# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_publ_contact_author_name 'Yaofeng Chen'
_publ_contact_author_email YAOFCHEN@MAIL.SIOC.AC.CN
_publ_section_title
;
Neodymium(III) phosphinidene complexes supported by
pentamethylcyclopentadienyl and hydrotris(pyrazolyl)borate
ligands
;
loop_
_publ_author_name
'Yaofeng Chen'
'Peng Cui'
'Jie Sun'
# Attachment 'complex_2.cif'
#==============================================================================
data_z
_database_code_depnum_ccdc_archive 'CCDC 763478'
#TrackingRef 'complex_2.cif'
# start Validation Reply Form
_vrf_PLAT242_ALERT_2_C
;
PROBLEM: Check Low U~eq~ as Compared to Neighbors for C7
RESPONSE: Atom C7 is a methyne carbon atom of one of the isopropyl groups. This
group, as a whole, is involved into thermal rocking vibrations around the
C2---C7 bond. At the experiment conditions (293 K) these rockings are well
pronounced what is indicated by nearly tangent orientations of the maximum
principal atom displacement ellipsoid axes (methyl groups atoms C8 and C9) in
respect to C2---C7 line.
;
_vrf_PLAT242_ALERT_2_B
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C10
RESPONSE: Atom C10 is a methyne carbon atom of one of the isopropyl groups.
This group, as a whole, is involved into thermal rocking vibrations around the
C6---C10 bond. At the experiment conditions (293 K) these rockings are
well-pronounced what is indicated by nearly tangent orientations of the
maximum principal atom displacement ellipsoid axes (methyl groups atoms C11
and C12) in respect to C6---C10 line.
;
_vrf_PLAT774_ALERT_1_B
;
PROBLEM: Suspect X-Y Bond in CIF: ND1 -- ND1 .. 4.12 Ang.
RESPONSE: Analysis of the Cambridge Structural Database (CSD; Version 5.27,
release February 2009; Allen, 2002; 7 entries, 17 fragments) reveals few
Nd---Nd interatomic contacts reported (range from 3.421 to 4.009 \%A, median
value 3.861 \%A). Despite of the fact that the Nd---Nd^i^ (symmetry operation:
1--x, 1--y, 1--z) distance in the case of the question [4.1164 (5) \%A]
exceeds the upper boundary by 0.11 \%A, this is only a 3% relative deviation
from the median value and, thus, there is no reason to exclude this value from
reported in CIF.
;
# end Validation Reply Form
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis{\m-[2,6-bis(1-methylethyl)phenyl]phosphinidene}bis(\h^5^-1,2,3,4,5-
pentamethylcyclopentadienyl)di(tetrahydrofuran)dineodymium(III)
;
_chemical_name_common
;
Bis(mu-(2,6-bis(1-methylethyl)phenyl)phosphinidene)bis(eta$5!-
1,2,3,4,5-
pentamethylcyclopentadienyl)di(tetrahydrofuran)dineodymium(iii)
;
_chemical_melting_point ?
_chemical_formula_moiety 'C52 H80 Nd2 O2 P2'
_chemical_formula_sum 'C52 H80 Nd2 O2 P2'
_chemical_formula_weight 1087.58
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.3913(10)
_cell_length_b 18.0366(16)
_cell_length_c 12.6070(11)
_cell_angle_alpha 90.00
_cell_angle_beta 97.184(2)
_cell_angle_gamma 90.00
_cell_volume 2569.9(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 4478
_cell_measurement_theta_min 2.28
_cell_measurement_theta_max 25.19
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.405
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1116
_exptl_absorpt_coefficient_mu 2.096
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5720
_exptl_absorpt_correction_T_max 0.7303
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'BRUKER SMART CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 12923
_diffrn_reflns_av_R_equivalents 0.0286
_diffrn_reflns_av_sigmaI/netI 0.0358
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 1.98
_diffrn_reflns_theta_max 25.10
_reflns_number_total 4570
_reflns_number_gt 3961
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'BRUKER AXS APEX-2 V1.0-8 (Bruker, 2007)'
_computing_cell_refinement 'SAINT v7.34A (Bruker, 2007)'
_computing_data_reduction 'SAINT v7.34A (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+1.0165P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4570
_refine_ls_number_parameters 290
_refine_ls_number_restraints 79
_refine_ls_R_factor_all 0.0415
_refine_ls_R_factor_gt 0.0347
_refine_ls_wR_factor_ref 0.0841
_refine_ls_wR_factor_gt 0.0813
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_restrained_S_all 1.063
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.514391(18) 0.387823(11) 0.528648(16) 0.03521(9) Uani 1 1 d . . .
P1 P 0.37277(10) 0.48452(6) 0.39661(8) 0.0423(3) Uani 1 1 d . . .
O1 O 0.6848(3) 0.32929(16) 0.4555(3) 0.0633(9) Uani 1 1 d DU A .
C13 C 0.7170(5) 0.2517(3) 0.4512(6) 0.0867(17) Uani 1 1 d DU . .
H13D H 0.7517 0.2346 0.5211 0.104 Uiso 0.596(14) 1 calc PR A 3
H13C H 0.6478 0.2217 0.4280 0.104 Uiso 0.596(14) 1 calc PR A 3
H13A H 0.6695 0.2268 0.3936 0.104 Uiso 0.404(14) 1 d PR A 2
H13B H 0.7076 0.2272 0.5172 0.104 Uiso 0.404(14) 1 d PR A 2
C14B C 0.8019(10) 0.2464(5) 0.3753(10) 0.092(3) Uani 0.596(14) 1 d PDU A 3
H14A H 0.7637 0.2460 0.3021 0.110 Uiso 0.596(14) 1 calc PR A 3
H14B H 0.8520 0.2031 0.3880 0.110 Uiso 0.596(14) 1 calc PR A 3
C15B C 0.8739(7) 0.3218(5) 0.4034(11) 0.090(3) Uani 0.596(14) 1 d PDU A 3
H15B H 0.9249 0.3184 0.4708 0.108 Uiso 0.596(14) 1 calc PR A 3
H15A H 0.9202 0.3360 0.3472 0.108 Uiso 0.596(14) 1 calc PR A 3
C16 C 0.7732(5) 0.3729(3) 0.4100(5) 0.0708(14) Uani 1 1 d DU . .
H16D H 0.7976 0.4149 0.4555 0.085 Uiso 0.596(14) 1 calc PR A 3
H16C H 0.7422 0.3909 0.3396 0.085 Uiso 0.596(14) 1 calc PR A 3
H16B H 0.8279 0.3950 0.4651 0.085 Uiso 0.404(14) 1 d PR A 2
H16A H 0.7361 0.4111 0.3648 0.085 Uiso 0.404(14) 1 d PR A 2
C1 C 0.3054(3) 0.4708(2) 0.2575(3) 0.0398(9) Uani 1 1 d . . .
C2 C 0.3649(4) 0.4335(2) 0.1817(3) 0.0463(10) Uani 1 1 d . . .
C3 C 0.3154(5) 0.4315(3) 0.0749(4) 0.0600(13) Uani 1 1 d . . .
H3 H 0.3563 0.4079 0.0251 0.072 Uiso 1 1 calc R . .
C4 C 0.2093(5) 0.4631(3) 0.0417(4) 0.0708(15) Uani 1 1 d . . .
H4 H 0.1788 0.4620 -0.0302 0.085 Uiso 1 1 calc R . .
C5 C 0.1475(5) 0.4966(3) 0.1145(4) 0.0605(13) Uani 1 1 d . . .
H5 H 0.0735 0.5168 0.0915 0.073 Uiso 1 1 calc R . .
C6 C 0.1926(4) 0.5012(2) 0.2228(3) 0.0487(11) Uani 1 1 d . . .
C7 C 0.4813(5) 0.3934(3) 0.2160(4) 0.0611(14) Uani 1 1 d . . .
H7 H 0.5233 0.4218 0.2753 0.073 Uiso 1 1 calc R . .
C8 C 0.4527(5) 0.3178(3) 0.2604(6) 0.099(2) Uani 1 1 d . . .
H8B H 0.4052 0.3242 0.3175 0.149 Uiso 1 1 calc R . .
H8C H 0.5249 0.2929 0.2870 0.149 Uiso 1 1 calc R . .
H8A H 0.4099 0.2886 0.2047 0.149 Uiso 1 1 calc R . .
C9 C 0.5642(6) 0.3867(4) 0.1305(5) 0.107(3) Uani 1 1 d . . .
H9B H 0.6409 0.3711 0.1630 0.160 Uiso 1 1 calc R . .
H9C H 0.5707 0.4339 0.0966 0.160 Uiso 1 1 calc R . .
H9A H 0.5332 0.3508 0.0781 0.160 Uiso 1 1 calc R . .
C10 C 0.1187(4) 0.5379(3) 0.2981(4) 0.0611(13) Uani 1 1 d . . .
H10 H 0.1717 0.5473 0.3641 0.073 Uiso 1 1 calc R . .
C11 C 0.0248(8) 0.4898(4) 0.3275(8) 0.151(4) Uani 1 1 d . . .
H11B H -0.0284 0.4776 0.2647 0.226 Uiso 1 1 calc R . .
H11C H -0.0178 0.5149 0.3778 0.226 Uiso 1 1 calc R . .
H11A H 0.0589 0.4451 0.3592 0.226 Uiso 1 1 calc R . .
C12 C 0.0674(8) 0.6118(3) 0.2620(8) 0.120(3) Uani 1 1 d . . .
H12B H 0.1276 0.6418 0.2366 0.180 Uiso 1 1 calc R . .
H12C H 0.0380 0.6362 0.3210 0.180 Uiso 1 1 calc R . .
H12A H 0.0038 0.6045 0.2055 0.180 Uiso 1 1 calc R . .
C15A C 0.8426(13) 0.3195(6) 0.3548(11) 0.077(4) Uani 0.404(14) 1 d PDU A 2
H15D H 0.9216 0.3377 0.3487 0.093 Uiso 0.404(14) 1 calc PR A 2
H15C H 0.8032 0.3064 0.2846 0.093 Uiso 0.404(14) 1 calc PR A 2
C14A C 0.8439(8) 0.2522(7) 0.4374(12) 0.077(4) Uani 0.404(14) 1 d PDU A 2
H14C H 0.8684 0.2061 0.4072 0.092 Uiso 0.404(14) 1 calc PR A 2
H14D H 0.8937 0.2625 0.5039 0.092 Uiso 0.404(14) 1 calc PR A 2
C21 C 0.3339(4) 0.3137(3) 0.6028(4) 0.0508(11) Uani 1 1 d . . .
C22 C 0.4197(4) 0.2575(2) 0.5974(3) 0.0499(11) Uani 1 1 d . . .
C23 C 0.5156(4) 0.2726(2) 0.6757(3) 0.0458(10) Uani 1 1 d . . .
C24 C 0.4898(4) 0.3379(2) 0.7293(3) 0.0459(10) Uani 1 1 d . . .
C25 C 0.3782(4) 0.3632(2) 0.6848(4) 0.0471(10) Uani 1 1 d . . .
C26 C 0.2126(5) 0.3165(3) 0.5396(5) 0.0840(18) Uani 1 1 d . . .
H26A H 0.2108 0.2850 0.4781 0.126 Uiso 1 1 calc R . .
H26C H 0.1950 0.3665 0.5168 0.126 Uiso 1 1 calc R . .
H26B H 0.1549 0.2999 0.5835 0.126 Uiso 1 1 calc R . .
C27 C 0.4051(6) 0.1903(3) 0.5263(4) 0.0787(17) Uani 1 1 d . . .
H27B H 0.3622 0.1528 0.5594 0.118 Uiso 1 1 calc R . .
H27C H 0.4816 0.1716 0.5155 0.118 Uiso 1 1 calc R . .
H27A H 0.3621 0.2037 0.4586 0.118 Uiso 1 1 calc R . .
C28 C 0.6208(5) 0.2243(3) 0.7074(5) 0.0756(16) Uani 1 1 d . . .
H28B H 0.6168 0.2047 0.7777 0.113 Uiso 1 1 calc R . .
H28C H 0.6918 0.2530 0.7076 0.113 Uiso 1 1 calc R . .
H28A H 0.6212 0.1842 0.6574 0.113 Uiso 1 1 calc R . .
C29 C 0.5657(5) 0.3690(3) 0.8267(4) 0.0703(15) Uani 1 1 d . . .
H29B H 0.6462 0.3730 0.8120 0.105 Uiso 1 1 calc R . .
H29A H 0.5620 0.3365 0.8865 0.105 Uiso 1 1 calc R . .
H29C H 0.5370 0.4172 0.8431 0.105 Uiso 1 1 calc R . .
C30 C 0.3116(5) 0.4287(3) 0.7225(5) 0.0778(16) Uani 1 1 d . . .
H30A H 0.2741 0.4556 0.6617 0.117 Uiso 1 1 calc R . .
H30C H 0.3658 0.4608 0.7651 0.117 Uiso 1 1 calc R . .
H30B H 0.2525 0.4114 0.7646 0.117 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nd1 0.03682(15) 0.03220(14) 0.03631(14) 0.00237(9) 0.00336(9) 0.00399(9)
P1 0.0434(6) 0.0423(6) 0.0382(5) 0.0008(5) -0.0067(5) 0.0013(5)
O1 0.063(2) 0.0477(18) 0.083(2) -0.0010(17) 0.0235(17) 0.0139(15)
C13 0.090(4) 0.057(3) 0.119(5) 0.009(3) 0.038(3) 0.024(3)
C14B 0.118(7) 0.076(4) 0.088(7) -0.005(5) 0.039(5) 0.035(4)
C15B 0.070(5) 0.108(6) 0.097(8) 0.015(6) 0.029(5) 0.018(3)
C16 0.072(3) 0.068(3) 0.077(3) -0.001(3) 0.027(3) 0.002(2)
C1 0.042(2) 0.034(2) 0.041(2) 0.0056(17) -0.0032(18) -0.0075(18)
C2 0.050(3) 0.040(2) 0.047(2) -0.005(2) -0.001(2) -0.003(2)
C3 0.075(4) 0.058(3) 0.045(2) -0.012(2) 0.000(2) 0.003(3)
C4 0.087(4) 0.071(4) 0.047(3) -0.005(3) -0.018(3) 0.000(3)
C5 0.056(3) 0.065(3) 0.055(3) 0.001(2) -0.019(2) 0.002(2)
C6 0.047(3) 0.045(3) 0.050(2) 0.001(2) -0.010(2) -0.004(2)
C7 0.056(3) 0.058(3) 0.066(3) -0.021(2) -0.003(3) 0.005(2)
C8 0.094(5) 0.045(3) 0.143(6) -0.003(3) -0.049(4) 0.010(3)
C9 0.085(5) 0.149(7) 0.087(4) -0.058(4) 0.011(4) 0.024(4)
C10 0.041(3) 0.081(4) 0.059(3) -0.002(3) -0.002(2) 0.012(2)
C11 0.153(8) 0.095(6) 0.232(10) 0.036(6) 0.130(8) 0.017(5)
C12 0.155(8) 0.058(4) 0.163(8) 0.003(4) 0.082(7) 0.015(4)
C15A 0.075(7) 0.084(7) 0.078(8) -0.011(5) 0.027(6) 0.004(5)
C14A 0.079(5) 0.080(6) 0.074(8) -0.008(6) 0.017(6) 0.028(5)
C21 0.041(2) 0.057(3) 0.055(3) 0.010(2) 0.006(2) -0.007(2)
C22 0.061(3) 0.039(2) 0.049(2) 0.003(2) 0.008(2) -0.010(2)
C23 0.050(3) 0.040(2) 0.048(2) 0.013(2) 0.011(2) -0.0018(19)
C24 0.053(3) 0.047(3) 0.038(2) 0.005(2) 0.0077(19) -0.010(2)
C25 0.053(3) 0.038(2) 0.054(3) 0.005(2) 0.019(2) -0.003(2)
C26 0.056(3) 0.092(4) 0.099(4) 0.019(4) -0.012(3) -0.020(3)
C27 0.109(5) 0.053(3) 0.074(4) -0.009(3) 0.011(3) -0.023(3)
C28 0.074(4) 0.076(4) 0.078(4) 0.031(3) 0.016(3) 0.022(3)
C29 0.085(4) 0.083(4) 0.042(3) 0.007(3) 0.000(3) -0.026(3)
C30 0.081(4) 0.068(4) 0.092(4) 0.001(3) 0.040(3) 0.012(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O1 2.486(3) . ?
Nd1 C25 2.691(4) . ?
Nd1 C21 2.714(4) . ?
Nd1 C24 2.732(4) . ?
Nd1 P1 2.7456(11) 3_666 ?
Nd1 C22 2.770(4) . ?
Nd1 P1 2.7827(10) . ?
Nd1 C23 2.784(4) . ?
Nd1 Nd1 4.1164(5) 3_666 ?
P1 C1 1.841(4) . ?
P1 Nd1 2.7457(11) 3_666 ?
O1 C13 1.450(5) . ?
O1 C16 1.451(5) . ?
C13 C14B 1.446(8) . ?
C13 C14A 1.478(8) . ?
C13 H13D 0.9700 . ?
C13 H13C 0.9700 . ?
C13 H13A 0.9599 . ?
C13 H13B 0.9601 . ?
C14B C15B 1.604(11) . ?
C14B H14A 0.9700 . ?
C14B H14B 0.9700 . ?
C15B C16 1.481(8) . ?
C15B H15B 0.9700 . ?
C15B H15A 0.9700 . ?
C16 C15A 1.474(8) . ?
C16 H16D 0.9700 . ?
C16 H16C 0.9700 . ?
C16 H16B 0.9598 . ?
C16 H16A 0.9597 . ?
C1 C2 1.410(6) . ?
C1 C6 1.415(6) . ?
C2 C3 1.394(6) . ?
C2 C7 1.524(7) . ?
C3 C4 1.353(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.366(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.400(6) . ?
C5 H5 0.9300 . ?
C6 C10 1.499(7) . ?
C7 C9 1.524(8) . ?
C7 C8 1.526(7) . ?
C7 H7 0.9800 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 H8A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 H9A 0.9600 . ?
C10 C11 1.461(9) . ?
C10 C12 1.502(8) . ?
C10 H10 0.9800 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 H11A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12A 0.9600 . ?
C15A C14A 1.597(11) . ?
C15A H15D 0.9700 . ?
C15A H15C 0.9700 . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C21 C25 1.410(6) . ?
C21 C22 1.416(6) . ?
C21 C26 1.508(6) . ?
C22 C23 1.404(6) . ?
C22 C27 1.504(6) . ?
C23 C24 1.408(6) . ?
C23 C28 1.495(6) . ?
C24 C25 1.400(6) . ?
C24 C29 1.518(6) . ?
C25 C30 1.513(7) . ?
C26 H26A 0.9600 . ?
C26 H26C 0.9600 . ?
C26 H26B 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 H27A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 H28A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30C 0.9600 . ?
C30 H30B 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nd1 C25 138.55(12) . . ?
O1 Nd1 C21 125.38(13) . . ?
C25 Nd1 C21 30.23(13) . . ?
O1 Nd1 C24 112.28(12) . . ?
C25 Nd1 C24 29.90(13) . . ?
C21 Nd1 C24 49.38(13) . . ?
O1 Nd1 P1 97.46(8) . 3_666 ?
C25 Nd1 P1 100.09(10) . 3_666 ?
C21 Nd1 P1 129.55(11) . 3_666 ?
C24 Nd1 P1 93.22(9) . 3_666 ?
O1 Nd1 C22 96.22(12) . . ?
C25 Nd1 C22 49.35(13) . . ?
C21 Nd1 C22 29.91(13) . . ?
C24 Nd1 C22 48.84(13) . . ?
P1 Nd1 C22 142.01(9) 3_666 . ?
O1 Nd1 P1 117.72(8) . . ?
C25 Nd1 P1 101.36(10) . . ?
C21 Nd1 P1 96.16(10) . . ?
C24 Nd1 P1 129.89(10) . . ?
P1 Nd1 P1 83.75(3) 3_666 . ?
C22 Nd1 P1 119.98(10) . . ?
O1 Nd1 C23 89.49(11) . . ?
C25 Nd1 C23 49.07(13) . . ?
C21 Nd1 C23 48.99(13) . . ?
C24 Nd1 C23 29.55(13) . . ?
P1 Nd1 C23 115.75(9) 3_666 . ?
C22 Nd1 C23 29.29(12) . . ?
P1 Nd1 C23 145.13(9) . . ?
O1 Nd1 Nd1 113.64(7) . 3_666 ?
C25 Nd1 Nd1 104.48(9) . 3_666 ?
C21 Nd1 Nd1 119.82(10) . 3_666 ?
C24 Nd1 Nd1 118.10(9) . 3_666 ?
P1 Nd1 Nd1 42.22(2) 3_666 3_666 ?
C22 Nd1 Nd1 149.71(10) . 3_666 ?
P1 Nd1 Nd1 41.53(2) . 3_666 ?
C23 Nd1 Nd1 147.60(9) . 3_666 ?
C1 P1 Nd1 124.14(13) . 3_666 ?
C1 P1 Nd1 128.82(14) . . ?
Nd1 P1 Nd1 96.25(3) 3_666 . ?
C13 O1 C16 108.5(4) . . ?
C13 O1 Nd1 129.5(3) . . ?
C16 O1 Nd1 122.0(3) . . ?
C14B C13 O1 106.3(5) . . ?
O1 C13 C14A 104.7(6) . . ?
C14B C13 H13D 110.5 . . ?
O1 C13 H13D 110.5 . . ?
C14B C13 H13C 110.5 . . ?
O1 C13 H13C 110.5 . . ?
H13D C13 H13C 108.7 . . ?
O1 C13 H13A 111.0 . . ?
C14A C13 H13A 112.4 . . ?
H13D C13 H13A 131.7 . . ?
C14B C13 H13B 134.4 . . ?
O1 C13 H13B 110.8 . . ?
C14A C13 H13B 108.8 . . ?
H13A C13 H13B 109.2 . . ?
C13 C14B C15B 99.5(6) . . ?
C13 C14B H14A 111.9 . . ?
C15B C14B H14A 111.9 . . ?
C13 C14B H14B 111.9 . . ?
C15B C14B H14B 111.9 . . ?
H14A C14B H14B 109.6 . . ?
C16 C15B C14B 99.3(6) . . ?
C16 C15B H15B 111.9 . . ?
C14B C15B H15B 111.9 . . ?
C16 C15B H15A 111.9 . . ?
C14B C15B H15A 111.9 . . ?
H15B C15B H15A 109.6 . . ?
O1 C16 C15A 105.8(5) . . ?
O1 C16 C15B 105.5(5) . . ?
O1 C16 H16D 110.6 . . ?
C15A C16 H16D 131.1 . . ?
C15B C16 H16D 110.6 . . ?
O1 C16 H16C 110.6 . . ?
C15B C16 H16C 110.6 . . ?
H16D C16 H16C 108.8 . . ?
O1 C16 H16B 111.1 . . ?
C15A C16 H16B 106.0 . . ?
O1 C16 H16A 110.4 . . ?
C15A C16 H16A 114.3 . . ?
C15B C16 H16A 134.5 . . ?
H16B C16 H16A 109.2 . . ?
C2 C1 C6 118.0(4) . . ?
C2 C1 P1 122.2(3) . . ?
C6 C1 P1 119.8(3) . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 C7 119.6(4) . . ?
C1 C2 C7 120.6(4) . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 121.6(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 119.2(4) . . ?
C5 C6 C10 118.5(4) . . ?
C1 C6 C10 122.3(4) . . ?
C9 C7 C2 115.6(5) . . ?
C9 C7 C8 111.6(5) . . ?
C2 C7 C8 108.0(4) . . ?
C9 C7 H7 107.1 . . ?
C2 C7 H7 107.1 . . ?
C8 C7 H7 107.1 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
C11 C10 C6 112.7(5) . . ?
C11 C10 C12 109.5(5) . . ?
C6 C10 C12 115.4(5) . . ?
C11 C10 H10 106.2 . . ?
C6 C10 H10 106.2 . . ?
C12 C10 H10 106.2 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
H11B C11 H11A 109.5 . . ?
H11C C11 H11A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
C16 C15A C14A 98.6(7) . . ?
C16 C15A H15D 112.0 . . ?
C14A C15A H15D 112.0 . . ?
C16 C15A H15C 112.0 . . ?
C14A C15A H15C 112.0 . . ?
H15D C15A H15C 109.7 . . ?
C13 C14A C15A 98.8(7) . . ?
C13 C14A H14C 112.0 . . ?
C15A C14A H14C 112.0 . . ?
C13 C14A H14D 112.0 . . ?
C15A C14A H14D 112.0 . . ?
H14C C14A H14D 109.7 . . ?
C25 C21 C22 107.6(4) . . ?
C25 C21 C26 125.9(5) . . ?
C22 C21 C26 126.2(4) . . ?
C25 C21 Nd1 74.0(2) . . ?
C22 C21 Nd1 77.2(2) . . ?
C26 C21 Nd1 119.0(3) . . ?
C23 C22 C21 107.9(4) . . ?
C23 C22 C27 126.4(4) . . ?
C21 C22 C27 125.5(4) . . ?
C23 C22 Nd1 75.9(2) . . ?
C21 C22 Nd1 72.9(2) . . ?
C27 C22 Nd1 121.1(3) . . ?
C22 C23 C24 108.0(4) . . ?
C22 C23 C28 127.0(4) . . ?
C24 C23 C28 124.6(4) . . ?
C22 C23 Nd1 74.8(2) . . ?
C24 C23 Nd1 73.2(2) . . ?
C28 C23 Nd1 123.4(3) . . ?
C25 C24 C23 108.3(4) . . ?
C25 C24 C29 126.9(5) . . ?
C23 C24 C29 124.4(4) . . ?
C25 C24 Nd1 73.4(2) . . ?
C23 C24 Nd1 77.3(2) . . ?
C29 C24 Nd1 120.9(3) . . ?
C24 C25 C21 108.1(4) . . ?
C24 C25 C30 126.5(4) . . ?
C21 C25 C30 125.2(5) . . ?
C24 C25 Nd1 76.7(2) . . ?
C21 C25 Nd1 75.8(2) . . ?
C30 C25 Nd1 117.3(3) . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26C C26 H26B 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
H27B C27 H27A 109.5 . . ?
H27C C27 H27A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C23 C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
C24 C29 H29A 109.5 . . ?
H29B C29 H29A 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30C C30 H30B 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Nd1 P1 C1 49.2(2) . . . . ?
C25 Nd1 P1 C1 -116.6(2) . . . . ?
C21 Nd1 P1 C1 -86.4(2) . . . . ?
C24 Nd1 P1 C1 -126.7(2) . . . . ?
P1 Nd1 P1 C1 144.36(18) 3_666 . . . ?
C22 Nd1 P1 C1 -67.2(2) . . . . ?
C23 Nd1 P1 C1 -88.3(2) . . . . ?
Nd1 Nd1 P1 C1 144.35(18) 3_666 . . . ?
O1 Nd1 P1 Nd1 -95.16(9) . . . 3_666 ?
C25 Nd1 P1 Nd1 99.08(10) . . . 3_666 ?
C21 Nd1 P1 Nd1 129.23(11) . . . 3_666 ?
C24 Nd1 P1 Nd1 88.98(12) . . . 3_666 ?
P1 Nd1 P1 Nd1 0.0 3_666 . . 3_666 ?
C22 Nd1 P1 Nd1 148.45(11) . . . 3_666 ?
C23 Nd1 P1 Nd1 127.39(16) . . . 3_666 ?
C25 Nd1 O1 C13 31.0(5) . . . . ?
C21 Nd1 O1 C13 -6.2(5) . . . . ?
C24 Nd1 O1 C13 48.9(5) . . . . ?
P1 Nd1 O1 C13 145.5(4) 3_666 . . . ?
C22 Nd1 O1 C13 1.0(5) . . . . ?
P1 Nd1 O1 C13 -127.7(4) . . . . ?
C23 Nd1 O1 C13 29.6(5) . . . . ?
Nd1 Nd1 O1 C13 -173.8(4) 3_666 . . . ?
C25 Nd1 O1 C16 -147.5(4) . . . . ?
C21 Nd1 O1 C16 175.3(4) . . . . ?
C24 Nd1 O1 C16 -129.5(4) . . . . ?
P1 Nd1 O1 C16 -32.9(4) 3_666 . . . ?
C22 Nd1 O1 C16 -177.4(4) . . . . ?
P1 Nd1 O1 C16 53.9(4) . . . . ?
C23 Nd1 O1 C16 -148.9(4) . . . . ?
Nd1 Nd1 O1 C16 7.8(4) 3_666 . . . ?
C16 O1 C13 C14B -17.2(8) . . . . ?
Nd1 O1 C13 C14B 164.2(6) . . . . ?
C16 O1 C13 C14A 18.8(8) . . . . ?
Nd1 O1 C13 C14A -159.8(7) . . . . ?
O1 C13 C14B C15B 37.8(10) . . . . ?
C14A C13 C14B C15B -54.5(8) . . . . ?
C13 C14B C15B C16 -44.7(11) . . . . ?
C13 O1 C16 C15A 13.5(9) . . . . ?
Nd1 O1 C16 C15A -167.8(7) . . . . ?
C13 O1 C16 C15B -13.7(8) . . . . ?
Nd1 O1 C16 C15B 165.0(6) . . . . ?
C14B C15B C16 O1 35.3(10) . . . . ?
C14B C15B C16 C15A -59.2(11) . . . . ?
Nd1 P1 C1 C2 97.4(3) 3_666 . . . ?
Nd1 P1 C1 C2 -38.1(4) . . . . ?
Nd1 P1 C1 C6 -79.6(3) 3_666 . . . ?
Nd1 P1 C1 C6 144.8(3) . . . . ?
C6 C1 C2 C3 4.0(6) . . . . ?
P1 C1 C2 C3 -173.1(3) . . . . ?
C6 C1 C2 C7 -174.4(4) . . . . ?
P1 C1 C2 C7 8.5(6) . . . . ?
C1 C2 C3 C4 -1.7(7) . . . . ?
C7 C2 C3 C4 176.7(5) . . . . ?
C2 C3 C4 C5 -1.3(8) . . . . ?
C3 C4 C5 C6 2.0(8) . . . . ?
C4 C5 C6 C1 0.4(7) . . . . ?
C4 C5 C6 C10 -179.2(5) . . . . ?
C2 C1 C6 C5 -3.3(6) . . . . ?
P1 C1 C6 C5 173.8(3) . . . . ?
C2 C1 C6 C10 176.2(4) . . . . ?
P1 C1 C6 C10 -6.6(6) . . . . ?
C3 C2 C7 C9 28.8(7) . . . . ?
C1 C2 C7 C9 -152.8(5) . . . . ?
C3 C2 C7 C8 -97.0(6) . . . . ?
C1 C2 C7 C8 81.4(5) . . . . ?
C5 C6 C10 C11 78.4(7) . . . . ?
C1 C6 C10 C11 -101.1(6) . . . . ?
C5 C6 C10 C12 -48.3(7) . . . . ?
C1 C6 C10 C12 132.1(6) . . . . ?
O1 C16 C15A C14A -37.0(12) . . . . ?
C15B C16 C15A C14A 55.9(10) . . . . ?
C14B C13 C14A C15A 57.3(9) . . . . ?
O1 C13 C14A C15A -40.2(11) . . . . ?
C16 C15A C14A C13 47.1(13) . . . . ?
O1 Nd1 C21 C25 127.4(3) . . . . ?
C24 Nd1 C21 C25 37.2(3) . . . . ?
P1 Nd1 C21 C25 -15.0(3) 3_666 . . . ?
C22 Nd1 C21 C25 112.9(4) . . . . ?
P1 Nd1 C21 C25 -102.0(3) . . . . ?
C23 Nd1 C21 C25 76.6(3) . . . . ?
Nd1 Nd1 C21 C25 -65.7(3) 3_666 . . . ?
O1 Nd1 C21 C22 14.6(3) . . . . ?
C25 Nd1 C21 C22 -112.9(4) . . . . ?
C24 Nd1 C21 C22 -75.6(3) . . . . ?
P1 Nd1 C21 C22 -127.9(2) 3_666 . . . ?
P1 Nd1 C21 C22 145.1(2) . . . . ?
C23 Nd1 C21 C22 -36.3(2) . . . . ?
Nd1 Nd1 C21 C22 -178.6(2) 3_666 . . . ?
O1 Nd1 C21 C26 -110.0(4) . . . . ?
C25 Nd1 C21 C26 122.6(5) . . . . ?
C24 Nd1 C21 C26 159.8(5) . . . . ?
P1 Nd1 C21 C26 107.6(4) 3_666 . . . ?
C22 Nd1 C21 C26 -124.5(5) . . . . ?
P1 Nd1 C21 C26 20.6(4) . . . . ?
C23 Nd1 C21 C26 -160.8(5) . . . . ?
Nd1 Nd1 C21 C26 56.9(4) 3_666 . . . ?
C25 C21 C22 C23 0.1(5) . . . . ?
C26 C21 C22 C23 -174.8(4) . . . . ?
Nd1 C21 C22 C23 68.4(3) . . . . ?
C25 C21 C22 C27 175.3(4) . . . . ?
C26 C21 C22 C27 0.4(7) . . . . ?
Nd1 C21 C22 C27 -116.3(4) . . . . ?
C25 C21 C22 Nd1 -68.4(3) . . . . ?
C26 C21 C22 Nd1 116.8(5) . . . . ?
O1 Nd1 C22 C23 77.7(3) . . . . ?
C25 Nd1 C22 C23 -76.5(3) . . . . ?
C21 Nd1 C22 C23 -114.2(4) . . . . ?
C24 Nd1 C22 C23 -36.6(2) . . . . ?
P1 Nd1 C22 C23 -32.9(3) 3_666 . . . ?
P1 Nd1 C22 C23 -155.2(2) . . . . ?
Nd1 Nd1 C22 C23 -111.7(3) 3_666 . . . ?
O1 Nd1 C22 C21 -168.1(3) . . . . ?
C25 Nd1 C22 C21 37.7(3) . . . . ?
C24 Nd1 C22 C21 77.6(3) . . . . ?
P1 Nd1 C22 C21 81.3(3) 3_666 . . . ?
P1 Nd1 C22 C21 -41.0(3) . . . . ?
C23 Nd1 C22 C21 114.2(4) . . . . ?
Nd1 Nd1 C22 C21 2.5(4) 3_666 . . . ?
O1 Nd1 C22 C27 -46.5(4) . . . . ?
C25 Nd1 C22 C27 159.3(5) . . . . ?
C21 Nd1 C22 C27 121.6(5) . . . . ?
C24 Nd1 C22 C27 -160.8(5) . . . . ?
P1 Nd1 C22 C27 -157.1(3) 3_666 . . . ?
P1 Nd1 C22 C27 80.5(4) . . . . ?
C23 Nd1 C22 C27 -124.3(5) . . . . ?
Nd1 Nd1 C22 C27 124.0(4) 3_666 . . . ?
C21 C22 C23 C24 -0.2(5) . . . . ?
C27 C22 C23 C24 -175.4(4) . . . . ?
Nd1 C22 C23 C24 66.2(3) . . . . ?
C21 C22 C23 C28 173.0(4) . . . . ?
C27 C22 C23 C28 -2.2(7) . . . . ?
Nd1 C22 C23 C28 -120.6(4) . . . . ?
C21 C22 C23 Nd1 -66.4(3) . . . . ?
C27 C22 C23 Nd1 118.4(5) . . . . ?
O1 Nd1 C23 C22 -103.7(3) . . . . ?
C25 Nd1 C23 C22 77.5(3) . . . . ?
C21 Nd1 C23 C22 37.1(3) . . . . ?
C24 Nd1 C23 C22 114.6(4) . . . . ?
P1 Nd1 C23 C22 158.2(2) 3_666 . . . ?
P1 Nd1 C23 C22 39.5(3) . . . . ?
Nd1 Nd1 C23 C22 119.0(3) 3_666 . . . ?
O1 Nd1 C23 C24 141.6(3) . . . . ?
C25 Nd1 C23 C24 -37.1(2) . . . . ?
C21 Nd1 C23 C24 -77.6(3) . . . . ?
P1 Nd1 C23 C24 43.6(3) 3_666 . . . ?
C22 Nd1 C23 C24 -114.6(4) . . . . ?
P1 Nd1 C23 C24 -75.1(3) . . . . ?
Nd1 Nd1 C23 C24 4.4(4) 3_666 . . . ?
O1 Nd1 C23 C28 20.9(4) . . . . ?
C25 Nd1 C23 C28 -157.9(5) . . . . ?
C21 Nd1 C23 C28 161.7(5) . . . . ?
C24 Nd1 C23 C28 -120.8(5) . . . . ?
P1 Nd1 C23 C28 -77.1(4) 3_666 . . . ?
C22 Nd1 C23 C28 124.6(5) . . . . ?
P1 Nd1 C23 C28 164.1(3) . . . . ?
Nd1 Nd1 C23 C28 -116.4(4) 3_666 . . . ?
C22 C23 C24 C25 0.2(5) . . . . ?
C28 C23 C24 C25 -173.1(4) . . . . ?
Nd1 C23 C24 C25 67.5(3) . . . . ?
C22 C23 C24 C29 173.8(4) . . . . ?
C28 C23 C24 C29 0.5(7) . . . . ?
Nd1 C23 C24 C29 -118.9(4) . . . . ?
C22 C23 C24 Nd1 -67.3(3) . . . . ?
C28 C23 C24 Nd1 119.3(4) . . . . ?
O1 Nd1 C24 C25 -155.9(2) . . . . ?
C21 Nd1 C24 C25 -37.6(3) . . . . ?
P1 Nd1 C24 C25 104.7(2) 3_666 . . . ?
C22 Nd1 C24 C25 -77.6(3) . . . . ?
P1 Nd1 C24 C25 20.2(3) . . . . ?
C23 Nd1 C24 C25 -113.8(4) . . . . ?
Nd1 Nd1 C24 C25 68.9(3) 3_666 . . . ?
O1 Nd1 C24 C23 -42.1(3) . . . . ?
C25 Nd1 C24 C23 113.8(4) . . . . ?
C21 Nd1 C24 C23 76.1(3) . . . . ?
P1 Nd1 C24 C23 -141.5(2) 3_666 . . . ?
C22 Nd1 C24 C23 36.2(2) . . . . ?
P1 Nd1 C24 C23 133.9(2) . . . . ?
Nd1 Nd1 C24 C23 -177.3(2) 3_666 . . . ?
O1 Nd1 C24 C29 80.6(4) . . . . ?
C25 Nd1 C24 C29 -123.6(5) . . . . ?
C21 Nd1 C24 C29 -161.2(5) . . . . ?
P1 Nd1 C24 C29 -18.8(4) 3_666 . . . ?
C22 Nd1 C24 C29 158.9(5) . . . . ?
P1 Nd1 C24 C29 -103.4(4) . . . . ?
C23 Nd1 C24 C29 122.7(5) . . . . ?
Nd1 Nd1 C24 C29 -54.7(4) 3_666 . . . ?
C23 C24 C25 C21 -0.2(5) . . . . ?
C29 C24 C25 C21 -173.6(4) . . . . ?
Nd1 C24 C25 C21 69.9(3) . . . . ?
C23 C24 C25 C30 175.6(4) . . . . ?
C29 C24 C25 C30 2.3(7) . . . . ?
Nd1 C24 C25 C30 -114.3(5) . . . . ?
C23 C24 C25 Nd1 -70.1(3) . . . . ?
C29 C24 C25 Nd1 116.5(4) . . . . ?
C22 C21 C25 C24 0.1(5) . . . . ?
C26 C21 C25 C24 175.0(4) . . . . ?
Nd1 C21 C25 C24 -70.5(3) . . . . ?
C22 C21 C25 C30 -175.8(4) . . . . ?
C26 C21 C25 C30 -0.9(7) . . . . ?
Nd1 C21 C25 C30 113.6(5) . . . . ?
C22 C21 C25 Nd1 70.6(3) . . . . ?
C26 C21 C25 Nd1 -114.5(5) . . . . ?
O1 Nd1 C25 C24 34.9(3) . . . . ?
C21 Nd1 C25 C24 113.0(4) . . . . ?
P1 Nd1 C25 C24 -78.8(3) 3_666 . . . ?
C22 Nd1 C25 C24 75.7(3) . . . . ?
P1 Nd1 C25 C24 -164.3(2) . . . . ?
C23 Nd1 C25 C24 36.7(2) . . . . ?
Nd1 Nd1 C25 C24 -121.8(2) 3_666 . . . ?
O1 Nd1 C25 C21 -78.1(3) . . . . ?
C24 Nd1 C25 C21 -113.0(4) . . . . ?
P1 Nd1 C25 C21 168.3(2) 3_666 . . . ?
C22 Nd1 C25 C21 -37.3(2) . . . . ?
P1 Nd1 C25 C21 82.7(3) . . . . ?
C23 Nd1 C25 C21 -76.3(3) . . . . ?
Nd1 Nd1 C25 C21 125.2(2) 3_666 . . . ?
O1 Nd1 C25 C30 159.3(3) . . . . ?
C21 Nd1 C25 C30 -122.6(5) . . . . ?
C24 Nd1 C25 C30 124.4(5) . . . . ?
P1 Nd1 C25 C30 45.7(4) 3_666 . . . ?
C22 Nd1 C25 C30 -159.9(4) . . . . ?
P1 Nd1 C25 C30 -39.9(4) . . . . ?
C23 Nd1 C25 C30 161.1(4) . . . . ?
Nd1 Nd1 C25 C30 2.6(4) 3_666 . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.710
_refine_diff_density_min -0.675
_refine_diff_density_rms 0.088
# Attachment 'complex_3.cif'
#==============================================================================
data_a
_database_code_depnum_ccdc_archive 'CCDC 763479'
#TrackingRef 'complex_3.cif'
_audit_update_record
;
2010-05-11 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis[bis(3-phenyl-1H-pyrazolyl)(5-phenyl-1H-pyrazolyl)borate-
\h^3^-\kN^2'^,N^2''^,N^2'''^]bis{\m-[2,6-
(1-methylethyl)phenyl]phosphinidene}di(tetrahydrofuran)dineodymium(III),
tetrahydrofuran adduct
;
_chemical_name_common
;
Bis(bis(3-phenyl-1H-pyrazolyl)(5-phenyl-1H-pyrazolyl)borate-
eta$3!-kappaN$2'!,N$2''!,N$2'''!)bis(mu-(2,6-(1-
methylethyl)phenyl)phosphinidene)di(tetrahydrofuran)dineodymium(iii),
tetrahydrofuran adduct
;
_chemical_melting_point ?
_chemical_formula_moiety 'C86 H94 B2 N12 Nd2 O2 P2, C4 H8 O'
_chemical_formula_sum 'C90 H102 B2 N12 Nd2 O3 P2'
_chemical_formula_weight 1771.88
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.9838(16)
_cell_length_b 14.2191(19)
_cell_length_c 14.739(2)
_cell_angle_alpha 98.263(2)
_cell_angle_beta 109.668(2)
_cell_angle_gamma 109.723(2)
_cell_volume 2130.4(5)
_cell_formula_units_Z 1
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 2669
_cell_measurement_theta_min 2.26
_cell_measurement_theta_max 23.92
_exptl_crystal_description Block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.26
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.381
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 910
_exptl_absorpt_coefficient_mu 1.299
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6521
_exptl_absorpt_correction_T_max 0.7289
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'BRUKER SMART CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 10502
_diffrn_reflns_av_R_equivalents 0.0375
_diffrn_reflns_av_sigmaI/netI 0.0827
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.86
_diffrn_reflns_theta_max 25.10
_reflns_number_total 7428
_reflns_number_gt 5860
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'BRUKER AXS APEX-2 V1.0-8 (Bruker, 2007)'
_computing_cell_refinement 'SAINT v7.34A (Bruker, 2007)'
_computing_data_reduction 'SAINT v7.34A (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7428
_refine_ls_number_parameters 550
_refine_ls_number_restraints 159
_refine_ls_R_factor_all 0.0727
_refine_ls_R_factor_gt 0.0535
_refine_ls_wR_factor_ref 0.1247
_refine_ls_wR_factor_gt 0.1179
_refine_ls_goodness_of_fit_ref 0.980
_refine_ls_restrained_S_all 0.974
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1S O 0.943(2) 0.5429(18) 0.9373(17) 0.177(7) Uani 0.50 1 d PDU A -1
C1S C 1.033(3) 0.5812(14) 1.0398(17) 0.170(8) Uani 0.50 1 d PDU A -1
H1SB H 1.0226 0.6377 1.0758 0.205 Uiso 0.50 1 calc PR A -1
H1SA H 1.1221 0.6065 1.0451 0.205 Uiso 0.50 1 calc PR A -1
C2S C 1.004(3) 0.491(2) 1.0810(14) 0.151(7) Uani 0.50 1 d PDU A -1
H2SA H 0.9385 0.4866 1.1065 0.181 Uiso 0.50 1 calc PR A -1
H2SB H 1.0821 0.4962 1.1347 0.181 Uiso 0.50 1 calc PR A -1
C3S C 0.956(3) 0.3989(15) 0.993(2) 0.171(8) Uani 0.50 1 d PDU A -1
H3SB H 1.0256 0.3798 0.9914 0.205 Uiso 0.50 1 calc PR A -1
H3SA H 0.8875 0.3393 0.9946 0.205 Uiso 0.50 1 calc PR A -1
C4S C 0.904(3) 0.4337(19) 0.9040(15) 0.171(8) Uani 0.50 1 d PDU A -1
H4SB H 0.9383 0.4177 0.8556 0.206 Uiso 0.50 1 calc PR A -1
H4SA H 0.8100 0.3981 0.8718 0.206 Uiso 0.50 1 calc PR A -1
Nd1 Nd 0.91357(3) 0.87883(2) 0.56220(2) 0.03590(12) Uani 1 1 d . . .
P1 P 0.95021(16) 0.90546(11) 0.38949(11) 0.0416(4) Uani 1 1 d . . .
N1 N 0.9111(4) 0.8442(4) 0.7380(4) 0.0451(12) Uani 1 1 d . . .
N2 N 0.9606(5) 0.7740(4) 0.7701(4) 0.0507(13) Uani 1 1 d . . .
N3 N 1.0999(5) 0.8282(4) 0.6240(4) 0.0484(12) Uani 1 1 d . . .
N4 N 1.1194(5) 0.7733(4) 0.6911(4) 0.0436(12) Uani 1 1 d . . .
N5 N 0.8149(4) 0.6710(4) 0.5393(4) 0.0438(12) Uani 1 1 d . . .
N6 N 0.8847(5) 0.6371(4) 0.6106(4) 0.0481(12) Uani 1 1 d . . .
C1 C 0.8745(5) 0.8086(4) 0.2652(4) 0.0407(13) Uani 1 1 d . . .
C2 C 0.8884(6) 0.7129(5) 0.2559(5) 0.0480(15) Uani 1 1 d . . .
C3 C 0.8311(7) 0.6408(5) 0.1613(5) 0.067(2) Uani 1 1 d . . .
H3 H 0.8401 0.5780 0.1552 0.080 Uiso 1 1 calc R . .
C4 C 0.7616(8) 0.6606(6) 0.0769(5) 0.079(2) Uani 1 1 d . . .
H4 H 0.7232 0.6113 0.0143 0.095 Uiso 1 1 calc R . .
C5 C 0.7489(7) 0.7528(5) 0.0851(5) 0.0609(18) Uani 1 1 d . . .
H5 H 0.7025 0.7660 0.0275 0.073 Uiso 1 1 calc R . .
C6 C 0.8033(6) 0.8266(5) 0.1767(4) 0.0461(14) Uani 1 1 d . . .
C7 C 0.9640(6) 0.6850(5) 0.3468(5) 0.0540(16) Uani 1 1 d . . .
H7 H 0.9623 0.7249 0.4060 0.065 Uiso 1 1 calc R . .
C8 C 1.1065(7) 0.7212(6) 0.3642(6) 0.073(2) Uani 1 1 d . . .
H8B H 1.1533 0.7068 0.4236 0.109 Uiso 1 1 calc R . .
H8C H 1.1434 0.7949 0.3726 0.109 Uiso 1 1 calc R . .
H8A H 1.1127 0.6847 0.3072 0.109 Uiso 1 1 calc R . .
C9 C 0.9070(8) 0.5717(5) 0.3431(6) 0.074(2) Uani 1 1 d . . .
H9B H 0.9169 0.5304 0.2913 0.111 Uiso 1 1 calc R . .
H9A H 0.8162 0.5493 0.3287 0.111 Uiso 1 1 calc R . .
H9C H 0.9515 0.5633 0.4069 0.111 Uiso 1 1 calc R . .
C10 C 0.7768(7) 0.9245(5) 0.1798(5) 0.0561(17) Uani 1 1 d . . .
H10 H 0.8477 0.9783 0.2405 0.067 Uiso 1 1 calc R . .
C11 C 0.7814(10) 0.9677(7) 0.0909(6) 0.102(3) Uani 1 1 d . . .
H11A H 0.7060 0.9224 0.0307 0.152 Uiso 1 1 calc R . .
H11B H 0.8585 0.9714 0.0822 0.152 Uiso 1 1 calc R . .
H11C H 0.7827 1.0362 0.1042 0.152 Uiso 1 1 calc R . .
C12 C 0.6543(8) 0.9084(7) 0.1931(7) 0.088(3) Uani 1 1 d . . .
H12A H 0.5838 0.8476 0.1417 0.131 Uiso 1 1 calc R . .
H12C H 0.6354 0.9684 0.1879 0.131 Uiso 1 1 calc R . .
H12B H 0.6648 0.8988 0.2581 0.131 Uiso 1 1 calc R . .
C20 C 0.9457(8) 0.7620(6) 0.8538(6) 0.074(2) Uani 1 1 d . . .
H20 H 0.9709 0.7184 0.8894 0.089 Uiso 1 1 calc R . .
C21 C 0.8891(9) 0.8219(7) 0.8793(6) 0.083(3) Uani 1 1 d . . .
H21 H 0.8698 0.8287 0.9353 0.100 Uiso 1 1 calc R . .
C22 C 0.8654(6) 0.8715(5) 0.8050(5) 0.0549(16) Uani 1 1 d . . .
C23 C 0.8057(7) 0.9464(5) 0.8007(5) 0.0538(16) Uani 1 1 d . . .
C24 C 0.8547(8) 1.0386(6) 0.7806(6) 0.079(2) Uani 1 1 d . . .
H24 H 0.9245 1.0537 0.7623 0.094 Uiso 1 1 calc R . .
C25 C 0.8006(11) 1.1093(8) 0.7876(8) 0.109(3) Uani 1 1 d . . .
H25 H 0.8355 1.1727 0.7752 0.131 Uiso 1 1 calc R . .
C26 C 0.6974(11) 1.0879(9) 0.8123(7) 0.107(3) Uani 1 1 d . . .
H26 H 0.6610 1.1360 0.8149 0.128 Uiso 1 1 calc R . .
C27 C 0.6467(8) 0.9978(8) 0.8332(6) 0.086(3) Uani 1 1 d . . .
H27 H 0.5767 0.9836 0.8511 0.104 Uiso 1 1 calc R . .
C28 C 0.7017(7) 0.9268(6) 0.8272(5) 0.071(2) Uani 1 1 d . . .
H28 H 0.6676 0.8644 0.8414 0.085 Uiso 1 1 calc R . .
C29 C 1.2069(7) 0.8611(5) 0.6085(5) 0.0600(18) Uani 1 1 d . . .
H29 H 1.2199 0.9001 0.5645 0.072 Uiso 1 1 calc R . .
C30 C 1.2977(6) 0.8296(5) 0.6670(5) 0.0595(18) Uani 1 1 d . . .
H30 H 1.3807 0.8435 0.6701 0.071 Uiso 1 1 calc R . .
C31 C 1.2390(6) 0.7741(5) 0.7188(5) 0.0493(15) Uani 1 1 d . . .
C32 C 1.2951(6) 0.7285(5) 0.7945(5) 0.0505(16) Uani 1 1 d . . .
C33 C 1.3679(7) 0.6760(5) 0.7794(5) 0.0636(19) Uani 1 1 d . . .
H33 H 1.3795 0.6692 0.7200 0.076 Uiso 1 1 calc R . .
C34 C 1.4239(8) 0.6335(6) 0.8502(7) 0.082(3) Uani 1 1 d . . .
H34 H 1.4717 0.5975 0.8379 0.099 Uiso 1 1 calc R . .
C35 C 1.4093(8) 0.6439(7) 0.9383(7) 0.088(3) Uani 1 1 d . . .
H35 H 1.4453 0.6136 0.9854 0.105 Uiso 1 1 calc R . .
C36 C 1.3416(8) 0.6992(7) 0.9575(6) 0.084(3) Uani 1 1 d . . .
H36 H 1.3345 0.7090 1.0187 0.101 Uiso 1 1 calc R . .
C37 C 1.2845(8) 0.7401(6) 0.8859(6) 0.077(2) Uani 1 1 d . . .
H37 H 1.2374 0.7766 0.8990 0.092 Uiso 1 1 calc R . .
C38 C 0.8241(7) 0.5337(5) 0.5872(6) 0.0619(18) Uani 1 1 d . . .
H38 H 0.8535 0.4925 0.6240 0.074 Uiso 1 1 calc R . .
C39 C 0.7148(7) 0.4979(5) 0.5030(6) 0.0651(19) Uani 1 1 d . . .
H39 H 0.6543 0.4289 0.4715 0.078 Uiso 1 1 calc R . .
C40 C 0.7103(6) 0.5850(5) 0.4722(5) 0.0481(15) Uani 1 1 d . . .
C41 C 0.6079(6) 0.5848(5) 0.3817(5) 0.0500(15) Uani 1 1 d . . .
C42 C 0.6363(6) 0.6535(5) 0.3278(5) 0.0538(16) Uani 1 1 d . . .
H42 H 0.7200 0.7053 0.3506 0.065 Uiso 1 1 calc R . .
C43 C 0.5397(8) 0.6449(6) 0.2398(6) 0.074(2) Uani 1 1 d . . .
H43 H 0.5606 0.6900 0.2023 0.089 Uiso 1 1 calc R . .
C44 C 0.4164(8) 0.5739(7) 0.2057(6) 0.083(2) Uani 1 1 d . . .
H44 H 0.3525 0.5713 0.1468 0.099 Uiso 1 1 calc R . .
C45 C 0.3858(7) 0.5043(7) 0.2601(6) 0.084(3) Uani 1 1 d . . .
H45 H 0.3013 0.4539 0.2375 0.100 Uiso 1 1 calc R . .
C46 C 0.4818(7) 0.5107(6) 0.3477(6) 0.068(2) Uani 1 1 d . . .
H46 H 0.4616 0.4645 0.3844 0.081 Uiso 1 1 calc R . .
O1 O 0.6875(4) 0.8509(3) 0.5280(3) 0.0574(11) Uani 1 1 d DU B .
C47 C 0.5903(6) 0.7788(5) 0.5502(5) 0.0623(17) Uani 1 1 d DU . .
H47D H 0.5965 0.8079 0.6164 0.075 Uiso 0.53(2) 1 calc PR B 3
H47C H 0.5999 0.7136 0.5480 0.075 Uiso 0.53(2) 1 calc PR B 3
H47B H 0.6267 0.7739 0.6172 0.075 Uiso 0.47(2) 1 d PR B 2
H47A H 0.5540 0.7109 0.5034 0.075 Uiso 0.47(2) 1 d PR B 2
C48 C 0.4703(12) 0.7971(18) 0.5094(17) 0.101(8) Uani 0.47(2) 1 d PDU B 2
H48B H 0.4676 0.8482 0.5589 0.121 Uiso 0.47(2) 1 calc PR B 2
H48A H 0.3923 0.7330 0.4854 0.121 Uiso 0.47(2) 1 calc PR B 2
C49 C 0.4878(10) 0.8395(12) 0.4213(11) 0.084(5) Uani 0.47(2) 1 d PDU B 2
H49A H 0.4708 0.7847 0.3645 0.101 Uiso 0.47(2) 1 calc PR B 2
H49B H 0.4340 0.8768 0.3992 0.101 Uiso 0.47(2) 1 calc PR B 2
C50 C 0.6297(7) 0.9114(7) 0.4756(8) 0.096(3) Uani 1 1 d DU . .
H50C H 0.6270 0.8997 0.4083 0.115 Uiso 0.53(2) 1 calc PR B 3
H50D H 0.6801 0.9852 0.5111 0.115 Uiso 0.53(2) 1 calc PR B 3
H50A H 0.6579 0.9236 0.4230 0.115 Uiso 0.47(2) 1 d PR B 2
H50B H 0.6526 0.9775 0.5204 0.115 Uiso 0.47(2) 1 d PR B 2
C49A C 0.4949(11) 0.8776(11) 0.4707(17) 0.096(6) Uani 0.53(2) 1 d PDU B 3
H49C H 0.4356 0.8829 0.4099 0.115 Uiso 0.53(2) 1 calc PR B 3
H49D H 0.4932 0.9174 0.5291 0.115 Uiso 0.53(2) 1 calc PR B 3
C48A C 0.4633(8) 0.7622(10) 0.4700(11) 0.065(4) Uani 0.53(2) 1 d PDU B 3
H48D H 0.3911 0.7330 0.4882 0.078 Uiso 0.53(2) 1 calc PR B 3
H48C H 0.4458 0.7185 0.4055 0.078 Uiso 0.53(2) 1 calc PR B 3
B1 B 1.0029(7) 0.7072(6) 0.7096(6) 0.0492(18) Uani 1 1 d . . .
H1 H 1.032(6) 0.658(5) 0.755(5) 0.065(19) Uiso 1 1 d . . .
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
O1S 0.182(14) 0.175(11) 0.171(11) 0.072(9) 0.056(10) 0.078(11)
C1S 0.178(15) 0.171(10) 0.171(12) 0.082(9) 0.059(11) 0.082(12)
C2S 0.166(15) 0.156(12) 0.181(10) 0.076(9) 0.079(11) 0.106(11)
C3S 0.170(15) 0.171(10) 0.175(14) 0.061(9) 0.052(12) 0.090(12)
C4S 0.164(15) 0.184(11) 0.181(10) 0.068(9) 0.056(11) 0.099(12)
Nd1 0.03593(18) 0.03104(18) 0.04209(19) 0.01565(13) 0.01771(13) 0.01180(13)
P1 0.0494(9) 0.0310(8) 0.0393(8) 0.0093(6) 0.0189(7) 0.0106(7)
N1 0.039(3) 0.052(3) 0.053(3) 0.022(2) 0.024(2) 0.021(2)
N2 0.052(3) 0.059(3) 0.051(3) 0.031(3) 0.022(3) 0.027(3)
N3 0.047(3) 0.052(3) 0.062(3) 0.031(3) 0.030(3) 0.025(3)
N4 0.042(3) 0.048(3) 0.049(3) 0.023(2) 0.021(2) 0.022(2)
N5 0.038(3) 0.038(3) 0.055(3) 0.019(2) 0.017(2) 0.015(2)
N6 0.047(3) 0.038(3) 0.064(3) 0.025(2) 0.023(3) 0.018(2)
C1 0.037(3) 0.032(3) 0.045(3) 0.005(3) 0.018(3) 0.007(3)
C2 0.039(3) 0.041(3) 0.061(4) 0.008(3) 0.026(3) 0.011(3)
C3 0.072(5) 0.047(4) 0.064(5) -0.011(4) 0.022(4) 0.023(4)
C4 0.087(6) 0.071(5) 0.049(4) -0.016(4) 0.011(4) 0.029(5)
C5 0.061(4) 0.062(5) 0.040(4) 0.003(3) 0.014(3) 0.015(4)
C6 0.042(3) 0.047(4) 0.042(3) 0.011(3) 0.018(3) 0.009(3)
C7 0.060(4) 0.042(4) 0.063(4) 0.012(3) 0.027(3) 0.025(3)
C8 0.055(5) 0.068(5) 0.093(6) 0.025(4) 0.025(4) 0.027(4)
C9 0.082(5) 0.046(4) 0.112(6) 0.031(4) 0.052(5) 0.031(4)
C10 0.064(4) 0.044(4) 0.044(4) 0.010(3) 0.008(3) 0.019(3)
C11 0.139(9) 0.081(6) 0.064(5) 0.032(5) 0.019(5) 0.039(6)
C12 0.073(6) 0.083(6) 0.105(7) 0.007(5) 0.029(5) 0.047(5)
C20 0.104(6) 0.088(6) 0.070(5) 0.054(4) 0.052(5) 0.057(5)
C21 0.127(7) 0.113(7) 0.066(5) 0.056(5) 0.067(5) 0.075(6)
C22 0.055(4) 0.066(4) 0.052(4) 0.022(3) 0.030(3) 0.024(4)
C23 0.062(4) 0.067(4) 0.046(4) 0.026(3) 0.029(3) 0.032(4)
C24 0.100(6) 0.087(6) 0.095(6) 0.048(5) 0.069(5) 0.053(5)
C25 0.159(10) 0.096(7) 0.146(9) 0.065(7) 0.109(8) 0.080(8)
C26 0.149(10) 0.140(10) 0.103(7) 0.060(7) 0.075(7) 0.110(9)
C27 0.075(6) 0.131(8) 0.072(5) 0.024(5) 0.038(5) 0.059(6)
C28 0.070(5) 0.091(6) 0.067(5) 0.033(4) 0.045(4) 0.032(5)
C29 0.059(4) 0.059(4) 0.072(5) 0.035(4) 0.036(4) 0.020(4)
C30 0.043(4) 0.075(5) 0.073(5) 0.030(4) 0.029(3) 0.030(4)
C31 0.044(4) 0.053(4) 0.052(4) 0.018(3) 0.016(3) 0.024(3)
C32 0.043(4) 0.041(4) 0.054(4) 0.010(3) 0.008(3) 0.016(3)
C33 0.057(4) 0.064(5) 0.064(4) 0.019(4) 0.012(4) 0.031(4)
C34 0.062(5) 0.073(6) 0.099(7) 0.023(5) 0.010(5) 0.039(4)
C35 0.065(5) 0.083(6) 0.095(7) 0.042(5) 0.007(5) 0.028(5)
C36 0.068(5) 0.108(7) 0.063(5) 0.037(5) 0.011(4) 0.032(5)
C37 0.074(5) 0.096(6) 0.062(5) 0.028(4) 0.019(4) 0.045(5)
C38 0.069(5) 0.043(4) 0.085(5) 0.032(4) 0.037(4) 0.025(4)
C39 0.066(5) 0.042(4) 0.079(5) 0.023(4) 0.027(4) 0.013(4)
C40 0.052(4) 0.035(3) 0.058(4) 0.016(3) 0.032(3) 0.009(3)
C41 0.048(4) 0.038(4) 0.056(4) 0.009(3) 0.022(3) 0.010(3)
C42 0.042(4) 0.046(4) 0.064(4) 0.013(3) 0.021(3) 0.009(3)
C43 0.066(5) 0.069(5) 0.072(5) 0.026(4) 0.022(4) 0.016(4)
C44 0.056(5) 0.103(7) 0.069(5) 0.015(5) 0.009(4) 0.031(5)
C45 0.040(4) 0.080(6) 0.081(6) -0.002(5) 0.009(4) -0.008(4)
C46 0.050(4) 0.059(5) 0.081(5) 0.019(4) 0.033(4) 0.002(4)
O1 0.044(2) 0.049(3) 0.084(3) 0.029(2) 0.029(2) 0.019(2)
C47 0.051(4) 0.058(4) 0.075(5) 0.021(3) 0.030(3) 0.014(3)
C48 0.066(7) 0.112(17) 0.161(18) 0.052(15) 0.073(11) 0.048(9)
C49 0.076(6) 0.079(11) 0.102(12) 0.021(9) 0.021(7) 0.057(6)
C50 0.074(4) 0.089(6) 0.154(8) 0.074(5) 0.053(5) 0.046(4)
C49A 0.073(7) 0.081(9) 0.151(18) 0.036(11) 0.046(10) 0.051(8)
C48A 0.046(4) 0.079(8) 0.096(11) 0.034(9) 0.043(5) 0.037(5)
B1 0.051(4) 0.050(4) 0.065(5) 0.034(4) 0.027(4) 0.034(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1S C4S 1.417(6) . ?
O1S C1S 1.419(6) . ?
C1S C2S 1.483(6) . ?
C1S H1SB 0.9700 . ?
C1S H1SA 0.9700 . ?
C2S C3S 1.495(6) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C3S C4S 1.476(6) . ?
C3S H3SB 0.9700 . ?
C3S H3SA 0.9700 . ?
C4S H4SB 0.9700 . ?
C4S H4SA 0.9700 . ?
Nd1 O1 2.460(4) . ?
Nd1 N3 2.497(5) . ?
Nd1 N5 2.707(5) . ?
Nd1 N1 2.714(5) . ?
Nd1 P1 2.7808(16) . ?
Nd1 P1 2.7911(15) 2_776 ?
P1 C1 1.841(6) . ?
P1 Nd1 2.7910(15) 2_776 ?
N1 C22 1.350(7) . ?
N1 N2 1.386(6) . ?
N2 C20 1.330(8) . ?
N2 B1 1.530(9) . ?
N3 C29 1.319(8) . ?
N3 N4 1.354(6) . ?
N4 C31 1.346(7) . ?
N4 B1 1.533(9) . ?
N5 C40 1.352(7) . ?
N5 N6 1.366(6) . ?
N6 C38 1.331(8) . ?
N6 B1 1.539(9) . ?
C1 C6 1.409(8) . ?
C1 C2 1.419(8) . ?
C2 C3 1.392(8) . ?
C2 C7 1.534(9) . ?
C3 C4 1.373(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(8) . ?
C5 H5 0.9300 . ?
C6 C10 1.527(8) . ?
C7 C9 1.506(9) . ?
C7 C8 1.524(9) . ?
C7 H7 0.9800 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 H8A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C12 1.492(10) . ?
C10 C11 1.535(10) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12B 0.9600 . ?
C20 C21 1.339(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.388(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.467(9) . ?
C23 C24 1.365(10) . ?
C23 C28 1.382(9) . ?
C24 C25 1.377(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.356(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.349(13) . ?
C26 H26 0.9300 . ?
C27 C28 1.386(11) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.392(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.364(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.454(8) . ?
C32 C33 1.374(9) . ?
C32 C37 1.388(10) . ?
C33 C34 1.375(10) . ?
C33 H33 0.9300 . ?
C34 C35 1.360(12) . ?
C34 H34 0.9300 . ?
C35 C36 1.371(12) . ?
C35 H35 0.9300 . ?
C36 C37 1.370(10) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.337(9) . ?
C38 H38 0.9300 . ?
C39 C40 1.390(8) . ?
C39 H39 0.9300 . ?
C40 C41 1.477(9) . ?
C41 C42 1.372(9) . ?
C41 C46 1.382(9) . ?
C42 C43 1.373(9) . ?
C42 H42 0.9300 . ?
C43 C44 1.343(10) . ?
C43 H43 0.9300 . ?
C44 C45 1.392(11) . ?
C44 H44 0.9300 . ?
C45 C46 1.376(10) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
O1 C50 1.432(7) . ?
O1 C47 1.435(6) . ?
C47 C48 1.488(10) . ?
C47 C48A 1.495(10) . ?
C47 H47D 0.9700 . ?
C47 H47C 0.9700 . ?
C47 H47B 0.9598 . ?
C47 H47A 0.9601 . ?
C48 C49 1.554(15) . ?
C48 H48B 0.9700 . ?
C48 H48A 0.9700 . ?
C49 C50 1.501(10) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C49A 1.495(10) . ?
C50 H50C 0.9700 . ?
C50 H50D 0.9700 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9598 . ?
C49A C48A 1.551(15) . ?
C49A H49C 0.9700 . ?
C49A H49D 0.9700 . ?
C48A H48D 0.9700 . ?
C48A H48C 0.9700 . ?
B1 H1 1.09(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4S O1S C1S 108.7(6) . . ?
O1S C1S C2S 105.5(7) . . ?
O1S C1S H1SB 110.6 . . ?
C2S C1S H1SB 110.6 . . ?
O1S C1S H1SA 110.6 . . ?
C2S C1S H1SA 110.6 . . ?
H1SB C1S H1SA 108.8 . . ?
C1S C2S C3S 103.7(7) . . ?
C1S C2S H2SA 111.0 . . ?
C3S C2S H2SA 111.0 . . ?
C1S C2S H2SB 111.0 . . ?
C3S C2S H2SB 111.0 . . ?
H2SA C2S H2SB 109.0 . . ?
C4S C3S C2S 104.7(6) . . ?
C4S C3S H3SB 110.8 . . ?
C2S C3S H3SB 110.8 . . ?
C4S C3S H3SA 110.8 . . ?
C2S C3S H3SA 110.8 . . ?
H3SB C3S H3SA 108.9 . . ?
O1S C4S C3S 108.1(5) . . ?
O1S C4S H4SB 110.1 . . ?
C3S C4S H4SB 110.1 . . ?
O1S C4S H4SA 110.1 . . ?
C3S C4S H4SA 110.1 . . ?
H4SB C4S H4SA 108.4 . . ?
O1 Nd1 N3 150.98(15) . . ?
O1 Nd1 N5 81.82(13) . . ?
N3 Nd1 N5 72.04(15) . . ?
O1 Nd1 N1 81.49(14) . . ?
N3 Nd1 N1 78.01(15) . . ?
N5 Nd1 N1 70.17(15) . . ?
O1 Nd1 P1 107.16(11) . . ?
N3 Nd1 P1 92.69(12) . . ?
N5 Nd1 P1 107.11(11) . . ?
N1 Nd1 P1 170.70(10) . . ?
O1 Nd1 P1 105.10(10) . 2_776 ?
N3 Nd1 P1 99.84(12) . 2_776 ?
N5 Nd1 P1 170.95(10) . 2_776 ?
N1 Nd1 P1 104.68(11) . 2_776 ?
P1 Nd1 P1 76.75(5) . 2_776 ?
C1 P1 Nd1 128.01(19) . . ?
C1 P1 Nd1 127.67(19) . 2_776 ?
Nd1 P1 Nd1 103.25(5) . 2_776 ?
C22 N1 N2 105.5(5) . . ?
C22 N1 Nd1 137.7(4) . . ?
N2 N1 Nd1 116.6(3) . . ?
C20 N2 N1 108.7(5) . . ?
C20 N2 B1 125.3(5) . . ?
N1 N2 B1 125.2(5) . . ?
C29 N3 N4 106.0(5) . . ?
C29 N3 Nd1 126.7(4) . . ?
N4 N3 Nd1 126.7(4) . . ?
C31 N4 N3 110.6(5) . . ?
C31 N4 B1 130.0(5) . . ?
N3 N4 B1 118.5(5) . . ?
C40 N5 N6 106.3(4) . . ?
C40 N5 Nd1 137.1(4) . . ?
N6 N5 Nd1 116.7(3) . . ?
C38 N6 N5 108.9(5) . . ?
C38 N6 B1 124.9(5) . . ?
N5 N6 B1 125.7(5) . . ?
C6 C1 C2 117.8(5) . . ?
C6 C1 P1 122.1(4) . . ?
C2 C1 P1 120.1(4) . . ?
C3 C2 C1 119.4(6) . . ?
C3 C2 C7 118.2(6) . . ?
C1 C2 C7 122.4(5) . . ?
C4 C3 C2 121.1(6) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.8(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.4(7) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 120.5(6) . . ?
C5 C6 C10 117.8(6) . . ?
C1 C6 C10 121.6(5) . . ?
C9 C7 C8 110.7(5) . . ?
C9 C7 C2 115.1(6) . . ?
C8 C7 C2 110.6(6) . . ?
C9 C7 H7 106.7 . . ?
C8 C7 H7 106.7 . . ?
C2 C7 H7 106.7 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
C12 C10 C6 111.3(6) . . ?
C12 C10 C11 112.6(7) . . ?
C6 C10 C11 113.5(6) . . ?
C12 C10 H10 106.3 . . ?
C6 C10 H10 106.3 . . ?
C11 C10 H10 106.3 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
N2 C20 C21 110.2(6) . . ?
N2 C20 H20 124.9 . . ?
C21 C20 H20 124.9 . . ?
C20 C21 C22 105.8(6) . . ?
C20 C21 H21 127.1 . . ?
C22 C21 H21 127.1 . . ?
N1 C22 C21 109.7(6) . . ?
N1 C22 C23 124.1(6) . . ?
C21 C22 C23 126.1(6) . . ?
C24 C23 C28 118.2(7) . . ?
C24 C23 C22 123.3(6) . . ?
C28 C23 C22 118.2(6) . . ?
C23 C24 C25 119.8(8) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 121.0(9) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C27 C26 C25 120.9(9) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C28 118.3(8) . . ?
C26 C27 H27 120.9 . . ?
C28 C27 H27 120.9 . . ?
C23 C28 C27 121.8(8) . . ?
C23 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
N3 C29 C30 110.7(6) . . ?
N3 C29 H29 124.6 . . ?
C30 C29 H29 124.6 . . ?
C31 C30 C29 105.3(6) . . ?
C31 C30 H30 127.3 . . ?
C29 C30 H30 127.3 . . ?
N4 C31 C30 107.4(5) . . ?
N4 C31 C32 125.2(6) . . ?
C30 C31 C32 127.4(6) . . ?
C33 C32 C37 117.1(6) . . ?
C33 C32 C31 120.2(6) . . ?
C37 C32 C31 122.6(6) . . ?
C32 C33 C34 121.6(8) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C35 C34 C33 120.0(8) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0(8) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 119.6(9) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C32 121.6(8) . . ?
C36 C37 H37 119.2 . . ?
C32 C37 H37 119.2 . . ?
N6 C38 C39 110.1(6) . . ?
N6 C38 H38 124.9 . . ?
C39 C38 H38 124.9 . . ?
C38 C39 C40 105.7(6) . . ?
C38 C39 H39 127.1 . . ?
C40 C39 H39 127.1 . . ?
N5 C40 C39 109.0(6) . . ?
N5 C40 C41 125.0(5) . . ?
C39 C40 C41 126.0(6) . . ?
C42 C41 C46 119.1(6) . . ?
C42 C41 C40 121.4(6) . . ?
C46 C41 C40 119.3(6) . . ?
C41 C42 C43 119.3(7) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C44 C43 C42 122.5(8) . . ?
C44 C43 H43 118.7 . . ?
C42 C43 H43 118.7 . . ?
C43 C44 C45 118.8(7) . . ?
C43 C44 H44 120.6 . . ?
C45 C44 H44 120.6 . . ?
C46 C45 C44 119.4(7) . . ?
C46 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
C45 C46 C41 120.8(7) . . ?
C45 C46 H46 119.6 . . ?
C41 C46 H46 119.6 . . ?
C50 O1 C47 107.3(5) . . ?
C50 O1 Nd1 121.0(4) . . ?
C47 O1 Nd1 131.7(3) . . ?
O1 C47 C48 107.4(6) . . ?
O1 C47 C48A 104.8(6) . . ?
O1 C47 H47D 110.8 . . ?
C48A C47 H47D 110.8 . . ?
O1 C47 H47C 110.8 . . ?
C48A C47 H47C 110.8 . . ?
H47D C47 H47C 108.9 . . ?
O1 C47 H47B 111.2 . . ?
C48 C47 H47B 123.6 . . ?
O1 C47 H47A 109.6 . . ?
C48 C47 H47A 94.9 . . ?
H47B C47 H47A 108.7 . . ?
C47 C48 C49 100.6(8) . . ?
C47 C48 H48B 111.7 . . ?
C49 C48 H48B 111.7 . . ?
C47 C48 H48A 111.7 . . ?
C49 C48 H48A 111.7 . . ?
H48B C48 H48A 109.4 . . ?
C50 C49 C48 98.0(8) . . ?
C50 C49 H49A 112.2 . . ?
C48 C49 H49A 112.2 . . ?
C50 C49 H49B 112.2 . . ?
C48 C49 H49B 112.2 . . ?
H49A C49 H49B 109.8 . . ?
O1 C50 C49A 107.2(6) . . ?
O1 C50 C49 104.2(7) . . ?
O1 C50 H50C 110.3 . . ?
C49A C50 H50C 110.3 . . ?
O1 C50 H50D 110.3 . . ?
C49A C50 H50D 110.3 . . ?
C49 C50 H50D 136.1 . . ?
H50C C50 H50D 108.5 . . ?
O1 C50 H50A 110.4 . . ?
C49 C50 H50A 104.5 . . ?
O1 C50 H50B 111.2 . . ?
C49 C50 H50B 117.5 . . ?
H50A C50 H50B 108.7 . . ?
C50 C49A C48A 100.3(7) . . ?
C50 C49A H49C 111.7 . . ?
C48A C49A H49C 111.7 . . ?
C50 C49A H49D 111.7 . . ?
C48A C49A H49D 111.7 . . ?
H49C C49A H49D 109.5 . . ?
C47 C48A C49A 98.2(8) . . ?
C49A C48A H47A 129.4 . . ?
C47 C48A H48D 112.1 . . ?
C49A C48A H48D 112.1 . . ?
H47A C48A H48D 108.6 . . ?
C47 C48A H48C 112.1 . . ?
C49A C48A H48C 112.1 . . ?
H48D C48A H48C 109.8 . . ?
N2 B1 N4 112.4(5) . . ?
N2 B1 N6 108.4(5) . . ?
N4 B1 N6 112.0(6) . . ?
N2 B1 H1 106(3) . . ?
N4 B1 H1 109(3) . . ?
N6 B1 H1 109(3) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4S O1S C1S C2S -25(3) . . . . ?
O1S C1S C2S C3S 31(2) . . . . ?
C1S C2S C3S C4S -25(3) . . . . ?
C1S O1S C4S C3S 9(3) . . . . ?
C2S C3S C4S O1S 11(3) . . . . ?
O1 Nd1 P1 C1 -66.8(3) . . . . ?
N3 Nd1 P1 C1 91.7(3) . . . . ?
N5 Nd1 P1 C1 19.7(3) . . . . ?
P1 Nd1 P1 C1 -168.8(3) 2_776 . . . ?
O1 Nd1 P1 Nd1 101.97(11) . . . 2_776 ?
N3 Nd1 P1 Nd1 -99.48(12) . . . 2_776 ?
N5 Nd1 P1 Nd1 -171.52(10) . . . 2_776 ?
P1 Nd1 P1 Nd1 0.0 2_776 . . 2_776 ?
O1 Nd1 N1 C22 -42.0(6) . . . . ?
N3 Nd1 N1 C22 158.6(6) . . . . ?
N5 Nd1 N1 C22 -126.4(6) . . . . ?
P1 Nd1 N1 C22 61.4(6) 2_776 . . . ?
O1 Nd1 N1 N2 132.1(4) . . . . ?
N3 Nd1 N1 N2 -27.2(4) . . . . ?
N5 Nd1 N1 N2 47.8(4) . . . . ?
P1 Nd1 N1 N2 -124.4(4) 2_776 . . . ?
C22 N1 N2 C20 -0.8(7) . . . . ?
Nd1 N1 N2 C20 -176.7(5) . . . . ?
C22 N1 N2 B1 169.3(6) . . . . ?
Nd1 N1 N2 B1 -6.6(7) . . . . ?
O1 Nd1 N3 C29 165.2(5) . . . . ?
N5 Nd1 N3 C29 138.4(6) . . . . ?
N1 Nd1 N3 C29 -148.8(6) . . . . ?
P1 Nd1 N3 C29 31.3(6) . . . . ?
P1 Nd1 N3 C29 -45.7(6) 2_776 . . . ?
O1 Nd1 N3 N4 -24.5(7) . . . . ?
N5 Nd1 N3 N4 -51.3(4) . . . . ?
N1 Nd1 N3 N4 21.5(4) . . . . ?
P1 Nd1 N3 N4 -158.4(4) . . . . ?
P1 Nd1 N3 N4 124.5(4) 2_776 . . . ?
C29 N3 N4 C31 1.4(7) . . . . ?
Nd1 N3 N4 C31 -170.5(4) . . . . ?
C29 N3 N4 B1 -168.5(6) . . . . ?
Nd1 N3 N4 B1 19.6(7) . . . . ?
O1 Nd1 N5 C40 48.5(6) . . . . ?
N3 Nd1 N5 C40 -144.3(6) . . . . ?
N1 Nd1 N5 C40 132.4(6) . . . . ?
P1 Nd1 N5 C40 -57.0(6) . . . . ?
O1 Nd1 N5 N6 -132.9(4) . . . . ?
N3 Nd1 N5 N6 34.3(4) . . . . ?
N1 Nd1 N5 N6 -49.0(4) . . . . ?
P1 Nd1 N5 N6 121.6(4) . . . . ?
C40 N5 N6 C38 0.0(7) . . . . ?
Nd1 N5 N6 C38 -179.0(4) . . . . ?
C40 N5 N6 B1 -171.9(6) . . . . ?
Nd1 N5 N6 B1 9.1(7) . . . . ?
Nd1 P1 C1 C6 123.9(4) . . . . ?
Nd1 P1 C1 C6 -42.3(6) 2_776 . . . ?
Nd1 P1 C1 C2 -57.2(5) . . . . ?
Nd1 P1 C1 C2 136.7(4) 2_776 . . . ?
C6 C1 C2 C3 -0.7(9) . . . . ?
P1 C1 C2 C3 -179.7(5) . . . . ?
C6 C1 C2 C7 179.8(5) . . . . ?
P1 C1 C2 C7 0.8(8) . . . . ?
C1 C2 C3 C4 0.1(11) . . . . ?
C7 C2 C3 C4 179.6(7) . . . . ?
C2 C3 C4 C5 0.6(12) . . . . ?
C3 C4 C5 C6 -0.7(12) . . . . ?
C4 C5 C6 C1 0.2(11) . . . . ?
C4 C5 C6 C10 -176.1(7) . . . . ?
C2 C1 C6 C5 0.5(9) . . . . ?
P1 C1 C6 C5 179.5(5) . . . . ?
C2 C1 C6 C10 176.6(6) . . . . ?
P1 C1 C6 C10 -4.4(8) . . . . ?
C3 C2 C7 C9 -36.5(9) . . . . ?
C1 C2 C7 C9 143.0(6) . . . . ?
C3 C2 C7 C8 89.8(7) . . . . ?
C1 C2 C7 C8 -90.7(7) . . . . ?
C5 C6 C10 C12 87.6(8) . . . . ?
C1 C6 C10 C12 -88.6(7) . . . . ?
C5 C6 C10 C11 -40.8(9) . . . . ?
C1 C6 C10 C11 143.0(6) . . . . ?
N1 N2 C20 C21 -0.5(9) . . . . ?
B1 N2 C20 C21 -170.5(7) . . . . ?
N2 C20 C21 C22 1.5(10) . . . . ?
N2 N1 C22 C21 1.7(8) . . . . ?
Nd1 N1 C22 C21 176.2(5) . . . . ?
N2 N1 C22 C23 179.1(6) . . . . ?
Nd1 N1 C22 C23 -6.4(10) . . . . ?
C20 C21 C22 N1 -2.0(10) . . . . ?
C20 C21 C22 C23 -179.3(8) . . . . ?
N1 C22 C23 C24 -43.4(11) . . . . ?
C21 C22 C23 C24 133.5(9) . . . . ?
N1 C22 C23 C28 142.6(7) . . . . ?
C21 C22 C23 C28 -40.4(11) . . . . ?
C28 C23 C24 C25 0.3(12) . . . . ?
C22 C23 C24 C25 -173.6(8) . . . . ?
C23 C24 C25 C26 -1.3(16) . . . . ?
C24 C25 C26 C27 1.6(17) . . . . ?
C25 C26 C27 C28 -1.0(16) . . . . ?
C24 C23 C28 C27 0.3(11) . . . . ?
C22 C23 C28 C27 174.6(7) . . . . ?
C26 C27 C28 C23 0.0(13) . . . . ?
N4 N3 C29 C30 -1.3(8) . . . . ?
Nd1 N3 C29 C30 170.7(4) . . . . ?
N3 C29 C30 C31 0.6(8) . . . . ?
N3 N4 C31 C30 -1.1(7) . . . . ?
B1 N4 C31 C30 167.4(6) . . . . ?
N3 N4 C31 C32 175.9(6) . . . . ?
B1 N4 C31 C32 -15.7(10) . . . . ?
C29 C30 C31 N4 0.3(8) . . . . ?
C29 C30 C31 C32 -176.6(6) . . . . ?
N4 C31 C32 C33 140.1(7) . . . . ?
C30 C31 C32 C33 -43.6(10) . . . . ?
N4 C31 C32 C37 -43.5(10) . . . . ?
C30 C31 C32 C37 132.8(8) . . . . ?
C37 C32 C33 C34 2.4(10) . . . . ?
C31 C32 C33 C34 179.0(7) . . . . ?
C32 C33 C34 C35 -0.9(12) . . . . ?
C33 C34 C35 C36 -1.7(13) . . . . ?
C34 C35 C36 C37 2.6(13) . . . . ?
C35 C36 C37 C32 -1.1(13) . . . . ?
C33 C32 C37 C36 -1.4(11) . . . . ?
C31 C32 C37 C36 -177.9(7) . . . . ?
N5 N6 C38 C39 -0.9(8) . . . . ?
B1 N6 C38 C39 171.2(6) . . . . ?
N6 C38 C39 C40 1.3(8) . . . . ?
N6 N5 C40 C39 0.8(7) . . . . ?
Nd1 N5 C40 C39 179.5(4) . . . . ?
N6 N5 C40 C41 -179.8(6) . . . . ?
Nd1 N5 C40 C41 -1.1(9) . . . . ?
C38 C39 C40 N5 -1.3(8) . . . . ?
C38 C39 C40 C41 179.3(6) . . . . ?
N5 C40 C41 C42 35.2(10) . . . . ?
C39 C40 C41 C42 -145.5(7) . . . . ?
N5 C40 C41 C46 -148.1(6) . . . . ?
C39 C40 C41 C46 31.2(10) . . . . ?
C46 C41 C42 C43 -2.0(10) . . . . ?
C40 C41 C42 C43 174.8(6) . . . . ?
C41 C42 C43 C44 2.5(12) . . . . ?
C42 C43 C44 C45 -1.9(13) . . . . ?
C43 C44 C45 C46 0.8(13) . . . . ?
C44 C45 C46 C41 -0.3(13) . . . . ?
C42 C41 C46 C45 0.9(11) . . . . ?
C40 C41 C46 C45 -175.9(7) . . . . ?
N3 Nd1 O1 C50 -172.9(6) . . . . ?
N5 Nd1 O1 C50 -147.2(6) . . . . ?
N1 Nd1 O1 C50 141.7(6) . . . . ?
P1 Nd1 O1 C50 -41.8(6) . . . . ?
P1 Nd1 O1 C50 38.7(6) 2_776 . . . ?
N3 Nd1 O1 C47 6.0(7) . . . . ?
N5 Nd1 O1 C47 31.7(5) . . . . ?
N1 Nd1 O1 C47 -39.4(5) . . . . ?
P1 Nd1 O1 C47 137.1(5) . . . . ?
P1 Nd1 O1 C47 -142.4(5) 2_776 . . . ?
C50 O1 C47 C48 0.1(13) . . . . ?
Nd1 O1 C47 C48 -178.9(11) . . . . ?
C50 O1 C47 C48A 26.9(10) . . . . ?
Nd1 O1 C47 C48A -152.1(7) . . . . ?
O1 C47 C48 C49 27.8(17) . . . . ?
C48A C47 C48 C49 -60.4(13) . . . . ?
C47 C48 C49 C50 -43.4(17) . . . . ?
C47 O1 C50 C49A 2.8(12) . . . . ?
Nd1 O1 C50 C49A -178.1(9) . . . . ?
C47 O1 C50 C49 -29.4(10) . . . . ?
Nd1 O1 C50 C49 149.7(8) . . . . ?
C48 C49 C50 O1 45.0(14) . . . . ?
C48 C49 C50 C49A -55.0(11) . . . . ?
O1 C50 C49A C48A -29.7(15) . . . . ?
C49 C50 C49A C48A 59.3(11) . . . . ?
O1 C47 C48A C49A -43.9(13) . . . . ?
C48 C47 C48A C49A 55.5(13) . . . . ?
C50 C49A C48A C47 43.7(15) . . . . ?
C20 N2 B1 N4 -127.1(7) . . . . ?
N1 N2 B1 N4 64.4(8) . . . . ?
C20 N2 B1 N6 108.5(7) . . . . ?
N1 N2 B1 N6 -60.0(7) . . . . ?
C31 N4 B1 N2 119.6(6) . . . . ?
N3 N4 B1 N2 -72.7(7) . . . . ?
C31 N4 B1 N6 -118.0(6) . . . . ?
N3 N4 B1 N6 49.6(7) . . . . ?
C38 N6 B1 N2 -112.0(7) . . . . ?
N5 N6 B1 N2 58.8(8) . . . . ?
C38 N6 B1 N4 123.5(6) . . . . ?
N5 N6 B1 N4 -65.8(7) . . . . ?
_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full 25.10
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max 1.429
_refine_diff_density_min -0.788
_refine_diff_density_rms 0.107
# Attachment 'complex_4.cif'
#==============================================================================
data_s
_database_code_depnum_ccdc_archive 'CCDC 763480'
#TrackingRef 'complex_4.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C54 H43 B2 N12 Nd'
_chemical_formula_sum 'C54 H43 B2 N12 Nd'
_chemical_formula_weight 1025.86
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 11.719(2)
_cell_length_b 18.458(3)
_cell_length_c 21.719(4)
_cell_angle_alpha 90.00
_cell_angle_beta 94.824(4)
_cell_angle_gamma 90.00
_cell_volume 4681.4(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 3503
_cell_measurement_theta_min 2.18
_cell_measurement_theta_max 28.10
_exptl_crystal_description prism
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.19
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.456
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2084
_exptl_absorpt_coefficient_mu 1.162
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6665
_exptl_absorpt_correction_T_max 0.8095
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
X-ray structural investigation of compound 4 met certain problems and
requires a special comment. After structure solution by a direct method, all
non-H atoms were unambiguously located and identified. The first refinement of
this way prepared model revealed a huge electron density peak (> 11 e\%A^--3^)
0.96 \%A away from the Nd1 atom. This peak could be treated only as a
disordered Nd atom (Nd1A, site occupancy factor, sof, ca. 0.1
after the next refinement cycle). Thorough examination of the model structure
revealed, that (i) centroids Nd1/Nd1A and B1A/B1B nearly coincide and,
moreover, (ii) the entire model exhibits distinct pseudo-symmetry in respect
to an inversion at the Nd1/Nd1A centroid. After all H-atoms placed into
calculated positions and all non-H atoms refined anisotropically, the
structure quality indicators were still far away from reasonable values. To
fix the problem, the model was changed as following: all atoms were considered
to be disordered between two positions, the initial one with sof 0.9 and the
"contaminant?with sof 0.1 generated by an inversion of the whole
original model at the Nd1-Nd1A centroid. In the minor component, (i) all 1,2-
and 1,3-interatomic distances were restrained to be the same as in the main
one [SAME instruction with a standard uncertainty (su) of 0.001 \%A], (ii) all
atoms except of the Nd1A were refined in an isotropic approximation, and (iii)
atom displacement parameters (ADP-s) for spatially close atoms in
"overlapping?dominant and minor components were restrained to be the same
within su of 0.02 \%A^2^ ("SIMU 0.02 0.04 0.7?instruction). Treatment of this
disordered model brought the refinement indicators into acceptable ranges.
Despite of the apparent lower quality of the X-ray structural experiment for
4, we consider that this is due to the "natural?chemical reasons and
crystal lattice package effects rather than just to the poor single crystal
quality. Hypothesis on racemic twinning of 4 in a chiral P2~1~
space group was especialy checked and rejected.
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'BRUKER SMART CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 23265
_diffrn_reflns_av_R_equivalents 0.0633
_diffrn_reflns_av_sigmaI/netI 0.0803
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 1.88
_diffrn_reflns_theta_max 25.10
_reflns_number_total 8312
_reflns_number_gt 6023
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'BRUKER AXS APEX-2 V1.0-8 (Bruker, 2007)'
_computing_cell_refinement 'SAINT v7.34A (Bruker, 2007)'
_computing_data_reduction 'SAINT v7.34A (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+4.4177P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8312
_refine_ls_number_parameters 904
_refine_ls_number_restraints 720
_refine_ls_R_factor_all 0.0905
_refine_ls_R_factor_gt 0.0613
_refine_ls_wR_factor_ref 0.1416
_refine_ls_wR_factor_gt 0.1323
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.28994(5) 0.194356(19) 0.14511(2) 0.03045(18) Uani 0.905(2) 1 d PD A 1
N1A N 0.0392(5) 0.2484(4) 0.2178(3) 0.0404(16) Uani 0.905(2) 1 d PDU A 1
N2A N 0.0593(5) 0.2409(3) 0.1568(3) 0.0357(14) Uani 0.905(2) 1 d PDU A 1
C1A C -0.0706(7) 0.2673(8) 0.2211(4) 0.059(2) Uani 0.905(2) 1 d PDU A 1
H1A H -0.1048 0.2756 0.2575 0.071 Uiso 0.905(2) 1 calc PR A 1
C2A C -0.1242(7) 0.2723(8) 0.1641(4) 0.057(3) Uani 0.905(2) 1 d PDU A 1
H2A H -0.2004 0.2845 0.1538 0.068 Uiso 0.905(2) 1 calc PR A 1
C3A C -0.0426(6) 0.2554(4) 0.1239(3) 0.0408(18) Uani 0.905(2) 1 d PDU A 1
C4A C -0.0591(6) 0.2531(4) 0.0559(3) 0.0420(19) Uani 0.905(2) 1 d PDU A 1
C5A C 0.0249(7) 0.2332(5) 0.0196(3) 0.057(2) Uani 0.905(2) 1 d PDU A 1
H5A H 0.0958 0.2191 0.0383 0.068 Uiso 0.905(2) 1 calc PR A 1
C6A C 0.0080(8) 0.2336(6) -0.0437(4) 0.068(2) Uani 0.905(2) 1 d PDU A 1
H6A H 0.0682 0.2218 -0.0672 0.081 Uiso 0.905(2) 1 calc PR A 1
C7A C -0.0940(10) 0.2506(6) -0.0717(4) 0.078(3) Uani 0.905(2) 1 d PDU A 1
H7A H -0.1056 0.2499 -0.1146 0.094 Uiso 0.905(2) 1 calc PR A 1
C8A C -0.1805(11) 0.2688(8) -0.0371(5) 0.104(5) Uani 0.905(2) 1 d PDU A 1
H8A H -0.2525 0.2795 -0.0562 0.125 Uiso 0.905(2) 1 calc PR A 1
C9A C -0.1620(9) 0.2714(7) 0.0259(4) 0.087(4) Uani 0.905(2) 1 d PDU A 1
H9A H -0.2214 0.2860 0.0490 0.105 Uiso 0.905(2) 1 calc PR A 1
N3A N 0.1659(5) 0.1578(3) 0.2777(2) 0.0390(15) Uani 0.905(2) 1 d PDU A 1
N4A N 0.2206(5) 0.1203(3) 0.2346(2) 0.0338(14) Uani 0.905(2) 1 d PDU A 1
C10A C 0.1452(8) 0.1135(4) 0.3243(3) 0.048(2) Uani 0.905(2) 1 d PDU A 1
H10A H 0.1085 0.1264 0.3590 0.057 Uiso 0.905(2) 1 calc PR A 1
C11A C 0.1868(9) 0.0464(4) 0.3126(4) 0.055(3) Uani 0.905(2) 1 d PDU A 1
H11A H 0.1841 0.0052 0.3371 0.066 Uiso 0.905(2) 1 calc PR A 1
C12A C 0.2338(7) 0.0525(4) 0.2566(3) 0.0383(18) Uani 0.905(2) 1 d PDU A 1
C13A C 0.2868(8) -0.0058(4) 0.2234(4) 0.0383(17) Uani 0.905(2) 1 d PDU A 1
C14A C 0.3570(13) 0.0084(5) 0.1757(6) 0.048(2) Uani 0.905(2) 1 d PDU A 1
H14A H 0.3727 0.0562 0.1656 0.057 Uiso 0.905(2) 1 calc PR A 1
C15A C 0.4034(16) -0.0473(5) 0.1432(7) 0.059(3) Uani 0.905(2) 1 d PDU A 1
H15A H 0.4468 -0.0368 0.1104 0.070 Uiso 0.905(2) 1 calc PR A 1
C16A C 0.3854(10) -0.1178(5) 0.1594(5) 0.059(3) Uani 0.905(2) 1 d PDU A 1
H16A H 0.4165 -0.1554 0.1377 0.071 Uiso 0.905(2) 1 calc PR A 1
C17A C 0.3217(8) -0.1326(4) 0.2075(4) 0.058(3) Uani 0.905(2) 1 d PDU A 1
H17A H 0.3112 -0.1805 0.2191 0.070 Uiso 0.905(2) 1 calc PR A 1
C18A C 0.2728(9) -0.0781(4) 0.2389(5) 0.052(3) Uani 0.905(2) 1 d PDU A 1
H18A H 0.2293 -0.0897 0.2714 0.063 Uiso 0.905(2) 1 calc PR A 1
N5A N 0.2268(5) 0.2911(3) 0.2698(3) 0.0379(15) Uani 0.905(2) 1 d PDU A 1
N6A N 0.2890(5) 0.2998(3) 0.2194(3) 0.0395(14) Uani 0.905(2) 1 d PDU A 1
C19A C 0.2536(7) 0.3455(4) 0.3096(4) 0.050(2) Uani 0.905(2) 1 d PDU A 1
H19A H 0.2231 0.3519 0.3474 0.060 Uiso 0.905(2) 1 calc PR A 1
C20A C 0.3315(7) 0.3894(4) 0.2864(4) 0.054(2) Uani 0.905(2) 1 d PDU A 1
H20A H 0.3644 0.4310 0.3045 0.065 Uiso 0.905(2) 1 calc PR A 1
C21A C 0.3521(6) 0.3590(4) 0.2297(3) 0.0394(17) Uani 0.905(2) 1 d PDU A 1
C22A C 0.4309(6) 0.3851(4) 0.1840(3) 0.0445(18) Uani 0.905(2) 1 d PDU A 1
C23A C 0.4856(7) 0.3369(4) 0.1487(4) 0.049(2) Uani 0.905(2) 1 d PDU A 1
H23A H 0.4759 0.2875 0.1547 0.059 Uiso 0.905(2) 1 calc PR A 1
C24A C 0.5544(7) 0.3600(5) 0.1044(4) 0.062(2) Uani 0.905(2) 1 d PDU A 1
H24A H 0.5907 0.3265 0.0808 0.074 Uiso 0.905(2) 1 calc PR A 1
C25A C 0.5694(9) 0.4330(6) 0.0953(6) 0.087(3) Uani 0.905(2) 1 d PD A 1
H25A H 0.6138 0.4495 0.0646 0.105 Uiso 0.905(2) 1 calc PR A 1
C26A C 0.5183(10) 0.4802(5) 0.1317(6) 0.090(4) Uani 0.905(2) 1 d PD A 1
H26A H 0.5312 0.5294 0.1265 0.108 Uiso 0.905(2) 1 calc PR A 1
C27A C 0.4487(8) 0.4593(4) 0.1758(5) 0.064(2) Uani 0.905(2) 1 d PD A 1
H27A H 0.4141 0.4934 0.1996 0.077 Uiso 0.905(2) 1 calc PR A 1
B1A B 0.1271(7) 0.2376(5) 0.2722(4) 0.041(2) Uani 0.905(2) 1 d PDU A 1
H1AA H 0.0856 0.2500 0.3130 0.050 Uiso 0.905(2) 1 calc PR A 1
N1B N 0.4857(5) 0.1450(4) 0.0403(3) 0.0437(16) Uani 0.905(2) 1 d PDU A 1
N2B N 0.4694(5) 0.1568(3) 0.1004(2) 0.0386(15) Uani 0.905(2) 1 d PDU A 1
C1B C 0.5945(7) 0.1260(7) 0.0362(4) 0.062(2) Uani 0.905(2) 1 d PDU A 1
H1B H 0.6276 0.1148 -0.0001 0.075 Uiso 0.905(2) 1 calc PR A 1
C2B C 0.6493(7) 0.1256(9) 0.0942(4) 0.061(2) Uani 0.905(2) 1 d PDU A 1
H2B H 0.7259 0.1146 0.1047 0.073 Uiso 0.905(2) 1 calc PR A 1
C3B C 0.5697(6) 0.1445(4) 0.1340(3) 0.0396(18) Uani 0.905(2) 1 d PDU A 1
C4B C 0.5703(6) 0.1534(5) 0.2011(3) 0.0375(18) Uani 0.905(2) 1 d PDU A 1
C5B C 0.4646(6) 0.1741(4) 0.2229(3) 0.0343(16) Uani 0.905(2) 1 d PDU A 1
C6B C 0.4692(6) 0.1821(4) 0.2869(3) 0.0432(18) Uani 0.905(2) 1 d PDU A 1
H6B H 0.4024 0.1949 0.3045 0.052 Uiso 0.905(2) 1 calc PR A 1
C7B C 0.5685(7) 0.1720(4) 0.3259(3) 0.049(2) Uani 0.905(2) 1 d PDU A 1
H7B H 0.5667 0.1783 0.3683 0.059 Uiso 0.905(2) 1 calc PR A 1
C8B C 0.6684(7) 0.1529(4) 0.3021(3) 0.051(2) Uani 0.905(2) 1 d PDU A 1
H8B H 0.7349 0.1460 0.3279 0.061 Uiso 0.905(2) 1 calc PR A 1
C9B C 0.6690(8) 0.1441(6) 0.2399(4) 0.049(3) Uani 0.905(2) 1 d PDU A 1
H9B H 0.7368 0.1316 0.2233 0.059 Uiso 0.905(2) 1 calc PR A 1
N3B N 0.3459(6) 0.2329(4) -0.0096(3) 0.0491(18) Uani 0.905(2) 1 d PDU A 1
N4B N 0.2991(5) 0.2694(3) 0.0378(3) 0.0415(15) Uani 0.905(2) 1 d PDU A 1
C10B C 0.3585(9) 0.2778(5) -0.0573(4) 0.069(3) Uani 0.905(2) 1 d PDU A 1
H10B H 0.3895 0.2656 -0.0939 0.083 Uiso 0.905(2) 1 calc PR A 1
C11B C 0.3181(9) 0.3441(5) -0.0429(4) 0.066(3) Uani 0.905(2) 1 d PDU A 1
H11B H 0.3157 0.3855 -0.0674 0.079 Uiso 0.905(2) 1 calc PR A 1
C12B C 0.2814(7) 0.3378(4) 0.0154(4) 0.052(2) Uani 0.905(2) 1 d PDU A 1
C13B C 0.2238(8) 0.3952(4) 0.0484(5) 0.070(2) Uani 0.905(2) 1 d PDU A 1
C14B C 0.1644(8) 0.3844(5) 0.0974(4) 0.065(2) Uani 0.905(2) 1 d PDU A 1
H14B H 0.1613 0.3377 0.1132 0.078 Uiso 0.905(2) 1 calc PR A 1
C15B C 0.1067(12) 0.4391(6) 0.1264(6) 0.088(3) Uani 0.905(2) 1 d PDU A 1
H15B H 0.0652 0.4284 0.1599 0.106 Uiso 0.905(2) 1 calc PR A 1
C16B C 0.1116(12) 0.5086(7) 0.1052(7) 0.127(4) Uani 0.905(2) 1 d PDU A 1
H16B H 0.0740 0.5458 0.1240 0.153 Uiso 0.905(2) 1 calc PR A 1
C17B C 0.1713(14) 0.5217(7) 0.0571(7) 0.148(4) Uani 0.905(2) 1 d PDU A 1
H17B H 0.1746 0.5690 0.0428 0.178 Uiso 0.905(2) 1 calc PR A 1
C18B C 0.2306(13) 0.4669(6) 0.0264(6) 0.128(4) Uani 0.905(2) 1 d PDU A 1
H18B H 0.2724 0.4780 -0.0069 0.153 Uiso 0.905(2) 1 calc PR A 1
N5B N 0.2895(6) 0.1011(3) 0.0037(3) 0.0464(17) Uani 0.905(2) 1 d PDU A 1
N6B N 0.2319(5) 0.1008(3) 0.0556(3) 0.0403(15) Uani 0.905(2) 1 d PDU A 1
C19B C 0.2584(8) 0.0434(5) -0.0317(4) 0.060(2) Uani 0.905(2) 1 d PDU A 1
H19B H 0.2863 0.0322 -0.0694 0.072 Uiso 0.905(2) 1 calc PR A 1
C20B C 0.1797(9) 0.0042(5) -0.0037(4) 0.058(2) Uani 0.905(2) 1 d PDU A 1
H20B H 0.1437 -0.0383 -0.0178 0.069 Uiso 0.905(2) 1 calc PR A 1
C21B C 0.1644(6) 0.0411(4) 0.0507(4) 0.0413(18) Uani 0.905(2) 1 d PDU A 1
C22B C 0.0869(6) 0.0210(4) 0.0971(4) 0.0437(18) Uani 0.905(2) 1 d PDU A 1
C23B C 0.0282(8) 0.0730(4) 0.1274(4) 0.056(2) Uani 0.905(2) 1 d PDU A 1
H23B H 0.0362 0.1215 0.1172 0.068 Uiso 0.905(2) 1 calc PR A 1
C24B C -0.0418(8) 0.0543(5) 0.1725(5) 0.069(3) Uani 0.905(2) 1 d PDU A 1
H24B H -0.0805 0.0900 0.1926 0.083 Uiso 0.905(2) 1 calc PR A 1
C25B C -0.0546(8) -0.0172(7) 0.1877(5) 0.081(3) Uani 0.905(2) 1 d PDU A 1
H25B H -0.1016 -0.0303 0.2184 0.097 Uiso 0.905(2) 1 calc PR A 1
C26B C 0.0025(10) -0.0691(6) 0.1573(6) 0.085(3) Uani 0.905(2) 1 d PDU A 1
H26B H -0.0060 -0.1176 0.1676 0.102 Uiso 0.905(2) 1 calc PR A 1
C27B C 0.0720(10) -0.0510(4) 0.1120(5) 0.065(2) Uani 0.905(2) 1 d PDU A 1
H27B H 0.1089 -0.0870 0.0912 0.079 Uiso 0.905(2) 1 calc PR A 1
B1B B 0.3881(8) 0.1530(5) -0.0087(4) 0.053(2) Uani 0.905(2) 1 d PDU A 1
H1BA H 0.4178 0.1402 -0.0526 0.064 Uiso 0.905(2) 1 calc PR A 1
Nd1A Nd 0.2224(5) 0.2030(2) 0.1181(3) 0.0483(18) Uani 0.095(2) 1 d PD A 2
N1C N 0.4704(14) 0.1473(17) 0.0437(10) 0.048(11) Uiso 0.095(2) 1 d PDU A 2
N2C N 0.4527(10) 0.1566(14) 0.1049(9) 0.043(11) Uiso 0.095(2) 1 d PDU A 2
C1C C 0.581(2) 0.131(6) 0.0395(14) 0.065(11) Uiso 0.095(2) 1 d PDU A 2
H1C H 0.6137 0.1211 0.0029 0.078 Uiso 0.095(2) 1 calc PR A 2
C2C C 0.638(2) 0.132(7) 0.0958(16) 0.065(11) Uiso 0.095(2) 1 d PDU A 2
H2C H 0.7160 0.1243 0.1053 0.078 Uiso 0.095(2) 1 calc PR A 2
C3C C 0.5564(14) 0.145(3) 0.1368(12) 0.040(11) Uiso 0.095(2) 1 d PDU A 2
C4C C 0.5767(17) 0.154(3) 0.2043(13) 0.037(11) Uiso 0.095(2) 1 d PDU A 2
C5C C 0.497(3) 0.181(4) 0.2400(12) 0.035(11) Uiso 0.095(2) 1 d PDU A 2
H5C H 0.4321 0.2039 0.2210 0.042 Uiso 0.095(2) 1 calc PR A 2
C6C C 0.509(4) 0.176(5) 0.3033(12) 0.047(11) Uiso 0.095(2) 1 d PDU A 2
H6C H 0.4499 0.1922 0.3262 0.056 Uiso 0.095(2) 1 calc PR A 2
C7C C 0.604(5) 0.149(4) 0.3321(14) 0.048(11) Uiso 0.095(2) 1 d PDU A 2
H7C H 0.6123 0.1462 0.3750 0.058 Uiso 0.095(2) 1 calc PR A 2
C8C C 0.689(4) 0.127(4) 0.2983(16) 0.052(11) Uiso 0.095(2) 1 d PDU A 2
H8C H 0.7582 0.1106 0.3180 0.062 Uiso 0.095(2) 1 calc PR A 2
C9C C 0.674(4) 0.128(6) 0.2351(16) 0.044(11) Uiso 0.095(2) 1 d PDU A 2
H9C H 0.7323 0.1099 0.2125 0.053 Uiso 0.095(2) 1 calc PR A 2
N3C N 0.341(2) 0.2364(12) -0.0167(7) 0.048(11) Uiso 0.095(2) 1 d PDU A 2
N4C N 0.2878(17) 0.2747(8) 0.0263(6) 0.036(11) Uiso 0.095(2) 1 d PDU A 2
C10C C 0.369(4) 0.2813(16) -0.0615(11) 0.070(11) Uiso 0.095(2) 1 d PDU A 2
H10C H 0.3994 0.2674 -0.0980 0.083 Uiso 0.095(2) 1 calc PR A 2
C11C C 0.346(7) 0.3505(14) -0.045(2) 0.063(11) Uiso 0.095(2) 1 d PDU A 2
H11C H 0.3607 0.3928 -0.0663 0.076 Uiso 0.095(2) 1 calc PR A 2
C12C C 0.294(4) 0.3447(10) 0.0097(12) 0.049(11) Uiso 0.095(2) 1 d PDU A 2
C13C C 0.243(4) 0.4038(8) 0.0427(16) 0.087(6) Uiso 0.095(2) 1 d PDU A 2
C14C C 0.146(5) 0.3929(18) 0.076(3) 0.079(6) Uiso 0.095(2) 1 d PDU A 2
H14C H 0.1043 0.3504 0.0696 0.094 Uiso 0.095(2) 1 calc PR A 2
C15C C 0.113(8) 0.444(3) 0.117(4) 0.096(6) Uiso 0.095(2) 1 d PDU A 2
H15C H 0.0524 0.4344 0.1408 0.115 Uiso 0.095(2) 1 calc PR A 2
C16C C 0.168(7) 0.509(4) 0.122(4) 0.122(7) Uiso 0.095(2) 1 d PDU A 2
H16C H 0.1470 0.5437 0.1506 0.147 Uiso 0.095(2) 1 calc PR A 2
C17C C 0.255(6) 0.524(2) 0.086(4) 0.130(8) Uiso 0.095(2) 1 d PDU A 2
H17C H 0.2877 0.5697 0.0869 0.156 Uiso 0.095(2) 1 calc PR A 2
C18C C 0.295(6) 0.4716(16) 0.049(3) 0.095(8) Uiso 0.095(2) 1 d PDU A 2
H18C H 0.3572 0.4816 0.0264 0.114 Uiso 0.095(2) 1 calc PR A 2
N5C N 0.282(2) 0.1032(10) -0.0056(7) 0.045(11) Uiso 0.095(2) 1 d PDU A 2
N6C N 0.2216(18) 0.0956(6) 0.0458(7) 0.040(11) Uiso 0.095(2) 1 d PDU A 2
C19C C 0.254(3) 0.0476(16) -0.0440(12) 0.057(11) Uiso 0.095(2) 1 d PDU A 2
H19C H 0.2835 0.0402 -0.0820 0.069 Uiso 0.095(2) 1 calc PR A 2
C20C C 0.177(7) 0.004(3) -0.019(2) 0.055(11) Uiso 0.095(2) 1 d PDU A 2
H20C H 0.1438 -0.0376 -0.0363 0.067 Uiso 0.095(2) 1 calc PR A 2
C21C C 0.159(3) 0.0360(10) 0.0373(11) 0.039(11) Uiso 0.095(2) 1 d PDU A 2
C22C C 0.088(3) 0.0083(13) 0.0862(15) 0.044(11) Uiso 0.095(2) 1 d PDU A 2
C23C C 0.032(6) 0.055(2) 0.122(3) 0.058(11) Uiso 0.095(2) 1 d PDU A 2
H23C H 0.0251 0.1038 0.1102 0.070 Uiso 0.095(2) 1 calc PR A 2
C24C C -0.013(8) 0.033(3) 0.175(3) 0.070(12) Uiso 0.095(2) 1 d PDU A 2
H24C H -0.0443 0.0663 0.2008 0.084 Uiso 0.095(2) 1 calc PR A 2
C25C C -0.012(9) -0.040(4) 0.190(3) 0.076(12) Uiso 0.095(2) 1 d PDU A 2
H25C H -0.0418 -0.0559 0.2256 0.091 Uiso 0.095(2) 1 calc PR A 2
C26C C 0.034(9) -0.087(3) 0.151(4) 0.084(12) Uiso 0.095(2) 1 d PDU A 2
H26C H 0.0287 -0.1360 0.1592 0.101 Uiso 0.095(2) 1 calc PR A 2
C27C C 0.088(10) -0.0656(14) 0.101(4) 0.065(11) Uiso 0.095(2) 1 d PDU A 2
H27C H 0.1229 -0.0992 0.0767 0.078 Uiso 0.095(2) 1 calc PR A 2
B1C B 0.3808(18) 0.1567(13) -0.0101(8) 0.052(11) Uiso 0.095(2) 1 d PDU A 2
H1CA H 0.4208 0.1433 -0.0511 0.063 Uiso 0.095(2) 1 calc PR A 2
N1D N 0.0301(16) 0.2539(17) 0.2242(8) 0.041(11) Uiso 0.095(2) 1 d PDU A 2
N2D N 0.0446(11) 0.2413(11) 0.1640(7) 0.038(11) Uiso 0.095(2) 1 d PDU A 2
C1D C -0.081(2) 0.266(6) 0.2298(13) 0.056(11) Uiso 0.095(2) 1 d PDU A 2
H1D H -0.1136 0.2748 0.2666 0.067 Uiso 0.095(2) 1 calc PR A 2
C2D C -0.138(2) 0.264(7) 0.1724(15) 0.053(11) Uiso 0.095(2) 1 d PDU A 2
H2D H -0.2157 0.2715 0.1628 0.063 Uiso 0.095(2) 1 calc PR A 2
C3D C -0.0577(14) 0.250(3) 0.1315(11) 0.041(11) Uiso 0.095(2) 1 d PDU A 2
C4D C -0.0606(15) 0.240(3) 0.0644(10) 0.040(11) Uiso 0.095(2) 1 d PDU A 2
C5D C 0.0451(12) 0.2208(13) 0.0417(7) 0.064(11) Uiso 0.095(2) 1 d PDU A 2
C6D C 0.041(2) 0.219(4) -0.0227(7) 0.064(11) Uiso 0.095(2) 1 d PDU A 2
H6D H 0.1089 0.2108 -0.0409 0.077 Uiso 0.095(2) 1 calc PR A 2
C7D C -0.059(3) 0.230(6) -0.0610(9) 0.074(12) Uiso 0.095(2) 1 d PDU A 2
H7D H -0.0569 0.2270 -0.1037 0.089 Uiso 0.095(2) 1 calc PR A 2
C8D C -0.159(4) 0.245(9) -0.0363(14) 0.101(12) Uiso 0.095(2) 1 d PDU A 2
H8D H -0.2263 0.2523 -0.0617 0.121 Uiso 0.095(2) 1 calc PR A 2
C9D C -0.160(2) 0.250(5) 0.0262(13) 0.079(12) Uiso 0.095(2) 1 d PDU A 2
H9D H -0.2280 0.2600 0.0435 0.095 Uiso 0.095(2) 1 calc PR A 2
N3D N 0.174(3) 0.1687(12) 0.2745(6) 0.040(11) Uiso 0.095(2) 1 d PDU A 2
N4D N 0.2178(19) 0.1308(8) 0.2271(5) 0.034(11) Uiso 0.095(2) 1 d PDU A 2
C10D C 0.171(7) 0.1265(19) 0.3248(12) 0.050(11) Uiso 0.095(2) 1 d PDU A 2
H10D H 0.1467 0.1408 0.3627 0.060 Uiso 0.095(2) 1 calc PR A 2
C11D C 0.208(9) 0.059(2) 0.3107(18) 0.055(11) Uiso 0.095(2) 1 d PDU A 2
H11D H 0.2136 0.0191 0.3365 0.066 Uiso 0.095(2) 1 calc PR A 2
C12D C 0.236(4) 0.0630(12) 0.2507(10) 0.034(11) Uiso 0.095(2) 1 d PDU A 2
C13D C 0.289(6) 0.0038(14) 0.2170(17) 0.036(11) Uiso 0.095(2) 1 d PDU A 2
C14D C 0.359(11) 0.013(3) 0.172(5) 0.045(11) Uiso 0.095(2) 1 d PDU A 2
H14D H 0.3849 0.0598 0.1652 0.054 Uiso 0.095(2) 1 calc PR A 2
C15D C 0.397(15) -0.043(4) 0.136(6) 0.060(11) Uiso 0.095(2) 1 d PDU A 2
H15D H 0.4431 -0.0331 0.1046 0.072 Uiso 0.095(2) 1 calc PR A 2
C16D C 0.365(11) -0.112(4) 0.148(5) 0.058(12) Uiso 0.095(2) 1 d PDU A 2
H16D H 0.3912 -0.1508 0.1250 0.069 Uiso 0.095(2) 1 calc PR A 2
C17D C 0.295(8) -0.124(2) 0.192(4) 0.056(12) Uiso 0.095(2) 1 d PDU A 2
H17D H 0.2704 -0.1711 0.1980 0.067 Uiso 0.095(2) 1 calc PR A 2
C18D C 0.256(10) -0.0680(14) 0.230(4) 0.052(11) Uiso 0.095(2) 1 d PDU A 2
H18D H 0.2112 -0.0782 0.2620 0.063 Uiso 0.095(2) 1 calc PR A 2
N5D N 0.226(2) 0.3005(12) 0.2575(7) 0.035(11) Uiso 0.095(2) 1 d PDU A 2
N6D N 0.2828(17) 0.2990(8) 0.2053(6) 0.038(11) Uiso 0.095(2) 1 d PDU A 2
C19D C 0.257(5) 0.360(2) 0.2909(17) 0.055(12) Uiso 0.095(2) 1 d PDU A 2
H19D H 0.2257 0.3741 0.3272 0.066 Uiso 0.095(2) 1 calc PR A 2
C20D C 0.339(4) 0.3959(18) 0.2632(14) 0.048(11) Uiso 0.095(2) 1 d PDU A 2
H20D H 0.3800 0.4365 0.2778 0.058 Uiso 0.095(2) 1 calc PR A 2
C21D C 0.350(3) 0.3590(12) 0.2082(10) 0.040(11) Uiso 0.095(2) 1 d PDU A 2
C22D C 0.413(3) 0.3833(12) 0.1569(13) 0.049(11) Uiso 0.095(2) 1 d PDU A 2
C23D C 0.479(5) 0.336(2) 0.126(2) 0.049(11) Uiso 0.095(2) 1 d PDU A 2
H23D H 0.4848 0.2877 0.1388 0.059 Uiso 0.095(2) 1 calc PR A 2
C24D C 0.538(5) 0.358(3) 0.077(2) 0.061(12) Uiso 0.095(2) 1 d PDU A 2
H24D H 0.5759 0.3250 0.0546 0.073 Uiso 0.095(2) 1 calc PR A 2
C25D C 0.539(7) 0.431(3) 0.062(3) 0.09(4) Uiso 0.095(2) 1 d PD A 2
H25D H 0.5811 0.4468 0.0306 0.105 Uiso 0.095(2) 1 calc PR A 2
C26D C 0.478(6) 0.479(2) 0.095(3) 0.09(4) Uiso 0.095(2) 1 d PD A 2
H26D H 0.4819 0.5279 0.0860 0.110 Uiso 0.095(2) 1 calc PR A 2
C27D C 0.412(5) 0.4556(16) 0.140(2) 0.07(3) Uiso 0.095(2) 1 d PD A 2
H27D H 0.3668 0.4884 0.1597 0.088 Uiso 0.095(2) 1 calc PR A 2
B1D B 0.130(2) 0.2482(12) 0.2723(6) 0.043(11) Uiso 0.095(2) 1 d PDU A 2
H1DA H 0.1014 0.2620 0.3164 0.052 Uiso 0.095(2) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nd1 0.0304(3) 0.0341(2) 0.0280(2) -0.00350(18) 0.0091(2) 0.0022(2)
N1A 0.036(4) 0.051(4) 0.036(3) -0.008(3) 0.012(3) 0.002(3)
N2A 0.026(3) 0.041(3) 0.041(3) -0.003(3) 0.008(3) 0.003(2)
C1A 0.047(5) 0.081(6) 0.053(5) -0.017(5) 0.021(4) 0.010(4)
C2A 0.036(4) 0.082(7) 0.052(5) 0.004(5) 0.006(4) 0.009(5)
C3A 0.039(4) 0.036(4) 0.049(4) 0.003(3) 0.013(3) 0.000(3)
C4A 0.041(4) 0.035(4) 0.049(4) 0.009(3) 0.003(3) 0.006(3)
C5A 0.048(5) 0.081(6) 0.041(4) -0.007(4) 0.004(4) 0.008(4)
C6A 0.060(6) 0.099(7) 0.044(5) -0.005(5) 0.004(4) 0.007(5)
C7A 0.098(8) 0.090(8) 0.047(5) 0.004(5) 0.005(5) 0.015(6)
C8A 0.091(8) 0.154(13) 0.063(6) 0.011(7) -0.017(6) 0.056(7)
C9A 0.065(6) 0.135(11) 0.063(6) 0.006(6) 0.008(5) 0.042(6)
N3A 0.042(4) 0.043(3) 0.033(3) -0.006(3) 0.010(3) 0.001(3)
N4A 0.036(3) 0.035(3) 0.032(3) 0.000(2) 0.008(2) 0.000(2)
C10A 0.055(6) 0.054(5) 0.037(4) 0.005(3) 0.022(4) 0.001(4)
C11A 0.064(7) 0.050(5) 0.051(5) 0.018(4) 0.012(4) -0.002(5)
C12A 0.040(4) 0.034(4) 0.042(4) 0.008(3) 0.009(3) -0.009(3)
C13A 0.034(4) 0.036(4) 0.044(4) 0.002(3) 0.005(3) -0.002(3)
C14A 0.046(5) 0.036(4) 0.062(5) 0.006(4) 0.011(4) 0.012(3)
C15A 0.065(6) 0.053(5) 0.060(6) -0.002(4) 0.020(6) 0.009(4)
C16A 0.058(7) 0.041(4) 0.080(7) -0.007(4) 0.009(6) 0.009(4)
C17A 0.062(7) 0.031(4) 0.081(7) 0.002(4) 0.001(5) -0.003(4)
C18A 0.053(6) 0.046(4) 0.059(5) 0.004(4) 0.009(5) -0.001(4)
N5A 0.041(4) 0.037(3) 0.037(3) -0.005(3) 0.011(3) 0.005(3)
N6A 0.041(3) 0.040(3) 0.038(3) -0.009(3) 0.008(3) 0.000(3)
C19A 0.046(5) 0.062(5) 0.041(4) -0.019(4) 0.004(4) -0.004(4)
C20A 0.050(5) 0.057(5) 0.055(5) -0.027(4) 0.006(4) -0.009(4)
C21A 0.031(4) 0.043(4) 0.044(4) -0.009(3) 0.004(3) 0.001(3)
C22A 0.043(4) 0.040(4) 0.051(5) -0.007(3) -0.001(4) -0.005(3)
C23A 0.045(5) 0.048(4) 0.054(5) 0.002(4) 0.005(4) -0.007(4)
C24A 0.051(5) 0.074(6) 0.064(6) -0.006(5) 0.022(5) -0.004(4)
C25A 0.077(8) 0.088(8) 0.102(10) 0.027(7) 0.039(8) -0.022(6)
C26A 0.079(8) 0.055(6) 0.139(11) 0.017(6) 0.030(9) -0.018(6)
C27A 0.059(6) 0.038(5) 0.097(8) -0.009(4) 0.013(6) -0.004(4)
B1A 0.040(5) 0.045(5) 0.041(5) -0.007(4) 0.018(4) 0.003(4)
N1B 0.034(4) 0.066(4) 0.033(3) -0.007(3) 0.016(3) 0.009(3)
N2B 0.039(4) 0.045(3) 0.034(3) -0.004(3) 0.016(3) 0.004(3)
C1B 0.051(5) 0.092(6) 0.047(5) -0.015(4) 0.024(4) 0.012(5)
C2B 0.038(5) 0.087(7) 0.059(5) -0.009(4) 0.011(4) 0.018(4)
C3B 0.032(4) 0.039(4) 0.050(4) 0.000(3) 0.013(3) 0.000(3)
C4B 0.038(4) 0.028(3) 0.048(4) -0.001(3) 0.011(3) -0.004(3)
C5B 0.032(4) 0.034(4) 0.037(4) -0.007(3) 0.009(3) -0.001(3)
C6B 0.040(5) 0.049(4) 0.041(4) -0.008(4) 0.004(3) 0.003(4)
C7B 0.059(6) 0.052(5) 0.036(4) -0.005(3) -0.001(4) 0.006(4)
C8B 0.045(5) 0.059(6) 0.048(5) 0.000(4) -0.004(4) 0.007(4)
C9B 0.036(4) 0.061(8) 0.050(5) -0.006(4) 0.007(4) 0.010(4)
N3B 0.054(4) 0.060(4) 0.035(3) 0.004(3) 0.015(3) -0.003(3)
N4B 0.037(4) 0.049(4) 0.039(3) 0.006(3) 0.009(3) 0.002(3)
C10B 0.084(7) 0.087(6) 0.040(5) 0.018(4) 0.024(4) -0.013(5)
C11B 0.079(7) 0.065(6) 0.054(5) 0.026(4) 0.010(5) -0.010(5)
C12B 0.044(5) 0.052(4) 0.059(5) 0.016(4) 0.005(4) -0.004(4)
C13B 0.078(6) 0.044(4) 0.092(6) 0.019(4) 0.025(5) -0.005(4)
C14B 0.066(5) 0.057(4) 0.073(5) 0.009(4) 0.013(4) 0.013(4)
C15B 0.091(6) 0.073(5) 0.104(7) 0.002(5) 0.026(5) 0.005(5)
C16B 0.146(8) 0.088(7) 0.156(8) 0.004(7) 0.064(7) 0.029(7)
C17B 0.190(9) 0.079(6) 0.185(9) 0.019(7) 0.074(8) 0.039(7)
C18B 0.162(8) 0.081(6) 0.150(8) 0.025(6) 0.072(7) 0.018(6)
N5B 0.054(4) 0.058(4) 0.027(3) -0.011(3) 0.000(3) 0.005(3)
N6B 0.042(4) 0.043(3) 0.036(3) -0.008(3) 0.004(3) 0.001(3)
C19B 0.068(6) 0.072(5) 0.040(4) -0.024(4) 0.000(4) 0.008(5)
C20B 0.066(6) 0.052(5) 0.052(5) -0.022(4) -0.007(5) -0.006(4)
C21B 0.034(4) 0.041(4) 0.047(4) -0.007(3) -0.004(3) 0.001(3)
C22B 0.034(4) 0.036(4) 0.060(5) -0.011(3) -0.005(4) 0.001(3)
C23B 0.045(5) 0.049(5) 0.076(6) -0.021(4) 0.008(4) -0.007(4)
C24B 0.049(6) 0.075(6) 0.085(6) -0.034(5) 0.018(5) -0.006(5)
C25B 0.043(6) 0.111(8) 0.090(7) 0.002(6) 0.009(5) -0.017(6)
C26B 0.062(7) 0.063(6) 0.132(9) 0.018(6) 0.014(7) -0.010(5)
C27B 0.055(6) 0.048(5) 0.094(7) -0.004(5) 0.014(5) 0.001(5)
B1B 0.053(6) 0.075(6) 0.033(5) -0.007(4) 0.014(4) 0.005(5)
Nd1A 0.040(3) 0.046(3) 0.057(3) -0.006(2) -0.005(3) 0.009(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 N2B 2.487(6) . ?
Nd1 N6A 2.529(5) . ?
Nd1 N4A 2.564(5) . ?
Nd1 C5B 2.569(7) . ?
Nd1 N6B 2.646(6) . ?
Nd1 N4B 2.722(6) . ?
Nd1 N2A 2.868(5) . ?
N1A C1A 1.341(9) . ?
N1A N2A 1.372(7) . ?
N1A B1A 1.514(10) . ?
N2A C3A 1.365(8) . ?
C1A C2A 1.343(10) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.383(10) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.474(9) . ?
C4A C5A 1.363(10) . ?
C4A C9A 1.365(11) . ?
C5A C6A 1.372(10) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.332(12) . ?
C6A H6A 0.9300 . ?
C7A C8A 1.355(14) . ?
C7A H7A 0.9300 . ?
C8A C9A 1.369(12) . ?
C8A H8A 0.9300 . ?
C9A H9A 0.9300 . ?
N3A C10A 1.339(8) . ?
N3A N4A 1.367(7) . ?
N3A B1A 1.543(10) . ?
N4A C12A 1.345(8) . ?
C10A C11A 1.362(10) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.381(10) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.463(9) . ?
C13A C18A 1.389(10) . ?
C13A C14A 1.402(10) . ?
C14A C15A 1.384(10) . ?
C14A H14A 0.9300 . ?
C15A C16A 1.370(10) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.362(11) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.368(10) . ?
C17A H17A 0.9300 . ?
C18A H18A 0.9300 . ?
N5A C19A 1.344(8) . ?
N5A N6A 1.376(8) . ?
N5A B1A 1.535(10) . ?
N6A C21A 1.327(8) . ?
C19A C20A 1.349(11) . ?
C19A H19A 0.9300 . ?
C20A C21A 1.394(10) . ?
C20A H20A 0.9300 . ?
C21A C22A 1.491(10) . ?
C22A C23A 1.369(10) . ?
C22A C27A 1.399(10) . ?
C23A C24A 1.373(11) . ?
C23A H23A 0.9300 . ?
C24A C25A 1.375(12) . ?
C24A H24A 0.9300 . ?
C25A C26A 1.350(14) . ?
C25A H25A 0.9300 . ?
C26A C27A 1.364(13) . ?
C26A H26A 0.9300 . ?
C27A H27A 0.9300 . ?
B1A H1AA 1.0700 . ?
N1B C1B 1.333(9) . ?
N1B N2B 1.353(7) . ?
N1B B1B 1.503(10) . ?
N2B C3B 1.350(8) . ?
C1B C2B 1.364(10) . ?
C1B H1B 0.9300 . ?
C2B C3B 1.368(10) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.468(9) . ?
C4B C9B 1.384(10) . ?
C4B C5B 1.415(9) . ?
C5B C6B 1.395(9) . ?
C6B C7B 1.393(10) . ?
C6B H6B 0.9300 . ?
C7B C8B 1.365(11) . ?
C7B H7B 0.9300 . ?
C8B C9B 1.360(10) . ?
C8B H8B 0.9300 . ?
C9B H9B 0.9300 . ?
N3B C10B 1.345(9) . ?
N3B N4B 1.381(8) . ?
N3B B1B 1.554(11) . ?
N4B C12B 1.362(9) . ?
C10B C11B 1.358(12) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.375(11) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.475(12) . ?
C13B C14B 1.335(12) . ?
C13B C18B 1.413(13) . ?
C14B C15B 1.394(12) . ?
C14B H14B 0.9300 . ?
C15B C16B 1.365(15) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.327(17) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.424(16) . ?
C17B H17B 0.9300 . ?
C18B H18B 0.9300 . ?
N5B C19B 1.347(9) . ?
N5B N6B 1.361(8) . ?
N5B B1B 1.542(11) . ?
N6B C21B 1.355(8) . ?
C19B C20B 1.356(11) . ?
C19B H19B 0.9300 . ?
C20B C21B 1.389(10) . ?
C20B H20B 0.9300 . ?
C21B C22B 1.460(10) . ?
C22B C23B 1.379(10) . ?
C22B C27B 1.383(10) . ?
C23B C24B 1.373(11) . ?
C23B H23B 0.9300 . ?
C24B C25B 1.372(13) . ?
C24B H24B 0.9300 . ?
C25B C26B 1.370(14) . ?
C25B H25B 0.9300 . ?
C26B C27B 1.372(13) . ?
C26B H26B 0.9300 . ?
C27B H27B 0.9300 . ?
B1B H1BA 1.0700 . ?
Nd1A N2D 2.487(6) . ?
Nd1A N6C 2.529(6) . ?
Nd1A N4C 2.563(6) . ?
Nd1A C5D 2.569(7) . ?
Nd1A N6D 2.646(6) . ?
Nd1A N4D 2.722(6) . ?
Nd1A N2C 2.868(6) . ?
N1C C1C 1.341(9) . ?
N1C N2C 1.372(7) . ?
N1C B1C 1.514(10) . ?
N2C C3C 1.365(8) . ?
C1C C2C 1.343(10) . ?
C1C H1C 0.9300 . ?
C2C C3C 1.383(10) . ?
C2C H2C 0.9300 . ?
C3C C4C 1.474(10) . ?
C4C C5C 1.363(10) . ?
C4C C9C 1.365(11) . ?
C5C C6C 1.373(10) . ?
C5C H5C 0.9300 . ?
C6C C7C 1.332(12) . ?
C6C H6C 0.9300 . ?
C7C C8C 1.355(14) . ?
C7C H7C 0.9300 . ?
C8C C9C 1.369(12) . ?
C8C H8C 0.9300 . ?
C9C H9C 0.9300 . ?
N3C C10C 1.340(9) . ?
N3C N4C 1.367(7) . ?
N3C B1C 1.543(10) . ?
N4C C12C 1.345(8) . ?
C10C C11C 1.362(10) . ?
C10C H10C 0.9300 . ?
C11C C12C 1.382(10) . ?
C11C H11C 0.9300 . ?
C12C C13C 1.463(9) . ?
C13C C18C 1.390(10) . ?
C13C C14C 1.402(10) . ?
C14C C15C 1.384(10) . ?
C14C H14C 0.9300 . ?
C15C C16C 1.370(11) . ?
C15C H15C 0.9300 . ?
C16C C17C 1.362(11) . ?
C16C H16C 0.9300 . ?
C17C C18C 1.368(10) . ?
C17C H17C 0.9300 . ?
C18C H18C 0.9300 . ?
N5C C19C 1.344(8) . ?
N5C N6C 1.376(8) . ?
N5C B1C 1.535(10) . ?
N6C C21C 1.327(8) . ?
C19C C20C 1.349(11) . ?
C19C H19C 0.9300 . ?
C20C C21C 1.394(10) . ?
C20C H20C 0.9300 . ?
C21C C22C 1.491(10) . ?
C22C C23C 1.370(10) . ?
C22C C27C 1.399(10) . ?
C23C C24C 1.373(11) . ?
C23C H23C 0.9300 . ?
C24C C25C 1.375(12) . ?
C24C H24C 0.9300 . ?
C25C C26C 1.350(14) . ?
C25C H25C 0.9300 . ?
C26C C27C 1.364(13) . ?
C26C H26C 0.9300 . ?
C27C H27C 0.9300 . ?
B1C H1CA 1.0700 . ?
N1D C1D 1.333(9) . ?
N1D N2D 1.353(7) . ?
N1D B1D 1.503(10) . ?
N2D C3D 1.350(8) . ?
C1D C2D 1.365(10) . ?
C1D H1D 0.9300 . ?
C2D C3D 1.368(10) . ?
C2D H2D 0.9300 . ?
C3D C4D 1.468(9) . ?
C4D C9D 1.384(10) . ?
C4D C5D 1.415(9) . ?
C5D C6D 1.395(9) . ?
C6D C7D 1.393(10) . ?
C6D H6D 0.9300 . ?
C7D C8D 1.365(11) . ?
C7D H7D 0.9300 . ?
C8D C9D 1.360(10) . ?
C8D H8D 0.9300 . ?
C9D H9D 0.9300 . ?
N3D C10D 1.345(9) . ?
N3D N4D 1.381(8) . ?
N3D B1D 1.554(11) . ?
N4D C12D 1.362(9) . ?
C10D C11D 1.358(12) . ?
C10D H10D 0.9300 . ?
C11D C12D 1.375(11) . ?
C11D H11D 0.9300 . ?
C12D C13D 1.475(12) . ?
C13D C14D 1.335(12) . ?
C13D C18D 1.413(13) . ?
C14D C15D 1.394(12) . ?
C14D H14D 0.9300 . ?
C15D C16D 1.365(15) . ?
C15D H15D 0.9300 . ?
C16D C17D 1.327(17) . ?
C16D H16D 0.9300 . ?
C17D C18D 1.424(16) . ?
C17D H17D 0.9300 . ?
C18D H18D 0.9300 . ?
N5D C19D 1.347(9) . ?
N5D N6D 1.361(8) . ?
N5D B1D 1.542(11) . ?
N6D C21D 1.355(8) . ?
C19D C20D 1.356(11) . ?
C19D H19D 0.9300 . ?
C20D C21D 1.389(10) . ?
C20D H20D 0.9300 . ?
C21D C22D 1.460(10) . ?
C22D C23D 1.379(10) . ?
C22D C27D 1.383(10) . ?
C23D C24D 1.373(11) . ?
C23D H23D 0.9300 . ?
C24D C25D 1.372(13) . ?
C24D H24D 0.9300 . ?
C25D C26D 1.370(14) . ?
C25D H25D 0.9300 . ?
C26D C27D 1.372(13) . ?
C26D H26D 0.9300 . ?
C27D H27D 0.9300 . ?
B1D H1DA 1.0700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2B Nd1 N6A 120.81(18) . . ?
N2B Nd1 N4A 118.67(18) . . ?
N6A Nd1 N4A 84.73(17) . . ?
N2B Nd1 C5B 64.09(19) . . ?
N6A Nd1 C5B 74.85(19) . . ?
N4A Nd1 C5B 73.12(19) . . ?
N2B Nd1 N6B 72.85(18) . . ?
N6A Nd1 N6B 163.0(2) . . ?
N4A Nd1 N6B 97.51(17) . . ?
C5B Nd1 N6B 121.94(18) . . ?
N2B Nd1 N4B 73.25(17) . . ?
N6A Nd1 N4B 99.04(18) . . ?
N4A Nd1 N4B 163.47(18) . . ?
C5B Nd1 N4B 123.4(2) . . ?
N6B Nd1 N4B 74.29(17) . . ?
N2B Nd1 N2A 162.18(18) . . ?
N6A Nd1 N2A 70.02(17) . . ?
N4A Nd1 N2A 74.41(16) . . ?
C5B Nd1 N2A 133.63(18) . . ?
N6B Nd1 N2A 94.29(16) . . ?
N4B Nd1 N2A 91.65(17) . . ?
C1A N1A N2A 108.6(6) . . ?
C1A N1A B1A 125.9(6) . . ?
N2A N1A B1A 125.5(6) . . ?
C3A N2A N1A 105.8(5) . . ?
C3A N2A Nd1 143.3(5) . . ?
N1A N2A Nd1 110.8(4) . . ?
N1A C1A C2A 110.3(7) . . ?
N1A C1A H1A 124.9 . . ?
C2A C1A H1A 124.9 . . ?
C1A C2A C3A 105.7(7) . . ?
C1A C2A H2A 127.1 . . ?
C3A C2A H2A 127.1 . . ?
N2A C3A C2A 109.6(6) . . ?
N2A C3A C4A 123.6(6) . . ?
C2A C3A C4A 126.8(7) . . ?
C5A C4A C9A 116.3(7) . . ?
C5A C4A C3A 123.2(7) . . ?
C9A C4A C3A 120.5(7) . . ?
C4A C5A C6A 121.9(8) . . ?
C4A C5A H5A 119.1 . . ?
C6A C5A H5A 119.1 . . ?
C7A C6A C5A 120.5(9) . . ?
C7A C6A H6A 119.8 . . ?
C5A C6A H6A 119.8 . . ?
C6A C7A C8A 119.3(9) . . ?
C6A C7A H7A 120.4 . . ?
C8A C7A H7A 120.4 . . ?
C7A C8A C9A 120.1(9) . . ?
C7A C8A H8A 119.9 . . ?
C9A C8A H8A 119.9 . . ?
C4A C9A C8A 121.9(9) . . ?
C4A C9A H9A 119.1 . . ?
C8A C9A H9A 119.1 . . ?
C10A N3A N4A 109.4(6) . . ?
C10A N3A B1A 124.8(6) . . ?
N4A N3A B1A 125.6(6) . . ?
C12A N4A N3A 105.9(5) . . ?
C12A N4A Nd1 137.0(4) . . ?
N3A N4A Nd1 116.5(4) . . ?
N3A C10A C11A 109.0(6) . . ?
N3A C10A H10A 125.5 . . ?
C11A C10A H10A 125.5 . . ?
C10A C11A C12A 105.4(6) . . ?
C10A C11A H11A 127.3 . . ?
C12A C11A H11A 127.3 . . ?
N4A C12A C11A 110.2(6) . . ?
N4A C12A C13A 123.4(6) . . ?
C11A C12A C13A 126.3(6) . . ?
C18A C13A C14A 116.7(7) . . ?
C18A C13A C12A 121.5(7) . . ?
C14A C13A C12A 121.8(6) . . ?
C15A C14A C13A 121.2(7) . . ?
C15A C14A H14A 119.4 . . ?
C13A C14A H14A 119.4 . . ?
C16A C15A C14A 120.0(8) . . ?
C16A C15A H15A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C17A C16A C15A 119.6(8) . . ?
C17A C16A H16A 120.2 . . ?
C15A C16A H16A 120.2 . . ?
C16A C17A C18A 121.0(7) . . ?
C16A C17A H17A 119.5 . . ?
C18A C17A H17A 119.5 . . ?
C17A C18A C13A 121.4(7) . . ?
C17A C18A H18A 119.3 . . ?
C13A C18A H18A 119.3 . . ?
C19A N5A N6A 108.3(6) . . ?
C19A N5A B1A 126.6(6) . . ?
N6A N5A B1A 124.0(5) . . ?
C21A N6A N5A 106.6(6) . . ?
C21A N6A Nd1 135.2(5) . . ?
N5A N6A Nd1 116.7(4) . . ?
N5A C19A C20A 109.8(7) . . ?
N5A C19A H19A 125.1 . . ?
C20A C19A H19A 125.1 . . ?
C19A C20A C21A 105.1(6) . . ?
C19A C20A H20A 127.4 . . ?
C21A C20A H20A 127.4 . . ?
N6A C21A C20A 110.2(7) . . ?
N6A C21A C22A 121.4(6) . . ?
C20A C21A C22A 128.4(6) . . ?
C23A C22A C27A 118.8(8) . . ?
C23A C22A C21A 120.6(6) . . ?
C27A C22A C21A 120.6(7) . . ?
C22A C23A C24A 121.4(7) . . ?
C22A C23A H23A 119.3 . . ?
C24A C23A H23A 119.3 . . ?
C23A C24A C25A 119.7(9) . . ?
C23A C24A H24A 120.2 . . ?
C25A C24A H24A 120.2 . . ?
C26A C25A C24A 118.6(9) . . ?
C26A C25A H25A 120.7 . . ?
C24A C25A H25A 120.7 . . ?
C25A C26A C27A 123.3(9) . . ?
C25A C26A H26A 118.3 . . ?
C27A C26A H26A 118.3 . . ?
C26A C27A C22A 118.1(9) . . ?
C26A C27A H27A 120.9 . . ?
C22A C27A H27A 120.9 . . ?
N1A B1A N5A 111.0(6) . . ?
N1A B1A N3A 111.3(6) . . ?
N5A B1A N3A 113.4(6) . . ?
N1A B1A H1AA 106.9 . . ?
N5A B1A H1AA 106.9 . . ?
N3A B1A H1AA 106.9 . . ?
C1B N1B N2B 108.8(6) . . ?
C1B N1B B1B 130.8(6) . . ?
N2B N1B B1B 120.4(6) . . ?
C3B N2B N1B 107.8(6) . . ?
C3B N2B Nd1 124.3(4) . . ?
N1B N2B Nd1 127.9(4) . . ?
N1B C1B C2B 108.5(6) . . ?
N1B C1B H1B 125.8 . . ?
C2B C1B H1B 125.8 . . ?
C1B C2B C3B 106.8(7) . . ?
C1B C2B H2B 126.6 . . ?
C3B C2B H2B 126.6 . . ?
N2B C3B C2B 108.2(6) . . ?
N2B C3B C4B 116.6(6) . . ?
C2B C3B C4B 135.2(7) . . ?
C9B C4B C5B 122.7(7) . . ?
C9B C4B C3B 121.7(7) . . ?
C5B C4B C3B 115.6(6) . . ?
C6B C5B C4B 113.6(6) . . ?
C6B C5B Nd1 127.0(5) . . ?
C4B C5B Nd1 119.4(5) . . ?
C7B C6B C5B 123.5(7) . . ?
C7B C6B H6B 118.3 . . ?
C5B C6B H6B 118.3 . . ?
C8B C7B C6B 120.3(7) . . ?
C8B C7B H7B 119.9 . . ?
C6B C7B H7B 119.9 . . ?
C9B C8B C7B 118.8(7) . . ?
C9B C8B H8B 120.6 . . ?
C7B C8B H8B 120.6 . . ?
C8B C9B C4B 121.1(8) . . ?
C8B C9B H9B 119.5 . . ?
C4B C9B H9B 119.5 . . ?
C10B N3B N4B 110.4(7) . . ?
C10B N3B B1B 122.7(7) . . ?
N4B N3B B1B 126.9(6) . . ?
C12B N4B N3B 104.2(6) . . ?
C12B N4B Nd1 139.6(5) . . ?
N3B N4B Nd1 115.8(4) . . ?
N3B C10B C11B 108.4(7) . . ?
N3B C10B H10B 125.8 . . ?
C11B C10B H10B 125.8 . . ?
C10B C11B C12B 106.1(7) . . ?
C10B C11B H11B 127.0 . . ?
C12B C11B H11B 127.0 . . ?
N4B C12B C11B 110.9(8) . . ?
N4B C12B C13B 123.6(7) . . ?
C11B C12B C13B 125.3(8) . . ?
C14B C13B C18B 117.2(9) . . ?
C14B C13B C12B 124.9(7) . . ?
C18B C13B C12B 117.8(9) . . ?
C13B C14B C15B 123.9(9) . . ?
C13B C14B H14B 118.1 . . ?
C15B C14B H14B 118.1 . . ?
C16B C15B C14B 119.5(11) . . ?
C16B C15B H15B 120.3 . . ?
C14B C15B H15B 120.3 . . ?
C17B C16B C15B 118.5(12) . . ?
C17B C16B H16B 120.8 . . ?
C15B C16B H16B 120.8 . . ?
C16B C17B C18B 123.4(13) . . ?
C16B C17B H17B 118.3 . . ?
C18B C17B H17B 118.3 . . ?
C13B C18B C17B 117.5(12) . . ?
C13B C18B H18B 121.2 . . ?
C17B C18B H18B 121.2 . . ?
C19B N5B N6B 109.9(6) . . ?
C19B N5B B1B 124.2(7) . . ?
N6B N5B B1B 125.3(6) . . ?
C21B N6B N5B 105.4(6) . . ?
C21B N6B Nd1 134.4(5) . . ?
N5B N6B Nd1 119.4(4) . . ?
N5B C19B C20B 109.0(7) . . ?
N5B C19B H19B 125.5 . . ?
C20B C19B H19B 125.5 . . ?
C19B C20B C21B 105.2(7) . . ?
C19B C20B H20B 127.4 . . ?
C21B C20B H20B 127.4 . . ?
N6B C21B C20B 110.4(7) . . ?
N6B C21B C22B 123.0(7) . . ?
C20B C21B C22B 126.5(7) . . ?
C23B C22B C27B 118.6(8) . . ?
C23B C22B C21B 121.2(7) . . ?
C27B C22B C21B 120.2(7) . . ?
C24B C23B C22B 121.2(8) . . ?
C24B C23B H23B 119.4 . . ?
C22B C23B H23B 119.4 . . ?
C25B C24B C23B 119.9(9) . . ?
C25B C24B H24B 120.1 . . ?
C23B C24B H24B 120.1 . . ?
C26B C25B C24B 119.2(9) . . ?
C26B C25B H25B 120.4 . . ?
C24B C25B H25B 120.4 . . ?
C25B C26B C27B 121.3(9) . . ?
C25B C26B H26B 119.4 . . ?
C27B C26B H26B 119.4 . . ?
C26B C27B C22B 119.8(9) . . ?
C26B C27B H27B 120.1 . . ?
C22B C27B H27B 120.1 . . ?
N1B B1B N5B 110.6(6) . . ?
N1B B1B N3B 108.9(6) . . ?
N5B B1B N3B 110.5(6) . . ?
N1B B1B H1BA 108.9 . . ?
N5B B1B H1BA 108.9 . . ?
N3B B1B H1BA 108.9 . . ?
N2D Nd1A N6C 120.8(2) . . ?
N2D Nd1A N4C 118.68(19) . . ?
N6C Nd1A N4C 84.72(18) . . ?
N2D Nd1A C5D 64.09(19) . . ?
N6C Nd1A C5D 74.9(2) . . ?
N4C Nd1A C5D 73.1(2) . . ?
N2D Nd1A N6D 72.85(18) . . ?
N6C Nd1A N6D 163.0(2) . . ?
N4C Nd1A N6D 97.52(18) . . ?
C5D Nd1A N6D 121.9(2) . . ?
N2D Nd1A N4D 73.25(18) . . ?
N6C Nd1A N4D 99.04(19) . . ?
N4C Nd1A N4D 163.5(2) . . ?
C5D Nd1A N4D 123.4(2) . . ?
N6D Nd1A N4D 74.29(18) . . ?
N2D Nd1A N2C 162.18(19) . . ?
N6C Nd1A N2C 70.02(17) . . ?
N4C Nd1A N2C 74.41(17) . . ?
C5D Nd1A N2C 133.64(19) . . ?
N6D Nd1A N2C 94.29(17) . . ?
N4D Nd1A N2C 91.65(17) . . ?
C1C N1C N2C 108.6(6) . . ?
C1C N1C B1C 125.9(6) . . ?
N2C N1C B1C 125.5(6) . . ?
C3C N2C N1C 105.8(5) . . ?
C3C N2C Nd1A 143.2(5) . . ?
N1C N2C Nd1A 110.8(4) . . ?
N1C C1C C2C 110.2(7) . . ?
N1C C1C H1C 124.9 . . ?
C2C C1C H1C 124.9 . . ?
C1C C2C C3C 105.7(7) . . ?
C1C C2C H2C 127.1 . . ?
C3C C2C H2C 127.1 . . ?
N2C C3C C2C 109.5(7) . . ?
N2C C3C C4C 123.4(7) . . ?
C2C C3C C4C 126.8(7) . . ?
C5C C4C C9C 116.2(8) . . ?
C5C C4C C3C 123.1(7) . . ?
C9C C4C C3C 120.4(7) . . ?
C4C C5C C6C 121.8(8) . . ?
C4C C5C H5C 119.1 . . ?
C6C C5C H5C 119.1 . . ?
C7C C6C C5C 120.4(9) . . ?
C7C C6C H6C 119.8 . . ?
C5C C6C H6C 119.8 . . ?
C6C C7C C8C 119.2(9) . . ?
C6C C7C H7C 120.4 . . ?
C8C C7C H7C 120.4 . . ?
C7C C8C C9C 120.1(10) . . ?
C7C C8C H8C 120.0 . . ?
C9C C8C H8C 120.0 . . ?
C4C C9C C8C 121.8(9) . . ?
C4C C9C H9C 119.1 . . ?
C8C C9C H9C 119.1 . . ?
C10C N3C N4C 109.2(6) . . ?
C10C N3C B1C 124.6(6) . . ?
N4C N3C B1C 125.5(6) . . ?
C12C N4C N3C 105.9(5) . . ?
C12C N4C Nd1A 137.1(5) . . ?
N3C N4C Nd1A 116.6(4) . . ?
N3C C10C C11C 108.9(7) . . ?
N3C C10C H10C 125.6 . . ?
C11C C10C H10C 125.6 . . ?
C10C C11C C12C 105.4(7) . . ?
C10C C11C H11C 127.3 . . ?
C12C C11C H11C 127.3 . . ?
N4C C12C C11C 110.2(6) . . ?
N4C C12C C13C 123.3(6) . . ?
C11C C12C C13C 126.2(7) . . ?
C18C C13C C14C 116.6(7) . . ?
C18C C13C C12C 121.4(7) . . ?
C14C C13C C12C 121.7(6) . . ?
C15C C14C C13C 121.1(7) . . ?
C15C C14C H14C 119.4 . . ?
C13C C14C H14C 119.4 . . ?
C16C C15C C14C 119.9(8) . . ?
C16C C15C H15C 120.1 . . ?
C14C C15C H15C 120.1 . . ?
C17C C16C C15C 119.5(8) . . ?
C17C C16C H16C 120.2 . . ?
C15C C16C H16C 120.2 . . ?
C16C C17C C18C 120.9(8) . . ?
C16C C17C H17C 119.5 . . ?
C18C C17C H17C 119.5 . . ?
C17C C18C C13C 121.4(8) . . ?
C17C C18C H18C 119.3 . . ?
C13C C18C H18C 119.3 . . ?
C19C N5C N6C 108.3(6) . . ?
C19C N5C B1C 126.6(6) . . ?
N6C N5C B1C 123.9(6) . . ?
C21C N6C N5C 106.7(6) . . ?
C21C N6C Nd1A 135.2(5) . . ?
N5C N6C Nd1A 116.7(4) . . ?
N5C C19C C20C 109.8(7) . . ?
N5C C19C H19C 125.1 . . ?
C20C C19C H19C 125.1 . . ?
C19C C20C C21C 105.1(6) . . ?
C19C C20C H20C 127.4 . . ?
C21C C20C H20C 127.4 . . ?
N6C C21C C20C 110.2(7) . . ?
N6C C21C C22C 121.3(7) . . ?
C20C C21C C22C 128.3(7) . . ?
C23C C22C C27C 118.7(8) . . ?
C23C C22C C21C 120.5(7) . . ?
C27C C22C C21C 120.5(7) . . ?
C22C C23C C24C 121.3(8) . . ?
C22C C23C H23C 119.3 . . ?
C24C C23C H23C 119.3 . . ?
C23C C24C C25C 119.6(9) . . ?
C23C C24C H24C 120.2 . . ?
C25C C24C H24C 120.2 . . ?
C26C C25C C24C 118.5(9) . . ?
C26C C25C H25C 120.7 . . ?
C24C C25C H25C 120.7 . . ?
C25C C26C C27C 123.3(9) . . ?
C25C C26C H26C 118.4 . . ?
C27C C26C H26C 118.4 . . ?
C26C C27C C22C 118.1(9) . . ?
C26C C27C H27C 121.0 . . ?
C22C C27C H27C 121.0 . . ?
N1C B1C N5C 111.0(6) . . ?
N1C B1C N3C 111.3(6) . . ?
N5C B1C N3C 113.4(6) . . ?
N1C B1C H1CA 106.9 . . ?
N5C B1C H1CA 106.9 . . ?
N3C B1C H1CA 106.9 . . ?
C1D N1D N2D 108.7(6) . . ?
C1D N1D B1D 130.8(6) . . ?
N2D N1D B1D 120.4(6) . . ?
C3D N2D N1D 107.7(6) . . ?
C3D N2D Nd1A 124.3(4) . . ?
N1D N2D Nd1A 127.9(4) . . ?
N1D C1D C2D 108.5(7) . . ?
N1D C1D H1D 125.8 . . ?
C2D C1D H1D 125.8 . . ?
C1D C2D C3D 106.8(7) . . ?
C1D C2D H2D 126.6 . . ?
C3D C2D H2D 126.6 . . ?
N2D C3D C2D 108.1(6) . . ?
N2D C3D C4D 116.6(6) . . ?
C2D C3D C4D 135.2(7) . . ?
C9D C4D C5D 122.7(7) . . ?
C9D C4D C3D 121.7(7) . . ?
C5D C4D C3D 115.6(6) . . ?
C6D C5D C4D 113.5(7) . . ?
C6D C5D Nd1A 126.9(5) . . ?
C4D C5D Nd1A 119.3(5) . . ?
C7D C6D C5D 123.5(7) . . ?
C7D C6D H6D 118.3 . . ?
C5D C6D H6D 118.3 . . ?
C8D C7D C6D 120.2(7) . . ?
C8D C7D H7D 119.9 . . ?
C6D C7D H7D 119.9 . . ?
C9D C8D C7D 118.8(7) . . ?
C9D C8D H8D 120.6 . . ?
C7D C8D H8D 120.6 . . ?
C8D C9D C4D 121.1(8) . . ?
C8D C9D H9D 119.5 . . ?
C4D C9D H9D 119.5 . . ?
C10D N3D N4D 110.4(7) . . ?
C10D N3D B1D 122.7(7) . . ?
N4D N3D B1D 126.9(6) . . ?
C12D N4D N3D 104.2(6) . . ?
C12D N4D Nd1A 139.6(5) . . ?
N3D N4D Nd1A 115.8(4) . . ?
N3D C10D C11D 108.4(8) . . ?
N3D C10D H10D 125.8 . . ?
C11D C10D H10D 125.8 . . ?
C10D C11D C12D 106.1(7) . . ?
C10D C11D H11D 127.0 . . ?
C12D C11D H11D 127.0 . . ?
N4D C12D C11D 110.9(8) . . ?
N4D C12D C13D 123.6(7) . . ?
C11D C12D C13D 125.3(8) . . ?
C14D C13D C18D 117.2(9) . . ?
C14D C13D C12D 124.9(8) . . ?
C18D C13D C12D 117.8(9) . . ?
C13D C14D C15D 123.9(9) . . ?
C13D C14D H14D 118.1 . . ?
C15D C14D H14D 118.1 . . ?
C16D C15D C14D 119.5(11) . . ?
C16D C15D H15D 120.3 . . ?
C14D C15D H15D 120.3 . . ?
C17D C16D C15D 118.5(12) . . ?
C17D C16D H16D 120.8 . . ?
C15D C16D H16D 120.8 . . ?
C16D C17D C18D 123.3(13) . . ?
C16D C17D H17D 118.3 . . ?
C18D C17D H17D 118.3 . . ?
C13D C18D C17D 117.5(12) . . ?
C13D C18D H18D 121.2 . . ?
C17D C18D H18D 121.2 . . ?
C19D N5D N6D 109.9(7) . . ?
C19D N5D B1D 124.3(7) . . ?
N6D N5D B1D 125.3(6) . . ?
C21D N6D N5D 105.4(6) . . ?
C21D N6D Nd1A 134.4(5) . . ?
N5D N6D Nd1A 119.3(4) . . ?
N5D C19D C20D 109.0(7) . . ?
N5D C19D H19D 125.5 . . ?
C20D C19D H19D 125.5 . . ?
C19D C20D C21D 105.1(7) . . ?
C19D C20D H20D 127.4 . . ?
C21D C20D H20D 127.4 . . ?
N6D C21D C20D 110.3(7) . . ?
N6D C21D C22D 123.0(7) . . ?
C20D C21D C22D 126.4(7) . . ?
C23D C22D C27D 118.6(8) . . ?
C23D C22D C21D 121.1(7) . . ?
C27D C22D C21D 120.2(7) . . ?
C24D C23D C22D 121.1(8) . . ?
C24D C23D H23D 119.4 . . ?
C22D C23D H23D 119.4 . . ?
C25D C24D C23D 119.8(9) . . ?
C25D C24D H24D 120.1 . . ?
C23D C24D H24D 120.1 . . ?
C26D C25D C24D 119.2(10) . . ?
C26D C25D H25D 120.4 . . ?
C24D C25D H25D 120.4 . . ?
C25D C26D C27D 121.2(9) . . ?
C25D C26D H26D 119.4 . . ?
C27D C26D H26D 119.4 . . ?
C26D C27D C22D 119.8(9) . . ?
C26D C27D H27D 120.1 . . ?
C22D C27D H27D 120.1 . . ?
N1D B1D N5D 110.6(7) . . ?
N1D B1D N3D 108.9(7) . . ?
N5D B1D N3D 110.5(7) . . ?
N1D B1D H1DA 108.9 . . ?
N5D B1D H1DA 108.9 . . ?
N3D B1D H1DA 108.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1A N1A N2A C3A -0.4(9) . . . . ?
B1A N1A N2A C3A 179.9(6) . . . . ?
C1A N1A N2A Nd1 -177.5(7) . . . . ?
B1A N1A N2A Nd1 2.9(8) . . . . ?
N2B Nd1 N2A C3A 5.8(11) . . . . ?
N6A Nd1 N2A C3A 136.3(8) . . . . ?
N4A Nd1 N2A C3A -133.7(8) . . . . ?
C5B Nd1 N2A C3A 179.3(7) . . . . ?
N6B Nd1 N2A C3A -37.1(8) . . . . ?
N4B Nd1 N2A C3A 37.3(8) . . . . ?
N2B Nd1 N2A N1A -179.0(5) . . . . ?
N6A Nd1 N2A N1A -48.4(4) . . . . ?
N4A Nd1 N2A N1A 41.5(4) . . . . ?
C5B Nd1 N2A N1A -5.4(5) . . . . ?
N6B Nd1 N2A N1A 138.2(4) . . . . ?
N4B Nd1 N2A N1A -147.5(4) . . . . ?
N2A N1A C1A C2A 0.2(12) . . . . ?
B1A N1A C1A C2A 179.8(9) . . . . ?
N1A C1A C2A C3A 0.1(14) . . . . ?
N1A N2A C3A C2A 0.5(9) . . . . ?
Nd1 N2A C3A C2A 175.9(8) . . . . ?
N1A N2A C3A C4A -179.7(6) . . . . ?
Nd1 N2A C3A C4A -4.3(12) . . . . ?
C1A C2A C3A N2A -0.4(12) . . . . ?
C1A C2A C3A C4A 179.8(9) . . . . ?
N2A C3A C4A C5A 2.8(12) . . . . ?
C2A C3A C4A C5A -177.4(10) . . . . ?
N2A C3A C4A C9A -177.1(9) . . . . ?
C2A C3A C4A C9A 2.7(13) . . . . ?
C9A C4A C5A C6A 1.8(13) . . . . ?
C3A C4A C5A C6A -178.1(8) . . . . ?
C4A C5A C6A C7A -2.9(14) . . . . ?
C5A C6A C7A C8A 1.1(17) . . . . ?
C6A C7A C8A C9A 2(2) . . . . ?
C5A C4A C9A C8A 1.0(16) . . . . ?
C3A C4A C9A C8A -179.1(12) . . . . ?
C7A C8A C9A C4A -3(2) . . . . ?
C10A N3A N4A C12A -0.8(8) . . . . ?
B1A N3A N4A C12A -177.4(7) . . . . ?
C10A N3A N4A Nd1 -173.9(5) . . . . ?
B1A N3A N4A Nd1 9.5(8) . . . . ?
N2B Nd1 N4A C12A -23.8(7) . . . . ?
N6A Nd1 N4A C12A -146.2(7) . . . . ?
C5B Nd1 N4A C12A -70.4(6) . . . . ?
N6B Nd1 N4A C12A 50.8(7) . . . . ?
N4B Nd1 N4A C12A 109.7(8) . . . . ?
N2A Nd1 N4A C12A 143.1(7) . . . . ?
N2B Nd1 N4A N3A 146.5(4) . . . . ?
N6A Nd1 N4A N3A 24.1(4) . . . . ?
C5B Nd1 N4A N3A 99.8(4) . . . . ?
N6B Nd1 N4A N3A -139.0(4) . . . . ?
N4B Nd1 N4A N3A -80.0(8) . . . . ?
N2A Nd1 N4A N3A -46.6(4) . . . . ?
N4A N3A C10A C11A 0.4(9) . . . . ?
B1A N3A C10A C11A 177.0(7) . . . . ?
N3A C10A C11A C12A 0.1(10) . . . . ?
N3A N4A C12A C11A 0.8(8) . . . . ?
Nd1 N4A C12A C11A 171.8(6) . . . . ?
N3A N4A C12A C13A 178.6(7) . . . . ?
Nd1 N4A C12A C13A -10.4(11) . . . . ?
C10A C11A C12A N4A -0.6(10) . . . . ?
C10A C11A C12A C13A -178.3(8) . . . . ?
N4A C12A C13A C18A -163.0(8) . . . . ?
C11A C12A C13A C18A 14.4(12) . . . . ?
N4A C12A C13A C14A 19.0(13) . . . . ?
C11A C12A C13A C14A -163.6(10) . . . . ?
C18A C13A C14A C15A 4.2(13) . . . . ?
C12A C13A C14A C15A -177.7(10) . . . . ?
C13A C14A C15A C16A -3.0(16) . . . . ?
C14A C15A C16A C17A 0.0(17) . . . . ?
C15A C16A C17A C18A 1.7(16) . . . . ?
C16A C17A C18A C13A -0.5(14) . . . . ?
C14A C13A C18A C17A -2.4(12) . . . . ?
C12A C13A C18A C17A 179.4(9) . . . . ?
C19A N5A N6A C21A 0.1(8) . . . . ?
B1A N5A N6A C21A 168.6(6) . . . . ?
C19A N5A N6A Nd1 168.2(5) . . . . ?
B1A N5A N6A Nd1 -23.3(8) . . . . ?
N2B Nd1 N6A C21A 25.8(7) . . . . ?
N4A Nd1 N6A C21A 146.2(7) . . . . ?
C5B Nd1 N6A C21A 72.3(7) . . . . ?
N6B Nd1 N6A C21A -115.3(8) . . . . ?
N4B Nd1 N6A C21A -50.0(7) . . . . ?
N2A Nd1 N6A C21A -138.5(7) . . . . ?
N2B Nd1 N6A N5A -138.0(4) . . . . ?
N4A Nd1 N6A N5A -17.6(5) . . . . ?
C5B Nd1 N6A N5A -91.5(5) . . . . ?
N6B Nd1 N6A N5A 80.8(8) . . . . ?
N4B Nd1 N6A N5A 146.1(5) . . . . ?
N2A Nd1 N6A N5A 57.7(4) . . . . ?
N6A N5A C19A C20A 0.1(9) . . . . ?
B1A N5A C19A C20A -168.1(7) . . . . ?
N5A C19A C20A C21A -0.2(9) . . . . ?
N5A N6A C21A C20A -0.2(8) . . . . ?
Nd1 N6A C21A C20A -165.1(5) . . . . ?
N5A N6A C21A C22A -179.9(6) . . . . ?
Nd1 N6A C21A C22A 15.2(11) . . . . ?
C19A C20A C21A N6A 0.2(9) . . . . ?
C19A C20A C21A C22A 179.9(7) . . . . ?
N6A C21A C22A C23A -33.4(11) . . . . ?
C20A C21A C22A C23A 147.0(8) . . . . ?
N6A C21A C22A C27A 145.5(8) . . . . ?
C20A C21A C22A C27A -34.1(12) . . . . ?
C27A C22A C23A C24A -1.9(12) . . . . ?
C21A C22A C23A C24A 177.0(7) . . . . ?
C22A C23A C24A C25A 0.2(14) . . . . ?
C23A C24A C25A C26A 2.0(17) . . . . ?
C24A C25A C26A C27A -3(2) . . . . ?
C25A C26A C27A C22A 0.9(18) . . . . ?
C23A C22A C27A C26A 1.3(14) . . . . ?
C21A C22A C27A C26A -177.6(9) . . . . ?
C1A N1A B1A N5A -118.6(9) . . . . ?
N2A N1A B1A N5A 61.0(8) . . . . ?
C1A N1A B1A N3A 114.1(10) . . . . ?
N2A N1A B1A N3A -66.3(8) . . . . ?
C19A N5A B1A N1A 113.3(8) . . . . ?
N6A N5A B1A N1A -53.0(8) . . . . ?
C19A N5A B1A N3A -120.6(8) . . . . ?
N6A N5A B1A N3A 73.1(8) . . . . ?
C10A N3A B1A N1A -113.8(8) . . . . ?
N4A N3A B1A N1A 62.3(8) . . . . ?
C10A N3A B1A N5A 120.2(8) . . . . ?
N4A N3A B1A N5A -63.7(8) . . . . ?
C1B N1B N2B C3B -0.3(9) . . . . ?
B1B N1B N2B C3B 178.8(7) . . . . ?
C1B N1B N2B Nd1 179.8(7) . . . . ?
B1B N1B N2B Nd1 -1.1(9) . . . . ?
N6A Nd1 N2B C3B 50.3(6) . . . . ?
N4A Nd1 N2B C3B -51.4(6) . . . . ?
C5B Nd1 N2B C3B -0.8(5) . . . . ?
N6B Nd1 N2B C3B -140.7(6) . . . . ?
N4B Nd1 N2B C3B 141.0(6) . . . . ?
N2A Nd1 N2B C3B 174.1(5) . . . . ?
N6A Nd1 N2B N1B -129.8(5) . . . . ?
N4A Nd1 N2B N1B 128.4(5) . . . . ?
C5B Nd1 N2B N1B 179.1(6) . . . . ?
N6B Nd1 N2B N1B 39.1(5) . . . . ?
N4B Nd1 N2B N1B -39.1(5) . . . . ?
N2A Nd1 N2B N1B -6.1(10) . . . . ?
N2B N1B C1B C2B -0.1(11) . . . . ?
B1B N1B C1B C2B -179.1(9) . . . . ?
N1B C1B C2B C3B 0.4(11) . . . . ?
N1B N2B C3B C2B 0.6(9) . . . . ?
Nd1 N2B C3B C2B -179.5(7) . . . . ?
N1B N2B C3B C4B -179.1(6) . . . . ?
Nd1 N2B C3B C4B 0.8(9) . . . . ?
C1B C2B C3B N2B -0.6(10) . . . . ?
C1B C2B C3B C4B 179.0(9) . . . . ?
N2B C3B C4B C9B -178.3(7) . . . . ?
C2B C3B C4B C9B 2.1(14) . . . . ?
N2B C3B C4B C5B 0.0(9) . . . . ?
C2B C3B C4B C5B -179.7(10) . . . . ?
C9B C4B C5B C6B -1.6(10) . . . . ?
C3B C4B C5B C6B -179.8(6) . . . . ?
C9B C4B C5B Nd1 177.6(6) . . . . ?
C3B C4B C5B Nd1 -0.6(8) . . . . ?
N2B Nd1 C5B C6B 179.7(6) . . . . ?
N6A Nd1 C5B C6B 43.6(6) . . . . ?
N4A Nd1 C5B C6B -45.5(6) . . . . ?
N6B Nd1 C5B C6B -133.8(6) . . . . ?
N4B Nd1 C5B C6B 134.5(6) . . . . ?
N2A Nd1 C5B C6B 1.9(7) . . . . ?
N2B Nd1 C5B C4B 0.7(5) . . . . ?
N6A Nd1 C5B C4B -135.5(5) . . . . ?
N4A Nd1 C5B C4B 135.5(5) . . . . ?
N6B Nd1 C5B C4B 47.1(6) . . . . ?
N4B Nd1 C5B C4B -44.5(6) . . . . ?
N2A Nd1 C5B C4B -177.1(5) . . . . ?
C4B C5B C6B C7B 0.9(10) . . . . ?
Nd1 C5B C6B C7B -178.1(6) . . . . ?
C5B C6B C7B C8B -0.3(12) . . . . ?
C6B C7B C8B C9B 0.1(12) . . . . ?
C7B C8B C9B C4B -0.7(13) . . . . ?
C5B C4B C9B C8B 1.6(12) . . . . ?
C3B C4B C9B C8B 179.7(9) . . . . ?
C10B N3B N4B C12B 1.6(8) . . . . ?
B1B N3B N4B C12B 177.4(7) . . . . ?
C10B N3B N4B Nd1 -172.7(5) . . . . ?
B1B N3B N4B Nd1 3.1(9) . . . . ?
N2B Nd1 N4B C12B -136.0(8) . . . . ?
N6A Nd1 N4B C12B -16.5(8) . . . . ?
N4A Nd1 N4B C12B 85.6(10) . . . . ?
C5B Nd1 N4B C12B -94.2(8) . . . . ?
N6B Nd1 N4B C12B 147.6(8) . . . . ?
N2A Nd1 N4B C12B 53.6(8) . . . . ?
N2B Nd1 N4B N3B 35.4(4) . . . . ?
N6A Nd1 N4B N3B 155.0(5) . . . . ?
N4A Nd1 N4B N3B -102.9(7) . . . . ?
C5B Nd1 N4B N3B 77.2(5) . . . . ?
N6B Nd1 N4B N3B -41.0(4) . . . . ?
N2A Nd1 N4B N3B -135.0(5) . . . . ?
N4B N3B C10B C11B -1.3(10) . . . . ?
B1B N3B C10B C11B -177.2(8) . . . . ?
N3B C10B C11B C12B 0.4(11) . . . . ?
N3B N4B C12B C11B -1.4(9) . . . . ?
Nd1 N4B C12B C11B 170.7(6) . . . . ?
N3B N4B C12B C13B 175.1(8) . . . . ?
Nd1 N4B C12B C13B -12.8(13) . . . . ?
C10B C11B C12B N4B 0.7(11) . . . . ?
C10B C11B C12B C13B -175.8(9) . . . . ?
N4B C12B C13B C14B -13.0(15) . . . . ?
C11B C12B C13B C14B 163.0(10) . . . . ?
N4B C12B C13B C18B 167.8(10) . . . . ?
C11B C12B C13B C18B -16.3(15) . . . . ?
C18B C13B C14B C15B 2.0(18) . . . . ?
C12B C13B C14B C15B -177.2(10) . . . . ?
C13B C14B C15B C16B -1(2) . . . . ?
C14B C15B C16B C17B 0(2) . . . . ?
C15B C16B C17B C18B 0(3) . . . . ?
C14B C13B C18B C17B -1.6(19) . . . . ?
C12B C13B C18B C17B 177.7(12) . . . . ?
C16B C17B C18B C13B 1(3) . . . . ?
C19B N5B N6B C21B -0.1(8) . . . . ?
B1B N5B N6B C21B -172.1(7) . . . . ?
C19B N5B N6B Nd1 171.3(5) . . . . ?
B1B N5B N6B Nd1 -0.7(9) . . . . ?
N2B Nd1 N6B C21B 132.1(6) . . . . ?
N6A Nd1 N6B C21B -82.3(9) . . . . ?
N4A Nd1 N6B C21B 14.3(6) . . . . ?
C5B Nd1 N6B C21B 89.1(6) . . . . ?
N4B Nd1 N6B C21B -151.0(6) . . . . ?
N2A Nd1 N6B C21B -60.5(6) . . . . ?
N2B Nd1 N6B N5B -36.2(5) . . . . ?
N6A Nd1 N6B N5B 109.4(7) . . . . ?
N4A Nd1 N6B N5B -154.0(5) . . . . ?
C5B Nd1 N6B N5B -79.2(5) . . . . ?
N4B Nd1 N6B N5B 40.7(5) . . . . ?
N2A Nd1 N6B N5B 131.2(5) . . . . ?
N6B N5B C19B C20B 0.0(10) . . . . ?
B1B N5B C19B C20B 172.1(8) . . . . ?
N5B C19B C20B C21B 0.1(11) . . . . ?
N5B N6B C21B C20B 0.1(8) . . . . ?
Nd1 N6B C21B C20B -169.3(6) . . . . ?
N5B N6B C21B C22B -179.4(6) . . . . ?
Nd1 N6B C21B C22B 11.2(10) . . . . ?
C19B C20B C21B N6B -0.2(10) . . . . ?
C19B C20B C21B C22B 179.3(8) . . . . ?
N6B C21B C22B C23B 37.0(11) . . . . ?
C20B C21B C22B C23B -142.4(9) . . . . ?
N6B C21B C22B C27B -142.3(9) . . . . ?
C20B C21B C22B C27B 38.3(12) . . . . ?
C27B C22B C23B C24B 1.5(12) . . . . ?
C21B C22B C23B C24B -177.9(8) . . . . ?
C22B C23B C24B C25B -0.3(13) . . . . ?
C23B C24B C25B C26B -0.4(14) . . . . ?
C24B C25B C26B C27B -0.1(16) . . . . ?
C25B C26B C27B C22B 1.2(17) . . . . ?
C23B C22B C27B C26B -1.9(14) . . . . ?
C21B C22B C27B C26B 177.5(9) . . . . ?
C1B N1B B1B N5B 119.9(10) . . . . ?
N2B N1B B1B N5B -59.1(9) . . . . ?
C1B N1B B1B N3B -118.5(10) . . . . ?
N2B N1B B1B N3B 62.5(9) . . . . ?
C19B N5B B1B N1B -111.5(8) . . . . ?
N6B N5B B1B N1B 59.4(9) . . . . ?
C19B N5B B1B N3B 127.8(7) . . . . ?
N6B N5B B1B N3B -61.3(9) . . . . ?
C10B N3B B1B N1B 112.5(8) . . . . ?
N4B N3B B1B N1B -62.7(9) . . . . ?
C10B N3B B1B N5B -125.8(8) . . . . ?
N4B N3B B1B N5B 59.0(9) . . . . ?
C1C N1C N2C C3C 0(4) . . . . ?
B1C N1C N2C C3C -178(2) . . . . ?
C1C N1C N2C Nd1A 175(4) . . . . ?
B1C N1C N2C Nd1A -2.5(14) . . . . ?
N2D Nd1A N2C C3C -8(3) . . . . ?
N6C Nd1A N2C C3C -139(3) . . . . ?
N4C Nd1A N2C C3C 131(3) . . . . ?
C5D Nd1A N2C C3C 178(3) . . . . ?
N6D Nd1A N2C C3C 35(3) . . . . ?
N4D Nd1A N2C C3C -40(3) . . . . ?
N2D Nd1A N2C N1C 178.8(8) . . . . ?
N6C Nd1A N2C N1C 48.3(7) . . . . ?
N4C Nd1A N2C N1C -41.7(7) . . . . ?
C5D Nd1A N2C N1C 5.2(8) . . . . ?
N6D Nd1A N2C N1C -138.3(7) . . . . ?
N4D Nd1A N2C N1C 147.3(7) . . . . ?
N2C N1C C1C C2C -2(5) . . . . ?
B1C N1C C1C C2C 176(4) . . . . ?
N1C C1C C2C C3C 3(6) . . . . ?
N1C N2C C3C C2C 2(4) . . . . ?
Nd1A N2C C3C C2C -171(6) . . . . ?
N1C N2C C3C C4C 176(3) . . . . ?
Nd1A N2C C3C C4C 3(5) . . . . ?
C1C C2C C3C N2C -3(5) . . . . ?
C1C C2C C3C C4C -177(4) . . . . ?
N2C C3C C4C C5C -7(5) . . . . ?
C2C C3C C4C C5C 166(6) . . . . ?
N2C C3C C4C C9C 167(5) . . . . ?
C2C C3C C4C C9C -20(6) . . . . ?
C9C C4C C5C C6C -6(4) . . . . ?
C3C C4C C5C C6C 167(5) . . . . ?
C4C C5C C6C C7C 5(8) . . . . ?
C5C C6C C7C C8C 0(10) . . . . ?
C6C C7C C8C C9C -4(8) . . . . ?
C5C C4C C9C C8C 2(8) . . . . ?
C3C C4C C9C C8C -172(8) . . . . ?
C7C C8C C9C C4C 3(9) . . . . ?
C10C N3C N4C C12C -6.2(18) . . . . ?
B1C N3C N4C C12C 165(2) . . . . ?
C10C N3C N4C Nd1A 179.5(13) . . . . ?
B1C N3C N4C Nd1A -9.1(13) . . . . ?
N2D Nd1A N4C C12C 41(2) . . . . ?
N6C Nd1A N4C C12C 164(3) . . . . ?
C5D Nd1A N4C C12C 88(3) . . . . ?
N6D Nd1A N4C C12C -33(3) . . . . ?
N4D Nd1A N4C C12C -92(3) . . . . ?
N2C Nd1A N4C C12C -126(3) . . . . ?
N2D Nd1A N4C N3C -146.7(6) . . . . ?
N6C Nd1A N4C N3C -24.3(7) . . . . ?
C5D Nd1A N4C N3C -100.1(7) . . . . ?
N6D Nd1A N4C N3C 138.8(7) . . . . ?
N4D Nd1A N4C N3C 79.8(9) . . . . ?
N2C Nd1A N4C N3C 46.4(6) . . . . ?
N4C N3C C10C C11C 7(3) . . . . ?
B1C N3C C10C C11C -165(3) . . . . ?
N3C C10C C11C C12C -4(4) . . . . ?
N3C N4C C12C C11C 3(3) . . . . ?
Nd1A N4C C12C C11C 176(3) . . . . ?
N3C N4C C12C C13C 178(3) . . . . ?
Nd1A N4C C12C C13C -10(4) . . . . ?
C10C C11C C12C N4C 0(4) . . . . ?
C10C C11C C12C C13C -173(4) . . . . ?
N4C C12C C13C C18C 145(5) . . . . ?
C11C C12C C13C C18C -41(5) . . . . ?
N4C C12C C13C C14C -28(5) . . . . ?
C11C C12C C13C C14C 146(5) . . . . ?
C18C C13C C14C C15C -7(4) . . . . ?
C12C C13C C14C C15C 166(5) . . . . ?
C13C C14C C15C C16C 5(9) . . . . ?
C14C C15C C16C C17C 1(10) . . . . ?
C15C C16C C17C C18C -6(6) . . . . ?
C16C C17C C18C C13C 4(7) . . . . ?
C14C C13C C18C C17C 2(7) . . . . ?
C12C C13C C18C C17C -171(6) . . . . ?
C19C N5C N6C C21C -0.2(17) . . . . ?
B1C N5C N6C C21C -168.2(13) . . . . ?
C19C N5C N6C Nd1A -168.4(15) . . . . ?
B1C N5C N6C Nd1A 23.7(13) . . . . ?
N2D Nd1A N6C C21C -25.9(15) . . . . ?
N4C Nd1A N6C C21C -146.3(15) . . . . ?
C5D Nd1A N6C C21C -72.4(15) . . . . ?
N6D Nd1A N6C C21C 115.2(15) . . . . ?
N4D Nd1A N6C C21C 49.9(15) . . . . ?
N2C Nd1A N6C C21C 138.3(15) . . . . ?
N2D Nd1A N6C N5C 137.8(7) . . . . ?
N4C Nd1A N6C N5C 17.4(7) . . . . ?
C5D Nd1A N6C N5C 91.4(7) . . . . ?
N6D Nd1A N6C N5C -81.0(10) . . . . ?
N4D Nd1A N6C N5C -146.3(7) . . . . ?
N2C Nd1A N6C N5C -57.9(7) . . . . ?
N6C N5C C19C C20C 0(5) . . . . ?
B1C N5C C19C C20C 168(5) . . . . ?
N5C C19C C20C C21C 0(7) . . . . ?
N5C N6C C21C C20C 0(4) . . . . ?
Nd1A N6C C21C C20C 165(4) . . . . ?
N5C N6C C21C C22C 176(2) . . . . ?
Nd1A N6C C21C C22C -19(3) . . . . ?
C19C C20C C21C N6C 0(7) . . . . ?
C19C C20C C21C C22C -175(4) . . . . ?
N6C C21C C22C C23C 37(5) . . . . ?
C20C C21C C22C C23C -147(7) . . . . ?
N6C C21C C22C C27C -136(6) . . . . ?
C20C C21C C22C C27C 40(7) . . . . ?
C27C C22C C23C C24C 7(4) . . . . ?
C21C C22C C23C C24C -166(4) . . . . ?
C22C C23C C24C C25C -6(8) . . . . ?
C23C C24C C25C C26C 0(10) . . . . ?
C24C C25C C26C C27C 6(7) . . . . ?
C25C C26C C27C C22C -5(7) . . . . ?
C23C C22C C27C C26C -2(7) . . . . ?
C21C C22C C27C C26C 171(6) . . . . ?
C1C N1C B1C N5C 121(5) . . . . ?
N2C N1C B1C N5C -61.3(12) . . . . ?
C1C N1C B1C N3C -111(5) . . . . ?
N2C N1C B1C N3C 66.1(12) . . . . ?
C19C N5C B1C N1C -113.0(18) . . . . ?
N6C N5C B1C N1C 52.8(11) . . . . ?
C19C N5C B1C N3C 120.9(18) . . . . ?
N6C N5C B1C N3C -73.4(11) . . . . ?
C10C N3C B1C N1C 107.5(16) . . . . ?
N4C N3C B1C N1C -62.6(11) . . . . ?
C10C N3C B1C N5C -126.5(15) . . . . ?
N4C N3C B1C N5C 63.4(11) . . . . ?
C1D N1D N2D C3D 4(5) . . . . ?
B1D N1D N2D C3D -180(2) . . . . ?
C1D N1D N2D Nd1A -174(5) . . . . ?
B1D N1D N2D Nd1A 3(2) . . . . ?
N6C Nd1A N2D C3D -48(3) . . . . ?
N4C Nd1A N2D C3D 54(3) . . . . ?
C5D Nd1A N2D C3D 3(3) . . . . ?
N6D Nd1A N2D C3D 143(3) . . . . ?
N4D Nd1A N2D C3D -139(3) . . . . ?
N2C Nd1A N2D C3D -172(3) . . . . ?
N6C Nd1A N2D N1D 129.0(13) . . . . ?
N4C Nd1A N2D N1D -129.2(13) . . . . ?
C5D Nd1A N2D N1D -179.9(13) . . . . ?
N6D Nd1A N2D N1D -39.9(13) . . . . ?
N4D Nd1A N2D N1D 38.4(13) . . . . ?
N2C Nd1A N2D N1D 5.3(16) . . . . ?
N2D N1D C1D C2D -2(8) . . . . ?
B1D N1D C1D C2D -178(6) . . . . ?
N1D C1D C2D C3D 0(10) . . . . ?
N1D N2D C3D C2D -3(5) . . . . ?
Nd1A N2D C3D C2D 174(5) . . . . ?
N1D N2D C3D C4D 179(3) . . . . ?
Nd1A N2D C3D C4D -3(5) . . . . ?
C1D C2D C3D N2D 2(8) . . . . ?
C1D C2D C3D C4D 178(6) . . . . ?
N2D C3D C4D C9D -178(4) . . . . ?
C2D C3D C4D C9D 6(7) . . . . ?
N2D C3D C4D C5D 0(5) . . . . ?
C2D C3D C4D C5D -176(7) . . . . ?
C9D C4D C5D C6D 5(4) . . . . ?
C3D C4D C5D C6D -173(5) . . . . ?
C9D C4D C5D Nd1A -180(3) . . . . ?
C3D C4D C5D Nd1A 2(4) . . . . ?
N2D Nd1A C5D C6D 172(4) . . . . ?
N6C Nd1A C5D C6D -52(4) . . . . ?
N4C Nd1A C5D C6D 37(4) . . . . ?
N6D Nd1A C5D C6D 126(4) . . . . ?
N4D Nd1A C5D C6D -143(4) . . . . ?
N2C Nd1A C5D C6D -10(4) . . . . ?
N2D Nd1A C5D C4D -3(2) . . . . ?
N6C Nd1A C5D C4D 133(2) . . . . ?
N4C Nd1A C5D C4D -138(2) . . . . ?
N6D Nd1A C5D C4D -49(2) . . . . ?
N4D Nd1A C5D C4D 43(2) . . . . ?
N2C Nd1A C5D C4D 175(2) . . . . ?
C4D C5D C6D C7D -4(7) . . . . ?
Nd1A C5D C6D C7D -180(6) . . . . ?
C5D C6D C7D C8D 2(15) . . . . ?
C6D C7D C8D C9D 0(21) . . . . ?
C7D C8D C9D C4D 0(19) . . . . ?
C5D C4D C9D C8D -3(11) . . . . ?
C3D C4D C9D C8D 175(11) . . . . ?
C10D N3D N4D C12D 2(4) . . . . ?
B1D N3D N4D C12D -176(3) . . . . ?
C10D N3D N4D Nd1A 177(3) . . . . ?
B1D N3D N4D Nd1A -2(2) . . . . ?
N2D Nd1A N4D C12D 136(3) . . . . ?
N6C Nd1A N4D C12D 16(3) . . . . ?
N4C Nd1A N4D C12D -86(3) . . . . ?
C5D Nd1A N4D C12D 94(3) . . . . ?
N6D Nd1A N4D C12D -148(3) . . . . ?
N2C Nd1A N4D C12D -54(3) . . . . ?
N2D Nd1A N4D N3D -36.1(11) . . . . ?
N6C Nd1A N4D N3D -155.7(12) . . . . ?
N4C Nd1A N4D N3D 102.3(13) . . . . ?
C5D Nd1A N4D N3D -77.9(12) . . . . ?
N6D Nd1A N4D N3D 40.3(11) . . . . ?
N2C Nd1A N4D N3D 134.3(12) . . . . ?
N4D N3D C10D C11D -2(6) . . . . ?
B1D N3D C10D C11D 176(6) . . . . ?
N3D C10D C11D C12D 1(8) . . . . ?
N3D N4D C12D C11D -2(5) . . . . ?
Nd1A N4D C12D C11D -174(5) . . . . ?
N3D N4D C12D C13D -177(3) . . . . ?
Nd1A N4D C12D C13D 10(5) . . . . ?
C10D C11D C12D N4D 0(7) . . . . ?
C10D C11D C12D C13D 176(6) . . . . ?
N4D C12D C13D C14D 25(8) . . . . ?
C11D C12D C13D C14D -149(8) . . . . ?
N4D C12D C13D C18D -150(6) . . . . ?
C11D C12D C13D C18D 35(7) . . . . ?
C18D C13D C14D C15D 4(7) . . . . ?
C12D C13D C14D C15D -172(8) . . . . ?
C13D C14D C15D C16D -3(11) . . . . ?
C14D C15D C16D C17D 2(11) . . . . ?
C15D C16D C17D C18D -3(10) . . . . ?
C14D C13D C18D C17D -4(5) . . . . ?
C12D C13D C18D C17D 172(6) . . . . ?
C16D C17D C18D C13D 4(8) . . . . ?
C19D N5D N6D C21D 1(3) . . . . ?
B1D N5D N6D C21D 173.0(19) . . . . ?
C19D N5D N6D Nd1A -170(2) . . . . ?
B1D N5D N6D Nd1A 2(2) . . . . ?
N2D Nd1A N6D C21D -132.0(15) . . . . ?
N6C Nd1A N6D C21D 82.3(17) . . . . ?
N4C Nd1A N6D C21D -14.3(15) . . . . ?
C5D Nd1A N6D C21D -89.0(15) . . . . ?
N4D Nd1A N6D C21D 151.0(15) . . . . ?
N2C Nd1A N6D C21D 60.5(15) . . . . ?
N2D Nd1A N6D N5D 35.5(12) . . . . ?
N6C Nd1A N6D N5D -110.2(13) . . . . ?
N4C Nd1A N6D N5D 153.2(12) . . . . ?
C5D Nd1A N6D N5D 78.5(12) . . . . ?
N4D Nd1A N6D N5D -41.4(12) . . . . ?
N2C Nd1A N6D N5D -131.9(12) . . . . ?
N6D N5D C19D C20D -4(3) . . . . ?
B1D N5D C19D C20D -176(3) . . . . ?
N5D C19D C20D C21D 5(3) . . . . ?
N5D N6D C21D C20D 2.7(19) . . . . ?
Nd1A N6D C21D C20D 171(2) . . . . ?
N5D N6D C21D C22D -171(2) . . . . ?
Nd1A N6D C21D C22D -3(2) . . . . ?
C19D C20D C21D N6D -5(2) . . . . ?
C19D C20D C21D C22D 169(3) . . . . ?
N6D C21D C22D C23D -49(4) . . . . ?
C20D C21D C22D C23D 138(4) . . . . ?
N6D C21D C22D C27D 135(4) . . . . ?
C20D C21D C22D C27D -38(5) . . . . ?
C27D C22D C23D C24D -4(6) . . . . ?
C21D C22D C23D C24D 179(4) . . . . ?
C22D C23D C24D C25D 6(5) . . . . ?
C23D C24D C25D C26D -3(8) . . . . ?
C24D C25D C26D C27D -3(9) . . . . ?
C25D C26D C27D C22D 5(6) . . . . ?
C23D C22D C27D C26D -1(7) . . . . ?
C21D C22D C27D C26D 175(4) . . . . ?
C1D N1D B1D N5D -126(6) . . . . ?
N2D N1D B1D N5D 58.2(16) . . . . ?
C1D N1D B1D N3D 112(6) . . . . ?
N2D N1D B1D N3D -63.4(15) . . . . ?
C19D N5D B1D N1D 111(2) . . . . ?
N6D N5D B1D N1D -60.4(17) . . . . ?
C19D N5D B1D N3D -129(2) . . . . ?
N6D N5D B1D N3D 60.2(17) . . . . ?
C10D N3D B1D N1D -117(4) . . . . ?
N4D N3D B1D N1D 61.7(18) . . . . ?
C10D N3D B1D N5D 122(4) . . . . ?
N4D N3D B1D N5D -60.0(18) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.511
_refine_diff_density_min -1.048
_refine_diff_density_rms 0.103