# 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