# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2014
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
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# data retrieval see:
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# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
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data_kr567q-srb
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C52 H46 N2 O6), C H2 Cl2'
_chemical_formula_sum 'C52.50 H47 Cl N2 O6'
_chemical_formula_weight 837.37
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 22.8894(13)
_cell_length_b 12.5211(6)
_cell_length_c 15.4873(7)
_cell_angle_alpha 90.00
_cell_angle_beta 90.723(3)
_cell_angle_gamma 90.00
_cell_volume 4438.3(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 8118
_cell_measurement_theta_min 2.63
_cell_measurement_theta_max 26.4
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max .2
_exptl_crystal_size_mid .2
_exptl_crystal_size_min .1
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.253
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1764
_exptl_absorpt_coefficient_mu 0.139
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min .6424
_exptl_absorpt_correction_T_max .7454
_exptl_absorpt_process_details Bruker-SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source rotating_anode
_diffrn_radiation_monochromator MONTEL_multi_layer_optics
_diffrn_measurement_device_type Bruker-kappa_APEX2_CCD
_diffrn_measurement_method omega_and_phi_scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 40123
_diffrn_reflns_av_R_equivalents 0.0334
_diffrn_reflns_av_sigmaI/netI 0.0187
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.27
_diffrn_reflns_theta_max 26.42
_reflns_number_total 4537
_reflns_number_gt 3634
_reflns_threshold_expression >2sigma(I)
_computing_data_collection Bruker-SAINT
_computing_cell_refinement Bruker-SAINT
_computing_data_reduction Bruker-SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics CCDC-Mercury
_computing_publication_material Bruker-SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The unit cell contains 4 PBI molecules positioned on a crystallographic centre
of symmetry, therefore Z =4, and furthermore 4 isolated regions (voids)
with additional electron density, positioned each about a crystallographic
2-fold axis. This additional density could only partly be modelled as
discrete atomic sites (GooF(F2) = 1.128, R1 = 0.073, wR2 = 0.229 for I>2s(I)
and was attributed to disordered solvent of 0.5 CH2Cl2 per hole.
The resulting formula C52H46N2O6 . 1/2 CH2Cl2 leads to the derived
constants rho(calcd) = 1.253 g cm -3, mu = 0.139 mm -1, F(000) = 1764.
# disordered solvent partially modelled
FVAR 0.11731 0.84667 0.10360 0.46315 0.04852 0.05569 0.05986
#.....
PART -1
SADI .005 Cl1 C28 Cl2 C28 Cl3 C29 Cl4 C29
EXYZ C28 C29
EADP C28 C29
ISOR .005 Cl1 Cl2 Cl3 Cl4
SIMU .005 Cl2 Cl3
CL1 5 0.493794 1.321239 0.248598 40.25000 51.00000 61.00000 =
71.00000 -0.00196 0.00488 0.01495
C28 1 0.504865 1.181213 0.245746 40.25000 0.04534
AFIX 23
H28A 2 0.511847 1.152645 0.304581 40.25000 -1.20000
H28B 2 0.470580 1.144550 0.219802 40.25000 -1.20000
AFIX 0
CL2 5 0.567339 1.164182 0.180962 40.25000 51.00000 61.00000 =
71.00000 -0.02140 0.00096 0.00652
PART -2
CL3 5 0.575834 1.149970 0.210561 -40.25000 51.00000 61.00000 =
0.04045 0.00199 0.00595 0.01979
C29 1 0.504865 1.181213 0.245746 -40.25000 0.04534
AFIX 23
H29A 2 0.474844 1.136483 0.216726 -40.25000 -1.20000
H29B 2 0.501418 1.173873 0.309125 -40.25000 -1.20000
AFIX 0
CL4 5 0.500332 1.315747 0.212748 -40.25000 51.00000 61.00000 =
71.00000 0.02636 -0.00218 -0.00734
REM R1 = 0.0735 for 3600 Fo > 4sig(Fo) and 0.0894 for all 4537 data
REM 323 parameters refined using 68 restraints
At this stage further additional electron density could still be found in
difference fourier maps. So the "squeeze" procedure with PLATON was
applied to calculate the contribution to the diffraction from this region,
which found 4 voids in the cell, each with a volume of 127 [A3] , each
occupied by 31 electrons. Compared to 42 electrons per molecule of CH2Cl2
this finding leads to a different sum formula of the investigated compound
namely C52H46N2O6 . 0.74 ( CH2Cl2 ) , which means there are 0.74 disordered
solvent molecules per hole.
Final refinements where calculated from "filtered intensity data" with masked
out regions of the disordered electron density: GooF(F2) = 1.066, R1 = 0.0587
, wR2 = 0.1722 for I>2s(I), R1 = 0.0692, wR2 = 0.1808 for all data, 4537
independent reflections [2THeta < 52.84 deg] and 294 parameters.
TITL KR567P in C2/c
CELL 0.71073 22.8894 12.5211 15.4873 90.000 90.723 90.000
ZERR 4.00 0.0013 0.0006 0.0007 0.000 0.003 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H N O Cl
UNIT 210 188 8 24 4
LIST 4
L.S. 22
ACTA
CONF
HTAB 2.5
BOND
FMAP -2
OMIT 0 2 1
OMIT 1 1 0
PLAN 20
TEMP -173.
WGHT 0.101800 2.997800
FVAR 1.16361 0.87540 0.08118 0.46786 0.04686 0.05838 0.07050
MOLE 1
C1 1 0.247014 0.629244 0.156352 11.00000 0.04680 0.04313 =
0.02654 0.00134 -0.00888 -0.00947
C2 1 0.248356 0.692975 0.081987 11.00000 0.03865 0.03201 =
0.02611 -0.00140 -0.00316 -0.00070
C3 1 0.288063 0.783971 0.070608 11.00000 0.04064 0.02734 =
0.02581 -0.00198 -0.00401 0.00074
C4 1 0.322353 0.824813 0.137824 11.00000 0.05240 0.03752 =
0.02609 0.00372 -0.00832 -0.00504
AFIX 43
H4 2 0.319162 0.794145 0.193672 11.00000 -1.20000
AFIX 0
C5 1 0.361189 0.909146 0.125935 11.00000 0.05829 0.03955 =
0.03148 0.00102 -0.01645 -0.01050
AFIX 43
H5 2 0.384652 0.933200 0.173086 11.00000 -1.20000
AFIX 0
C6 1 0.365920 0.957638 0.047289 11.00000 0.04680 0.03343 =
0.03222 0.00217 -0.00897 -0.00490
C7 1 0.328915 0.924146 -0.021545 11.00000 0.04238 0.02958 =
0.02671 -0.00215 -0.00418 -0.00058
C8 1 0.289935 0.836646 -0.011802 11.00000 0.04013 0.02851 =
0.02531 -0.00310 -0.00323 0.00176
C9 1 0.290820 0.958219 -0.164632 11.00000 0.05017 0.04253 =
0.02774 0.00730 -0.00674 -0.00989
AFIX 43
H9 2 0.290294 0.999555 -0.216073 11.00000 -1.20000
AFIX 0
C10 1 0.328668 0.984038 -0.098199 11.00000 0.04104 0.03326 =
0.03017 0.00109 -0.00299 -0.00353
C11 1 0.366812 1.079120 -0.108284 11.00000 0.04042 0.03568 =
0.03109 0.00056 -0.00304 -0.00229
C12 1 0.407831 1.045908 0.036066 11.00000 0.05955 0.04014 =
0.03755 0.00538 -0.01688 -0.01134
EXYZ C13 C13B
EADP C13 C13B
PART 1
SAME C13 C19 C17 C16 C15 C14
SAME C13B C14b C15B C16B C17B C19B
C13 1 0.447886 1.193540 -0.050364 21.00000 0.04264 0.03573 =
0.04042 0.00290 -0.00653 -0.00728
AFIX 13
H13 2 0.475860 1.187550 -0.000479 21.00000 -1.20000
AFIX 0
C14 1 0.416349 1.297401 -0.037774 21.00000 0.04050 0.03537 =
0.04995 -0.00392 0.00050 -0.00468
AFIX 23
H14A 2 0.395604 1.295958 0.017919 21.00000 -1.20000
H14B 2 0.386932 1.307015 -0.084538 21.00000 -1.20000
AFIX 0
C15 1 0.459112 1.390597 -0.038311 21.00000 0.04700 0.03133 =
0.06067 -0.00246 -0.00524 -0.00523
AFIX 23
H15A 2 0.437222 1.458584 -0.034418 21.00000 -1.20000
H15B 2 0.485479 1.385611 0.012694 21.00000 -1.20000
AFIX 0
C16 1 0.494943 1.390392 -0.119571 21.00000 0.05609 0.03852 =
0.05999 0.00508 -0.00203 -0.01287
AFIX 23
H16A 2 0.523099 1.450389 -0.117641 21.00000 -1.20000
H16B 2 0.468870 1.400769 -0.170368 21.00000 -1.20000
AFIX 0
C17 1 0.527860 1.285821 -0.128759 21.00000 0.04123 0.05178 =
0.06559 -0.00142 0.00694 -0.00911
AFIX 23
H17A 2 0.555618 1.277501 -0.079681 21.00000 -1.20000
H17B 2 0.550617 1.287000 -0.182687 21.00000 -1.20000
AFIX 0
C19 1 0.485320 1.190378 -0.130796 21.00000 0.04118 0.04168 =
0.05760 -0.00479 0.00602 -0.00308
AFIX 23
H19A 2 0.460102 1.194269 -0.183107 21.00000 -1.20000
H19B 2 0.507554 1.122611 -0.132578 21.00000 -1.20000
AFIX 0
PART 2
C13B 1 0.447886 1.193540 -0.050364 -21.00000 0.04264 0.03573 =
0.04042 0.00290 -0.00653 -0.00728
AFIX 13
H13B 2 0.440418 1.217261 -0.111162 -21.00000 -1.20000
AFIX 0
C14B 1 0.426209 1.286289 0.000297 -21.00000 31.00000
AFIX 23
H14C 2 0.385038 1.301469 -0.015758 -21.00000 -1.20000
H14D 2 0.428005 1.269568 0.062752 -21.00000 -1.20000
AFIX 0
C15B 1 0.464093 1.383678 -0.018612 -21.00000 31.00000
AFIX 23
H15C 2 0.456924 1.438780 0.025856 -21.00000 -1.20000
H15D 2 0.452178 1.413822 -0.075245 -21.00000 -1.20000
AFIX 0
C16B 1 0.528242 1.359156 -0.020038 -21.00000 31.00000
AFIX 23
H16C 2 0.548993 1.422286 -0.042905 -21.00000 -1.20000
H16D 2 0.542054 1.348024 0.040124 -21.00000 -1.20000
AFIX 0
C17B 1 0.545004 1.264039 -0.072190 -21.00000 31.00000
AFIX 23
H17C 2 0.586850 1.248313 -0.061397 -21.00000 -1.20000
H17D 2 0.540184 1.281544 -0.134209 -21.00000 -1.20000
AFIX 0
C19B 1 0.509136 1.163656 -0.052353 -21.00000 31.00000
AFIX 23
H19C 2 0.515446 1.108902 -0.097398 -21.00000 -1.20000
H19D 2 0.521408 1.133471 0.004105 -21.00000 -1.20000
AFIX 0
PART 0
C20 1 0.272328 0.602937 0.369788 11.00000 0.05370 0.06206 =
0.03670 0.00534 -0.01267 -0.02687
C21 1 0.290273 0.535895 0.437657 11.00000 0.06098 0.07524 =
0.03238 0.00947 -0.00844 -0.03079
AFIX 43
H21 2 0.276172 0.548626 0.494161 11.00000 -1.20000
AFIX 0
C22 1 0.327768 0.452345 0.424050 11.00000 0.05986 0.07918 =
0.04900 0.02926 -0.01760 -0.02422
AFIX 43
H22 2 0.339413 0.408545 0.471305 11.00000 -1.20000
AFIX 0
C23 1 0.348823 0.430913 0.342919 11.00000 0.05279 0.07139 =
0.06114 0.01785 -0.01087 -0.01341
AFIX 43
H23 2 0.373972 0.371578 0.334432 11.00000 -1.20000
AFIX 0
C24 1 0.333391 0.495856 0.273336 11.00000 0.04951 0.06947 =
0.04593 0.01436 -0.00838 -0.01978
C25 1 0.231783 0.694628 0.381841 11.00000 0.07460 0.07175 =
0.05664 -0.00448 -0.01105 -0.01858
AFIX 137
H25A 2 0.252708 0.761651 0.371667 11.00000 -1.50000
H25B 2 0.216983 0.693919 0.440940 11.00000 -1.50000
H25C 2 0.198981 0.688642 0.340846 11.00000 -1.50000
AFIX 0
C26 1 0.357170 0.475387 0.184172 11.00000 0.06497 0.10116 =
0.05678 0.00980 0.00713 -0.01468
AFIX 137
H26A 2 0.326483 0.443960 0.147518 11.00000 -1.50000
H26B 2 0.390295 0.425991 0.188374 11.00000 -1.50000
H26C 2 0.370139 0.542947 0.158854 11.00000 -1.50000
AFIX 0
PART 0
PART 0
N1 3 0.407452 1.100150 -0.042483 11.00000 0.04336 0.03279 =
0.03438 0.00227 -0.00587 -0.00635
O1 4 0.441948 1.070750 0.093292 11.00000 0.11356 0.07384 =
0.05858 0.02900 -0.04749 -0.05641
O2 4 0.362448 1.137273 -0.170771 11.00000 0.05763 0.04621 =
0.03825 0.01068 -0.01284 -0.01462
O3 4 0.284163 0.653692 0.223099 11.00000 0.07815 0.06086 =
0.03616 0.01929 -0.02685 -0.03413
C18 1 0.295657 0.579878 0.289004 11.00000 0.05068 0.05909 =
0.03350 0.01519 -0.01476 -0.02554
HKLF 4
REM KR567P in C2/c
REM R1 = 0.0587 for 3634 Fo > 4sig(Fo) and 0.0695 for all 4537 data
REM 294 parameters refined using 32 restraints
END
WGHT 0.1007 3.3037
REM Highest difference peak 0.270, deepest hole -0.174, 1-sigma level 0.051
Q1 1 0.3540 0.9432 0.0097 11.00000 0.05 0.27
Q2 1 0.3026 0.9795 -0.1222 11.00000 0.05 0.26
Q3 1 0.2709 0.8188 -0.0445 11.00000 0.05 0.23
Q4 1 0.5000 1.1852 0.2500 10.50000 0.05 0.23
Q5 1 0.3081 0.8010 0.1021 11.00000 0.05 0.21
Q6 1 0.3577 0.4963 0.3073 11.00000 0.05 0.20
Q7 1 0.4292 1.0583 -0.1780 11.00000 0.05 0.20
Q8 1 0.3280 0.5576 0.2838 11.00000 0.05 0.20
Q9 1 0.3813 1.1033 -0.0619 11.00000 0.05 0.20
Q10 1 0.4987 0.3173 0.2191 11.00000 0.05 0.19
Q11 1 0.4108 1.1132 0.0989 11.00000 0.05 0.19
Q12 1 0.2210 0.5956 0.1571 11.00000 0.05 0.19
Q13 1 0.4986 1.1783 -0.0590 11.00000 0.05 0.19
Q14 1 0.4572 1.3763 -0.1023 11.00000 0.05 0.19
Q15 1 0.3261 0.6844 0.2094 11.00000 0.05 0.18
Q16 1 0.3394 1.0328 -0.0957 11.00000 0.05 0.18
Q17 1 0.3710 0.4823 0.2441 11.00000 0.05 0.18
Q18 1 0.5317 1.1822 0.1552 11.00000 0.05 0.18
Q19 1 0.2616 0.7546 0.0803 11.00000 0.05 0.18
Q20 1 0.2205 0.7587 0.3399 11.00000 0.05 0.18
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.203 0.250 127 31 ' '
2 0.000 0.297 0.750 127 31 ' '
3 0.000 0.703 0.250 127 31 ' '
4 0.500 0.797 0.750 127 31 ' '
_platon_squeeze_details
;
;
_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^)+(0.1018P)^2^+2.9978P] 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 4537
_refine_ls_number_parameters 294
_refine_ls_number_restraints 32
_refine_ls_R_factor_all 0.0695
_refine_ls_R_factor_gt 0.0587
_refine_ls_wR_factor_ref 0.1816
_refine_ls_wR_factor_gt 0.1729
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_restrained_S_all 1.072
_refine_ls_shift/su_max 0.000
_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
C1 C 0.24701(8) 0.62924(15) 0.15635(10) 0.0389(4) Uani 1 1 d . . .
C2 C 0.24836(7) 0.69298(13) 0.08199(10) 0.0323(4) Uani 1 1 d . . .
C3 C 0.28806(7) 0.78397(12) 0.07061(10) 0.0313(4) Uani 1 1 d . . .
C4 C 0.32235(8) 0.82481(14) 0.13782(11) 0.0387(4) Uani 1 1 d . . .
H4 H 0.3192 0.7941 0.1937 0.046 Uiso 1 1 calc R . .
C5 C 0.36119(9) 0.90915(15) 0.12594(11) 0.0433(4) Uani 1 1 d . . .
H5 H 0.3847 0.9332 0.1731 0.052 Uiso 1 1 calc R . .
C6 C 0.36592(8) 0.95764(14) 0.04729(11) 0.0376(4) Uani 1 1 d . . .
C7 C 0.32891(7) 0.92415(13) -0.02154(10) 0.0329(4) Uani 1 1 d . . .
C8 C 0.28994(7) 0.83665(13) -0.01180(10) 0.0313(4) Uani 1 1 d . . .
C9 C 0.29082(8) 0.95822(15) -0.16463(11) 0.0402(4) Uani 1 1 d . . .
H9 H 0.2903 0.9996 -0.2161 0.048 Uiso 1 1 calc R . .
C10 C 0.32867(8) 0.98404(14) -0.09820(10) 0.0349(4) Uani 1 1 d . . .
C11 C 0.36681(8) 1.07912(14) -0.10828(11) 0.0358(4) Uani 1 1 d . A .
C12 C 0.40783(9) 1.04591(15) 0.03607(12) 0.0459(5) Uani 1 1 d . A .
C13 C 0.44789(8) 1.19354(14) -0.05036(12) 0.0397(4) Uani 0.875(4) 1 d PD A 1
H13 H 0.4759 1.1876 -0.0005 0.048 Uiso 0.875(4) 1 calc PR A 1
C14 C 0.41635(10) 1.29740(16) -0.03777(17) 0.0419(5) Uani 0.875(4) 1 d PD A 1
H14A H 0.3956 1.2960 0.0179 0.050 Uiso 0.875(4) 1 calc PR A 1
H14B H 0.3869 1.3070 -0.0845 0.050 Uiso 0.875(4) 1 calc PR A 1
C15 C 0.45911(12) 1.39060(19) -0.03831(19) 0.0464(7) Uani 0.875(4) 1 d PD A 1
H15A H 0.4372 1.4586 -0.0344 0.056 Uiso 0.875(4) 1 calc PR A 1
H15B H 0.4855 1.3856 0.0127 0.056 Uiso 0.875(4) 1 calc PR A 1
C16 C 0.49494(11) 1.39039(18) -0.11957(16) 0.0516(6) Uani 0.875(4) 1 d PD A 1
H16A H 0.5231 1.4504 -0.1176 0.062 Uiso 0.875(4) 1 calc PR A 1
H16B H 0.4689 1.4008 -0.1704 0.062 Uiso 0.875(4) 1 calc PR A 1
C17 C 0.52786(10) 1.28582(19) -0.12876(18) 0.0528(7) Uani 0.875(4) 1 d PD A 1
H17A H 0.5556 1.2775 -0.0797 0.063 Uiso 0.875(4) 1 calc PR A 1
H17B H 0.5506 1.2870 -0.1827 0.063 Uiso 0.875(4) 1 calc PR A 1
C19 C 0.48532(10) 1.19038(18) -0.13080(16) 0.0468(6) Uani 0.875(4) 1 d PD A 1
H19A H 0.4601 1.1943 -0.1831 0.056 Uiso 0.875(4) 1 calc PR A 1
H19B H 0.5076 1.1226 -0.1326 0.056 Uiso 0.875(4) 1 calc PR A 1
C13B C 0.44789(8) 1.19354(14) -0.05036(12) 0.0397(4) Uani 0.125(4) 1 d PD A 2
H13B H 0.4404 1.2173 -0.1112 0.048 Uiso 0.125(4) 1 calc PR A 2
C14B C 0.4262(10) 1.2863(15) 0.0003(18) 0.081(4) Uiso 0.125(4) 1 d PD A 2
H14C H 0.3850 1.3015 -0.0158 0.097 Uiso 0.125(4) 1 calc PR A 2
H14D H 0.4280 1.2696 0.0628 0.097 Uiso 0.125(4) 1 calc PR A 2
C15B C 0.4641(10) 1.3837(17) -0.019(3) 0.081(4) Uiso 0.125(4) 1 d PD A 2
H15C H 0.4569 1.4388 0.0259 0.097 Uiso 0.125(4) 1 calc PR A 2
H15D H 0.4522 1.4138 -0.0752 0.097 Uiso 0.125(4) 1 calc PR A 2
C16B C 0.5282(9) 1.3592(16) -0.0200(16) 0.081(4) Uiso 0.125(4) 1 d PD A 2
H16C H 0.5490 1.4223 -0.0429 0.097 Uiso 0.125(4) 1 calc PR A 2
H16D H 0.5421 1.3480 0.0401 0.097 Uiso 0.125(4) 1 calc PR A 2
C17B C 0.5450(9) 1.2640(15) -0.0722(16) 0.081(4) Uiso 0.125(4) 1 d PD A 2
H17C H 0.5869 1.2483 -0.0614 0.097 Uiso 0.125(4) 1 calc PR A 2
H17D H 0.5402 1.2815 -0.1342 0.097 Uiso 0.125(4) 1 calc PR A 2
C19B C 0.5091(6) 1.1637(14) -0.0524(16) 0.081(4) Uiso 0.125(4) 1 d PD A 2
H19C H 0.5154 1.1089 -0.0974 0.097 Uiso 0.125(4) 1 calc PR A 2
H19D H 0.5214 1.1335 0.0041 0.097 Uiso 0.125(4) 1 calc PR A 2
C20 C 0.27233(9) 0.60294(18) 0.36979(12) 0.0509(5) Uani 1 1 d . . .
C21 C 0.29027(10) 0.5359(2) 0.43766(12) 0.0563(6) Uani 1 1 d . . .
H21 H 0.2762 0.5486 0.4942 0.068 Uiso 1 1 calc R . .
C22 C 0.32777(10) 0.4523(2) 0.42405(14) 0.0628(7) Uani 1 1 d . . .
H22 H 0.3394 0.4085 0.4713 0.075 Uiso 1 1 calc R . .
C23 C 0.34882(10) 0.4309(2) 0.34292(15) 0.0619(6) Uani 1 1 d . . .
H23 H 0.3740 0.3716 0.3344 0.074 Uiso 1 1 calc R . .
C24 C 0.33339(9) 0.4959(2) 0.27334(13) 0.0550(6) Uani 1 1 d . . .
C25 C 0.23178(12) 0.6946(2) 0.38184(16) 0.0678(7) Uani 1 1 d . . .
H25A H 0.2527 0.7617 0.3717 0.102 Uiso 1 1 calc R . .
H25B H 0.2170 0.6939 0.4409 0.102 Uiso 1 1 calc R . .
H25C H 0.1990 0.6886 0.3408 0.102 Uiso 1 1 calc R . .
C26 C 0.35717(12) 0.4754(3) 0.18417(16) 0.0743(8) Uani 1 1 d . . .
H26A H 0.3265 0.4440 0.1475 0.111 Uiso 1 1 calc R . .
H26B H 0.3903 0.4260 0.1884 0.111 Uiso 1 1 calc R . .
H26C H 0.3701 0.5429 0.1589 0.111 Uiso 1 1 calc R . .
N1 N 0.40745(6) 1.10015(11) -0.04248(9) 0.0369(4) Uani 1 1 d . . .
O1 O 0.44195(9) 1.07075(15) 0.09329(11) 0.0824(7) Uani 1 1 d . . .
O2 O 0.36245(6) 1.13727(11) -0.17077(8) 0.0475(4) Uani 1 1 d . . .
O3 O 0.28416(7) 0.65369(12) 0.22310(9) 0.0586(5) Uani 1 1 d . . .
C18 C 0.29566(9) 0.57988(17) 0.28900(12) 0.0479(5) Uani 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
C1 0.0468(10) 0.0431(10) 0.0265(8) 0.0013(7) -0.0089(7) -0.0095(8)
C2 0.0387(9) 0.0320(8) 0.0261(8) -0.0014(6) -0.0032(6) -0.0007(7)
C3 0.0406(9) 0.0273(8) 0.0258(8) -0.0020(6) -0.0040(6) 0.0007(7)
C4 0.0524(10) 0.0375(9) 0.0261(8) 0.0037(7) -0.0083(7) -0.0050(8)
C5 0.0583(11) 0.0396(10) 0.0315(9) 0.0010(7) -0.0165(8) -0.0105(8)
C6 0.0468(10) 0.0334(9) 0.0322(8) 0.0022(7) -0.0090(7) -0.0049(7)
C7 0.0424(9) 0.0296(8) 0.0267(8) -0.0022(6) -0.0042(6) -0.0006(7)
C8 0.0401(9) 0.0285(8) 0.0253(8) -0.0031(6) -0.0032(6) 0.0018(6)
C9 0.0502(10) 0.0425(10) 0.0277(8) 0.0073(7) -0.0067(7) -0.0099(8)
C10 0.0410(9) 0.0333(9) 0.0302(8) 0.0011(7) -0.0030(7) -0.0035(7)
C11 0.0404(9) 0.0357(9) 0.0311(8) 0.0006(7) -0.0030(7) -0.0023(7)
C12 0.0596(12) 0.0401(10) 0.0376(9) 0.0054(8) -0.0169(8) -0.0113(9)
C13 0.0426(9) 0.0357(9) 0.0404(9) 0.0029(7) -0.0065(7) -0.0073(7)
C14 0.0405(11) 0.0354(11) 0.0499(12) -0.0039(9) 0.0005(9) -0.0047(9)
C15 0.0470(12) 0.0313(11) 0.0607(19) -0.0025(10) -0.0052(11) -0.0052(9)
C16 0.0561(14) 0.0385(12) 0.0600(14) 0.0051(10) -0.0020(11) -0.0129(10)
C17 0.0412(12) 0.0518(14) 0.0656(16) -0.0014(11) 0.0069(11) -0.0091(10)
C19 0.0412(11) 0.0417(12) 0.0576(14) -0.0048(10) 0.0060(10) -0.0031(9)
C13B 0.0426(9) 0.0357(9) 0.0404(9) 0.0029(7) -0.0065(7) -0.0073(7)
C20 0.0537(11) 0.0621(13) 0.0367(10) 0.0053(9) -0.0127(8) -0.0269(10)
C21 0.0610(13) 0.0752(15) 0.0324(9) 0.0095(9) -0.0084(9) -0.0308(12)
C22 0.0599(13) 0.0792(16) 0.0490(12) 0.0293(11) -0.0176(10) -0.0242(12)
C23 0.0528(12) 0.0714(15) 0.0611(14) 0.0178(11) -0.0109(10) -0.0134(11)
C24 0.0495(11) 0.0695(14) 0.0459(11) 0.0144(10) -0.0084(9) -0.0198(11)
C25 0.0746(16) 0.0718(16) 0.0566(13) -0.0045(12) -0.0111(12) -0.0186(13)
C26 0.0650(15) 0.101(2) 0.0568(14) 0.0098(14) 0.0071(11) -0.0147(14)
N1 0.0434(8) 0.0328(7) 0.0344(7) 0.0023(6) -0.0059(6) -0.0063(6)
O1 0.1136(15) 0.0738(11) 0.0586(10) 0.0290(8) -0.0475(10) -0.0564(11)
O2 0.0576(8) 0.0462(8) 0.0382(7) 0.0107(6) -0.0128(6) -0.0146(6)
O3 0.0781(10) 0.0609(9) 0.0362(7) 0.0193(6) -0.0269(7) -0.0341(8)
C18 0.0507(11) 0.0591(12) 0.0335(9) 0.0152(8) -0.0148(8) -0.0255(10)
_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
C1 O3 1.365(2) . ?
C1 C2 1.402(2) . ?
C1 C9 1.403(2) 7_565 ?
C2 C8 1.436(2) 7_565 ?
C2 C3 1.469(2) . ?
C3 C4 1.393(2) . ?
C3 C8 1.438(2) . ?
C4 C5 1.394(3) . ?
C5 C6 1.366(2) . ?
C6 C7 1.417(2) . ?
C6 C12 1.475(3) . ?
C7 C10 1.404(2) . ?
C7 C8 1.422(2) . ?
C8 C2 1.436(2) 7_565 ?
C9 C10 1.375(2) . ?
C9 C1 1.403(2) 7_565 ?
C10 C11 1.486(2) . ?
C11 O2 1.214(2) . ?
C11 N1 1.396(2) . ?
C12 O1 1.214(2) . ?
C12 N1 1.393(2) . ?
C13 N1 1.497(2) . ?
C13 C14 1.501(3) . ?
C13 C19 1.521(3) . ?
C14 C15 1.523(3) . ?
C15 C16 1.511(4) . ?
C16 C17 1.518(3) . ?
C17 C19 1.542(3) . ?
C14B C15B 1.527(16) . ?
C15B C16B 1.501(16) . ?
C16B C17B 1.492(15) . ?
C17B C19B 1.534(15) . ?
C20 C18 1.397(3) . ?
C20 C21 1.403(3) . ?
C20 C25 1.489(4) . ?
C21 C22 1.371(4) . ?
C22 C23 1.378(4) . ?
C23 C24 1.392(3) . ?
C24 C18 1.385(3) . ?
C24 C26 1.513(3) . ?
O3 C18 1.399(2) . ?
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
O3 C1 C2 118.34(15) . . ?
O3 C1 C9 119.02(15) . 7_565 ?
C2 C1 C9 122.64(15) . 7_565 ?
C1 C2 C8 117.08(15) . 7_565 ?
C1 C2 C3 124.05(15) . . ?
C8 C2 C3 118.81(14) 7_565 . ?
C4 C3 C8 118.17(15) . . ?
C4 C3 C2 122.58(14) . . ?
C8 C3 C2 119.18(14) . . ?
C3 C4 C5 122.25(15) . . ?
C6 C5 C4 120.81(16) . . ?
C5 C6 C7 119.07(16) . . ?
C5 C6 C12 119.79(15) . . ?
C7 C6 C12 121.11(15) . . ?
C10 C7 C6 118.30(15) . . ?
C10 C7 C8 120.35(15) . . ?
C6 C7 C8 121.21(15) . . ?
C7 C8 C2 119.75(14) . 7_565 ?
C7 C8 C3 118.25(14) . . ?
C2 C8 C3 121.91(15) 7_565 . ?
C10 C9 C1 119.92(15) . 7_565 ?
C9 C10 C7 120.19(16) . . ?
C9 C10 C11 118.37(15) . . ?
C7 C10 C11 121.38(15) . . ?
O2 C11 N1 121.07(15) . . ?
O2 C11 C10 121.45(15) . . ?
N1 C11 C10 117.48(14) . . ?
O1 C12 N1 120.62(17) . . ?
O1 C12 C6 121.27(17) . . ?
N1 C12 C6 118.11(15) . . ?
N1 C13 C14 111.54(15) . . ?
N1 C13 C19 113.67(15) . . ?
C14 C13 C19 113.93(17) . . ?
C13 C14 C15 110.66(18) . . ?
C16 C15 C14 111.0(2) . . ?
C15 C16 C17 110.78(19) . . ?
C16 C17 C19 110.88(18) . . ?
C13 C19 C17 108.98(18) . . ?
C14B C15B C16B 113.4(17) . . ?
C17B C16B C15B 115.4(18) . . ?
C16B C17B C19B 113.8(15) . . ?
C18 C20 C21 115.8(2) . . ?
C18 C20 C25 121.16(19) . . ?
C21 C20 C25 123.0(2) . . ?
C22 C21 C20 121.3(2) . . ?
C21 C22 C23 121.0(2) . . ?
C22 C23 C24 120.3(3) . . ?
C18 C24 C23 117.4(2) . . ?
C18 C24 C26 121.4(2) . . ?
C23 C24 C26 121.1(2) . . ?
C12 N1 C11 122.83(14) . . ?
C12 N1 C13 117.06(14) . . ?
C11 N1 C13 119.65(14) . . ?
C1 O3 C18 120.92(14) . . ?
C24 C18 C20 124.09(18) . . ?
C24 C18 O3 119.08(19) . . ?
C20 C18 O3 116.5(2) . . ?
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
O3 C1 C2 C8 178.13(16) . . . 7_565 ?
C9 C1 C2 C8 -1.8(3) 7_565 . . 7_565 ?
O3 C1 C2 C3 1.0(3) . . . . ?
C9 C1 C2 C3 -178.94(17) 7_565 . . . ?
C1 C2 C3 C4 -9.5(3) . . . . ?
C8 C2 C3 C4 173.40(16) 7_565 . . . ?
C1 C2 C3 C8 173.45(16) . . . . ?
C8 C2 C3 C8 -3.6(3) 7_565 . . . ?
C8 C3 C4 C5 -4.9(3) . . . . ?
C2 C3 C4 C5 178.07(17) . . . . ?
C3 C4 C5 C6 1.9(3) . . . . ?
C4 C5 C6 C7 2.7(3) . . . . ?
C4 C5 C6 C12 -179.29(18) . . . . ?
C5 C6 C7 C10 171.47(17) . . . . ?
C12 C6 C7 C10 -6.5(3) . . . . ?
C5 C6 C7 C8 -4.3(3) . . . . ?
C12 C6 C7 C8 177.76(16) . . . . ?
C10 C7 C8 C2 2.3(2) . . . 7_565 ?
C6 C7 C8 C2 177.95(16) . . . 7_565 ?
C10 C7 C8 C3 -174.38(15) . . . . ?
C6 C7 C8 C3 1.3(2) . . . . ?
C4 C3 C8 C7 3.2(2) . . . . ?
C2 C3 C8 C7 -179.65(14) . . . . ?
C4 C3 C8 C2 -173.42(16) . . . 7_565 ?
C2 C3 C8 C2 3.7(3) . . . 7_565 ?
C1 C9 C10 C7 -1.0(3) 7_565 . . . ?
C1 C9 C10 C11 -178.20(16) 7_565 . . . ?
C6 C7 C10 C9 -176.01(17) . . . . ?
C8 C7 C10 C9 -0.2(3) . . . . ?
C6 C7 C10 C11 1.1(3) . . . . ?
C8 C7 C10 C11 176.86(15) . . . . ?
C9 C10 C11 O2 4.8(3) . . . . ?
C7 C10 C11 O2 -172.38(18) . . . . ?
C9 C10 C11 N1 -176.12(16) . . . . ?
C7 C10 C11 N1 6.7(2) . . . . ?
C5 C6 C12 O1 6.4(3) . . . . ?
C7 C6 C12 O1 -175.7(2) . . . . ?
C5 C6 C12 N1 -173.90(18) . . . . ?
C7 C6 C12 N1 4.1(3) . . . . ?
N1 C13 C14 C15 175.12(18) . . . . ?
C19 C13 C14 C15 -54.5(3) . . . . ?
C13 C14 C15 C16 54.8(3) . . . . ?
C14 C15 C16 C17 -57.6(3) . . . . ?
C15 C16 C17 C19 58.4(3) . . . . ?
N1 C13 C19 C17 -176.17(17) . . . . ?
C14 C13 C19 C17 54.5(2) . . . . ?
C16 C17 C19 C13 -55.5(3) . . . . ?
C14B C15B C16B C17B 48(4) . . . . ?
C15B C16B C17B C19B -50(3) . . . . ?
C18 C20 C21 C22 -0.9(3) . . . . ?
C25 C20 C21 C22 -179.9(2) . . . . ?
C20 C21 C22 C23 -0.5(3) . . . . ?
C21 C22 C23 C24 1.6(3) . . . . ?
C22 C23 C24 C18 -1.3(3) . . . . ?
C22 C23 C24 C26 178.5(2) . . . . ?
O1 C12 N1 C11 -176.0(2) . . . . ?
C6 C12 N1 C11 4.3(3) . . . . ?
O1 C12 N1 C13 -3.8(3) . . . . ?
C6 C12 N1 C13 176.43(16) . . . . ?
O2 C11 N1 C12 169.66(18) . . . . ?
C10 C11 N1 C12 -9.4(3) . . . . ?
O2 C11 N1 C13 -2.3(3) . . . . ?
C10 C11 N1 C13 178.62(15) . . . . ?
C14 C13 N1 C12 -99.7(2) . . . . ?
C19 C13 N1 C12 129.82(19) . . . . ?
C14 C13 N1 C11 72.7(2) . . . . ?
C19 C13 N1 C11 -57.8(2) . . . . ?
C2 C1 O3 C18 -163.89(19) . . . . ?
C9 C1 O3 C18 16.1(3) 7_565 . . . ?
C23 C24 C18 C20 -0.1(3) . . . . ?
C26 C24 C18 C20 -179.9(2) . . . . ?
C23 C24 C18 O3 173.09(17) . . . . ?
C26 C24 C18 O3 -6.7(3) . . . . ?
C21 C20 C18 C24 1.2(3) . . . . ?
C25 C20 C18 C24 -179.82(19) . . . . ?
C21 C20 C18 O3 -172.16(16) . . . . ?
C25 C20 C18 O3 6.8(3) . . . . ?
C1 O3 C18 C24 77.0(2) . . . . ?
C1 O3 C18 C20 -109.3(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 26.42
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max 0.270
_refine_diff_density_min -0.174
_refine_diff_density_rms 0.051
_database_code_depnum_ccdc_archive 'CCDC 952111'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_kr673t-
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C60 H62 N2 O6'
_chemical_formula_sum 'C60 H62 N2 O6'
_chemical_formula_weight 907.12
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M Pna21
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a 22.956(2)
_cell_length_b 9.4115(19)
_cell_length_c 22.7754(8)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 4920.7(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 7874
_cell_measurement_theta_min 2.34
_cell_measurement_theta_max 26.44
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.224
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1936
_exptl_absorpt_coefficient_mu 0.078
_exptl_transmission_factor_min .6585
_exptl_transmission_factor_max .7454
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9784
_exptl_absorpt_correction_T_max 0.9922
_exptl_absorpt_process_details Bruker-SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source rotating_anode
_diffrn_radiation_monochromator MONTEL_multi_layer_optics
_diffrn_measurement_device_type Bruker-Kappa_CCD_Apex2
_diffrn_measurement_method omega_and_phi_scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 63885
_diffrn_reflns_av_R_equivalents 0.0407
_diffrn_reflns_av_sigmaI/netI 0.0317
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 1.77
_diffrn_reflns_theta_max 26.37
_reflns_number_total 10041
_reflns_number_gt 8289
_reflns_threshold_expression >2sigma(I)
_computing_data_collection Bruker-SAINT
_computing_cell_refinement Bruker-SAINT
_computing_data_reduction Bruker-SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics CCDC-Mercury
_computing_publication_material Bruker-SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
TITL KR673t in P n a 21
CELL 0.71073 22.9565 9.4115 22.7754 90 90 90
ZERR 4 0.0021 0.0019 0.0008 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,0.5+Z
SFAC C H N O
UNIT 240 248 8 24
DELU .005 C91 C93
DELU .005 C91B C93B
SADI .01 C94 C96 C94B C96B
SADI .01 C91 C93 C91B C93B
SADI N2 C10 N2B C10 N2 C24 N2B C24
FLAT C79 C80 C81 C82 C83 C84
FLAT C73 C74 C75 C76 C77 C78
DELU 0.005 0.005 C94 C95
DELU 0.005 0.005 C94 C96
DELU 0.005 0.005 C94B C95B
DELU 0.005 0.005 C94B C96B
SIMU 0.01 0.02 1.7 C71 C71B
SIMU 0.005 0.01 1.7 C95 C95B
SIMU .005 .01 1.7 C96 C96b
ISOR C96
ISOR 0.005 0.01 N2 N2B
ISOR 0.005 0.01 N1
ISOR 0.005 0.01 C67 > C72B
ISOR 0.005 0.01 C92 > C95B
EADP C72 C72B
EADP C88 C88B
EADP C67 C67B
EADP C91 C91B
EADP C94 C94B
EADP N2 N2B
EXYZ C88 C88B
EXYZ C91 C91B
EXYZ C94 C94B
EXYZ N2 N2B
L.S. 8
PLAN 20
SIZE 0.1 0.17 0.28
TEMP -173
MORE -1
CONF
BOND
LIST 4
fmap -2
acta
SHEL 999 0.8
REM C:\daten\xray_daten\oc\KR673\work\kr673_l\KR673r.hkl
WGHT 0.086300 0.477500
FVAR 0.33487 0.72196 0.37186 0.18571 0.53069
PART 1
N1 3 0.297867 0.018306 0.557708 11.00000 0.03180 0.03985 =
0.01450 -0.00101 0.00184 -0.00237
C1 1 0.345799 0.030730 0.595298 11.00000 0.02760 0.04272 =
0.02226 -0.00519 0.00160 -0.00458
O1 4 0.395089 0.044086 0.576498 11.00000 0.03256 0.07346 =
0.02112 -0.00595 0.00513 -0.01059
C2 1 0.334004 0.027482 0.659451 11.00000 0.02712 0.03541 =
0.02074 -0.00159 0.00401 -0.00430
C3 1 0.379813 0.035755 0.698150 11.00000 0.02379 0.05997 =
0.02120 -0.00867 0.00424 -0.00724
AFIX 43
H3 2 0.418546 0.041237 0.683641 11.00000 -1.20000
AFIX 0
C4 1 0.369950 0.036161 0.758095 11.00000 0.02725 0.04966 =
0.02109 -0.00682 -0.00188 -0.00662
AFIX 43
H4 2 0.402490 0.041416 0.783774 11.00000 -1.20000
AFIX 0
C5 1 0.314311 0.029187 0.782384 11.00000 0.01961 0.03454 =
0.01812 -0.00162 -0.00138 -0.00024
C6 1 0.302975 0.039218 0.845800 11.00000 0.02505 0.03005 =
0.01680 -0.00007 -0.00294 0.00318
C7 1 0.344927 0.075457 0.887793 11.00000 0.02555 0.03710 =
0.01753 0.00157 -0.00115 0.00059
O2 4 0.400720 0.103983 0.869049 11.00000 0.02588 0.05610 =
0.02031 -0.00252 -0.00623 -0.00607
C8 1 0.332267 0.081838 0.948335 11.00000 0.03871 0.04008 =
0.02069 -0.00185 -0.00719 -0.00220
AFIX 43
H8 2 0.361381 0.110588 0.975494 11.00000 -1.20000
AFIX 0
C9 1 0.277991 0.046474 0.967575 11.00000 0.03778 0.03479 =
0.01671 0.00159 0.00048 0.00274
C10 1 0.266921 0.048363 1.032175 11.00000 0.06126 0.03746 =
0.01695 0.00015 -0.00279 0.00061
O3 4 0.304342 0.083383 1.066318 11.00000 0.07322 0.07283 =
0.01888 -0.00116 -0.00320 -0.01940
C11 1 0.233788 0.012904 0.928148 11.00000 0.03493 0.02918 =
0.01816 0.00198 0.00508 0.00564
C12 1 0.244798 0.012874 0.866190 11.00000 0.02641 0.02997 =
0.01707 0.00155 0.00109 0.00411
C13 1 0.265710 0.013356 0.742957 11.00000 0.02507 0.02760 =
0.01708 -0.00101 0.00062 0.00116
C14 1 0.276901 0.014965 0.681275 11.00000 0.02205 0.03400 =
0.01796 -0.00236 0.00102 -0.00057
C15 1 0.241111 -0.006553 0.577078 11.00000 0.03187 0.04137 =
0.01801 -0.00077 -0.00617 -0.00021
O6 4 0.202025 -0.035269 0.543279 11.00000 0.03536 0.06667 =
0.02101 -0.00189 -0.00308 -0.00660
C16 1 0.230483 0.002394 0.641613 11.00000 0.02940 0.03759 =
0.01652 -0.00141 -0.00166 0.00045
C17 1 0.174486 -0.004556 0.661347 11.00000 0.02595 0.04435 =
0.02112 -0.00326 -0.00760 0.00312
AFIX 43
H17 2 0.143248 -0.010125 0.634085 11.00000 -1.20000
AFIX 0
C18 1 0.162951 -0.003508 0.721526 11.00000 0.02310 0.03724 =
0.02390 0.00033 0.00097 0.00110
O5 4 0.105556 -0.009846 0.739776 11.00000 0.02039 0.06094 =
0.02508 -0.00099 -0.00041 0.00430
C19 1 0.207338 -0.002846 0.763787 11.00000 0.02513 0.02868 =
0.01932 -0.00118 -0.00020 0.00062
C20 1 0.197277 -0.013150 0.827468 11.00000 0.02498 0.03196 =
0.01926 0.00002 0.00131 0.00175
C21 1 0.142979 -0.047986 0.850773 11.00000 0.02657 0.04377 =
0.02602 0.00206 0.00256 0.00240
AFIX 43
H21 2 0.111647 -0.068688 0.824901 11.00000 -1.20000
AFIX 0
C22 1 0.133579 -0.053147 0.911665 11.00000 0.02722 0.04895 =
0.02692 0.00478 0.00778 0.00278
AFIX 43
H22 2 0.096483 -0.079710 0.926539 11.00000 -1.20000
AFIX 0
C23 1 0.177552 -0.020139 0.949451 11.00000 0.03807 0.03861 =
0.02263 0.00436 0.01087 0.00539
C24 1 0.164950 -0.020817 1.013158 11.00000 0.04535 0.04770 =
0.02408 0.00680 0.00745 0.00987
O4 4 0.116465 -0.047403 1.032079 11.00000 0.04702 0.07700 =
0.03224 0.01616 0.02315 0.01227
SAME 0.02 0.04 C67 > C72
PART 0
C61 1 0.311116 0.014599 0.493459 11.00000 0.03432 0.04322 =
0.01575 -0.00047 0.00401 -0.00424
AFIX 13
H61 2 0.352121 0.048699 0.488876 11.00000 -1.20000
AFIX 0
C62 1 0.273000 0.114660 0.457542 11.00000 0.05261 0.04052 =
0.02329 0.00155 0.00210 -0.00008
AFIX 23
H62A 2 0.277249 0.213012 0.472352 11.00000 -1.20000
H62B 2 0.231613 0.086654 0.461444 11.00000 -1.20000
AFIX 0
C63 1 0.291317 0.108035 0.392791 11.00000 0.05303 0.05406 =
0.02437 0.01053 0.00024 -0.00003
AFIX 23
H63A 2 0.264595 0.167547 0.369143 11.00000 -1.20000
H63B 2 0.331104 0.147336 0.388611 11.00000 -1.20000
AFIX 0
C64 1 0.290336 -0.041855 0.369622 11.00000 0.04821 0.06443 =
0.01956 -0.00240 0.00160 -0.00243
AFIX 23
H64A 2 0.304305 -0.042292 0.328498 11.00000 -1.20000
H64B 2 0.249779 -0.077607 0.369854 11.00000 -1.20000
AFIX 0
C65 1 0.328213 -0.139650 0.406097 11.00000 0.04980 0.04700 =
0.01855 -0.00575 0.00652 -0.00552
AFIX 23
H65A 2 0.369422 -0.109732 0.402735 11.00000 -1.20000
H65B 2 0.324997 -0.237909 0.390921 11.00000 -1.20000
AFIX 0
C66 1 0.309701 -0.136399 0.470799 11.00000 0.04238 0.03913 =
0.02130 0.00124 0.00289 -0.00053
AFIX 23
H66A 2 0.269842 -0.175379 0.474786 11.00000 -1.20000
H66B 2 0.336409 -0.196253 0.494315 11.00000 -1.20000
AFIX 0
PART 1
N2 3 0.210824 0.010109 1.051241 21.00000 0.05337 0.04407 =
0.01844 0.00388 0.01246 0.00659
SAME 0.02 0.04 C67B > C72B
C67 1 0.193498 0.004781 1.114582 21.00000 0.01998 0.04152 =
0.01599 0.00127 0.00177 -0.00801
AFIX 13
H67 2 0.153141 -0.034951 1.116479 21.00000 -1.20000
AFIX 0
C68 1 0.232819 -0.094749 1.148132 21.00000 0.03859 0.03713 =
0.01932 0.00479 0.00303 0.00770
AFIX 23
H68A 2 0.273740 -0.062523 1.144830 21.00000 -1.20000
H68B 2 0.230075 -0.191626 1.131422 21.00000 -1.20000
AFIX 0
C69 1 0.214301 -0.097033 1.213154 21.00000 0.03087 0.04522 =
0.02397 0.00555 0.00011 -0.00216
AFIX 23
H69A 2 0.175776 -0.143592 1.216534 21.00000 -1.20000
H69B 2 0.242667 -0.154201 1.235825 21.00000 -1.20000
AFIX 0
C70 1 0.210804 0.049247 1.239212 21.00000 0.03329 0.04784 =
0.01806 0.00144 -0.00005 -0.00336
AFIX 23
H70A 2 0.250347 0.091071 1.240682 21.00000 -1.20000
H70B 2 0.196080 0.042368 1.279969 21.00000 -1.20000
AFIX 0
C71 1 0.170935 0.146718 1.203893 21.00000 0.03223 0.03539 =
0.02287 -0.00057 0.00527 0.00015
AFIX 23
H71A 2 0.171331 0.243202 1.221205 21.00000 -1.20000
H71B 2 0.130497 0.110357 1.205432 21.00000 -1.20000
AFIX 0
C72 1 0.191421 0.153786 1.139845 21.00000 0.04046 0.03908 =
0.02059 0.00112 0.00106 0.00044
AFIX 23
H72A 2 0.164264 0.213146 1.116639 21.00000 -1.20000
H72B 2 0.230590 0.197539 1.137898 21.00000 -1.20000
AFIX 0
PART 0
PART 2
N2B 3 0.210824 0.010109 1.051241 -21.00000 0.05337 0.04407 =
0.01844 0.00388 0.01246 0.00659
C67B 1 0.218038 0.022992 1.119769 -21.00000 0.01998 0.04152 =
0.01599 0.00127 0.00177 -0.00801
AFIX 13
H67B 2 0.259826 0.038771 1.130314 -21.00000 -1.20000
AFIX 0
C68B 1 0.196959 -0.118391 1.143604 -21.00000 0.03596 0.03941 =
0.03353 -0.00329 0.00058 0.00641
AFIX 23
H68C 2 0.222019 -0.196060 1.128727 -21.00000 -1.20000
H68D 2 0.156554 -0.136382 1.130354 -21.00000 -1.20000
AFIX 0
C69B 1 0.199200 -0.114532 1.211086 -21.00000 0.02703 0.02465 =
0.01795 0.00113 0.00102 -0.00340
AFIX 23
H69C 2 0.183191 -0.204133 1.227153 -21.00000 -1.20000
H69D 2 0.240133 -0.105676 1.224270 -21.00000 -1.20000
AFIX 0
C70B 1 0.163822 0.011112 1.233885 -21.00000 0.04400 0.05473 =
0.02834 0.00038 -0.00014 -0.00178
AFIX 23
H70C 2 0.166125 0.014280 1.277271 -21.00000 -1.20000
H70D 2 0.122435 -0.000959 1.222736 -21.00000 -1.20000
AFIX 0
C71B 1 0.187018 0.150621 1.208349 -21.00000 0.04042 0.04683 =
0.03244 -0.00148 0.00720 0.00151
AFIX 23
H71C 2 0.228496 0.162859 1.219122 -21.00000 -1.20000
H71D 2 0.164774 0.231737 1.224572 -21.00000 -1.20000
AFIX 0
C72B 1 0.180666 0.146952 1.140819 -21.00000 0.04046 0.03908 =
0.02059 0.00112 0.00106 0.00044
AFIX 23
H72C 2 0.139437 0.132379 1.129586 -21.00000 -1.20000
H72D 2 0.194439 0.237233 1.123357 -21.00000 -1.20000
AFIX 0
PART 0
C73 1 0.063146 0.047999 0.701737 11.00000 0.01901 0.05646 =
0.02441 -0.00179 0.00040 0.00277
C74 1 0.056236 0.192822 0.700193 11.00000 0.02318 0.05488 =
0.03288 -0.00727 -0.00129 0.00305
C75 1 0.013110 0.246877 0.663029 11.00000 0.03032 0.04905 =
0.04542 -0.00274 -0.00220 0.00578
AFIX 43
H75 2 0.007588 0.346680 0.660200 11.00000 -1.20000
AFIX 0
C76 1 -0.021685 0.156161 0.630254 11.00000 0.02525 0.05739 =
0.03545 0.00464 -0.00515 0.00036
AFIX 43
H76 2 -0.051196 0.193870 0.605510 11.00000 -1.20000
AFIX 0
C77 1 -0.013447 0.011305 0.633583 11.00000 0.02555 0.05760 =
0.03541 -0.00028 -0.00817 -0.00275
AFIX 43
H77 2 -0.037730 -0.049656 0.611084 11.00000 -1.20000
AFIX 0
C78 1 0.029513 -0.047918 0.669042 11.00000 0.02502 0.05380 =
0.02967 -0.00106 -0.00099 -0.00176
C79 1 0.441787 0.163833 0.908459 11.00000 0.02819 0.05037 =
0.02046 -0.00480 -0.00514 -0.00694
C80 1 0.447278 0.311365 0.908556 11.00000 0.03464 0.05416 =
0.02475 -0.00257 0.00254 -0.00532
C81 1 0.491358 0.367369 0.943517 11.00000 0.04406 0.05042 =
0.03634 -0.00542 0.00046 -0.01033
AFIX 43
H81 2 0.496496 0.467445 0.945213 11.00000 -1.20000
AFIX 0
C82 1 0.527670 0.280950 0.975687 11.00000 0.03405 0.06106 =
0.03113 -0.00943 -0.00318 -0.00966
AFIX 43
H82 2 0.557992 0.321802 0.998508 11.00000 -1.20000
AFIX 0
C83 1 0.520324 0.134030 0.975061 11.00000 0.02936 0.06228 =
0.02569 -0.00176 -0.00725 -0.00006
AFIX 43
H83 2 0.545304 0.075529 0.997898 11.00000 -1.20000
AFIX 0
C84 1 0.476589 0.072297 0.941169 11.00000 0.03242 0.05188 =
0.02255 -0.00045 -0.00311 -0.00336
C85 1 0.092201 0.293468 0.738115 11.00000 0.03160 0.05247 =
0.04562 -0.01051 -0.01016 0.00552
AFIX 13
H85 2 0.125271 0.237657 0.754994 11.00000 -1.20000
AFIX 0
C86 1 0.056318 0.348822 0.788671 11.00000 0.05777 0.08400 =
0.04025 -0.01851 -0.00314 -0.00940
AFIX 137
H86A 2 0.078889 0.419709 0.810485 11.00000 -1.50000
H86B 2 0.046115 0.270003 0.814842 11.00000 -1.50000
H86C 2 0.020640 0.392713 0.773529 11.00000 -1.50000
AFIX 0
C87 1 0.117935 0.413583 0.702473 11.00000 0.05957 0.09571 =
0.05228 -0.01205 -0.00275 -0.03045
AFIX 137
H87A 2 0.141887 0.374360 0.670757 11.00000 -1.50000
H87B 2 0.142151 0.473316 0.727898 11.00000 -1.50000
H87C 2 0.086447 0.470930 0.685663 11.00000 -1.50000
AFIX 0
PART 1
C88 1 0.038646 -0.206821 0.673823 10.50000 0.04310 0.04943 =
0.05084 -0.00354 -0.01444 -0.00009
AFIX 13
H88 2 0.068782 -0.224396 0.704684 10.50000 -1.20000
AFIX 0
C89 1 -0.010127 -0.284233 0.688084 31.00000 0.04735 0.09550 =
0.10691 0.03063 0.01613 0.00575
AFIX 137
H89A 2 -0.024391 -0.254555 0.726742 31.00000 -1.50000
H89B 2 -0.000288 -0.385529 0.689087 31.00000 -1.50000
H89C 2 -0.040472 -0.267800 0.658590 31.00000 -1.50000
AFIX 0
C90 1 0.065766 -0.260832 0.609226 31.00000 0.09791 0.06745 =
0.05912 -0.01662 -0.00704 0.02501
AFIX 137
H90A 2 0.073807 -0.363016 0.610902 31.00000 -1.50000
H90B 2 0.101948 -0.209317 0.600961 31.00000 -1.50000
H90C 2 0.037398 -0.241736 0.578056 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C88B 1 0.038646 -0.206821 0.673823 10.50000 0.04310 0.04943 =
0.05084 -0.00354 -0.01444 -0.00009
AFIX 13
H88B 2 0.081168 -0.226597 0.678725 10.50000 -1.20000
AFIX 0
C89B 1 0.003956 -0.262087 0.731905 -31.00000 0.05291 0.05241 =
0.06092 0.01736 0.00726 -0.00054
AFIX 137
H89D 2 -0.037950 -0.246935 0.726605 -31.00000 -1.50000
H89E 2 0.017391 -0.208982 0.766351 -31.00000 -1.50000
H89F 2 0.011563 -0.363586 0.737695 -31.00000 -1.50000
AFIX 0
C90B 1 0.016305 -0.289033 0.622814 -31.00000 0.09510 0.04402 =
0.05821 -0.00830 -0.03465 0.00112
AFIX 137
H90D 2 -0.026373 -0.286632 0.622784 -31.00000 -1.50000
H90E 2 0.029603 -0.387732 0.625700 -31.00000 -1.50000
H90F 2 0.030962 -0.246912 0.586341 -31.00000 -1.50000
AFIX 0
SAME 0.02 0.04 C92B C91B C93B
SAME 0.02 0.04 C93 C91 C92
PART 0
PART 1
C92 1 0.488950 -0.177192 0.993192 41.00000 0.05906 0.05885 =
0.04127 0.00036 -0.00922 0.00151
AFIX 137
H92A 2 0.505258 -0.266921 0.978825 41.00000 -1.50000
H92B 2 0.455920 -0.197009 1.019192 41.00000 -1.50000
H92C 2 0.518911 -0.124899 1.014931 41.00000 -1.50000
AFIX 0
C91 1 0.468101 -0.087023 0.940637 41.00000 0.03926 0.05081 =
0.03993 0.00437 -0.01433 -0.00563
AFIX 13
H91 2 0.426610 -0.110179 0.931295 41.00000 -1.20000
AFIX 0
C93 1 0.508463 -0.146150 0.892142 41.00000 0.02591 0.03229 =
0.07564 0.00930 -0.00856 0.00834
AFIX 33
H93A 2 0.485036 -0.173990 0.858061 41.00000 -1.50000
H93B 2 0.529495 -0.229174 0.907144 41.00000 -1.50000
H93C 2 0.536455 -0.072783 0.880469 41.00000 -1.50000
AFIX 0
SAME 0.02 0.04 C93B C91B C92B
PART 0
PART 2
C92B 1 0.456583 -0.141179 1.003830 -41.00000 0.09737 0.06081 =
0.04844 0.01821 -0.02033 -0.02043
AFIX 137
H92D 2 0.450742 -0.244312 1.003098 -41.00000 -1.50000
H92E 2 0.421644 -0.095015 1.019558 -41.00000 -1.50000
H92F 2 0.490079 -0.118460 1.028799 -41.00000 -1.50000
AFIX 0
C91B 1 0.468101 -0.087023 0.940637 -41.00000 0.03926 0.05081 =
0.03993 0.00437 -0.01433 -0.00563
AFIX 13
H91B 2 0.432877 -0.108478 0.916374 -41.00000 -1.20000
AFIX 0
C93B 1 0.519681 -0.161505 0.912952 -41.00000 0.04603 0.05027 =
0.11132 -0.00254 -0.01793 0.01384
AFIX 137
H93D 2 0.525077 -0.126733 0.872760 -41.00000 -1.50000
H93E 2 0.512545 -0.264151 0.912170 -41.00000 -1.50000
H93F 2 0.554817 -0.141857 0.936003 -41.00000 -1.50000
AFIX 0
SAME 0.02 0.04 C96B C94B C95B
SAME 0.02 0.04 C96 C94 C95
PART 1
C95 1 0.387100 0.542551 0.900525 51.00000 0.05448 0.07378 =
0.05126 -0.01148 -0.00982 0.00989
AFIX 33
H95A 2 0.419176 0.587700 0.921930 51.00000 -1.50000
H95B 2 0.355583 0.519574 0.927950 51.00000 -1.50000
H95C 2 0.372546 0.607770 0.870360 51.00000 -1.50000
AFIX 0
C94 1 0.408968 0.406011 0.871363 51.00000 0.04734 0.05004 =
0.03519 0.00442 0.00425 0.00057
AFIX 13
H94 2 0.373150 0.348673 0.863423 51.00000 -1.20000
AFIX 0
C96 1 0.434744 0.438774 0.810541 51.00000 0.04690 0.07872 =
0.02478 0.00756 -0.00672 0.01791
AFIX 137
H96A 2 0.471956 0.488533 0.815221 51.00000 -1.50000
H96B 2 0.407631 0.498927 0.788480 51.00000 -1.50000
H96C 2 0.441076 0.349743 0.789158 51.00000 -1.50000
AFIX 0
PART 2
C96B 1 0.452054 0.482859 0.827728 -51.00000 0.08116 0.08847 =
0.03251 0.01457 0.01554 0.02027
AFIX 137
H96D 2 0.430241 0.550006 0.803270 -51.00000 -1.50000
H96E 2 0.470959 0.411994 0.802611 -51.00000 -1.50000
H96F 2 0.481725 0.534314 0.850199 -51.00000 -1.50000
AFIX 0
C94B 1 0.408968 0.406011 0.871363 -51.00000 0.04734 0.05004 =
0.03519 0.00442 0.00425 0.00057
AFIX 13
H94B 2 0.378148 0.351082 0.850207 -51.00000 -1.20000
AFIX 0
C95B 1 0.383452 0.520710 0.910348 -51.00000 0.03486 0.06782 =
0.05135 -0.00092 0.00178 0.00924
AFIX 137
H95D 2 0.367200 0.477255 0.945854 -51.00000 -1.50000
H95E 2 0.352559 0.570876 0.889084 -51.00000 -1.50000
H95F 2 0.414097 0.588169 0.921315 -51.00000 -1.50000
HKLF 4
REM KR673p in P n a 21
REM R1 = 0.0537 for 8289 Fo > 4sig(Fo) and 0.0661 for all 10041 data
REM 725 parameters refined using 263 restraints
END
WGHT 0.0863 0.4776
REM Highest difference peak 0.350, deepest hole -0.312, 1-sigma level 0.053
Q1 1 0.2064 0.0732 0.5404 11.00000 0.05 0.35
Q2 1 0.1049 0.1011 0.7384 11.00000 0.05 0.34
Q3 1 0.3899 -0.0110 0.8679 11.00000 0.05 0.33
Q4 1 0.2674 0.0671 1.0701 11.00000 0.05 -0.31
Q5 1 0.2988 -0.0291 1.0610 11.00000 0.05 0.29
Q6 1 0.3179 -0.0108 0.5802 11.00000 0.05 0.29
Q7 1 0.4669 0.0014 0.9470 11.00000 0.05 0.29
Q8 1 0.1030 -0.1290 0.7420 11.00000 0.05 0.29
Q9 1 0.2888 -0.0080 0.7641 11.00000 0.05 0.28
Q10 1 0.1393 0.0111 1.0426 11.00000 0.05 0.25
Q11 1 0.4013 -0.0587 0.5769 11.00000 0.05 0.25
Q12 1 0.2522 -0.0340 0.6607 11.00000 0.05 0.25
Q13 1 0.3297 -0.0174 0.8702 11.00000 0.05 0.24
Q14 1 0.1490 0.0284 0.9293 11.00000 0.05 0.24
Q15 1 0.1894 0.0185 1.0308 11.00000 0.05 0.24
Q16 1 0.3831 -0.0512 0.5763 11.00000 0.05 0.23
Q17 1 0.1042 0.0704 1.0298 11.00000 0.05 0.23
Q18 1 0.1644 -0.0181 0.5494 11.00000 0.05 0.23
Q19 1 0.2591 -0.0323 0.9528 11.00000 0.05 0.23
Q20 1 -0.0295 -0.1360 0.6319 11.00000 0.05 0.23
;
_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^)+(0.0863P)^2^+0.4775P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.2(9)
_refine_ls_number_reflns 10041
_refine_ls_number_parameters 725
_refine_ls_number_restraints 263
_refine_ls_R_factor_all 0.0661
_refine_ls_R_factor_gt 0.0537
_refine_ls_wR_factor_ref 0.1382
_refine_ls_wR_factor_gt 0.1315
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_restrained_S_all 1.076
_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
N1 N 0.29787(8) 0.0183(2) 0.55771(8) 0.0287(4) Uani 1 1 d U A 1
C1 C 0.34580(10) 0.0307(3) 0.59530(10) 0.0309(5) Uani 1 1 d . A 1
O1 O 0.39509(8) 0.0441(2) 0.57650(7) 0.0424(4) Uani 1 1 d . A 1
C2 C 0.33400(10) 0.0275(2) 0.65945(9) 0.0278(5) Uani 1 1 d . A 1
C3 C 0.37981(10) 0.0358(3) 0.69815(10) 0.0350(6) Uani 1 1 d . A 1
H3 H 0.4185 0.0412 0.6836 0.042 Uiso 1 1 calc R A 1
C4 C 0.36995(11) 0.0362(3) 0.75809(10) 0.0327(5) Uani 1 1 d . A 1
H4 H 0.4025 0.0414 0.7838 0.039 Uiso 1 1 calc R A 1
C5 C 0.31431(10) 0.0292(2) 0.78238(9) 0.0241(5) Uani 1 1 d . A 1
C6 C 0.30297(9) 0.0392(2) 0.84580(9) 0.0240(5) Uani 1 1 d . A 1
C7 C 0.34493(10) 0.0755(2) 0.88779(9) 0.0267(5) Uani 1 1 d . A 1
O2 O 0.40072(7) 0.10398(18) 0.86905(6) 0.0341(4) Uani 1 1 d . A 1
C8 C 0.33227(11) 0.0818(3) 0.94834(10) 0.0332(5) Uani 1 1 d . A 1
H8 H 0.3614 0.1106 0.9755 0.040 Uiso 1 1 calc R A 1
C9 C 0.27799(10) 0.0465(2) 0.96757(9) 0.0298(5) Uani 1 1 d . A 1
C10 C 0.26692(13) 0.0484(3) 1.03218(10) 0.0386(6) Uani 1 1 d D A 1
O3 O 0.30434(10) 0.0834(2) 1.06632(8) 0.0550(6) Uani 1 1 d . A 1
C11 C 0.23379(10) 0.0129(2) 0.92815(9) 0.0274(5) Uani 1 1 d . A 1
C12 C 0.24480(10) 0.0129(2) 0.86619(9) 0.0245(4) Uani 1 1 d . A 1
C13 C 0.26571(10) 0.0134(2) 0.74296(9) 0.0232(4) Uani 1 1 d . A 1
C14 C 0.27690(10) 0.0150(2) 0.68128(9) 0.0247(4) Uani 1 1 d . A 1
C15 C 0.24111(11) -0.0066(2) 0.57708(9) 0.0304(5) Uani 1 1 d . A 1
O6 O 0.20202(8) -0.0353(2) 0.54328(7) 0.0410(4) Uani 1 1 d . A 1
C16 C 0.23048(10) 0.0024(2) 0.64161(9) 0.0278(5) Uani 1 1 d . A 1
C17 C 0.17449(11) -0.0046(2) 0.66135(10) 0.0305(5) Uani 1 1 d . A 1
H17 H 0.1432 -0.0101 0.6341 0.037 Uiso 1 1 calc R A 1
C18 C 0.16295(10) -0.0035(2) 0.72153(10) 0.0281(5) Uani 1 1 d . A 1
O5 O 0.10556(7) -0.00985(19) 0.73978(7) 0.0355(4) Uani 1 1 d . A 1
C19 C 0.20734(10) -0.0028(2) 0.76379(9) 0.0244(4) Uani 1 1 d . A 1
C20 C 0.19728(10) -0.0132(2) 0.82747(10) 0.0254(5) Uani 1 1 d . A 1
C21 C 0.14298(11) -0.0480(3) 0.85077(11) 0.0321(5) Uani 1 1 d . A 1
H21 H 0.1116 -0.0687 0.8249 0.039 Uiso 1 1 calc R A 1
C22 C 0.13358(11) -0.0531(3) 0.91167(11) 0.0344(5) Uani 1 1 d . A 1
H22 H 0.0965 -0.0797 0.9265 0.041 Uiso 1 1 calc R A 1
C23 C 0.17755(11) -0.0201(2) 0.94945(10) 0.0331(5) Uani 1 1 d . A 1
C24 C 0.16495(12) -0.0208(3) 1.01316(11) 0.0390(6) Uani 1 1 d D A 1
O4 O 0.11647(9) -0.0474(2) 1.03208(8) 0.0521(5) Uani 1 1 d . A 1
C61 C 0.31112(11) 0.0146(2) 0.49346(9) 0.0311(5) Uani 1 1 d D . .
H61 H 0.3521 0.0487 0.4889 0.037 Uiso 1 1 calc R A 1
C62 C 0.27300(12) 0.1147(3) 0.45754(10) 0.0388(6) Uani 1 1 d D A .
H62A H 0.2772 0.2130 0.4724 0.047 Uiso 1 1 calc R . .
H62B H 0.2316 0.0867 0.4614 0.047 Uiso 1 1 calc R . .
C63 C 0.29132(13) 0.1080(3) 0.39279(10) 0.0438(6) Uani 1 1 d D . .
H63A H 0.2646 0.1675 0.3691 0.053 Uiso 1 1 calc R A .
H63B H 0.3311 0.1473 0.3886 0.053 Uiso 1 1 calc R . .
C64 C 0.29034(12) -0.0419(3) 0.36962(11) 0.0441(6) Uani 1 1 d D A .
H64A H 0.3043 -0.0423 0.3285 0.053 Uiso 1 1 calc R . .
H64B H 0.2498 -0.0776 0.3699 0.053 Uiso 1 1 calc R . .
C65 C 0.32821(12) -0.1397(3) 0.40610(10) 0.0385(6) Uani 1 1 d D . .
H65A H 0.3694 -0.1097 0.4027 0.046 Uiso 1 1 calc R A .
H65B H 0.3250 -0.2379 0.3909 0.046 Uiso 1 1 calc R . .
C66 C 0.30970(11) -0.1364(2) 0.47080(10) 0.0343(5) Uani 1 1 d D A .
H66A H 0.2698 -0.1754 0.4748 0.041 Uiso 1 1 calc R . .
H66B H 0.3364 -0.1963 0.4943 0.041 Uiso 1 1 calc R . .
N2 N 0.21082(10) 0.0101(2) 1.05124(8) 0.0386(5) Uani 0.722(5) 1 d PDU A 1
C67 C 0.19350(17) 0.0048(4) 1.11458(14) 0.0258(8) Uani 0.722(5) 1 d PDU A 1
H67 H 0.1531 -0.0350 1.1165 0.031 Uiso 0.722(5) 1 calc PR A 1
C68 C 0.23282(19) -0.0947(4) 1.14813(13) 0.0317(8) Uani 0.722(5) 1 d PDU A 1
H68A H 0.2737 -0.0625 1.1448 0.038 Uiso 0.722(5) 1 calc PR A 1
H68B H 0.2301 -0.1916 1.1314 0.038 Uiso 0.722(5) 1 calc PR A 1
C69 C 0.2143(3) -0.0970(6) 1.2132(2) 0.0334(15) Uani 0.722(5) 1 d PDU A 1
H69A H 0.1758 -0.1436 1.2165 0.040 Uiso 0.722(5) 1 calc PR A 1
H69B H 0.2427 -0.1542 1.2358 0.040 Uiso 0.722(5) 1 calc PR A 1
C70 C 0.21080(15) 0.0492(4) 1.23921(14) 0.0331(9) Uani 0.722(5) 1 d PDU A 1
H70A H 0.2503 0.0911 1.2407 0.040 Uiso 0.722(5) 1 calc PR A 1
H70B H 0.1961 0.0424 1.2800 0.040 Uiso 0.722(5) 1 calc PR A 1
C71 C 0.1709(3) 0.1467(5) 1.2039(2) 0.0302(12) Uani 0.722(5) 1 d PDU A 1
H71A H 0.1713 0.2432 1.2212 0.036 Uiso 0.722(5) 1 calc PR A 1
H71B H 0.1305 0.1104 1.2054 0.036 Uiso 0.722(5) 1 calc PR A 1
C72 C 0.1914(3) 0.1538(7) 1.1398(3) 0.0334(12) Uani 0.722(5) 1 d PDU A 1
H72A H 0.1643 0.2131 1.1166 0.040 Uiso 0.722(5) 1 calc PR A 1
H72B H 0.2306 0.1975 1.1379 0.040 Uiso 0.722(5) 1 calc PR A 1
N2B N 0.21082(10) 0.0101(2) 1.05124(8) 0.0386(5) Uani 0.278(5) 1 d PDU A 2
C67B C 0.2180(5) 0.0230(10) 1.1198(4) 0.0258(8) Uani 0.278(5) 1 d PDU A 2
H67B H 0.2598 0.0388 1.1303 0.031 Uiso 0.278(5) 1 calc PR A 2
C68B C 0.1970(5) -0.1184(9) 1.1436(4) 0.036(2) Uani 0.278(5) 1 d PDU A 2
H68C H 0.2220 -0.1961 1.1287 0.044 Uiso 0.278(5) 1 calc PR A 2
H68D H 0.1566 -0.1364 1.1304 0.044 Uiso 0.278(5) 1 calc PR A 2
C69B C 0.1992(6) -0.1145(14) 1.2111(5) 0.023(3) Uani 0.278(5) 1 d PDU A 2
H69C H 0.1832 -0.2041 1.2272 0.028 Uiso 0.278(5) 1 calc PR A 2
H69D H 0.2401 -0.1057 1.2243 0.028 Uiso 0.278(5) 1 calc PR A 2
C70B C 0.1638(4) 0.0111(10) 1.2339(4) 0.042(3) Uani 0.278(5) 1 d PDU A 2
H70C H 0.1661 0.0143 1.2773 0.051 Uiso 0.278(5) 1 calc PR A 2
H70D H 0.1224 -0.0010 1.2227 0.051 Uiso 0.278(5) 1 calc PR A 2
C71B C 0.1870(8) 0.1506(16) 1.2083(7) 0.040(4) Uani 0.278(5) 1 d PDU A 2
H71C H 0.2285 0.1629 1.2191 0.048 Uiso 0.278(5) 1 calc PR A 2
H71D H 0.1648 0.2317 1.2246 0.048 Uiso 0.278(5) 1 calc PR A 2
C72B C 0.1807(10) 0.1470(18) 1.1408(7) 0.0334(12) Uani 0.278(5) 1 d PDU A 2
H72C H 0.1394 0.1324 1.1296 0.040 Uiso 0.278(5) 1 calc PR A 2
H72D H 0.1944 0.2372 1.1234 0.040 Uiso 0.278(5) 1 calc PR A 2
C73 C 0.06315(9) 0.0480(3) 0.70174(10) 0.0333(5) Uani 1 1 d D . .
C74 C 0.05624(10) 0.1928(3) 0.70019(11) 0.0370(5) Uani 1 1 d D A .
C75 C 0.01311(11) 0.2469(3) 0.66303(12) 0.0416(6) Uani 1 1 d D . .
H75 H 0.0076 0.3467 0.6602 0.050 Uiso 1 1 calc R A .
C76 C -0.02168(10) 0.1562(3) 0.63025(11) 0.0394(6) Uani 1 1 d D A .
H76 H -0.0512 0.1939 0.6055 0.047 Uiso 1 1 calc R . .
C77 C -0.01345(10) 0.0113(3) 0.63358(11) 0.0395(6) Uani 1 1 d D . .
H77 H -0.0377 -0.0497 0.6111 0.047 Uiso 1 1 calc R A .
C78 C 0.02951(10) -0.0479(3) 0.66904(11) 0.0362(6) Uani 1 1 d D A .
C79 C 0.44179(10) 0.1638(3) 0.90846(10) 0.0330(5) Uani 1 1 d D . .
C80 C 0.44728(11) 0.3114(3) 0.90856(11) 0.0378(5) Uani 1 1 d D A .
C81 C 0.49136(12) 0.3674(3) 0.94352(12) 0.0436(6) Uani 1 1 d D . .
H81 H 0.4965 0.4674 0.9452 0.052 Uiso 1 1 calc R A .
C82 C 0.52767(11) 0.2810(3) 0.97569(11) 0.0421(6) Uani 1 1 d D A .
H82 H 0.5580 0.3218 0.9985 0.051 Uiso 1 1 calc R . .
C83 C 0.52032(11) 0.1340(3) 0.97506(11) 0.0391(6) Uani 1 1 d D . .
H83 H 0.5453 0.0755 0.9979 0.047 Uiso 1 1 calc R A .
C84 C 0.47659(11) 0.0723(3) 0.94117(10) 0.0356(5) Uani 1 1 d D A .
C85 C 0.09220(11) 0.2935(3) 0.73811(12) 0.0432(6) Uani 1 1 d . . .
H85 H 0.1253 0.2377 0.7550 0.052 Uiso 1 1 calc R A .
C86 C 0.05632(15) 0.3488(4) 0.78867(13) 0.0607(8) Uani 1 1 d . A .
H86A H 0.0789 0.4197 0.8105 0.091 Uiso 1 1 calc R . .
H86B H 0.0461 0.2700 0.8148 0.091 Uiso 1 1 calc R . .
H86C H 0.0206 0.3927 0.7735 0.091 Uiso 1 1 calc R . .
C87 C 0.11793(16) 0.4136(4) 0.70247(15) 0.0692(10) Uani 1 1 d . A .
H87A H 0.1419 0.3744 0.6708 0.104 Uiso 1 1 calc R . .
H87B H 0.1422 0.4733 0.7279 0.104 Uiso 1 1 calc R . .
H87C H 0.0864 0.4709 0.6857 0.104 Uiso 1 1 calc R . .
C88 C 0.03865(13) -0.2068(3) 0.67382(13) 0.0478(7) Uani 0.50 1 d P A 1
H88 H 0.0688 -0.2244 0.7047 0.057 Uiso 0.50 1 calc PR A 1
C89 C -0.0101(4) -0.2842(13) 0.6881(7) 0.083(5) Uani 0.372(10) 1 d P A 1
H89A H -0.0244 -0.2546 0.7267 0.125 Uiso 0.372(10) 1 calc PR A 1
H89B H -0.0003 -0.3855 0.6891 0.125 Uiso 0.372(10) 1 calc PR A 1
H89C H -0.0405 -0.2678 0.6586 0.125 Uiso 0.372(10) 1 calc PR A 1
C90 C 0.0658(7) -0.2608(11) 0.6092(4) 0.075(4) Uani 0.372(10) 1 d P A 1
H90A H 0.0738 -0.3630 0.6109 0.112 Uiso 0.372(10) 1 calc PR A 1
H90B H 0.1019 -0.2093 0.6010 0.112 Uiso 0.372(10) 1 calc PR A 1
H90C H 0.0374 -0.2417 0.5781 0.112 Uiso 0.372(10) 1 calc PR A 1
C88B C 0.03865(13) -0.2068(3) 0.67382(13) 0.0478(7) Uani 0.50 1 d P A 2
H88B H 0.0812 -0.2266 0.6787 0.057 Uiso 0.50 1 calc PR A 2
C89B C 0.0040(2) -0.2621(5) 0.7319(3) 0.0554(16) Uani 0.628(10) 1 d P A 2
H89D H -0.0380 -0.2469 0.7266 0.083 Uiso 0.628(10) 1 calc PR A 2
H89E H 0.0174 -0.2090 0.7664 0.083 Uiso 0.628(10) 1 calc PR A 2
H89F H 0.0116 -0.3636 0.7377 0.083 Uiso 0.628(10) 1 calc PR A 2
C90B C 0.0163(4) -0.2890(5) 0.6228(3) 0.066(2) Uani 0.628(10) 1 d P A 2
H90D H -0.0264 -0.2866 0.6228 0.099 Uiso 0.628(10) 1 calc PR A 2
H90E H 0.0296 -0.3877 0.6257 0.099 Uiso 0.628(10) 1 calc PR A 2
H90F H 0.0310 -0.2469 0.5863 0.099 Uiso 0.628(10) 1 calc PR A 2
C92 C 0.4890(12) -0.177(2) 0.9932(8) 0.053(6) Uani 0.186(16) 1 d PDU A 1
H92A H 0.5053 -0.2669 0.9788 0.080 Uiso 0.186(16) 1 calc PR A 1
H92B H 0.4559 -0.1970 1.0192 0.080 Uiso 0.186(16) 1 calc PR A 1
H92C H 0.5189 -0.1249 1.0149 0.080 Uiso 0.186(16) 1 calc PR A 1
C91 C 0.46810(12) -0.0870(3) 0.94064(11) 0.0433(6) Uani 0.186(16) 1 d PDU A 1
H91 H 0.4266 -0.1102 0.9313 0.052 Uiso 0.186(16) 1 calc PR A 1
C93 C 0.5085(9) -0.146(2) 0.8921(8) 0.045(5) Uani 0.186(16) 1 d PDU A 1
H93A H 0.4850 -0.1740 0.8581 0.067 Uiso 0.186(16) 1 calc PR A 1
H93B H 0.5295 -0.2292 0.9071 0.067 Uiso 0.186(16) 1 calc PR A 1
H93C H 0.5365 -0.0728 0.8805 0.067 Uiso 0.186(16) 1 calc PR A 1
C92B C 0.4566(4) -0.1412(6) 1.0038(2) 0.069(2) Uani 0.814(16) 1 d PDU A 2
H92D H 0.4507 -0.2443 1.0031 0.103 Uiso 0.814(16) 1 calc PR A 2
H92E H 0.4216 -0.0950 1.0196 0.103 Uiso 0.814(16) 1 calc PR A 2
H92F H 0.4901 -0.1185 1.0288 0.103 Uiso 0.814(16) 1 calc PR A 2
C91B C 0.46810(12) -0.0870(3) 0.94064(11) 0.0433(6) Uani 0.814(16) 1 d PDU A 2
H91B H 0.4329 -0.1085 0.9164 0.052 Uiso 0.814(16) 1 calc PR A 2
C93B C 0.5197(2) -0.1615(7) 0.9130(4) 0.0692(17) Uani 0.814(16) 1 d PDU A 2
H93D H 0.5251 -0.1267 0.8728 0.104 Uiso 0.814(16) 1 calc PR A 2
H93E H 0.5125 -0.2642 0.9122 0.104 Uiso 0.814(16) 1 calc PR A 2
H93F H 0.5548 -0.1419 0.9360 0.104 Uiso 0.814(16) 1 calc PR A 2
C95 C 0.3871(9) 0.5426(17) 0.9005(8) 0.060(3) Uani 0.53(2) 1 d PDU A 1
H95A H 0.4192 0.5877 0.9219 0.090 Uiso 0.53(2) 1 calc PR A 1
H95B H 0.3556 0.5196 0.9280 0.090 Uiso 0.53(2) 1 calc PR A 1
H95C H 0.3725 0.6078 0.8704 0.090 Uiso 0.53(2) 1 calc PR A 1
C94 C 0.40897(12) 0.4060(3) 0.87136(11) 0.0442(6) Uani 0.53(2) 1 d PDU A 1
H94 H 0.3732 0.3487 0.8634 0.053 Uiso 0.53(2) 1 calc PR A 1
C96 C 0.4347(4) 0.4388(12) 0.8105(3) 0.050(2) Uani 0.53(2) 1 d PDU A 1
H96A H 0.4720 0.4885 0.8152 0.075 Uiso 0.53(2) 1 calc PR A 1
H96B H 0.4076 0.4989 0.7885 0.075 Uiso 0.53(2) 1 calc PR A 1
H96C H 0.4411 0.3497 0.7892 0.075 Uiso 0.53(2) 1 calc PR A 1
C96B C 0.4521(6) 0.4829(13) 0.8277(6) 0.067(3) Uani 0.47(2) 1 d PDU A 2
H96D H 0.4302 0.5500 0.8033 0.101 Uiso 0.47(2) 1 calc PR A 2
H96E H 0.4710 0.4120 0.8026 0.101 Uiso 0.47(2) 1 calc PR A 2
H96F H 0.4817 0.5343 0.8502 0.101 Uiso 0.47(2) 1 calc PR A 2
C94B C 0.40897(12) 0.4060(3) 0.87136(11) 0.0442(6) Uani 0.47(2) 1 d PDU A 2
H94B H 0.3781 0.3511 0.8502 0.053 Uiso 0.47(2) 1 calc PR A 2
C95B C 0.3835(9) 0.5207(17) 0.9103(8) 0.051(3) Uani 0.47(2) 1 d PDU A 2
H95D H 0.3672 0.4773 0.9459 0.077 Uiso 0.47(2) 1 calc PR A 2
H95E H 0.3526 0.5709 0.8891 0.077 Uiso 0.47(2) 1 calc PR A 2
H95F H 0.4141 0.5882 0.9213 0.077 Uiso 0.47(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
N1 0.0318(11) 0.0398(10) 0.0145(9) -0.0010(7) 0.0018(8) -0.0024(8)
C1 0.0276(13) 0.0427(13) 0.0223(11) -0.0052(9) 0.0016(10) -0.0046(10)
O1 0.0326(10) 0.0735(12) 0.0211(8) -0.0060(8) 0.0051(7) -0.0106(9)
C2 0.0271(12) 0.0354(12) 0.0207(11) -0.0016(9) 0.0040(9) -0.0043(9)
C3 0.0238(12) 0.0600(15) 0.0212(12) -0.0087(10) 0.0042(10) -0.0072(10)
C4 0.0272(13) 0.0497(14) 0.0211(11) -0.0068(10) -0.0019(9) -0.0066(10)
C5 0.0196(11) 0.0345(11) 0.0181(11) -0.0016(8) -0.0014(8) -0.0002(8)
C6 0.0251(12) 0.0301(10) 0.0168(10) -0.0001(8) -0.0029(9) 0.0032(8)
C7 0.0256(12) 0.0371(11) 0.0175(10) 0.0016(9) -0.0011(8) 0.0006(9)
O2 0.0259(8) 0.0561(10) 0.0203(8) -0.0025(7) -0.0062(7) -0.0061(7)
C8 0.0387(14) 0.0401(12) 0.0207(11) -0.0018(9) -0.0072(10) -0.0022(10)
C9 0.0378(13) 0.0348(12) 0.0167(11) 0.0016(8) 0.0005(9) 0.0027(9)
C10 0.0613(18) 0.0375(13) 0.0170(12) 0.0001(9) -0.0028(12) 0.0006(12)
O3 0.0732(15) 0.0728(13) 0.0189(9) -0.0012(9) -0.0032(9) -0.0194(11)
C11 0.0349(13) 0.0292(11) 0.0182(11) 0.0020(8) 0.0051(9) 0.0056(9)
C12 0.0264(11) 0.0300(11) 0.0171(10) 0.0016(8) 0.0011(9) 0.0041(8)
C13 0.0251(12) 0.0276(10) 0.0171(10) -0.0010(8) 0.0006(9) 0.0012(8)
C14 0.0220(10) 0.0340(11) 0.0180(10) -0.0024(8) 0.0010(9) -0.0006(9)
C15 0.0319(13) 0.0414(13) 0.0180(11) -0.0008(9) -0.0062(10) -0.0002(10)
O6 0.0354(10) 0.0667(12) 0.0210(8) -0.0019(8) -0.0031(8) -0.0066(8)
C16 0.0294(12) 0.0376(12) 0.0165(10) -0.0014(9) -0.0017(9) 0.0005(9)
C17 0.0259(12) 0.0444(13) 0.0211(11) -0.0033(9) -0.0076(9) 0.0031(9)
C18 0.0231(12) 0.0372(11) 0.0239(11) 0.0003(9) 0.0010(9) 0.0011(9)
O5 0.0204(8) 0.0609(10) 0.0251(8) -0.0010(7) -0.0004(7) 0.0043(7)
C19 0.0251(11) 0.0287(11) 0.0193(10) -0.0012(8) -0.0002(9) 0.0006(9)
C20 0.0250(12) 0.0320(11) 0.0193(11) 0.0000(8) 0.0013(9) 0.0017(9)
C21 0.0266(12) 0.0438(13) 0.0260(12) 0.0021(10) 0.0026(10) 0.0024(10)
C22 0.0272(12) 0.0489(13) 0.0269(12) 0.0048(10) 0.0078(10) 0.0028(10)
C23 0.0381(14) 0.0386(12) 0.0226(12) 0.0044(9) 0.0109(10) 0.0054(10)
C24 0.0453(16) 0.0477(14) 0.0241(12) 0.0068(10) 0.0074(11) 0.0099(11)
O4 0.0470(12) 0.0770(14) 0.0322(11) 0.0162(9) 0.0231(9) 0.0123(10)
C61 0.0343(13) 0.0432(13) 0.0157(11) -0.0005(9) 0.0040(9) -0.0042(10)
C62 0.0526(16) 0.0405(13) 0.0233(12) 0.0015(10) 0.0021(11) -0.0001(11)
C63 0.0530(17) 0.0541(16) 0.0244(13) 0.0105(11) 0.0002(11) 0.0000(12)
C64 0.0482(16) 0.0644(17) 0.0196(12) -0.0024(11) 0.0016(12) -0.0024(13)
C65 0.0498(16) 0.0470(14) 0.0186(11) -0.0057(10) 0.0065(11) -0.0055(11)
C66 0.0424(14) 0.0391(12) 0.0213(11) 0.0012(9) 0.0029(10) -0.0005(10)
N2 0.0534(13) 0.0441(11) 0.0184(10) 0.0039(8) 0.0125(9) 0.0066(9)
C67 0.0200(19) 0.0415(15) 0.0160(13) 0.0013(10) 0.0018(15) -0.0080(15)
C68 0.039(2) 0.0371(17) 0.0193(16) 0.0048(12) 0.0030(14) 0.0077(15)
C69 0.031(3) 0.045(3) 0.024(2) 0.0055(16) 0.0001(17) -0.002(2)
C70 0.0333(19) 0.0478(18) 0.0181(15) 0.0014(13) -0.0001(13) -0.0034(14)
C71 0.032(3) 0.0354(18) 0.0229(19) -0.0006(14) 0.0053(18) 0.0002(17)
C72 0.040(3) 0.0391(14) 0.0206(11) 0.0011(10) 0.0011(15) 0.0004(16)
N2B 0.0534(13) 0.0441(11) 0.0184(10) 0.0039(8) 0.0125(9) 0.0066(9)
C67B 0.0200(19) 0.0415(15) 0.0160(13) 0.0013(10) 0.0018(15) -0.0080(15)
C68B 0.036(4) 0.039(4) 0.034(4) -0.003(3) 0.001(3) 0.006(3)
C69B 0.027(5) 0.025(4) 0.018(4) 0.001(3) 0.001(3) -0.003(4)
C70B 0.044(4) 0.055(4) 0.028(4) 0.000(3) 0.000(3) -0.002(3)
C71B 0.040(6) 0.047(5) 0.032(5) -0.001(4) 0.007(4) 0.002(4)
C72B 0.040(3) 0.0391(14) 0.0206(11) 0.0011(10) 0.0011(15) 0.0004(16)
C73 0.0190(11) 0.0565(15) 0.0244(11) -0.0018(10) 0.0004(9) 0.0028(10)
C74 0.0232(12) 0.0549(15) 0.0329(12) -0.0073(11) -0.0013(10) 0.0030(10)
C75 0.0303(14) 0.0491(14) 0.0454(15) -0.0027(12) -0.0022(11) 0.0058(11)
C76 0.0252(12) 0.0574(15) 0.0354(13) 0.0046(12) -0.0051(10) 0.0004(11)
C77 0.0256(13) 0.0576(16) 0.0354(13) -0.0003(12) -0.0082(10) -0.0027(11)
C78 0.0250(12) 0.0538(14) 0.0297(13) -0.0011(11) -0.0010(10) -0.0018(11)
C79 0.0282(12) 0.0504(14) 0.0205(10) -0.0048(10) -0.0051(9) -0.0069(10)
C80 0.0346(13) 0.0542(14) 0.0247(11) -0.0026(11) 0.0025(10) -0.0053(11)
C81 0.0441(16) 0.0504(14) 0.0363(14) -0.0054(11) 0.0005(12) -0.0103(12)
C82 0.0341(14) 0.0611(16) 0.0311(13) -0.0094(12) -0.0032(11) -0.0097(12)
C83 0.0294(13) 0.0623(16) 0.0257(12) -0.0018(11) -0.0073(10) -0.0001(11)
C84 0.0324(13) 0.0519(14) 0.0226(12) -0.0004(10) -0.0031(10) -0.0034(10)
C85 0.0316(14) 0.0525(15) 0.0456(15) -0.0105(12) -0.0102(12) 0.0055(11)
C86 0.058(2) 0.084(2) 0.0403(16) -0.0185(15) -0.0031(14) -0.0094(16)
C87 0.060(2) 0.096(3) 0.0523(19) -0.0121(18) -0.0028(16) -0.0304(18)
C88 0.0431(16) 0.0494(14) 0.0508(16) -0.0035(13) -0.0144(13) -0.0001(12)
C89 0.047(6) 0.095(8) 0.107(13) 0.031(8) 0.016(6) 0.006(5)
C90 0.098(11) 0.067(6) 0.059(6) -0.017(5) -0.007(6) 0.025(6)
C88B 0.0431(16) 0.0494(14) 0.0508(16) -0.0035(13) -0.0144(13) -0.0001(12)
C89B 0.053(3) 0.052(3) 0.061(4) 0.017(3) 0.007(3) -0.001(2)
C90B 0.095(6) 0.044(3) 0.058(3) -0.008(2) -0.035(4) 0.001(3)
C92 0.059(10) 0.059(8) 0.041(8) 0.000(6) -0.009(7) 0.002(7)
C91 0.0393(14) 0.0508(13) 0.0399(13) 0.0044(11) -0.0143(11) -0.0056(11)
C93 0.026(8) 0.032(7) 0.076(8) 0.009(7) -0.009(6) 0.008(6)
C92B 0.097(5) 0.061(3) 0.048(2) 0.018(2) -0.020(3) -0.020(3)
C91B 0.0393(14) 0.0508(13) 0.0399(13) 0.0044(11) -0.0143(11) -0.0056(11)
C93B 0.046(3) 0.050(3) 0.111(4) -0.003(3) -0.018(3) 0.014(2)
C95 0.054(5) 0.074(5) 0.051(5) -0.011(4) -0.010(4) 0.010(4)
C94 0.0473(15) 0.0500(14) 0.0352(13) 0.0044(11) 0.0042(11) 0.0006(11)
C96 0.047(4) 0.079(5) 0.025(3) 0.008(3) -0.007(3) 0.018(3)
C96B 0.081(5) 0.088(5) 0.033(4) 0.015(4) 0.016(4) 0.020(4)
C94B 0.0473(15) 0.0500(14) 0.0352(13) 0.0044(11) 0.0042(11) 0.0006(11)
C95B 0.035(4) 0.068(5) 0.051(5) -0.001(4) 0.002(4) 0.009(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
N1 C15 1.395(3) . ?
N1 C1 1.399(3) . ?
N1 C61 1.495(3) . ?
C1 O1 1.216(3) . ?
C1 C2 1.486(3) . ?
C2 C3 1.374(3) . ?
C2 C14 1.407(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.393(3) . ?
C5 C13 1.440(3) . ?
C5 C6 1.471(3) . ?
C6 C7 1.399(3) . ?
C6 C12 1.436(3) . ?
C7 O2 1.377(3) . ?
C7 C8 1.410(3) . ?
O2 C79 1.418(3) . ?
C8 C9 1.362(3) . ?
C9 C11 1.391(3) . ?
C9 C10 1.493(3) . ?
C10 O3 1.205(3) . ?
C10 N2 1.406(3) . ?
C11 C23 1.414(3) . ?
C11 C12 1.434(3) . ?
C12 C20 1.424(3) . ?
C13 C14 1.428(3) . ?
C13 C19 1.430(3) . ?
C14 C16 1.402(3) . ?
C15 O6 1.213(3) . ?
C15 C16 1.492(3) . ?
C16 C17 1.363(3) . ?
C17 C18 1.396(3) . ?
C18 O5 1.383(3) . ?
C18 C19 1.402(3) . ?
O5 C73 1.412(3) . ?
C19 C20 1.472(3) . ?
C20 C21 1.394(3) . ?
C21 C22 1.404(3) . ?
C22 C23 1.362(4) . ?
C23 C24 1.480(3) . ?
C24 O4 1.219(3) . ?
C24 N2 1.395(4) . ?
C61 C66 1.512(3) . ?
C61 C62 1.524(3) . ?
C62 C63 1.535(3) . ?
C63 C64 1.506(4) . ?
C64 C65 1.514(4) . ?
C65 C66 1.534(3) . ?
N2 C67 1.497(4) . ?
C67 C68 1.509(5) . ?
C67 C72 1.517(7) . ?
C68 C69 1.541(6) . ?
C69 C70 1.501(6) . ?
C70 C71 1.525(6) . ?
C71 C72 1.534(6) . ?
C67B C68B 1.516(11) . ?
C67B C72B 1.525(14) . ?
C68B C69B 1.538(12) . ?
C69B C70B 1.526(12) . ?
C70B C71B 1.532(14) . ?
C71B C72B 1.545(14) . ?
C73 C74 1.373(4) . ?
C73 C78 1.402(3) . ?
C74 C75 1.398(4) . ?
C74 C85 1.525(3) . ?
C75 C76 1.387(4) . ?
C76 C77 1.378(4) . ?
C77 C78 1.391(3) . ?
C78 C88 1.514(4) . ?
C79 C84 1.391(3) . ?
C79 C80 1.394(4) . ?
C80 C81 1.391(4) . ?
C80 C94 1.511(4) . ?
C81 C82 1.376(4) . ?
C82 C83 1.393(4) . ?
C83 C84 1.393(3) . ?
C84 C91 1.512(4) . ?
C85 C86 1.509(4) . ?
C85 C87 1.512(5) . ?
C88 C89 1.375(10) . ?
C88 C90 1.676(11) . ?
C92 C91 1.543(12) . ?
C91 C93 1.545(8) . ?
C95 C94 1.531(10) . ?
C94 C96 1.538(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
C15 N1 C1 123.71(18) . . ?
C15 N1 C61 119.70(18) . . ?
C1 N1 C61 116.16(19) . . ?
O1 C1 N1 121.7(2) . . ?
O1 C1 C2 121.2(2) . . ?
N1 C1 C2 117.2(2) . . ?
C3 C2 C14 119.4(2) . . ?
C3 C2 C1 119.3(2) . . ?
C14 C2 C1 121.3(2) . . ?
C2 C3 C4 120.5(2) . . ?
C3 C4 C5 122.8(2) . . ?
C4 C5 C13 117.88(19) . . ?
C4 C5 C6 123.30(19) . . ?
C13 C5 C6 118.82(19) . . ?
C7 C6 C12 117.47(19) . . ?
C7 C6 C5 124.41(19) . . ?
C12 C6 C5 118.12(18) . . ?
O2 C7 C6 118.42(18) . . ?
O2 C7 C8 119.12(19) . . ?
C6 C7 C8 122.5(2) . . ?
C7 O2 C79 119.98(16) . . ?
C9 C8 C7 119.5(2) . . ?
C8 C9 C11 121.00(19) . . ?
C8 C9 C10 118.0(2) . . ?
C11 C9 C10 121.0(2) . . ?
O3 C10 N2 121.6(2) . . ?
O3 C10 C9 121.2(2) . . ?
N2 C10 C9 117.2(2) . . ?
C9 C11 C23 119.63(19) . . ?
C9 C11 C12 120.4(2) . . ?
C23 C11 C12 119.9(2) . . ?
C20 C12 C11 118.3(2) . . ?
C20 C12 C6 122.82(19) . . ?
C11 C12 C6 118.84(19) . . ?
C14 C13 C19 119.74(19) . . ?
C14 C13 C5 118.22(19) . . ?
C19 C13 C5 122.03(18) . . ?
C16 C14 C2 119.18(19) . . ?
C16 C14 C13 119.75(19) . . ?
C2 C14 C13 121.07(19) . . ?
O6 C15 N1 121.8(2) . . ?
O6 C15 C16 121.1(2) . . ?
N1 C15 C16 117.04(19) . . ?
C17 C16 C14 120.55(19) . . ?
C17 C16 C15 118.4(2) . . ?
C14 C16 C15 121.0(2) . . ?
C16 C17 C18 120.1(2) . . ?
O5 C18 C17 118.4(2) . . ?
O5 C18 C19 119.11(19) . . ?
C17 C18 C19 122.4(2) . . ?
C18 O5 C73 117.11(17) . . ?
C18 C19 C13 117.00(18) . . ?
C18 C19 C20 124.2(2) . . ?
C13 C19 C20 118.76(19) . . ?
C21 C20 C12 119.3(2) . . ?
C21 C20 C19 122.1(2) . . ?
C12 C20 C19 118.60(19) . . ?
C20 C21 C22 121.4(2) . . ?
C23 C22 C21 120.1(2) . . ?
C22 C23 C11 120.7(2) . . ?
C22 C23 C24 118.3(2) . . ?
C11 C23 C24 121.1(2) . . ?
O4 C24 N2 120.8(2) . . ?
O4 C24 C23 121.7(3) . . ?
N2 C24 C23 117.5(2) . . ?
N1 C61 C66 110.58(18) . . ?
N1 C61 C62 113.22(19) . . ?
C66 C61 C62 112.7(2) . . ?
C61 C62 C63 109.5(2) . . ?
C64 C63 C62 111.8(2) . . ?
C63 C64 C65 111.6(2) . . ?
C64 C65 C66 110.8(2) . . ?
C61 C66 C65 109.92(19) . . ?
C24 N2 C10 123.6(2) . . ?
C24 N2 C67 113.0(2) . . ?
C10 N2 C67 123.3(2) . . ?
N2 C67 C68 110.5(3) . . ?
N2 C67 C72 110.1(3) . . ?
C68 C67 C72 113.6(4) . . ?
C67 C68 C69 109.3(3) . . ?
C70 C69 C68 112.5(4) . . ?
C69 C70 C71 112.0(4) . . ?
C70 C71 C72 110.1(4) . . ?
C67 C72 C71 109.3(5) . . ?
C68B C67B C72B 112.3(11) . . ?
C67B C68B C69B 109.0(8) . . ?
C70B C69B C68B 109.9(9) . . ?
C69B C70B C71B 110.5(10) . . ?
C70B C71B C72B 109.0(13) . . ?
C67B C72B C71B 106.1(12) . . ?
C74 C73 C78 124.2(2) . . ?
C74 C73 O5 118.6(2) . . ?
C78 C73 O5 117.2(2) . . ?
C73 C74 C75 117.3(2) . . ?
C73 C74 C85 122.7(2) . . ?
C75 C74 C85 120.0(2) . . ?
C76 C75 C74 120.6(3) . . ?
C77 C76 C75 120.0(2) . . ?
C76 C77 C78 121.7(2) . . ?
C77 C78 C73 116.2(2) . . ?
C77 C78 C88 122.4(2) . . ?
C73 C78 C88 121.4(2) . . ?
C84 C79 C80 124.3(2) . . ?
C84 C79 O2 118.3(2) . . ?
C80 C79 O2 117.2(2) . . ?
C81 C80 C79 116.4(2) . . ?
C81 C80 C94 121.4(2) . . ?
C79 C80 C94 122.2(2) . . ?
C82 C81 C80 121.4(3) . . ?
C81 C82 C83 120.5(2) . . ?
C82 C83 C84 120.5(2) . . ?
C79 C84 C83 116.9(2) . . ?
C79 C84 C91 122.4(2) . . ?
C83 C84 C91 120.7(2) . . ?
C86 C85 C87 111.4(3) . . ?
C86 C85 C74 110.6(2) . . ?
C87 C85 C74 111.8(2) . . ?
C89 C88 C78 115.3(5) . . ?
C89 C88 C90 110.4(8) . . ?
C78 C88 C90 106.7(4) . . ?
C84 C91 C92 119.9(8) . . ?
C84 C91 C93 106.6(9) . . ?
C92 C91 C93 99.8(10) . . ?
C80 C94 C95 116.2(8) . . ?
C80 C94 C96 113.5(3) . . ?
C95 C94 C96 110.4(8) . . ?
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
C15 N1 C1 O1 175.6(2) . . . . ?
C61 N1 C1 O1 3.2(3) . . . . ?
C15 N1 C1 C2 -4.6(3) . . . . ?
C61 N1 C1 C2 -177.07(19) . . . . ?
O1 C1 C2 C3 -1.8(4) . . . . ?
N1 C1 C2 C3 178.4(2) . . . . ?
O1 C1 C2 C14 178.7(2) . . . . ?
N1 C1 C2 C14 -1.1(3) . . . . ?
C14 C2 C3 C4 -2.0(4) . . . . ?
C1 C2 C3 C4 178.5(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C3 C4 C5 C13 3.4(4) . . . . ?
C3 C4 C5 C6 -175.7(2) . . . . ?
C4 C5 C6 C7 8.9(3) . . . . ?
C13 C5 C6 C7 -170.2(2) . . . . ?
C4 C5 C6 C12 -172.3(2) . . . . ?
C13 C5 C6 C12 8.6(3) . . . . ?
C12 C6 C7 O2 -178.70(19) . . . . ?
C5 C6 C7 O2 0.0(3) . . . . ?
C12 C6 C7 C8 2.2(3) . . . . ?
C5 C6 C7 C8 -179.1(2) . . . . ?
C6 C7 O2 C79 169.4(2) . . . . ?
C8 C7 O2 C79 -11.4(3) . . . . ?
O2 C7 C8 C9 -176.5(2) . . . . ?
C6 C7 C8 C9 2.6(3) . . . . ?
C7 C8 C9 C11 -4.1(3) . . . . ?
C7 C8 C9 C10 177.4(2) . . . . ?
C8 C9 C10 O3 1.8(4) . . . . ?
C11 C9 C10 O3 -176.7(2) . . . . ?
C8 C9 C10 N2 -179.3(2) . . . . ?
C11 C9 C10 N2 2.2(3) . . . . ?
C8 C9 C11 C23 -178.5(2) . . . . ?
C10 C9 C11 C23 -0.1(3) . . . . ?
C8 C9 C11 C12 0.9(3) . . . . ?
C10 C9 C11 C12 179.4(2) . . . . ?
C9 C11 C12 C20 -176.0(2) . . . . ?
C23 C11 C12 C20 3.4(3) . . . . ?
C9 C11 C12 C6 3.9(3) . . . . ?
C23 C11 C12 C6 -176.67(19) . . . . ?
C7 C6 C12 C20 174.6(2) . . . . ?
C5 C6 C12 C20 -4.2(3) . . . . ?
C7 C6 C12 C11 -5.3(3) . . . . ?
C5 C6 C12 C11 175.91(18) . . . . ?
C4 C5 C13 C14 -4.0(3) . . . . ?
C6 C5 C13 C14 175.16(18) . . . . ?
C4 C5 C13 C19 176.4(2) . . . . ?
C6 C5 C13 C19 -4.5(3) . . . . ?
C3 C2 C14 C16 -178.2(2) . . . . ?
C1 C2 C14 C16 1.3(3) . . . . ?
C3 C2 C14 C13 1.2(3) . . . . ?
C1 C2 C14 C13 -179.3(2) . . . . ?
C19 C13 C14 C16 0.8(3) . . . . ?
C5 C13 C14 C16 -178.85(19) . . . . ?
C19 C13 C14 C2 -178.5(2) . . . . ?
C5 C13 C14 C2 1.8(3) . . . . ?
C1 N1 C15 O6 -170.1(2) . . . . ?
C61 N1 C15 O6 2.1(3) . . . . ?
C1 N1 C15 C16 9.4(3) . . . . ?
C61 N1 C15 C16 -178.45(19) . . . . ?
C2 C14 C16 C17 -177.5(2) . . . . ?
C13 C14 C16 C17 3.1(3) . . . . ?
C2 C14 C16 C15 3.7(3) . . . . ?
C13 C14 C16 C15 -175.7(2) . . . . ?
O6 C15 C16 C17 -8.2(3) . . . . ?
N1 C15 C16 C17 172.3(2) . . . . ?
O6 C15 C16 C14 170.6(2) . . . . ?
N1 C15 C16 C14 -8.8(3) . . . . ?
C14 C16 C17 C18 -1.9(3) . . . . ?
C15 C16 C17 C18 176.9(2) . . . . ?
C16 C17 C18 O5 179.6(2) . . . . ?
C16 C17 C18 C19 -3.4(3) . . . . ?
C17 C18 O5 C73 -28.9(3) . . . . ?
C19 C18 O5 C73 154.0(2) . . . . ?
O5 C18 C19 C13 -175.94(19) . . . . ?
C17 C18 C19 C13 7.1(3) . . . . ?
O5 C18 C19 C20 2.1(3) . . . . ?
C17 C18 C19 C20 -174.9(2) . . . . ?
C14 C13 C19 C18 -5.7(3) . . . . ?
C5 C13 C19 C18 174.0(2) . . . . ?
C14 C13 C19 C20 176.23(19) . . . . ?
C5 C13 C19 C20 -4.1(3) . . . . ?
C11 C12 C20 C21 -4.7(3) . . . . ?
C6 C12 C20 C21 175.4(2) . . . . ?
C11 C12 C20 C19 175.52(18) . . . . ?
C6 C12 C20 C19 -4.4(3) . . . . ?
C18 C19 C20 C21 10.8(3) . . . . ?
C13 C19 C20 C21 -171.2(2) . . . . ?
C18 C19 C20 C12 -169.4(2) . . . . ?
C13 C19 C20 C12 8.5(3) . . . . ?
C12 C20 C21 C22 2.3(3) . . . . ?
C19 C20 C21 C22 -178.0(2) . . . . ?
C20 C21 C22 C23 1.7(4) . . . . ?
C21 C22 C23 C11 -3.1(3) . . . . ?
C21 C22 C23 C24 177.3(2) . . . . ?
C9 C11 C23 C22 179.9(2) . . . . ?
C12 C11 C23 C22 0.5(3) . . . . ?
C9 C11 C23 C24 -0.5(3) . . . . ?
C12 C11 C23 C24 -180.0(2) . . . . ?
C22 C23 C24 O4 -1.3(4) . . . . ?
C11 C23 C24 O4 179.1(2) . . . . ?
C22 C23 C24 N2 178.6(2) . . . . ?
C11 C23 C24 N2 -1.0(3) . . . . ?
C15 N1 C61 C66 -72.5(3) . . . . ?
C1 N1 C61 C66 100.2(2) . . . . ?
C15 N1 C61 C62 55.0(3) . . . . ?
C1 N1 C61 C62 -132.3(2) . . . . ?
N1 C61 C62 C63 177.8(2) . . . . ?
C66 C61 C62 C63 -55.8(3) . . . . ?
C61 C62 C63 C64 54.7(3) . . . . ?
C62 C63 C64 C65 -56.1(3) . . . . ?
C63 C64 C65 C66 56.3(3) . . . . ?
N1 C61 C66 C65 -175.4(2) . . . . ?
C62 C61 C66 C65 56.8(3) . . . . ?
C64 C65 C66 C61 -55.9(3) . . . . ?
O4 C24 N2 C10 -176.8(2) . . . . ?
C23 C24 N2 C10 3.3(3) . . . . ?
O4 C24 N2 C67 0.6(4) . . . . ?
C23 C24 N2 C67 -179.3(2) . . . . ?
O3 C10 N2 C24 175.0(3) . . . . ?
C9 C10 N2 C24 -3.9(3) . . . . ?
O3 C10 N2 C67 -2.1(4) . . . . ?
C9 C10 N2 C67 179.0(2) . . . . ?
C24 N2 C67 C68 125.5(3) . . . . ?
C10 N2 C67 C68 -57.1(4) . . . . ?
C24 N2 C67 C72 -108.3(4) . . . . ?
C10 N2 C67 C72 69.2(5) . . . . ?
N2 C67 C68 C69 179.5(4) . . . . ?
C72 C67 C68 C69 55.3(6) . . . . ?
C67 C68 C69 C70 -52.8(5) . . . . ?
C68 C69 C70 C71 54.9(5) . . . . ?
C69 C70 C71 C72 -56.4(6) . . . . ?
N2 C67 C72 C71 177.5(4) . . . . ?
C68 C67 C72 C71 -58.1(7) . . . . ?
C70 C71 C72 C67 56.6(7) . . . . ?
C72B C67B C68B C69B -60.0(15) . . . . ?
C67B C68B C69B C70B 55.8(13) . . . . ?
C68B C69B C70B C71B -58.0(14) . . . . ?
C69B C70B C71B C72B 61.7(16) . . . . ?
C68B C67B C72B C71B 62.4(18) . . . . ?
C70B C71B C72B C67B -61.7(19) . . . . ?
C18 O5 C73 C74 -78.3(3) . . . . ?
C18 O5 C73 C78 103.5(2) . . . . ?
C78 C73 C74 C75 -0.6(4) . . . . ?
O5 C73 C74 C75 -178.7(2) . . . . ?
C78 C73 C74 C85 177.7(2) . . . . ?
O5 C73 C74 C85 -0.4(3) . . . . ?
C73 C74 C75 C76 1.3(4) . . . . ?
C85 C74 C75 C76 -177.1(2) . . . . ?
C74 C75 C76 C77 -0.8(4) . . . . ?
C75 C76 C77 C78 -0.4(4) . . . . ?
C76 C77 C78 C73 1.0(4) . . . . ?
C76 C77 C78 C88 179.2(3) . . . . ?
C74 C73 C78 C77 -0.5(4) . . . . ?
O5 C73 C78 C77 177.6(2) . . . . ?
C74 C73 C78 C88 -178.7(2) . . . . ?
O5 C73 C78 C88 -0.6(3) . . . . ?
C7 O2 C79 C84 90.8(3) . . . . ?
C7 O2 C79 C80 -93.7(2) . . . . ?
C84 C79 C80 C81 0.9(4) . . . . ?
O2 C79 C80 C81 -174.4(2) . . . . ?
C84 C79 C80 C94 178.9(2) . . . . ?
O2 C79 C80 C94 3.7(3) . . . . ?
C79 C80 C81 C82 0.6(4) . . . . ?
C94 C80 C81 C82 -177.5(2) . . . . ?
C80 C81 C82 C83 -1.4(4) . . . . ?
C81 C82 C83 C84 0.9(4) . . . . ?
C80 C79 C84 C83 -1.3(4) . . . . ?
O2 C79 C84 C83 173.8(2) . . . . ?
C80 C79 C84 C91 178.6(2) . . . . ?
O2 C79 C84 C91 -6.2(3) . . . . ?
C82 C83 C84 C79 0.4(4) . . . . ?
C82 C83 C84 C91 -179.6(2) . . . . ?
C73 C74 C85 C86 -104.5(3) . . . . ?
C75 C74 C85 C86 73.8(3) . . . . ?
C73 C74 C85 C87 130.8(3) . . . . ?
C75 C74 C85 C87 -50.9(3) . . . . ?
C77 C78 C88 C89 -53.2(9) . . . . ?
C73 C78 C88 C89 124.9(8) . . . . ?
C77 C78 C88 C90 69.8(6) . . . . ?
C73 C78 C88 C90 -112.0(6) . . . . ?
C79 C84 C91 C92 -155.6(13) . . . . ?
C83 C84 C91 C92 24.3(13) . . . . ?
C79 C84 C91 C93 92.2(11) . . . . ?
C83 C84 C91 C93 -87.8(10) . . . . ?
C81 C80 C94 C95 -43.2(10) . . . . ?
C79 C80 C94 C95 138.8(10) . . . . ?
C81 C80 C94 C96 86.5(6) . . . . ?
C79 C80 C94 C96 -91.5(6) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.350
_refine_diff_density_min -0.312
_refine_diff_density_rms 0.053
_database_code_depnum_ccdc_archive 'CCDC 952112'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_mj06qr
_audit_creation_method SHELXL-2012
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C60 H62 N2 O6, 0.89(C H2 Cl2)'
_chemical_formula_sum 'C61 H64 Cl2 N2 O6'
_chemical_formula_weight 992.04
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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 13.495(3)
_cell_length_b 14.896(3)
_cell_length_c 26.835(5)
_cell_angle_alpha 90
_cell_angle_beta 99.08(3)
_cell_angle_gamma 90
_cell_volume 5326.8(19)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 14693
_cell_measurement_theta_min 3.0326
_cell_measurement_theta_max 27.5156
_exptl_crystal_description prism
_exptl_crystal_colour red
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.237
_exptl_crystal_F_000 2104
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max .36
_exptl_crystal_size_mid .32
_exptl_crystal_size_min .26
_exptl_absorpt_coefficient_mu 0.175
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min .974
_exptl_absorpt_correction_T_max .981
_exptl_absorpt_process_details ?
_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
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number 31594
_diffrn_reflns_av_unetI/netI 0.0617
_diffrn_reflns_av_R_equivalents 0.0678
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 3.057
_diffrn_reflns_theta_max 23.256
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.792
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.792
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.792
_reflns_number_total 7622
_reflns_number_gt 6540
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics ?
_computing_publication_material 'SHELXL-2012 (Sheldrick, 2012)'
_refine_special_details
;
Despite extremely hard efforts only few crystals suitable for X-ray
investigation
could be obtained of this compound. Disorder of the i-propyl groups
and one N-hexyl
substituent requested a number of suitable restraints to keep distances and
thermal ellipsoids at reasonable values. Interestingly the central scaffold
of the molecule seems not to be disordered and thus the observed twist angle
of the central C6 unit deserves special attention in comparison
with similar compounds.
?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+7.6166P]
where P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 7622
_refine_ls_number_parameters 688
_refine_ls_number_restraints 128
_refine_ls_R_factor_all 0.1537
_refine_ls_R_factor_gt 0.1354
_refine_ls_wR_factor_ref 0.2485
_refine_ls_wR_factor_gt 0.2393
_refine_ls_goodness_of_fit_ref 1.326
_refine_ls_restrained_S_all 1.329
_refine_ls_shift/su_max 0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2045(4) 0.6708(4) 0.52267(19) 0.0519(14) Uani 1 1 d . . . . .
C2 C 0.1332(4) 0.7038(4) 0.4833(2) 0.0582(15) Uani 1 1 d . . . . .
H2 H 0.1541 0.7401 0.4588 0.070 Uiso 1 1 calc R U . . .
C3 C 0.0337(4) 0.6838(4) 0.48022(19) 0.0541(14) Uani 1 1 d . . . C .
C4 C -0.0384(5) 0.7201(5) 0.4380(2) 0.0694(17) Uani 1 1 d . . . . .
C5 C -0.1744(5) 0.6367(4) 0.4687(2) 0.0634(16) Uani 1 1 d . . . . .
C6 C -0.1017(4) 0.6055(4) 0.5115(2) 0.0569(14) Uani 1 1 d . . . C .
C7 C -0.1315(4) 0.5501(4) 0.5469(2) 0.0634(16) Uani 1 1 d . . . . .
H7 H -0.1974 0.5295 0.5422 0.076 Uiso 1 1 calc R U . C .
C8 C -0.0665(4) 0.5238(4) 0.5894(2) 0.0612(15) Uani 1 1 d . . . C .
H8 H -0.0905 0.4869 0.6128 0.073 Uiso 1 1 calc R U . . .
C9 C 0.0341(4) 0.5507(3) 0.59859(18) 0.0463(13) Uani 1 1 d . . . . .
C10 C 0.1012(4) 0.5337(3) 0.64637(18) 0.0464(13) Uani 1 1 d . . . C .
C11 C 0.0697(4) 0.5042(4) 0.69081(19) 0.0532(14) Uani 1 1 d . . . . .
C12 C 0.1373(4) 0.4887(4) 0.7340(2) 0.0605(15) Uani 1 1 d . . . C .
H12 H 0.1130 0.4736 0.7635 0.073 Uiso 1 1 calc R U . . .
C13 C 0.2385(4) 0.4947(4) 0.73520(19) 0.0548(14) Uani 1 1 d . . . . .
C14 C 0.3086(4) 0.4684(4) 0.7813(2) 0.0621(15) Uani 1 1 d . . . C .
C15 C 0.4517(5) 0.4968(4) 0.7366(2) 0.0669(16) Uani 1 1 d . . . C .
C16 C 0.3801(4) 0.5260(4) 0.6920(2) 0.0544(14) Uani 1 1 d . . . . .
C17 C 0.4155(4) 0.5531(4) 0.6495(2) 0.0646(16) Uani 1 1 d . . . C .
H17 H 0.4842 0.5523 0.6489 0.077 Uiso 1 1 calc R U . . .
C18 C 0.3503(4) 0.5819(4) 0.6071(2) 0.0604(15) Uani 1 1 d . . . . .
H18 H 0.3771 0.6010 0.5790 0.072 Uiso 1 1 calc R U . C .
C19 C 0.2464(4) 0.5834(3) 0.60487(19) 0.0499(13) Uani 1 1 d . . . C .
C20 C 0.1769(4) 0.6183(3) 0.56167(18) 0.0466(13) Uani 1 1 d . . . . .
C21 C 0.2751(4) 0.5236(4) 0.69112(19) 0.0519(13) Uani 1 1 d . . . C .
C22 C 0.2062(4) 0.5479(3) 0.64742(18) 0.0468(13) Uani 1 1 d . . . . .
C23 C 0.0715(4) 0.5997(3) 0.55944(17) 0.0457(12) Uani 1 1 d . . . C .
C24 C 0.0013(4) 0.6288(3) 0.51744(19) 0.0524(14) Uani 1 1 d . . . . .
C25 C 0.3346(4) 0.7518(4) 0.4902(2) 0.0563(14) Uani 1 1 d . . . . .
C26 C 0.3402(5) 0.8405(4) 0.5042(2) 0.0638(16) Uani 1 1 d . . . . .
C27 C 0.3794(5) 0.8998(4) 0.4728(3) 0.085(2) Uani 1 1 d . . . . .
H27 H 0.3858 0.9602 0.4814 0.102 Uiso 1 1 calc R U . . .
C28 C 0.4091(5) 0.8703(5) 0.4286(3) 0.089(2) Uani 1 1 d . . . . .
H28 H 0.4344 0.9111 0.4076 0.107 Uiso 1 1 calc R U . A .
C29 C 0.4017(5) 0.7812(5) 0.4156(2) 0.0789(19) Uani 1 1 d . . . . .
H29 H 0.4220 0.7625 0.3857 0.095 Uiso 1 1 calc R U . . .
C30 C 0.3646(4) 0.7188(4) 0.4459(2) 0.0638(16) Uani 1 1 d . . . . .
C48 C -0.2151(6) 0.6403(6) 0.6884(3) 0.114(3) Uani 1 1 d D . . . .
H48A H -0.2737 0.6260 0.7030 0.171 Uiso 1 1 calc R U . . .
H48B H -0.2080 0.5975 0.6624 0.171 Uiso 1 1 calc R U . . .
H48C H -0.2219 0.6995 0.6741 0.171 Uiso 1 1 calc R U . . .
C46 C -0.1236(5) 0.6368(5) 0.7286(3) 0.087(2) Uani 1 1 d D . . . .
H46 H -0.0646 0.6433 0.7118 0.104 Uiso 1 1 calc R U . . .
C47 C -0.1233(7) 0.7148(6) 0.7650(3) 0.131(3) Uani 1 1 d . . . . .
H47A H -0.0647 0.7114 0.7903 0.197 Uiso 1 1 calc R U . . .
H47B H -0.1823 0.7122 0.7808 0.197 Uiso 1 1 calc R U . . .
H47C H -0.1227 0.7703 0.7468 0.197 Uiso 1 1 calc R U . . .
C33 C 0.3918(17) 0.869(2) 0.5962(8) 0.103(5) Uani 0.45(3) 1 d D U P A 1
H33A H 0.4478 0.9028 0.5879 0.154 Uiso 0.45(3) 1 calc R U P A 1
H33B H 0.4115 0.8081 0.6031 0.154 Uiso 0.45(3) 1 calc R U P A 1
H33C H 0.3701 0.8952 0.6254 0.154 Uiso 0.45(3) 1 calc R U P A 1
C31 C 0.3087(6) 0.8723(5) 0.5532(3) 0.086(2) Uani 0.5 1 d D . P A 1
H31 H 0.2578 0.8298 0.5610 0.103 Uiso 0.5 1 calc R U P A 1
C34 C 0.256(2) 0.9664(19) 0.5460(10) 0.109(5) Uani 0.45(3) 1 d . U P A 1
H34A H 0.3043 1.0111 0.5404 0.164 Uiso 0.45(3) 1 calc R U P A 1
H34B H 0.2281 0.9813 0.5757 0.164 Uiso 0.45(3) 1 calc R U P A 1
H34C H 0.2033 0.9642 0.5174 0.164 Uiso 0.45(3) 1 calc R U P A 1
C34B C 0.2211(16) 0.9328(16) 0.5446(8) 0.109(5) Uani 0.55(3) 1 d D U P A 2
H34D H 0.1656 0.9022 0.5250 0.164 Uiso 0.55(3) 1 calc R U P A 2
H34E H 0.2375 0.9852 0.5268 0.164 Uiso 0.55(3) 1 calc R U P A 2
H34F H 0.2033 0.9502 0.5765 0.164 Uiso 0.55(3) 1 calc R U P A 2
C31B C 0.3087(6) 0.8723(5) 0.5532(3) 0.086(2) Uani 0.5 1 d D . P A 2
H31B H 0.2891 0.8191 0.5709 0.103 Uiso 0.5 1 calc R U P A 2
C33B C 0.4004(14) 0.9167(19) 0.5881(7) 0.103(5) Uani 0.55(3) 1 d . . P A 2
H33D H 0.3792 0.9380 0.6185 0.154 Uiso 0.55(3) 1 calc R U P A 2
H33E H 0.4251 0.9662 0.5707 0.154 Uiso 0.55(3) 1 calc R U P A 2
H33F H 0.4527 0.8731 0.5964 0.154 Uiso 0.55(3) 1 calc R U P A 2
C35 C 0.2984(17) 0.6012(15) 0.3863(8) 0.115(7) Uani 0.54(3) 1 d D U P A 1
H35A H 0.3228 0.6336 0.3597 0.173 Uiso 0.54(3) 1 calc R U P A 1
H35B H 0.2305 0.6190 0.3878 0.173 Uiso 0.54(3) 1 calc R U P A 1
H35C H 0.3003 0.5379 0.3796 0.173 Uiso 0.54(3) 1 calc R U P A 1
C32 C 0.3601(6) 0.6206(5) 0.4333(3) 0.084(2) Uani 0.5 1 d D . P A 1
H32 H 0.3301 0.5901 0.4597 0.101 Uiso 0.5 1 calc R U P A 1
C36 C 0.4719(15) 0.5839(14) 0.4366(9) 0.109(5) Uani 0.54(3) 1 d . U P A 1
H36A H 0.5033 0.6118 0.4109 0.163 Uiso 0.54(3) 1 calc R U P A 1
H36B H 0.4704 0.5200 0.4317 0.163 Uiso 0.54(3) 1 calc R U P A 1
H36C H 0.5092 0.5977 0.4692 0.163 Uiso 0.54(3) 1 calc R U P A 1
C36B C 0.4418(18) 0.5671(16) 0.4577(11) 0.109(5) Uani 0.46(3) 1 d D U P A 2
H36D H 0.4365 0.5075 0.4440 0.163 Uiso 0.46(3) 1 calc R U P A 2
H36E H 0.4396 0.5646 0.4932 0.163 Uiso 0.46(3) 1 calc R U P A 2
H36F H 0.5041 0.5935 0.4522 0.163 Uiso 0.46(3) 1 calc R U P A 2
C32B C 0.3601(6) 0.6206(5) 0.4333(3) 0.084(2) Uani 0.5 1 d D . P A 2
H32B H 0.3001 0.5976 0.4454 0.101 Uiso 0.5 1 calc R U P A 2
C35B C 0.342(2) 0.6019(16) 0.3728(8) 0.106(8) Uani 0.46(3) 1 d . U P A 2
H35D H 0.3240 0.5402 0.3665 0.159 Uiso 0.46(3) 1 calc R U P A 2
H35E H 0.4030 0.6146 0.3597 0.159 Uiso 0.46(3) 1 calc R U P A 2
H35F H 0.2894 0.6400 0.3566 0.159 Uiso 0.46(3) 1 calc R U P A 2
C45 C -0.0922(8) 0.2446(7) 0.7040(4) 0.164(4) Uani 1 1 d D U . B 1
H45A H -0.1334 0.2744 0.6764 0.246 Uiso 1 1 calc R U . B 1
H45B H -0.1337 0.2218 0.7270 0.246 Uiso 1 1 calc R U . B 1
H45C H -0.0571 0.1959 0.6912 0.246 Uiso 1 1 calc R U . B 1
C43 C -0.0186(6) 0.3093(6) 0.7307(3) 0.102(2) Uani 1 1 d D U . B 1
H43 H 0.0181 0.3351 0.7054 0.123 Uiso 1 1 calc R U . B 1
C44 C 0.0584(8) 0.2610(7) 0.7695(4) 0.167(4) Uani 1 1 d . U . B 1
H44A H 0.0243 0.2290 0.7928 0.250 Uiso 1 1 calc R U . B 1
H44B H 0.1032 0.3042 0.7875 0.250 Uiso 1 1 calc R U . B 1
H44C H 0.0960 0.2194 0.7525 0.250 Uiso 1 1 calc R U . B 1
C37 C -0.0699(4) 0.4729(5) 0.7350(2) 0.0694(18) Uani 1 1 d D . . . .
C38 C -0.1169(4) 0.5466(5) 0.7539(2) 0.0761(19) Uani 1 1 d D . . C .
C39 C -0.1641(6) 0.5280(7) 0.7956(3) 0.110(3) Uani 1 1 d . . . . .
H39 H -0.1973 0.5739 0.8097 0.132 Uiso 1 1 calc R U . C .
C40 C -0.1624(7) 0.4443(9) 0.8159(3) 0.126(4) Uani 1 1 d . . . C .
H40 H -0.1943 0.4345 0.8437 0.151 Uiso 1 1 calc R U . . .
C41 C -0.1151(6) 0.3745(7) 0.7967(3) 0.109(3) Uani 1 1 d . . . . .
H41 H -0.1150 0.3181 0.8117 0.131 Uiso 1 1 calc R U . C .
C42 C -0.0666(5) 0.3866(5) 0.7545(3) 0.087(2) Uani 1 1 d . . . B .
N1 N 0.4104(3) 0.4692(3) 0.77946(17) 0.0619(13) Uani 1 1 d . . . . .
C49 C 0.4824(5) 0.4389(4) 0.8239(2) 0.0709(17) Uani 1 1 d . . . C .
H49 H 0.5491 0.4421 0.8139 0.085 Uiso 1 1 calc R U . . .
C50 C 0.4852(6) 0.5015(5) 0.8686(2) 0.097(2) Uani 1 1 d . . . . .
H50A H 0.4195 0.5034 0.8788 0.117 Uiso 1 1 calc R U . C .
H50B H 0.5018 0.5617 0.8588 0.117 Uiso 1 1 calc R U . . .
C51 C 0.5630(7) 0.4701(7) 0.9131(3) 0.126(3) Uani 1 1 d . . . C .
H51A H 0.6297 0.4755 0.9042 0.151 Uiso 1 1 calc R U . . .
H51B H 0.5598 0.5084 0.9420 0.151 Uiso 1 1 calc R U . . .
C52 C 0.5452(7) 0.3735(9) 0.9272(4) 0.141(4) Uani 1 1 d . . . . .
H52A H 0.4806 0.3684 0.9384 0.169 Uiso 1 1 calc R U . C .
H52B H 0.5967 0.3549 0.9547 0.169 Uiso 1 1 calc R U . . .
C53 C 0.5476(6) 0.3133(6) 0.8818(3) 0.121(3) Uani 1 1 d . . . C .
H53A H 0.5365 0.2516 0.8910 0.145 Uiso 1 1 calc R U . . .
H53B H 0.6133 0.3168 0.8715 0.145 Uiso 1 1 calc R U . . .
C54 C 0.4669(6) 0.3411(5) 0.8373(3) 0.098(2) Uani 1 1 d . . . . .
H54A H 0.4714 0.3032 0.8083 0.118 Uiso 1 1 calc R U . C .
H54B H 0.4007 0.3335 0.8465 0.118 Uiso 1 1 calc R U . . .
N2 N -0.1387(4) 0.6965(4) 0.43544(16) 0.0687(14) Uani 0.5 1 d . . P C 1
C55 C -0.2146(6) 0.7325(5) 0.3937(3) 0.094(2) Uani 0.590(9) 1 d . U P C 1
H55 H -0.2766 0.7012 0.3980 0.112 Uiso 0.590(9) 1 calc R U P C 1
C56 C -0.1966(9) 0.7044(9) 0.3418(5) 0.064(3) Uani 0.590(9) 1 d . U P C 1
H56A H -0.1789 0.6413 0.3413 0.077 Uiso 0.590(9) 1 calc R U P C 1
H56B H -0.1430 0.7395 0.3312 0.077 Uiso 0.590(9) 1 calc R U P C 1
C57 C -0.3021(11) 0.7232(10) 0.3052(6) 0.080(3) Uani 0.590(9) 1 d . U P C 1
H57A H -0.2990 0.7034 0.2711 0.096 Uiso 0.590(9) 1 calc R U P C 1
H57B H -0.3567 0.6920 0.3174 0.096 Uiso 0.590(9) 1 calc R U P C 1
C58 C -0.3167(12) 0.8226(10) 0.3069(5) 0.096(3) Uani 0.590(9) 1 d . . P C 1
H58A H -0.3760 0.8390 0.2833 0.115 Uiso 0.590(9) 1 calc R U P C 1
H58B H -0.2595 0.8524 0.2964 0.115 Uiso 0.590(9) 1 calc R U P C 1
C59 C -0.3293(13) 0.8565(12) 0.3625(6) 0.091(4) Uani 0.590(9) 1 d . U P C 1
H59A H -0.3321 0.9215 0.3635 0.109 Uiso 0.590(9) 1 calc R U P C 1
H59B H -0.3905 0.8327 0.3721 0.109 Uiso 0.590(9) 1 calc R U P C 1
C60 C -0.2381(10) 0.8222(8) 0.3982(5) 0.080(3) Uani 0.590(9) 1 d . U P C 1
H60A H -0.1804 0.8577 0.3928 0.096 Uiso 0.590(9) 1 calc R U P C 1
H60B H -0.2491 0.8329 0.4326 0.096 Uiso 0.590(9) 1 calc R U P C 1
N2B N -0.1387(4) 0.6965(4) 0.43544(16) 0.0687(14) Uani 0.5 1 d . . P C 2
C55B C -0.2146(6) 0.7325(5) 0.3937(3) 0.094(2) Uani 0.410(9) 1 d . U P C 2
H55B H -0.1705 0.7782 0.3828 0.112 Uiso 0.410(9) 1 calc R U P C 2
C56B C -0.2339(14) 0.6889(13) 0.3478(7) 0.064(3) Uani 0.410(9) 1 d . U P C 2
H56C H -0.2834 0.6426 0.3503 0.077 Uiso 0.410(9) 1 calc R U P C 2
H56D H -0.1727 0.6590 0.3423 0.077 Uiso 0.410(9) 1 calc R U P C 2
C57B C -0.2724(16) 0.7474(16) 0.2997(8) 0.080(3) Uani 0.410(9) 1 d . U P C 2
H57C H -0.2249 0.7939 0.2944 0.096 Uiso 0.410(9) 1 calc R U P C 2
H57D H -0.2880 0.7110 0.2695 0.096 Uiso 0.410(9) 1 calc R U P C 2
C58B C -0.3693(16) 0.7870(15) 0.3169(8) 0.096(3) Uani 0.410(9) 1 d . U P C 2
H58C H -0.4057 0.8213 0.2892 0.115 Uiso 0.410(9) 1 calc R U P C 2
H58D H -0.4119 0.7375 0.3238 0.115 Uiso 0.410(9) 1 calc R U P C 2
C59B C -0.354(2) 0.8344(18) 0.3538(10) 0.091(4) Uani 0.410(9) 1 d . U P C 2
H59C H -0.4193 0.8539 0.3608 0.109 Uiso 0.410(9) 1 calc R U P C 2
H59D H -0.3199 0.8876 0.3445 0.109 Uiso 0.410(9) 1 calc R U P C 2
C60B C -0.2917(15) 0.7974(13) 0.4064(6) 0.080(3) Uani 0.410(9) 1 d . U P C 2
H60C H -0.2592 0.8469 0.4261 0.096 Uiso 0.410(9) 1 calc R U P C 2
H60D H -0.3365 0.7677 0.4261 0.096 Uiso 0.410(9) 1 calc R U P C 2
O1 O 0.3042(3) 0.6886(3) 0.52400(13) 0.0651(11) Uani 1 1 d . . . . .
O2 O -0.0307(3) 0.4896(3) 0.68975(13) 0.0641(11) Uani 1 1 d . . . C .
O3 O -0.0119(4) 0.7702(4) 0.40660(18) 0.1029(17) Uani 1 1 d . . . C .
O4 O -0.2620(3) 0.6148(3) 0.46280(17) 0.0911(15) Uani 1 1 d . . . C .
O5 O 0.2760(3) 0.4456(4) 0.81928(15) 0.0911(15) Uani 1 1 d . . . . .
O6 O 0.5413(3) 0.4961(4) 0.73687(17) 0.1023(17) Uani 1 1 d . . . . .
Cl1 Cl 0.5879(2) 0.6897(2) 0.58271(10) 0.1421(14) Uani 0.890(6) 1 d . . P . .
C90 C 0.6104(6) 0.7509(6) 0.5312(3) 0.109(3) Uani 0.890(6) 1 d . U P . .
H90A H 0.6424 0.7120 0.5094 0.131 Uiso 0.890(6) 1 calc R U P . .
H90B H 0.5466 0.7698 0.5123 0.131 Uiso 0.890(6) 1 calc R U P . .
Cl2 Cl 0.6814(3) 0.8403(2) 0.54471(12) 0.1756(18) Uani 0.890(6) 1 d . U P . .
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
C1 0.052(3) 0.056(3) 0.049(3) 0.007(3) 0.014(3) -0.004(3)
C2 0.064(4) 0.062(4) 0.052(3) 0.008(3) 0.019(3) -0.004(3)
C3 0.055(3) 0.061(4) 0.046(3) 0.000(3) 0.007(3) 0.002(3)
C4 0.069(4) 0.085(5) 0.055(4) 0.008(4) 0.008(3) 0.001(4)
C5 0.067(4) 0.072(4) 0.050(4) -0.006(3) 0.004(3) 0.007(3)
C6 0.056(3) 0.064(4) 0.053(3) -0.006(3) 0.014(3) -0.004(3)
C7 0.051(3) 0.079(4) 0.060(4) -0.006(3) 0.007(3) -0.015(3)
C8 0.060(4) 0.073(4) 0.052(3) 0.001(3) 0.010(3) -0.017(3)
C9 0.053(3) 0.039(3) 0.048(3) -0.005(2) 0.012(3) -0.009(2)
C10 0.046(3) 0.050(3) 0.045(3) 0.000(2) 0.012(2) 0.001(2)
C11 0.046(3) 0.070(4) 0.045(3) 0.002(3) 0.014(3) -0.006(3)
C12 0.062(4) 0.073(4) 0.051(3) 0.006(3) 0.022(3) -0.003(3)
C13 0.056(4) 0.055(4) 0.054(3) 0.005(3) 0.012(3) 0.002(3)
C14 0.058(4) 0.071(4) 0.056(4) 0.006(3) 0.005(3) 0.007(3)
C15 0.062(4) 0.079(4) 0.060(4) 0.008(3) 0.009(3) 0.002(3)
C16 0.054(3) 0.054(3) 0.056(3) 0.004(3) 0.011(3) 0.002(3)
C17 0.042(3) 0.090(5) 0.063(4) 0.012(3) 0.012(3) 0.000(3)
C18 0.047(3) 0.076(4) 0.060(4) 0.019(3) 0.014(3) -0.001(3)
C19 0.054(3) 0.049(3) 0.049(3) 0.000(3) 0.016(3) -0.006(3)
C20 0.045(3) 0.047(3) 0.050(3) -0.001(3) 0.015(3) 0.002(2)
C21 0.052(3) 0.052(3) 0.053(3) 0.001(3) 0.015(3) -0.003(3)
C22 0.051(3) 0.046(3) 0.046(3) 0.002(2) 0.012(3) 0.003(2)
C23 0.055(3) 0.046(3) 0.036(3) -0.004(2) 0.006(2) -0.001(3)
C24 0.065(4) 0.048(3) 0.047(3) -0.005(3) 0.018(3) -0.002(3)
C25 0.055(3) 0.063(4) 0.053(3) 0.012(3) 0.016(3) -0.005(3)
C26 0.080(4) 0.058(4) 0.055(4) 0.009(3) 0.017(3) -0.003(3)
C27 0.115(6) 0.058(4) 0.086(5) 0.003(4) 0.031(4) -0.020(4)
C28 0.111(6) 0.086(5) 0.077(5) 0.016(4) 0.034(4) -0.025(4)
C29 0.095(5) 0.087(5) 0.062(4) 0.003(4) 0.034(4) -0.012(4)
C30 0.070(4) 0.061(4) 0.064(4) 0.000(3) 0.022(3) -0.010(3)
C48 0.123(7) 0.115(7) 0.092(6) -0.014(5) -0.021(5) 0.031(5)
C46 0.084(5) 0.099(6) 0.080(5) -0.012(4) 0.022(4) 0.010(4)
C47 0.136(8) 0.132(8) 0.130(7) -0.046(6) 0.035(6) -0.003(6)
C33 0.115(6) 0.107(10) 0.088(6) -0.015(8) 0.022(5) 0.007(8)
C31 0.110(6) 0.083(5) 0.069(4) -0.008(4) 0.030(4) -0.002(4)
C34 0.109(8) 0.116(8) 0.109(6) -0.017(6) 0.033(6) 0.005(6)
C34B 0.109(8) 0.116(8) 0.109(6) -0.017(6) 0.033(6) 0.005(6)
C31B 0.110(6) 0.083(5) 0.069(4) -0.008(4) 0.030(4) -0.002(4)
C33B 0.115(6) 0.107(10) 0.088(6) -0.015(8) 0.022(5) 0.007(8)
C35 0.113(10) 0.118(10) 0.117(10) -0.009(8) 0.022(8) -0.021(8)
C32 0.089(5) 0.081(5) 0.087(5) -0.011(4) 0.030(4) -0.012(4)
C36 0.116(7) 0.096(6) 0.114(8) -0.011(6) 0.021(6) 0.009(5)
C36B 0.116(7) 0.096(6) 0.114(8) -0.011(6) 0.021(6) 0.009(5)
C32B 0.089(5) 0.081(5) 0.087(5) -0.011(4) 0.030(4) -0.012(4)
C35B 0.109(11) 0.104(11) 0.103(10) -0.025(8) 0.011(8) -0.004(9)
C45 0.154(8) 0.165(9) 0.184(10) -0.039(8) 0.059(7) -0.026(7)
C43 0.100(4) 0.101(4) 0.112(4) 0.019(3) 0.033(3) 0.001(3)
C44 0.152(8) 0.156(9) 0.193(9) 0.061(8) 0.029(7) 0.047(7)
C37 0.044(3) 0.116(6) 0.053(4) 0.012(4) 0.020(3) 0.004(3)
C38 0.055(4) 0.123(6) 0.055(4) -0.001(4) 0.021(3) 0.006(4)
C39 0.097(6) 0.164(9) 0.078(5) 0.006(6) 0.038(5) 0.029(6)
C40 0.097(6) 0.195(11) 0.098(6) 0.033(7) 0.056(5) 0.020(7)
C41 0.082(5) 0.151(8) 0.099(6) 0.064(6) 0.030(5) 0.006(5)
C42 0.076(5) 0.111(6) 0.078(5) 0.039(4) 0.028(4) 0.007(4)
N1 0.054(3) 0.076(3) 0.053(3) 0.010(2) 0.002(2) 0.007(2)
C49 0.071(4) 0.077(5) 0.061(4) 0.015(3) 0.001(3) 0.001(3)
C50 0.106(6) 0.107(6) 0.074(5) -0.009(4) -0.003(4) 0.004(5)
C51 0.126(7) 0.163(9) 0.072(5) -0.004(6) -0.032(5) 0.011(7)
C52 0.117(7) 0.207(12) 0.095(7) 0.058(8) 0.002(6) 0.044(8)
C53 0.114(7) 0.130(8) 0.116(7) 0.053(6) 0.007(6) 0.024(6)
C54 0.102(6) 0.097(6) 0.091(5) 0.021(4) 0.000(4) 0.020(5)
N2 0.061(3) 0.097(4) 0.043(3) 0.007(3) -0.005(2) 0.014(3)
C55 0.093(3) 0.099(4) 0.089(3) -0.002(3) 0.012(3) 0.014(3)
C56 0.066(4) 0.062(4) 0.064(3) -0.001(3) 0.009(3) 0.002(3)
C57 0.082(5) 0.083(5) 0.074(4) 0.002(3) 0.007(3) -0.004(3)
C58 0.091(5) 0.095(5) 0.097(5) 0.014(4) 0.005(4) -0.002(4)
C59 0.090(5) 0.085(5) 0.094(5) 0.000(3) 0.007(3) 0.008(3)
C60 0.082(4) 0.078(4) 0.078(4) -0.002(3) 0.009(3) 0.003(3)
N2B 0.061(3) 0.097(4) 0.043(3) 0.007(3) -0.005(2) 0.014(3)
C55B 0.093(3) 0.099(4) 0.089(3) -0.002(3) 0.012(3) 0.014(3)
C56B 0.066(4) 0.062(4) 0.064(3) -0.001(3) 0.009(3) 0.002(3)
C57B 0.082(5) 0.083(5) 0.074(4) 0.002(3) 0.007(3) -0.004(3)
C58B 0.091(5) 0.095(5) 0.097(5) 0.014(4) 0.005(4) -0.002(4)
C59B 0.090(5) 0.085(5) 0.094(5) 0.000(3) 0.007(3) 0.008(3)
C60B 0.082(4) 0.078(4) 0.078(4) -0.002(3) 0.009(3) 0.003(3)
O1 0.050(2) 0.084(3) 0.064(2) 0.025(2) 0.0184(19) -0.005(2)
O2 0.048(2) 0.095(3) 0.053(2) 0.012(2) 0.0204(18) 0.000(2)
O3 0.091(3) 0.131(4) 0.083(3) 0.052(3) 0.003(3) -0.002(3)
O4 0.054(3) 0.117(4) 0.094(3) 0.005(3) -0.014(2) -0.011(3)
O5 0.076(3) 0.144(4) 0.055(3) 0.028(3) 0.018(2) 0.007(3)
O6 0.052(3) 0.169(5) 0.086(3) 0.040(3) 0.011(2) 0.006(3)
Cl1 0.177(3) 0.130(2) 0.118(2) 0.0246(17) 0.0194(19) -0.033(2)
C90 0.094(6) 0.141(7) 0.096(6) -0.012(6) 0.026(5) -0.024(6)
Cl2 0.192(3) 0.185(3) 0.151(3) -0.006(2) 0.031(2) -0.105(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
C1 O1 1.367(6) . ?
C1 C2 1.401(7) . ?
C1 C20 1.403(7) . ?
C2 C3 1.365(7) . ?
C3 C24 1.414(7) . ?
C3 C4 1.476(8) . ?
C4 O3 1.220(7) . ?
C4 N2 1.389(7) . ?
C5 O4 1.212(7) . ?
C5 N2 1.399(7) . ?
C5 C6 1.463(8) . ?
C6 C7 1.366(7) . ?
C6 C24 1.417(7) . ?
C7 C8 1.382(7) . ?
C8 C9 1.399(7) . ?
C9 C23 1.435(6) . ?
C9 C10 1.471(7) . ?
C10 C11 1.399(7) . ?
C10 C22 1.428(7) . ?
C11 O2 1.368(6) . ?
C11 C12 1.376(7) . ?
C12 C13 1.364(7) . ?
C13 C21 1.418(7) . ?
C13 C14 1.486(7) . ?
C14 O5 1.220(6) . ?
C14 N1 1.383(7) . ?
C15 O6 1.208(6) . ?
C15 N1 1.416(7) . ?
C15 C16 1.480(8) . ?
C16 C17 1.365(7) . ?
C16 C21 1.414(7) . ?
C17 C18 1.393(7) . ?
C18 C19 1.395(7) . ?
C19 C22 1.439(7) . ?
C19 C20 1.466(7) . ?
C20 C23 1.440(7) . ?
C21 C22 1.423(7) . ?
C23 C24 1.421(7) . ?
C25 C26 1.373(8) . ?
C25 C30 1.403(7) . ?
C25 O1 1.412(6) . ?
C26 C27 1.384(8) . ?
C26 C31 1.520(8) . ?
C27 C28 1.382(9) . ?
C28 C29 1.372(9) . ?
C29 C30 1.381(8) . ?
C30 C32 1.501(8) . ?
C48 C46 1.508(8) . ?
C46 C38 1.502(9) . ?
C46 C47 1.517(9) . ?
C33 C31 1.477(16) . ?
C31 C34 1.57(2) . ?
C35 C32 1.428(16) . ?
C32 C36 1.59(2) . ?
C45 C43 1.485(10) . ?
C43 C42 1.512(10) . ?
C43 C44 1.530(11) . ?
C37 C42 1.386(9) . ?
C37 C38 1.402(8) . ?
C37 O2 1.420(6) . ?
C38 C39 1.399(9) . ?
C39 C40 1.359(12) . ?
C40 C41 1.364(12) . ?
C41 C42 1.406(9) . ?
N1 C49 1.484(7) . ?
C49 C50 1.514(9) . ?
C49 C54 1.524(9) . ?
C50 C51 1.533(9) . ?
C51 C52 1.516(12) . ?
C52 C53 1.517(12) . ?
C53 C54 1.540(9) . ?
N2 C55 1.493(8) . ?
C55 C60 1.383(13) . ?
C55 C56 1.513(14) . ?
C56 C57 1.621(19) . ?
C57 C58 1.50(2) . ?
C58 C59 1.61(2) . ?
C59 C60 1.52(2) . ?
C56B C57B 1.58(3) . ?
C57B C58B 1.57(3) . ?
C58B C59B 1.21(3) . ?
C59B C60B 1.62(3) . ?
Cl1 C90 1.723(9) . ?
C90 Cl2 1.648(9) . ?
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 C1 C2 120.5(4) . . ?
O1 C1 C20 117.7(5) . . ?
C2 C1 C20 121.8(5) . . ?
C3 C2 C1 121.4(5) . . ?
C2 C3 C24 119.6(5) . . ?
C2 C3 C4 119.4(5) . . ?
C24 C3 C4 121.0(5) . . ?
O3 C4 N2 120.7(6) . . ?
O3 C4 C3 121.6(6) . . ?
N2 C4 C3 117.6(5) . . ?
O4 C5 N2 121.0(6) . . ?
O4 C5 C6 122.4(6) . . ?
N2 C5 C6 116.5(5) . . ?
C7 C6 C24 117.5(5) . . ?
C7 C6 C5 120.2(5) . . ?
C24 C6 C5 122.3(5) . . ?
C6 C7 C8 121.8(5) . . ?
C7 C8 C9 122.4(5) . . ?
C8 C9 C23 117.5(5) . . ?
C8 C9 C10 123.5(5) . . ?
C23 C9 C10 119.1(4) . . ?
C11 C10 C22 117.6(5) . . ?
C11 C10 C9 124.7(5) . . ?
C22 C10 C9 117.7(4) . . ?
O2 C11 C12 120.9(4) . . ?
O2 C11 C10 117.7(5) . . ?
C12 C11 C10 121.4(5) . . ?
C13 C12 C11 122.5(5) . . ?
C12 C13 C21 118.6(5) . . ?
C12 C13 C14 120.4(5) . . ?
C21 C13 C14 121.0(5) . . ?
O5 C14 N1 121.5(5) . . ?
O5 C14 C13 120.2(5) . . ?
N1 C14 C13 118.3(5) . . ?
O6 C15 N1 121.0(5) . . ?
O6 C15 C16 122.2(5) . . ?
N1 C15 C16 116.9(5) . . ?
C17 C16 C21 118.4(5) . . ?
C17 C16 C15 119.5(5) . . ?
C21 C16 C15 122.1(5) . . ?
C16 C17 C18 121.0(5) . . ?
C17 C18 C19 122.7(5) . . ?
C18 C19 C22 117.6(5) . . ?
C18 C19 C20 123.5(4) . . ?
C22 C19 C20 118.9(4) . . ?
C1 C20 C23 116.9(5) . . ?
C1 C20 C19 125.1(5) . . ?
C23 C20 C19 117.9(4) . . ?
C16 C21 C13 118.2(5) . . ?
C16 C21 C22 122.0(5) . . ?
C13 C21 C22 119.8(5) . . ?
C21 C22 C10 119.7(4) . . ?
C21 C22 C19 117.9(5) . . ?
C10 C22 C19 122.4(5) . . ?
C24 C23 C9 117.9(5) . . ?
C24 C23 C20 120.3(4) . . ?
C9 C23 C20 121.8(5) . . ?
C3 C24 C6 118.0(5) . . ?
C3 C24 C23 119.7(5) . . ?
C6 C24 C23 122.3(5) . . ?
C26 C25 C30 124.0(5) . . ?
C26 C25 O1 118.3(5) . . ?
C30 C25 O1 117.5(5) . . ?
C25 C26 C27 117.2(5) . . ?
C25 C26 C31 121.8(5) . . ?
C27 C26 C31 121.0(6) . . ?
C28 C27 C26 120.7(6) . . ?
C29 C28 C27 120.5(6) . . ?
C28 C29 C30 121.3(6) . . ?
C29 C30 C25 116.3(6) . . ?
C29 C30 C32 121.9(6) . . ?
C25 C30 C32 121.7(5) . . ?
C38 C46 C48 109.8(6) . . ?
C38 C46 C47 113.7(6) . . ?
C48 C46 C47 110.7(6) . . ?
C33 C31 C26 112.6(11) . . ?
C33 C31 C34 113.4(14) . . ?
C26 C31 C34 110.8(11) . . ?
C35 C32 C30 113.2(11) . . ?
C35 C32 C36 113.2(11) . . ?
C30 C32 C36 108.5(9) . . ?
C45 C43 C42 113.6(7) . . ?
C45 C43 C44 110.7(8) . . ?
C42 C43 C44 111.2(7) . . ?
C42 C37 C38 125.3(6) . . ?
C42 C37 O2 119.4(6) . . ?
C38 C37 O2 115.1(6) . . ?
C39 C38 C37 115.1(7) . . ?
C39 C38 C46 122.4(7) . . ?
C37 C38 C46 122.4(5) . . ?
C40 C39 C38 121.4(8) . . ?
C39 C40 C41 121.8(8) . . ?
C40 C41 C42 120.7(8) . . ?
C37 C42 C41 115.7(7) . . ?
C37 C42 C43 122.4(6) . . ?
C41 C42 C43 121.8(7) . . ?
C14 N1 C15 123.5(5) . . ?
C14 N1 C49 119.8(5) . . ?
C15 N1 C49 116.7(5) . . ?
N1 C49 C50 112.4(5) . . ?
N1 C49 C54 112.5(5) . . ?
C50 C49 C54 112.9(6) . . ?
C49 C50 C51 110.9(6) . . ?
C52 C51 C50 111.6(7) . . ?
C51 C52 C53 109.6(8) . . ?
C52 C53 C54 111.2(7) . . ?
C49 C54 C53 109.4(7) . . ?
C4 N2 C5 124.1(5) . . ?
C4 N2 C55 119.6(5) . . ?
C5 N2 C55 116.2(5) . . ?
C60 C55 N2 115.0(8) . . ?
C60 C55 C56 114.9(9) . . ?
N2 C55 C56 113.6(7) . . ?
C55 C56 C57 104.8(9) . . ?
C58 C57 C56 105.1(11) . . ?
C57 C58 C59 111.8(12) . . ?
C60 C59 C58 106.5(13) . . ?
C55 C60 C59 116.3(11) . . ?
C58B C57B C56B 98.6(16) . . ?
C59B C58B C57B 115(2) . . ?
C58B C59B C60B 121(2) . . ?
C1 O1 C25 119.8(4) . . ?
C11 O2 C37 120.8(4) . . ?
Cl2 C90 Cl1 114.9(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 C1 C2 C3 177.4(5) . . . . ?
C20 C1 C2 C3 -2.3(9) . . . . ?
C1 C2 C3 C24 0.2(8) . . . . ?
C1 C2 C3 C4 -179.8(5) . . . . ?
C2 C3 C4 O3 -2.7(9) . . . . ?
C24 C3 C4 O3 177.3(6) . . . . ?
C2 C3 C4 N2 178.5(5) . . . . ?
C24 C3 C4 N2 -1.5(8) . . . . ?
O4 C5 C6 C7 -0.5(9) . . . . ?
N2 C5 C6 C7 177.2(5) . . . . ?
O4 C5 C6 C24 177.8(6) . . . . ?
N2 C5 C6 C24 -4.5(8) . . . . ?
C24 C6 C7 C8 5.7(8) . . . . ?
C5 C6 C7 C8 -175.9(5) . . . . ?
C6 C7 C8 C9 -1.2(9) . . . . ?
C7 C8 C9 C23 -6.4(8) . . . . ?
C7 C8 C9 C10 171.7(5) . . . . ?
C8 C9 C10 C11 -12.2(8) . . . . ?
C23 C9 C10 C11 165.9(5) . . . . ?
C8 C9 C10 C22 167.5(5) . . . . ?
C23 C9 C10 C22 -14.4(7) . . . . ?
C22 C10 C11 O2 -179.3(5) . . . . ?
C9 C10 C11 O2 0.4(8) . . . . ?
C22 C10 C11 C12 -0.4(8) . . . . ?
C9 C10 C11 C12 179.2(5) . . . . ?
O2 C11 C12 C13 173.9(5) . . . . ?
C10 C11 C12 C13 -4.9(9) . . . . ?
C11 C12 C13 C21 4.2(9) . . . . ?
C11 C12 C13 C14 -173.8(5) . . . . ?
C12 C13 C14 O5 -3.7(9) . . . . ?
C21 C13 C14 O5 178.4(6) . . . . ?
C12 C13 C14 N1 175.1(5) . . . . ?
C21 C13 C14 N1 -2.7(8) . . . . ?
O6 C15 C16 C17 -0.1(10) . . . . ?
N1 C15 C16 C17 -179.8(5) . . . . ?
O6 C15 C16 C21 177.6(6) . . . . ?
N1 C15 C16 C21 -2.2(8) . . . . ?
C21 C16 C17 C18 3.1(9) . . . . ?
C15 C16 C17 C18 -179.2(6) . . . . ?
C16 C17 C18 C19 -1.2(10) . . . . ?
C17 C18 C19 C22 -4.0(8) . . . . ?
C17 C18 C19 C20 176.3(5) . . . . ?
O1 C1 C20 C23 -179.6(4) . . . . ?
C2 C1 C20 C23 0.1(8) . . . . ?
O1 C1 C20 C19 2.1(8) . . . . ?
C2 C1 C20 C19 -178.2(5) . . . . ?
C18 C19 C20 C1 -14.1(8) . . . . ?
C22 C19 C20 C1 166.3(5) . . . . ?
C18 C19 C20 C23 167.7(5) . . . . ?
C22 C19 C20 C23 -11.9(7) . . . . ?
C17 C16 C21 C13 179.5(5) . . . . ?
C15 C16 C21 C13 1.9(8) . . . . ?
C17 C16 C21 C22 0.5(8) . . . . ?
C15 C16 C21 C22 -177.2(5) . . . . ?
C12 C13 C21 C16 -177.3(5) . . . . ?
C14 C13 C21 C16 0.6(8) . . . . ?
C12 C13 C21 C22 1.7(8) . . . . ?
C14 C13 C21 C22 179.7(5) . . . . ?
C16 C21 C22 C10 172.2(5) . . . . ?
C13 C21 C22 C10 -6.9(8) . . . . ?
C16 C21 C22 C19 -5.6(8) . . . . ?
C13 C21 C22 C19 175.3(5) . . . . ?
C11 C10 C22 C21 6.2(7) . . . . ?
C9 C10 C22 C21 -173.6(5) . . . . ?
C11 C10 C22 C19 -176.2(5) . . . . ?
C9 C10 C22 C19 4.1(7) . . . . ?
C18 C19 C22 C21 7.2(7) . . . . ?
C20 C19 C22 C21 -173.2(5) . . . . ?
C18 C19 C22 C10 -170.5(5) . . . . ?
C20 C19 C22 C10 9.1(7) . . . . ?
C8 C9 C23 C24 8.9(7) . . . . ?
C10 C9 C23 C24 -169.2(4) . . . . ?
C8 C9 C23 C20 -170.1(5) . . . . ?
C10 C9 C23 C20 11.7(7) . . . . ?
C1 C20 C23 C24 4.2(7) . . . . ?
C19 C20 C23 C24 -177.5(5) . . . . ?
C1 C20 C23 C9 -176.8(5) . . . . ?
C19 C20 C23 C9 1.6(7) . . . . ?
C2 C3 C24 C6 -176.6(5) . . . . ?
C4 C3 C24 C6 3.4(8) . . . . ?
C2 C3 C24 C23 4.1(8) . . . . ?
C4 C3 C24 C23 -175.9(5) . . . . ?
C7 C6 C24 C3 178.0(5) . . . . ?
C5 C6 C24 C3 -0.3(8) . . . . ?
C7 C6 C24 C23 -2.7(8) . . . . ?
C5 C6 C24 C23 178.9(5) . . . . ?
C9 C23 C24 C3 174.6(5) . . . . ?
C20 C23 C24 C3 -6.3(7) . . . . ?
C9 C23 C24 C6 -4.6(7) . . . . ?
C20 C23 C24 C6 174.4(5) . . . . ?
C30 C25 C26 C27 -1.0(9) . . . . ?
O1 C25 C26 C27 173.8(5) . . . . ?
C30 C25 C26 C31 -178.7(6) . . . . ?
O1 C25 C26 C31 -3.8(9) . . . . ?
C25 C26 C27 C28 1.5(10) . . . . ?
C31 C26 C27 C28 179.1(7) . . . . ?
C26 C27 C28 C29 -1.0(12) . . . . ?
C27 C28 C29 C30 0.0(11) . . . . ?
C28 C29 C30 C25 0.5(10) . . . . ?
C28 C29 C30 C32 -177.3(7) . . . . ?
C26 C25 C30 C29 0.1(9) . . . . ?
O1 C25 C30 C29 -174.8(5) . . . . ?
C26 C25 C30 C32 177.9(6) . . . . ?
O1 C25 C30 C32 3.0(9) . . . . ?
C25 C26 C31 C33 88.9(16) . . . . ?
C27 C26 C31 C33 -88.6(16) . . . . ?
C25 C26 C31 C34 -143.0(14) . . . . ?
C27 C26 C31 C34 39.5(16) . . . . ?
C29 C30 C32 C35 -61.0(14) . . . . ?
C25 C30 C32 C35 121.3(13) . . . . ?
C29 C30 C32 C36 65.6(13) . . . . ?
C25 C30 C32 C36 -112.1(12) . . . . ?
C42 C37 C38 C39 -0.6(10) . . . . ?
O2 C37 C38 C39 174.0(6) . . . . ?
C42 C37 C38 C46 -175.7(6) . . . . ?
O2 C37 C38 C46 -1.0(9) . . . . ?
C48 C46 C38 C39 -88.1(8) . . . . ?
C47 C46 C38 C39 36.5(10) . . . . ?
C48 C46 C38 C37 86.5(8) . . . . ?
C47 C46 C38 C37 -148.9(7) . . . . ?
C37 C38 C39 C40 0.7(12) . . . . ?
C46 C38 C39 C40 175.8(8) . . . . ?
C38 C39 C40 C41 -0.2(15) . . . . ?
C39 C40 C41 C42 -0.4(15) . . . . ?
C38 C37 C42 C41 0.0(10) . . . . ?
O2 C37 C42 C41 -174.4(6) . . . . ?
C38 C37 C42 C43 177.1(7) . . . . ?
O2 C37 C42 C43 2.6(10) . . . . ?
C40 C41 C42 C37 0.5(12) . . . . ?
C40 C41 C42 C43 -176.6(8) . . . . ?
C45 C43 C42 C37 -107.0(9) . . . . ?
C44 C43 C42 C37 127.4(8) . . . . ?
C45 C43 C42 C41 69.9(10) . . . . ?
C44 C43 C42 C41 -55.7(10) . . . . ?
O5 C14 N1 C15 -178.7(6) . . . . ?
C13 C14 N1 C15 2.5(8) . . . . ?
O5 C14 N1 C49 1.9(9) . . . . ?
C13 C14 N1 C49 -176.9(5) . . . . ?
O6 C15 N1 C14 -179.9(6) . . . . ?
C16 C15 N1 C14 -0.1(9) . . . . ?
O6 C15 N1 C49 -0.5(9) . . . . ?
C16 C15 N1 C49 179.3(5) . . . . ?
C14 N1 C49 C50 -67.1(7) . . . . ?
C15 N1 C49 C50 113.5(6) . . . . ?
C14 N1 C49 C54 61.7(7) . . . . ?
C15 N1 C49 C54 -117.8(6) . . . . ?
N1 C49 C50 C51 -177.9(6) . . . . ?
C54 C49 C50 C51 53.5(9) . . . . ?
C49 C50 C51 C52 -54.6(10) . . . . ?
C50 C51 C52 C53 57.6(10) . . . . ?
C51 C52 C53 C54 -59.3(10) . . . . ?
N1 C49 C54 C53 177.0(6) . . . . ?
C50 C49 C54 C53 -54.6(8) . . . . ?
C52 C53 C54 C49 57.3(10) . . . . ?
O3 C4 N2 C5 177.4(6) . . . . ?
C3 C4 N2 C5 -3.8(9) . . . . ?
O3 C4 N2 C55 0.4(9) . . . . ?
C3 C4 N2 C55 179.2(5) . . . . ?
O4 C5 N2 C4 -175.7(6) . . . . ?
C6 C5 N2 C4 6.6(8) . . . . ?
O4 C5 N2 C55 1.5(9) . . . . ?
C6 C5 N2 C55 -176.3(5) . . . . ?
C4 N2 C55 C60 -73.6(10) . . . . ?
C5 N2 C55 C60 109.1(10) . . . . ?
C4 N2 C55 C56 61.5(10) . . . . ?
C5 N2 C55 C56 -115.7(8) . . . . ?
C60 C55 C56 C57 -61.9(15) . . . . ?
N2 C55 C56 C57 162.9(8) . . . . ?
C55 C56 C57 C58 64.0(15) . . . . ?
C56 C57 C58 C59 -64.0(16) . . . . ?
C57 C58 C59 C60 54.5(17) . . . . ?
N2 C55 C60 C59 -168.2(10) . . . . ?
C56 C55 C60 C59 57.2(17) . . . . ?
C58 C59 C60 C55 -48.6(17) . . . . ?
C56B C57B C58B C59B 63(3) . . . . ?
C57B C58B C59B C60B -56(3) . . . . ?
C2 C1 O1 C25 9.8(8) . . . . ?
C20 C1 O1 C25 -170.5(5) . . . . ?
C26 C25 O1 C1 87.8(6) . . . . ?
C30 C25 O1 C1 -97.0(6) . . . . ?
C12 C11 O2 C37 10.8(8) . . . . ?
C10 C11 O2 C37 -170.4(5) . . . . ?
C42 C37 O2 C11 -83.6(7) . . . . ?
C38 C37 O2 C11 101.4(6) . . . . ?
_refine_diff_density_max 0.412
_refine_diff_density_min -0.269
_refine_diff_density_rms 0.040
_shelxl_version_number 2012-6
_shelx_res_file
;
TITL MJ06
CELL 0.71073 13.495 14.896 26.835 90 99.08 90
ZERR 4 0.003 0.003 0.005 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O Cl
UNIT 244 256 8 24 8
ISOR 0.005 0.01 C34 C34B C35 C35B C43 C36 C36B C56 C56B
ISOR 0.005 0.01 C58B C33 C55 C55B C59 C59B C60 C60B C57 C57B
EADP N2 N2B
EADP C32 C32B
EADP C34 C34B
EADP C33 C33B
EADP C36 C36B
EADP C31 C31B
EADP C55 C55B
EADP C57 C57B
EADP C59 C59B
EADP C56 C56B
EADP C58 C58B
EADP C60 C60B
EXYZ N2 N2B
EXYZ C55 C55B
EXYZ C32 C32B
EXYZ C31 C31B
OMIT 0 2 2
L.S. 18
PLAN 20
CONF
MORE -1
BOND
fmap -2
acta
SHEL 12 0.9
REM C:/daten/xray_daten/oc/Kristallstrukturen/mj06/mj06qr.hkl
WGHT 0.046800 7.616600
FVAR 2.23008 0.59015 0.89046 0.44633 0.53815
C1 1 0.204504 0.670759 0.522667 11.00000 0.05192 0.05634 =
0.04938 0.00706 0.01413 -0.00398
C2 1 0.133181 0.703799 0.483318 11.00000 0.06388 0.06192 =
0.05182 0.00760 0.01866 -0.00435
AFIX 43
H2 2 0.154083 0.740136 0.458777 11.00000 -1.20000
AFIX 0
C3 1 0.033713 0.683825 0.480218 11.00000 0.05482 0.06148 =
0.04578 0.00033 0.00728 0.00197
C4 1 -0.038418 0.720079 0.437952 11.00000 0.06867 0.08461 =
0.05453 0.00816 0.00850 0.00087
C5 1 -0.174420 0.636735 0.468716 11.00000 0.06747 0.07156 =
0.04951 -0.00568 0.00400 0.00664
C6 1 -0.101707 0.605533 0.511501 11.00000 0.05580 0.06402 =
0.05253 -0.00613 0.01359 -0.00444
C7 1 -0.131542 0.550119 0.546877 11.00000 0.05093 0.07948 =
0.05951 -0.00575 0.00742 -0.01497
AFIX 43
H7 2 -0.197415 0.529525 0.542217 11.00000 -1.20000
AFIX 0
C8 1 -0.066518 0.523808 0.589410 11.00000 0.05956 0.07294 =
0.05173 0.00053 0.01049 -0.01746
AFIX 43
H8 2 -0.090491 0.486878 0.612788 11.00000 -1.20000
AFIX 0
C9 1 0.034055 0.550700 0.598586 11.00000 0.05294 0.03916 =
0.04804 -0.00493 0.01199 -0.00868
C10 1 0.101234 0.533703 0.646367 11.00000 0.04612 0.04986 =
0.04471 0.00031 0.01166 0.00083
C11 1 0.069742 0.504193 0.690814 11.00000 0.04624 0.07005 =
0.04550 0.00245 0.01427 -0.00601
C12 1 0.137294 0.488725 0.733995 11.00000 0.06163 0.07306 =
0.05113 0.00632 0.02207 -0.00288
AFIX 43
H12 2 0.113035 0.473608 0.763462 11.00000 -1.20000
AFIX 0
C13 1 0.238525 0.494735 0.735200 11.00000 0.05612 0.05517 =
0.05419 0.00530 0.01224 0.00163
C14 1 0.308600 0.468448 0.781311 11.00000 0.05783 0.07088 =
0.05636 0.00639 0.00530 0.00727
C15 1 0.451726 0.496829 0.736618 11.00000 0.06192 0.07891 =
0.05956 0.00761 0.00870 0.00226
C16 1 0.380124 0.525973 0.692001 11.00000 0.05379 0.05435 =
0.05562 0.00434 0.01063 0.00215
C17 1 0.415492 0.553107 0.649492 11.00000 0.04246 0.08990 =
0.06265 0.01159 0.01234 -0.00006
AFIX 43
H17 2 0.484195 0.552326 0.648869 11.00000 -1.20000
AFIX 0
C18 1 0.350278 0.581936 0.607051 11.00000 0.04743 0.07586 =
0.05979 0.01866 0.01428 -0.00108
AFIX 43
H18 2 0.377146 0.601033 0.579006 11.00000 -1.20000
AFIX 0
C19 1 0.246350 0.583351 0.604868 11.00000 0.05411 0.04942 =
0.04853 -0.00020 0.01581 -0.00558
C20 1 0.176897 0.618296 0.561668 11.00000 0.04516 0.04741 =
0.04961 -0.00098 0.01455 0.00157
C21 1 0.275085 0.523623 0.691119 11.00000 0.05245 0.05246 =
0.05270 0.00062 0.01455 -0.00346
C22 1 0.206200 0.547925 0.647419 11.00000 0.05065 0.04558 =
0.04583 0.00219 0.01233 0.00295
C23 1 0.071545 0.599737 0.559443 11.00000 0.05518 0.04596 =
0.03568 -0.00367 0.00610 -0.00144
C24 1 0.001295 0.628834 0.517441 11.00000 0.06499 0.04825 =
0.04698 -0.00458 0.01781 -0.00184
C25 1 0.334590 0.751794 0.490194 11.00000 0.05526 0.06338 =
0.05283 0.01221 0.01602 -0.00486
C26 1 0.340164 0.840497 0.504239 11.00000 0.08021 0.05819 =
0.05504 0.00853 0.01721 -0.00337
C27 1 0.379385 0.899819 0.472773 11.00000 0.11501 0.05802 =
0.08592 0.00279 0.03071 -0.01965
AFIX 43
H27 2 0.385792 0.960224 0.481445 11.00000 -1.20000
AFIX 0
C28 1 0.409131 0.870289 0.428611 11.00000 0.11146 0.08577 =
0.07702 0.01639 0.03377 -0.02466
AFIX 43
H28 2 0.434375 0.911091 0.407572 11.00000 -1.20000
AFIX 0
C29 1 0.401694 0.781227 0.415583 11.00000 0.09474 0.08669 =
0.06232 0.00282 0.03372 -0.01206
AFIX 43
H29 2 0.422045 0.762507 0.385718 11.00000 -1.20000
AFIX 0
C30 1 0.364581 0.718776 0.445933 11.00000 0.06992 0.06125 =
0.06386 0.00017 0.02216 -0.00970
SAME 0.02 0.04 C36 C32 C35
SAME 0.02 0.04 C35 C32 C36
SAME 0.02 0.04 C36B C32B C35B
SAME 0.02 0.04 C44 C43 C45
SAME 0.02 0.04 C45 C43 C44
SAME 0.02 0.04 C47 C46 C48
SAME 0.02 0.04 C33 C31 C34
SAME 0.02 0.04 C34 C31 C33
SAME 0.02 0.04 C34B C31B C33B
PART 0
C48 1 -0.215115 0.640267 0.688357 11.00000 0.12282 0.11469 =
0.09231 -0.01355 -0.02107 0.03121
AFIX 137
H48A 2 -0.273676 0.626021 0.702986 11.00000 -1.50000
H48B 2 -0.208016 0.597531 0.662376 11.00000 -1.50000
H48C 2 -0.221911 0.699459 0.674076 11.00000 -1.50000
AFIX 0
C46 1 -0.123603 0.636798 0.728621 11.00000 0.08432 0.09938 =
0.07970 -0.01236 0.02163 0.00951
AFIX 13
H46 2 -0.064571 0.643271 0.711825 11.00000 -1.20000
AFIX 0
C47 1 -0.123282 0.714836 0.764976 11.00000 0.13600 0.13171 =
0.13007 -0.04625 0.03524 -0.00296
AFIX 137
H47A 2 -0.064666 0.711393 0.790336 11.00000 -1.50000
H47B 2 -0.182303 0.712158 0.780750 11.00000 -1.50000
H47C 2 -0.122674 0.770338 0.746844 11.00000 -1.50000
AFIX 0
PART 1
C33 1 0.391781 0.869354 0.596179 41.00000 0.11480 0.10744 =
0.08802 -0.01467 0.02231 0.00740
AFIX 137
H33A 2 0.447792 0.902820 0.587933 41.00000 -1.50000
H33B 2 0.411537 0.808139 0.603122 41.00000 -1.50000
H33C 2 0.370052 0.895178 0.625403 41.00000 -1.50000
AFIX 0
C31 1 0.308659 0.872312 0.553227 10.50000 0.11025 0.08343 =
0.06941 -0.00833 0.03031 -0.00248
AFIX 13
H31 2 0.257847 0.829816 0.561049 10.50000 -1.20000
AFIX 0
C34 1 0.255967 0.966372 0.545982 41.00000 0.10872 0.11586 =
0.10854 -0.01709 0.03280 0.00460
AFIX 137
H34A 2 0.304251 1.011084 0.540387 41.00000 -1.50000
H34B 2 0.228120 0.981325 0.575705 41.00000 -1.50000
H34C 2 0.203298 0.964244 0.517424 41.00000 -1.50000
AFIX 0
PART 2
C34B 1 0.221128 0.932766 0.544645 -41.00000 0.10872 0.11586 =
0.10854 -0.01709 0.03280 0.00460
AFIX 137
H34D 2 0.165590 0.902241 0.525004 -41.00000 -1.50000
H34E 2 0.237506 0.985233 0.526829 -41.00000 -1.50000
H34F 2 0.203291 0.950189 0.576512 -41.00000 -1.50000
AFIX 0
C31B 1 0.308659 0.872312 0.553227 10.50000 0.11025 0.08343 =
0.06941 -0.00833 0.03031 -0.00248
AFIX 13
H31B 2 0.289087 0.819131 0.570851 10.50000 -1.20000
AFIX 0
C33B 1 0.400370 0.916726 0.588136 -41.00000 0.11480 0.10744 =
0.08802 -0.01467 0.02231 0.00740
AFIX 137
H33D 2 0.379222 0.938039 0.618544 -41.00000 -1.50000
H33E 2 0.425101 0.966157 0.570706 -41.00000 -1.50000
H33F 2 0.452682 0.873051 0.596434 -41.00000 -1.50000
AFIX 0
PART 1
C35 1 0.298351 0.601194 0.386251 51.00000 0.11314 0.11772 =
0.11667 -0.00860 0.02219 -0.02105
AFIX 137
H35A 2 0.322759 0.633614 0.359745 51.00000 -1.50000
H35B 2 0.230526 0.619005 0.387770 51.00000 -1.50000
H35C 2 0.300297 0.537947 0.379603 51.00000 -1.50000
AFIX 0
C32 1 0.360054 0.620559 0.433321 10.50000 0.08901 0.08057 =
0.08737 -0.01052 0.03018 -0.01165
AFIX 13
H32 2 0.330114 0.590072 0.459689 10.50000 -1.20000
AFIX 0
C36 1 0.471892 0.583872 0.436611 51.00000 0.11558 0.09647 =
0.11437 -0.01075 0.02068 0.00945
AFIX 137
H36A 2 0.503328 0.611822 0.410904 51.00000 -1.50000
H36B 2 0.470441 0.520014 0.431724 51.00000 -1.50000
H36C 2 0.509244 0.597691 0.469188 51.00000 -1.50000
AFIX 0
PART 2
C36B 1 0.441819 0.567137 0.457692 -51.00000 0.11558 0.09647 =
0.11437 -0.01075 0.02068 0.00945
AFIX 137
H36D 2 0.436512 0.507511 0.443952 -51.00000 -1.50000
H36E 2 0.439631 0.564611 0.493248 -51.00000 -1.50000
H36F 2 0.504128 0.593475 0.452212 -51.00000 -1.50000
AFIX 0
C32B 1 0.360054 0.620559 0.433321 10.50000 0.08901 0.08057 =
0.08737 -0.01052 0.03018 -0.01165
AFIX 13
H32B 2 0.300081 0.597599 0.445422 10.50000 -1.20000
AFIX 0
C35B 1 0.342299 0.601942 0.372832 -51.00000 0.10921 0.10366 =
0.10302 -0.02540 0.01101 -0.00392
AFIX 137
H35D 2 0.323996 0.540235 0.366491 -51.00000 -1.50000
H35E 2 0.402975 0.614593 0.359686 -51.00000 -1.50000
H35F 2 0.289447 0.640013 0.356622 -51.00000 -1.50000
AFIX 0
RIGU C43 C44
RIGU C43 C45
PART 1
C45 1 -0.092212 0.244633 0.703951 11.00000 0.15446 0.16492 =
0.18360 -0.03928 0.05931 -0.02577
AFIX 137
H45A 2 -0.133401 0.274421 0.676433 11.00000 -1.50000
H45B 2 -0.133741 0.221768 0.726987 11.00000 -1.50000
H45C 2 -0.057075 0.195874 0.691158 11.00000 -1.50000
AFIX 0
C43 1 -0.018615 0.309343 0.730670 11.00000 0.10015 0.10062 =
0.11203 0.01877 0.03348 0.00054
AFIX 13
H43 2 0.018105 0.335107 0.705359 11.00000 -1.20000
AFIX 0
C44 1 0.058399 0.260971 0.769457 11.00000 0.15232 0.15592 =
0.19293 0.06113 0.02873 0.04695
AFIX 133
H44A 2 0.024303 0.228977 0.792783 11.00000 -1.50000
H44B 2 0.103238 0.304171 0.787470 11.00000 -1.50000
H44C 2 0.095975 0.219415 0.752451 11.00000 -1.50000
AFIX 0
PART 0
C37 1 -0.069897 0.472888 0.734970 11.00000 0.04353 0.11606 =
0.05274 0.01231 0.02018 0.00442
C38 1 -0.116889 0.546562 0.753901 11.00000 0.05510 0.12281 =
0.05453 -0.00102 0.02111 0.00630
C39 1 -0.164062 0.528017 0.795591 11.00000 0.09707 0.16357 =
0.07754 0.00577 0.03768 0.02885
AFIX 43
H39 2 -0.197271 0.573914 0.809688 11.00000 -1.20000
AFIX 0
C40 1 -0.162383 0.444344 0.815928 11.00000 0.09718 0.19548 =
0.09814 0.03298 0.05558 0.01961
AFIX 43
H40 2 -0.194332 0.434478 0.843713 11.00000 -1.20000
AFIX 0
C41 1 -0.115131 0.374469 0.796701 11.00000 0.08185 0.15120 =
0.09907 0.06381 0.02994 0.00629
AFIX 43
H41 2 -0.114993 0.318143 0.811661 11.00000 -1.20000
AFIX 0
C42 1 -0.066622 0.386642 0.754514 11.00000 0.07606 0.11078 =
0.07832 0.03887 0.02757 0.00686
N1 3 0.410425 0.469165 0.779465 11.00000 0.05444 0.07594 =
0.05315 0.00966 0.00155 0.00680
C49 1 0.482423 0.438925 0.823910 11.00000 0.07128 0.07696 =
0.06149 0.01522 0.00097 0.00051
AFIX 13
H49 2 0.549102 0.442133 0.813901 11.00000 -1.20000
AFIX 0
C50 1 0.485216 0.501473 0.868593 11.00000 0.10572 0.10748 =
0.07359 -0.00915 -0.00312 0.00386
AFIX 23
H50A 2 0.419457 0.503399 0.878838 11.00000 -1.20000
H50B 2 0.501824 0.561658 0.858845 11.00000 -1.20000
AFIX 0
C51 1 0.563023 0.470058 0.913081 11.00000 0.12613 0.16289 =
0.07221 -0.00381 -0.03211 0.01090
AFIX 23
H51A 2 0.629693 0.475517 0.904185 11.00000 -1.20000
H51B 2 0.559753 0.508437 0.941978 11.00000 -1.20000
AFIX 0
C52 1 0.545226 0.373478 0.927190 11.00000 0.11682 0.20655 =
0.09507 0.05845 0.00240 0.04417
AFIX 23
H52A 2 0.480590 0.368361 0.938439 11.00000 -1.20000
H52B 2 0.596712 0.354885 0.954650 11.00000 -1.20000
AFIX 0
C53 1 0.547639 0.313304 0.881778 11.00000 0.11379 0.12973 =
0.11598 0.05324 0.00664 0.02443
AFIX 23
H53A 2 0.536460 0.251569 0.890962 11.00000 -1.20000
H53B 2 0.613314 0.316838 0.871527 11.00000 -1.20000
AFIX 0
C54 1 0.466880 0.341081 0.837305 11.00000 0.10182 0.09698 =
0.09102 0.02058 0.00035 0.02017
AFIX 23
H54A 2 0.471402 0.303233 0.808335 11.00000 -1.20000
H54B 2 0.400709 0.333465 0.846510 11.00000 -1.20000
AFIX 0
SAME 0.02 0.04 N2B > C60B
PART 1
N2 3 -0.138689 0.696490 0.435443 10.50000 0.06117 0.09717 =
0.04342 0.00673 -0.00529 0.01425
C55 1 -0.214646 0.732534 0.393734 21.00000 0.09291 0.09871 =
0.08850 -0.00178 0.01187 0.01436
AFIX 13
H55 2 -0.276618 0.701181 0.397966 21.00000 -1.20000
AFIX 0
C56 1 -0.196598 0.704366 0.341753 21.00000 0.06598 0.06224 =
0.06433 -0.00096 0.00930 0.00170
AFIX 23
H56A 2 -0.178914 0.641283 0.341344 21.00000 -1.20000
H56B 2 -0.143013 0.739489 0.331227 21.00000 -1.20000
AFIX 0
C57 1 -0.302128 0.723174 0.305217 21.00000 0.08202 0.08287 =
0.07422 0.00236 0.00734 -0.00369
AFIX 23
H57A 2 -0.298980 0.703424 0.271058 21.00000 -1.20000
H57B 2 -0.356658 0.691977 0.317424 21.00000 -1.20000
AFIX 0
C58 1 -0.316733 0.822593 0.306863 21.00000 0.09149 0.09451 =
0.09748 0.01394 0.00542 -0.00212
AFIX 23
H58A 2 -0.375995 0.839042 0.283261 21.00000 -1.20000
H58B 2 -0.259482 0.852383 0.296410 21.00000 -1.20000
AFIX 0
C59 1 -0.329284 0.856513 0.362535 21.00000 0.08982 0.08537 =
0.09382 0.00014 0.00655 0.00777
AFIX 23
H59A 2 -0.332093 0.921546 0.363524 21.00000 -1.20000
H59B 2 -0.390508 0.832702 0.372084 21.00000 -1.20000
AFIX 0
C60 1 -0.238113 0.822239 0.398194 21.00000 0.08190 0.07783 =
0.07818 -0.00169 0.00950 0.00281
AFIX 23
H60A 2 -0.180401 0.857658 0.392840 21.00000 -1.20000
H60B 2 -0.249115 0.832940 0.432555 21.00000 -1.20000
AFIX 0
PART 0
PART 2
N2B 3 -0.138689 0.696490 0.435443 10.50000 0.06117 0.09717 =
0.04342 0.00673 -0.00529 0.01425
C55B 1 -0.214646 0.732534 0.393734 -21.00000 0.09291 0.09871 =
0.08850 -0.00178 0.01187 0.01436
AFIX 13
H55B 2 -0.170491 0.778240 0.382775 -21.00000 -1.20000
AFIX 0
C56B 1 -0.233862 0.688926 0.347845 -21.00000 0.06598 0.06224 =
0.06433 -0.00096 0.00930 0.00170
AFIX 23
H56C 2 -0.283360 0.642603 0.350339 -21.00000 -1.20000
H56D 2 -0.172673 0.659011 0.342331 -21.00000 -1.20000
AFIX 0
C57B 1 -0.272411 0.747390 0.299728 -21.00000 0.08202 0.08287 =
0.07422 0.00236 0.00734 -0.00369
AFIX 23
H57C 2 -0.224923 0.793939 0.294396 -21.00000 -1.20000
H57D 2 -0.287973 0.710996 0.269532 -21.00000 -1.20000
AFIX 0
C58B 1 -0.369266 0.786961 0.316945 -21.00000 0.09149 0.09451 =
0.09748 0.01394 0.00542 -0.00212
AFIX 23
H58C 2 -0.405699 0.821321 0.289245 -21.00000 -1.20000
H58D 2 -0.411949 0.737531 0.323779 -21.00000 -1.20000
AFIX 0
C59B 1 -0.354300 0.834399 0.353755 -21.00000 0.08982 0.08537 =
0.09382 0.00014 0.00655 0.00777
AFIX 23
H59C 2 -0.419289 0.853885 0.360766 -21.00000 -1.20000
H59D 2 -0.319875 0.887578 0.344531 -21.00000 -1.20000
AFIX 0
C60B 1 -0.291680 0.797419 0.406444 -21.00000 0.08190 0.07783 =
0.07818 -0.00169 0.00950 0.00281
AFIX 23
H60C 2 -0.259243 0.846890 0.426137 -21.00000 -1.20000
H60D 2 -0.336515 0.767726 0.426106 -21.00000 -1.20000
AFIX 0
PART 0
O1 4 0.304237 0.688631 0.524004 11.00000 0.05049 0.08367 =
0.06417 0.02531 0.01843 -0.00498
O2 4 -0.030664 0.489561 0.689749 11.00000 0.04803 0.09497 =
0.05341 0.01224 0.02042 0.00030
O3 4 -0.011940 0.770241 0.406603 11.00000 0.09146 0.13075 =
0.08281 0.05186 0.00266 -0.00157
O4 4 -0.262000 0.614815 0.462798 11.00000 0.05414 0.11730 =
0.09354 0.00493 -0.01393 -0.01094
O5 4 0.276027 0.445615 0.819277 11.00000 0.07578 0.14443 =
0.05534 0.02820 0.01765 0.00709
O6 4 0.541346 0.496051 0.736868 11.00000 0.05198 0.16864 =
0.08628 0.03952 0.01069 0.00642
MOLE 2
RIGU C90 Cl2
CL1 5 0.587869 0.689749 0.582712 31.00000 0.17706 0.13020 =
0.11773 0.02463 0.01936 -0.03260
C90 1 0.610446 0.750892 0.531154 31.00000 0.09435 0.14119 =
0.09614 -0.01230 0.02568 -0.02395
AFIX 23
H90A 2 0.642381 0.711972 0.509432 31.00000 -1.20000
H90B 2 0.546601 0.769785 0.512252 31.00000 -1.20000
AFIX 0
CL2 5 0.681408 0.840342 0.544713 31.00000 0.19174 0.18535 =
0.15088 -0.00619 0.03054 -0.10491
HKLF 4
REM MJ06
REM R1 = 0.1354 for 6540 Fo > 4sig(Fo) and 0.1537 for all 7622 data
REM 688 parameters refined using 128 restraints
END
WGHT 0.0468 7.6263
REM Highest difference peak 0.412, deepest hole -0.269, 1-sigma level 0.040
Q1 1 0.6698 0.7064 0.5713 11.00000 0.05 0.41
Q2 1 0.6987 0.7489 0.5529 11.00000 0.05 0.29
Q3 1 0.6266 0.8957 0.5468 11.00000 0.05 -0.27
Q4 1 0.5611 0.7009 0.5812 11.00000 0.05 0.23
Q5 1 0.6150 0.6323 0.5582 11.00000 0.05 0.20
Q6 1 -0.2989 0.8656 0.3374 11.00000 0.05 0.20
Q7 1 0.5211 0.6607 0.5696 11.00000 0.05 -0.19
Q8 1 0.6112 0.8412 0.5188 11.00000 0.05 0.19
Q9 1 0.5734 0.6890 0.5920 11.00000 0.05 0.19
Q10 1 0.6643 0.8080 0.5445 11.00000 0.05 -0.18
Q11 1 0.6813 0.8620 0.5518 11.00000 0.05 0.18
Q12 1 0.6798 0.8178 0.5337 11.00000 0.05 -0.18
Q13 1 -0.2448 0.7436 0.3665 11.00000 0.05 -0.17
Q14 1 -0.0029 0.6950 0.3975 11.00000 0.05 0.17
Q15 1 0.2325 0.8881 0.5617 11.00000 0.05 0.17
Q16 1 0.6164 0.6804 0.5818 11.00000 0.05 -0.17
Q17 1 0.6376 0.5357 0.9103 11.00000 0.05 0.17
Q18 1 0.7290 0.8200 0.5673 11.00000 0.05 -0.17
Q19 1 0.4990 0.6945 0.5801 11.00000 0.05 -0.16
Q20 1 -0.2561 0.6995 0.2994 11.00000 0.05 0.16
;
_shelx_res_checksum 79591
_database_code_depnum_ccdc_archive 'CCDC 952113'