# Electronic Supplementary Material (ESI) for Dalton Transactions.
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# CCDC
#
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#
# 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.
#
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# fide research purposes only. It may contain copyright material
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data_H2L
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C35 H30 N6 O2'
_chemical_formula_sum 'C35 H30 N6 O2'
_chemical_formula_weight 566.65
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'I 1 2/a 1'
_space_group_name_Hall '-I 2ya'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
_cell_length_a 22.9576(10)
_cell_length_b 5.8417(3)
_cell_length_c 43.823(4)
_cell_angle_alpha 90.00
_cell_angle_beta 100.200(5)
_cell_angle_gamma 90.00
_cell_volume 5784.3(7)
_cell_formula_units_Z 8
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 4329
_cell_measurement_theta_min 2.8675
_cell_measurement_theta_max 32.5132
_exptl_crystal_description BLOCK
_exptl_crystal_colour COLORLESS
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.304
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2388.7
_exptl_absorpt_coefficient_mu 0.084
_exptl_absorpt_correction_T_min 0.9786
_exptl_absorpt_correction_T_max 0.9876
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method \w/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 22316
_diffrn_reflns_av_R_equivalents 0.0513
_diffrn_reflns_av_sigmaI/netI 0.0490
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_l_min -52
_diffrn_reflns_limit_l_max 46
_diffrn_reflns_theta_min 3.08
_diffrn_reflns_theta_max 25.04
_reflns_number_total 5086
_reflns_number_gt 3387
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Ortep3
_computing_publication_material Shelx97
_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.
Larger part of the molecule is disordered between two positions, A and B,
with occupancies refined to 0.637(3) and 0.363(3), respectively. The restraints
and constraints used in refinement include:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Restrained distances
C22A-C17A \\sim C18A-C17A \\sim C19A-C18A \\sim C20A-C19A \\sim C21A-C20A
\\sim C22A-C21A
with sigma of 0.02
C22B-C17B \\sim C18B-C17B \\sim C19B-C18B \\sim C20B-C19B \\sim C21B-C20B
\\sim C22B-C21B
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11B) = Uanis(C11A)
Uanis(C12B) = Uanis(C12A)
Uanis(C13B) = Uanis(C13A)
Uanis(C14B) = Uanis(C14A)
Uanis(C15B) = Uanis(C15A)
Uanis(C16B) = Uanis(C16A)
Uanis(N2B) = Uanis(N2A)
Uanis(C3A) = Uanis(C3B)
Uanis(C2B) = Uanis(C2A)
Uanis(C7A) = Uanis(C7B)
Uanis(C1B) = Uanis(C1A)
Uanis(C6B) = Uanis(C6A)
Uanis(C5B) = Uanis(C5A)
Uanis(C4B) = Uanis(C4A)
Uanis(C8B) = Uanis(C8A)
Uanis(N3A) = Uanis(N4B)
Uanis(N3B) = Uanis(N4A)
Uanis(C17B) = Uanis(C17A)
Uanis(C18A) = Uanis(C18B)
Uanis(C19B) = Uanis(C19A)
Uanis(C22B) = Uanis(C22A)
Uanis(C20B) = Uanis(C20A)
Uanis(C21B) = Uanis(C21A)
Uanis(O1A) = Uanis(O1B)
4. Rigid body (RIGU) restrains
C17B, C22B, C22A, C21B, C20B, C19B, C18B
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C17A, C18A, C19A, C20A, C21A, C22A
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Sof(O1B)=Sof(H1B)=Sof(N1B)=Sof(N2B)=Sof(N3B)=Sof(N4B)=Sof(C1B)=Sof(C2B)=
Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=
Sof(H7BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
Sof(H9BC)=Sof(H10B)=Sof(C11B)=Sof(C12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=
Sof(H14B)=Sof(C15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(C18B)=Sof(H18B)=
Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=
Sof(H22B)=Sof(H23B)=1-FVAR(1)
Sof(O1A)=Sof(H1A)=Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(N4A)=Sof(C1A)=Sof(C2A)=
Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A1)=Sof(H7A2)=
Sof(H7A3)=Sof(C8A)=Sof(H8A1)=Sof(H8A2)=Sof(H8A3)=Sof(C9A)=Sof(H9A1)=Sof(H9A2)=
Sof(H9A3)=Sof(H10A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=
Sof(H14A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=
Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
Sof(H22A)=Sof(H23A)=FVAR(1)
6.a Riding coordinates:
O1A(H1A), O1B(H1B), O2(H02), C5A(H5A), C7A(H7A1,H7A2,H7A3), C8A(H8A1,H8A2,
H8A3), C9A(H9A1,H9A2,H9A3), C5B(H5B), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC),
C9B(H9BA,H9BB,H9BC), C10(H10A,H10B), C13A(H13A), C14A(H14A), C16A(H16A),
C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), C13B(H13B),
C14B(H14B), C16B(H16B), C18B(H18B), C19B(H19B), C20B(H20B), C21B(H21B),
C22B(H22B), C23(H23A,H23B), C26(H26), C27(H27), C29(H29), C31(H31), C32(H32),
C33(H33), C34(H34), C35(H35)
;
_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^)+(0.0482P)^2^+20.2422P]
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 riding
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef 0.00047(10)
_refine_ls_number_reflns 5086
_refine_ls_number_parameters 480
_refine_ls_number_restraints 102
_refine_ls_R_factor_all 0.1162
_refine_ls_R_factor_gt 0.0813
_refine_ls_wR_factor_ref 0.1998
_refine_ls_wR_factor_gt 0.1763
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_restrained_S_all 1.006
_refine_ls_shift/su_max 0.007
_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
O1A O 0.2447(2) -0.5144(10) 0.36535(11) 0.0572(13) Uani 0.637(3) 1 d . . P A 1
H1A H 0.2202 -0.4237 0.3552 0.086 Uiso 0.637(3) 1 d R . P A 1
O1B O 0.2557(5) -0.552(2) 0.3818(2) 0.0572(13) Uani 0.363(3) 1 d . . P A 2
H1B H 0.2333 -0.4774 0.3686 0.086 Uiso 0.363(3) 1 d R . P A 2
O2 O 0.17659(12) 0.7919(7) 0.25696(8) 0.0991(13) Uani 1 1 d . . . . .
H02 H 0.1680 0.6923 0.2687 0.149 Uiso 1 1 d R . . . .
N1A N 0.1846(6) -0.143(2) 0.3514(3) 0.047(2) Uani 0.637(3) 1 d . . P A 1
N2A N 0.1313(5) 0.4377(13) 0.2712(2) 0.048(2) Uani 0.637(3) 1 d . . P A 1
N3A N 0.32896(18) -0.1675(7) 0.48280(12) 0.0451(10) Uani 0.637(3) 1 d . . P A 1
N4A N 0.3193(3) 0.0446(11) 0.4898(2) 0.0400(13) Uani 0.637(3) 1 d . . P A 1
N1B N 0.1850(12) -0.210(4) 0.3596(5) 0.045(4) Uani 0.363(3) 1 d . . P A 2
N2B N 0.1335(9) 0.350(3) 0.2766(5) 0.048(2) Uani 0.363(3) 1 d . . P A 2
N3B N 0.3067(7) -0.024(3) 0.4883(5) 0.0400(13) Uani 0.363(3) 1 d . . P A 2
N4B N 0.3463(3) -0.0938(12) 0.5100(2) 0.0451(10) Uani 0.363(3) 1 d . . P A 2
N5 N 0.11025(14) 0.5506(6) 0.13343(8) 0.0638(10) Uani 1 1 d . . . . .
N6 N 0.08545(13) 0.3590(6) 0.12688(7) 0.0545(8) Uani 1 1 d . . . . .
C1A C 0.1396(8) -0.008(3) 0.3323(4) 0.052(3) Uani 0.637(3) 1 d . . P A 1
C2A C 0.1591(6) 0.1508(17) 0.3113(3) 0.047(2) Uani 0.637(3) 1 d . . P A 1
C3A C 0.1118(7) 0.273(3) 0.2929(4) 0.052(3) Uani 0.637(3) 1 d . . P A 1
C4A C 0.0549(5) 0.2627(14) 0.2959(3) 0.051(3) Uani 0.637(3) 1 d . . P A 1
C5A C 0.0395(6) 0.1006(15) 0.3169(3) 0.060(3) Uani 0.637(3) 1 d . . P A 1
H5A H -0.0004 0.0897 0.3199 0.071 Uiso 0.637(3) 1 d R . P A 1
C6A C 0.0815(7) -0.0405(17) 0.3339(4) 0.056(3) Uani 0.637(3) 1 d . . P A 1
C7A C 0.2209(10) 0.173(4) 0.3083(6) 0.064(4) Uani 0.637(3) 1 d . . P A 1
H7A1 H 0.2461 0.1284 0.3279 0.096 Uiso 0.637(3) 1 d R . P A 1
H7A2 H 0.2287 0.3326 0.3036 0.096 Uiso 0.637(3) 1 d R . P A 1
H7A3 H 0.2294 0.0743 0.2916 0.096 Uiso 0.637(3) 1 d R . P A 1
C8A C 0.0078(6) 0.4244(17) 0.2789(3) 0.067(3) Uani 0.637(3) 1 d . . P A 1
H8A1 H 0.0014 0.3935 0.2565 0.101 Uiso 0.637(3) 1 d R . P A 1
H8A2 H 0.0223 0.5814 0.2827 0.101 Uiso 0.637(3) 1 d R . P A 1
H8A3 H -0.0297 0.4062 0.2864 0.101 Uiso 0.637(3) 1 d R . P A 1
C9A C 0.0626(6) -0.2212(18) 0.3545(3) 0.066(3) Uani 0.637(3) 1 d . . P A 1
H9A1 H 0.0754 -0.3702 0.3478 0.099 Uiso 0.637(3) 1 d R . P A 1
H9A2 H 0.0195 -0.2208 0.3528 0.099 Uiso 0.637(3) 1 d R . P A 1
H9A3 H 0.0812 -0.1931 0.3761 0.099 Uiso 0.637(3) 1 d R . P A 1
C1B C 0.1448(17) -0.083(5) 0.3377(9) 0.052(3) Uani 0.363(3) 1 d . . P A 2
C2B C 0.1579(12) 0.070(4) 0.3174(6) 0.047(2) Uani 0.363(3) 1 d . . P A 2
C3B C 0.1198(14) 0.199(6) 0.2977(8) 0.052(3) Uani 0.363(3) 1 d . . P A 2
C4B C 0.0551(10) 0.155(3) 0.2985(5) 0.051(3) Uani 0.363(3) 1 d . . P A 2
C5B C 0.0419(12) -0.008(3) 0.3170(6) 0.060(3) Uani 0.363(3) 1 d . . P A 2
H5B H 0.0011 -0.0353 0.3171 0.071 Uiso 0.363(3) 1 d R . P A 2
C6B C 0.0826(13) -0.139(4) 0.3367(7) 0.056(3) Uani 0.363(3) 1 d . . P A 2
C7B C 0.2276(19) 0.123(7) 0.3152(11) 0.064(4) Uani 0.363(3) 1 d . . P A 2
H7BA H 0.2517 0.0059 0.3275 0.096 Uiso 0.363(3) 1 d R . P A 2
H7BB H 0.2403 0.2752 0.3232 0.096 Uiso 0.363(3) 1 d R . P A 2
H7BC H 0.2324 0.1115 0.2935 0.096 Uiso 0.363(3) 1 d R . P A 2
C8B C 0.0096(11) 0.312(4) 0.2799(7) 0.067(3) Uani 0.363(3) 1 d . . P A 2
H8BA H 0.0195 0.4727 0.2844 0.101 Uiso 0.363(3) 1 d R . P A 2
H8BB H -0.0286 0.2766 0.2859 0.101 Uiso 0.363(3) 1 d R . P A 2
H8BC H 0.0071 0.2828 0.2577 0.101 Uiso 0.363(3) 1 d R . P A 2
C9B C 0.0663(10) -0.329(2) 0.3559(5) 0.044(4) Uani 0.363(3) 1 d . . P A 2
H9BA H 0.0819 -0.4750 0.3498 0.066 Uiso 0.363(3) 1 d R . P A 2
H9BB H 0.0231 -0.3373 0.3531 0.066 Uiso 0.363(3) 1 d R . P A 2
H9BC H 0.0825 -0.2986 0.3778 0.066 Uiso 0.363(3) 1 d R . P A 2
C10 C 0.20391(14) -0.0801(7) 0.38107(10) 0.0573(10) Uani 1 1 d . . . . .
H10A H 0.1873 0.0503 0.3892 0.069 Uiso 0.637(3) 1 d R . P A 1
H10B H 0.1956 0.0791 0.3812 0.069 Uiso 0.363(3) 1 d R . P A 2
C11A C 0.2464(6) -0.198(3) 0.4011(2) 0.038(2) Uani 0.637(3) 1 d . . P A 1
C12A C 0.2646(4) -0.4144(19) 0.39358(19) 0.048(2) Uani 0.637(3) 1 d . . P A 1
C13A C 0.3025(3) -0.5426(13) 0.41395(17) 0.0482(17) Uani 0.637(3) 1 d . . P A 1
H13A H 0.3156 -0.6875 0.4080 0.058 Uiso 0.637(3) 1 d R . P A 1
C14A C 0.3222(3) -0.4617(11) 0.44273(19) 0.0427(17) Uani 0.637(3) 1 d . . P A 1
H14A H 0.3478 -0.5537 0.4572 0.051 Uiso 0.637(3) 1 d R . P A 1
C15A C 0.3047(3) -0.2447(11) 0.45215(16) 0.0393(15) Uani 0.637(3) 1 d . . P A 1
C16A C 0.2666(11) -0.114(5) 0.4313(7) 0.048(4) Uani 0.637(3) 1 d . . P A 1
H16A H 0.2549 0.0337 0.4370 0.057 Uiso 0.637(3) 1 d R . P A 1
C17A C 0.3453(2) 0.1125(9) 0.51859(14) 0.0387(12) Uani 0.637(3) 1 d . . P A 1
C18A C 0.3299(5) 0.3260(12) 0.5292(2) 0.046(2) Uani 0.637(3) 1 d . . P A 1
H18A H 0.3019 0.4201 0.5164 0.055 Uiso 0.637(3) 1 d R . P A 1
C19A C 0.3556(5) 0.403(3) 0.5588(3) 0.052(3) Uani 0.637(3) 1 d . . P A 1
H19A H 0.3452 0.5477 0.5661 0.062 Uiso 0.637(3) 1 d R . P A 1
C20A C 0.3975(3) 0.2663(12) 0.57743(18) 0.0561(15) Uani 0.637(3) 1 d . . P A 1
H20A H 0.4138 0.3162 0.5978 0.067 Uiso 0.637(3) 1 d R . P A 1
C21A C 0.4154(3) 0.0565(12) 0.56652(16) 0.0502(16) Uani 0.637(3) 1 d . . P A 1
H21A H 0.4455 -0.0314 0.5789 0.060 Uiso 0.637(3) 1 d R . P A 1
C22A C 0.3884(2) -0.0200(9) 0.53761(13) 0.0405(12) Uani 0.637(3) 1 d . . P A 1
H22A H 0.3989 -0.1653 0.5305 0.049 Uiso 0.637(3) 1 d R . P A 1
C11B C 0.2424(13) -0.211(5) 0.4112(5) 0.038(2) Uani 0.363(3) 1 d . . P A 2
C12B C 0.2681(9) -0.436(4) 0.4076(4) 0.048(2) Uani 0.363(3) 1 d . . P A 2
C13B C 0.3066(6) -0.529(3) 0.4318(4) 0.0482(17) Uani 0.363(3) 1 d . . P A 2
H13B H 0.3232 -0.6754 0.4290 0.058 Uiso 0.363(3) 1 d R . P A 2
C14B C 0.3207(5) -0.410(2) 0.4596(3) 0.0427(17) Uani 0.363(3) 1 d . . P A 2
H14B H 0.3468 -0.4792 0.4763 0.051 Uiso 0.363(3) 1 d R . P A 2
C15B C 0.2979(7) -0.187(2) 0.4638(3) 0.0393(15) Uani 0.363(3) 1 d . . P A 2
C16B C 0.257(2) -0.092(10) 0.4370(14) 0.048(4) Uani 0.363(3) 1 d . . P A 2
H16B H 0.2403 0.0544 0.4393 0.057 Uiso 0.363(3) 1 d R . P A 2
C17B C 0.3565(5) 0.0770(17) 0.5337(3) 0.0387(12) Uani 0.363(3) 1 d . . P A 2
C18B C 0.3272(11) 0.277(2) 0.5360(4) 0.046(2) Uani 0.363(3) 1 d . . P A 2
H18B H 0.2957 0.3224 0.5200 0.055 Uiso 0.363(3) 1 d R . P A 2
C19B C 0.3426(11) 0.417(5) 0.5609(5) 0.052(3) Uani 0.363(3) 1 d . . P A 2
H19B H 0.3224 0.5572 0.5622 0.062 Uiso 0.363(3) 1 d R . P A 2
C20B C 0.3869(5) 0.356(2) 0.5847(3) 0.0561(15) Uani 0.363(3) 1 d . . P A 2
H20B H 0.3966 0.4494 0.6026 0.067 Uiso 0.363(3) 1 d R . P A 2
C21B C 0.4173(4) 0.1562(19) 0.5824(3) 0.0502(16) Uani 0.363(3) 1 d . . P A 2
H21B H 0.4495 0.1146 0.5981 0.060 Uiso 0.363(3) 1 d R . P A 2
C22B C 0.4007(5) 0.0165(19) 0.5573(3) 0.0405(12) Uani 0.363(3) 1 d . . P A 2
H22B H 0.4205 -0.1253 0.5563 0.049 Uiso 0.363(3) 1 d R . P A 2
C23 C 0.11950(14) 0.3547(9) 0.24406(10) 0.0677(13) Uani 1 1 d . . . . .
H23A H 0.1042 0.2040 0.2407 0.081 Uiso 0.637(3) 1 d R . P A 1
H23B H 0.0966 0.2251 0.2363 0.081 Uiso 0.363(3) 1 d R . P A 2
C24 C 0.13340(14) 0.5068(8) 0.22003(10) 0.0649(12) Uani 1 1 d . . . . .
C25 C 0.16062(17) 0.7214(10) 0.22728(12) 0.0802(15) Uani 1 1 d . . . . .
C26 C 0.17191(19) 0.8660(10) 0.20398(14) 0.0893(17) Uani 1 1 d . . . . .
H26 H 0.1914 1.0080 0.2090 0.107 Uiso 1 1 d R . . . .
C27 C 0.15474(18) 0.8035(9) 0.17352(13) 0.0789(15) Uani 1 1 d . . . . .
H27 H 0.1619 0.9044 0.1576 0.095 Uiso 1 1 d R . . . .
C28 C 0.12691(16) 0.5938(8) 0.16557(10) 0.0625(11) Uani 1 1 d . . . . .
C29 C 0.11682(14) 0.4453(8) 0.18886(9) 0.0595(11) Uani 1 1 d . . . . .
H29 H 0.0985 0.3014 0.1836 0.071 Uiso 1 1 d R . . . .
C30 C 0.06770(16) 0.3211(7) 0.09441(8) 0.0506(10) Uani 1 1 d . . . . .
C31 C 0.04014(17) 0.1157(7) 0.08593(8) 0.0536(10) Uani 1 1 d . . . . .
H31 H 0.0345 0.0082 0.1014 0.064 Uiso 1 1 d R . . . .
C32 C 0.02066(18) 0.0648(7) 0.05494(8) 0.0560(11) Uani 1 1 d . . . . .
H32 H 0.0016 -0.0769 0.0491 0.067 Uiso 1 1 d R . . . .
C33 C 0.02927(19) 0.2232(7) 0.03246(9) 0.0626(12) Uani 1 1 d . . . . .
H33 H 0.0160 0.1897 0.0111 0.075 Uiso 1 1 d R . . . .
C34 C 0.05714(19) 0.4293(7) 0.04104(10) 0.0659(13) Uani 1 1 d . . . . .
H34 H 0.0629 0.5367 0.0256 0.079 Uiso 1 1 d R . . . .
C35 C 0.07647(18) 0.4795(7) 0.07174(9) 0.0589(11) Uani 1 1 d . . . . .
H35 H 0.0956 0.6211 0.0775 0.071 Uiso 1 1 d R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1A 0.043(2) 0.068(3) 0.060(4) -0.020(3) 0.010(3) -0.0039(19)
O1B 0.043(2) 0.068(3) 0.060(4) -0.020(3) 0.010(3) -0.0039(19)
O2 0.0540(17) 0.150(3) 0.100(3) -0.062(2) 0.0326(18) -0.029(2)
N1A 0.025(3) 0.065(7) 0.049(7) 0.000(4) 0.005(4) -0.009(4)
N2A 0.0263(17) 0.073(7) 0.045(4) 0.001(4) 0.006(2) -0.003(4)
N3A 0.033(2) 0.022(2) 0.072(3) 0.0065(19) -0.012(2) -0.0040(16)
N4A 0.025(4) 0.028(5) 0.059(2) 0.004(4) -0.012(3) -0.010(2)
N1B 0.032(6) 0.066(12) 0.038(9) 0.010(6) 0.006(6) -0.008(7)
N2B 0.0263(17) 0.073(7) 0.045(4) 0.001(4) 0.006(2) -0.003(4)
N3B 0.025(4) 0.028(5) 0.059(2) 0.004(4) -0.012(3) -0.010(2)
N4B 0.033(2) 0.022(2) 0.072(3) 0.0065(19) -0.012(2) -0.0040(16)
N5 0.057(2) 0.072(2) 0.072(3) -0.0024(19) 0.0388(18) 0.0100(18)
N6 0.0531(18) 0.068(2) 0.050(2) 0.0038(16) 0.0295(15) 0.0203(17)
C1A 0.028(4) 0.086(11) 0.039(7) -0.008(7) -0.005(4) -0.001(7)
C2A 0.0251(19) 0.065(8) 0.050(6) -0.004(5) 0.008(3) -0.012(5)
C3A 0.022(5) 0.099(12) 0.032(6) -0.010(6) -0.004(4) 0.007(5)
C4A 0.0291(19) 0.094(8) 0.030(3) 0.000(6) 0.0037(19) -0.008(6)
C5A 0.025(2) 0.119(10) 0.034(2) -0.016(7) 0.0051(18) -0.005(7)
C6A 0.030(2) 0.104(10) 0.034(4) -0.004(7) 0.007(2) -0.015(7)
C7A 0.022(5) 0.076(10) 0.091(12) 0.003(6) -0.001(6) 0.001(5)
C8A 0.028(2) 0.134(11) 0.037(3) 0.005(8) -0.0009(18) 0.017(7)
C9A 0.038(4) 0.102(9) 0.058(6) -0.013(8) 0.008(4) -0.006(7)
C1B 0.028(4) 0.086(11) 0.039(7) -0.008(7) -0.005(4) -0.001(7)
C2B 0.0251(19) 0.065(8) 0.050(6) -0.004(5) 0.008(3) -0.012(5)
C3B 0.022(5) 0.099(12) 0.032(6) -0.010(6) -0.004(4) 0.007(5)
C4B 0.0291(19) 0.094(8) 0.030(3) 0.000(6) 0.0037(19) -0.008(6)
C5B 0.025(2) 0.119(10) 0.034(2) -0.016(7) 0.0051(18) -0.005(7)
C6B 0.030(2) 0.104(10) 0.034(4) -0.004(7) 0.007(2) -0.015(7)
C7B 0.022(5) 0.076(10) 0.091(12) 0.003(6) -0.001(6) 0.001(5)
C8B 0.028(2) 0.134(11) 0.037(3) 0.005(8) -0.0009(18) 0.017(7)
C9B 0.031(6) 0.062(10) 0.041(7) -0.002(9) 0.011(5) -0.004(8)
C10 0.0255(16) 0.069(3) 0.074(3) -0.018(2) -0.0019(17) -0.0050(17)
C11A 0.025(3) 0.038(3) 0.051(8) 0.002(5) 0.008(5) -0.006(2)
C12A 0.026(2) 0.044(3) 0.075(8) 0.007(6) 0.011(5) -0.004(2)
C13A 0.032(2) 0.044(3) 0.068(5) -0.003(4) 0.008(4) -0.004(2)
C14A 0.029(2) 0.029(4) 0.071(6) 0.008(4) 0.010(4) 0.003(2)
C15A 0.035(3) 0.031(4) 0.047(5) -0.009(3) -0.005(3) -0.013(3)
C16A 0.027(8) 0.032(6) 0.077(12) 0.002(6) -0.008(5) -0.007(5)
C17A 0.031(2) 0.026(2) 0.054(4) 0.018(2) -0.007(3) -0.0040(17)
C18A 0.035(2) 0.024(3) 0.073(4) 0.013(3) -0.006(3) -0.006(3)
C19A 0.035(6) 0.038(2) 0.079(3) 0.002(2) -0.001(3) -0.008(3)
C20A 0.035(3) 0.058(4) 0.071(4) -0.006(3) -0.003(2) 0.005(3)
C21A 0.030(2) 0.063(4) 0.051(4) -0.005(2) -0.013(2) 0.007(2)
C22A 0.032(2) 0.037(2) 0.044(3) 0.011(2) -0.015(2) -0.0011(19)
C11B 0.025(3) 0.038(3) 0.051(8) 0.002(5) 0.008(5) -0.006(2)
C12B 0.026(2) 0.044(3) 0.075(8) 0.007(6) 0.011(5) -0.004(2)
C13B 0.032(2) 0.044(3) 0.068(5) -0.003(4) 0.008(4) -0.004(2)
C14B 0.029(2) 0.029(4) 0.071(6) 0.008(4) 0.010(4) 0.003(2)
C15B 0.035(3) 0.031(4) 0.047(5) -0.009(3) -0.005(3) -0.013(3)
C16B 0.027(8) 0.032(6) 0.077(12) 0.002(6) -0.008(5) -0.007(5)
C17B 0.031(2) 0.026(2) 0.054(4) 0.018(2) -0.007(3) -0.0040(17)
C18B 0.035(2) 0.024(3) 0.073(4) 0.013(3) -0.006(3) -0.006(3)
C19B 0.035(6) 0.038(2) 0.079(3) 0.002(2) -0.001(3) -0.008(3)
C20B 0.035(3) 0.058(4) 0.071(4) -0.006(3) -0.003(2) 0.005(3)
C21B 0.030(2) 0.063(4) 0.051(4) -0.005(2) -0.013(2) 0.007(2)
C22B 0.032(2) 0.037(2) 0.044(3) 0.011(2) -0.015(2) -0.0011(19)
C23 0.0224(16) 0.123(4) 0.060(3) -0.023(3) 0.0124(17) -0.004(2)
C24 0.0233(16) 0.108(3) 0.068(3) -0.028(3) 0.0195(18) -0.006(2)
C25 0.034(2) 0.125(4) 0.090(4) -0.043(3) 0.032(2) -0.010(2)
C26 0.052(3) 0.108(4) 0.122(5) -0.045(4) 0.057(3) -0.014(3)
C27 0.055(2) 0.087(3) 0.109(4) -0.021(3) 0.052(3) -0.001(2)
C28 0.0372(19) 0.091(3) 0.066(3) -0.012(2) 0.0296(19) 0.006(2)
C29 0.0250(16) 0.095(3) 0.063(3) -0.018(2) 0.0191(17) 0.0009(18)
C30 0.058(2) 0.055(2) 0.048(2) 0.0141(18) 0.0339(18) 0.0285(19)
C31 0.070(2) 0.056(2) 0.043(2) 0.0162(18) 0.0335(19) 0.029(2)
C32 0.082(3) 0.052(2) 0.042(2) 0.0111(18) 0.031(2) 0.033(2)
C33 0.091(3) 0.061(3) 0.044(2) 0.0199(19) 0.036(2) 0.047(2)
C34 0.091(3) 0.053(3) 0.067(3) 0.028(2) 0.048(2) 0.045(2)
C35 0.072(3) 0.053(2) 0.063(3) 0.0169(19) 0.040(2) 0.032(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1A C12A 1.371(11) . ?
O1B C12B 1.30(2) . ?
O2 C25 1.351(5) . ?
N1A C1A 1.442(16) . ?
N1A C10 1.347(15) . ?
N2A C3A 1.476(18) . ?
N2A C23 1.267(12) . ?
N3A N4A 1.304(10) . ?
N3A C15A 1.432(8) . ?
N4A C17A 1.358(11) . ?
N1B C1B 1.42(3) . ?
N1B C10 1.22(3) . ?
N2B C3B 1.35(4) . ?
N2B C23 1.40(2) . ?
N3B N4B 1.26(2) . ?
N3B C15B 1.42(2) . ?
N4B C17B 1.429(14) . ?
N5 N6 1.265(5) . ?
N5 C28 1.415(5) . ?
N6 C30 1.426(5) . ?
C1A C2A 1.434(17) . ?
C1A C6A 1.36(2) . ?
C2A C3A 1.427(14) . ?
C2A C7A 1.45(3) . ?
C3A C4A 1.34(2) . ?
C4A C5A 1.408(16) . ?
C4A C8A 1.528(14) . ?
C5A C6A 1.382(19) . ?
C6A C9A 1.500(16) . ?
C1B C2B 1.33(3) . ?
C1B C6B 1.46(5) . ?
C2B C3B 1.34(3) . ?
C2B C7B 1.65(5) . ?
C3B C4B 1.51(4) . ?
C4B C5B 1.32(3) . ?
C4B C8B 1.51(3) . ?
C5B C6B 1.39(4) . ?
C6B C9B 1.48(3) . ?
C10 C11A 1.378(15) . ?
C10 C11B 1.64(3) . ?
C11A C12A 1.386(19) . ?
C11A C16A 1.41(3) . ?
C12A C13A 1.357(12) . ?
C13A C14A 1.347(10) . ?
C14A C15A 1.413(9) . ?
C15A C16A 1.38(3) . ?
C17A C18A 1.399(8) . ?
C17A C22A 1.407(6) . ?
C18A C19A 1.398(9) . ?
C19A C20A 1.397(10) . ?
C20A C21A 1.404(8) . ?
C21A C22A 1.382(7) . ?
C11B C12B 1.46(4) . ?
C11B C16B 1.32(6) . ?
C12B C13B 1.37(2) . ?
C13B C14B 1.394(19) . ?
C14B C15B 1.427(16) . ?
C15B C16B 1.47(6) . ?
C17B C18B 1.363(13) . ?
C17B C22B 1.362(11) . ?
C18B C19B 1.358(14) . ?
C19B C20B 1.366(13) . ?
C20B C21B 1.372(11) . ?
C21B C22B 1.368(12) . ?
C23 C24 1.456(6) . ?
C24 C25 1.412(6) . ?
C24 C29 1.398(5) . ?
C25 C26 1.385(7) . ?
C26 C27 1.373(7) . ?
C27 C28 1.397(6) . ?
C28 C29 1.390(6) . ?
C30 C31 1.376(6) . ?
C30 C35 1.398(5) . ?
C31 C32 1.385(5) . ?
C32 C33 1.391(5) . ?
C33 C34 1.384(6) . ?
C34 C35 1.372(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
C10 N1A C1A 119.4(14) . . ?
C23 N2A C3A 108.4(10) . . ?
N4A N3A C15A 117.7(6) . . ?
N3A N4A C17A 115.5(7) . . ?
C10 N1B C1B 107(2) . . ?
C3B N2B C23 132(2) . . ?
N4B N3B C15B 110.0(15) . . ?
N3B N4B C17B 109.1(10) . . ?
N6 N5 C28 114.5(4) . . ?
N5 N6 C30 113.7(3) . . ?
C2A C1A N1A 117.0(14) . . ?
C6A C1A N1A 120.0(12) . . ?
C6A C1A C2A 123.0(11) . . ?
C1A C2A C7A 122.4(12) . . ?
C3A C2A C1A 113.2(12) . . ?
C3A C2A C7A 124.2(11) . . ?
C2A C3A N2A 113.8(12) . . ?
C4A C3A N2A 120.5(8) . . ?
C4A C3A C2A 125.4(13) . . ?
C3A C4A C5A 117.3(10) . . ?
C3A C4A C8A 122.8(9) . . ?
C5A C4A C8A 119.9(10) . . ?
C6A C5A C4A 121.5(12) . . ?
C1A C6A C5A 119.0(10) . . ?
C1A C6A C9A 121.3(11) . . ?
C5A C6A C9A 119.7(13) . . ?
N1B C1B C6B 115(3) . . ?
C2B C1B N1B 127(3) . . ?
C2B C1B C6B 118(3) . . ?
C1B C2B C3B 127(3) . . ?
C1B C2B C7B 120(3) . . ?
C3B C2B C7B 113(2) . . ?
N2B C3B C4B 118.2(19) . . ?
C2B C3B N2B 127(3) . . ?
C2B C3B C4B 115(3) . . ?
C5B C4B C3B 118(2) . . ?
C5B C4B C8B 124(2) . . ?
C8B C4B C3B 118.2(18) . . ?
C4B C5B C6B 125(2) . . ?
C1B C6B C9B 120(2) . . ?
C5B C6B C1B 116(2) . . ?
C5B C6B C9B 124(3) . . ?
N1A C10 C11A 123.6(9) . . ?
N1B C10 C11B 113.3(14) . . ?
C10 C11A C12A 120.9(11) . . ?
C10 C11A C16A 120.0(15) . . ?
C12A C11A C16A 118.6(16) . . ?
O1A C12A C11A 122.4(9) . . ?
C13A C12A O1A 115.5(9) . . ?
C13A C12A C11A 122.1(10) . . ?
C14A C13A C12A 119.4(8) . . ?
C13A C14A C15A 121.5(6) . . ?
C14A C15A N3A 118.3(6) . . ?
C16A C15A N3A 122.8(12) . . ?
C16A C15A C14A 118.9(12) . . ?
C15A C16A C11A 119.5(19) . . ?
N4A C17A C18A 118.4(7) . . ?
N4A C17A C22A 122.5(6) . . ?
C18A C17A C22A 119.0(6) . . ?
C19A C18A C17A 120.4(9) . . ?
C20A C19A C18A 119.4(10) . . ?
C19A C20A C21A 120.9(8) . . ?
C22A C21A C20A 118.9(6) . . ?
C21A C22A C17A 121.3(6) . . ?
C12B C11B C10 120.1(18) . . ?
C16B C11B C10 118(3) . . ?
C16B C11B C12B 121(3) . . ?
O1B C12B C11B 122.0(18) . . ?
O1B C12B C13B 119(2) . . ?
C13B C12B C11B 119.4(19) . . ?
C12B C13B C14B 119.8(18) . . ?
C13B C14B C15B 122.5(14) . . ?
N3B C15B C14B 134.5(15) . . ?
N3B C15B C16B 110(2) . . ?
C14B C15B C16B 116(2) . . ?
C11B C16B C15B 121(4) . . ?
C18B C17B N4B 129.3(11) . . ?
C22B C17B N4B 112.1(10) . . ?
C22B C17B C18B 118.6(13) . . ?
C19B C18B C17B 120.8(17) . . ?
C18B C19B C20B 120.7(19) . . ?
C19B C20B C21B 119.0(15) . . ?
C22B C21B C20B 119.5(11) . . ?
C17B C22B C21B 121.3(11) . . ?
N2A C23 C24 114.0(5) . . ?
N2B C23 C24 134.9(8) . . ?
C25 C24 C23 121.6(4) . . ?
C29 C24 C23 119.5(4) . . ?
C29 C24 C25 118.8(5) . . ?
O2 C25 C24 121.4(5) . . ?
O2 C25 C26 118.0(5) . . ?
C26 C25 C24 120.6(5) . . ?
C27 C26 C25 119.7(5) . . ?
C26 C27 C28 121.0(5) . . ?
C27 C28 N5 115.8(4) . . ?
C29 C28 N5 124.7(4) . . ?
C29 C28 C27 119.5(4) . . ?
C28 C29 C24 120.3(4) . . ?
C31 C30 N6 116.2(3) . . ?
C31 C30 C35 120.1(4) . . ?
C35 C30 N6 123.7(4) . . ?
C30 C31 C32 120.4(3) . . ?
C31 C32 C33 119.3(4) . . ?
C34 C33 C32 120.2(4) . . ?
C35 C34 C33 120.4(4) . . ?
C34 C35 C30 119.6(4) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.04
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.285
_refine_diff_density_min -0.376
_refine_diff_density_rms 0.054
_database_code_depnum_ccdc_archive 'CCDC 941801'
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1A H1A N1A 0.84 1.83 2.587(14) 149.3 .
O1A H1A N1B 0.84 1.52 2.23(3) 140.4 .
O1B H1B N1B 0.83 1.92 2.65(3) 147.0 .
O2 H02 N2A 0.82 1.72 2.445(8) 145.5 .
_iucr_refine_instructions_details
;
TITL H2L
CELL 0.71073 22.9576 5.8417 43.823 90 100.2 90
ZERR 8 0.001 0.0003 0.004 0 0.005 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H N O
DISP C 0.003 0.002
DISP H 0 0
DISP N 0.006 0.003
DISP O 0.011 0.006
UNIT 280 240 48 16
SADI C22A C17A C18A C17A C19A C18A C20A C19A C21A C20A C22A C21A
SADI C22B C17B C18B C17B C19B C18B C20B C19B C21B C20B C22B C21B
RIGU C17B C22B C22A C21B C20B C19B C18B
RIGU C17A C18A C19A C20A C21A C22A
EADP C11B C11A
EADP C12B C12A
EADP C13B C13A
EADP C14B C14A
EADP C15B C15A
EADP C16B C16A
EADP N2B N2A
EADP C3A C3B
EADP C2B C2A
EADP C7A C7B
EADP C1B C1A
EADP C6B C6A
EADP C5B C5A
EADP C4B C4A
EADP C8B C8A
EADP N3A N4B
EADP N3B N4A
EADP C17B C17A
EADP C18A C18B
EADP C19B C19A
EADP C22B C22A
EADP C20B C20A
EADP C21B C21A
EADP O1A O1B
HTAB O1A N1A
HTAB O1A N1B
HTAB O1B N1B
HTAB O2 N2A
L.S. 7
PLAN 5
SIZE 0.26 0.21 0.15
TEMP -123(2)
fmap 2 53
acta 50
EXTI 0.00047(10)
REM I:/andrei/RSC/DT-ART-07-2013-051821.R4/h2l.hkl
WGHT 0.0482 20.2422
FVAR 1.14025 0.63693
PART 1
O1A 4 0.24471 -0.51440 0.36536 21.00000 0.04333 0.06820 0.06068 =
-0.01961 0.00964 -0.00396
AFIX 3
H1A 2 0.22025 -0.42370 0.35517 21.00000 -1.50000
AFIX 0
PART 0
PART 2
O1B 4 0.25574 -0.55160 0.38182 -21.00000 0.04333 0.06820 0.06068 =
-0.01961 0.00964 -0.00396
AFIX 3
H1B 2 0.23326 -0.47737 0.36862 -21.00000 -1.50000
AFIX 0
PART 0
O2 4 0.17659 0.79186 0.25695 11.00000 0.05403 0.15029 0.10001 =
-0.06203 0.03261 -0.02929
AFIX 3
H02 2 0.16798 0.69229 0.26868 11.00000 -1.50000
AFIX 0
PART 1
N1A 3 0.18457 -0.14276 0.35143 21.00000 0.02544 0.06528 0.04878 =
-0.00029 0.00465 -0.00953
N2A 3 0.13130 0.43761 0.27117 21.00000 0.02629 0.07323 0.04485 =
0.00106 0.00619 -0.00293
N3A 3 0.32896 -0.16749 0.48279 21.00000 0.03304 0.02239 0.07215 =
0.00650 -0.01240 -0.00398
N4A 3 0.31930 0.04459 0.48975 21.00000 0.02555 0.02820 0.05938 =
0.00408 -0.01179 -0.00958
PART 0
PART 2
N1B 3 0.18499 -0.20978 0.35962 -21.00000 0.03243 0.06549 0.03811 =
0.01040 0.00584 -0.00797
N2B 3 0.13348 0.35013 0.27657 -21.00000 0.02629 0.07323 0.04485 =
0.00106 0.00619 -0.00293
N3B 3 0.30668 -0.02442 0.48826 -21.00000 0.02555 0.02820 0.05938 =
0.00408 -0.01179 -0.00958
N4B 3 0.34634 -0.09378 0.50997 -21.00000 0.03304 0.02239 0.07215 =
0.00650 -0.01240 -0.00398
PART 0
N5 3 0.11025 0.55056 0.13343 11.00000 0.05695 0.07250 0.07196 =
-0.00240 0.03877 0.00997
N6 3 0.08545 0.35901 0.12687 11.00000 0.05311 0.06827 0.04976 =
0.00381 0.02950 0.02024
PART 1
C1A 1 0.13963 -0.00799 0.33235 21.00000 0.02806 0.08607 0.03915 =
-0.00822 -0.00480 -0.00081
C2A 1 0.15914 0.15075 0.31131 21.00000 0.02504 0.06459 0.05034 =
-0.00423 0.00788 -0.01233
C3A 1 0.11171 0.27261 0.29281 21.00000 0.02151 0.10154 0.03101 =
-0.00938 -0.00436 0.00702
C4A 1 0.05488 0.26259 0.29592 21.00000 0.02911 0.09457 0.02995 =
-0.00063 0.00364 -0.00825
C5A 1 0.03954 0.10050 0.31692 21.00000 0.02477 0.11980 0.03446 =
-0.01647 0.00514 -0.00538
AFIX 3
H5A 2 -0.00036 0.08966 0.31992 21.00000 -1.20000
AFIX 0
C6A 1 0.08151 -0.04061 0.33394 21.00000 0.03024 0.10434 0.03363 =
-0.00411 0.00685 -0.01536
C7A 1 0.22086 0.17275 0.30837 21.00000 0.02183 0.07603 0.09192 =
0.00246 -0.00096 0.00083
AFIX 3
H7A1 2 0.24611 0.12836 0.32791 21.00000 -1.50000
H7A2 2 0.22871 0.33264 0.30367 21.00000 -1.50000
H7A3 2 0.22941 0.07426 0.29161 21.00000 -1.50000
AFIX 0
C8A 1 0.00776 0.42431 0.27885 21.00000 0.02818 0.13491 0.03668 =
0.00471 -0.00090 0.01723
AFIX 3
H8A1 2 0.00142 0.39334 0.25652 21.00000 -1.50000
H8A2 2 0.02226 0.58126 0.28274 21.00000 -1.50000
H8A3 2 -0.02967 0.40609 0.28640 21.00000 -1.50000
AFIX 0
C9A 1 0.06260 -0.22125 0.35448 21.00000 0.03745 0.10256 0.05842 =
-0.01280 0.00810 -0.00615
AFIX 3
H9A1 2 0.07544 -0.37028 0.34782 21.00000 -1.50000
H9A2 2 0.01947 -0.22087 0.35284 21.00000 -1.50000
H9A3 2 0.08124 -0.19310 0.37605 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C1B 1 0.14483 -0.08304 0.33765 -21.00000 0.02806 0.08607 0.03915 =
-0.00822 -0.00480 -0.00081
C2B 1 0.15787 0.07018 0.31738 -21.00000 0.02504 0.06459 0.05034 =
-0.00423 0.00788 -0.01233
C3B 1 0.11997 0.19988 0.29777 -21.00000 0.02151 0.10154 0.03101 =
-0.00938 -0.00436 0.00702
C4B 1 0.05508 0.15470 0.29844 -21.00000 0.02911 0.09457 0.02995 =
-0.00063 0.00364 -0.00825
C5B 1 0.04190 -0.00824 0.31697 -21.00000 0.02477 0.11980 0.03446 =
-0.01647 0.00514 -0.00538
AFIX 3
H5B 2 0.00114 -0.03528 0.31712 -21.00000 -1.20000
AFIX 0
C6B 1 0.08260 -0.13914 0.33674 -21.00000 0.03024 0.10434 0.03363 =
-0.00411 0.00685 -0.01536
C7B 1 0.22757 0.12325 0.31512 -21.00000 0.02183 0.07603 0.09192 =
0.00246 -0.00096 0.00083
AFIX 3
H7BA 2 0.25167 0.00586 0.32741 -21.00000 -1.50000
H7BB 2 0.24033 0.27520 0.32314 -21.00000 -1.50000
H7BC 2 0.23243 0.11143 0.29341 -21.00000 -1.50000
AFIX 0
C8B 1 0.00961 0.31160 0.27996 -21.00000 0.02818 0.13491 0.03668 =
0.00471 -0.00090 0.01723
AFIX 3
H8BA 2 0.01951 0.47274 0.28442 -21.00000 -1.50000
H8BB 2 -0.02858 0.27667 0.28594 -21.00000 -1.50000
H8BC 2 0.00715 0.28285 0.25773 -21.00000 -1.50000
AFIX 0
C9B 1 0.06632 -0.32917 0.35595 -21.00000 0.03104 0.06203 0.04043 =
-0.00197 0.01126 -0.00387
AFIX 3
H9BA 2 0.08189 -0.47503 0.34980 -21.00000 -1.50000
H9BB 2 0.02307 -0.33734 0.35308 -21.00000 -1.50000
H9BC 2 0.08249 -0.29865 0.37779 -21.00000 -1.50000
AFIX 0
PART 0
C10 1 0.20391 -0.08013 0.38107 11.00000 0.02555 0.06852 0.07402 =
-0.01756 -0.00196 -0.00496
PART 1
AFIX 3
H10A 2 0.18726 0.05026 0.38923 21.00000 -1.20000
PART 0
PART 2
H10B 2 0.19558 0.07913 0.38118 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C11A 1 0.24643 -0.19847 0.40111 21.00000 0.02514 0.03789 0.05118 =
0.00193 0.00829 -0.00582
C12A 1 0.26456 -0.41444 0.39359 21.00000 0.02575 0.04389 0.07519 =
0.00664 0.01111 -0.00446
C13A 1 0.30255 -0.54262 0.41396 21.00000 0.03193 0.04412 0.06866 =
-0.00260 0.00806 -0.00387
AFIX 3
H13A 2 0.31558 -0.68753 0.40799 21.00000 -1.20000
AFIX 0
C14A 1 0.32220 -0.46170 0.44274 21.00000 0.02862 0.02877 0.07133 =
0.00788 0.00985 0.00348
AFIX 3
H14A 2 0.34780 -0.55367 0.45717 21.00000 -1.20000
AFIX 0
C15A 1 0.30474 -0.24469 0.45216 21.00000 0.03516 0.03105 0.04765 =
-0.00846 -0.00504 -0.01297
C16A 1 0.26661 -0.11393 0.43133 21.00000 0.02737 0.03247 0.07706 =
0.00180 -0.00860 -0.00699
AFIX 3
H16A 2 0.25489 0.03375 0.43701 21.00000 -1.20000
AFIX 0
C17A 1 0.34533 0.11254 0.51859 21.00000 0.03055 0.02601 0.05421 =
0.01847 -0.00696 -0.00395
C18A 1 0.32991 0.32595 0.52925 21.00000 0.03528 0.02409 0.07330 =
0.01266 -0.00650 -0.00618
AFIX 3
H18A 2 0.30192 0.42006 0.51644 21.00000 -1.20000
AFIX 0
C19A 1 0.35557 0.40300 0.55878 21.00000 0.03481 0.03768 0.07876 =
0.00191 -0.00111 -0.00835
AFIX 3
H19A 2 0.34516 0.54765 0.56614 21.00000 -1.20000
AFIX 0
C20A 1 0.39747 0.26631 0.57743 21.00000 0.03543 0.05797 0.07083 =
-0.00561 -0.00271 0.00464
AFIX 3
H20A 2 0.41381 0.31621 0.59778 21.00000 -1.20000
AFIX 0
C21A 1 0.41543 0.05650 0.56651 21.00000 0.03021 0.06263 0.05062 =
-0.00498 -0.01268 0.00677
AFIX 3
H21A 2 0.44552 -0.03141 0.57887 21.00000 -1.20000
AFIX 0
C22A 1 0.38842 -0.01994 0.53761 21.00000 0.03244 0.03748 0.04405 =
0.01118 -0.01462 -0.00112
AFIX 3
H22A 2 0.39891 -0.16527 0.53050 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C11B 1 0.24243 -0.21107 0.41119 -21.00000 0.02514 0.03789 0.05118 =
0.00193 0.00829 -0.00582
C12B 1 0.26815 -0.43619 0.40756 -21.00000 0.02575 0.04389 0.07519 =
0.00664 0.01111 -0.00446
C13B 1 0.30661 -0.52929 0.43179 -21.00000 0.03193 0.04412 0.06866 =
-0.00260 0.00806 -0.00387
AFIX 3
H13B 2 0.32316 -0.67532 0.42906 -21.00000 -1.20000
AFIX 0
C14B 1 0.32072 -0.40944 0.45961 -21.00000 0.02862 0.02877 0.07133 =
0.00788 0.00985 0.00348
AFIX 3
H14B 2 0.34681 -0.47917 0.47627 -21.00000 -1.20000
AFIX 0
C15B 1 0.29793 -0.18659 0.46379 -21.00000 0.03516 0.03105 0.04765 =
-0.00846 -0.00504 -0.01297
C16B 1 0.25727 -0.09171 0.43700 -21.00000 0.02737 0.03247 0.07706 =
0.00180 -0.00860 -0.00699
AFIX 3
H16B 2 0.24035 0.05437 0.43927 -21.00000 -1.20000
AFIX 0
C17B 1 0.35652 0.07695 0.53367 -21.00000 0.03055 0.02601 0.05421 =
0.01847 -0.00696 -0.00395
C18B 1 0.32717 0.27721 0.53599 -21.00000 0.03528 0.02409 0.07330 =
0.01266 -0.00650 -0.00618
AFIX 3
H18B 2 0.29568 0.32236 0.52002 -21.00000 -1.20000
AFIX 0
C19B 1 0.34266 0.41667 0.56092 -21.00000 0.03481 0.03768 0.07876 =
0.00191 -0.00111 -0.00835
AFIX 3
H19B 2 0.32246 0.55727 0.56222 -21.00000 -1.20000
AFIX 0
C20B 1 0.38689 0.35574 0.58467 -21.00000 0.03543 0.05797 0.07083 =
-0.00561 -0.00271 0.00464
AFIX 3
H20B 2 0.39663 0.44938 0.60257 -21.00000 -1.20000
AFIX 0
C21B 1 0.41734 0.15614 0.58238 -21.00000 0.03021 0.06263 0.05062 =
-0.00498 -0.01268 0.00677
AFIX 3
H21B 2 0.44954 0.11451 0.59814 -21.00000 -1.20000
AFIX 0
C22B 1 0.40074 0.01652 0.55729 -21.00000 0.03244 0.03748 0.04405 =
0.01118 -0.01462 -0.00112
AFIX 3
H22B 2 0.42051 -0.12534 0.55626 -21.00000 -1.20000
AFIX 0
PART 0
C23 1 0.11951 0.35475 0.24406 11.00000 0.02242 0.12300 0.05962 =
-0.02289 0.01242 -0.00387
PART 1
AFIX 3
H23A 2 0.10423 0.20399 0.24067 21.00000 -1.20000
PART 0
PART 2
H23B 2 0.09663 0.22512 0.23626 -21.00000 -1.20000
AFIX 0
PART 0
C24 1 0.13340 0.50681 0.22003 11.00000 0.02328 0.10761 0.06808 =
-0.02796 0.01951 -0.00637
C25 1 0.16063 0.72141 0.22728 11.00000 0.03361 0.12512 0.08956 =
-0.04339 0.03223 -0.01024
C26 1 0.17190 0.86599 0.20398 11.00000 0.05245 0.10846 0.12245 =
-0.04548 0.05734 -0.01434
AFIX 3
H26 2 0.19137 1.00802 0.20904 11.00000 -1.20000
AFIX 0
C27 1 0.15474 0.80351 0.17352 11.00000 0.05475 0.08694 0.10863 =
-0.02149 0.05160 -0.00061
AFIX 3
H27 2 0.16189 0.90436 0.15758 11.00000 -1.20000
AFIX 0
C28 1 0.12690 0.59381 0.16557 11.00000 0.03716 0.09151 0.06644 =
-0.01188 0.02958 0.00644
C29 1 0.11682 0.44527 0.18886 11.00000 0.02503 0.09460 0.06297 =
-0.01837 0.01906 0.00095
AFIX 3
H29 2 0.09847 0.30140 0.18356 11.00000 -1.20000
AFIX 0
C30 1 0.06770 0.32113 0.09442 11.00000 0.05775 0.05552 0.04769 =
0.01409 0.03392 0.02847
C31 1 0.04014 0.11573 0.08593 11.00000 0.06975 0.05638 0.04338 =
0.01613 0.03350 0.02929
AFIX 3
H31 2 0.03447 0.00823 0.10141 11.00000 -1.20000
AFIX 0
C32 1 0.02066 0.06478 0.05494 11.00000 0.08189 0.05174 0.04188 =
0.01110 0.03121 0.03257
AFIX 3
H32 2 0.00159 -0.07690 0.04912 11.00000 -1.20000
AFIX 0
C33 1 0.02927 0.22317 0.03246 11.00000 0.09151 0.06124 0.04407 =
0.01992 0.03623 0.04711
AFIX 3
H33 2 0.01604 0.18973 0.01115 11.00000 -1.20000
AFIX 0
C34 1 0.05714 0.42927 0.04104 11.00000 0.09069 0.05266 0.06677 =
0.02790 0.04758 0.04531
AFIX 3
H34 2 0.06295 0.53672 0.02558 11.00000 -1.20000
AFIX 0
C35 1 0.07646 0.47943 0.07174 11.00000 0.07148 0.05268 0.06285 =
0.01695 0.04020 0.03231
AFIX 3
H35 2 0.09563 0.62105 0.07751 11.00000 -1.20000
AFIX 0
HKLF 4
END
;
#######################################################################
#
# 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_1
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C35 H28 N6 O2 Zn),1.2(C H2 Cl2)'
_chemical_formula_sum 'C71.2 H58.4 Cl2.4 N12 O4 Zn2'
_chemical_formula_weight 1361.92
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0180 0.0090 '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 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0490 0.0320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5490 0.6780 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.0742(8)
_cell_length_b 15.6117(12)
_cell_length_c 17.5354(11)
_cell_angle_alpha 82.851(6)
_cell_angle_beta 68.389(6)
_cell_angle_gamma 77.788(6)
_cell_volume 3248.0(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 7582
_cell_measurement_theta_min 4.1470
_cell_measurement_theta_max 71.4870
_exptl_crystal_description BLOCK
_exptl_crystal_colour COLORLESS
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.21
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.393
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1405.2
_exptl_absorpt_coefficient_mu 2.296
_exptl_absorpt_correction_T_min 0.5179
_exptl_absorpt_correction_T_max 0.6442
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'Micro-Focus (Cu) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method \w/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 23807
_diffrn_reflns_av_R_equivalents 0.0506
_diffrn_reflns_av_sigmaI/netI 0.0618
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 3.70
_diffrn_reflns_theta_max 72.87
_reflns_number_total 12617
_reflns_number_gt 9048
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Ortep3
_computing_publication_material Shelx97
_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 N~2~Ph group at C(15) is disordered equally between orientations
A and B, in both cases the Ph ring was refined as a rigid body. The structures
contains infinite channels filled with DCM of crystallization. There are
3 symmetrically independent positions of DCM molecules, A, B and C, with
occupancies of 0.67, 0.33 and 0.2. Adjacent positions A and B cannot be
occupied simultaneously, due to short intermolecular contacts. Other
constraints and restraints used include:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
Cl1A-C1A \\sim Cl2A-C1A
with sigma of 0.02
Cl1B-C1B \\sim Cl2B-C1B
with sigma of 0.02
Cl2C-C1C \\sim Cl1C-C1C
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30B) = Uanis(C30A)
Uiso(N3A) = Uiso(N3B)
Uiso(N2A) = Uiso(N2B)
Uanis(C35A) = Uanis(C35B)
Uanis(C31B) = Uanis(C31A)
Uiso(C33A) = Uiso(C33B)
Uanis(C34B) = Uanis(C34A)
Uanis(C32A) = Uanis(C32B)
Uanis(C31A) = Uanis(C31B)
4. Others
Fixed Sof: N2A(0.5) N3A(0.5) N2B(0.5) N3B(0.5) C30A(0.5) C31A(0.5) H31A(0.5)
C32A(0.5) H32A(0.5) C33A(0.5) H33A(0.5) C34A(0.5) H34A(0.5) C35A(0.5)
H35A(0.5) C30B(0.5) C31B(0.5) H31B(0.5) C32B(0.5) H32B(0.5) C33B(0.5)
H33B(0.5) C34B(0.5) H34B(0.5) C35B(0.5) H35B(0.5) Cl1A(0.67) Cl2A(0.67)
C1A(0.67) H1AA(0.67) H1AB(0.67) Cl1B(0.33) Cl2B(0.33) C1B(0.33) H1BA(0.33)
H1BB(0.33) Cl1C(0.2) Cl2C(0.2) C1C(0.2) H1CA(0.2) H1CB(0.2)
5.a Secondary CH2 refined with riding coordinates:
C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB)
5.b Aromatic/amide H refined with riding coordinates:
C4(H4), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17), C20(H20), C21(H21),
C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31A(H31A),
C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C31B(H31B), C32B(H32B),
C33B(H33B), C34B(H34B), C35B(H35B), C39(H39), C42(H42), C43(H43), C45(H45),
C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C57(H57), C58(H58), C60(H60),
C62(H62), C63(H63), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
5.c Fitted hexagon refined as free rotating group:
C30A(C31A,C32A,C33A,C34A,C35A), C30B(C31B,C32B,C33B,C34B,C35B)
5.d Idealised Me refined as rotating group:
C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C38(H38A,H38B,H38C),
C54(H54A,H54B,H54C), C56(H56A,H56B,H56C)
;
_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^)+(0.1420P)^2^+1.5000P]
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 riding
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 12617
_refine_ls_number_parameters 850
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0994
_refine_ls_R_factor_gt 0.0789
_refine_ls_wR_factor_gt 0.2216
_refine_ls_wR_factor_ref 0.2456
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_restrained_S_all 1.036
_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_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
Zn1 Zn 0.16737(4) 0.37557(4) 0.82851(3) 0.05210(19) Uani 1 1 d . . . . .
Zn2 Zn 0.72795(5) 0.02463(4) 0.65232(4) 0.0579(2) Uani 1 1 d . . . . .
O1 O 0.2290(3) 0.2531(2) 0.83074(18) 0.0580(7) Uani 1 1 d . . . . .
O2 O 0.2159(2) 0.4279(2) 0.71918(17) 0.0581(8) Uani 1 1 d . . . . .
O3 O 0.6019(3) 0.1100(2) 0.6454(2) 0.0661(9) Uani 1 1 d . . . . .
O4 O 0.6827(3) -0.0428(2) 0.7538(2) 0.0743(10) Uani 1 1 d . . . . .
N1 N 0.2335(3) 0.4068(2) 0.9063(2) 0.0510(8) Uani 1 1 d . . . . .
N2A N 0.5711(7) 0.0732(6) 0.9296(5) 0.0526(13) Uiso 0.5 1 d . . P A 1
N3A N 0.5987(7) 0.1100(5) 0.9823(6) 0.0622(13) Uiso 0.5 1 d . . P A 1
N2B N 0.5828(7) 0.1066(5) 0.9441(5) 0.0526(13) Uiso 0.5 1 d . . P A 2
N3B N 0.6203(7) 0.0324(6) 0.9318(5) 0.0622(13) Uiso 0.5 1 d . . P A 2
N4 N 0.0045(3) 0.4261(2) 0.85464(19) 0.0464(7) Uani 1 1 d . . . . .
N5 N -0.0448(3) 0.6072(3) 0.5433(2) 0.0563(9) Uani 1 1 d . . . . .
N6 N 0.0057(3) 0.6322(3) 0.4705(2) 0.0580(9) Uani 1 1 d . . . . .
N7 N 0.8314(3) 0.1102(2) 0.6291(2) 0.0527(8) Uani 1 1 d . . . . .
N8 N 0.5636(3) 0.4722(3) 0.6245(2) 0.0622(10) Uani 1 1 d . . . . .
N9 N 0.4790(3) 0.5154(3) 0.6128(2) 0.0626(10) Uani 1 1 d . . . . .
N10 N 0.7973(3) -0.0788(2) 0.5818(2) 0.0523(8) Uani 1 1 d . . . . .
N11 N 0.6896(3) -0.4001(2) 0.7995(2) 0.0579(9) Uani 1 1 d . . . . .
N12 N 0.6467(3) -0.4309(3) 0.8718(2) 0.0596(9) Uani 1 1 d . . . . .
C1 C -0.1170(3) 0.5099(3) 0.9733(2) 0.0482(9) Uani 1 1 d . . . . .
C2 C 0.1931(3) 0.4888(3) 0.9455(3) 0.0517(10) Uani 1 1 d . . . . .
C3 C 0.2238(4) 0.5655(3) 0.9014(3) 0.0565(10) Uani 1 1 d . . . . .
C4 C 0.1777(4) 0.6438(3) 0.9397(3) 0.0586(11) Uani 1 1 d . . . . .
H4 H 0.1983 0.6965 0.9101 0.070 Uiso 1 1 calc R . . . .
C5 C -0.1026(4) 0.3516(3) 0.9806(3) 0.0532(10) Uani 1 1 d . . . . .
C6 C -0.0749(3) 0.4295(3) 0.9381(2) 0.0491(9) Uani 1 1 d . . . . .
C7 C -0.0826(4) 0.5940(3) 0.9283(3) 0.0545(10) Uani 1 1 d . . . . .
H7A H -0.1387 0.6245 0.9047 0.082 Uiso 1 1 calc GR . . . .
H7B H -0.0099 0.5804 0.8841 0.082 Uiso 1 1 calc GR . . . .
H7C H -0.0769 0.6317 0.9667 0.082 Uiso 1 1 calc GR . . . .
C8 C 0.3096(5) 0.5624(4) 0.8149(3) 0.0746(15) Uani 1 1 d . . . . .
H8A H 0.3820 0.5305 0.8164 0.112 Uiso 1 1 calc GR . . . .
H8B H 0.3168 0.6223 0.7921 0.112 Uiso 1 1 calc GR . . . .
H8C H 0.2854 0.5323 0.7804 0.112 Uiso 1 1 calc GR . . . .
C9 C -0.0586(4) 0.2652(3) 0.9402(3) 0.0672(13) Uani 1 1 d . . . . .
H9A H -0.0847 0.2179 0.9805 0.101 Uiso 1 1 calc GR . . . .
H9B H 0.0233 0.2549 0.9189 0.101 Uiso 1 1 calc GR . . . .
H9C H -0.0857 0.2666 0.8948 0.101 Uiso 1 1 calc GR . . . .
C10 C 0.3081(3) 0.3515(3) 0.9266(3) 0.0563(10) Uani 1 1 d . . . . .
H10 H 0.3371 0.3711 0.9623 0.068 Uiso 1 1 calc R . . . .
C11 C 0.3524(3) 0.2631(3) 0.9010(3) 0.0557(11) Uani 1 1 d . . . . .
C12 C 0.3114(3) 0.2189(3) 0.8551(2) 0.0534(10) Uani 1 1 d . . . . .
C13 C 0.3652(4) 0.1312(3) 0.8372(3) 0.0626(12) Uani 1 1 d . . . . .
H13 H 0.3406 0.0998 0.8061 0.075 Uiso 1 1 calc R . . . .
C14 C 0.4499(4) 0.0902(3) 0.8622(3) 0.0648(13) Uani 1 1 d . . . . .
H14 H 0.4836 0.0314 0.8481 0.078 Uiso 1 1 calc R . . . .
C15 C 0.4890(4) 0.1328(4) 0.9085(3) 0.0691(14) Uani 1 1 d . . . . .
C16 C 0.4399(4) 0.2185(4) 0.9270(3) 0.0643(12) Uani 1 1 d . . . . .
H16 H 0.4661 0.2483 0.9583 0.077 Uiso 1 1 calc R . . . .
C17 C -0.0309(3) 0.4682(3) 0.7979(2) 0.0480(9) Uani 1 1 d . . . . .
H17 H -0.1093 0.4884 0.8138 0.058 Uiso 1 1 calc R . . . .
C18 C 0.0340(3) 0.4881(3) 0.7138(2) 0.0482(9) Uani 1 1 d . . . . .
C19 C 0.1525(3) 0.4685(3) 0.6795(3) 0.0522(10) Uani 1 1 d . . . . .
C20 C 0.2047(4) 0.4964(3) 0.5964(3) 0.0588(11) Uani 1 1 d . . . . .
H20 H 0.2839 0.4841 0.5721 0.071 Uiso 1 1 calc R . . . .
C21 C 0.1433(4) 0.5406(3) 0.5504(3) 0.0590(11) Uani 1 1 d . . . . .
H21 H 0.1806 0.5579 0.4947 0.071 Uiso 1 1 calc R . . . .
C22 C 0.0256(4) 0.5609(3) 0.5844(3) 0.0525(10) Uani 1 1 d . . . . .
C23 C -0.0261(4) 0.5330(3) 0.6654(3) 0.0525(10) Uani 1 1 d . . . . .
H23 H -0.1055 0.5449 0.6886 0.063 Uiso 1 1 calc R . . . .
C24 C -0.0694(4) 0.6780(3) 0.4299(3) 0.0581(11) Uani 1 1 d . . . . .
C25 C -0.0164(5) 0.7075(3) 0.3490(3) 0.0664(12) Uani 1 1 d . . . . .
H25 H 0.0628 0.6953 0.3243 0.080 Uiso 1 1 calc R . . . .
C26 C -0.0818(5) 0.7553(4) 0.3047(3) 0.0722(14) Uani 1 1 d . . . . .
H26 H -0.0471 0.7765 0.2499 0.087 Uiso 1 1 calc R . . . .
C27 C -0.1944(6) 0.7710(4) 0.3403(4) 0.0778(15) Uani 1 1 d . . . . .
H27 H -0.2381 0.8039 0.3101 0.093 Uiso 1 1 calc R . . . .
C28 C -0.2475(5) 0.7402(4) 0.4200(3) 0.0737(14) Uani 1 1 d . . . . .
H28 H -0.3268 0.7516 0.4439 0.088 Uiso 1 1 calc R . . . .
C29 C -0.1843(5) 0.6930(4) 0.4642(3) 0.0664(12) Uani 1 1 d . . . . .
H29 H -0.2201 0.6708 0.5185 0.080 Uiso 1 1 calc R . . . .
C30A C 0.6902(6) 0.0581(5) 1.0007(5) 0.072(3) Uani 0.5 1 d . . P A 1
C31A C 0.7125(7) 0.0895(5) 1.0627(5) 0.089(3) Uani 0.5 1 d G . P A 1
H31A H 0.6680 0.1417 1.0883 0.107 Uiso 0.5 1 calc R . P A 1
C32A C 0.7999(8) 0.0444(6) 1.0873(6) 0.113(6) Uani 0.5 1 d G . P A 1
H32A H 0.8151 0.0658 1.1296 0.136 Uiso 0.5 1 calc R . P A 1
C33A C 0.8649(7) -0.0320(6) 1.0498(6) 0.082(2) Uiso 0.5 1 d G . P A 1
H33A H 0.9247 -0.0628 1.0666 0.099 Uiso 0.5 1 calc R . P A 1
C34A C 0.8426(7) -0.0634(5) 0.9878(5) 0.089(3) Uani 0.5 1 d G . P A 1
H34A H 0.8871 -0.1156 0.9622 0.106 Uiso 0.5 1 calc R . P A 1
C35A C 0.7553(7) -0.0183(6) 0.9633(5) 0.082(3) Uani 0.5 1 d G . P A 1
H35A H 0.7400 -0.0397 0.9209 0.099 Uiso 0.5 1 calc R . P A 1
C30B C 0.7105(6) 0.0062(5) 0.9619(5) 0.072(3) Uani 0.5 1 d . . P A 2
C31B C 0.7386(8) 0.0575(4) 1.0079(6) 0.089(3) Uani 0.5 1 d G . P A 2
H31B H 0.6970 0.1148 1.0209 0.107 Uiso 0.5 1 calc R . P A 2
C32B C 0.8275(8) 0.0249(5) 1.0350(6) 0.113(6) Uani 0.5 1 d G . P A 2
H32B H 0.8468 0.0599 1.0664 0.136 Uiso 0.5 1 calc R . P A 2
C33B C 0.8884(7) -0.0591(6) 1.0160(6) 0.082(2) Uiso 0.5 1 d G . P A 2
H33B H 0.9491 -0.0814 1.0345 0.099 Uiso 0.5 1 calc R . P A 2
C34B C 0.8602(7) -0.1103(5) 0.9700(6) 0.089(3) Uani 0.5 1 d G . P A 2
H34B H 0.9018 -0.1677 0.9570 0.106 Uiso 0.5 1 calc R . P A 2
C35B C 0.7713(7) -0.0777(5) 0.9429(5) 0.082(3) Uani 0.5 1 d G . P A 2
H35B H 0.7520 -0.1128 0.9115 0.099 Uiso 0.5 1 calc R . P A 2
C36 C 0.9509(3) 0.0845(3) 0.6062(2) 0.0500(9) Uani 1 1 d . . . . .
C37 C 0.9963(4) 0.0486(3) 0.6659(3) 0.0588(11) Uani 1 1 d . . . . .
C38 C 0.9228(5) 0.0390(4) 0.7546(3) 0.0763(15) Uani 1 1 d . . . . .
H38A H 0.8835 0.0971 0.7749 0.114 Uiso 1 1 calc GR . . . .
H38B H 0.9690 0.0114 0.7872 0.114 Uiso 1 1 calc GR . . . .
H38C H 0.8681 0.0025 0.7595 0.114 Uiso 1 1 calc GR . . . .
C39 C 0.7957(4) 0.1927(3) 0.6230(2) 0.0529(10) Uani 1 1 d . . . . .
H39 H 0.8500 0.2293 0.6101 0.063 Uiso 1 1 calc R . . . .
C40 C 0.6839(4) 0.2367(3) 0.6333(3) 0.0553(10) Uani 1 1 d . . . . .
C41 C 0.5936(4) 0.1944(3) 0.6435(3) 0.0553(10) Uani 1 1 d . . . . .
C42 C 0.4902(4) 0.2488(3) 0.6521(3) 0.0626(12) Uani 1 1 d . . . . .
H42 H 0.4270 0.2223 0.6621 0.075 Uiso 1 1 calc R . . . .
C43 C 0.4766(4) 0.3383(3) 0.6466(3) 0.0608(11) Uani 1 1 d . . . . .
H43 H 0.4052 0.3723 0.6517 0.073 Uiso 1 1 calc R . . . .
C44 C 0.5669(4) 0.3804(3) 0.6334(3) 0.0589(11) Uani 1 1 d . . . . .
C45 C 0.6680(4) 0.3289(3) 0.6283(3) 0.0582(11) Uani 1 1 d . . . . .
H45 H 0.7293 0.3565 0.6213 0.070 Uiso 1 1 calc R . . . .
C46 C 0.4749(4) 0.6070(3) 0.6058(3) 0.0614(12) Uani 1 1 d . . . . .
C47 C 0.3975(5) 0.6585(4) 0.5744(3) 0.0724(14) Uani 1 1 d . . . . .
H47 H 0.3503 0.6312 0.5589 0.087 Uiso 1 1 calc R . . . .
C48 C 0.3882(5) 0.7462(4) 0.5655(4) 0.0778(15) Uani 1 1 d . . . . .
H48 H 0.3377 0.7799 0.5410 0.093 Uiso 1 1 calc R . . . .
C49 C 0.4502(6) 0.7863(4) 0.5912(5) 0.094(2) Uani 1 1 d . . . . .
H49 H 0.4435 0.8483 0.5848 0.113 Uiso 1 1 calc R . . . .
C50 C 0.5234(6) 0.7378(4) 0.6266(6) 0.112(3) Uani 1 1 d . . . . .
H50 H 0.5653 0.7666 0.6462 0.135 Uiso 1 1 calc R . . . .
C51 C 0.5361(5) 0.6485(4) 0.6339(5) 0.0897(19) Uani 1 1 d . . . . .
H51 H 0.5870 0.6152 0.6582 0.108 Uiso 1 1 calc R . . . .
C52 C 0.8683(3) -0.0707(3) 0.4969(2) 0.0496(9) Uani 1 1 d . . . . .
C53 C 0.9831(3) -0.0963(3) 0.4764(2) 0.0488(9) Uani 1 1 d . . . . .
C54 C 1.0352(3) -0.1330(3) 0.5402(2) 0.0528(10) Uani 1 1 d . . . . .
H54A H 1.0432 -0.1971 0.5447 0.079 Uiso 1 1 calc GR . . . .
H54B H 0.9873 -0.1091 0.5934 0.079 Uiso 1 1 calc GR . . . .
H54C H 1.1091 -0.1167 0.5239 0.079 Uiso 1 1 calc GR . . . .
C55 C 0.8186(4) -0.0347(3) 0.4387(3) 0.0543(10) Uani 1 1 d . . . . .
C56 C 0.6940(4) -0.0123(4) 0.4625(3) 0.0691(13) Uani 1 1 d . . . . .
H56A H 0.6615 -0.0648 0.4869 0.104 Uiso 1 1 calc GR . . . .
H56B H 0.6748 0.0091 0.4137 0.104 Uiso 1 1 calc GR . . . .
H56C H 0.6642 0.0334 0.5026 0.104 Uiso 1 1 calc GR . . . .
C57 C 0.8884(4) -0.0248(3) 0.3582(3) 0.0599(11) Uani 1 1 d . . . . .
H57 H 0.8562 -0.0009 0.3179 0.072 Uiso 1 1 calc R . . . .
C58 C 0.7922(3) -0.1579(3) 0.6128(2) 0.0487(9) Uani 1 1 d . . . . .
H58 H 0.8304 -0.2037 0.5760 0.058 Uiso 1 1 calc R . . . .
C59 C 0.7347(3) -0.1843(3) 0.6971(2) 0.0519(10) Uani 1 1 d . . . . .
C60 C 0.7349(3) -0.2742(3) 0.7134(2) 0.0526(10) Uani 1 1 d . . . . .
H60 H 0.7724 -0.3128 0.6697 0.063 Uiso 1 1 calc R . . . .
C61 C 0.6820(4) -0.3085(3) 0.7914(3) 0.0569(11) Uani 1 1 d . . . . .
C62 C 0.6271(5) -0.2507(3) 0.8546(3) 0.0726(14) Uani 1 1 d . . . . .
H62 H 0.5879 -0.2730 0.9080 0.087 Uiso 1 1 calc R . . . .
C63 C 0.6284(5) -0.1645(4) 0.8415(3) 0.0774(16) Uani 1 1 d . . . . .
H63 H 0.5921 -0.1275 0.8865 0.093 Uiso 1 1 calc R . . . .
C64 C 0.6820(4) -0.1264(3) 0.7627(3) 0.0617(12) Uani 1 1 d . . . . .
C65 C 0.6553(4) -0.5235(3) 0.8774(3) 0.0600(11) Uani 1 1 d . . . . .
C66 C 0.6872(6) -0.5745(4) 0.8096(4) 0.0834(17) Uani 1 1 d . . . . .
H66 H 0.7014 -0.5481 0.7557 0.100 Uiso 1 1 calc R . . . .
C67 C 0.6972(6) -0.6628(4) 0.8230(4) 0.0924(19) Uani 1 1 d . . . . .
H67 H 0.7186 -0.6981 0.7773 0.111 Uiso 1 1 calc R . . . .
C68 C 0.6776(6) -0.7032(4) 0.8998(5) 0.0876(18) Uani 1 1 d . . . . .
H68 H 0.6870 -0.7653 0.9066 0.105 Uiso 1 1 calc R . . . .
C69 C 0.6447(5) -0.6537(4) 0.9659(4) 0.0769(15) Uani 1 1 d . . . . .
H69 H 0.6300 -0.6811 1.0194 0.092 Uiso 1 1 calc R . . . .
C70 C 0.6328(4) -0.5634(4) 0.9552(3) 0.0695(13) Uani 1 1 d . . . . .
H70 H 0.6090 -0.5286 1.0015 0.083 Uiso 1 1 calc R . . . .
Cl1A Cl -0.0299(3) 0.7548(3) 0.7505(2) 0.1389(14) Uani 0.67 1 d . . P B 1
Cl2A Cl 0.1548(4) 0.8113(3) 0.7729(3) 0.1413(13) Uani 0.67 1 d . . P B 1
C1A C 0.1141(10) 0.7300(9) 0.7301(10) 0.127(5) Uani 0.67 1 d . . P B 1
H1AA H 0.1547 0.7293 0.6700 0.152 Uiso 0.67 1 calc R . P B 1
H1AB H 0.1338 0.6710 0.7546 0.152 Uiso 0.67 1 calc R . P B 1
Cl1B Cl 0.2791(11) 0.8524(8) 0.7833(8) 0.213(5) Uani 0.33 1 d . . P C 2
Cl2B Cl 0.4615(6) 0.9554(5) 0.6941(5) 0.124(2) Uani 0.33 1 d . . P C 2
C1B C 0.409(3) 0.876(3) 0.771(3) 0.222(19) Uiso 0.33 1 d . . P C 2
H1BA H 0.4647 0.8203 0.7597 0.266 Uiso 0.33 1 calc R . P C 2
H1BB H 0.4048 0.8949 0.8243 0.266 Uiso 0.33 1 calc R . P C 2
Cl1C Cl -0.007(3) 0.8134(10) 0.8300(13) 0.265(14) Uani 0.2 1 d . . P D 3
Cl2C Cl 0.0723(13) 0.7018(9) 0.7071(8) 0.130(4) Uiso 0.2 1 d . . P D 3
C1C C 0.111(4) 0.800(3) 0.729(2) 0.120(14) Uiso 0.2 1 d . . P D 3
H1CA H 0.1054 0.8496 0.6886 0.144 Uiso 0.2 1 calc R . P D 3
H1CB H 0.1856 0.7883 0.7339 0.144 Uiso 0.2 1 calc R . P D 3
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
Zn1 0.0434(3) 0.0602(4) 0.0413(3) 0.0014(2) -0.0093(2) 0.0022(2)
Zn2 0.0478(3) 0.0507(4) 0.0536(3) 0.0016(3) 0.0015(3) -0.0009(2)
O1 0.0516(16) 0.0603(18) 0.0543(16) -0.0047(14) -0.0176(14) 0.0057(14)
O2 0.0418(15) 0.074(2) 0.0446(15) 0.0057(14) -0.0083(12) 0.0019(13)
O3 0.0479(17) 0.0570(19) 0.074(2) 0.0008(15) -0.0046(15) -0.0015(14)
O4 0.087(2) 0.0524(19) 0.0498(17) -0.0008(14) 0.0082(16) -0.0015(16)
N1 0.0431(17) 0.059(2) 0.0417(17) -0.0032(15) -0.0073(14) -0.0035(15)
N4 0.0367(15) 0.0530(19) 0.0406(16) 0.0003(14) -0.0077(13) -0.0021(13)
N5 0.063(2) 0.063(2) 0.0421(18) 0.0018(16) -0.0197(16) -0.0107(18)
N6 0.062(2) 0.062(2) 0.0468(19) 0.0000(16) -0.0183(17) -0.0068(18)
N7 0.0432(17) 0.056(2) 0.0439(17) 0.0026(15) -0.0034(14) -0.0019(15)
N8 0.050(2) 0.061(2) 0.057(2) 0.0061(17) -0.0070(17) 0.0014(17)
N9 0.053(2) 0.065(2) 0.051(2) 0.0063(17) -0.0063(17) 0.0027(18)
N10 0.0432(17) 0.053(2) 0.0456(18) 0.0026(15) -0.0037(14) -0.0015(14)
N11 0.053(2) 0.057(2) 0.053(2) 0.0087(16) -0.0101(16) -0.0086(16)
N12 0.051(2) 0.062(2) 0.051(2) 0.0070(17) -0.0050(16) -0.0056(17)
C1 0.0398(19) 0.057(2) 0.0390(19) 0.0039(17) -0.0073(16) -0.0058(17)
C2 0.0400(19) 0.062(3) 0.045(2) -0.0005(18) -0.0081(16) -0.0056(17)
C3 0.047(2) 0.067(3) 0.044(2) 0.0029(19) -0.0046(18) -0.012(2)
C4 0.054(2) 0.063(3) 0.048(2) 0.014(2) -0.0076(19) -0.016(2)
C5 0.046(2) 0.057(2) 0.050(2) 0.0054(18) -0.0137(18) -0.0058(18)
C6 0.0373(18) 0.062(3) 0.0390(19) 0.0047(17) -0.0078(15) -0.0050(17)
C7 0.051(2) 0.059(3) 0.042(2) 0.0011(18) -0.0072(18) -0.0035(19)
C8 0.064(3) 0.089(4) 0.048(2) 0.006(2) 0.005(2) -0.017(3)
C9 0.062(3) 0.060(3) 0.062(3) 0.005(2) -0.006(2) -0.006(2)
C10 0.041(2) 0.074(3) 0.046(2) -0.002(2) -0.0100(17) -0.0037(19)
C11 0.042(2) 0.069(3) 0.042(2) 0.0009(19) -0.0072(17) 0.0034(19)
C12 0.045(2) 0.059(3) 0.042(2) 0.0065(18) -0.0069(17) -0.0010(18)
C13 0.056(3) 0.067(3) 0.051(2) -0.003(2) -0.011(2) 0.004(2)
C14 0.054(3) 0.063(3) 0.054(2) 0.009(2) -0.006(2) 0.008(2)
C15 0.047(2) 0.090(4) 0.047(2) 0.011(2) -0.0068(19) 0.010(2)
C16 0.045(2) 0.087(4) 0.050(2) 0.001(2) -0.0141(19) 0.003(2)
C17 0.0396(19) 0.052(2) 0.046(2) 0.0002(17) -0.0112(16) -0.0030(16)
C18 0.0414(19) 0.052(2) 0.044(2) 0.0033(17) -0.0110(16) -0.0024(16)
C19 0.042(2) 0.059(3) 0.046(2) -0.0004(18) -0.0096(17) -0.0035(18)
C20 0.044(2) 0.072(3) 0.050(2) 0.004(2) -0.0081(18) -0.006(2)
C21 0.054(2) 0.068(3) 0.044(2) 0.0078(19) -0.0106(19) -0.009(2)
C22 0.053(2) 0.053(2) 0.045(2) 0.0020(17) -0.0127(18) -0.0052(18)
C23 0.046(2) 0.057(2) 0.048(2) -0.0022(18) -0.0109(18) -0.0048(18)
C24 0.072(3) 0.058(3) 0.048(2) 0.0004(19) -0.027(2) -0.010(2)
C25 0.077(3) 0.072(3) 0.051(2) -0.001(2) -0.025(2) -0.013(2)
C26 0.098(4) 0.070(3) 0.053(3) 0.003(2) -0.035(3) -0.013(3)
C27 0.095(4) 0.078(4) 0.071(3) 0.001(3) -0.046(3) -0.008(3)
C28 0.074(3) 0.083(4) 0.069(3) -0.013(3) -0.036(3) 0.002(3)
C29 0.069(3) 0.078(3) 0.053(2) -0.005(2) -0.025(2) -0.007(2)
C30A 0.056(4) 0.089(7) 0.068(6) 0.031(4) -0.024(4) -0.021(5)
C31A 0.090(7) 0.073(7) 0.115(9) 0.032(6) -0.057(8) -0.021(5)
C32A 0.111(8) 0.094(8) 0.162(16) 0.053(10) -0.086(11) -0.043(7)
C34A 0.066(5) 0.076(8) 0.099(7) 0.020(6) -0.018(5) 0.007(5)
C35A 0.057(4) 0.096(8) 0.073(5) 0.025(6) -0.016(4) 0.000(5)
C30B 0.056(4) 0.089(7) 0.068(6) 0.031(4) -0.024(4) -0.021(5)
C31B 0.090(7) 0.073(7) 0.115(9) 0.032(6) -0.057(8) -0.021(5)
C32B 0.111(8) 0.094(8) 0.162(16) 0.053(10) -0.086(11) -0.043(7)
C34B 0.066(5) 0.076(8) 0.099(7) 0.020(6) -0.018(5) 0.007(5)
C35B 0.057(4) 0.096(8) 0.073(5) 0.025(6) -0.016(4) 0.000(5)
C36 0.043(2) 0.051(2) 0.046(2) 0.0052(17) -0.0083(17) -0.0055(17)
C37 0.067(3) 0.056(3) 0.045(2) 0.0043(18) -0.016(2) -0.004(2)
C38 0.072(3) 0.096(4) 0.044(2) 0.011(2) -0.010(2) -0.007(3)
C39 0.049(2) 0.053(2) 0.045(2) 0.0040(17) -0.0062(17) -0.0076(18)
C40 0.049(2) 0.056(3) 0.046(2) 0.0002(18) -0.0040(18) -0.0035(18)
C41 0.046(2) 0.053(3) 0.050(2) 0.0048(18) -0.0032(18) -0.0014(18)
C42 0.047(2) 0.064(3) 0.062(3) 0.005(2) -0.006(2) -0.006(2)
C43 0.042(2) 0.064(3) 0.059(3) 0.003(2) -0.0061(19) 0.0024(19)
C44 0.051(2) 0.055(3) 0.054(2) 0.0036(19) -0.0066(19) 0.0004(19)
C45 0.051(2) 0.059(3) 0.054(2) 0.0052(19) -0.0103(19) -0.0052(19)
C46 0.052(2) 0.058(3) 0.058(3) 0.007(2) -0.009(2) -0.003(2)
C47 0.077(3) 0.069(3) 0.065(3) 0.002(2) -0.028(3) 0.001(3)
C48 0.078(4) 0.073(4) 0.072(3) 0.006(3) -0.026(3) 0.003(3)
C49 0.082(4) 0.058(3) 0.121(5) 0.020(3) -0.027(4) -0.001(3)
C50 0.084(4) 0.061(4) 0.208(9) 0.012(4) -0.078(5) -0.011(3)
C51 0.068(3) 0.060(3) 0.139(6) 0.012(3) -0.045(4) -0.002(3)
C52 0.046(2) 0.048(2) 0.0418(19) 0.0030(16) -0.0057(17) -0.0017(17)
C53 0.044(2) 0.044(2) 0.048(2) 0.0013(16) -0.0089(17) -0.0006(16)
C54 0.045(2) 0.054(2) 0.045(2) 0.0052(17) -0.0062(17) 0.0008(17)
C55 0.051(2) 0.049(2) 0.053(2) 0.0013(18) -0.0133(19) -0.0008(18)
C56 0.054(3) 0.073(3) 0.071(3) 0.004(2) -0.022(2) 0.003(2)
C57 0.056(2) 0.062(3) 0.054(2) 0.006(2) -0.018(2) -0.001(2)
C58 0.044(2) 0.051(2) 0.042(2) -0.0022(17) -0.0088(16) -0.0005(16)
C59 0.046(2) 0.053(2) 0.044(2) 0.0021(17) -0.0056(17) -0.0041(17)
C60 0.048(2) 0.056(2) 0.041(2) 0.0010(17) -0.0042(17) -0.0047(18)
C61 0.054(2) 0.056(3) 0.047(2) 0.0060(18) -0.0080(19) -0.0040(19)
C62 0.078(3) 0.068(3) 0.043(2) 0.004(2) 0.005(2) -0.006(3)
C63 0.091(4) 0.063(3) 0.046(2) -0.002(2) 0.004(2) 0.001(3)
C64 0.058(3) 0.054(3) 0.050(2) 0.0016(19) 0.002(2) 0.000(2)
C65 0.048(2) 0.068(3) 0.057(3) 0.014(2) -0.013(2) -0.014(2)
C66 0.101(4) 0.072(4) 0.063(3) 0.010(3) -0.012(3) -0.024(3)
C67 0.118(5) 0.071(4) 0.075(4) 0.004(3) -0.015(4) -0.031(4)
C68 0.084(4) 0.062(3) 0.108(5) 0.018(3) -0.026(4) -0.023(3)
C69 0.069(3) 0.079(4) 0.079(4) 0.029(3) -0.026(3) -0.025(3)
C70 0.059(3) 0.076(3) 0.064(3) 0.014(2) -0.015(2) -0.016(2)
Cl1A 0.116(2) 0.172(3) 0.131(3) 0.079(2) -0.059(2) -0.053(2)
Cl2A 0.151(3) 0.138(3) 0.150(3) 0.053(2) -0.076(3) -0.049(2)
C1A 0.098(8) 0.133(11) 0.185(14) -0.002(10) -0.093(10) -0.018(7)
Cl1B 0.192(11) 0.208(11) 0.203(11) 0.001(8) -0.016(8) -0.064(9)
Cl2B 0.107(4) 0.119(5) 0.169(6) -0.060(4) -0.061(4) -0.015(3)
Cl1C 0.40(4) 0.093(9) 0.201(18) 0.015(10) -0.04(2) 0.040(14)
_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
Zn1 O1 1.913(3) . ?
Zn1 O2 1.918(3) . ?
Zn1 N1 2.014(4) . ?
Zn1 N4 2.007(3) . ?
Zn2 O3 1.920(3) . ?
Zn2 O4 1.910(3) . ?
Zn2 N7 2.000(4) . ?
Zn2 N10 2.003(4) . ?
O1 C12 1.291(5) . ?
O2 C19 1.291(5) . ?
O3 C41 1.296(5) . ?
O4 C64 1.296(6) . ?
N1 C2 1.434(6) . ?
N1 C10 1.282(5) . ?
N2A N3A 1.335(11) . ?
N2A C15 1.392(9) . ?
N3A C30A 1.415(10) . ?
N2B N3B 1.171(12) . ?
N2B C15 1.533(10) . ?
N3B C30B 1.427(10) . ?
N4 C6 1.448(5) . ?
N4 C17 1.299(5) . ?
N5 N6 1.259(5) . ?
N5 C22 1.402(5) . ?
N6 C24 1.440(6) . ?
N7 C36 1.441(5) . ?
N7 C39 1.279(5) . ?
N8 N9 1.241(5) . ?
N8 C44 1.415(6) . ?
N9 C46 1.411(6) . ?
N10 C52 1.442(5) . ?
N10 C58 1.290(5) . ?
N11 N12 1.261(5) . ?
N11 C61 1.406(6) . ?
N12 C65 1.419(6) . ?
C1 C2 1.405(5) 2_567 ?
C1 C6 1.382(6) . ?
C1 C7 1.511(6) . ?
C2 C1 1.405(5) 2_567 ?
C2 C3 1.392(6) . ?
C3 C4 1.379(7) . ?
C3 C8 1.518(6) . ?
C4 C5 1.382(6) 2_567 ?
C5 C4 1.382(6) 2_567 ?
C5 C6 1.389(6) . ?
C5 C9 1.503(7) . ?
C10 C11 1.438(7) . ?
C11 C12 1.423(7) . ?
C11 C16 1.404(6) . ?
C12 C13 1.417(6) . ?
C13 C14 1.347(7) . ?
C14 C15 1.396(8) . ?
C15 C16 1.377(7) . ?
C17 C18 1.437(5) . ?
C18 C19 1.418(5) . ?
C18 C23 1.393(6) . ?
C19 C20 1.420(6) . ?
C20 C21 1.369(6) . ?
C21 C22 1.410(6) . ?
C22 C23 1.389(6) . ?
C24 C25 1.397(6) . ?
C24 C29 1.377(7) . ?
C25 C26 1.402(7) . ?
C26 C27 1.350(8) . ?
C27 C28 1.388(8) . ?
C28 C29 1.378(7) . ?
C30A C31A 1.3900 . ?
C30A C35A 1.3900 . ?
C31A C32A 1.3900 . ?
C32A C33A 1.3900 . ?
C33A C34A 1.3900 . ?
C34A C35A 1.3900 . ?
C30B C31B 1.3900 . ?
C30B C35B 1.3900 . ?
C31B C32B 1.3900 . ?
C32B C33B 1.3900 . ?
C33B C34B 1.3900 . ?
C34B C35B 1.3900 . ?
C36 C37 1.390(6) . ?
C36 C53 1.400(5) 2_756 ?
C37 C38 1.506(6) . ?
C37 C57 1.386(7) 2_756 ?
C39 C40 1.432(6) . ?
C40 C41 1.416(6) . ?
C40 C45 1.407(6) . ?
C41 C42 1.404(6) . ?
C42 C43 1.366(7) . ?
C43 C44 1.404(7) . ?
C44 C45 1.372(6) . ?
C46 C47 1.390(7) . ?
C46 C51 1.375(8) . ?
C47 C48 1.343(8) . ?
C48 C49 1.345(9) . ?
C49 C50 1.374(9) . ?
C50 C51 1.363(8) . ?
C52 C53 1.388(6) . ?
C52 C55 1.403(6) . ?
C53 C36 1.400(5) 2_756 ?
C53 C54 1.510(6) . ?
C55 C56 1.499(6) . ?
C55 C57 1.380(6) . ?
C57 C37 1.386(7) 2_756 ?
C58 C59 1.443(5) . ?
C59 C60 1.396(6) . ?
C59 C64 1.423(6) . ?
C60 C61 1.384(6) . ?
C61 C62 1.394(7) . ?
C62 C63 1.340(7) . ?
C63 C64 1.419(6) . ?
C65 C66 1.398(8) . ?
C65 C70 1.380(6) . ?
C66 C67 1.357(8) . ?
C67 C68 1.371(8) . ?
C68 C69 1.357(9) . ?
C69 C70 1.382(8) . ?
Cl1A C1A 1.747(11) . ?
Cl2A C1A 1.810(13) . ?
Cl1B C1B 1.75(3) . ?
Cl2B C1B 1.76(3) . ?
Cl1C C1C 1.87(4) . ?
Cl2C C1C 1.83(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O2 111.47(13) . . ?
O1 Zn1 N1 95.25(14) . . ?
O1 Zn1 N4 125.14(14) . . ?
O2 Zn1 N1 116.46(14) . . ?
O2 Zn1 N4 95.65(12) . . ?
N4 Zn1 N1 114.40(14) . . ?
O3 Zn2 N7 95.74(14) . . ?
O3 Zn2 N10 123.97(16) . . ?
O4 Zn2 O3 108.91(15) . . ?
O4 Zn2 N7 122.89(17) . . ?
O4 Zn2 N10 95.53(14) . . ?
N7 Zn2 N10 112.13(14) . . ?
C12 O1 Zn1 125.0(3) . . ?
C19 O2 Zn1 126.3(3) . . ?
C41 O3 Zn2 125.6(3) . . ?
C64 O4 Zn2 126.5(3) . . ?
C2 N1 Zn1 121.2(3) . . ?
C10 N1 Zn1 121.0(3) . . ?
C10 N1 C2 117.6(4) . . ?
N3A N2A C15 108.4(8) . . ?
N2A N3A C30A 112.7(8) . . ?
N3B N2B C15 107.3(9) . . ?
N2B N3B C30B 108.9(8) . . ?
C6 N4 Zn1 122.2(2) . . ?
C17 N4 Zn1 120.4(3) . . ?
C17 N4 C6 116.7(3) . . ?
N6 N5 C22 114.4(4) . . ?
N5 N6 C24 112.7(4) . . ?
C36 N7 Zn2 123.4(3) . . ?
C39 N7 Zn2 120.6(3) . . ?
C39 N7 C36 115.4(4) . . ?
N9 N8 C44 114.3(4) . . ?
N8 N9 C46 114.0(4) . . ?
C52 N10 Zn2 122.3(3) . . ?
C58 N10 Zn2 121.3(3) . . ?
C58 N10 C52 115.8(3) . . ?
N12 N11 C61 115.2(4) . . ?
N11 N12 C65 113.6(4) . . ?
C2 C1 C7 120.0(4) 2_567 . ?
C6 C1 C2 117.5(4) . 2_567 ?
C6 C1 C7 122.5(4) . . ?
C1 C2 N1 118.5(4) 2_567 . ?
C3 C2 N1 119.9(4) . . ?
C3 C2 C1 121.5(4) . 2_567 ?
C2 C3 C8 120.7(4) . . ?
C4 C3 C2 118.2(4) . . ?
C4 C3 C8 121.0(4) . . ?
C3 C4 C5 122.4(4) . 2_567 ?
C4 C5 C6 117.8(4) 2_567 . ?
C4 C5 C9 120.5(4) 2_567 . ?
C6 C5 C9 121.6(4) . . ?
C1 C6 N4 118.7(4) . . ?
C1 C6 C5 122.5(4) . . ?
C5 C6 N4 118.8(4) . . ?
N1 C10 C11 126.9(4) . . ?
C12 C11 C10 124.8(4) . . ?
C16 C11 C10 115.5(5) . . ?
C16 C11 C12 119.6(4) . . ?
O1 C12 C11 124.4(4) . . ?
O1 C12 C13 119.4(4) . . ?
C13 C12 C11 116.2(4) . . ?
C14 C13 C12 122.9(5) . . ?
C13 C14 C15 121.0(5) . . ?
N2A C15 C14 108.2(6) . . ?
C14 C15 N2B 133.9(5) . . ?
C16 C15 N2A 133.4(6) . . ?
C16 C15 N2B 107.7(6) . . ?
C16 C15 C14 118.3(4) . . ?
C15 C16 C11 121.9(5) . . ?
N4 C17 C18 128.0(4) . . ?
C19 C18 C17 124.6(4) . . ?
C23 C18 C17 115.9(4) . . ?
C23 C18 C19 119.5(4) . . ?
O2 C19 C18 124.4(4) . . ?
O2 C19 C20 117.8(4) . . ?
C18 C19 C20 117.8(4) . . ?
C21 C20 C19 121.4(4) . . ?
C20 C21 C22 121.0(4) . . ?
N5 C22 C21 125.6(4) . . ?
C23 C22 N5 116.5(4) . . ?
C23 C22 C21 117.9(4) . . ?
C22 C23 C18 122.4(4) . . ?
C25 C24 N6 114.4(4) . . ?
C29 C24 N6 125.3(4) . . ?
C29 C24 C25 120.2(4) . . ?
C24 C25 C26 119.0(5) . . ?
C27 C26 C25 119.8(5) . . ?
C26 C27 C28 121.4(5) . . ?
C29 C28 C27 119.5(6) . . ?
C24 C29 C28 120.0(5) . . ?
C31A C30A N3A 114.1(7) . . ?
C31A C30A C35A 120.0 . . ?
C35A C30A N3A 125.9(7) . . ?
C30A C31A C32A 120.0 . . ?
C33A C32A C31A 120.0 . . ?
C34A C33A C32A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C34A C35A C30A 120.0 . . ?
C31B C30B N3B 124.8(6) . . ?
C31B C30B C35B 120.0 . . ?
C35B C30B N3B 115.2(6) . . ?
C32B C31B C30B 120.0 . . ?
C31B C32B C33B 120.0 . . ?
C34B C33B C32B 120.0 . . ?
C33B C34B C35B 120.0 . . ?
C34B C35B C30B 120.0 . . ?
C37 C36 N7 119.5(4) . . ?
C37 C36 C53 122.5(4) . 2_756 ?
C53 C36 N7 117.9(4) 2_756 . ?
C36 C37 C38 121.0(4) . . ?
C57 C37 C36 118.0(4) 2_756 . ?
C57 C37 C38 121.0(4) 2_756 . ?
N7 C39 C40 128.0(4) . . ?
C41 C40 C39 124.9(4) . . ?
C45 C40 C39 115.3(4) . . ?
C45 C40 C41 119.7(4) . . ?
O3 C41 C40 123.9(4) . . ?
O3 C41 C42 119.5(4) . . ?
C42 C41 C40 116.7(4) . . ?
C43 C42 C41 122.7(5) . . ?
C42 C43 C44 120.7(4) . . ?
C43 C44 N8 125.8(4) . . ?
C45 C44 N8 116.3(4) . . ?
C45 C44 C43 117.9(4) . . ?
C44 C45 C40 122.3(5) . . ?
C47 C46 N9 117.4(5) . . ?
C51 C46 N9 124.3(4) . . ?
C51 C46 C47 118.2(5) . . ?
C48 C47 C46 121.4(6) . . ?
C47 C48 C49 120.0(6) . . ?
C48 C49 C50 120.2(6) . . ?
C51 C50 C49 120.4(7) . . ?
C50 C51 C46 119.7(6) . . ?
C53 C52 N10 118.7(4) . . ?
C53 C52 C55 122.7(4) . . ?
C55 C52 N10 118.6(4) . . ?
C36 C53 C54 121.2(4) 2_756 . ?
C52 C53 C36 116.8(4) . 2_756 ?
C52 C53 C54 122.0(4) . . ?
C52 C55 C56 121.0(4) . . ?
C57 C55 C52 117.6(4) . . ?
C57 C55 C56 121.3(4) . . ?
C55 C57 C37 122.4(4) . 2_756 ?
N10 C58 C59 127.1(4) . . ?
C60 C59 C58 115.6(4) . . ?
C60 C59 C64 119.5(4) . . ?
C64 C59 C58 124.9(4) . . ?
C61 C60 C59 121.7(4) . . ?
C60 C61 N11 115.9(4) . . ?
C60 C61 C62 118.3(4) . . ?
C62 C61 N11 125.8(4) . . ?
C63 C62 C61 121.4(4) . . ?
C62 C63 C64 122.2(5) . . ?
O4 C64 C59 123.5(4) . . ?
O4 C64 C63 119.7(4) . . ?
C63 C64 C59 116.8(4) . . ?
C66 C65 N12 123.8(4) . . ?
C70 C65 N12 116.4(5) . . ?
C70 C65 C66 119.8(5) . . ?
C67 C66 C65 118.0(5) . . ?
C66 C67 C68 122.6(6) . . ?
C69 C68 C67 119.5(6) . . ?
C68 C69 C70 119.8(5) . . ?
C65 C70 C69 120.2(6) . . ?
Cl1A C1A Cl2A 109.6(9) . . ?
Cl1B C1B Cl2B 117(3) . . ?
Cl2C C1C Cl1C 93(3) . . ?
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full 72.87
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max 1.363
_refine_diff_density_min -0.958
_refine_diff_density_rms 0.089
_database_code_depnum_ccdc_archive 'CCDC 941802'
_iucr_refine_instructions_details
;
TITL 1
CELL 1.54184 13.0742 15.6117 17.5354 82.851 68.389 77.788
ZERR 2 0.0008 0.0012 0.0011 0.006 0.006 0.006
LATT 1
SFAC C H Cl N O Zn
DISP C 0.018 0.009
DISP H 0 0
DISP N 0.031 0.018
DISP O 0.049 0.032
DISP Zn -1.549 0.678
UNIT 142.4 116.8 4.8 24 8 4
SADI Cl1A C1A Cl2A C1A
SADI Cl1B C1B Cl2B C1B
SADI Cl2C C1C Cl1C C1C
EADP C30B C30A
EADP N3A N3B
EADP N2A N2B
EADP C35A C35B
EADP C31B C31A
EADP C33A C33B
EADP C34B C34A
EADP C32A C32B
EADP C31A C31B
L.S. 7
PLAN 6
SIZE 0.33 0.26 0.21
TEMP -123(2)
fmap 2 53
acta 145.7
OMIT 0 1 0
OMIT 0 -1 1
REM I:/andrei/RSC/DT-ART-07-2013-051821.R4/1.hkl
WGHT 0.142 1.5
FVAR 3.2823
Zn1 6 0.16737 0.37557 0.82851 11.00000 0.04337 0.06023 0.04127 =
0.00142 -0.00931 0.00221
Zn2 6 0.72795 0.02463 0.65233 11.00000 0.04778 0.05071 0.05364 =
0.00156 0.00148 -0.00093
O1 5 0.22898 0.25309 0.83074 11.00000 0.05159 0.06025 0.05433 =
-0.00474 -0.01759 0.00575
O2 5 0.21594 0.42794 0.71918 11.00000 0.04182 0.07358 0.04457 =
0.00569 -0.00829 0.00194
O3 5 0.60192 0.11003 0.64539 11.00000 0.04785 0.05702 0.07386 =
0.00082 -0.00455 -0.00150
O4 5 0.68272 -0.04282 0.75383 11.00000 0.08693 0.05241 0.04978 =
-0.00077 0.00817 -0.00149
N1 4 0.23352 0.40675 0.90628 11.00000 0.04310 0.05921 0.04168 =
-0.00322 -0.00730 -0.00349
PART 1
N2A 4 0.57105 0.07320 0.92960 10.50000 0.05264
N3A 4 0.59873 0.11004 0.98229 10.50000 0.06218
PART 0
PART 2
N2B 4 0.58284 0.10661 0.94411 10.50000 0.05264
N3B 4 0.62026 0.03245 0.93181 10.50000 0.06218
PART 0
N4 4 0.00450 0.42608 0.85464 11.00000 0.03670 0.05302 0.04063 =
0.00032 -0.00770 -0.00208
N5 4 -0.04478 0.60716 0.54334 11.00000 0.06301 0.06317 0.04212 =
0.00180 -0.01975 -0.01070
N6 4 0.00570 0.63224 0.47046 11.00000 0.06153 0.06217 0.04678 =
0.00003 -0.01827 -0.00676
N7 4 0.83139 0.11017 0.62910 11.00000 0.04321 0.05596 0.04392 =
0.00259 -0.00337 -0.00186
N8 4 0.56364 0.47216 0.62448 11.00000 0.05046 0.06120 0.05660 =
0.00615 -0.00704 0.00144
N9 4 0.47896 0.51541 0.61276 11.00000 0.05256 0.06536 0.05072 =
0.00630 -0.00631 0.00270
N10 4 0.79727 -0.07882 0.58180 11.00000 0.04321 0.05302 0.04556 =
0.00257 -0.00373 -0.00154
N11 4 0.68956 -0.40008 0.79953 11.00000 0.05334 0.05656 0.05270 =
0.00873 -0.01012 -0.00856
N12 4 0.64666 -0.43090 0.87176 11.00000 0.05064 0.06159 0.05065 =
0.00695 -0.00498 -0.00562
C1 1 -0.11701 0.50987 0.97327 11.00000 0.03976 0.05695 0.03902 =
0.00387 -0.00734 -0.00577
C2 1 0.19310 0.48877 0.94553 11.00000 0.04002 0.06191 0.04481 =
-0.00048 -0.00813 -0.00560
C3 1 0.22376 0.56552 0.90141 11.00000 0.04741 0.06725 0.04381 =
0.00288 -0.00455 -0.01157
C4 1 0.17770 0.64382 0.93967 11.00000 0.05369 0.06310 0.04798 =
0.01381 -0.00757 -0.01609
AFIX 43
H4 2 0.19835 0.69649 0.91010 11.00000 -1.20000
AFIX 0
C5 1 -0.10261 0.35155 0.98056 11.00000 0.04602 0.05658 0.05031 =
0.00541 -0.01374 -0.00578
C6 1 -0.07492 0.42950 0.93806 11.00000 0.03732 0.06225 0.03897 =
0.00467 -0.00778 -0.00501
C7 1 -0.08260 0.59402 0.92826 11.00000 0.05077 0.05868 0.04218 =
0.00111 -0.00723 -0.00355
AFIX 137
H7a 2 -0.13866 0.62451 0.90472 11.00000 -1.50000
H7b 2 -0.00992 0.58045 0.88414 11.00000 -1.50000
H7c 2 -0.07691 0.63171 0.96670 11.00000 -1.50000
AFIX 0
C8 1 0.30960 0.56239 0.81490 11.00000 0.06382 0.08946 0.04803 =
0.00643 0.00490 -0.01701
AFIX 137
H8a 2 0.38204 0.53054 0.81635 11.00000 -1.50000
H8b 2 0.31675 0.62231 0.79207 11.00000 -1.50000
H8c 2 0.28541 0.53230 0.78043 11.00000 -1.50000
AFIX 0
C9 1 -0.05860 0.26522 0.94017 11.00000 0.06159 0.06029 0.06176 =
0.00468 -0.00596 -0.00622
AFIX 137
H9a 2 -0.08475 0.21793 0.98048 11.00000 -1.50000
H9b 2 0.02334 0.25488 0.91894 11.00000 -1.50000
H9c 2 -0.08569 0.26655 0.89477 11.00000 -1.50000
AFIX 0
C10 1 0.30810 0.35155 0.92660 11.00000 0.04133 0.07354 0.04576 =
-0.00153 -0.00998 -0.00366
AFIX 43
H10 2 0.33715 0.37115 0.96232 11.00000 -1.20000
AFIX 0
C11 1 0.35239 0.26308 0.90101 11.00000 0.04186 0.06896 0.04225 =
0.00091 -0.00715 0.00335
C12 1 0.31137 0.21892 0.85508 11.00000 0.04520 0.05912 0.04219 =
0.00655 -0.00693 -0.00101
C13 1 0.36524 0.13115 0.83715 11.00000 0.05593 0.06688 0.05113 =
-0.00323 -0.01082 0.00357
AFIX 43
H13 2 0.34056 0.09980 0.80611 11.00000 -1.20000
AFIX 0
C14 1 0.44992 0.09018 0.86218 11.00000 0.05430 0.06281 0.05369 =
0.00911 -0.00577 0.00783
AFIX 43
H14 2 0.48356 0.03140 0.84806 11.00000 -1.20000
AFIX 0
C15 1 0.48895 0.13283 0.90854 11.00000 0.04728 0.09048 0.04662 =
0.01071 -0.00682 0.01008
C16 1 0.43993 0.21849 0.92702 11.00000 0.04519 0.08749 0.04962 =
0.00059 -0.01408 0.00337
AFIX 43
H16 2 0.46610 0.24827 0.95829 11.00000 -1.20000
AFIX 0
C17 1 -0.03088 0.46823 0.79785 11.00000 0.03959 0.05186 0.04586 =
0.00018 -0.01117 -0.00298
AFIX 43
H17 2 -0.10929 0.48841 0.81383 11.00000 -1.20000
AFIX 0
C18 1 0.03403 0.48810 0.71380 11.00000 0.04144 0.05153 0.04368 =
0.00333 -0.01104 -0.00236
C19 1 0.15245 0.46845 0.67951 11.00000 0.04244 0.05918 0.04632 =
-0.00035 -0.00956 -0.00345
C20 1 0.20470 0.49638 0.59636 11.00000 0.04358 0.07172 0.04965 =
0.00377 -0.00809 -0.00576
AFIX 43
H20 2 0.28394 0.48410 0.57212 11.00000 -1.20000
AFIX 0
C21 1 0.14335 0.54062 0.55036 11.00000 0.05449 0.06832 0.04448 =
0.00781 -0.01057 -0.00943
AFIX 43
H21 2 0.18062 0.55794 0.49471 11.00000 -1.20000
AFIX 0
C22 1 0.02563 0.56086 0.58438 11.00000 0.05310 0.05253 0.04469 =
0.00195 -0.01267 -0.00521
C23 1 -0.02614 0.53295 0.66538 11.00000 0.04566 0.05724 0.04765 =
-0.00224 -0.01088 -0.00482
AFIX 43
H23 2 -0.10548 0.54489 0.68864 11.00000 -1.20000
AFIX 0
C24 1 -0.06938 0.67799 0.42985 11.00000 0.07224 0.05779 0.04788 =
0.00040 -0.02717 -0.01031
C25 1 -0.01641 0.70745 0.34895 11.00000 0.07730 0.07176 0.05144 =
-0.00068 -0.02542 -0.01253
AFIX 43
H25 2 0.06278 0.69526 0.32429 11.00000 -1.20000
AFIX 0
C26 1 -0.08185 0.75526 0.30472 11.00000 0.09848 0.06960 0.05257 =
0.00325 -0.03463 -0.01298
AFIX 43
H26 2 -0.04714 0.77650 0.24992 11.00000 -1.20000
AFIX 0
C27 1 -0.19436 0.77101 0.34026 11.00000 0.09454 0.07815 0.07058 =
0.00097 -0.04626 -0.00776
AFIX 43
H27 2 -0.23813 0.80385 0.31005 11.00000 -1.20000
AFIX 0
C28 1 -0.24747 0.74024 0.42001 11.00000 0.07360 0.08303 0.06874 =
-0.01309 -0.03594 0.00218
AFIX 43
H28 2 -0.32676 0.75165 0.44391 11.00000 -1.20000
AFIX 0
C29 1 -0.18432 0.69303 0.46425 11.00000 0.06949 0.07764 0.05263 =
-0.00526 -0.02508 -0.00678
AFIX 43
H29 2 -0.22010 0.67084 0.51850 11.00000 -1.20000
AFIX 0
PART 1
AFIX 66
C30A 1 0.69019 0.05814 1.00074 10.50000 0.05613 0.08908 0.06809 =
0.03067 -0.02442 -0.02118
C31A 1 0.71250 0.08947 1.06272 10.50000 0.08979 0.07282 0.11536 =
0.03249 -0.05717 -0.02131
AFIX 43
H31A 2 0.66803 0.14170 1.08832 10.50000 -1.20000
AFIX 0
AFIX 65
C32A 1 0.79988 0.04440 1.08726 10.50000 0.11093 0.09404 0.16236 =
0.05293 -0.08558 -0.04272
AFIX 43
H32A 2 0.81513 0.06581 1.12963 10.50000 -1.20000
AFIX 0
AFIX 65
C33A 1 0.86495 -0.03202 1.04982 10.50000 0.08243
AFIX 43
H33A 2 0.92467 -0.06282 1.06659 10.50000 -1.20000
AFIX 0
AFIX 65
C34A 1 0.84264 -0.06335 0.98783 10.50000 0.06593 0.07611 0.09868 =
0.02020 -0.01808 0.00665
AFIX 43
H34A 2 0.88711 -0.11558 0.96224 10.50000 -1.20000
AFIX 0
AFIX 65
C35A 1 0.75526 -0.01827 0.96329 10.50000 0.05676 0.09636 0.07322 =
0.02470 -0.01625 -0.00047
AFIX 43
H35A 2 0.74001 -0.03969 0.92093 10.50000 -1.20000
AFIX 0
PART 0
PART 2
AFIX 66
C30B 1 0.71047 0.00621 0.96191 10.50000 0.05613 0.08908 0.06809 =
0.03067 -0.02442 -0.02118
C31B 1 0.73860 0.05749 1.00794 10.50000 0.08979 0.07282 0.11536 =
0.03249 -0.05717 -0.02131
AFIX 43
H31B 2 0.69705 0.11485 1.02092 10.50000 -1.20000
AFIX 0
AFIX 65
C32B 1 0.82755 0.02486 1.03499 10.50000 0.11093 0.09404 0.16236 =
0.05293 -0.08558 -0.04272
AFIX 43
H32B 2 0.84678 0.05991 1.06645 10.50000 -1.20000
AFIX 0
AFIX 65
C33B 1 0.88835 -0.05905 1.01600 10.50000 0.08243
AFIX 43
H33B 2 0.94914 -0.08135 1.03448 10.50000 -1.20000
AFIX 0
AFIX 65
C34B 1 0.86022 -0.11034 0.96996 10.50000 0.06593 0.07611 0.09868 =
0.02020 -0.01808 0.00665
AFIX 43
H34B 2 0.90177 -0.16769 0.95698 10.50000 -1.20000
AFIX 0
AFIX 65
C35B 1 0.77127 -0.07770 0.94292 10.50000 0.05676 0.09636 0.07322 =
0.02470 -0.01625 -0.00047
AFIX 43
H35B 2 0.75204 -0.11275 0.91146 10.50000 -1.20000
AFIX 0
PART 0
C36 1 0.95091 0.08446 0.60624 11.00000 0.04291 0.05068 0.04633 =
0.00519 -0.00830 -0.00547
C37 1 0.99633 0.04861 0.66591 11.00000 0.06705 0.05579 0.04480 =
0.00432 -0.01567 -0.00391
C38 1 0.92281 0.03905 0.75465 11.00000 0.07173 0.09635 0.04416 =
0.01051 -0.01018 -0.00717
AFIX 137
H38a 2 0.88351 0.09710 0.77491 11.00000 -1.50000
H38b 2 0.96898 0.01135 0.78725 11.00000 -1.50000
H38c 2 0.86811 0.00247 0.75952 11.00000 -1.50000
AFIX 0
C39 1 0.79567 0.19266 0.62300 11.00000 0.04922 0.05321 0.04467 =
0.00396 -0.00621 -0.00755
AFIX 43
H39 2 0.84996 0.22926 0.61006 11.00000 -1.20000
AFIX 0
C40 1 0.68390 0.23667 0.63328 11.00000 0.04901 0.05581 0.04631 =
0.00020 -0.00400 -0.00348
C41 1 0.59365 0.19440 0.64353 11.00000 0.04622 0.05257 0.04964 =
0.00482 -0.00325 -0.00140
C42 1 0.49018 0.24881 0.65207 11.00000 0.04677 0.06441 0.06150 =
0.00475 -0.00647 -0.00561
AFIX 43
H42 2 0.42705 0.22233 0.66209 11.00000 -1.20000
AFIX 0
C43 1 0.47656 0.33826 0.64655 11.00000 0.04244 0.06360 0.05899 =
0.00268 -0.00612 0.00236
AFIX 43
H43 2 0.40517 0.37235 0.65170 11.00000 -1.20000
AFIX 0
C44 1 0.56691 0.38039 0.63337 11.00000 0.05090 0.05535 0.05364 =
0.00362 -0.00659 0.00038
C45 1 0.66795 0.32890 0.62833 11.00000 0.05061 0.05903 0.05359 =
0.00522 -0.01029 -0.00517
AFIX 43
H45 2 0.72926 0.35647 0.62126 11.00000 -1.20000
AFIX 0
C46 1 0.47491 0.60696 0.60584 11.00000 0.05203 0.05821 0.05845 =
0.00691 -0.00863 -0.00293
C47 1 0.39753 0.65853 0.57440 11.00000 0.07722 0.06865 0.06522 =
0.00219 -0.02777 0.00112
AFIX 43
H47 2 0.35025 0.63118 0.55891 11.00000 -1.20000
AFIX 0
C48 1 0.38819 0.74619 0.56546 11.00000 0.07769 0.07291 0.07185 =
0.00579 -0.02598 0.00350
AFIX 43
H48 2 0.33772 0.77990 0.54096 11.00000 -1.20000
AFIX 0
C49 1 0.45025 0.78630 0.59118 11.00000 0.08226 0.05846 0.12105 =
0.01973 -0.02741 -0.00106
AFIX 43
H49 2 0.44352 0.84834 0.58483 11.00000 -1.20000
AFIX 0
C50 1 0.52338 0.73776 0.62661 11.00000 0.08439 0.06118 0.20782 =
0.01191 -0.07752 -0.01109
AFIX 43
H50 2 0.56532 0.76658 0.64618 11.00000 -1.20000
AFIX 0
C51 1 0.53613 0.64851 0.63386 11.00000 0.06816 0.05969 0.13924 =
0.01173 -0.04498 -0.00168
AFIX 43
H51 2 0.58705 0.61518 0.65815 11.00000 -1.20000
AFIX 0
C52 1 0.86826 -0.07070 0.49687 11.00000 0.04594 0.04805 0.04176 =
0.00301 -0.00574 -0.00167
C53 1 0.98306 -0.09633 0.47645 11.00000 0.04374 0.04436 0.04762 =
0.00127 -0.00885 -0.00063
C54 1 1.03525 -0.13303 0.54019 11.00000 0.04455 0.05433 0.04467 =
0.00517 -0.00620 0.00083
AFIX 137
H54a 2 1.04324 -0.19712 0.54467 11.00000 -1.50000
H54b 2 0.98731 -0.10909 0.59342 11.00000 -1.50000
H54c 2 1.10905 -0.11671 0.52387 11.00000 -1.50000
AFIX 0
C55 1 0.81863 -0.03470 0.43872 11.00000 0.05133 0.04925 0.05296 =
0.00133 -0.01325 -0.00078
C56 1 0.69399 -0.01229 0.46253 11.00000 0.05412 0.07297 0.07093 =
0.00372 -0.02163 0.00321
AFIX 137
H56a 2 0.66148 -0.06475 0.48687 11.00000 -1.50000
H56b 2 0.67483 0.00914 0.41365 11.00000 -1.50000
H56c 2 0.66417 0.03341 0.50262 11.00000 -1.50000
AFIX 0
C57 1 0.88839 -0.02485 0.35823 11.00000 0.05609 0.06150 0.05393 =
0.00625 -0.01829 -0.00092
AFIX 43
H57 2 0.85624 -0.00092 0.31793 11.00000 -1.20000
AFIX 0
C58 1 0.79217 -0.15792 0.61275 11.00000 0.04376 0.05094 0.04221 =
-0.00217 -0.00883 -0.00053
AFIX 43
H58 2 0.83040 -0.20374 0.57603 11.00000 -1.20000
AFIX 0
C59 1 0.73470 -0.18433 0.69710 11.00000 0.04592 0.05346 0.04379 =
0.00213 -0.00556 -0.00407
C60 1 0.73494 -0.27420 0.71336 11.00000 0.04773 0.05574 0.04125 =
0.00101 -0.00420 -0.00471
AFIX 43
H60 2 0.77237 -0.31282 0.66973 11.00000 -1.20000
AFIX 0
C61 1 0.68200 -0.30847 0.79144 11.00000 0.05416 0.05648 0.04653 =
0.00600 -0.00800 -0.00396
C62 1 0.62709 -0.25070 0.85458 11.00000 0.07830 0.06795 0.04304 =
0.00394 0.00520 -0.00564
AFIX 43
H62 2 0.58792 -0.27297 0.90804 11.00000 -1.20000
AFIX 0
C63 1 0.62836 -0.16445 0.84149 11.00000 0.09101 0.06346 0.04605 =
-0.00219 0.00418 0.00102
AFIX 43
H63 2 0.59213 -0.12753 0.88653 11.00000 -1.20000
AFIX 0
C64 1 0.68198 -0.12640 0.76267 11.00000 0.05753 0.05417 0.04954 =
0.00155 0.00219 -0.00044
C65 1 0.65529 -0.52346 0.87743 11.00000 0.04754 0.06751 0.05743 =
0.01414 -0.01305 -0.01421
C66 1 0.68717 -0.57447 0.80958 11.00000 0.10100 0.07193 0.06294 =
0.00994 -0.01228 -0.02361
AFIX 43
H66 2 0.70138 -0.54807 0.75573 11.00000 -1.20000
AFIX 0
C67 1 0.69718 -0.66283 0.82296 11.00000 0.11833 0.07126 0.07548 =
0.00353 -0.01451 -0.03149
AFIX 43
H67 2 0.71860 -0.69814 0.77731 11.00000 -1.20000
AFIX 0
C68 1 0.67761 -0.70316 0.89976 11.00000 0.08393 0.06216 0.10849 =
0.01841 -0.02626 -0.02277
AFIX 43
H68 2 0.68700 -0.76531 0.90665 11.00000 -1.20000
AFIX 0
C69 1 0.64475 -0.65368 0.96588 11.00000 0.06906 0.07865 0.07911 =
0.02944 -0.02558 -0.02547
AFIX 43
H69 2 0.62999 -0.68105 1.01941 11.00000 -1.20000
AFIX 0
C70 1 0.63280 -0.56336 0.95517 11.00000 0.05902 0.07564 0.06445 =
0.01423 -0.01461 -0.01573
AFIX 43
H70 2 0.60901 -0.52864 1.00149 11.00000 -1.20000
AFIX 0
PART 1
Cl1A 3 -0.02993 0.75477 0.75047 10.67000 0.11601 0.17207 0.13105 =
0.07888 -0.05886 -0.05302
Cl2A 3 0.15481 0.81130 0.77288 10.67000 0.15068 0.13759 0.14989 =
0.05288 -0.07611 -0.04857
C1A 1 0.11407 0.72996 0.73010 10.67000 0.09758 0.13346 0.18472 =
-0.00152 -0.09318 -0.01807
AFIX 23
H1Aa 2 0.15473 0.72932 0.67003 10.67000 -1.20000
H1Ab 2 0.13376 0.67104 0.75461 10.67000 -1.20000
AFIX 0
PART 0
PART 2
Cl1B 3 0.27907 0.85236 0.78331 10.33000 0.19215 0.20783 0.20340 =
0.00103 -0.01623 -0.06438
Cl2B 3 0.46146 0.95535 0.69406 10.33000 0.10707 0.11889 0.16927 =
-0.06011 -0.06085 -0.01451
C1B 1 0.40940 0.87557 0.77123 10.33000 0.22147
AFIX 23
H1Ba 2 0.46466 0.82028 0.75967 10.33000 -1.20000
H1Bb 2 0.40478 0.89488 0.82427 10.33000 -1.20000
AFIX 0
PART 0
PART 3
Cl1C 3 -0.00669 0.81343 0.83001 10.20000 0.40143 0.09339 0.20068 =
0.01508 -0.04384 0.04048
Cl2C 3 0.07229 0.70180 0.70713 10.20000 0.13038
C1C 1 0.11094 0.79985 0.72867 10.20000 0.12017
AFIX 23
H1Ca 2 0.10544 0.84961 0.68859 10.20000 -1.20000
H1Cb 2 0.18559 0.78827 0.73386 10.20000 -1.20000
AFIX 0
HKLF 4
END
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