) 0.011(3) 0.062(3) 0.016(3) C63 0.060(3) 0.084(4) 0.063(3) 0.020(3) 0.038(3) 0.032(3) C65 0.076(4) 0.048(3) 0.061(3) 0.000(3) 0.014(3) 0.003(3) C69 0.047(2) 0.054(3) 0.064(3) 0.011(2) 0.034(2) 0.020(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.21781(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 . Co1 . 2.8492(4) yes Nb1 . P1 . 2.9182(7) yes Nb1 . P2 . 2.9181(8) yes Nb1 . P3 . 2.9446(7) yes Nb1 . N1 . 2.055(2) yes Nb1 . N2 . 2.057(3) yes Nb1 . N3 . 2.057(3) yes Nb1 . N6 . 1.810(3) yes Co1 . P1 . 2.1231(8) yes Co1 . P2 . 2.1231(8) yes Co1 . P3 . 2.1355(8) yes Co1 . N4 . 1.768(3) yes P1 . N1 . 1.697(3) yes P1 . C1 . 1.859(3) yes P1 . C7 . 1.850(3) yes P2 . N2 . 1.689(3) yes P2 . C16 . 1.845(3) yes P2 . C22 . 1.853(3) yes P3 . N3 . 1.697(3) yes P3 . C31 . 1.840(3) yes P3 . C37 . 1.857(3) yes Na1 . O1 . 2.429(3) yes Na1 . O2 . 2.409(4) yes Na1 . O3 . 2.407(3) yes Na1 . O4 . 2.370(4) yes Na1 . O5 . 2.353(3) yes Na1 . N5 . 2.489(3) yes O1 . C500 . 1.402(13) yes O1 . C530 . 1.527(13) yes O1 . C501 . 1.501(10) yes O1 . C531 . 1.378(10) yes O2 . C57 . 1.413(6) yes O2 . C541 . 1.633(11) yes O2 . C57 . 1.413(6) yes O2 . C540 . 1.332(8) yes O3 . C58 . 1.433(5) yes O3 . C61 . 1.406(5) yes O4 . C62 . 1.432(6) yes O4 . C65 . 1.400(6) yes O5 . C69 . 1.431(5) yes O5 . C660 . 1.428(11) yes O5 . C69 . 1.431(5) yes O5 . C661 . 1.448(10) yes N1 . C13 . 1.470(4) yes N2 . C28 . 1.478(4) yes N3 . C43 . 1.471(4) yes N4 . N5 . 1.115(4) yes N6 . C46 . 1.471(5) yes C1 . C2 . 1.389(4) yes C1 . C6 . 1.408(4) yes C2 . C3 . 1.393(4) yes C2 . H21 . 0.926 no C3 . C4 . 1.382(5) yes C3 . H31 . 0.928 no C4 . C5 . 1.389(6) yes C4 . H41 . 0.927 no C5 . C6 . 1.386(5) yes C5 . H51 . 0.928 no C6 . H61 . 0.938 no C7 . C8 . 1.394(4) yes C7 . C12 . 1.393(4) yes C8 . C9 . 1.392(5) yes C8 . H81 . 0.949 no C9 . C10 . 1.388(5) yes C9 . H91 . 0.958 no C10 . C11 . 1.385(5) yes C10 . H101 . 0.932 no C11 . C12 . 1.393(5) yes C11 . H111 . 0.941 no C12 . H121 . 0.929 no C13 . C14 . 1.531(6) yes C13 . C15 . 1.499(5) yes C13 . H131 . 0.980 no C14 . H141 . 0.960 no C14 . H142 . 0.943 no C14 . H143 . 0.963 no C15 . H151 . 0.947 no C15 . H152 . 0.957 no C15 . H153 . 0.957 no C16 . C17 . 1.407(5) yes C16 . C21 . 1.374(6) yes C17 . C18 . 1.385(6) yes C17 . H171 . 0.946 no C18 . C19 . 1.391(10) yes C18 . H181 . 0.940 no C19 . C20 . 1.347(10) yes C19 . H191 . 0.935 no C20 . C21 . 1.390(6) yes C20 . H201 . 0.925 no C21 . H211 . 0.918 no C22 . C23 . 1.400(4) yes C22 . C27 . 1.392(4) yes C23 . C24 . 1.385(5) yes C23 . H231 . 0.958 no C24 . C25 . 1.382(5) yes C24 . H241 . 0.930 no C25 . C26 . 1.391(5) yes C25 . H251 . 0.931 no C26 . C27 . 1.391(4) yes C26 . H261 . 0.932 no C27 . H271 . 0.933 no C28 . C29 . 1.524(5) yes C28 . C30 . 1.525(5) yes C28 . H281 . 0.990 no C29 . H291 . 0.976 no C29 . H292 . 0.962 no C29 . H293 . 0.958 no C30 . H301 . 0.960 no C30 . H302 . 0.962 no C30 . H303 . 0.979 no C31 . C32 . 1.397(4) yes C31 . C36 . 1.394(4) yes C32 . C33 . 1.400(5) yes C32 . H321 . 0.917 no C33 . C34 . 1.370(6) yes C33 . H331 . 0.932 no C34 . C35 . 1.377(6) yes C34 . H341 . 0.930 no C35 . C36 . 1.394(5) yes C35 . H351 . 0.931 no C36 . H361 . 0.933 no C37 . C38 . 1.390(4) yes C37 . C42 . 1.396(4) yes C38 . C39 . 1.393(5) yes C38 . H381 . 0.931 no C39 . C40 . 1.377(5) yes C39 . H391 . 0.932 no C40 . C41 . 1.385(5) yes C40 . H401 . 0.936 no C41 . C42 . 1.377(4) yes C41 . H411 . 0.930 no C42 . H421 . 0.934 no C43 . C44 . 1.516(5) yes C43 . C45 . 1.541(5) yes C43 . H431 . 1.001 no C44 . H441 . 0.957 no C44 . H442 . 0.982 no C44 . H443 . 0.975 no C45 . H451 . 0.964 no C45 . H452 . 0.977 no C45 . H453 . 0.985 no C46 . C47 . 1.531(5) yes C46 . C48 . 1.528(6) yes C46 . C49 . 1.524(5) yes C47 . H471 . 0.935 no C47 . H472 . 0.955 no C47 . H473 . 0.949 no C48 . H481 . 0.963 no C48 . H482 . 0.966 no C48 . H483 . 0.950 no C49 . H491 . 0.971 no C49 . H492 . 0.980 no C49 . H493 . 0.946 no C57 . C561 . 1.566(10) yes C57 . H571 . 0.971 no C57 . H572 . 0.964 no C57 . C560 . 1.458(10) yes C57 . H573 . 0.973 no C57 . H574 . 0.964 no C58 . C59 . 1.474(6) yes C58 . H581 . 0.986 no C58 . H582 . 0.974 no C59 . C60 . 1.451(7) yes C59 . H591 . 0.962 no C59 . H592 . 0.971 no C60 . C61 . 1.513(7) yes C60 . H601 . 0.969 no C60 . H602 . 0.948 no C61 . H611 . 0.948 no C61 . H612 . 0.969 no C62 . C63 . 1.487(7) yes C62 . H621 . 0.977 no C62 . H622 . 0.987 no C63 . C640 . 1.536(13) yes C63 . H631 . 0.975 no C63 . H632 . 0.969 no C63 . C641 . 1.528(14) yes C63 . H631 . 0.975 no C63 . H632 . 0.969 no C65 . C640 . 1.456(13) yes C65 . H651 . 0.970 no C65 . H652 . 0.961 no C65 . C641 . 1.453(14) yes C65 . H651 . 0.970 no C65 . H652 . 0.961 no C69 . C680 . 1.591(12) yes C69 . H691 . 0.976 no C69 . H692 . 0.971 no C69 . C681 . 1.401(15) yes C69 . H693 . 0.974 no C69 . H694 . 0.973 no C500 . C510 . 1.524(19) yes C500 . H5001 . 0.950 no C500 . H5002 . 0.950 no C501 . C511 . 1.585(15) yes C501 . H5011 . 0.950 no C501 . H5012 . 0.950 no C510 . C520 . 1.472(18) yes C510 . H5101 . 0.973 no C510 . H5102 . 0.972 no C511 . C521 . 1.487(15) yes C511 . H5111 . 0.980 no C511 . H5112 . 0.965 no C520 . C530 . 1.482(18) yes C520 . H5201 . 0.977 no C520 . H5202 . 0.978 no C521 . C531 . 1.499(14) yes C521 . H5211 . 0.970 no C521 . H5212 . 0.965 no C530 . H5301 . 0.977 no C530 . H5302 . 0.968 no C531 . H5311 . 0.983 no C531 . H5312 . 0.976 no C540 . C550 . 1.480(11) yes C540 . H5401 . 0.958 no C540 . H5402 . 0.968 no C541 . C551 . 1.469(14) yes C541 . H5411 . 0.964 no C541 . H5412 . 0.962 no C550 . C560 . 1.474(13) yes C550 . H5501 . 0.964 no C550 . H5502 . 0.962 no C551 . C561 . 1.502(13) yes C551 . H5511 . 0.971 no C551 . H5512 . 0.974 no C560 . H5601 . 0.970 no C560 . H5602 . 0.975 no C561 . H5611 . 0.963 no C561 . H5612 . 0.971 no C640 . H6401 . 0.982 no C640 . H6402 . 0.971 no C641 . H6411 . 0.975 no C641 . H6412 . 0.973 no C660 . C670 . 1.394(15) yes C660 . H6601 . 0.981 no C660 . H6602 . 0.976 no C661 . C671 . 1.392(17) yes C661 . H6611 . 0.970 no C661 . H6612 . 0.975 no C670 . C680 . 1.323(15) yes C670 . H6701 . 0.977 no C670 . H6702 . 0.959 no C671 . C681 . 1.58(2) yes C671 . H6711 . 0.982 no C671 . H6712 . 0.967 no C680 . H6801 . 0.982 no C680 . H6802 . 0.967 no C681 . H6811 . 0.978 no C681 . H6812 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Nb1 . P2 . 74.91(2) yes P1 . Nb1 . P3 . 71.16(2) yes P2 . Nb1 . P3 . 71.92(2) yes Co1 . Nb1 . N1 . 77.33(7) yes P2 . Nb1 . N1 . 98.91(7) yes P3 . Nb1 . N1 . 102.19(7) yes Co1 . Nb1 . N2 . 77.59(7) yes P1 . Nb1 . N2 . 105.06(8) yes P3 . Nb1 . N2 . 97.24(7) yes N1 . Nb1 . N2 . 116.58(10) yes Co1 . Nb1 . N3 . 77.23(7) yes P1 . Nb1 . N3 . 95.48(7) yes P2 . Nb1 . N3 . 101.07(7) yes P3 . Nb1 . N3 . 34.17(7) yes N1 . Nb1 . N3 . 115.21(10) yes Co1 . Nb1 . N6 . 179.73(9) yes P1 . Nb1 . N6 . 136.55(9) yes P2 . Nb1 . N6 . 137.02(10) yes P3 . Nb1 . N6 . 136.86(10) yes N1 . Nb1 . N6 . 102.41(11) yes N2 . Nb1 . N3 . 114.31(10) yes N2 . Nb1 . N6 . 102.62(12) yes N3 . Nb1 . N6 . 102.82(12) yes Nb1 . Co1 . P1 . 70.14(2) yes Nb1 . Co1 . P2 . 70.14(2) yes P1 . Co1 . P2 . 113.42(3) yes Nb1 . Co1 . P3 . 70.77(2) yes P1 . Co1 . P3 . 106.46(3) yes P2 . Co1 . P3 . 107.88(3) yes Nb1 . Co1 . N4 . 172.65(9) yes P1 . Co1 . N4 . 109.15(9) yes P2 . Co1 . N4 . 104.14(9) yes P3 . Co1 . N4 . 116.00(9) yes Nb1 . P1 . Co1 . 66.68(2) yes Co1 . P1 . N1 . 109.35(9) yes Nb1 . P1 . C1 . 135.85(9) yes Co1 . P1 . C1 . 119.73(10) yes N1 . P1 . C1 . 105.41(13) yes Nb1 . P1 . C7 . 115.41(9) yes Co1 . P1 . C7 . 118.05(9) yes N1 . P1 . C7 . 102.53(13) yes C1 . P1 . C7 . 99.79(13) yes Nb1 . P2 . Co1 . 66.68(2) yes Co1 . P2 . N2 . 110.12(10) yes Nb1 . P2 . C16 . 122.76(12) yes Co1 . P2 . C16 . 119.50(10) yes N2 . P2 . C16 . 103.57(15) yes Nb1 . P2 . C22 . 133.01(10) yes Co1 . P2 . C22 . 115.93(10) yes N2 . P2 . C22 . 108.84(13) yes C16 . P2 . C22 . 97.54(14) yes Nb1 . P3 . Co1 . 66.01(2) yes Co1 . P3 . N3 . 108.66(9) yes Nb1 . P3 . C31 . 119.55(10) yes Co1 . P3 . C31 . 121.29(10) yes N3 . P3 . C31 . 100.83(13) yes Nb1 . P3 . C37 . 133.32(10) yes Co1 . P3 . C37 . 116.44(10) yes N3 . P3 . C37 . 108.91(13) yes C31 . P3 . C37 . 99.17(13) yes O1 . Na1 . O2 . 93.17(12) yes O1 . Na1 . O3 . 171.37(13) yes O2 . Na1 . O3 . 95.02(12) yes O1 . Na1 . O4 . 84.71(12) yes O2 . Na1 . O4 . 174.41(13) yes O3 . Na1 . O4 . 86.89(12) yes O1 . Na1 . O5 . 91.75(12) yes O2 . Na1 . O5 . 87.99(12) yes O3 . Na1 . O5 . 91.26(12) yes O4 . Na1 . O5 . 97.23(13) yes O1 . Na1 . N5 . 91.38(12) yes O2 . Na1 . N5 . 81.73(12) yes O3 . Na1 . N5 . 87.12(10) yes O4 . Na1 . N5 . 93.13(12) yes O5 . Na1 . N5 . 169.41(13) yes Na1 . O1 . C500 . 128.9(6) yes Na1 . O1 . C530 . 110.7(5) yes C500 . O1 . C530 . 110.6(8) yes Na1 . O1 . C501 . 119.1(4) yes Na1 . O1 . C531 . 130.7(5) yes C501 . O1 . C531 . 108.7(6) yes Na1 . O2 . C57 . 121.5(3) yes Na1 . O2 . C541 . 123.4(4) yes C57 . O2 . C541 . 93.4(5) yes Na1 . O2 . C57 . 121.5(3) yes Na1 . O2 . C540 . 108.7(4) yes C57 . O2 . C540 . 119.2(5) yes Na1 . O3 . C58 . 121.9(2) yes Na1 . O3 . C61 . 128.8(3) yes C58 . O3 . C61 . 107.2(3) yes Na1 . O4 . C62 . 121.7(3) yes Na1 . O4 . C65 . 127.3(3) yes C62 . O4 . C65 . 108.7(4) yes Na1 . O5 . C69 . 121.9(3) yes Na1 . O5 . C660 . 129.6(5) yes C69 . O5 . C660 . 106.9(5) yes Na1 . O5 . C69 . 121.9(3) yes Na1 . O5 . C661 . 130.8(4) yes C69 . O5 . C661 . 105.9(5) yes P1 . N1 . Nb1 . 101.70(12) yes P1 . N1 . C13 . 121.9(2) yes Nb1 . N1 . C13 . 136.36(19) yes P2 . N2 . Nb1 . 101.88(12) yes P2 . N2 . C28 . 124.0(2) yes Nb1 . N2 . C28 . 134.1(2) yes P3 . N3 . Nb1 . 102.93(12) yes P3 . N3 . C43 . 122.0(2) yes Nb1 . N3 . C43 . 134.9(2) yes Co1 . N4 . N5 . 175.7(3) yes Na1 . N5 . N4 . 172.3(3) yes Nb1 . N6 . C46 . 179.1(3) yes P1 . C1 . C2 . 117.0(2) yes P1 . C1 . C6 . 125.2(2) yes C2 . C1 . C6 . 117.8(3) yes C1 . C2 . C3 . 121.2(3) yes C1 . C2 . H21 . 119.8 no C3 . C2 . H21 . 118.9 no C2 . C3 . C4 . 119.9(3) yes C2 . C3 . H31 . 118.6 no C4 . C3 . H31 . 121.5 no C3 . C4 . C5 . 120.2(3) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 119.4 no C4 . C5 . C6 . 119.6(3) yes C4 . C5 . H51 . 119.5 no C6 . C5 . H51 . 120.9 no C1 . C6 . C5 . 121.2(3) yes C1 . C6 . H61 . 119.6 no C5 . C6 . H61 . 119.2 no P1 . C7 . C8 . 122.8(2) yes P1 . C7 . C12 . 119.2(2) yes C8 . C7 . C12 . 117.3(3) yes C7 . C8 . C9 . 121.5(3) yes C7 . C8 . H81 . 118.8 no C9 . C8 . H81 . 119.6 no C8 . C9 . C10 . 120.2(3) yes C8 . C9 . H91 . 118.4 no C10 . C9 . H91 . 121.3 no C9 . C10 . C11 . 119.1(3) yes C9 . C10 . H101 . 121.6 no C11 . C10 . H101 . 119.3 no C10 . C11 . C12 . 120.2(3) yes C10 . C11 . H111 . 120.2 no C12 . C11 . H111 . 119.6 no C11 . C12 . C7 . 121.6(3) yes C11 . C12 . H121 . 120.6 no C7 . C12 . H121 . 117.9 no N1 . C13 . C14 . 108.6(3) yes N1 . C13 . C15 . 113.0(3) yes C14 . C13 . C15 . 113.3(3) yes N1 . C13 . H131 . 107.6 no C14 . C13 . H131 . 107.8 no C15 . C13 . H131 . 106.2 no C13 . C14 . H141 . 109.7 no C13 . C14 . H142 . 108.9 no H141 . C14 . H142 . 110.3 no C13 . C14 . H143 . 112.1 no H141 . C14 . H143 . 107.1 no H142 . C14 . H143 . 108.6 no C13 . C15 . H151 . 109.3 no C13 . C15 . H152 . 109.8 no H151 . C15 . H152 . 109.4 no C13 . C15 . H153 . 108.4 no H151 . C15 . H153 . 110.7 no H152 . C15 . H153 . 109.2 no P2 . C16 . C17 . 119.6(3) yes P2 . C16 . C21 . 122.1(3) yes C17 . C16 . C21 . 118.0(4) yes C16 . C17 . C18 . 120.0(5) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 119.7 no C17 . C18 . C19 . 120.6(5) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 119.2(4) yes C18 . C19 . H191 . 121.3 no C20 . C19 . H191 . 119.5 no C19 . C20 . C21 . 121.1(6) yes C19 . C20 . H201 . 119.1 no C21 . C20 . H201 . 119.8 no C20 . C21 . C16 . 121.1(5) yes C20 . C21 . H211 . 119.5 no C16 . C21 . H211 . 119.4 no P2 . C22 . C23 . 125.4(2) yes P2 . C22 . C27 . 117.7(2) yes C23 . C22 . C27 . 116.8(3) yes C22 . C23 . C24 . 121.9(3) yes C22 . C23 . H231 . 118.0 no C24 . C23 . H231 . 120.1 no C23 . C24 . C25 . 120.1(3) yes C23 . C24 . H241 . 120.3 no C25 . C24 . H241 . 119.6 no C24 . C25 . C26 . 119.3(3) yes C24 . C25 . H251 . 119.4 no C26 . C25 . H251 . 121.3 no C25 . C26 . C27 . 120.0(3) yes C25 . C26 . H261 . 120.3 no C27 . C26 . H261 . 119.7 no C22 . C27 . C26 . 121.7(3) yes C22 . C27 . H271 . 118.7 no C26 . C27 . H271 . 119.5 no N2 . C28 . C29 . 111.8(3) yes N2 . C28 . C30 . 109.4(3) yes C29 . C28 . C30 . 112.1(3) yes N2 . C28 . H281 . 108.5 no C29 . C28 . H281 . 107.4 no C30 . C28 . H281 . 107.5 no C28 . C29 . H291 . 110.8 no C28 . C29 . H292 . 111.4 no H291 . C29 . H292 . 108.4 no C28 . C29 . H293 . 109.3 no H291 . C29 . H293 . 107.5 no H292 . C29 . H293 . 109.3 no C28 . C30 . H301 . 110.9 no C28 . C30 . H302 . 110.2 no H301 . C30 . H302 . 108.6 no C28 . C30 . H303 . 109.4 no H301 . C30 . H303 . 109.1 no H302 . C30 . H303 . 108.7 no P3 . C31 . C32 . 123.3(2) yes P3 . C31 . C36 . 119.1(2) yes C32 . C31 . C36 . 117.2(3) yes C31 . C32 . C33 . 121.2(3) yes C31 . C32 . H321 . 120.4 no C33 . C32 . H321 . 118.3 no C32 . C33 . C34 . 120.5(4) yes C32 . C33 . H331 . 120.3 no C34 . C33 . H331 . 119.3 no C33 . C34 . C35 . 119.2(3) yes C33 . C34 . H341 . 119.8 no C35 . C34 . H341 . 121.0 no C34 . C35 . C36 . 120.9(3) yes C34 . C35 . H351 . 120.0 no C36 . C35 . H351 . 119.1 no C31 . C36 . C35 . 121.0(3) yes C31 . C36 . H361 . 118.5 no C35 . C36 . H361 . 120.5 no P3 . C37 . C38 . 126.8(2) yes P3 . C37 . C42 . 116.2(2) yes C38 . C37 . C42 . 117.0(3) yes C37 . C38 . C39 . 121.2(3) yes C37 . C38 . H381 . 118.7 no C39 . C38 . H381 . 120.1 no C38 . C39 . C40 . 120.7(3) yes C38 . C39 . H391 . 120.5 no C40 . C39 . H391 . 118.8 no C39 . C40 . C41 . 118.7(3) yes C39 . C40 . H401 . 119.6 no C41 . C40 . H401 . 121.7 no C40 . C41 . C42 . 120.6(3) yes C40 . C41 . H411 . 119.0 no C42 . C41 . H411 . 120.4 no C37 . C42 . C41 . 121.7(3) yes C37 . C42 . H421 . 119.5 no C41 . C42 . H421 . 118.8 no N3 . C43 . C44 . 112.5(3) yes N3 . C43 . C45 . 109.5(3) yes C44 . C43 . C45 . 111.3(3) yes N3 . C43 . H431 . 108.5 no C44 . C43 . H431 . 106.4 no C45 . C43 . H431 . 108.5 no C43 . C44 . H441 . 109.7 no C43 . C44 . H442 . 107.5 no H441 . C44 . H442 . 111.5 no C43 . C44 . H443 . 109.7 no H441 . C44 . H443 . 109.7 no H442 . C44 . H443 . 108.6 no C43 . C45 . H451 . 110.0 no C43 . C45 . H452 . 110.9 no H451 . C45 . H452 . 108.5 no C43 . C45 . H453 . 111.6 no H451 . C45 . H453 . 107.3 no H452 . C45 . H453 . 108.4 no N6 . C46 . C47 . 110.7(3) yes N6 . C46 . C48 . 109.8(3) yes C47 . C46 . C48 . 108.4(3) yes N6 . C46 . C49 . 110.3(3) yes C47 . C46 . C49 . 108.3(3) yes C48 . C46 . C49 . 109.3(3) yes C46 . C47 . H471 . 109.9 no C46 . C47 . H472 . 110.0 no H471 . C47 . H472 . 108.6 no C46 . C47 . H473 . 110.3 no H471 . C47 . H473 . 108.2 no H472 . C47 . H473 . 109.7 no C46 . C48 . H481 . 108.0 no C46 . C48 . H482 . 109.2 no H481 . C48 . H482 . 109.8 no C46 . C48 . H483 . 109.1 no H481 . C48 . H483 . 110.5 no H482 . C48 . H483 . 110.2 no C46 . C49 . H491 . 108.7 no C46 . C49 . H492 . 106.2 no H491 . C49 . H492 . 109.6 no C46 . C49 . H493 . 109.5 no H491 . C49 . H493 . 111.9 no H492 . C49 . H493 . 110.7 no O2 . C57 . C561 . 114.9(5) yes O2 . C57 . H571 . 107.7 no C561 . C57 . H571 . 108.3 no O2 . C57 . H572 . 107.6 no C561 . C57 . H572 . 108.9 no H571 . C57 . H572 . 109.4 no O2 . C57 . C560 . 98.1(5) yes O2 . C57 . H573 . 111.0 no C560 . C57 . H573 . 111.4 no O2 . C57 . H574 . 112.2 no C560 . C57 . H574 . 114.4 no H573 . C57 . H574 . 109.4 no O3 . C58 . C59 . 108.2(4) yes O3 . C58 . H581 . 110.7 no C59 . C58 . H581 . 111.6 no O3 . C58 . H582 . 109.4 no C59 . C58 . H582 . 110.4 no H581 . C58 . H582 . 106.6 no C58 . C59 . C60 . 106.7(4) yes C58 . C59 . H591 . 108.8 no C60 . C59 . H591 . 109.4 no C58 . C59 . H592 . 110.8 no C60 . C59 . H592 . 109.9 no H591 . C59 . H592 . 111.2 no C59 . C60 . C61 . 105.3(4) yes C59 . C60 . H601 . 109.9 no C61 . C60 . H601 . 113.4 no C59 . C60 . H602 . 108.1 no C61 . C60 . H602 . 111.0 no H601 . C60 . H602 . 109.0 no C60 . C61 . O3 . 106.7(4) yes C60 . C61 . H611 . 110.7 no O3 . C61 . H611 . 108.3 no C60 . C61 . H612 . 113.1 no O3 . C61 . H612 . 109.5 no H611 . C61 . H612 . 108.5 no O4 . C62 . C63 . 108.1(4) yes O4 . C62 . H621 . 109.4 no C63 . C62 . H621 . 110.4 no O4 . C62 . H622 . 108.8 no C63 . C62 . H622 . 110.5 no H621 . C62 . H622 . 109.6 no C62 . C63 . C640 . 99.3(6) yes C62 . C63 . H631 . 111.6 no C640 . C63 . H631 . 102.2 no C62 . C63 . H632 . 110.4 no C640 . C63 . H632 . 124.2 no H631 . C63 . H632 . 108.6 no C62 . C63 . C641 . 106.6(6) yes C62 . C63 . H631 . 111.6 no C641 . C63 . H631 . 121.3 no C62 . C63 . H632 . 110.4 no C641 . C63 . H632 . 97.3 no H631 . C63 . H632 . 108.6 no O4 . C65 . C640 . 105.4(6) yes O4 . C65 . H651 . 109.1 no C640 . C65 . H651 . 122.1 no O4 . C65 . H652 . 111.4 no C640 . C65 . H652 . 100.6 no H651 . C65 . H652 . 107.9 no O4 . C65 . C641 . 112.3(7) yes O4 . C65 . H651 . 109.1 no C641 . C65 . H651 . 94.1 no O4 . C65 . H652 . 111.4 no C641 . C65 . H652 . 120.2 no H651 . C65 . H652 . 107.9 no O5 . C69 . C680 . 99.6(5) yes O5 . C69 . H691 . 112.7 no C680 . C69 . H691 . 111.6 no O5 . C69 . H692 . 111.1 no C680 . C69 . H692 . 112.1 no H691 . C69 . H692 . 109.5 no O5 . C69 . C681 . 111.6(7) yes O5 . C69 . H693 . 110.5 no C681 . C69 . H693 . 108.7 no O5 . C69 . H694 . 107.8 no C681 . C69 . H694 . 108.6 no H693 . C69 . H694 . 109.5 no O1 . C500 . C510 . 103.7(10) yes O1 . C500 . H5001 . 103.2 no C510 . C500 . H5001 . 103.8 no O1 . C500 . H5002 . 117.1 no C510 . C500 . H5002 . 117.9 no H5001 . C500 . H5002 . 109.5 no O1 . C501 . C511 . 97.8(8) yes O1 . C501 . H5011 . 117.1 no C511 . C501 . H5011 . 117.5 no O1 . C501 . H5012 . 106.7 no C511 . C501 . H5012 . 107.2 no H5011 . C501 . H5012 . 109.5 no C500 . C510 . C520 . 107.8(11) yes C500 . C510 . H5101 . 114.4 no C520 . C510 . H5101 . 112.9 no C500 . C510 . H5102 . 101.6 no C520 . C510 . H5102 . 109.1 no H5101 . C510 . H5102 . 110.4 no C501 . C511 . C521 . 104.6(8) yes C501 . C511 . H5111 . 101.3 no C521 . C511 . H5111 . 111.3 no C501 . C511 . H5112 . 115.4 no C521 . C511 . H5112 . 112.9 no H5111 . C511 . H5112 . 110.7 no C510 . C520 . C530 . 102.3(11) yes C510 . C520 . H5201 . 111.4 no C530 . C520 . H5201 . 111.5 no C510 . C520 . H5202 . 111.7 no C530 . C520 . H5202 . 111.4 no H5201 . C520 . H5202 . 108.5 no C511 . C521 . C531 . 100.3(8) yes C511 . C521 . H5211 . 111.8 no C531 . C521 . H5211 . 112.5 no C511 . C521 . H5212 . 110.1 no C531 . C521 . H5212 . 111.7 no H5211 . C521 . H5212 . 110.2 no O1 . C530 . C520 . 103.2(10) yes O1 . C530 . H5301 . 110.5 no C520 . C530 . H5301 . 108.5 no O1 . C530 . H5302 . 111.9 no C520 . C530 . H5302 . 112.0 no H5301 . C530 . H5302 . 110.5 no C521 . C531 . O1 . 112.0(8) yes C521 . C531 . H5311 . 109.1 no O1 . C531 . H5311 . 110.1 no C521 . C531 . H5312 . 108.5 no O1 . C531 . H5312 . 106.9 no H5311 . C531 . H5312 . 110.2 no O2 . C540 . C550 . 100.4(6) yes O2 . C540 . H5401 . 111.3 no C550 . C540 . H5401 . 112.1 no O2 . C540 . H5402 . 112.4 no C550 . C540 . H5402 . 110.6 no H5401 . C540 . H5402 . 109.8 no O2 . C541 . C551 . 109.0(7) yes O2 . C541 . H5411 . 108.5 no C551 . C541 . H5411 . 110.2 no O2 . C541 . H5412 . 110.4 no C551 . C541 . H5412 . 110.0 no H5411 . C541 . H5412 . 108.8 no C540 . C550 . C560 . 102.2(7) yes C540 . C550 . H5501 . 111.2 no C560 . C550 . H5501 . 111.9 no C540 . C550 . H5502 . 110.8 no C560 . C550 . H5502 . 111.0 no H5501 . C550 . H5502 . 109.7 no C541 . C551 . C561 . 104.5(8) yes C541 . C551 . H5511 . 110.5 no C561 . C551 . H5511 . 110.5 no C541 . C551 . H5512 . 112.4 no C561 . C551 . H5512 . 109.7 no H5511 . C551 . H5512 . 109.2 no C550 . C560 . C57 . 104.7(7) yes C550 . C560 . H5601 . 111.1 no C57 . C560 . H5601 . 110.6 no C550 . C560 . H5602 . 110.7 no C57 . C560 . H5602 . 111.3 no H5601 . C560 . H5602 . 108.4 no C57 . C561 . C551 . 102.3(7) yes C57 . C561 . H5611 . 110.8 no C551 . C561 . H5611 . 111.4 no C57 . C561 . H5612 . 111.7 no C551 . C561 . H5612 . 111.5 no H5611 . C561 . H5612 . 109.1 no C63 . C640 . C65 . 103.1(8) yes C63 . C640 . H6401 . 111.4 no C65 . C640 . H6401 . 111.1 no C63 . C640 . H6402 . 111.4 no C65 . C640 . H6402 . 109.9 no H6401 . C640 . H6402 . 109.8 no C63 . C641 . C65 . 103.6(8) yes C63 . C641 . H6411 . 111.6 no C65 . C641 . H6411 . 110.0 no C63 . C641 . H6412 . 111.6 no C65 . C641 . H6412 . 110.8 no H6411 . C641 . H6412 . 109.1 no O5 . C660 . C670 . 111.8(9) yes O5 . C660 . H6601 . 107.2 no C670 . C660 . H6601 . 111.0 no O5 . C660 . H6602 . 108.2 no C670 . C660 . H6602 . 108.6 no H6601 . C660 . H6602 . 110.0 no O5 . C661 . C671 . 108.9(9) yes O5 . C661 . H6611 . 108.1 no C671 . C661 . H6611 . 112.3 no O5 . C661 . H6612 . 110.2 no C671 . C661 . H6612 . 107.9 no H6611 . C661 . H6612 . 109.5 no C660 . C670 . C680 . 106.4(10) yes C660 . C670 . H6701 . 111.5 no C680 . C670 . H6701 . 111.7 no C660 . C670 . H6702 . 109.5 no C680 . C670 . H6702 . 108.0 no H6701 . C670 . H6702 . 109.6 no C661 . C671 . C681 . 107.5(11) yes C661 . C671 . H6711 . 108.2 no C681 . C671 . H6711 . 109.7 no C661 . C671 . H6712 . 108.9 no C681 . C671 . H6712 . 112.3 no H6711 . C671 . H6712 . 110.2 no C69 . C680 . C670 . 108.5(9) yes C69 . C680 . H6801 . 110.4 no C670 . C680 . H6801 . 110.3 no C69 . C680 . H6802 . 108.6 no C670 . C680 . H6802 . 109.6 no H6801 . C680 . H6802 . 109.5 no C671 . C681 . C69 . 101.8(11) yes C671 . C681 . H6811 . 111.7 no C69 . C681 . H6811 . 111.8 no C671 . C681 . H6812 . 111.8 no C69 . C681 . H6812 . 109.4 no H6811 . C681 . H6812 . 110.2 no _iucr_refine_instruction_details_constraints ; # # Punched on 14/07/11 at 17:12:00 # #LIST 12 BLOCK SCALE NB(1,X'S, U'S ) UNTIL C(69) CONT C(500,X'S,U[ISO]) UNTIL C(681) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) H ( 473,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) H ( 483,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) H ( 493,X'S) RIDE C ( 500,X'S) H ( 5001,X'S) H ( 5002,X'S) RIDE C ( 501,X'S) H ( 5011,X'S) H ( 5012,X'S) REM TOO MANY H ATOMS ON C ( 57), - 4 RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) CONT H ( 573,X'S) H ( 574,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S) RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) RIDE C ( 65,X'S) H ( 651,X'S) H ( 652,X'S) REM TOO MANY H ATOMS ON C ( 69), - 4 RIDE C ( 69,X'S) H ( 691,X'S) H ( 692,X'S) CONT H ( 693,X'S) H ( 694,X'S) RIDE C ( 510,X'S) H (5101,X'S) H (5102,X'S) RIDE C ( 511,X'S) H (5111,X'S) H (5112,X'S) RIDE C ( 520,X'S) H (5201,X'S) H (5202,X'S) RIDE C ( 521,X'S) H (5211,X'S) H (5212,X'S) RIDE C ( 530,X'S) H (5301,X'S) H (5302,X'S) RIDE C ( 531,X'S) H (5311,X'S) H (5312,X'S) RIDE C ( 540,X'S) H (5401,X'S) H (5402,X'S) RIDE C ( 541,X'S) H (5411,X'S) H (5412,X'S) RIDE C ( 550,X'S) H (5501,X'S) H (5502,X'S) RIDE C ( 551,X'S) H (5511,X'S) H (5512,X'S) RIDE C ( 560,X'S) H (5601,X'S) H (5602,X'S) RIDE C ( 561,X'S) H (5611,X'S) H (5612,X'S) RIDE C ( 640,X'S) H (6401,X'S) H (6402,X'S) RIDE C ( 641,X'S) H (6411,X'S) H (6412,X'S) RIDE C ( 660,X'S) H (6601,X'S) H (6602,X'S) RIDE C ( 661,X'S) H (6611,X'S) H (6612,X'S) RIDE C ( 670,X'S) H (6701,X'S) H (6702,X'S) RIDE C ( 671,X'S) H (6711,X'S) H (6712,X'S) RIDE C ( 680,X'S) H (6801,X'S) H (6802,X'S) RIDE C ( 681,X'S) H (6811,X'S) H (6812,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 14/07/11 at 17:12:00 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END data_3Ta _database_code_depnum_ccdc_archive 'CCDC 862677' #TrackingRef '- combined_22Feb.cif' _audit_creation_date 11-03-13 _audit_creation_method CRYSTALS_ver_14.11 _vrf_PLAT220_3Ta ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.95 Ratio RESPONSE: The warning is appropriate, but can be ignored owing to remaining unresolved disorder in the weakly coordinated THF molecules as well as the phenyl ring atoms c(16) - C(21). The THF molecules should not be defined as 'non-solvent' molecules on this case. ; _oxford_structure_analysis_title 'cmt49_0m in P1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.8488(3) _cell_length_b 12.9768(3) _cell_length_c 13.2265(3) _cell_angle_alpha 91.961(1) _cell_angle_beta 117.278(1) _cell_angle_gamma 112.849(1) _cell_volume 1744.62(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ta -0.7052 6.5227 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C60 H90 Co1 N3 Na1 O5 P3 Ta1 # Dc = 1.23 Fooo = 752.00 Mu = 19.22 M = 1289.18 # Found Formula = C69 H100 Co1 N6 Na1 O5 P3 Ta1 # Dc = 1.38 FOOO = 752.00 Mu = 19.31 M = 1449.38 _chemical_formula_sum 'C69 H100 Co1 N6 Na1 O5 P3 Ta1' _chemical_formula_moiety 'C69 H100 Co1 N6 Na1 O5 P3 Ta1' _chemical_compound_source ? _chemical_formula_weight 1449.38 _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'prism fragment' _exptl_crystal_colour red _exptl_crystal_size_min 0.149 _exptl_crystal_size_mid 0.205 _exptl_crystal_size_max 0.415 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.931 # Sheldrick geometric approximatio 0.67 0.75 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.75 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 34788 _reflns_number_total 19327 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections without Friedels Law is 19327 # Number of reflections with Friedels Law is 10163 # Theoretical number of reflections is about 10220 _diffrn_reflns_theta_min 2.823 _diffrn_reflns_theta_max 30.046 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.445 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min -18 _reflns_limit_k_max 18 _reflns_limit_l_min -17 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.64 _oxford_diffrn_Wilson_scale 1.22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.44 _refine_diff_density_max 3.11 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 19327 _refine_ls_number_restraints 3 _refine_ls_number_parameters 765 _oxford_refine_ls_R_factor_ref 0.0341 _refine_ls_wR_factor_ref 0.0723 _refine_ls_goodness_of_fit_ref 0.9713 _refine_ls_shift/su_max 0.0065663 _refine_ls_shift/su_mean 0.0002846 # The values computed from all data _oxford_reflns_number_all 19327 _refine_ls_R_factor_all 0.0341 _refine_ls_wR_factor_all 0.0723 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 18844 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_gt 0.0714 _refine_ls_abs_structure_Flack -0.017(3) _refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.42P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ta1 Ta 0.00221(7) -0.00283(6) -0.00072(6) 0.0174 1.0000 Uani . . . . . . Co1 Co 0.27329(9) 0.15943(8) 0.10723(8) 0.0146 1.0000 Uani . . . . . . P1 P 0.25585(10) -0.00201(9) 0.14572(9) 0.0163 1.0000 Uani . . . . . . P2 P 0.17603(11) 0.22905(9) 0.16012(10) 0.0181 1.0000 Uani . . . . . . P3 P 0.18355(10) 0.12874(9) -0.07950(9) 0.0164 1.0000 Uani . . . . . . Na1 Na 0.78480(17) 0.46502(15) 0.36457(18) 0.0406 1.0000 Uani . . . . . . O1 O 0.7437(4) 0.6312(3) 0.3819(4) 0.0547 1.0000 Uani . . . . . . O2 O 0.7518(4) 0.4673(3) 0.1704(4) 0.0560 1.0000 Uani . . . . . . O3 O 0.8186(3) 0.2954(3) 0.3715(3) 0.0456 1.0000 Uani . . . . . . O4 O 0.7935(4) 0.4564(3) 0.5469(4) 0.0595 1.0000 Uani . . . . . . O5 O 1.0100(3) 0.5876(3) 0.4409(4) 0.0578 1.0000 Uani . . . . . . N1 N 0.0960(3) -0.0901(2) 0.0996(3) 0.0204 1.0000 Uani . . . . . . N2 N 0.0130(3) 0.1362(2) 0.0890(3) 0.0232 1.0000 Uani . . . . . . N3 N 0.0257(3) 0.0237(2) -0.1417(2) 0.0193 1.0000 Uani . . . . . . N4 N 0.4402(3) 0.2644(3) 0.1904(3) 0.0219 1.0000 Uani . . . . . . N5 N 0.5452(3) 0.3323(3) 0.2475(3) 0.0356 1.0000 Uani . . . . . . N6 N -0.1696(3) -0.1061(3) -0.0684(3) 0.0231 1.0000 Uani . . . . . . C1 C 0.3509(3) -0.0072(3) 0.3002(3) 0.0215 1.0000 Uani . . . . . . C2 C 0.3931(4) 0.0853(3) 0.3886(3) 0.0260 1.0000 Uani . . . . . . C3 C 0.4614(4) 0.0878(4) 0.5072(3) 0.0331 1.0000 Uani . . . . . . C4 C 0.4929(4) -0.0015(4) 0.5375(4) 0.0379 1.0000 Uani . . . . . . C5 C 0.4547(4) -0.0928(4) 0.4524(4) 0.0336 1.0000 Uani . . . . . . C6 C 0.3820(4) -0.0976(3) 0.3337(3) 0.0272 1.0000 Uani . . . . . . C7 C 0.2955(3) -0.0917(3) 0.0711(3) 0.0193 1.0000 Uani . . . . . . C8 C 0.4221(3) -0.0819(3) 0.1181(3) 0.0236 1.0000 Uani . . . . . . C9 C 0.4519(4) -0.1413(3) 0.0546(4) 0.0275 1.0000 Uani . . . . . . C10 C 0.3562(4) -0.2105(3) -0.0580(4) 0.0308 1.0000 Uani . . . . . . C11 C 0.2318(4) -0.2185(3) -0.1069(3) 0.0293 1.0000 Uani . . . . . . C12 C 0.2015(4) -0.1599(3) -0.0430(3) 0.0249 1.0000 Uani . . . . . . C13 C 0.0563(4) -0.1998(3) 0.1332(4) 0.0322 1.0000 Uani . . . . . . C14 C 0.0079(5) -0.1894(5) 0.2172(5) 0.0481 1.0000 Uani . . . . . . C15 C -0.0447(4) -0.3033(3) 0.0271(4) 0.0404 1.0000 Uani . . . . . . C16 C 0.2218(4) 0.2588(4) 0.3154(3) 0.0294 1.0000 Uani . . . . . . C17 C 0.1626(5) 0.1711(5) 0.3590(4) 0.0447 1.0000 Uani . . . . . . C18 C 0.2024(7) 0.1873(8) 0.4755(6) 0.0724 1.0000 Uani . . . . . . C19 C 0.3053(10) 0.2914(9) 0.5555(6) 0.0911 1.0000 Uani . . . . . . C20 C 0.3655(8) 0.3780(7) 0.5161(5) 0.0753 1.0000 Uani . . . . . . C21 C 0.3244(6) 0.3629(4) 0.3964(4) 0.0492 1.0000 Uani . . . . . . C22 C 0.1974(3) 0.3753(3) 0.1399(3) 0.0217 1.0000 Uani . . . . . . C23 C 0.1460(4) 0.4387(3) 0.1730(4) 0.0334 1.0000 Uani . . . . . . C24 C 0.1655(5) 0.5470(4) 0.1532(4) 0.0399 1.0000 Uani . . . . . . C25 C 0.2403(4) 0.5968(3) 0.1027(4) 0.0344 1.0000 Uani . . . . . . C26 C 0.2974(4) 0.5382(3) 0.0747(4) 0.0322 1.0000 Uani . . . . . . C27 C 0.2758(4) 0.4291(3) 0.0929(3) 0.0258 1.0000 Uani . . . . . . C28 C -0.0855(4) 0.1640(3) 0.0951(4) 0.0317 1.0000 Uani . . . . . . C29 C -0.1713(4) 0.0700(4) 0.1274(4) 0.0415 1.0000 Uani . . . . . . C30 C -0.1657(4) 0.1869(4) -0.0207(4) 0.0404 1.0000 Uani . . . . . . C31 C 0.1596(3) 0.2426(3) -0.1537(3) 0.0218 1.0000 Uani . . . . . . C32 C 0.2444(4) 0.3127(3) -0.1876(4) 0.0331 1.0000 Uani . . . . . . C33 C 0.2319(6) 0.4063(4) -0.2308(5) 0.0478 1.0000 Uani . . . . . . C34 C 0.1347(6) 0.4325(4) -0.2386(4) 0.0482 1.0000 Uani . . . . . . C35 C 0.0494(5) 0.3643(4) -0.2050(4) 0.0430 1.0000 Uani . . . . . . C36 C 0.0610(4) 0.2707(3) -0.1635(4) 0.0299 1.0000 Uani . . . . . . C37 C 0.2661(3) 0.0879(3) -0.1462(3) 0.0199 1.0000 Uani . . . . . . C38 C 0.2216(4) 0.0567(4) -0.2661(3) 0.0299 1.0000 Uani . . . . . . C39 C 0.2938(5) 0.0288(4) -0.3046(4) 0.0365 1.0000 Uani . . . . . . C40 C 0.4130(4) 0.0326(4) -0.2240(4) 0.0333 1.0000 Uani . . . . . . C41 C 0.4595(4) 0.0652(3) -0.1052(4) 0.0287 1.0000 Uani . . . . . . C42 C 0.3879(3) 0.0931(3) -0.0665(3) 0.0223 1.0000 Uani . . . . . . C43 C -0.0619(4) -0.0217(3) -0.2711(3) 0.0267 1.0000 Uani . . . . . . C44 C -0.1921(4) -0.0171(4) -0.3148(4) 0.0350 1.0000 Uani . . . . . . C45 C -0.0836(5) -0.1441(4) -0.3088(4) 0.0360 1.0000 Uani . . . . . . C46 C -0.3109(5) -0.1921(4) -0.1249(5) 0.0358 1.0000 Uani . . . . . . C47 C -0.3982(4) -0.1315(4) -0.1704(4) 0.0378 1.0000 Uani . . . . . . C48 C -0.3486(4) -0.2847(4) -0.2249(4) 0.0413 1.0000 Uani . . . . . . C49 C -0.3341(4) -0.2489(4) -0.0314(5) 0.0412 1.0000 Uani . . . . . . C50 C 0.8063(10) 0.7368(6) 0.3594(8) 0.0957 1.0000 Uani . . . . . . C57 C 0.7481(6) 0.3780(5) 0.1020(5) 0.0558 1.0000 Uani . . . . . . C58 C 0.7111(5) 0.1806(4) 0.3258(5) 0.0461 1.0000 Uani . . . . . . C59 C 0.7595(6) 0.1093(6) 0.4030(7) 0.0786 1.0000 Uani . . . . . . C60 C 0.8997(6) 0.1797(6) 0.4835(6) 0.0741 1.0000 Uani . . . . . . C61 C 0.9372(5) 0.2879(5) 0.4405(6) 0.0575 1.0000 Uani . . . . . . C62 C 0.7037(8) 0.3593(5) 0.5592(6) 0.0732 1.0000 Uani . . . . . . C63 C 0.7151(7) 0.3909(6) 0.6730(6) 0.0706 1.0000 Uani . . . . . . C65 C 0.8534(8) 0.5486(6) 0.6433(6) 0.0856 1.0000 Uani . . . . . . C69 C 1.0796(5) 0.5689(5) 0.3899(5) 0.0543 1.0000 Uani . . . . . . C510 C 0.6650(17) 0.7549(14) 0.2892(14) 0.074(4) 0.5000 Uiso . . . 1 1 . C511 C 0.7338(19) 0.7879(16) 0.3065(16) 0.086(4) 0.5000 Uiso . . . 1 2 . C520 C 0.5990(12) 0.7091(11) 0.3576(11) 0.056(3) 0.5000 Uiso . . . 1 1 . C521 C 0.6325(9) 0.7497(8) 0.3376(9) 0.0390(18) 0.5000 Uiso . . . 1 2 . C530 C 0.6112(15) 0.5954(13) 0.3716(13) 0.065(4) 0.5000 Uiso . . . 1 1 . C531 C 0.6337(12) 0.6378(11) 0.3692(11) 0.050(3) 0.5000 Uiso . . . 1 2 . C540 C 0.6685(9) 0.5130(8) 0.1183(8) 0.0355(17) 0.5000 Uiso . . . 1 2 . C541 C 0.6223(14) 0.4668(12) 0.0624(13) 0.058(3) 0.5000 Uiso . . . 1 1 . C550 C 0.5762(10) 0.4267(9) 0.0012(10) 0.044(2) 0.5000 Uiso . . . 1 2 . C551 C 0.6220(10) 0.4523(8) -0.0496(8) 0.043(2) 0.5000 Uiso . . . 1 1 . C560 C 0.6628(11) 0.3854(9) -0.0145(9) 0.046(2) 0.5000 Uiso . . . 1 2 . C561 C 0.6959(10) 0.3786(8) -0.0296(9) 0.041(2) 0.5000 Uiso . . . 1 1 . C640 C 0.7640(14) 0.5194(11) 0.6912(12) 0.064(3) 0.5000 Uiso . . . 1 1 . C641 C 0.8261(16) 0.5151(12) 0.7346(13) 0.071(3) 0.5000 Uiso . . . 1 2 . C660 C 1.1106(13) 0.6696(11) 0.5562(12) 0.056(3) 0.5000 Uiso . . . 1 1 . C661 C 1.0935(12) 0.7005(11) 0.5223(11) 0.051(3) 0.5000 Uiso . . . 1 2 . C670 C 1.2326(15) 0.6881(14) 0.5829(14) 0.074(4) 0.5000 Uiso . . . 1 1 . C671 C 1.2227(17) 0.7342(15) 0.5464(15) 0.086(4) 0.5000 Uiso . . . 1 2 . C680 C 1.2210(13) 0.6144(12) 0.5048(12) 0.061(3) 0.5000 Uiso . . . 1 1 . C681 C 1.2148(18) 0.6422(16) 0.4598(17) 0.091(5) 0.5000 Uiso . . . 1 2 . H21 H 0.3761 0.1481 0.3685 0.0307 1.0000 Uiso R . . . . . H31 H 0.4869 0.1506 0.5654 0.0401 1.0000 Uiso R . . . . . H41 H 0.5411 0.0020 0.6174 0.0452 1.0000 Uiso R . . . . . H51 H 0.4759 -0.1522 0.4730 0.0410 1.0000 Uiso R . . . . . H61 H 0.3545 -0.1617 0.2765 0.0324 1.0000 Uiso R . . . . . H81 H 0.4882 -0.0351 0.1945 0.0284 1.0000 Uiso R . . . . . H91 H 0.5382 -0.1329 0.0893 0.0333 1.0000 Uiso R . . . . . H101 H 0.3754 -0.2521 -0.0999 0.0374 1.0000 Uiso R . . . . . H111 H 0.1684 -0.2631 -0.1835 0.0351 1.0000 Uiso R . . . . . H121 H 0.1165 -0.1654 -0.0770 0.0302 1.0000 Uiso R . . . . . H131 H 0.1352 -0.2120 0.1761 0.0385 1.0000 Uiso R . . . . . H141 H -0.0645 -0.1709 0.1820 0.0718 1.0000 Uiso R . . . . . H142 H -0.0194 -0.2604 0.2390 0.0719 1.0000 Uiso R . . . . . H143 H 0.0780 -0.1282 0.2877 0.0717 1.0000 Uiso R . . . . . H151 H -0.0764 -0.3722 0.0505 0.0600 1.0000 Uiso R . . . . . H152 H -0.0063 -0.3178 -0.0164 0.0598 1.0000 Uiso R . . . . . H153 H -0.1188 -0.2906 -0.0251 0.0593 1.0000 Uiso R . . . . . H171 H 0.0927 0.0985 0.3049 0.0537 1.0000 Uiso R . . . . . H181 H 0.1595 0.1275 0.5012 0.0839 1.0000 Uiso R . . . . . H191 H 0.3309 0.3005 0.6350 0.1091 1.0000 Uiso R . . . . . H201 H 0.4349 0.4480 0.5692 0.0908 1.0000 Uiso R . . . . . H211 H 0.3652 0.4237 0.3705 0.0586 1.0000 Uiso R . . . . . H231 H 0.0988 0.4081 0.2100 0.0412 1.0000 Uiso R . . . . . H241 H 0.1280 0.5866 0.1734 0.0484 1.0000 Uiso R . . . . . H251 H 0.2528 0.6692 0.0898 0.0409 1.0000 Uiso R . . . . . H261 H 0.3513 0.5723 0.0423 0.0375 1.0000 Uiso R . . . . . H271 H 0.3136 0.3908 0.0715 0.0318 1.0000 Uiso R . . . . . H281 H -0.0376 0.2344 0.1592 0.0379 1.0000 Uiso R . . . . . H291 H -0.2386 0.0896 0.1223 0.0630 1.0000 Uiso R . . . . . H292 H -0.1207 0.0672 0.2073 0.0625 1.0000 Uiso R . . . . . H293 H -0.2110 -0.0025 0.0739 0.0626 1.0000 Uiso R . . . . . H301 H -0.2315 0.2019 -0.0181 0.0612 1.0000 Uiso R . . . . . H302 H -0.2088 0.1203 -0.0856 0.0605 1.0000 Uiso R . . . . . H303 H -0.1092 0.2529 -0.0330 0.0604 1.0000 Uiso R . . . . . H321 H 0.3101 0.2966 -0.1808 0.0399 1.0000 Uiso R . . . . . H331 H 0.2893 0.4527 -0.2552 0.0566 1.0000 Uiso R . . . . . H341 H 0.1285 0.4965 -0.2644 0.0582 1.0000 Uiso R . . . . . H351 H -0.0184 0.3810 -0.2107 0.0520 1.0000 Uiso R . . . . . H361 H 0.0023 0.2244 -0.1413 0.0355 1.0000 Uiso R . . . . . H381 H 0.1426 0.0552 -0.3219 0.0362 1.0000 Uiso R . . . . . H391 H 0.2634 0.0084 -0.3857 0.0439 1.0000 Uiso R . . . . . H401 H 0.4614 0.0139 -0.2501 0.0401 1.0000 Uiso R . . . . . H411 H 0.5399 0.0677 -0.0518 0.0342 1.0000 Uiso R . . . . . H421 H 0.4209 0.1154 0.0147 0.0268 1.0000 Uiso R . . . . . H431 H -0.0170 0.0271 -0.3072 0.0318 1.0000 Uiso R . . . . . H441 H -0.2373 -0.0598 -0.2770 0.0531 1.0000 Uiso R . . . . . H442 H -0.1781 0.0621 -0.2980 0.0525 1.0000 Uiso R . . . . . H443 H -0.2469 -0.0498 -0.3990 0.0531 1.0000 Uiso R . . . . . H451 H 0.0009 -0.1415 -0.2862 0.0546 1.0000 Uiso R . . . . . H452 H -0.1409 -0.1746 -0.3923 0.0548 1.0000 Uiso R . . . . . H453 H -0.1222 -0.1938 -0.2705 0.0548 1.0000 Uiso R . . . . . H471 H -0.4892 -0.1866 -0.2056 0.0568 1.0000 Uiso R . . . . . H472 H -0.3757 -0.0735 -0.1046 0.0567 1.0000 Uiso R . . . . . H473 H -0.3836 -0.0949 -0.2255 0.0572 1.0000 Uiso R . . . . . H481 H -0.2884 -0.3165 -0.1990 0.0629 1.0000 Uiso R . . . . . H482 H -0.3469 -0.2540 -0.2904 0.0628 1.0000 Uiso R . . . . . H483 H -0.4363 -0.3471 -0.2538 0.0630 1.0000 Uiso R . . . . . H491 H -0.2889 -0.2956 -0.0082 0.0624 1.0000 Uiso R . . . . . H492 H -0.2999 -0.1890 0.0363 0.0620 1.0000 Uiso R . . . . . H493 H -0.4271 -0.2981 -0.0621 0.0619 1.0000 Uiso R . . . . . H501 H 0.8766 0.7955 0.4317 0.1159 1.0000 Uiso R . . . . . H502 H 0.8375 0.7244 0.3094 0.1162 1.0000 Uiso R . . . . . H571 H 0.8329 0.3940 0.1158 0.0676 0.5000 Uiso R . . 1 1 . H572 H 0.7100 0.3049 0.1155 0.0676 0.5000 Uiso R . . 1 1 . H573 H 0.8348 0.3859 0.1357 0.0676 0.5000 Uiso R . . 1 2 . H574 H 0.6925 0.3057 0.1051 0.0676 0.5000 Uiso R . . 1 2 . H581 H 0.6386 0.1841 0.3274 0.0551 1.0000 Uiso R . . . . . H582 H 0.6841 0.1511 0.2445 0.0552 1.0000 Uiso R . . . . . H591 H 0.7154 0.0866 0.4471 0.0926 1.0000 Uiso R . . . . . H592 H 0.7436 0.0407 0.3557 0.0928 1.0000 Uiso R . . . . . H601 H 0.9463 0.1370 0.4815 0.0905 1.0000 Uiso R . . . . . H602 H 0.9164 0.1996 0.5619 0.0903 1.0000 Uiso R . . . . . H611 H 0.9958 0.3559 0.5049 0.0689 1.0000 Uiso R . . . . . H612 H 0.9763 0.2826 0.3946 0.0694 1.0000 Uiso R . . . . . H621 H 0.6150 0.3384 0.4946 0.0890 1.0000 Uiso R . . . . . H622 H 0.7227 0.2953 0.5553 0.0895 1.0000 Uiso R . . . . . H631 H 0.6291 0.3689 0.6637 0.0853 1.0000 Uiso R . . . . . H632 H 0.7579 0.3525 0.7291 0.0852 1.0000 Uiso R . . . . . H651 H 0.9472 0.5655 0.6917 0.1015 1.0000 Uiso R . . . . . H652 H 0.8503 0.6159 0.6171 0.1009 1.0000 Uiso R . . . . . H691 H 1.0821 0.6133 0.3347 0.0670 0.5000 Uiso R . . 1 1 . H692 H 1.0428 0.4894 0.3529 0.0670 0.5000 Uiso R . . 1 1 . H693 H 1.0489 0.5851 0.3150 0.0670 0.5000 Uiso R . . 1 2 . H694 H 1.0633 0.4902 0.3806 0.0670 0.5000 Uiso R . . 1 2 . H5101 H 0.6862 0.8342 0.2927 0.0911 0.5000 Uiso R . . 1 1 . H5102 H 0.6110 0.7111 0.2093 0.0911 0.5000 Uiso R . . 1 1 . H5111 H 0.7850 0.8695 0.3361 0.1043 0.5000 Uiso R . . 1 2 . H5112 H 0.6962 0.7675 0.2235 0.1043 0.5000 Uiso R . . 1 2 . H5201 H 0.6454 0.7608 0.4332 0.0692 0.5000 Uiso R . . 1 1 . H5202 H 0.5104 0.6971 0.3172 0.0692 0.5000 Uiso R . . 1 1 . H5211 H 0.6534 0.8044 0.4021 0.0482 0.5000 Uiso R . . 1 2 . H5212 H 0.5492 0.7339 0.2724 0.0482 0.5000 Uiso R . . 1 2 . H5301 H 0.6082 0.5724 0.4380 0.0849 0.5000 Uiso R . . 1 1 . H5302 H 0.5438 0.5347 0.3024 0.0849 0.5000 Uiso R . . 1 1 . H5311 H 0.6367 0.6378 0.4423 0.0568 0.5000 Uiso R . . 1 2 . H5312 H 0.5566 0.5726 0.3101 0.0568 0.5000 Uiso R . . 1 2 . H5401 H 0.7118 0.5879 0.1108 0.0440 0.5000 Uiso R . . 1 2 . H5402 H 0.6256 0.5166 0.1598 0.0440 0.5000 Uiso R . . 1 2 . H5411 H 0.6221 0.5384 0.0796 0.0720 0.5000 Uiso R . . 1 1 . H5412 H 0.5461 0.4051 0.0544 0.0720 0.5000 Uiso R . . 1 1 . H5501 H 0.5403 0.4612 -0.0595 0.0549 0.5000 Uiso R . . 1 2 . H5502 H 0.5068 0.3650 0.0030 0.0549 0.5000 Uiso R . . 1 2 . H5511 H 0.6666 0.5247 -0.0607 0.0525 0.5000 Uiso R . . 1 1 . H5512 H 0.5347 0.4124 -0.1149 0.0525 0.5000 Uiso R . . 1 1 . H5601 H 0.7135 0.4390 -0.0409 0.0556 0.5000 Uiso R . . 1 2 . H5602 H 0.6118 0.3117 -0.0695 0.0556 0.5000 Uiso R . . 1 2 . H5611 H 0.7667 0.4136 -0.0433 0.0526 0.5000 Uiso R . . 1 1 . H5612 H 0.6384 0.3025 -0.0800 0.0526 0.5000 Uiso R . . 1 1 . H6401 H 0.8111 0.5574 0.7726 0.0759 0.5000 Uiso R . . 1 1 . H6402 H 0.6944 0.5390 0.6497 0.0759 0.5000 Uiso R . . 1 1 . H6411 H 0.9011 0.5166 0.8005 0.0850 0.5000 Uiso R . . 1 2 . H6412 H 0.7983 0.5637 0.7593 0.0850 0.5000 Uiso R . . 1 2 . H6601 H 1.1046 0.7402 0.5549 0.0637 0.5000 Uiso R . . 1 1 . H6602 H 1.0940 0.6385 0.6143 0.0637 0.5000 Uiso R . . 1 1 . H6611 H 1.0921 0.6972 0.5933 0.0587 0.5000 Uiso R . . 1 2 . H6612 H 1.0634 0.7541 0.4888 0.0587 0.5000 Uiso R . . 1 2 . H6701 H 1.2786 0.7642 0.5793 0.0872 0.5000 Uiso R . . 1 1 . H6702 H 1.2789 0.6802 0.6600 0.0872 0.5000 Uiso R . . 1 1 . H6711 H 1.2555 0.8075 0.5311 0.1031 0.5000 Uiso R . . 1 2 . H6712 H 1.2789 0.7386 0.6261 0.1031 0.5000 Uiso R . . 1 2 . H6801 H 1.2875 0.6494 0.4859 0.0721 0.5000 Uiso R . . 1 1 . H6802 H 1.2287 0.5513 0.5362 0.0721 0.5000 Uiso R . . 1 1 . H6811 H 1.2514 0.6760 0.4139 0.1052 0.5000 Uiso R . . 1 2 . H6812 H 1.2587 0.6003 0.5029 0.1052 0.5000 Uiso R . . 1 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 Ta1 0.01536(5) 0.01918(6) 0.02431(6) 0.01130(4) 0.01157(5) 0.01160(4) Co1 0.0160(3) 0.0156(2) 0.0170(2) 0.00713(19) 0.0095(2) 0.0102(2) P1 0.0165(4) 0.0166(3) 0.0196(4) 0.0084(3) 0.0092(3) 0.0107(3) P2 0.0224(4) 0.0198(4) 0.0217(4) 0.0101(3) 0.0143(3) 0.0143(3) P3 0.0174(4) 0.0190(4) 0.0190(4) 0.0086(3) 0.0107(3) 0.0118(3) Na1 0.0275(8) 0.0264(8) 0.0606(11) 0.0014(7) 0.0207(8) 0.0087(7) O1 0.064(2) 0.050(2) 0.082(3) 0.0315(19) 0.050(2) 0.0377(18) O2 0.061(2) 0.0406(18) 0.086(3) 0.0229(18) 0.050(2) 0.0264(17) O3 0.0334(16) 0.0305(15) 0.0476(18) 0.0001(13) 0.0014(14) 0.0161(13) O4 0.064(2) 0.0443(19) 0.068(2) 0.0071(17) 0.041(2) 0.0155(18) O5 0.0338(17) 0.053(2) 0.065(2) -0.0154(17) 0.0261(17) 0.0023(15) N1 0.0168(12) 0.0181(12) 0.0273(14) 0.0111(11) 0.0099(11) 0.0099(11) N2 0.0244(14) 0.0227(13) 0.0343(16) 0.0123(12) 0.0193(13) 0.0158(12) N3 0.0143(12) 0.0244(13) 0.0193(13) 0.0085(11) 0.0068(11) 0.0111(11) N4 0.0226(14) 0.0244(14) 0.0249(14) 0.0097(12) 0.0134(12) 0.0146(12) N5 0.0228(16) 0.0304(17) 0.044(2) 0.0099(15) 0.0116(15) 0.0100(14) N6 0.0209(14) 0.0251(14) 0.0321(16) 0.0156(12) 0.0153(12) 0.0156(12) C1 0.0191(15) 0.0259(16) 0.0248(16) 0.0118(13) 0.0122(13) 0.0135(13) C2 0.0276(17) 0.0380(19) 0.0218(16) 0.0133(14) 0.0132(14) 0.0224(16) C3 0.036(2) 0.046(2) 0.0242(18) 0.0107(16) 0.0153(16) 0.0256(19) C4 0.041(2) 0.065(3) 0.0279(19) 0.0249(19) 0.0196(18) 0.039(2) C5 0.041(2) 0.047(2) 0.033(2) 0.0262(18) 0.0210(18) 0.034(2) C6 0.0304(18) 0.0344(18) 0.0329(18) 0.0211(15) 0.0202(16) 0.0234(16) C7 0.0202(15) 0.0179(14) 0.0252(16) 0.0095(12) 0.0126(13) 0.0119(12) C8 0.0221(16) 0.0209(15) 0.0298(17) 0.0096(13) 0.0134(14) 0.0111(13) C9 0.0265(18) 0.0282(18) 0.040(2) 0.0148(15) 0.0212(16) 0.0180(15) C10 0.045(2) 0.0282(18) 0.039(2) 0.0139(16) 0.0294(19) 0.0236(17) C11 0.0348(19) 0.0263(17) 0.0256(17) 0.0027(14) 0.0142(16) 0.0148(15) C12 0.0245(16) 0.0218(15) 0.0247(16) 0.0044(13) 0.0098(14) 0.0109(13) C13 0.0216(16) 0.0275(18) 0.052(2) 0.0249(17) 0.0194(17) 0.0127(14) C14 0.043(2) 0.055(3) 0.062(3) 0.042(3) 0.034(2) 0.025(2) C15 0.0244(18) 0.0187(17) 0.070(3) 0.0182(18) 0.018(2) 0.0093(15) C16 0.043(2) 0.044(2) 0.0271(17) 0.0180(16) 0.0243(17) 0.0354(19) C17 0.051(3) 0.079(4) 0.046(3) 0.044(3) 0.038(2) 0.049(3) C18 0.094(5) 0.150(7) 0.056(3) 0.073(4) 0.062(4) 0.099(5) C19 0.152(7) 0.178(8) 0.039(3) 0.061(5) 0.062(5) 0.143(7) C20 0.108(5) 0.094(5) 0.029(2) 0.006(3) 0.016(3) 0.075(5) C21 0.072(3) 0.052(3) 0.028(2) 0.0051(19) 0.018(2) 0.043(3) C22 0.0258(16) 0.0187(14) 0.0242(16) 0.0083(12) 0.0120(14) 0.0140(13) C23 0.045(2) 0.0312(19) 0.048(2) 0.0190(17) 0.032(2) 0.0275(18) C24 0.049(2) 0.030(2) 0.060(3) 0.0180(19) 0.033(2) 0.0289(19) C25 0.046(2) 0.0214(17) 0.040(2) 0.0114(15) 0.0223(19) 0.0188(17) C26 0.045(2) 0.0217(17) 0.036(2) 0.0125(15) 0.0250(19) 0.0155(16) C27 0.0337(19) 0.0200(15) 0.0297(18) 0.0086(13) 0.0184(16) 0.0148(14) C28 0.0269(18) 0.0333(19) 0.048(2) 0.0107(17) 0.0251(18) 0.0190(16) C29 0.037(2) 0.051(3) 0.056(3) 0.019(2) 0.036(2) 0.023(2) C30 0.032(2) 0.045(2) 0.061(3) 0.022(2) 0.028(2) 0.0275(19) C31 0.0273(16) 0.0220(15) 0.0204(15) 0.0084(12) 0.0117(13) 0.0153(14) C32 0.044(2) 0.0311(19) 0.045(2) 0.0214(17) 0.032(2) 0.0234(18) C33 0.074(3) 0.037(2) 0.066(3) 0.036(2) 0.052(3) 0.034(2) C34 0.077(4) 0.041(2) 0.052(3) 0.032(2) 0.037(3) 0.044(3) C35 0.052(3) 0.044(2) 0.051(3) 0.024(2) 0.025(2) 0.039(2) C36 0.0313(19) 0.0304(19) 0.039(2) 0.0163(16) 0.0189(17) 0.0226(16) C37 0.0229(15) 0.0198(14) 0.0246(16) 0.0090(12) 0.0145(13) 0.0135(13) C38 0.0341(19) 0.045(2) 0.0244(17) 0.0140(15) 0.0170(16) 0.0277(18) C39 0.050(2) 0.052(2) 0.0297(19) 0.0169(18) 0.0263(19) 0.035(2) C40 0.044(2) 0.040(2) 0.047(2) 0.0226(18) 0.035(2) 0.0317(19) C41 0.0300(19) 0.0344(19) 0.041(2) 0.0205(17) 0.0250(17) 0.0234(17) C42 0.0234(16) 0.0217(15) 0.0275(17) 0.0079(13) 0.0153(14) 0.0124(13) C43 0.0226(16) 0.0317(18) 0.0211(16) 0.0064(14) 0.0067(14) 0.0138(14) C44 0.0263(18) 0.044(2) 0.0302(19) 0.0157(17) 0.0082(16) 0.0189(17) C45 0.035(2) 0.030(2) 0.027(2) -0.0012(16) 0.0065(17) 0.0125(18) C46 0.015(2) 0.028(2) 0.058(3) 0.015(2) 0.014(2) 0.0085(19) C47 0.0186(17) 0.041(2) 0.058(3) 0.027(2) 0.0181(18) 0.0185(16) C48 0.0203(18) 0.032(2) 0.057(3) 0.0051(19) 0.0117(18) 0.0090(16) C49 0.0240(18) 0.043(2) 0.065(3) 0.033(2) 0.025(2) 0.0191(18) C50 0.180(9) 0.056(4) 0.133(7) 0.052(4) 0.126(7) 0.068(5) C57 0.057(3) 0.062(3) 0.053(3) 0.015(3) 0.024(3) 0.037(3) C58 0.041(2) 0.032(2) 0.053(3) 0.0070(19) 0.015(2) 0.0161(19) C59 0.059(4) 0.056(3) 0.095(5) 0.035(3) 0.017(4) 0.028(3) C60 0.045(3) 0.076(4) 0.070(4) 0.042(3) 0.010(3) 0.021(3) C61 0.037(3) 0.063(3) 0.060(3) 0.031(3) 0.016(2) 0.022(2) C62 0.100(5) 0.043(3) 0.073(4) 0.005(3) 0.059(4) 0.014(3) C63 0.061(4) 0.088(5) 0.067(4) 0.016(3) 0.037(3) 0.033(3) C65 0.088(5) 0.048(3) 0.057(4) -0.009(3) 0.014(4) 0.004(3) C69 0.051(3) 0.059(3) 0.066(3) 0.015(3) 0.040(3) 0.024(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.19515(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ta1 . Co1 . 2.8538(5) yes Ta1 . P1 . 2.9255(8) yes Ta1 . P2 . 2.9251(8) yes Ta1 . P3 . 2.9475(8) yes Ta1 . N1 . 2.047(3) yes Ta1 . N2 . 2.047(3) yes Ta1 . N3 . 2.041(3) yes Ta1 . N6 . 1.811(3) yes Co1 . P1 . 2.1240(9) yes Co1 . P2 . 2.1219(9) yes Co1 . P3 . 2.1339(9) yes Co1 . N4 . 1.769(3) yes P1 . N1 . 1.697(3) yes P1 . C1 . 1.859(3) yes P1 . C7 . 1.852(3) yes P2 . N2 . 1.697(3) yes P2 . C16 . 1.837(4) yes P2 . C22 . 1.856(3) yes P3 . N3 . 1.702(3) yes P3 . C31 . 1.848(3) yes P3 . C37 . 1.856(3) yes Na1 . O1 . 2.438(4) yes Na1 . O2 . 2.406(5) yes Na1 . O3 . 2.401(3) yes Na1 . O4 . 2.371(4) yes Na1 . O5 . 2.358(4) yes Na1 . N5 . 2.484(4) yes O1 . C50 . 1.416(7) yes O1 . C530 . 1.517(15) yes O1 . C50 . 1.416(7) yes O1 . C531 . 1.381(12) yes O2 . C57 . 1.418(6) yes O2 . C541 . 1.620(14) yes O2 . C57 . 1.418(6) yes O2 . C540 . 1.349(9) yes O3 . C58 . 1.438(5) yes O3 . C61 . 1.418(6) yes O4 . C62 . 1.415(7) yes O4 . C65 . 1.389(7) yes O5 . C69 . 1.422(6) yes O5 . C660 . 1.464(13) yes O5 . C69 . 1.422(6) yes O5 . C661 . 1.439(12) yes N1 . C13 . 1.473(4) yes N2 . C28 . 1.478(4) yes N3 . C43 . 1.481(4) yes N4 . N5 . 1.124(4) yes N6 . C46 . 1.492(5) yes C1 . C2 . 1.385(5) yes C1 . C6 . 1.404(4) yes C2 . C3 . 1.394(5) yes C2 . H21 . 0.940 no C3 . C4 . 1.384(6) yes C3 . H31 . 0.939 no C4 . C5 . 1.364(6) yes C4 . H41 . 0.937 no C5 . C6 . 1.396(5) yes C5 . H51 . 0.923 no C6 . H61 . 0.933 no C7 . C8 . 1.398(4) yes C7 . C12 . 1.389(5) yes C8 . C9 . 1.388(5) yes C8 . H81 . 0.939 no C9 . C10 . 1.382(6) yes C9 . H91 . 0.943 no C10 . C11 . 1.380(6) yes C10 . H101 . 0.932 no C11 . C12 . 1.389(5) yes C11 . H111 . 0.928 no C12 . H121 . 0.942 no C13 . C14 . 1.527(7) yes C13 . C15 . 1.518(6) yes C13 . H131 . 0.989 no C14 . H141 . 0.961 no C14 . H142 . 0.957 no C14 . H143 . 0.967 no C15 . H151 . 0.956 no C15 . H152 . 0.967 no C15 . H153 . 0.967 no C16 . C17 . 1.408(6) yes C16 . C21 . 1.391(7) yes C17 . C18 . 1.362(7) yes C17 . H171 . 0.955 no C18 . C19 . 1.388(12) yes C18 . H181 . 0.938 no C19 . C20 . 1.366(12) yes C19 . H191 . 0.934 no C20 . C21 . 1.398(7) yes C20 . H201 . 0.931 no C21 . H211 . 0.936 no C22 . C23 . 1.403(5) yes C22 . C27 . 1.394(5) yes C23 . C24 . 1.385(5) yes C23 . H231 . 0.930 no C24 . C25 . 1.386(6) yes C24 . H241 . 0.933 no C25 . C26 . 1.384(6) yes C25 . H251 . 0.926 no C26 . C27 . 1.385(5) yes C26 . H261 . 0.953 no C27 . H271 . 0.931 no C28 . C29 . 1.520(6) yes C28 . C30 . 1.523(6) yes C28 . H281 . 0.982 no C29 . H291 . 0.967 no C29 . H292 . 0.965 no C29 . H293 . 0.947 no C30 . H301 . 0.953 no C30 . H302 . 0.966 no C30 . H303 . 0.960 no C31 . C32 . 1.387(5) yes C31 . C36 . 1.402(5) yes C32 . C33 . 1.393(5) yes C32 . H321 . 0.913 no C33 . C34 . 1.378(7) yes C33 . H331 . 0.948 no C34 . C35 . 1.380(7) yes C34 . H341 . 0.926 no C35 . C36 . 1.382(5) yes C35 . H351 . 0.947 no C36 . H361 . 0.939 no C37 . C38 . 1.396(5) yes C37 . C42 . 1.402(5) yes C38 . C39 . 1.390(5) yes C38 . H381 . 0.933 no C39 . C40 . 1.387(6) yes C39 . H391 . 0.944 no C40 . C41 . 1.379(6) yes C40 . H401 . 0.934 no C41 . C42 . 1.387(5) yes C41 . H411 . 0.932 no C42 . H421 . 0.939 no C43 . C44 . 1.527(5) yes C43 . C45 . 1.525(5) yes C43 . H431 . 0.975 no C44 . H441 . 0.964 no C44 . H442 . 0.970 no C44 . H443 . 0.966 no C45 . H451 . 0.970 no C45 . H452 . 0.958 no C45 . H453 . 0.961 no C46 . C47 . 1.530(6) yes C46 . C48 . 1.509(8) yes C46 . C49 . 1.546(7) yes C47 . H471 . 0.961 no C47 . H472 . 0.981 no C47 . H473 . 0.934 no C48 . H481 . 0.949 no C48 . H482 . 0.972 no C48 . H483 . 0.973 no C49 . H491 . 0.960 no C49 . H492 . 0.962 no C49 . H493 . 0.973 no C50 . C510 . 1.736(19) yes C50 . H501 . 0.967 no C50 . H502 . 0.953 no C50 . C511 . 1.308(18) yes C50 . H501 . 0.967 no C50 . H502 . 0.953 no C57 . C561 . 1.554(11) yes C57 . H571 . 0.950 no C57 . H572 . 0.950 no C57 . C560 . 1.459(12) yes C57 . H573 . 0.950 no C57 . H574 . 0.950 no C58 . C59 . 1.488(7) yes C58 . H581 . 0.960 no C58 . H582 . 0.975 no C59 . C60 . 1.452(8) yes C59 . H591 . 0.966 no C59 . H592 . 0.964 no C60 . C61 . 1.519(8) yes C60 . H601 . 0.968 no C60 . H602 . 0.961 no C61 . H611 . 0.957 no C61 . H612 . 0.964 no C62 . C63 . 1.471(9) yes C62 . H621 . 0.977 no C62 . H622 . 0.958 no C63 . C640 . 1.500(15) yes C63 . H631 . 0.972 no C63 . H632 . 0.982 no C63 . C641 . 1.535(16) yes C63 . H631 . 0.972 no C63 . H632 . 0.982 no C65 . C640 . 1.487(15) yes C65 . H651 . 0.994 no C65 . H652 . 0.959 no C65 . C641 . 1.441(16) yes C65 . H651 . 0.994 no C65 . H652 . 0.959 no C69 . C680 . 1.592(14) yes C69 . H691 . 0.950 no C69 . H692 . 0.950 no C69 . C681 . 1.401(18) yes C69 . H693 . 0.950 no C69 . H694 . 0.950 no C510 . C520 . 1.50(2) yes C510 . H5101 . 0.950 no C510 . H5102 . 0.950 no C511 . C521 . 1.45(2) yes C511 . H5111 . 0.950 no C511 . H5112 . 0.950 no C520 . C530 . 1.552(19) yes C520 . H5201 . 0.950 no C520 . H5202 . 0.950 no C521 . C531 . 1.529(16) yes C521 . H5211 . 0.950 no C521 . H5212 . 0.950 no C530 . H5301 . 0.950 no C530 . H5302 . 0.950 no C531 . H5311 . 0.950 no C531 . H5312 . 0.950 no C540 . C550 . 1.492(13) yes C540 . H5401 . 0.950 no C540 . H5402 . 0.950 no C541 . C551 . 1.484(17) yes C541 . H5411 . 0.950 no C541 . H5412 . 0.950 no C550 . C560 . 1.495(15) yes C550 . H5501 . 0.950 no C550 . H5502 . 0.950 no C551 . C561 . 1.542(14) yes C551 . H5511 . 0.950 no C551 . H5512 . 0.950 no C560 . H5601 . 0.950 no C560 . H5602 . 0.950 no C561 . H5611 . 0.950 no C561 . H5612 . 0.950 no C640 . H6401 . 0.950 no C640 . H6402 . 0.950 no C641 . H6411 . 0.950 no C641 . H6412 . 0.950 no C660 . C670 . 1.354(19) yes C660 . H6601 . 0.950 no C660 . H6602 . 0.950 no C661 . C671 . 1.41(2) yes C661 . H6611 . 0.950 no C661 . H6612 . 0.950 no C670 . C680 . 1.297(19) yes C670 . H6701 . 0.950 no C670 . H6702 . 0.950 no C671 . C681 . 1.57(2) yes C671 . H6711 . 0.950 no C671 . H6712 . 0.950 no C680 . H6801 . 0.950 no C680 . H6802 . 0.950 no C681 . H6811 . 0.950 no C681 . H6812 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Ta1 . P2 . 74.73(2) yes P1 . Ta1 . P3 . 71.06(2) yes P2 . Ta1 . P3 . 71.75(2) yes Co1 . Ta1 . N1 . 77.08(8) yes P2 . Ta1 . N1 . 98.70(8) yes P3 . Ta1 . N1 . 101.88(8) yes Co1 . Ta1 . N2 . 77.49(8) yes P1 . Ta1 . N2 . 104.80(8) yes P3 . Ta1 . N2 . 97.25(8) yes N1 . Ta1 . N2 . 116.35(12) yes Co1 . Ta1 . N3 . 77.13(8) yes P1 . Ta1 . N3 . 95.44(7) yes P2 . Ta1 . N3 . 100.89(8) yes N1 . Ta1 . N3 . 115.07(11) yes Co1 . Ta1 . N6 . 179.65(9) yes P1 . Ta1 . N6 . 136.65(9) yes P2 . Ta1 . N6 . 136.88(10) yes P3 . Ta1 . N6 . 137.20(10) yes N1 . Ta1 . N6 . 102.64(11) yes N2 . Ta1 . N3 . 114.36(11) yes N2 . Ta1 . N6 . 102.47(12) yes N3 . Ta1 . N6 . 103.19(12) yes Ta1 . Co1 . P1 . 70.25(3) yes Ta1 . Co1 . P2 . 70.26(3) yes P1 . Co1 . P2 . 113.49(4) yes Ta1 . Co1 . P3 . 70.78(3) yes P1 . Co1 . P3 . 106.56(4) yes P2 . Co1 . P3 . 107.94(4) yes Ta1 . Co1 . N4 . 172.56(10) yes P1 . Co1 . N4 . 109.33(10) yes P2 . Co1 . N4 . 103.77(10) yes P3 . Co1 . N4 . 115.96(10) yes Co1 . P1 . N1 . 108.89(9) yes Ta1 . P1 . C1 . 135.57(10) yes Co1 . P1 . C1 . 119.89(11) yes N1 . P1 . C1 . 105.55(14) yes Ta1 . P1 . C7 . 115.21(11) yes Co1 . P1 . C7 . 118.28(10) yes N1 . P1 . C7 . 102.26(14) yes C1 . P1 . C7 . 99.96(14) yes Co1 . P2 . N2 . 109.66(10) yes Ta1 . P2 . C16 . 122.76(13) yes Co1 . P2 . C16 . 119.95(11) yes N2 . P2 . C16 . 103.34(17) yes Ta1 . P2 . C22 . 132.71(11) yes Co1 . P2 . C22 . 116.04(11) yes N2 . P2 . C22 . 109.01(14) yes C16 . P2 . C22 . 97.53(16) yes Co1 . P3 . N3 . 108.18(10) yes Ta1 . P3 . C31 . 119.78(11) yes Co1 . P3 . C31 . 121.28(11) yes N3 . P3 . C31 . 101.26(14) yes Ta1 . P3 . C37 . 133.17(10) yes Co1 . P3 . C37 . 116.58(11) yes N3 . P3 . C37 . 109.12(14) yes C31 . P3 . C37 . 98.99(14) yes O1 . Na1 . O2 . 93.22(14) yes O1 . Na1 . O3 . 171.21(16) yes O2 . Na1 . O3 . 95.10(13) yes O1 . Na1 . O4 . 84.73(14) yes O2 . Na1 . O4 . 174.04(15) yes O3 . Na1 . O4 . 86.71(15) yes O1 . Na1 . O5 . 91.10(14) yes O2 . Na1 . O5 . 88.00(14) yes O3 . Na1 . O5 . 92.02(14) yes O4 . Na1 . O5 . 97.62(15) yes O1 . Na1 . N5 . 91.35(13) yes O2 . Na1 . N5 . 81.25(14) yes O3 . Na1 . N5 . 87.13(12) yes O4 . Na1 . N5 . 93.18(14) yes O5 . Na1 . N5 . 169.09(15) yes Na1 . O1 . C50 . 123.8(4) yes Na1 . O1 . C530 . 111.5(6) yes C50 . O1 . C530 . 120.7(7) yes Na1 . O1 . C50 . 123.8(4) yes Na1 . O1 . C531 . 131.1(6) yes C50 . O1 . C531 . 100.8(7) yes Na1 . O2 . C57 . 121.6(3) yes Na1 . O2 . C541 . 123.6(5) yes C57 . O2 . C541 . 93.7(6) yes Na1 . O2 . C57 . 121.6(3) yes Na1 . O2 . C540 . 108.1(4) yes C57 . O2 . C540 . 119.8(6) yes Na1 . O3 . C58 . 122.1(3) yes Na1 . O3 . C61 . 128.1(3) yes C58 . O3 . C61 . 108.2(4) yes Na1 . O4 . C62 . 122.0(3) yes Na1 . O4 . C65 . 127.3(4) yes C62 . O4 . C65 . 108.1(5) yes Na1 . O5 . C69 . 121.8(3) yes Na1 . O5 . C660 . 130.4(5) yes C69 . O5 . C660 . 105.8(6) yes Na1 . O5 . C69 . 121.8(3) yes Na1 . O5 . C661 . 130.0(5) yes C69 . O5 . C661 . 107.0(6) yes P1 . N1 . Ta1 . 102.38(13) yes P1 . N1 . C13 . 121.4(2) yes Ta1 . N1 . C13 . 136.2(2) yes P2 . N2 . Ta1 . 102.35(13) yes P2 . N2 . C28 . 123.6(2) yes Ta1 . N2 . C28 . 134.0(2) yes P3 . N3 . Ta1 . 103.53(13) yes P3 . N3 . C43 . 121.6(2) yes Ta1 . N3 . C43 . 134.7(2) yes Co1 . N4 . N5 . 176.7(3) yes Na1 . N5 . N4 . 172.8(3) yes Ta1 . N6 . C46 . 179.3(3) yes P1 . C1 . C2 . 117.1(2) yes P1 . C1 . C6 . 125.1(3) yes C2 . C1 . C6 . 117.9(3) yes C1 . C2 . C3 . 121.5(3) yes C1 . C2 . H21 . 119.5 no C3 . C2 . H21 . 119.0 no C2 . C3 . C4 . 119.3(4) yes C2 . C3 . H31 . 119.8 no C4 . C3 . H31 . 120.9 no C3 . C4 . C5 . 120.5(4) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 120.6 no C4 . C5 . C6 . 120.2(4) yes C4 . C5 . H51 . 120.3 no C6 . C5 . H51 . 119.5 no C1 . C6 . C5 . 120.5(4) yes C1 . C6 . H61 . 120.2 no C5 . C6 . H61 . 119.2 no P1 . C7 . C8 . 122.7(3) yes P1 . C7 . C12 . 119.1(2) yes C8 . C7 . C12 . 117.6(3) yes C7 . C8 . C9 . 121.3(3) yes C7 . C8 . H81 . 119.6 no C9 . C8 . H81 . 119.0 no C8 . C9 . C10 . 120.0(3) yes C8 . C9 . H91 . 119.0 no C10 . C9 . H91 . 121.0 no C9 . C10 . C11 . 119.3(3) yes C9 . C10 . H101 . 120.2 no C11 . C10 . H101 . 120.5 no C10 . C11 . C12 . 120.6(3) yes C10 . C11 . H111 . 119.2 no C12 . C11 . H111 . 120.2 no C7 . C12 . C11 . 121.0(3) yes C7 . C12 . H121 . 118.8 no C11 . C12 . H121 . 120.2 no N1 . C13 . C14 . 109.2(3) yes N1 . C13 . C15 . 112.5(3) yes C14 . C13 . C15 . 112.0(3) yes N1 . C13 . H131 . 107.8 no C14 . C13 . H131 . 107.9 no C15 . C13 . H131 . 107.2 no C13 . C14 . H141 . 111.3 no C13 . C14 . H142 . 110.1 no H141 . C14 . H142 . 109.0 no C13 . C14 . H143 . 109.8 no H141 . C14 . H143 . 107.8 no H142 . C14 . H143 . 108.7 no C13 . C15 . H151 . 111.2 no C13 . C15 . H152 . 110.8 no H151 . C15 . H152 . 106.4 no C13 . C15 . H153 . 110.9 no H151 . C15 . H153 . 108.6 no H152 . C15 . H153 . 108.8 no P2 . C16 . C17 . 120.3(4) yes P2 . C16 . C21 . 122.0(3) yes C17 . C16 . C21 . 117.4(4) yes C16 . C17 . C18 . 121.7(6) yes C16 . C17 . H171 . 118.7 no C18 . C17 . H171 . 119.6 no C17 . C18 . C19 . 120.3(6) yes C17 . C18 . H181 . 119.4 no C19 . C18 . H181 . 120.3 no C18 . C19 . C20 . 119.4(5) yes C18 . C19 . H191 . 118.7 no C20 . C19 . H191 . 121.8 no C19 . C20 . C21 . 120.8(7) yes C19 . C20 . H201 . 119.9 no C21 . C20 . H201 . 119.3 no C20 . C21 . C16 . 120.4(6) yes C20 . C21 . H211 . 119.8 no C16 . C21 . H211 . 119.8 no P2 . C22 . C23 . 125.3(3) yes P2 . C22 . C27 . 117.6(2) yes C23 . C22 . C27 . 117.0(3) yes C22 . C23 . C24 . 121.4(4) yes C22 . C23 . H231 . 119.5 no C24 . C23 . H231 . 119.1 no C23 . C24 . C25 . 120.2(4) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 119.7 no C24 . C25 . C26 . 119.3(3) yes C24 . C25 . H251 . 119.6 no C26 . C25 . H251 . 121.1 no C25 . C26 . C27 . 120.2(4) yes C25 . C26 . H261 . 120.3 no C27 . C26 . H261 . 119.4 no C22 . C27 . C26 . 121.7(3) yes C22 . C27 . H271 . 119.8 no C26 . C27 . H271 . 118.5 no N2 . C28 . C29 . 111.7(3) yes N2 . C28 . C30 . 109.4(3) yes C29 . C28 . C30 . 112.4(3) yes N2 . C28 . H281 . 107.6 no C29 . C28 . H281 . 106.2 no C30 . C28 . H281 . 109.3 no C28 . C29 . H291 . 107.4 no C28 . C29 . H292 . 110.9 no H291 . C29 . H292 . 108.1 no C28 . C29 . H293 . 109.9 no H291 . C29 . H293 . 109.6 no H292 . C29 . H293 . 110.8 no C28 . C30 . H301 . 109.5 no C28 . C30 . H302 . 110.5 no H301 . C30 . H302 . 108.3 no C28 . C30 . H303 . 109.7 no H301 . C30 . H303 . 109.2 no H302 . C30 . H303 . 109.6 no P3 . C31 . C32 . 123.5(3) yes P3 . C31 . C36 . 119.1(3) yes C32 . C31 . C36 . 117.0(3) yes C31 . C32 . C33 . 121.8(4) yes C31 . C32 . H321 . 118.3 no C33 . C32 . H321 . 119.9 no C32 . C33 . C34 . 120.0(4) yes C32 . C33 . H331 . 121.0 no C34 . C33 . H331 . 119.0 no C33 . C34 . C35 . 119.3(4) yes C33 . C34 . H341 . 120.1 no C35 . C34 . H341 . 120.6 no C34 . C35 . C36 . 120.5(4) yes C34 . C35 . H351 . 120.1 no C36 . C35 . H351 . 119.3 no C31 . C36 . C35 . 121.4(4) yes C31 . C36 . H361 . 118.5 no C35 . C36 . H361 . 120.1 no P3 . C37 . C38 . 126.9(3) yes P3 . C37 . C42 . 115.7(2) yes C38 . C37 . C42 . 117.4(3) yes C37 . C38 . C39 . 121.1(3) yes C37 . C38 . H381 . 120.0 no C39 . C38 . H381 . 118.9 no C38 . C39 . C40 . 120.4(4) yes C38 . C39 . H391 . 120.6 no C40 . C39 . H391 . 118.9 no C39 . C40 . C41 . 119.3(3) yes C39 . C40 . H401 . 120.3 no C41 . C40 . H401 . 120.4 no C40 . C41 . C42 . 120.5(3) yes C40 . C41 . H411 . 118.6 no C42 . C41 . H411 . 120.9 no C37 . C42 . C41 . 121.2(3) yes C37 . C42 . H421 . 119.2 no C41 . C42 . H421 . 119.6 no N3 . C43 . C44 . 112.4(3) yes N3 . C43 . C45 . 109.8(3) yes C44 . C43 . C45 . 111.5(3) yes N3 . C43 . H431 . 107.6 no C44 . C43 . H431 . 107.8 no C45 . C43 . H431 . 107.6 no C43 . C44 . H441 . 110.7 no C43 . C44 . H442 . 111.1 no H441 . C44 . H442 . 108.0 no C43 . C44 . H443 . 109.4 no H441 . C44 . H443 . 109.3 no H442 . C44 . H443 . 108.3 no C43 . C45 . H451 . 108.5 no C43 . C45 . H452 . 110.4 no H451 . C45 . H452 . 109.5 no C43 . C45 . H453 . 110.1 no H451 . C45 . H453 . 109.3 no H452 . C45 . H453 . 108.9 no N6 . C46 . C47 . 110.2(4) yes N6 . C46 . C48 . 111.0(4) yes C47 . C46 . C48 . 109.8(4) yes N6 . C46 . C49 . 108.9(4) yes C47 . C46 . C49 . 107.6(4) yes C48 . C46 . C49 . 109.3(4) yes C46 . C47 . H471 . 110.3 no C46 . C47 . H472 . 109.6 no H471 . C47 . H472 . 108.5 no C46 . C47 . H473 . 108.6 no H471 . C47 . H473 . 110.4 no H472 . C47 . H473 . 109.5 no C46 . C48 . H481 . 110.0 no C46 . C48 . H482 . 111.8 no H481 . C48 . H482 . 107.3 no C46 . C48 . H483 . 111.0 no H481 . C48 . H483 . 108.2 no H482 . C48 . H483 . 108.3 no C46 . C49 . H491 . 109.5 no C46 . C49 . H492 . 108.9 no H491 . C49 . H492 . 109.2 no C46 . C49 . H493 . 111.3 no H491 . C49 . H493 . 108.4 no H492 . C49 . H493 . 109.5 no O1 . C50 . C510 . 94.0(8) yes O1 . C50 . H501 . 111.4 no C510 . C50 . H501 . 114.5 no O1 . C50 . H502 . 110.1 no C510 . C50 . H502 . 114.3 no H501 . C50 . H502 . 111.3 no O1 . C50 . C511 . 116.4(11) yes O1 . C50 . H501 . 111.4 no C511 . C50 . H501 . 102.3 no O1 . C50 . H502 . 110.1 no C511 . C50 . H502 . 104.9 no H501 . C50 . H502 . 111.3 no O2 . C57 . C561 . 114.5(5) yes O2 . C57 . H571 . 112.0 no C561 . C57 . H571 . 92.3 no O2 . C57 . H572 . 111.8 no C561 . C57 . H572 . 115.2 no H571 . C57 . H572 . 109.5 no O2 . C57 . C560 . 98.2(6) yes O2 . C57 . H573 . 108.1 no C560 . C57 . H573 . 129.6 no O2 . C57 . H574 . 108.2 no C560 . C57 . H574 . 101.5 no H573 . C57 . H574 . 109.5 no O3 . C58 . C59 . 106.7(4) yes O3 . C58 . H581 . 109.0 no C59 . C58 . H581 . 111.2 no O3 . C58 . H582 . 108.8 no C59 . C58 . H582 . 112.0 no H581 . C58 . H582 . 109.0 no C58 . C59 . C60 . 107.3(5) yes C58 . C59 . H591 . 110.8 no C60 . C59 . H591 . 109.8 no C58 . C59 . H592 . 109.8 no C60 . C59 . H592 . 110.3 no H591 . C59 . H592 . 108.9 no C59 . C60 . C61 . 105.6(5) yes C59 . C60 . H601 . 109.5 no C61 . C60 . H601 . 111.8 no C59 . C60 . H602 . 109.6 no C61 . C60 . H602 . 110.3 no H601 . C60 . H602 . 110.0 no C60 . C61 . O3 . 105.8(4) yes C60 . C61 . H611 . 111.3 no O3 . C61 . H611 . 107.6 no C60 . C61 . H612 . 110.9 no O3 . C61 . H612 . 111.1 no H611 . C61 . H612 . 110.1 no O4 . C62 . C63 . 108.5(5) yes O4 . C62 . H621 . 108.4 no C63 . C62 . H621 . 110.2 no O4 . C62 . H622 . 109.9 no C63 . C62 . H622 . 110.5 no H621 . C62 . H622 . 109.2 no C62 . C63 . C640 . 100.6(7) yes C62 . C63 . H631 . 111.1 no C640 . C63 . H631 . 99.8 no C62 . C63 . H632 . 111.1 no C640 . C63 . H632 . 125.3 no H631 . C63 . H632 . 108.2 no C62 . C63 . C641 . 106.6(7) yes C62 . C63 . H631 . 111.1 no C641 . C63 . H631 . 121.5 no C62 . C63 . H632 . 111.1 no C641 . C63 . H632 . 97.6 no H631 . C63 . H632 . 108.2 no O4 . C65 . C640 . 105.6(7) yes O4 . C65 . H651 . 107.5 no C640 . C65 . H651 . 122.5 no O4 . C65 . H652 . 109.8 no C640 . C65 . H652 . 102.8 no H651 . C65 . H652 . 108.1 no O4 . C65 . C641 . 113.3(7) yes O4 . C65 . H651 . 107.5 no C641 . C65 . H651 . 93.0 no O4 . C65 . H652 . 109.8 no C641 . C65 . H652 . 122.7 no H651 . C65 . H652 . 108.1 no O5 . C69 . C680 . 99.8(6) yes O5 . C69 . H691 . 111.8 no C680 . C69 . H691 . 111.5 no O5 . C69 . H692 . 111.7 no C680 . C69 . H692 . 112.4 no H691 . C69 . H692 . 109.5 no O5 . C69 . C681 . 111.2(9) yes O5 . C69 . H693 . 108.8 no C681 . C69 . H693 . 108.2 no O5 . C69 . H694 . 109.0 no C681 . C69 . H694 . 110.2 no H693 . C69 . H694 . 109.5 no C50 . C510 . C520 . 103.0(10) yes C50 . C510 . H5101 . 111.1 no C520 . C510 . H5101 . 111.6 no C50 . C510 . H5102 . 110.8 no C520 . C510 . H5102 . 110.7 no H5101 . C510 . H5102 . 109.5 no C50 . C511 . C521 . 104.9(13) yes C50 . C511 . H5111 . 109.9 no C521 . C511 . H5111 . 109.3 no C50 . C511 . H5112 . 112.1 no C521 . C511 . H5112 . 111.1 no H5111 . C511 . H5112 . 109.5 no C510 . C520 . C530 . 102.9(11) yes C510 . C520 . H5201 . 110.6 no C530 . C520 . H5201 . 109.2 no C510 . C520 . H5202 . 111.4 no C530 . C520 . H5202 . 113.1 no H5201 . C520 . H5202 . 109.5 no C511 . C521 . C531 . 100.7(10) yes C511 . C521 . H5211 . 112.3 no C531 . C521 . H5211 . 112.2 no C511 . C521 . H5212 . 111.5 no C531 . C521 . H5212 . 110.6 no H5211 . C521 . H5212 . 109.5 no C520 . C530 . O1 . 99.9(10) yes C520 . C530 . H5301 . 113.2 no O1 . C530 . H5301 . 113.6 no C520 . C530 . H5302 . 110.2 no O1 . C530 . H5302 . 110.3 no H5301 . C530 . H5302 . 109.5 no C521 . C531 . O1 . 110.9(9) yes C521 . C531 . H5311 . 108.4 no O1 . C531 . H5311 . 108.1 no C521 . C531 . H5312 . 110.2 no O1 . C531 . H5312 . 109.7 no H5311 . C531 . H5312 . 109.5 no O2 . C540 . C550 . 100.1(7) yes O2 . C540 . H5401 . 111.9 no C550 . C540 . H5401 . 111.4 no O2 . C540 . H5402 . 111.6 no C550 . C540 . H5402 . 112.2 no H5401 . C540 . H5402 . 109.5 no O2 . C541 . C551 . 111.0(9) yes O2 . C541 . H5411 . 108.6 no C551 . C541 . H5411 . 109.2 no O2 . C541 . H5412 . 109.1 no C551 . C541 . H5412 . 109.4 no H5411 . C541 . H5412 . 109.5 no C540 . C550 . C560 . 102.4(8) yes C540 . C550 . H5501 . 111.7 no C560 . C550 . H5501 . 111.5 no C540 . C550 . H5502 . 110.6 no C560 . C550 . H5502 . 111.0 no H5501 . C550 . H5502 . 109.5 no C541 . C551 . C561 . 101.4(8) yes C541 . C551 . H5511 . 111.5 no C561 . C551 . H5511 . 111.9 no C541 . C551 . H5512 . 110.9 no C561 . C551 . H5512 . 111.5 no H5511 . C551 . H5512 . 109.5 no C550 . C560 . C57 . 105.1(9) yes C550 . C560 . H5601 . 110.6 no C57 . C560 . H5601 . 110.4 no C550 . C560 . H5602 . 110.6 no C57 . C560 . H5602 . 110.6 no H5601 . C560 . H5602 . 109.5 no C551 . C561 . C57 . 103.9(8) yes C551 . C561 . H5611 . 110.4 no C57 . C561 . H5611 . 110.7 no C551 . C561 . H5612 . 110.9 no C57 . C561 . H5612 . 111.4 no H5611 . C561 . H5612 . 109.5 no C63 . C640 . C65 . 101.8(9) yes C63 . C640 . H6401 . 110.9 no C65 . C640 . H6401 . 110.9 no C63 . C640 . H6402 . 111.9 no C65 . C640 . H6402 . 111.7 no H6401 . C640 . H6402 . 109.5 no C63 . C641 . C65 . 102.3(9) yes C63 . C641 . H6411 . 111.1 no C65 . C641 . H6411 . 111.1 no C63 . C641 . H6412 . 111.4 no C65 . C641 . H6412 . 111.4 no H6411 . C641 . H6412 . 109.5 no O5 . C660 . C670 . 111.4(11) yes O5 . C660 . H6601 . 108.4 no C670 . C660 . H6601 . 110.2 no O5 . C660 . H6602 . 108.7 no C670 . C660 . H6602 . 108.7 no H6601 . C660 . H6602 . 109.5 no O5 . C661 . C671 . 108.1(11) yes O5 . C661 . H6611 . 109.6 no C671 . C661 . H6611 . 109.4 no O5 . C661 . H6612 . 109.8 no C671 . C661 . H6612 . 110.5 no H6611 . C661 . H6612 . 109.5 no C660 . C670 . C680 . 108.3(13) yes C660 . C670 . H6701 . 108.9 no C680 . C670 . H6701 . 108.8 no C660 . C670 . H6702 . 110.0 no C680 . C670 . H6702 . 111.3 no H6701 . C670 . H6702 . 109.5 no C661 . C671 . C681 . 107.0(13) yes C661 . C671 . H6711 . 109.6 no C681 . C671 . H6711 . 108.6 no C661 . C671 . H6712 . 110.8 no C681 . C671 . H6712 . 111.2 no H6711 . C671 . H6712 . 109.5 no C69 . C680 . C670 . 108.8(11) yes C69 . C680 . H6801 . 110.1 no C670 . C680 . H6801 . 110.7 no C69 . C680 . H6802 . 109.4 no C670 . C680 . H6802 . 108.5 no H6801 . C680 . H6802 . 109.5 no C671 . C681 . C69 . 103.2(13) yes C671 . C681 . H6811 . 112.5 no C69 . C681 . H6811 . 111.8 no C671 . C681 . H6812 . 109.9 no C69 . C681 . H6812 . 109.9 no H6811 . C681 . H6812 . 109.5 no _iucr_refine_instruction_details_constraints ; # # Punched on 13/03/11 at 16:41:53 # #LIST 12 BLOCK SCALE TA(1,X'S, U'S ) UNTIL C(69) CONT C(510,X'S,U[ISO]) UNTIL C(681) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) H ( 473,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) H ( 483,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) H ( 493,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) REM TOO MANY H ATOMS ON C ( 57), - 4 RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) CONT H ( 573,X'S) H ( 574,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S) RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) RIDE C ( 65,X'S) H ( 651,X'S) H ( 652,X'S) REM TOO MANY H ATOMS ON C ( 69), - 4 RIDE C ( 69,X'S) H ( 691,X'S) H ( 692,X'S) CONT H ( 693,X'S) H ( 694,X'S) RIDE C ( 510,X'S) H (5101,X'S) H (5102,X'S) RIDE C ( 511,X'S) H (5111,X'S) H (5112,X'S) RIDE C ( 520,X'S) H (5201,X'S) H (5202,X'S) RIDE C ( 521,X'S) H (5211,X'S) H (5212,X'S) RIDE C ( 530,X'S) H (5301,X'S) H (5302,X'S) RIDE C ( 531,X'S) H (5311,X'S) H (5312,X'S) RIDE C ( 540,X'S) H (5401,X'S) H (5402,X'S) RIDE C ( 541,X'S) H (5411,X'S) H (5412,X'S) RIDE C ( 550,X'S) H (5501,X'S) H (5502,X'S) RIDE C ( 551,X'S) H (5511,X'S) H (5512,X'S) RIDE C ( 560,X'S) H (5601,X'S) H (5602,X'S) RIDE C ( 561,X'S) H (5611,X'S) H (5612,X'S) RIDE C ( 640,X'S) H (6401,X'S) H (6402,X'S) RIDE C ( 641,X'S) H (6411,X'S) H (6412,X'S) RIDE C ( 660,X'S) H (6601,X'S) H (6602,X'S) RIDE C ( 661,X'S) H (6611,X'S) H (6612,X'S) RIDE C ( 670,X'S) H (6701,X'S) H (6702,X'S) RIDE C ( 671,X'S) H (6711,X'S) H (6712,X'S) RIDE C ( 680,X'S) H (6801,X'S) H (6802,X'S) RIDE C ( 681,X'S) H (6811,X'S) H (6812,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/03/11 at 16:41:53 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END