# Electronic Supplementary Material (ESI) for Nanoscale.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
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# Crystallographic Data Centre (CCDC).
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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data_CC2-R_para-xylene
_database_code_depnum_ccdc_archive 'CCDC 1520508'
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_audit_creation_date 2015-07-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C54 H60 N12, 1.7(C8 H10)'
_chemical_formula_sum 'C67.59 H76.99 N12'
_chemical_formula_weight 1057.51
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a 11.1553(19)
_cell_length_b 19.490(4)
_cell_length_c 30.332(6)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 6595(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9950
_cell_measurement_temperature 100
_cell_measurement_theta_max 23.76
_cell_measurement_theta_min 2.20
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.060
_exptl_absorpt_correction_T_max 0.9280
_exptl_absorpt_correction_T_min 0.8285
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0829 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.8928.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.065
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 2266
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0507
_diffrn_reflns_av_unetI/netI 0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 34167
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 22.400
_diffrn_reflns_theta_max 22.501
_diffrn_reflns_theta_min 1.649
_diffrn_ambient_temperature 100.0
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type 'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation 0.3
_diffrn_radiation_monochromator Confocal
_diffrn_radiation_probe x-ray
_diffrn_radiation_type ?
_diffrn_radiation_wavelength 0.6889
_diffrn_source 'Rotating Anode'
_diffrn_source_current 24.0
_diffrn_source_power 1.2
_diffrn_source_target Mo
_diffrn_source_type 'Rotating Anode'
_diffrn_source_voltage 50.0
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.794
_reflns_Friedel_fraction_full 0.996
_reflns_Friedel_fraction_max 0.996
_reflns_number_gt 7494
_reflns_number_total 9431
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution ?
_refine_diff_density_max 0.537
_refine_diff_density_min -0.313
_refine_diff_density_rms 0.070
_refine_ls_abs_structure_details
;
Flack x determined using 2894 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -1.0(10)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 749
_refine_ls_number_reflns 9431
_refine_ls_number_restraints 76
_refine_ls_R_factor_all 0.0948
_refine_ls_R_factor_gt 0.0786
_refine_ls_restrained_S_all 1.084
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1520P)^2^+0.6927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2120
_refine_ls_wR_factor_ref 0.2297
_refine_special_details ?
_olex2_refinement_description
;
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
C75-C72
1.52 with sigma of 0.02
C68-C74
1.52 with sigma of 0.02
C74-C68 = C75-C72 = C71-C77 = C69-C76
1.49 with sigma of 0.02
C68-C76 \\sim C76-C70
with sigma of 0.02
C73-C75 \\sim C71-C75
with sigma of 0.02
C73-C75 \\sim C75-C71
with sigma of 0.02
C72-C77 \\sim C77-C70
with sigma of 0.02
C69-C74 \\sim C73-C74
with sigma of 0.02
C73-C74 \\sim C74-C69
with sigma of 0.02
3. Restrained planarity
C60, C61, C62, C63, C64, C65, C66, C67
with sigma of 0.001
C68, C69, C70, C71, C72, C73, C74, C75, C76, C77
with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uiso(C73) = Uiso(C68) = Uiso(C69) = Uiso(C74) = Uiso(C70) = Uiso(C76) =
Uiso(C72) = Uiso(C71) = Uiso(C75) = Uiso(C77)
5. Rigid body (RIGU) restrains
C66, C60, C61, C62, C63, C64, C65, C67
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(H48B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=1-FVAR(1)
Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
Sof(H52B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(2)
Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
Sof(H37B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(3)
Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(3)
Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=1-FVAR(4)
Sof(H56B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(4)
Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(5)
Sof(H41B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(5)
Sof(H68)=Sof(H69)=Sof(H71)=Sof(H72)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=
Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=0.5*FVAR(7)
Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=
Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=
Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(C69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(C72)=
Sof(C73)=Sof(H73)=FVAR(6)
7.a Ternary CH refined with riding coordinates:
C46(H46)
7.b Secondary CH2 refined with riding coordinates:
C37(H37A,H37B), C38(H38A,H38B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,
H45B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B), C53(H53A,H53B),
C56(H56A,H56B), C57(H57A,H57B)
7.c Me refined with riding coordinates:
C59(H59A,H59B,H59C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,
H76C), C77(H77A,H77B,H77C)
7.d Aromatic/amide H refined with riding coordinates:
C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26),
C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
C61(H61), C62(H62), C63(H63), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71),
C72(H72), C73(H73)
7.e Fitted hexagon refined as free rotating group:
C68(C69,C70,C71,C72,C73)
7.f Idealised Me refined as rotating group:
C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C55(H55A,H55B,
H55C), C54(H54A,H54B,H54C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C58(H58A,
H58B,H58C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C66(H66A,H66B,H66C),
C67(H67A,H67B,H67C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
N1 N 0.2922(5) 0.4386(3) 0.6608(3) 0.1011(19) Uani 1 1 d . . . . .
N2 N 0.3133(5) 0.4893(3) 0.7506(2) 0.0921(18) Uani 1 1 d . . . . .
N3 N 0.7687(5) 0.6588(3) 0.81988(18) 0.0807(15) Uani 1 1 d . . . . .
N4 N 0.9979(4) 0.6569(3) 0.77024(17) 0.0755(13) Uani 1 1 d . . . . .
N5 N 0.7283(4) 0.9525(2) 0.59298(18) 0.0710(13) Uani 1 1 d . . . . .
N6 N 0.9584(4) 0.8765(3) 0.61647(16) 0.0661(12) Uani 1 1 d . . . . .
N7 N 0.2685(4) 0.8131(3) 0.78332(18) 0.0785(14) Uani 1 1 d . . . . .
N8 N 0.2699(4) 0.9270(3) 0.71913(19) 0.0747(13) Uani 1 1 d . . . . .
N9 N 0.2609(4) 0.8022(3) 0.52127(17) 0.0755(13) Uani 1 1 d . . . . .
N10 N 0.3222(4) 0.6548(3) 0.50445(19) 0.0780(14) Uani 1 1 d . . . . .
N11 N 0.7839(4) 0.4698(3) 0.5501(2) 0.0824(15) Uani 1 1 d . . . . .
N12 N 1.0007(4) 0.5542(2) 0.56917(18) 0.0694(12) Uani 1 1 d . . . . .
C1 C 0.4169(5) 0.7230(3) 0.7804(2) 0.0732(16) Uani 1 1 d . . . . .
C2 C 0.5338(5) 0.7055(3) 0.7910(2) 0.0777(16) Uani 1 1 d . . . . .
H2 H 0.5878 0.7401 0.8006 0.093 Uiso 1 1 calc R . . . .
C3 C 0.5729(5) 0.6379(3) 0.7877(2) 0.0734(16) Uani 1 1 d . . . . .
C4 C 0.4945(6) 0.5886(3) 0.7740(2) 0.0771(16) Uani 1 1 d . . . . .
H4 H 0.5206 0.5423 0.7719 0.093 Uiso 1 1 calc R . . . .
C5 C 0.3757(6) 0.6053(3) 0.7630(2) 0.0754(16) Uani 1 1 d . . . . .
C6 C 0.3394(5) 0.6719(3) 0.7664(2) 0.0757(17) Uani 1 1 d . . . . .
H6 H 0.2591 0.6835 0.7590 0.091 Uiso 1 1 calc R . . . .
C7 C 0.3756(6) 0.7943(3) 0.7861(2) 0.0835(18) Uani 1 1 d . . . . .
H7 H 0.4342 0.8283 0.7924 0.100 Uiso 1 1 calc R . . . .
C8 C 0.6940(6) 0.6172(4) 0.8029(2) 0.0774(17) Uani 1 1 d . . . . .
H8 H 0.7169 0.5706 0.7998 0.093 Uiso 1 1 calc R . . . .
C9 C 0.2909(6) 0.5521(3) 0.7497(2) 0.0783(17) Uani 1 1 d . . . . .
H9 H 0.2140 0.5661 0.7397 0.094 Uiso 1 1 calc R . . . .
C10 C 0.3298(5) 0.9034(3) 0.6446(2) 0.0750(17) Uani 1 1 d . . . . .
C11 C 0.3007(5) 0.8725(3) 0.6054(2) 0.0793(17) Uani 1 1 d . . . . .
H11 H 0.2242 0.8518 0.6021 0.095 Uiso 1 1 calc R . . . .
C12 C 0.3825(5) 0.8712(3) 0.5700(2) 0.0746(16) Uani 1 1 d . . . . .
C13 C 0.4933(5) 0.9014(3) 0.5753(2) 0.0748(15) Uani 1 1 d . . . . .
H13 H 0.5483 0.9017 0.5514 0.090 Uiso 1 1 calc R . . . .
C14 C 0.5261(5) 0.9319(3) 0.6156(2) 0.0765(17) Uani 1 1 d . . . . .
C15 C 0.4456(5) 0.9329(3) 0.6498(2) 0.0784(17) Uani 1 1 d . . . . .
H15 H 0.4672 0.9535 0.6770 0.094 Uiso 1 1 calc R . . . .
C16 C 0.2460(6) 0.9012(3) 0.6814(3) 0.0819(18) Uani 1 1 d . . . . .
H16 H 0.1705 0.8796 0.6772 0.098 Uiso 1 1 calc R . . . .
C17 C 0.3553(5) 0.8351(3) 0.5287(2) 0.0751(16) Uani 1 1 d . . . . .
H17 H 0.4136 0.8367 0.5059 0.090 Uiso 1 1 calc R . . . .
C18 C 0.6489(6) 0.9587(3) 0.6220(2) 0.0737(16) Uani 1 1 d . . . . .
H18 H 0.6682 0.9813 0.6488 0.088 Uiso 1 1 calc R . . . .
C19 C 1.0073(4) 0.7010(3) 0.69642(18) 0.0618(14) Uani 1 1 d . . . . .
C20 C 0.9977(4) 0.7599(3) 0.67148(18) 0.0610(13) Uani 1 1 d . . . . .
H20 H 0.9935 0.8033 0.6856 0.073 Uiso 1 1 calc R . . . .
C21 C 0.9940(4) 0.7561(3) 0.62533(18) 0.0610(13) Uani 1 1 d . . . . .
C22 C 1.0011(4) 0.6931(3) 0.60510(19) 0.0618(13) Uani 1 1 d . . . . .
H22 H 1.0001 0.6903 0.5738 0.074 Uiso 1 1 calc R . . . .
C23 C 1.0099(4) 0.6319(3) 0.63049(19) 0.0625(13) Uani 1 1 d . . . . .
C24 C 1.0140(4) 0.6375(3) 0.67622(19) 0.0628(13) Uani 1 1 d . . . . .
H24 H 1.0216 0.5973 0.6937 0.075 Uiso 1 1 calc R . . . .
C25 C 1.0027(5) 0.7073(3) 0.74515(19) 0.0666(14) Uani 1 1 d . . . . .
H25 H 1.0034 0.7519 0.7578 0.080 Uiso 1 1 calc R . . . .
C26 C 0.9765(4) 0.8189(3) 0.59900(19) 0.0595(13) Uani 1 1 d . . . . .
H26 H 0.9790 0.8158 0.5678 0.071 Uiso 1 1 calc R . . . .
C27 C 1.0103(4) 0.5648(3) 0.6101(2) 0.0658(14) Uani 1 1 d . . . . .
H27 H 1.0182 0.5259 0.6289 0.079 Uiso 1 1 calc R . . . .
C28 C 0.5815(6) 0.5124(4) 0.5542(3) 0.0823(18) Uani 1 1 d . . . . .
C29 C 0.5014(6) 0.5582(4) 0.5365(2) 0.0859(18) Uani 1 1 d . . . . .
H29 H 0.5251 0.5861 0.5123 0.103 Uiso 1 1 calc R . . . .
C30 C 0.3836(6) 0.5643(4) 0.5538(2) 0.0844(18) Uani 1 1 d . . . . .
C31 C 0.3522(6) 0.5233(4) 0.5884(3) 0.097(2) Uani 1 1 d . . . . .
H31 H 0.2729 0.5261 0.5996 0.116 Uiso 1 1 calc R . . . .
C32 C 0.4320(6) 0.4773(4) 0.6078(3) 0.102(2) Uani 1 1 d . . . . .
C33 C 0.5465(6) 0.4720(4) 0.5911(3) 0.097(2) Uani 1 1 d . . . . .
H33 H 0.6022 0.4413 0.6042 0.117 Uiso 1 1 calc R . . . .
C34 C 0.7019(6) 0.5082(4) 0.5355(2) 0.0823(18) Uani 1 1 d . . . . .
H34 H 0.7196 0.5362 0.5107 0.099 Uiso 1 1 calc R . . . .
C35 C 0.2978(6) 0.6119(4) 0.5350(2) 0.0843(19) Uani 1 1 d . . . . .
H35 H 0.2182 0.6110 0.5460 0.101 Uiso 1 1 calc R . . . .
C36 C 0.3960(7) 0.4364(4) 0.6447(3) 0.105(3) Uani 1 1 d . . . . .
H36 H 0.4530 0.4063 0.6575 0.126 Uiso 1 1 calc R . . . .
C37 C 0.2201(6) 0.4417(4) 0.7359(3) 0.097(2) Uani 1 1 d . . . . .
H37A H 0.1500 0.4679 0.7251 0.116 Uiso 1 1 calc R . . A 7
H37B H 0.1938 0.4129 0.7610 0.116 Uiso 0.634(19) 1 calc R . P B 7
C38 C 0.2680(7) 0.3965(4) 0.6995(3) 0.106(3) Uani 1 1 d . . . . .
H38A H 0.3426 0.3736 0.7093 0.128 Uiso 1 1 calc R . . B 6
H38B H 0.2084 0.3606 0.6921 0.128 Uiso 0.366(19) 1 calc R . P B 6
C41 C 1.0014(5) 0.4828(3) 0.5537(2) 0.0788(17) Uani 1 1 d . . . . .
H41A H 0.9999 0.4515 0.5795 0.095 Uiso 1 1 calc R . . C 10
H41B H 1.0761 0.4740 0.5371 0.095 Uiso 0.556(16) 1 calc R . P D 10
C42 C 0.8948(6) 0.4683(4) 0.5247(3) 0.0866(19) Uani 1 1 d . . . . .
H42A H 0.8908 0.5031 0.5009 0.104 Uiso 1 1 calc R . . D 11
H42B H 0.9042 0.4227 0.5108 0.104 Uiso 0.444(16) 1 calc R . P D 11
C45 C 0.2247(5) 0.6921(3) 0.4855(2) 0.0746(16) Uani 1 1 d . . . . .
H45A H 0.1539 0.6876 0.5049 0.089 Uiso 1 1 calc R . . . .
H45B H 0.2040 0.6711 0.4567 0.089 Uiso 1 1 calc R . . . .
C46 C 0.2502(6) 0.7661(4) 0.4785(2) 0.0799(18) Uani 1 1 d . . . . .
H46 H 0.3279 0.7706 0.4623 0.096 Uiso 1 1 calc R . . . .
C47 C 0.1519(7) 0.7972(4) 0.4508(3) 0.099(2) Uani 1 1 d . . . . .
H47A H 0.0753 0.7932 0.4664 0.148 Uiso 1 1 calc GR . . . .
H47B H 0.1470 0.7728 0.4226 0.148 Uiso 1 1 calc GR . . . .
H47C H 0.1697 0.8457 0.4454 0.148 Uiso 1 1 calc GR . . . .
C48 C 0.1824(5) 0.9188(3) 0.7539(2) 0.0770(17) Uani 1 1 d . . . . .
H48A H 0.1143 0.8909 0.7431 0.092 Uiso 1 1 calc R . . E 1
H48B H 0.1512 0.9643 0.7628 0.092 Uiso 0.773(18) 1 calc R . P F 1
C49 C 0.2398(6) 0.8840(3) 0.7930(2) 0.0830(18) Uani 1 1 d . . . . .
H49A H 0.3141 0.9088 0.8011 0.100 Uiso 1 1 calc R . . F 2
H49B H 0.1845 0.8859 0.8184 0.100 Uiso 0.227(18) 1 calc R . P F 2
C52 C 0.8456(5) 0.9829(3) 0.6016(2) 0.0727(15) Uani 1 1 d . . . . .
H52A H 0.8539 0.9921 0.6336 0.087 Uiso 1 1 calc R . . G 5
H52B H 0.8522 1.0271 0.5858 0.087 Uiso 0.612(16) 1 calc R . P H 5
C53 C 0.9451(5) 0.9356(3) 0.5868(2) 0.0689(15) Uani 1 1 d . . . . .
H53A H 0.9277 0.9190 0.5566 0.083 Uiso 1 1 calc R . . H 4
H53B H 1.0215 0.9615 0.5859 0.083 Uiso 0.388(16) 1 calc R . P H 4
C56 C 0.9875(6) 0.6697(4) 0.8173(2) 0.0824(18) Uani 1 1 d . . . . .
H56A H 0.9775 0.7195 0.8226 0.099 Uiso 1 1 calc R . . I 8
H56B H 1.0615 0.6545 0.8324 0.099 Uiso 0.534(19) 1 calc R . P J 8
C57 C 0.8812(6) 0.6314(4) 0.8358(2) 0.0841(18) Uani 1 1 d . . . . .
H57A H 0.8871 0.5824 0.8274 0.101 Uiso 1 1 calc R . . J 9
H57B H 0.8828 0.6342 0.8684 0.101 Uiso 0.466(19) 1 calc R . P J 9
C51 C 0.1570(10) 0.8851(7) 0.8331(4) 0.115(4) Uani 0.773(18) 1 d . . P F 1
H51A H 0.0781 0.8671 0.8248 0.172 Uiso 0.773(18) 1 calc GR . P F 1
H51B H 0.1485 0.9323 0.8437 0.172 Uiso 0.773(18) 1 calc GR . P F 1
H51C H 0.1912 0.8565 0.8565 0.172 Uiso 0.773(18) 1 calc GR . P F 1
C50 C 0.137(3) 0.9835(15) 0.7684(10) 0.079(10) Uani 0.227(18) 1 d . . P F 2
H50A H 0.2034 1.0124 0.7784 0.118 Uiso 0.227(18) 1 calc GR . P F 2
H50B H 0.0807 0.9763 0.7928 0.118 Uiso 0.227(18) 1 calc GR . P F 2
H50C H 0.0952 1.0063 0.7440 0.118 Uiso 0.227(18) 1 calc GR . P F 2
C55 C 1.0618(9) 0.9775(5) 0.5856(4) 0.078(4) Uani 0.612(16) 1 d . . P H 3
H55A H 1.0810 0.9937 0.6154 0.117 Uiso 0.612(16) 1 calc GR . P H 3
H55B H 1.0515 1.0170 0.5659 0.117 Uiso 0.612(16) 1 calc GR . P H 3
H55C H 1.1273 0.9486 0.5747 0.117 Uiso 0.612(16) 1 calc GR . P H 3
C54 C 0.8558(17) 1.0425(8) 0.5655(7) 0.093(7) Uani 0.388(16) 1 d . . P H 4
H54A H 0.8435 1.0231 0.5360 0.139 Uiso 0.388(16) 1 calc GR . P H 4
H54B H 0.9355 1.0635 0.5671 0.139 Uiso 0.388(16) 1 calc GR . P H 4
H54C H 0.7946 1.0775 0.5712 0.139 Uiso 0.388(16) 1 calc GR . P H 4
C40 C 0.1821(14) 0.3424(8) 0.6905(8) 0.159(9) Uani 0.634(19) 1 d . . P B 5
H40A H 0.1806 0.3102 0.7153 0.239 Uiso 0.634(19) 1 calc GR . P B 5
H40B H 0.2055 0.3179 0.6636 0.239 Uiso 0.634(19) 1 calc GR . P B 5
H40C H 0.1023 0.3624 0.6866 0.239 Uiso 0.634(19) 1 calc GR . P B 5
C39 C 0.1810(19) 0.3950(10) 0.7712(6) 0.093(8) Uani 0.366(19) 1 d . . P B 6
H39A H 0.2504 0.3815 0.7890 0.139 Uiso 0.366(19) 1 calc GR . P B 6
H39B H 0.1444 0.3541 0.7581 0.139 Uiso 0.366(19) 1 calc GR . P B 6
H39C H 0.1223 0.4184 0.7899 0.139 Uiso 0.366(19) 1 calc GR . P B 6
C58 C 1.1045(10) 0.6540(7) 0.8407(4) 0.067(5) Uani 0.466(19) 1 d . . P J 7
H58A H 1.1305 0.6074 0.8333 0.101 Uiso 0.466(19) 1 calc GR . P J 7
H58B H 1.0928 0.6576 0.8726 0.101 Uiso 0.466(19) 1 calc GR . P J 7
H58C H 1.1658 0.6869 0.8313 0.101 Uiso 0.466(19) 1 calc GR . P J 7
C59 C 0.883(2) 0.6363(17) 0.8882(7) 0.194(14) Uani 0.534(19) 1 d . . P J 8
H59A H 0.9583 0.6178 0.8994 0.291 Uiso 0.534(19) 1 calc R . P J 8
H59B H 0.8745 0.6844 0.8972 0.291 Uiso 0.534(19) 1 calc R . P J 8
H59C H 0.8156 0.6097 0.9003 0.291 Uiso 0.534(19) 1 calc R . P J 8
C43 C 1.1090(10) 0.4653(7) 0.5254(5) 0.072(5) Uani 0.444(16) 1 d . . P D 9
H43A H 1.1192 0.5006 0.5027 0.109 Uiso 0.444(16) 1 calc GR . P D 9
H43B H 1.0965 0.4206 0.5114 0.109 Uiso 0.444(16) 1 calc GR . P D 9
H43C H 1.1810 0.4635 0.5439 0.109 Uiso 0.444(16) 1 calc GR . P D 9
C44 C 0.9198(16) 0.3950(11) 0.5055(9) 0.167(11) Uani 0.556(16) 1 d . . P D 10
H44A H 0.9528 0.3656 0.5288 0.251 Uiso 0.556(16) 1 calc GR . P D 10
H44B H 0.9774 0.3984 0.4812 0.251 Uiso 0.556(16) 1 calc GR . P D 10
H44C H 0.8447 0.3751 0.4946 0.251 Uiso 0.556(16) 1 calc GR . P D 10
C60 C 0.6357(6) 0.6330(5) 0.67097(13) 0.090(2) Uani 0.849(7) 1 d . U P . .
C61 C 0.6949(6) 0.6916(5) 0.67520(11) 0.093(2) Uani 0.849(7) 1 d . U P . .
H61 H 0.7786 0.6909 0.6811 0.112 Uiso 0.849(7) 1 calc R . P . .
C62 C 0.6372(7) 0.7532(6) 0.67116(16) 0.115(3) Uani 0.849(7) 1 d . U P . .
H62 H 0.6803 0.7950 0.6742 0.138 Uiso 0.849(7) 1 calc R . P . .
C63 C 0.5158(7) 0.7540(5) 0.66258(16) 0.099(3) Uani 0.849(7) 1 d . U P . .
H63 H 0.4756 0.7968 0.6598 0.118 Uiso 0.849(7) 1 calc R . P . .
C64 C 0.4539(6) 0.6959(4) 0.65815(14) 0.0723(19) Uani 0.849(7) 1 d . U P . .
C65 C 0.5133(6) 0.6356(4) 0.66230(15) 0.088(2) Uani 0.849(7) 1 d . U P . .
H65 H 0.4701 0.5939 0.6592 0.105 Uiso 0.849(7) 1 calc R . P . .
C66 C 0.7017(9) 0.5683(6) 0.6756(2) 0.134(4) Uani 0.849(7) 1 d . U P . .
H66A H 0.7496 0.5601 0.6490 0.201 Uiso 0.849(7) 1 calc GR . P . .
H66B H 0.6448 0.5305 0.6796 0.201 Uiso 0.849(7) 1 calc GR . P . .
H66C H 0.7548 0.5709 0.7013 0.201 Uiso 0.849(7) 1 calc GR . P . .
C67 C 0.3201(6) 0.6964(5) 0.6487(2) 0.091(3) Uani 0.849(7) 1 d . U P . .
H67A H 0.2803 0.7287 0.6686 0.137 Uiso 0.849(7) 1 calc GR . P . .
H67B H 0.2874 0.6503 0.6532 0.137 Uiso 0.849(7) 1 calc GR . P . .
H67C H 0.3065 0.7106 0.6181 0.137 Uiso 0.849(7) 1 calc GR . P . .
C68 C 0.435(2) 0.7251(6) 0.9060(4) 0.398(10) Uiso 0.849(7) 1 d D . P . .
H68 H 0.3975 0.6950 0.8856 0.478 Uiso 0.424(3) 1 calc R . P K 2
C69 C 0.365(2) 0.7628(7) 0.9353(5) 0.398(10) Uiso 0.849(7) 1 d DG . P K .
H69 H 0.2804 0.7585 0.9349 0.478 Uiso 0.424(3) 1 calc R . P K 1
C70 C 0.420(2) 0.8069(7) 0.9652(5) 0.398(10) Uiso 0.849(7) 1 d DG . P K .
H70 H 0.3723 0.8327 0.9853 0.478 Uiso 0.849(7) 1 calc R . P . .
C71 C 0.544(2) 0.8133(7) 0.9658(5) 0.398(10) Uiso 0.849(7) 1 d DG . P K .
H71 H 0.5812 0.8435 0.9863 0.478 Uiso 0.424(3) 1 calc R . P K 1
C72 C 0.613(2) 0.7756(7) 0.9366(5) 0.398(10) Uiso 0.849(7) 1 d DG . P K .
H72 H 0.6982 0.7799 0.9370 0.478 Uiso 0.424(3) 1 calc R . P K 2
C73 C 0.559(2) 0.7315(7) 0.9066(5) 0.398(10) Uiso 0.849(7) 1 d DG . P K .
H73 H 0.6064 0.7057 0.8866 0.478 Uiso 0.849(7) 1 calc R . P . .
C74 C 0.376(3) 0.6774(10) 0.8737(7) 0.398(10) Uiso 0.424(3) 1 d D . P K 1
H74A H 0.4379 0.6551 0.8557 0.598 Uiso 0.424(3) 1 calc R . P K 1
H74B H 0.3304 0.6424 0.8897 0.598 Uiso 0.424(3) 1 calc R . P K 1
H74C H 0.3221 0.7035 0.8545 0.598 Uiso 0.424(3) 1 calc R . P K 1
C75 C 0.751(3) 0.7826(12) 0.9372(9) 0.398(10) Uiso 0.424(3) 1 d D . P K 1
H75A H 0.7741 0.8155 0.9601 0.598 Uiso 0.424(3) 1 calc R . P K 1
H75B H 0.7869 0.7379 0.9436 0.598 Uiso 0.424(3) 1 calc R . P K 1
H75C H 0.7786 0.7990 0.9085 0.598 Uiso 0.424(3) 1 calc R . P K 1
C76 C 0.228(3) 0.7558(12) 0.9346(8) 0.398(10) Uiso 0.424(3) 1 d D . P K 2
H76A H 0.2048 0.7229 0.9118 0.598 Uiso 0.424(3) 1 calc R . P K 2
H76B H 0.2002 0.7394 0.9634 0.598 Uiso 0.424(3) 1 calc R . P K 2
H76C H 0.1920 0.8005 0.9283 0.598 Uiso 0.424(3) 1 calc R . P K 2
C77 C 0.605(3) 0.8617(12) 0.9987(8) 0.398(10) Uiso 0.424(3) 1 d D . P K 2
H77A H 0.6917 0.8599 0.9946 0.598 Uiso 0.424(3) 1 calc R . P K 2
H77B H 0.5763 0.9087 0.9937 0.598 Uiso 0.424(3) 1 calc R . P K 2
H77C H 0.5846 0.8476 1.0288 0.598 Uiso 0.424(3) 1 calc R . P K 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 0.055(3) 0.083(4) 0.166(6) 0.002(4) 0.019(4) -0.012(3)
N2 0.056(3) 0.076(4) 0.145(5) 0.022(3) 0.014(3) -0.005(3)
N3 0.054(3) 0.099(4) 0.089(3) 0.016(3) 0.001(3) 0.011(3)
N4 0.049(3) 0.096(4) 0.082(3) 0.015(3) -0.002(2) 0.012(3)
N5 0.048(3) 0.064(3) 0.100(3) -0.003(2) -0.004(3) -0.004(2)
N6 0.039(2) 0.076(3) 0.084(3) 0.005(3) -0.004(2) -0.003(2)
N7 0.053(3) 0.084(3) 0.098(4) -0.005(3) 0.014(3) 0.006(3)
N8 0.050(3) 0.069(3) 0.105(4) -0.011(3) 0.011(3) 0.008(2)
N9 0.047(3) 0.092(3) 0.087(3) -0.002(3) -0.003(2) 0.001(3)
N10 0.043(3) 0.102(4) 0.089(3) -0.020(3) -0.006(3) -0.004(3)
N11 0.049(3) 0.078(3) 0.121(4) -0.011(3) 0.009(3) -0.003(3)
N12 0.035(2) 0.078(3) 0.096(4) -0.005(3) 0.015(2) 0.001(2)
C1 0.047(3) 0.078(4) 0.094(4) -0.002(3) 0.007(3) 0.005(3)
C2 0.056(4) 0.078(4) 0.099(4) 0.000(3) 0.015(3) 0.001(3)
C3 0.054(3) 0.077(4) 0.089(4) 0.016(3) 0.012(3) 0.005(3)
C4 0.064(4) 0.073(4) 0.095(4) 0.017(3) 0.010(3) 0.000(3)
C5 0.055(3) 0.072(4) 0.100(4) 0.014(3) 0.010(3) 0.007(3)
C6 0.048(3) 0.087(4) 0.092(4) 0.011(3) 0.008(3) 0.009(3)
C7 0.057(4) 0.082(4) 0.112(5) -0.012(4) -0.001(3) 0.001(3)
C8 0.065(4) 0.081(4) 0.087(4) 0.019(3) 0.013(3) 0.013(4)
C9 0.055(4) 0.077(4) 0.102(5) 0.014(3) 0.008(3) 0.002(3)
C10 0.054(4) 0.075(4) 0.096(4) -0.017(3) 0.013(3) -0.001(3)
C11 0.046(3) 0.084(4) 0.108(5) -0.019(4) 0.009(3) -0.001(3)
C12 0.044(3) 0.086(4) 0.094(4) -0.008(3) 0.004(3) 0.004(3)
C13 0.052(3) 0.081(4) 0.092(4) -0.011(3) -0.004(3) 0.004(3)
C14 0.048(3) 0.074(4) 0.107(5) -0.006(3) 0.006(3) 0.004(3)
C15 0.056(4) 0.079(4) 0.100(4) -0.025(3) 0.005(3) 0.000(3)
C16 0.053(4) 0.076(4) 0.117(5) -0.021(4) 0.006(3) 0.004(3)
C17 0.043(3) 0.096(4) 0.086(4) -0.004(3) 0.000(3) 0.002(3)
C18 0.062(4) 0.064(3) 0.095(4) -0.009(3) 0.001(3) -0.001(3)
C19 0.025(2) 0.082(4) 0.078(3) -0.001(3) -0.001(2) -0.001(3)
C20 0.036(3) 0.066(3) 0.081(4) 0.004(3) -0.005(2) 0.001(2)
C21 0.031(3) 0.073(3) 0.078(3) 0.004(3) -0.002(2) -0.003(3)
C22 0.034(3) 0.070(3) 0.081(3) 0.000(3) 0.003(2) 0.001(3)
C23 0.028(2) 0.074(4) 0.086(4) 0.004(3) 0.007(2) 0.002(2)
C24 0.030(3) 0.073(3) 0.085(4) 0.005(3) 0.000(2) 0.003(2)
C25 0.037(3) 0.085(4) 0.078(3) 0.004(3) -0.006(2) 0.005(3)
C26 0.035(3) 0.070(4) 0.073(3) 0.000(3) -0.001(2) -0.006(2)
C27 0.032(3) 0.077(4) 0.089(4) 0.005(3) 0.012(3) 0.007(3)
C28 0.045(3) 0.083(4) 0.119(5) 0.001(4) 0.001(3) 0.001(3)
C29 0.056(4) 0.100(5) 0.102(4) -0.002(4) 0.007(3) -0.013(4)
C30 0.051(4) 0.092(4) 0.110(5) 0.001(4) 0.000(3) 0.004(3)
C31 0.054(4) 0.112(5) 0.124(6) 0.017(5) 0.007(4) -0.012(4)
C32 0.050(4) 0.092(5) 0.163(7) 0.014(5) 0.011(4) 0.000(4)
C33 0.049(4) 0.090(5) 0.153(7) 0.007(5) 0.011(4) -0.006(3)
C34 0.057(4) 0.085(4) 0.105(5) -0.013(4) 0.005(3) -0.010(3)
C35 0.050(4) 0.106(5) 0.097(5) -0.012(4) 0.010(3) -0.010(4)
C36 0.058(4) 0.089(5) 0.169(8) 0.027(5) 0.025(4) -0.008(4)
C37 0.057(4) 0.082(4) 0.151(6) 0.020(5) 0.017(4) -0.006(4)
C38 0.071(5) 0.070(4) 0.178(8) 0.009(5) 0.035(5) -0.013(4)
C41 0.048(3) 0.079(4) 0.109(4) -0.006(3) 0.019(3) 0.004(3)
C42 0.063(4) 0.083(4) 0.114(5) -0.024(4) 0.015(3) 0.003(3)
C45 0.052(3) 0.092(4) 0.080(4) -0.014(3) -0.003(3) -0.004(3)
C46 0.052(3) 0.117(5) 0.070(3) 0.000(3) -0.001(3) 0.007(3)
C47 0.084(5) 0.099(5) 0.114(5) 0.007(4) -0.025(4) 0.008(4)
C48 0.050(3) 0.080(4) 0.101(5) -0.019(3) 0.007(3) 0.006(3)
C49 0.060(4) 0.081(4) 0.109(5) -0.027(4) 0.011(3) 0.006(3)
C52 0.054(3) 0.064(3) 0.100(4) 0.002(3) -0.014(3) -0.005(3)
C53 0.052(3) 0.071(3) 0.084(4) 0.007(3) -0.003(3) -0.008(3)
C56 0.053(4) 0.118(5) 0.076(4) 0.012(3) -0.005(3) 0.010(3)
C57 0.071(4) 0.098(5) 0.084(4) 0.021(4) 0.003(3) 0.014(4)
C51 0.100(8) 0.135(9) 0.111(8) -0.024(7) 0.028(6) 0.008(7)
C50 0.066(18) 0.080(18) 0.090(19) -0.004(14) 0.025(14) 0.011(14)
C55 0.051(6) 0.071(6) 0.113(8) 0.020(6) -0.016(5) -0.012(5)
C54 0.082(12) 0.062(10) 0.135(16) 0.010(9) -0.031(11) -0.029(9)
C40 0.091(11) 0.104(10) 0.28(2) -0.029(12) 0.054(12) -0.043(8)
C39 0.092(14) 0.098(14) 0.090(13) 0.005(10) 0.008(10) -0.052(11)
C58 0.042(7) 0.102(10) 0.057(7) 0.028(6) -0.005(5) 0.019(6)
C59 0.17(2) 0.29(4) 0.118(15) 0.048(18) 0.026(14) 0.11(2)
C43 0.039(7) 0.077(9) 0.101(10) -0.027(7) 0.019(6) 0.002(6)
C44 0.082(11) 0.141(15) 0.28(3) -0.103(18) -0.003(13) -0.014(10)
C60 0.046(4) 0.106(5) 0.117(6) 0.032(4) 0.008(3) 0.000(3)
C61 0.036(4) 0.116(5) 0.128(7) 0.025(5) -0.003(4) -0.003(4)
C62 0.047(4) 0.109(6) 0.188(10) -0.002(6) -0.009(5) -0.010(4)
C63 0.047(4) 0.104(5) 0.146(7) -0.008(5) -0.007(4) 0.000(4)
C64 0.032(3) 0.103(5) 0.082(4) 0.013(4) 0.004(3) 0.000(3)
C65 0.044(4) 0.093(5) 0.126(6) 0.019(4) 0.001(3) -0.002(3)
C66 0.069(6) 0.127(7) 0.207(12) 0.030(7) -0.008(6) 0.007(5)
C67 0.036(3) 0.119(6) 0.119(6) 0.004(5) -0.003(3) 0.002(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 C36 1.258(9) . ?
N1 C38 1.455(11) . ?
N2 C9 1.248(8) . ?
N2 C37 1.463(10) . ?
N3 C8 1.272(9) . ?
N3 C57 1.447(8) . ?
N4 C25 1.243(7) . ?
N4 C56 1.454(8) . ?
N5 C18 1.254(8) . ?
N5 C52 1.460(7) . ?
N6 C26 1.256(7) . ?
N6 C53 1.469(8) . ?
N7 C7 1.253(8) . ?
N7 C49 1.447(8) . ?
N8 C16 1.278(9) . ?
N8 C48 1.445(8) . ?
N9 C17 1.253(8) . ?
N9 C46 1.479(8) . ?
N10 C35 1.277(9) . ?
N10 C45 1.430(8) . ?
N11 C34 1.263(8) . ?
N11 C42 1.457(8) . ?
N12 C27 1.264(8) . ?
N12 C41 1.468(8) . ?
C1 C2 1.385(9) . ?
C1 C6 1.386(9) . ?
C1 C7 1.474(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(9) . ?
C3 C4 1.363(9) . ?
C3 C8 1.482(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.404(9) . ?
C5 C6 1.364(9) . ?
C5 C9 1.462(9) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.372(9) . ?
C10 C15 1.422(9) . ?
C10 C16 1.456(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.410(9) . ?
C12 C13 1.378(9) . ?
C12 C17 1.468(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.408(9) . ?
C14 C15 1.371(9) . ?
C14 C18 1.479(9) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.380(8) . ?
C19 C24 1.383(8) . ?
C19 C25 1.484(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.402(8) . ?
C21 C22 1.376(8) . ?
C21 C26 1.475(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.422(8) . ?
C23 C24 1.392(8) . ?
C23 C27 1.447(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.373(10) . ?
C28 C33 1.421(11) . ?
C28 C34 1.461(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.420(9) . ?
C30 C31 1.364(10) . ?
C30 C35 1.450(10) . ?
C31 H31 0.9500 . ?
C31 C32 1.394(11) . ?
C32 C33 1.379(10) . ?
C32 C36 1.430(12) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.512(11) . ?
C37 C39 1.471(19) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C40 1.451(16) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.507(10) . ?
C41 C43 1.515(13) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C44 1.567(18) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.486(10) . ?
C46 H46 1.0000 . ?
C46 C47 1.509(9) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.510(10) . ?
C48 C50 1.43(3) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C51 1.528(12) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.511(9) . ?
C52 C54 1.602(19) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C55 1.537(11) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.509(10) . ?
C56 C58 1.517(12) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C59 1.59(2) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C60 C61 1.326(12) . ?
C60 C65 1.392(11) . ?
C60 C66 1.467(13) . ?
C61 H61 0.9500 . ?
C61 C62 1.367(13) . ?
C62 H62 0.9500 . ?
C62 C63 1.379(11) . ?
C63 H63 0.9500 . ?
C63 C64 1.334(12) . ?
C64 C65 1.356(11) . ?
C64 C67 1.519(10) . ?
C65 H65 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68 0.9500 . ?
C68 C69 1.3900 . ?
C68 C73 1.3900 . ?
C68 C74 1.502(19) . ?
C69 H69 0.9500 . ?
C69 C70 1.3900 . ?
C69 C76 1.54(3) . ?
C70 H70 0.9500 . ?
C70 C71 1.3900 . ?
C71 H71 0.9500 . ?
C71 C72 1.3900 . ?
C71 C77 1.53(2) . ?
C72 H72 0.9500 . ?
C72 C73 1.3900 . ?
C72 C75 1.54(2) . ?
C73 H73 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
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
C36 N1 C38 117.7(7) . . ?
C9 N2 C37 118.2(6) . . ?
C8 N3 C57 117.9(6) . . ?
C25 N4 C56 118.0(6) . . ?
C18 N5 C52 117.9(5) . . ?
C26 N6 C53 117.3(5) . . ?
C7 N7 C49 118.4(6) . . ?
C16 N8 C48 117.9(5) . . ?
C17 N9 C46 117.9(5) . . ?
C35 N10 C45 117.6(5) . . ?
C34 N11 C42 116.2(6) . . ?
C27 N12 C41 117.8(6) . . ?
C2 C1 C6 118.8(6) . . ?
C2 C1 C7 119.9(6) . . ?
C6 C1 C7 121.3(6) . . ?
C1 C2 H2 119.6 . . ?
C1 C2 C3 120.8(6) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C8 121.3(6) . . ?
C4 C3 C2 119.2(6) . . ?
C4 C3 C8 119.2(6) . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 120.9(6) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C9 120.8(6) . . ?
C6 C5 C4 118.9(6) . . ?
C6 C5 C9 120.2(6) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 C1 121.4(6) . . ?
C5 C6 H6 119.3 . . ?
N7 C7 C1 124.5(6) . . ?
N7 C7 H7 117.8 . . ?
C1 C7 H7 117.8 . . ?
N3 C8 C3 123.4(6) . . ?
N3 C8 H8 118.3 . . ?
C3 C8 H8 118.3 . . ?
N2 C9 C5 124.0(6) . . ?
N2 C9 H9 118.0 . . ?
C5 C9 H9 118.0 . . ?
C11 C10 C15 119.1(6) . . ?
C11 C10 C16 119.9(6) . . ?
C15 C10 C16 120.7(6) . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.0(6) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C17 121.7(6) . . ?
C13 C12 C11 118.9(6) . . ?
C13 C12 C17 119.4(5) . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.0(6) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C18 120.2(6) . . ?
C15 C14 C13 119.5(6) . . ?
C15 C14 C18 120.2(6) . . ?
C10 C15 H15 119.8 . . ?
C14 C15 C10 120.4(6) . . ?
C14 C15 H15 119.8 . . ?
N8 C16 C10 122.7(6) . . ?
N8 C16 H16 118.6 . . ?
C10 C16 H16 118.6 . . ?
N9 C17 C12 124.9(6) . . ?
N9 C17 H17 117.5 . . ?
C12 C17 H17 117.5 . . ?
N5 C18 C14 121.9(6) . . ?
N5 C18 H18 119.1 . . ?
C14 C18 H18 119.1 . . ?
C20 C19 C24 120.4(5) . . ?
C20 C19 C25 118.3(5) . . ?
C24 C19 C25 121.1(6) . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.4(5) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C26 120.0(5) . . ?
C22 C21 C20 119.4(5) . . ?
C22 C21 C26 120.5(5) . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.7(5) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 C27 121.8(5) . . ?
C24 C23 C22 118.5(5) . . ?
C24 C23 C27 119.7(5) . . ?
C19 C24 C23 120.6(5) . . ?
C19 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
N4 C25 C19 123.1(6) . . ?
N4 C25 H25 118.5 . . ?
C19 C25 H25 118.5 . . ?
N6 C26 C21 122.3(5) . . ?
N6 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
N12 C27 C23 124.5(6) . . ?
N12 C27 H27 117.8 . . ?
C23 C27 H27 117.8 . . ?
C29 C28 C33 119.3(6) . . ?
C29 C28 C34 118.8(7) . . ?
C33 C28 C34 121.9(7) . . ?
C28 C29 H29 119.6 . . ?
C28 C29 C30 120.8(7) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C35 121.2(7) . . ?
C31 C30 C29 118.2(7) . . ?
C31 C30 C35 120.6(6) . . ?
C30 C31 H31 118.7 . . ?
C30 C31 C32 122.6(7) . . ?
C32 C31 H31 118.7 . . ?
C31 C32 C36 120.6(6) . . ?
C33 C32 C31 118.9(8) . . ?
C33 C32 C36 120.5(8) . . ?
C28 C33 H33 119.9 . . ?
C32 C33 C28 120.2(7) . . ?
C32 C33 H33 119.9 . . ?
N11 C34 C28 124.2(7) . . ?
N11 C34 H34 117.9 . . ?
C28 C34 H34 117.9 . . ?
N10 C35 C30 124.3(6) . . ?
N10 C35 H35 117.8 . . ?
C30 C35 H35 117.8 . . ?
N1 C36 C32 123.0(8) . . ?
N1 C36 H36 118.5 . . ?
C32 C36 H36 118.5 . . ?
N2 C37 H37A 109.7 . . ?
N2 C37 H37B 109.7 . . ?
N2 C37 C38 110.0(6) . . ?
N2 C37 C39 112.4(10) . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 H37A 109.7 . . ?
C38 C37 H37B 109.7 . . ?
C39 C37 C38 106.0(10) . . ?
N1 C38 C37 109.0(6) . . ?
N1 C38 H38A 109.9 . . ?
N1 C38 H38B 109.9 . . ?
C37 C38 H38A 109.9 . . ?
C37 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
C40 C38 N1 112.4(12) . . ?
C40 C38 C37 109.1(9) . . ?
N12 C41 H41A 109.4 . . ?
N12 C41 H41B 109.4 . . ?
N12 C41 C42 111.1(5) . . ?
N12 C41 C43 113.4(7) . . ?
H41A C41 H41B 108.0 . . ?
C42 C41 H41A 109.4 . . ?
C42 C41 H41B 109.4 . . ?
C42 C41 C43 104.6(7) . . ?
N11 C42 C41 110.9(6) . . ?
N11 C42 H42A 109.5 . . ?
N11 C42 H42B 109.5 . . ?
N11 C42 C44 111.4(10) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 C44 104.3(9) . . ?
H42A C42 H42B 108.1 . . ?
N10 C45 H45A 108.8 . . ?
N10 C45 H45B 108.8 . . ?
N10 C45 C46 113.9(5) . . ?
H45A C45 H45B 107.7 . . ?
C46 C45 H45A 108.8 . . ?
C46 C45 H45B 108.8 . . ?
N9 C46 C45 110.7(5) . . ?
N9 C46 H46 108.7 . . ?
N9 C46 C47 110.9(6) . . ?
C45 C46 H46 108.7 . . ?
C45 C46 C47 109.2(6) . . ?
C47 C46 H46 108.7 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N8 C48 H48A 109.8 . . ?
N8 C48 H48B 109.8 . . ?
N8 C48 C49 109.6(5) . . ?
H48A C48 H48B 108.2 . . ?
C49 C48 H48A 109.8 . . ?
C49 C48 H48B 109.8 . . ?
C50 C48 N8 111.6(12) . . ?
C50 C48 C49 107.7(14) . . ?
N7 C49 C48 111.4(6) . . ?
N7 C49 H49A 109.4 . . ?
N7 C49 H49B 109.4 . . ?
N7 C49 C51 107.9(7) . . ?
C48 C49 H49A 109.4 . . ?
C48 C49 H49B 109.4 . . ?
C48 C49 C51 111.2(7) . . ?
H49A C49 H49B 108.0 . . ?
N5 C52 H52A 109.4 . . ?
N5 C52 H52B 109.4 . . ?
N5 C52 C53 111.0(5) . . ?
N5 C52 C54 103.6(7) . . ?
H52A C52 H52B 108.0 . . ?
C53 C52 H52A 109.4 . . ?
C53 C52 H52B 109.4 . . ?
C53 C52 C54 100.8(9) . . ?
N6 C53 C52 111.8(5) . . ?
N6 C53 H53A 109.3 . . ?
N6 C53 H53B 109.3 . . ?
N6 C53 C55 110.3(5) . . ?
C52 C53 H53A 109.3 . . ?
C52 C53 H53B 109.3 . . ?
C52 C53 C55 107.7(6) . . ?
H53A C53 H53B 107.9 . . ?
N4 C56 H56A 109.6 . . ?
N4 C56 H56B 109.6 . . ?
N4 C56 C57 110.1(6) . . ?
N4 C56 C58 110.9(7) . . ?
H56A C56 H56B 108.2 . . ?
C57 C56 H56A 109.6 . . ?
C57 C56 H56B 109.6 . . ?
C57 C56 C58 113.8(7) . . ?
N3 C57 C56 112.0(5) . . ?
N3 C57 H57A 109.2 . . ?
N3 C57 H57B 109.2 . . ?
N3 C57 C59 108.6(10) . . ?
C56 C57 H57A 109.2 . . ?
C56 C57 H57B 109.2 . . ?
C56 C57 C59 109.5(13) . . ?
H57A C57 H57B 107.9 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C61 C60 C65 118.4(8) . . ?
C61 C60 C66 118.8(8) . . ?
C65 C60 C66 122.8(8) . . ?
C60 C61 H61 119.6 . . ?
C60 C61 C62 120.8(7) . . ?
C62 C61 H61 119.6 . . ?
C61 C62 H62 120.3 . . ?
C61 C62 C63 119.4(9) . . ?
C63 C62 H62 120.3 . . ?
C62 C63 H63 119.4 . . ?
C64 C63 C62 121.2(9) . . ?
C64 C63 H63 119.4 . . ?
C63 C64 C65 118.3(7) . . ?
C63 C64 C67 121.5(8) . . ?
C65 C64 C67 120.2(8) . . ?
C60 C65 H65 119.0 . . ?
C64 C65 C60 122.0(8) . . ?
C64 C65 H65 119.0 . . ?
C60 C66 H66A 109.5 . . ?
C60 C66 H66B 109.5 . . ?
C60 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C69 C68 H68 120.0 . . ?
C69 C68 C73 120.0 . . ?
C69 C68 C74 120.2(11) . . ?
C73 C68 H68 120.0 . . ?
C73 C68 C74 119.8(11) . . ?
C68 C69 H69 120.0 . . ?
C68 C69 C76 120.0(10) . . ?
C70 C69 C68 120.0 . . ?
C70 C69 H69 120.0 . . ?
C70 C69 C76 120.0(10) . . ?
C69 C70 H70 120.0 . . ?
C69 C70 C71 120.0 . . ?
C71 C70 H70 120.0 . . ?
C70 C71 H71 120.0 . . ?
C70 C71 C72 120.0 . . ?
C70 C71 C77 120.3(11) . . ?
C72 C71 H71 120.0 . . ?
C72 C71 C77 119.7(11) . . ?
C71 C72 H72 120.0 . . ?
C71 C72 C75 120.0(10) . . ?
C73 C72 C71 120.0 . . ?
C73 C72 H72 120.0 . . ?
C73 C72 C75 120.0(10) . . ?
C68 C73 H73 120.0 . . ?
C72 C73 C68 120.0 . . ?
C72 C73 H73 120.0 . . ?
C68 C74 H74A 109.5 . . ?
C68 C74 H74B 109.5 . . ?
C68 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C72 C75 H75A 109.5 . . ?
C72 C75 H75B 109.5 . . ?
C72 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C69 C76 H76A 109.5 . . ?
C69 C76 H76B 109.5 . . ?
C69 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C71 C77 H77A 109.5 . . ?
C71 C77 H77B 109.5 . . ?
C71 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C37 C38 N1 -66.4(8) . . . . ?
N2 C37 C38 C40 170.4(11) . . . . ?
N4 C56 C57 N3 -68.2(8) . . . . ?
N4 C56 C57 C59 171.3(11) . . . . ?
N5 C52 C53 N6 -73.2(6) . . . . ?
N5 C52 C53 C55 165.5(6) . . . . ?
N8 C48 C49 N7 -69.1(7) . . . . ?
N8 C48 C49 C51 170.5(7) . . . . ?
N10 C45 C46 N9 -68.3(7) . . . . ?
N10 C45 C46 C47 169.3(6) . . . . ?
N12 C41 C42 N11 -68.5(7) . . . . ?
N12 C41 C42 C44 171.5(12) . . . . ?
C1 C2 C3 C4 -0.2(10) . . . . ?
C1 C2 C3 C8 -174.2(6) . . . . ?
C2 C1 C6 C5 0.2(10) . . . . ?
C2 C1 C7 N7 -169.7(7) . . . . ?
C2 C3 C4 C5 0.3(9) . . . . ?
C2 C3 C8 N3 0.5(10) . . . . ?
C3 C4 C5 C6 -0.2(10) . . . . ?
C3 C4 C5 C9 -178.1(6) . . . . ?
C4 C3 C8 N3 -173.5(6) . . . . ?
C4 C5 C6 C1 0.0(10) . . . . ?
C4 C5 C9 N2 6.2(10) . . . . ?
C6 C1 C2 C3 0.0(10) . . . . ?
C6 C1 C7 N7 7.2(11) . . . . ?
C6 C5 C9 N2 -171.6(7) . . . . ?
C7 N7 C49 C48 120.6(7) . . . . ?
C7 N7 C49 C51 -117.0(8) . . . . ?
C7 C1 C2 C3 177.0(6) . . . . ?
C7 C1 C6 C5 -176.8(6) . . . . ?
C8 N3 C57 C56 128.0(7) . . . . ?
C8 N3 C57 C59 -110.9(15) . . . . ?
C8 C3 C4 C5 174.4(6) . . . . ?
C9 N2 C37 C38 124.1(8) . . . . ?
C9 N2 C37 C39 -118.0(12) . . . . ?
C9 C5 C6 C1 177.9(6) . . . . ?
C10 C11 C12 C13 0.1(10) . . . . ?
C10 C11 C12 C17 176.5(6) . . . . ?
C11 C10 C15 C14 1.4(10) . . . . ?
C11 C10 C16 N8 177.7(6) . . . . ?
C11 C12 C13 C14 1.5(10) . . . . ?
C11 C12 C17 N9 -1.1(10) . . . . ?
C12 C13 C14 C15 -1.6(10) . . . . ?
C12 C13 C14 C18 174.7(6) . . . . ?
C13 C12 C17 N9 175.4(6) . . . . ?
C13 C14 C15 C10 0.2(10) . . . . ?
C13 C14 C18 N5 -3.4(9) . . . . ?
C15 C10 C11 C12 -1.5(10) . . . . ?
C15 C10 C16 N8 2.2(10) . . . . ?
C15 C14 C18 N5 172.9(6) . . . . ?
C16 N8 C48 C49 123.3(6) . . . . ?
C16 N8 C48 C50 -117.4(16) . . . . ?
C16 C10 C11 C12 -177.0(6) . . . . ?
C16 C10 C15 C14 176.8(6) . . . . ?
C17 N9 C46 C45 124.4(6) . . . . ?
C17 N9 C46 C47 -114.3(7) . . . . ?
C17 C12 C13 C14 -175.0(6) . . . . ?
C18 N5 C52 C53 138.5(6) . . . . ?
C18 N5 C52 C54 -114.1(10) . . . . ?
C18 C14 C15 C10 -176.1(6) . . . . ?
C19 C20 C21 C22 -0.5(8) . . . . ?
C19 C20 C21 C26 176.3(4) . . . . ?
C20 C19 C24 C23 -0.7(7) . . . . ?
C20 C19 C25 N4 172.2(5) . . . . ?
C20 C21 C22 C23 1.1(7) . . . . ?
C20 C21 C26 N6 -3.7(7) . . . . ?
C21 C22 C23 C24 -1.5(7) . . . . ?
C21 C22 C23 C27 176.2(5) . . . . ?
C22 C21 C26 N6 173.2(5) . . . . ?
C22 C23 C24 C19 1.3(7) . . . . ?
C22 C23 C27 N12 -1.4(8) . . . . ?
C24 C19 C20 C21 0.3(7) . . . . ?
C24 C19 C25 N4 -4.1(8) . . . . ?
C24 C23 C27 N12 176.3(5) . . . . ?
C25 N4 C56 C57 126.3(6) . . . . ?
C25 N4 C56 C58 -107.0(8) . . . . ?
C25 C19 C20 C21 -176.0(5) . . . . ?
C25 C19 C24 C23 175.5(4) . . . . ?
C26 N6 C53 C52 138.4(5) . . . . ?
C26 N6 C53 C55 -101.8(7) . . . . ?
C26 C21 C22 C23 -175.8(5) . . . . ?
C27 N12 C41 C42 127.7(6) . . . . ?
C27 N12 C41 C43 -114.9(9) . . . . ?
C27 C23 C24 C19 -176.5(5) . . . . ?
C28 C29 C30 C31 -0.4(11) . . . . ?
C28 C29 C30 C35 -179.2(7) . . . . ?
C29 C28 C33 C32 2.1(12) . . . . ?
C29 C28 C34 N11 177.4(7) . . . . ?
C29 C30 C31 C32 1.8(12) . . . . ?
C29 C30 C35 N10 -5.6(11) . . . . ?
C30 C31 C32 C33 -1.2(13) . . . . ?
C30 C31 C32 C36 178.5(8) . . . . ?
C31 C30 C35 N10 175.6(7) . . . . ?
C31 C32 C33 C28 -0.8(13) . . . . ?
C31 C32 C36 N1 1.3(14) . . . . ?
C33 C28 C29 C30 -1.6(11) . . . . ?
C33 C28 C34 N11 -0.6(11) . . . . ?
C33 C32 C36 N1 -179.0(9) . . . . ?
C34 N11 C42 C41 127.4(6) . . . . ?
C34 N11 C42 C44 -116.9(13) . . . . ?
C34 C28 C29 C30 -179.6(6) . . . . ?
C34 C28 C33 C32 -179.9(8) . . . . ?
C35 N10 C45 C46 136.9(6) . . . . ?
C35 C30 C31 C32 -179.4(7) . . . . ?
C36 N1 C38 C37 124.8(8) . . . . ?
C36 N1 C38 C40 -114.0(11) . . . . ?
C36 C32 C33 C28 179.5(8) . . . . ?
C37 N2 C9 C5 -179.5(6) . . . . ?
C38 N1 C36 C32 -177.6(8) . . . . ?
C41 N12 C27 C23 -179.4(5) . . . . ?
C42 N11 C34 C28 174.9(6) . . . . ?
C45 N10 C35 C30 172.2(6) . . . . ?
C46 N9 C17 C12 -177.3(6) . . . . ?
C48 N8 C16 C10 -177.0(6) . . . . ?
C49 N7 C7 C1 175.5(6) . . . . ?
C52 N5 C18 C14 177.8(5) . . . . ?
C53 N6 C26 C21 178.6(4) . . . . ?
C56 N4 C25 C19 -176.8(5) . . . . ?
C57 N3 C8 C3 176.3(5) . . . . ?
C50 C48 C49 N7 169.3(13) . . . . ?
C54 C52 C53 N6 177.5(7) . . . . ?
C39 C37 C38 N1 171.8(10) . . . . ?
C58 C56 C57 N3 166.7(8) . . . . ?
C43 C41 C42 N11 168.8(8) . . . . ?
C60 C61 C62 C63 0.00(4) . . . . ?
C61 C60 C65 C64 -0.03(10) . . . . ?
C61 C62 C63 C64 0.00(10) . . . . ?
C62 C63 C64 C65 -0.02(13) . . . . ?
C62 C63 C64 C67 180.00(7) . . . . ?
C63 C64 C65 C60 0.04(14) . . . . ?
C65 C60 C61 C62 0.01(4) . . . . ?
C66 C60 C61 C62 -179.98(4) . . . . ?
C66 C60 C65 C64 179.96(8) . . . . ?
C67 C64 C65 C60 -179.99(7) . . . . ?
C68 C69 C70 C71 0.0 . . . . ?
C69 C68 C73 C72 0.0 . . . . ?
C69 C70 C71 C72 0.0 . . . . ?
C69 C70 C71 C77 180.0 . . . . ?
C70 C71 C72 C73 0.0 . . . . ?
C70 C71 C72 C75 180.0 . . . . ?
C71 C72 C73 C68 0.0 . . . . ?
C73 C68 C69 C70 0.0 . . . . ?
C73 C68 C69 C76 180.0 . . . . ?
C74 C68 C69 C70 180.0 . . . . ?
C74 C68 C73 C72 180.0 . . . . ?
C75 C72 C73 C68 180.0 . . . . ?
C76 C69 C70 C71 180.0 . . . . ?
C77 C71 C72 C73 180.0 . . . . ?
_shelx_res_file
;
TITL THL_397_A2_100K_Solvate in P2(1)2(1)2(1)
REM Best SHELXD solution FINAL CC 66.92
CELL 0.6889 11.1553 19.4897 30.3319 90 90 90
ZERR 4 0.0019 0.0035 0.0055 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H N
DISP C 0.003 0.002 10.64
DISP H -0 0 0.67
DISP N 0.006 0.003 18.02
UNIT 270.37 307.97 48
DFIX 1.52 C75 C72
DFIX 1.52 C68 C74
DFIX 1.49 C74 C68 C75 C72 C71 C77 C69 C76
SADI C68 C76 C76 C70
SADI C73 C75 C71 C75
SADI C73 C75 C75 C71
SADI C72 C77 C77 C70
SADI C69 C74 C73 C74
SADI C73 C74 C74 C69
FLAT 0.001 C60 > C67
FLAT 0.001 C68 > C77
RIGU C66 C60 C61 C62 C63 C64 C65 C67
EADP C73 C68 C69 C74 C70 C76 C72 C71 C75 C77
L.S. 100 0 0
PLAN 20
TEMP -173.15
MORE -1
BOND $H
CONF
fmap 2 53
acta 44.8
OMIT 6 0 1
OMIT 1 0 9
OMIT 0 0 2
REM
REM
REM
WGHT 0.152000 0.692700
FVAR 0.11001 0.22721 0.38752 0.36632 0.53431 0.55572 0.84895
N1 3 0.292169 0.438561 0.660833 11.00000 0.05496 0.08274 =
0.16568 0.00235 0.01855 -0.01196
N2 3 0.313305 0.489349 0.750611 11.00000 0.05568 0.07562 =
0.14509 0.02237 0.01414 -0.00502
N3 3 0.768705 0.658836 0.819877 11.00000 0.05425 0.09901 =
0.08892 0.01576 0.00134 0.01097
N4 3 0.997917 0.656916 0.770238 11.00000 0.04882 0.09605 =
0.08174 0.01459 -0.00219 0.01212
N5 3 0.728265 0.952520 0.592981 11.00000 0.04848 0.06433 =
0.10030 -0.00338 -0.00399 -0.00375
N6 3 0.958436 0.876483 0.616466 11.00000 0.03853 0.07613 =
0.08352 0.00488 -0.00442 -0.00259
N7 3 0.268469 0.813125 0.783318 11.00000 0.05343 0.08397 =
0.09814 -0.00501 0.01363 0.00592
N8 3 0.269906 0.927013 0.719130 11.00000 0.04954 0.06927 =
0.10529 -0.01143 0.01121 0.00797
N9 3 0.260873 0.802194 0.521267 11.00000 0.04691 0.09211 =
0.08741 -0.00162 -0.00306 0.00133
N10 3 0.322234 0.654777 0.504449 11.00000 0.04318 0.10222 =
0.08865 -0.02046 -0.00620 -0.00372
N11 3 0.783935 0.469775 0.550076 11.00000 0.04856 0.07768 =
0.12093 -0.01121 0.00923 -0.00263
N12 3 1.000704 0.554217 0.569171 11.00000 0.03453 0.07768 =
0.09608 -0.00535 0.01462 0.00118
C1 1 0.416884 0.723033 0.780359 11.00000 0.04736 0.07808 =
0.09402 -0.00198 0.00658 0.00537
C2 1 0.533752 0.705534 0.790973 11.00000 0.05618 0.07778 =
0.09908 0.00050 0.01491 0.00067
AFIX 43
H2 2 0.587820 0.740094 0.800586 11.00000 -1.20000
AFIX 0
C3 1 0.572896 0.637850 0.787711 11.00000 0.05388 0.07740 =
0.08893 0.01637 0.01201 0.00465
C4 1 0.494492 0.588601 0.774030 11.00000 0.06359 0.07260 =
0.09515 0.01686 0.00965 0.00017
AFIX 43
H4 2 0.520571 0.542318 0.771896 11.00000 -1.20000
AFIX 0
C5 1 0.375749 0.605299 0.763047 11.00000 0.05454 0.07197 =
0.09983 0.01382 0.01018 0.00684
C6 1 0.339363 0.671891 0.766387 11.00000 0.04771 0.08707 =
0.09222 0.01073 0.00828 0.00866
AFIX 43
H6 2 0.259136 0.683481 0.758976 11.00000 -1.20000
AFIX 0
C7 1 0.375598 0.794302 0.786133 11.00000 0.05670 0.08221 =
0.11161 -0.01180 -0.00134 0.00054
AFIX 43
H7 2 0.434206 0.828287 0.792417 11.00000 -1.20000
AFIX 0
C8 1 0.693956 0.617245 0.802900 11.00000 0.06451 0.08064 =
0.08713 0.01890 0.01303 0.01298
AFIX 43
H8 2 0.716896 0.570553 0.799792 11.00000 -1.20000
AFIX 0
C9 1 0.290872 0.552080 0.749686 11.00000 0.05544 0.07725 =
0.10234 0.01424 0.00820 0.00218
AFIX 43
H9 2 0.213963 0.566085 0.739690 11.00000 -1.20000
AFIX 0
C10 1 0.329850 0.903384 0.644638 11.00000 0.05408 0.07517 =
0.09567 -0.01658 0.01311 -0.00068
C11 1 0.300698 0.872533 0.605409 11.00000 0.04638 0.08395 =
0.10770 -0.01942 0.00924 -0.00077
AFIX 43
H11 2 0.224183 0.851775 0.602066 11.00000 -1.20000
AFIX 0
C12 1 0.382523 0.871154 0.569981 11.00000 0.04373 0.08585 =
0.09432 -0.00767 0.00379 0.00418
C13 1 0.493282 0.901407 0.575288 11.00000 0.05209 0.08052 =
0.09193 -0.01149 -0.00405 0.00433
AFIX 43
H13 2 0.548283 0.901714 0.551377 11.00000 -1.20000
AFIX 0
C14 1 0.526132 0.931859 0.615608 11.00000 0.04804 0.07443 =
0.10697 -0.00599 0.00594 0.00387
C15 1 0.445588 0.932923 0.649752 11.00000 0.05644 0.07904 =
0.09987 -0.02453 0.00456 -0.00016
AFIX 43
H15 2 0.467241 0.953524 0.676997 11.00000 -1.20000
AFIX 0
C16 1 0.246037 0.901166 0.681424 11.00000 0.05297 0.07579 =
0.11686 -0.02150 0.00624 0.00396
AFIX 43
H16 2 0.170513 0.879617 0.677213 11.00000 -1.20000
AFIX 0
C17 1 0.355275 0.835053 0.528709 11.00000 0.04278 0.09626 =
0.08629 -0.00364 -0.00022 0.00249
AFIX 43
H17 2 0.413618 0.836728 0.505919 11.00000 -1.20000
AFIX 0
C18 1 0.648899 0.958708 0.621981 11.00000 0.06201 0.06417 =
0.09495 -0.00893 0.00088 -0.00090
AFIX 43
H18 2 0.668188 0.981291 0.648815 11.00000 -1.20000
AFIX 0
C19 1 1.007282 0.700987 0.696416 11.00000 0.02519 0.08198 =
0.07812 -0.00055 -0.00066 -0.00078
C20 1 0.997686 0.759937 0.671478 11.00000 0.03593 0.06572 =
0.08143 0.00405 -0.00524 0.00079
AFIX 43
H20 2 0.993534 0.803343 0.685646 11.00000 -1.20000
AFIX 0
C21 1 0.994030 0.756119 0.625327 11.00000 0.03146 0.07331 =
0.07836 0.00399 -0.00240 -0.00260
C22 1 1.001102 0.693051 0.605095 11.00000 0.03382 0.07038 =
0.08112 -0.00025 0.00269 0.00059
AFIX 43
H22 2 1.000079 0.690318 0.573827 11.00000 -1.20000
AFIX 0
C23 1 1.009927 0.631920 0.630490 11.00000 0.02810 0.07373 =
0.08579 0.00443 0.00678 0.00223
C24 1 1.014047 0.637506 0.676219 11.00000 0.02979 0.07346 =
0.08526 0.00524 -0.00017 0.00261
AFIX 43
H24 2 1.021581 0.597311 0.693719 11.00000 -1.20000
AFIX 0
C25 1 1.002691 0.707272 0.745148 11.00000 0.03673 0.08489 =
0.07818 0.00450 -0.00559 0.00531
AFIX 43
H25 2 1.003437 0.751885 0.757763 11.00000 -1.20000
AFIX 0
C26 1 0.976510 0.818945 0.599003 11.00000 0.03496 0.07008 =
0.07338 0.00042 -0.00102 -0.00586
AFIX 43
H26 2 0.978975 0.815803 0.567761 11.00000 -1.20000
AFIX 0
C27 1 1.010277 0.564762 0.610141 11.00000 0.03204 0.07677 =
0.08872 0.00500 0.01228 0.00741
AFIX 43
H27 2 1.018247 0.525942 0.628853 11.00000 -1.20000
AFIX 0
C28 1 0.581513 0.512362 0.554231 11.00000 0.04499 0.08310 =
0.11871 0.00114 0.00074 0.00068
C29 1 0.501423 0.558159 0.536496 11.00000 0.05601 0.09966 =
0.10207 -0.00203 0.00706 -0.01299
AFIX 43
H29 2 0.525064 0.586069 0.512335 11.00000 -1.20000
AFIX 0
C30 1 0.383631 0.564326 0.553831 11.00000 0.05115 0.09189 =
0.11002 0.00108 0.00044 0.00399
C31 1 0.352205 0.523257 0.588381 11.00000 0.05436 0.11192 =
0.12370 0.01714 0.00715 -0.01188
AFIX 43
H31 2 0.272875 0.526125 0.599622 11.00000 -1.20000
AFIX 0
C32 1 0.431967 0.477253 0.607831 11.00000 0.05017 0.09240 =
0.16255 0.01388 0.01059 -0.00046
C33 1 0.546541 0.471992 0.591061 11.00000 0.04897 0.08974 =
0.15327 0.00732 0.01123 -0.00626
AFIX 43
H33 2 0.602241 0.441284 0.604175 11.00000 -1.20000
AFIX 0
C34 1 0.701866 0.508201 0.535457 11.00000 0.05688 0.08539 =
0.10451 -0.01285 0.00480 -0.00977
AFIX 43
H34 2 0.719563 0.536195 0.510657 11.00000 -1.20000
AFIX 0
C35 1 0.297843 0.611868 0.534968 11.00000 0.04982 0.10640 =
0.09680 -0.01246 0.00960 -0.00993
AFIX 43
H35 2 0.218202 0.611042 0.546049 11.00000 -1.20000
AFIX 0
C36 1 0.395965 0.436420 0.644676 11.00000 0.05810 0.08888 =
0.16882 0.02687 0.02507 -0.00781
AFIX 43
H36 2 0.453031 0.406290 0.657549 11.00000 -1.20000
AFIX 0
C37 1 0.220132 0.441731 0.735914 11.00000 0.05734 0.08231 =
0.15100 0.02023 0.01744 -0.00639
PART 7
AFIX 23
H37A 2 0.149969 0.467865 0.725075 11.00000 -1.20000
H37B 2 0.193757 0.412943 0.760994 -41.00000 -1.20000
AFIX 0
PART 0
C38 1 0.267998 0.396496 0.699464 11.00000 0.07115 0.07007 =
0.17784 0.00930 0.03473 -0.01313
PART 6
AFIX 23
H38A 2 0.342600 0.373604 0.709271 11.00000 -1.20000
H38B 2 0.208435 0.360634 0.692086 41.00000 -1.20000
AFIX 0
PART 0
C41 1 1.001382 0.482805 0.553744 11.00000 0.04800 0.07900 =
0.10936 -0.00574 0.01883 0.00399
PART 10
AFIX 23
H41A 2 0.999886 0.451533 0.579458 11.00000 -1.20000
H41B 2 1.076087 0.473950 0.537069 61.00000 -1.20000
AFIX 0
PART 0
C42 1 0.894776 0.468303 0.524657 11.00000 0.06278 0.08340 =
0.11351 -0.02371 0.01516 0.00281
PART 11
AFIX 23
H42A 2 0.890772 0.503057 0.500899 11.00000 -1.20000
H42B 2 0.904248 0.422656 0.510768 -61.00000 -1.20000
AFIX 0
PART 0
C45 1 0.224704 0.692084 0.485460 11.00000 0.05172 0.09202 =
0.07993 -0.01407 -0.00291 -0.00361
AFIX 23
H45A 2 0.153932 0.687644 0.504945 11.00000 -1.20000
H45B 2 0.204008 0.671091 0.456730 11.00000 -1.20000
AFIX 0
C46 1 0.250218 0.766145 0.478546 11.00000 0.05244 0.11702 =
0.07032 -0.00027 -0.00104 0.00692
AFIX 13
H46 2 0.327871 0.770620 0.462327 11.00000 -1.20000
AFIX 0
C47 1 0.151950 0.797190 0.450801 11.00000 0.08381 0.09918 =
0.11377 0.00681 -0.02466 0.00765
AFIX 137
H47A 2 0.075293 0.793198 0.466373 11.00000 -1.50000
H47B 2 0.147024 0.772822 0.422597 11.00000 -1.50000
H47C 2 0.169698 0.845716 0.445409 11.00000 -1.50000
AFIX 0
C48 1 0.182386 0.918838 0.753854 11.00000 0.05009 0.07955 =
0.10127 -0.01933 0.00665 0.00568
PART 1
AFIX 23
H48A 2 0.114316 0.890905 0.743064 11.00000 -1.20000
H48B 2 0.151154 0.964320 0.762759 -21.00000 -1.20000
AFIX 0
PART 0
C49 1 0.239848 0.883979 0.792966 11.00000 0.05968 0.08068 =
0.10864 -0.02710 0.01053 0.00607
PART 2
AFIX 23
H49A 2 0.314085 0.908765 0.801105 11.00000 -1.20000
H49B 2 0.184479 0.885895 0.818444 21.00000 -1.20000
AFIX 0
PART 0
C52 1 0.845637 0.982877 0.601611 11.00000 0.05371 0.06438 =
0.10012 0.00229 -0.01384 -0.00504
PART 5
AFIX 23
H52A 2 0.853933 0.992096 0.633563 11.00000 -1.20000
H52B 2 0.852241 1.027139 0.585783 -31.00000 -1.20000
AFIX 0
PART 0
C53 1 0.945122 0.935598 0.586818 11.00000 0.05176 0.07135 =
0.08366 0.00686 -0.00317 -0.00799
PART 4
AFIX 23
H53A 2 0.927750 0.919021 0.556635 11.00000 -1.20000
H53B 2 1.021463 0.961460 0.585879 31.00000 -1.20000
AFIX 0
PART 0
C56 1 0.987455 0.669675 0.817300 11.00000 0.05277 0.11814 =
0.07625 0.01242 -0.00458 0.01016
PART 8
AFIX 23
H56A 2 0.977488 0.719472 0.822599 11.00000 -1.20000
H56B 2 1.061532 0.654497 0.832398 51.00000 -1.20000
AFIX 0
PART 0
C57 1 0.881160 0.631389 0.835795 11.00000 0.07071 0.09762 =
0.08404 0.02125 0.00342 0.01387
PART 9
AFIX 23
H57A 2 0.887094 0.582403 0.827438 11.00000 -1.20000
H57B 2 0.882829 0.634186 0.868379 -51.00000 -1.20000
AFIX 0
PART 0
PART 1
C51 1 0.156966 0.885087 0.833084 -21.00000 0.09960 0.13453 =
0.11062 -0.02385 0.02808 0.00754
AFIX 137
H51A 2 0.078079 0.867134 0.824772 -21.00000 -1.50000
H51B 2 0.148487 0.932328 0.843703 -21.00000 -1.50000
H51C 2 0.191187 0.856510 0.856501 -21.00000 -1.50000
AFIX 0
PART 0
PART 2
C50 1 0.136850 0.983532 0.768430 21.00000 0.06637 0.07975 =
0.09016 -0.00351 0.02530 0.01111
AFIX 137
H50A 2 0.203411 1.012426 0.778428 21.00000 -1.50000
H50B 2 0.080714 0.976269 0.792840 21.00000 -1.50000
H50C 2 0.095207 1.006255 0.744014 21.00000 -1.50000
AFIX 0
PART 0
PART 3
C55 1 1.061787 0.977540 0.585587 -31.00000 0.05080 0.07070 =
0.11323 0.01953 -0.01562 -0.01220
AFIX 137
H55A 2 1.080953 0.993713 0.615357 -31.00000 -1.50000
H55B 2 1.051521 1.017020 0.565938 -31.00000 -1.50000
H55C 2 1.127259 0.948626 0.574683 -31.00000 -1.50000
AFIX 0
PART 0
PART 4
C54 1 0.855821 1.042538 0.565485 31.00000 0.08198 0.06177 =
0.13478 0.01026 -0.03066 -0.02863
AFIX 137
H54A 2 0.843506 1.023116 0.536029 31.00000 -1.50000
H54B 2 0.935550 1.063509 0.567080 31.00000 -1.50000
H54C 2 0.794639 1.077492 0.571242 31.00000 -1.50000
AFIX 0
PART 0
PART 5
C40 1 0.182113 0.342351 0.690520 -41.00000 0.09080 0.10416 =
0.28210 -0.02904 0.05437 -0.04254
AFIX 137
H40A 2 0.180569 0.310177 0.715343 -41.00000 -1.50000
H40B 2 0.205497 0.317917 0.663623 -41.00000 -1.50000
H40C 2 0.102264 0.362387 0.686552 -41.00000 -1.50000
AFIX 0
PART 0
PART 6
C39 1 0.181021 0.395037 0.771186 41.00000 0.09187 0.09752 =
0.08954 0.00488 0.00847 -0.05227
AFIX 137
H39A 2 0.250398 0.381498 0.788996 41.00000 -1.50000
H39B 2 0.144352 0.354114 0.758125 41.00000 -1.50000
H39C 2 0.122255 0.418386 0.789940 41.00000 -1.50000
AFIX 0
PART 0
PART 7
C58 1 1.104485 0.654021 0.840702 -51.00000 0.04237 0.10240 =
0.05667 0.02759 -0.00512 0.01933
AFIX 137
H58A 2 1.130494 0.607412 0.833253 -51.00000 -1.50000
H58B 2 1.092757 0.657597 0.872639 -51.00000 -1.50000
H58C 2 1.165808 0.686941 0.831330 -51.00000 -1.50000
AFIX 0
PART 0
PART 8
C59 1 0.882545 0.636292 0.888210 51.00000 0.17265 0.29083 =
0.11769 0.04778 0.02599 0.11004
AFIX 33
H59A 2 0.958347 0.617841 0.899442 51.00000 -1.50000
H59B 2 0.874523 0.684384 0.897171 51.00000 -1.50000
H59C 2 0.815618 0.609668 0.900268 51.00000 -1.50000
AFIX 0
PART 0
PART 9
C43 1 1.109011 0.465336 0.525440 -61.00000 0.03916 0.07696 =
0.10124 -0.02668 0.01896 0.00207
AFIX 137
H43A 2 1.119153 0.500551 0.502681 -61.00000 -1.50000
H43B 2 1.096513 0.420613 0.511406 -61.00000 -1.50000
H43C 2 1.181000 0.463542 0.543923 -61.00000 -1.50000
AFIX 0
PART 0
PART 10
C44 1 0.919770 0.395008 0.505531 61.00000 0.08173 0.14094 =
0.27876 -0.10346 -0.00328 -0.01394
AFIX 137
H44A 2 0.952815 0.365631 0.528767 61.00000 -1.50000
H44B 2 0.977404 0.398411 0.481245 61.00000 -1.50000
H44C 2 0.844722 0.375136 0.494620 61.00000 -1.50000
AFIX 0
PART 0
C60 1 0.635741 0.632983 0.670974 71.00000 0.04570 0.10627 =
0.11744 0.03193 0.00781 0.00028
C61 1 0.694950 0.691632 0.675205 71.00000 0.03609 0.11570 =
0.12750 0.02483 -0.00340 -0.00280
AFIX 43
H61 2 0.778567 0.690860 0.681121 71.00000 -1.20000
AFIX 0
C62 1 0.637196 0.753179 0.671161 71.00000 0.04698 0.10936 =
0.18755 -0.00200 -0.00920 -0.01031
AFIX 43
H62 2 0.680270 0.794954 0.674237 71.00000 -1.20000
AFIX 0
C63 1 0.515842 0.754036 0.662577 71.00000 0.04662 0.10388 =
0.14567 -0.00795 -0.00654 0.00002
AFIX 43
H63 2 0.475640 0.796782 0.659762 71.00000 -1.20000
AFIX 0
C64 1 0.453871 0.695902 0.658153 71.00000 0.03220 0.10298 =
0.08171 0.01335 0.00446 -0.00036
C65 1 0.513317 0.635587 0.662304 71.00000 0.04358 0.09350 =
0.12571 0.01905 0.00121 -0.00185
AFIX 43
H65 2 0.470128 0.593855 0.659202 71.00000 -1.20000
AFIX 0
C66 1 0.701696 0.568256 0.675608 71.00000 0.06864 0.12696 =
0.20682 0.02984 -0.00780 0.00688
AFIX 137
H66A 2 0.749552 0.560128 0.649022 71.00000 -1.50000
H66B 2 0.644787 0.530459 0.679611 71.00000 -1.50000
H66C 2 0.754804 0.570945 0.701287 71.00000 -1.50000
AFIX 0
C67 1 0.320149 0.696408 0.648690 71.00000 0.03571 0.11864 =
0.11919 0.00396 -0.00317 0.00242
AFIX 137
H67A 2 0.280261 0.728701 0.668643 71.00000 -1.50000
H67B 2 0.287423 0.650281 0.653225 71.00000 -1.50000
H67C 2 0.306497 0.710568 0.618098 71.00000 -1.50000
AFIX 66
C68 1 0.434746 0.725098 0.906037 71.00000 0.39847
PART 2
AFIX 43
H68 2 0.397455 0.694955 0.885599 70.50000 -1.20000
AFIX 65
PART 0
C69 1 0.365214 0.762834 0.935331 71.00000 0.39847
PART 1
AFIX 43
H69 2 0.280400 0.758481 0.934915 70.50000 -1.20000
AFIX 65
PART 0
C70 1 0.419776 0.806938 0.965236 71.00000 0.39847
AFIX 43
H70 2 0.372253 0.832729 0.985258 71.00000 -1.20000
AFIX 65
C71 1 0.543871 0.813308 0.965845 71.00000 0.39847
PART 1
AFIX 43
H71 2 0.581161 0.843452 0.986283 70.50000 -1.20000
AFIX 65
PART 0
C72 1 0.613405 0.775572 0.936551 71.00000 0.39847
PART 2
AFIX 43
H72 2 0.698218 0.779926 0.936967 70.50000 -1.20000
AFIX 65
PART 0
C73 1 0.558844 0.731468 0.906647 71.00000 0.39847
AFIX 43
H73 2 0.606367 0.705677 0.886625 71.00000 -1.20000
AFIX 0
PART 1
C74 1 0.376200 0.677386 0.873673 70.50000 0.39847
AFIX 33
H74A 2 0.437892 0.655066 0.855689 70.50000 -1.50000
H74B 2 0.330396 0.642444 0.889674 70.50000 -1.50000
H74C 2 0.322103 0.703510 0.854534 70.50000 -1.50000
AFIX 0
C75 1 0.750683 0.782633 0.937234 70.50000 0.39847
AFIX 33
H75A 2 0.774079 0.815540 0.960099 70.50000 -1.50000
H75B 2 0.786877 0.737896 0.943590 70.50000 -1.50000
H75C 2 0.778583 0.798963 0.908451 70.50000 -1.50000
AFIX 0
PART 0
PART 2
C76 1 0.228159 0.755776 0.934639 70.50000 0.39847
AFIX 33
H76A 2 0.204781 0.722868 0.911773 70.50000 -1.50000
H76B 2 0.200247 0.739444 0.963421 70.50000 -1.50000
H76C 2 0.191960 0.800511 0.928281 70.50000 -1.50000
AFIX 0
C77 1 0.604584 0.861738 0.998659 70.50000 0.39847
AFIX 33
H77A 2 0.691661 0.859885 0.994550 70.50000 -1.50000
H77B 2 0.576346 0.908712 0.993656 70.50000 -1.50000
H77C 2 0.584638 0.847643 1.028793 70.50000 -1.50000
AFIX 0
HKLF 4
REM THL_397_A2_100K_Solvate in P2(1)2(1)2(1)
REM R1 = 0.0786 for 7494 Fo > 4sig(Fo) and 0.0948 for all 9431 data
REM 749 parameters refined using 76 restraints
END
WGHT 0.1535 0.7074
REM Highest difference peak 0.537, deepest hole -0.313, 1-sigma level 0.070
Q1 1 0.6901 0.8021 0.7012 11.00000 0.05 0.54
Q2 1 0.4782 0.6248 0.9068 11.00000 0.05 0.41
Q3 1 0.5616 0.6203 0.9142 11.00000 0.05 0.40
Q4 1 0.6566 0.5983 0.9196 11.00000 0.05 0.34
Q5 1 0.7936 0.7990 0.9228 11.00000 0.05 0.33
Q6 1 0.2929 0.6387 0.9353 11.00000 0.05 0.33
Q7 1 0.8939 0.7634 0.9399 11.00000 0.05 0.32
Q8 1 0.8651 0.7059 0.9598 11.00000 0.05 0.32
Q9 1 0.9114 0.7045 0.9624 11.00000 0.05 0.32
Q10 1 0.9205 0.7950 0.9253 11.00000 0.05 0.31
Q11 1 0.0223 0.7648 0.9384 11.00000 0.05 0.31
Q12 1 0.0641 0.7819 0.9285 11.00000 0.05 0.31
Q13 1 0.1861 0.7135 0.4393 11.00000 0.05 0.31
Q14 1 0.4804 0.6647 0.6559 11.00000 0.05 0.30
Q15 1 0.3796 0.6925 0.6479 11.00000 0.05 0.30
Q16 1 0.0531 0.7400 0.9547 11.00000 0.05 0.29
Q17 1 0.5078 0.6232 0.6460 11.00000 0.05 0.27
Q18 1 0.4716 0.7157 0.6485 11.00000 0.05 0.27
Q19 1 0.6415 0.6266 0.6595 11.00000 0.05 0.26
Q20 1 0.7640 0.6397 0.9353 11.00000 0.05 0.25
;
_shelx_res_checksum 39216
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_CC3-R_0-65_CC13-S_0-35_CC13-R
_database_code_depnum_ccdc_archive 'CCDC 1520511'
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_audit_creation_date 2015-07-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C72 H84 N12, C60 H72 N12, 2.25(C H2 Cl2), 6(H2 O), 1.96(C4 H8 O2)'
_chemical_formula_sum 'C142.09 H188.18 Cl5.50 N24 O9.92'
_chemical_formula_weight 2586.19
_chemical_absolute_configuration CC3-R
_chemical_melting_point ?
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'
Cl Cl 0.1484 0.1585 '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'
_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.
;
_space_group_crystal_system trigonal
_space_group_IT_number 150
_space_group_name_H-M_alt 'P 3 2 1'
_space_group_name_Hall 'P 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
_cell_length_a 17.5575(7)
_cell_length_b 17.5575(7)
_cell_length_c 28.6921(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 7659.8(7)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9882
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 26.25
_cell_measurement_theta_min 2.43
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.164
_exptl_absorpt_correction_T_max 0.9585
_exptl_absorpt_correction_T_min 0.7876
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1335 before and 0.1143 after correction.
The Ratio of minimum to maximum transmission is 0.8217.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.121
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 2763
_exptl_crystal_size_max 0.163
_exptl_crystal_size_mid 0.145
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0948
_diffrn_reflns_av_unetI/netI 0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.630
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 53335
_diffrn_reflns_point_group_measured_fraction_full 0.620
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 21.966
_diffrn_reflns_theta_min 0.710
_diffrn_ambient_temperature 100.0
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type 'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.630
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation 0.3
_diffrn_radiation_monochromator Confocal
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Rotating Anode'
_diffrn_source_current 24.0
_diffrn_source_power 1.2
_diffrn_source_target Mo
_diffrn_source_type 'Rotating Anode'
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.785
_reflns_Friedel_fraction_full 0.609
_reflns_Friedel_fraction_max 0.999
_reflns_number_gt 5557
_reflns_number_total 6254
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution ?
_refine_diff_density_max 0.713
_refine_diff_density_min -0.686
_refine_diff_density_rms 0.151
_refine_ls_abs_structure_details
;
Flack x determined using 2216 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.69(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 2.372
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 595
_refine_ls_number_reflns 6254
_refine_ls_number_restraints 230
_refine_ls_R_factor_all 0.1435
_refine_ls_R_factor_gt 0.1285
_refine_ls_restrained_S_all 2.359
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3302
_refine_ls_wR_factor_ref 0.3421
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, {H4SA,H4SB,H4S} of C4S, All C(H,H) groups
At 1.5 times of:
{H17B,H17C,H17D} of C17C, {H1B,H1C,H1D} of C1, {H19C,H19D,H19E} of C19B,
{H18B,H18C,H18D} of C18B, {H17E,H17F,H17G} of C17B
2. Restrained distances
N3C_$1-C13C_$1
1.49 with sigma of 0.015
C14C-C13C_$1
1.54 with sigma of 0.015
C11C_$1-C10C_$1 = C11C_$1-C10C_$2
1.39 with sigma of 0.015
N3C-C13C = N2C-C15C = N4C-C14C = N1C-C16C
1.47 with sigma of 0.015
C16C-C15C
1.54 with sigma of 0.015
Cl4S-C5S = Cl3S-C5S = Cl5S-C7S
1.74 with sigma of 0.02
C7C-C2C = C9C-C6C = C8C-C4C
1.47 with sigma of 0.015
N4C-C9C = N3C-C7C = N2C-C8C
1.23 with sigma of 0.015
N4C-C13C_$1
2.4 with sigma of 0.02
C14C-N3C_$1
2.4 with sigma of 0.02
C10C_$1-C10C
2.41 with sigma of 0.02
C11C-C11C_$1
2.41 with sigma of 0.02
C10C_$1-C10C_$2
2.41 with sigma of 0.02
C4S-C7C \\sim C7C-C3C
with sigma of 0.02
C3C-C8C \\sim C8C-C5C
with sigma of 0.02
C5C-C9C \\sim C9C-C4S
with sigma of 0.02
3. Restrained planarity
N3C, N4C, N2C, C4C, C3C, C2C, C4S, C6C, C5C, C7C, C8C, C9C
with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C7C) = Uiso(N3C) = Uiso(C13C) = Uiso(C14C) = Uiso(N4C) = Uiso(C9C)
5. Rigid body (RIGU) restrains
N3B, N2B, N4B, N1B, C1B, C6B, C5B, C4B, C3B, C2B, C7B, C8B, C9B, C10B, C11B,
C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
Cl5S, C7S
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C4A, C5A, C6A, C7A, C8A, C9A
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(N3C)=Sof(N1C)=Sof(N4C)=Sof(N2C)=Sof(C4C)=Sof(C3C)=Sof(H3C)=Sof(C2C)=
Sof(H4S)=Sof(C6C)=Sof(C5C)=Sof(H5C)=Sof(C7C)=Sof(H7C)=Sof(C8C)=Sof(H8C)=
Sof(C9C)=Sof(H9C)=Sof(C10C)=Sof(H10C)=Sof(C11C)=Sof(C12C)=Sof(H12C)=Sof(C13C)=
Sof(H13C)=Sof(C15C)=Sof(H15A)=Sof(H15B)=Sof(C16C)=Sof(C17C)=Sof(H17B)=
Sof(H17C)=Sof(H17D)=1-FVAR(1)
Sof(O2S)=Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=
Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H4SA)=Sof(H4SB)=Sof(C14C)=Sof(H14B)=Sof(H14C)=
Sof(N3B)=Sof(N2B)=Sof(N4B)=Sof(N1B)=Sof(C1B)=Sof(C6B)=Sof(H6B)=Sof(C5B)=
Sof(C4B)=Sof(H4B)=Sof(C3B)=Sof(C2B)=Sof(H2B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=
Sof(H8B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(C13B)=
Sof(H13A)=Sof(H13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(C15B)=Sof(C16B)=
Sof(H16B)=Sof(C17B)=Sof(H17E)=Sof(H17F)=Sof(H17G)=Sof(C18B)=Sof(H18B)=
Sof(H18C)=Sof(H18D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(H19E)=Sof(C1)=Sof(H1B)=
Sof(H1C)=Sof(H1D)=FVAR(1)
Fixed Sof: Cl4S(0.33333) Cl3S(0.33333) C5S(0.33333) O8S(0.08333) O9S(0.25)
Cl5S(0.5) C7S(0.25) H7SA(0.25) H7SB(0.25) O3S(0.05556) O7S(0.33333)
O6S(0.11111) O5S(0.08333) C2(0.33333) Cl1S(0.33333) O10S(0.08333)
7.a Ternary CH refined with riding coordinates:
C4A(H4A), C9A(H9A), C18A(H18A), C23A(H23A)
7.b Secondary CH2 refined with riding coordinates:
C5A(H5AA,H5AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C19A(H19A,
H19B), C20A(H20A,H20B), C21A(H21A,H21B), C22A(H22A,H22B), C1S(H1SA,H1SB),
C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C14C(H14B,H14C), C15C(H15A,
H15B), C13B(H13A,H13B), C14B(H14D,H14E), C7S(H7SA,H7SB)
7.c Aromatic/amide H refined with riding coordinates:
C1A(H1A), C3A(H3A), C10A(H10A), C16A(H16A), C14A(H14A), C12A(H12A),
C17A(H17A), C24A(H24A), C3C(H3C), C4S(H4S), C5C(H5C), C7C(H7C), C8C(H8C),
C9C(H9C), C10C(H10C), C12C(H12C), C13C(H13C), C6B(H6B), C4B(H4B), C2B(H2B),
C7B(H7B), C8B(H8B), C9B(H9B), C11B(H11B), C16B(H16B)
7.d Fitted hexagon refined as free rotating group:
C11A(C16A,C15A,C14A,C13A,C12A), C4C(C3C,C2C,C4S,C6C,C5C), C1B(C6B,C5B,C4B,C3B,
C2B)
7.e Idealised Me refined as rotating group:
C17C(H17B,H17C,H17D), C17B(H17E,H17F,H17G), C18B(H18B,H18C,H18D), C19B(H19C,
H19D,H19E), C1(H1B,H1C,H1D)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
N4A N 0.9279(5) 0.6933(6) 0.4279(3) 0.060(2) Uani 1 1 d . . . . .
N3A N 0.7748(5) 0.7132(5) 0.4361(3) 0.054(2) Uani 1 1 d . . . . .
N1A N 0.7563(5) 0.8906(5) 0.1664(2) 0.053(2) Uani 1 1 d . . . . .
N2A N 0.6509(6) 0.8173(5) 0.2484(3) 0.062(2) Uani 1 1 d . . . . .
C1A C 0.9371(7) 1.0256(6) 0.1689(3) 0.059(3) Uani 1 1 d . . . . .
H1A H 0.8941 1.0434 0.1695 0.070 Uiso 1 1 calc R . . . .
C2A C 0.9111(7) 0.9376(6) 0.1685(3) 0.056(2) Uani 1 1 d . . . . .
C3A C 0.8178(6) 0.8693(6) 0.1682(3) 0.052(2) Uani 1 1 d . . . . .
H3A H 0.8020 0.8091 0.1694 0.063 Uiso 1 1 calc R . . . .
C4A C 0.6663(6) 0.8183(7) 0.1635(4) 0.063(3) Uani 1 1 d . U . . .
H4A H 0.6653 0.7611 0.1664 0.075 Uiso 1 1 calc R . . . .
C5A C 0.6284(8) 0.8230(8) 0.1163(4) 0.086(3) Uani 1 1 d . U . . .
H5AA H 0.6610 0.8131 0.0912 0.104 Uiso 1 1 calc R . . . .
H5AB H 0.6363 0.8825 0.1121 0.104 Uiso 1 1 calc R . . . .
C6A C 0.5300(10) 0.7541(11) 0.1126(7) 0.122(5) Uani 1 1 d . U . . .
H6AA H 0.5065 0.7614 0.0826 0.146 Uiso 1 1 calc R . . . .
H6AB H 0.5223 0.6943 0.1134 0.146 Uiso 1 1 calc R . . . .
C7A C 0.4810(10) 0.7648(12) 0.1518(7) 0.131(6) Uani 1 1 d . U . . .
H7AA H 0.4183 0.7188 0.1496 0.157 Uiso 1 1 calc R . . . .
H7AB H 0.4845 0.8227 0.1490 0.157 Uiso 1 1 calc R . . . .
C8A C 0.5160(8) 0.7587(10) 0.1988(6) 0.105(4) Uani 1 1 d . U . . .
H8AA H 0.5083 0.6992 0.2028 0.126 Uiso 1 1 calc R . . . .
H8AB H 0.4823 0.7679 0.2236 0.126 Uiso 1 1 calc R . . . .
C9A C 0.6134(6) 0.8275(6) 0.2032(4) 0.062(2) Uani 1 1 d . U . . .
H9A H 0.6201 0.8875 0.2020 0.075 Uiso 1 1 calc R . . . .
C10A C 0.6762(7) 0.8787(8) 0.2767(4) 0.067(3) Uani 1 1 d . . . . .
H10A H 0.6721 0.9289 0.2683 0.080 Uiso 1 1 calc R . . . .
C11A C 0.7133(4) 0.8767(4) 0.32379(18) 0.059(3) Uani 1 1 d . . . . .
C16A C 0.7365(5) 0.9462(3) 0.3545(2) 0.058(3) Uani 1 1 d G . . . .
H16A H 0.7311 0.9952 0.3452 0.070 Uiso 1 1 calc R . . . .
C15A C 0.7677(5) 0.9439(3) 0.3987(2) 0.063(3) Uani 1 1 d G . . . .
C14A C 0.7756(5) 0.8722(4) 0.41222(17) 0.064(3) Uani 1 1 d G . . . .
H14A H 0.7969 0.8707 0.4424 0.077 Uiso 1 1 calc R . . . .
C13A C 0.7524(5) 0.8027(3) 0.3815(2) 0.059(3) Uani 1 1 d G . . . .
C12A C 0.7212(4) 0.8050(3) 0.33732(19) 0.059(3) Uani 1 1 d G . . . .
H12A H 0.7054 0.7575 0.3163 0.070 Uiso 1 1 calc R . . . .
C17A C 0.7568(7) 0.7234(6) 0.3955(4) 0.058(3) Uani 1 1 d . . . . .
H17A H 0.7456 0.6795 0.3729 0.070 Uiso 1 1 calc R . . . .
C18A C 0.7740(6) 0.6324(6) 0.4478(3) 0.049(2) Uani 1 1 d . . . . .
H18A H 0.7598 0.5948 0.4193 0.059 Uiso 1 1 calc R . . . .
C19A C 0.7035(7) 0.5822(7) 0.4857(4) 0.063(3) Uani 1 1 d . . . . .
H19A H 0.7142 0.6218 0.5125 0.075 Uiso 1 1 calc R . . . .
H19B H 0.6446 0.5646 0.4729 0.075 Uiso 1 1 calc R . . . .
C20A C 0.7048(8) 0.5015(7) 0.5023(4) 0.069(3) Uani 1 1 d . . . . .
H20A H 0.6908 0.4601 0.4760 0.082 Uiso 1 1 calc R . . . .
H20B H 0.6596 0.4717 0.5267 0.082 Uiso 1 1 calc R . . . .
C21A C 0.7961(7) 0.5272(7) 0.5221(4) 0.062(3) Uani 1 1 d . . . . .
H21A H 0.8100 0.5674 0.5490 0.075 Uiso 1 1 calc R . . . .
H21B H 0.7973 0.4742 0.5326 0.075 Uiso 1 1 calc R . . . .
C22A C 0.8631(7) 0.5731(7) 0.4829(4) 0.065(3) Uani 1 1 d . . . . .
H22A H 0.9224 0.5885 0.4942 0.078 Uiso 1 1 calc R . . . .
H22B H 0.8484 0.5318 0.4564 0.078 Uiso 1 1 calc R . . . .
C23A C 0.8648(6) 0.6546(6) 0.4662(3) 0.050(2) Uani 1 1 d . . . . .
H23A H 0.8822 0.6977 0.4924 0.060 Uiso 1 1 calc R . . . .
C24A C 0.9834(7) 0.7748(7) 0.4327(4) 0.063(3) Uani 1 1 d . . . . .
H24A H 0.9784 0.8053 0.4587 0.076 Uiso 1 1 calc R . . . .
O2S O 0.9160(8) 0.6598(8) 0.2514(4) 0.070(3) Uiso 0.654(6) 1 d . . . A 1
O1S O 0.7673(8) 0.6738(8) 0.2736(4) 0.075(3) Uiso 0.654(6) 1 d . . . A 1
C1S C 0.8307(11) 0.5802(11) 0.2562(6) 0.069(4) Uiso 0.654(6) 1 d . . . A 1
H1SA H 0.8408 0.5301 0.2608 0.083 Uiso 0.654(6) 1 calc R . . A 1
H1SB H 0.7986 0.5702 0.2264 0.083 Uiso 0.654(6) 1 calc R . . A 1
C2S C 0.9041(13) 0.7304(13) 0.2366(6) 0.080(5) Uiso 0.654(6) 1 d . . . A 1
H2SA H 0.8746 0.7165 0.2058 0.096 Uiso 0.654(6) 1 calc R . . A 1
H2SB H 0.9620 0.7846 0.2334 0.096 Uiso 0.654(6) 1 calc R . . A 1
C3S C 0.8520(13) 0.7436(13) 0.2699(7) 0.081(5) Uiso 0.654(6) 1 d . . . A 1
H3SA H 0.8808 0.7544 0.3008 0.098 Uiso 0.654(6) 1 calc R . . A 1
H3SB H 0.8495 0.7969 0.2613 0.098 Uiso 0.654(6) 1 calc R . . A 1
N3C N 0.6057(19) 0.5686(7) 0.3137(8) 0.121(6) Uiso 0.346(6) 1 d D . . A 2
N1C N 0.802(3) 0.578(2) 0.0484(12) 0.106(11) Uiso 0.346(6) 1 d D . . A 2
N4C N 0.9686(15) 0.5639(7) 0.3169(8) 0.121(6) Uiso 0.346(6) 1 d D . . A 2
N2C N 0.8502(19) 0.6798(5) 0.1324(7) 0.112(11) Uiso 0.346(6) 1 d D . . A 2
C4C C 0.8463(10) 0.6328(3) 0.2078(4) 0.078(9) Uiso 0.346(6) 1 d D . . A 2
C3C C 0.7662(9) 0.6273(4) 0.2177(4) 0.093(11) Uiso 0.346(6) 1 d DG . . A 2
H3C H 0.7371 0.6420 0.1945 0.111 Uiso 0.346(6) 1 calc R . . A 2
C2C C 0.7285(8) 0.6002(4) 0.2616(5) 0.122(15) Uiso 0.346(6) 1 d DG . . A 2
C4S C 0.7711(9) 0.5787(4) 0.2955(4) 0.139(6) Uiso 1 1 d DG . . . .
H4SA H 0.7989 0.5888 0.3267 0.166 Uiso 0.654(6) 1 calc R . . A 1
H4SB H 0.7127 0.5245 0.2957 0.166 Uiso 0.654(6) 1 calc R . . A 1
H4S H 0.7454 0.5602 0.3255 0.166 Uiso 0.346(6) 1 calc R . . A 2
C6C C 0.8512(9) 0.5843(4) 0.2857(4) 0.092(11) Uiso 0.346(6) 1 d DG . . A 2
C5C C 0.8888(8) 0.6113(4) 0.2418(4) 0.097(12) Uiso 0.346(6) 1 d DG . . A 2
H5C H 0.9436 0.6152 0.2350 0.116 Uiso 0.346(6) 1 calc R . . A 2
C7C C 0.6426(14) 0.5929(6) 0.2743(8) 0.121(6) Uiso 0.346(6) 1 d D . . A 2
H7C H 0.6135 0.6076 0.2511 0.145 Uiso 0.346(6) 1 calc R . . A 2
C8C C 0.8876(15) 0.6608(5) 0.1625(6) 0.086(10) Uiso 0.346(6) 1 d D . . A 2
H8C H 0.9424 0.6643 0.1562 0.103 Uiso 0.346(6) 1 calc R . . A 2
C9C C 0.8971(14) 0.5612(6) 0.3221(7) 0.121(6) Uiso 0.346(6) 1 d D . . A 2
H9C H 0.8694 0.5430 0.3517 0.145 Uiso 0.346(6) 1 calc R . . A 2
C10C C 0.6047(17) 0.360(2) 0.0553(14) 0.102(12) Uiso 0.346(6) 1 d D . . A 2
H10C H 0.5623 0.3787 0.0573 0.122 Uiso 0.346(6) 1 calc R . . A 2
C11C C 0.694(2) 0.4227(10) 0.0538(14) 0.098(12) Uiso 0.346(6) 1 d D . . A 2
C12C C 0.728(3) 0.523(3) 0.0550(14) 0.097(12) Uiso 0.346(6) 1 d . . . A 2
H12C H 0.6867 0.5419 0.0616 0.116 Uiso 0.346(6) 1 calc R . . A 2
C13C C 0.519(2) 0.562(2) 0.317(2) 0.121(6) Uiso 0.346(6) 1 d D . . A 2
H13C H 0.5012 0.5999 0.3026 0.145 Uiso 0.346(6) 1 calc R . . A 2
C14C C 1.020(2) 0.538(2) 0.3477(9) 0.121(6) Uiso 0.654(6) 1 d D . . A 2
H14B H 0.9840 0.5043 0.3748 0.145 Uiso 0.654(6) 1 calc R . . A 2
H14C H 1.0734 0.5910 0.3591 0.145 Uiso 0.654(6) 1 calc R . . A 2
C15C C 0.898(2) 0.722(3) 0.0891(10) 0.075(11) Uiso 0.346(6) 1 d D . . A 2
H15A H 0.9493 0.7132 0.0849 0.090 Uiso 0.346(6) 1 calc R . . A 2
H15B H 0.9185 0.7854 0.0889 0.090 Uiso 0.346(6) 1 calc R . . A 2
C16C C 0.827(3) 0.672(2) 0.0509(18) 0.078(15) Uiso 0.346(6) 1 d D . . A 2
C17C C 0.770(4) 0.705(4) 0.0485(18) 0.119(15) Uiso 0.346(6) 1 d . . . A 2
H17B H 0.7348 0.6836 0.0201 0.178 Uiso 0.346(6) 1 calc GR . . A 2
H17C H 0.8042 0.7695 0.0480 0.178 Uiso 0.346(6) 1 calc GR . . A 2
H17D H 0.7314 0.6854 0.0758 0.178 Uiso 0.346(6) 1 calc GR . . A 2
N3B N 0.5071(10) 0.5206(8) 0.2783(5) 0.068(3) Uani 0.654(6) 1 d . U . A 1
N2B N 0.3812(10) 0.2981(10) 0.0899(5) 0.072(4) Uani 0.654(6) 1 d . U . A 1
N4B N 0.5620(8) 0.4733(8) 0.3639(4) 0.055(3) Uani 0.654(6) 1 d . U . A 1
N1B N 0.3534(10) 0.1171(11) 0.0985(5) 0.078(4) Uani 0.654(6) 1 d . U . A 1
C1B C 0.5579(7) 0.5217(7) 0.2016(3) 0.070(4) Uani 0.654(6) 1 d . U . A 1
C6B C 0.4839(6) 0.4433(7) 0.1886(3) 0.067(4) Uani 0.654(6) 1 d G U . A 1
H6B H 0.4371 0.4130 0.2101 0.081 Uiso 0.654(6) 1 calc R . . A 1
C5B C 0.4785(6) 0.4092(6) 0.1443(3) 0.069(4) Uani 0.654(6) 1 d G U . A 1
C4B C 0.5471(7) 0.4535(8) 0.1128(3) 0.076(4) Uani 0.654(6) 1 d G U . A 1
H4B H 0.5434 0.4302 0.0825 0.091 Uiso 0.654(6) 1 calc R . . A 1
C3B C 0.6211(6) 0.5319(8) 0.1257(3) 0.079(4) Uani 0.654(6) 1 d G U . A 1
C2B C 0.6265(6) 0.5660(6) 0.1701(4) 0.073(4) Uani 0.654(6) 1 d G U . A 1
H2B H 0.6771 0.6196 0.1790 0.088 Uiso 0.654(6) 1 calc R . . A 1
C7B C 0.5645(13) 0.5618(12) 0.2469(6) 0.071(4) Uani 0.654(6) 1 d . U . A 1
H7B H 0.6121 0.6192 0.2531 0.085 Uiso 0.654(6) 1 calc R . . A 1
C8B C 0.3949(13) 0.3258(13) 0.1319(6) 0.077(4) Uani 0.654(6) 1 d . U . A 1
H8B H 0.3525 0.2939 0.1553 0.092 Uiso 0.654(6) 1 calc R . . A 1
C9B C 0.6966(11) 0.4226(11) 0.3674(4) 0.056(3) Uani 0.654(6) 1 d . U . A 1
H9B H 0.7172 0.4840 0.3680 0.067 Uiso 0.654(6) 1 calc R . . A 1
C10B C 0.6068(10) 0.3638(10) 0.3670(4) 0.054(3) Uani 0.654(6) 1 d . U . A 1
C11B C 0.5419(10) 0.3929(11) 0.3654(4) 0.056(3) Uani 0.654(6) 1 d . U . A 1
H11B H 0.4814 0.3493 0.3654 0.067 Uiso 0.654(6) 1 calc R . . A 1
C12B C 0.4948(12) 0.4999(14) 0.3655(7) 0.075(4) Uani 0.654(6) 1 d . U . A 1
C13B C 0.511(2) 0.5594(16) 0.3271(8) 0.104(7) Uani 0.654(6) 1 d . U . A 1
H13A H 0.5701 0.6118 0.3313 0.125 Uiso 0.654(6) 1 calc R . . A 1
H13B H 0.4675 0.5793 0.3285 0.125 Uiso 0.654(6) 1 calc R . . A 1
C14B C 0.3020(15) 0.2231(17) 0.0826(7) 0.084(5) Uani 0.654(6) 1 d . U . A 1
H14D H 0.2675 0.2372 0.0605 0.101 Uiso 0.654(6) 1 calc R . . A 1
H14E H 0.2694 0.2060 0.1125 0.101 Uiso 0.654(6) 1 calc R . . A 1
C15B C 0.3057(18) 0.1431(18) 0.0636(8) 0.086(6) Uani 0.654(6) 1 d . U . A 1
C16B C 0.4222(13) 0.1162(13) 0.0900(6) 0.077(5) Uani 0.654(6) 1 d . U . A 1
H16B H 0.4474 0.1332 0.0598 0.092 Uiso 0.654(6) 1 calc R . . A 1
C17B C 0.2196(14) 0.0653(14) 0.0527(7) 0.088(5) Uani 0.654(6) 1 d . U . A 1
H17E H 0.2276 0.0152 0.0455 0.132 Uiso 0.654(6) 1 calc GR . . A 1
H17F H 0.1937 0.0782 0.0257 0.132 Uiso 0.654(6) 1 calc GR . . A 1
H17G H 0.1803 0.0510 0.0796 0.132 Uiso 0.654(6) 1 calc GR . . A 1
C18B C 0.3580(16) 0.1733(16) 0.0172(6) 0.096(6) Uani 0.654(6) 1 d . U . A 1
H18B H 0.4090 0.2323 0.0212 0.144 Uiso 0.654(6) 1 calc GR . . A 1
H18C H 0.3200 0.1746 -0.0074 0.144 Uiso 0.654(6) 1 calc GR . . A 1
H18D H 0.3780 0.1322 0.0086 0.144 Uiso 0.654(6) 1 calc GR . . A 1
C19B C 0.5098(13) 0.5552(13) 0.4070(7) 0.088(5) Uani 0.654(6) 1 d . U . A 1
H19C H 0.5090 0.5229 0.4350 0.133 Uiso 0.654(6) 1 calc GR . . A 1
H19D H 0.4634 0.5706 0.4091 0.133 Uiso 0.654(6) 1 calc GR . . A 1
H19E H 0.5671 0.6091 0.4043 0.133 Uiso 0.654(6) 1 calc GR . . A 1
Cl2S Cl 1.0000 1.0000 0.2865(6) 0.216(5) Uiso 1 3 d S T P B 1
Cl4S Cl 0.6357(17) 0.3605(16) 0.1597(7) 0.175(6) Uiso 0.3333 1 d D . . C 1
Cl3S Cl 0.6688(14) 0.3589(8) 0.2495(3) 0.101(4) Uiso 0.3333 1 d D . . C 1
C5S C 0.623(4) 0.286(2) 0.2022(12) 0.16(2) Uiso 0.3333 1 d D . . C 1
O8S O 0.3333 0.6667 0.040(5) 0.20(5) Uiso 0.25 3 d S T P D 1
O9S O 0.382(6) 0.716(6) -0.007(3) 0.24(4) Uiso 0.25 1 d . . . E 3
Cl5S Cl 0.4605(8) 0.5434(7) 0.0292(3) 0.135(3) Uani 0.5 1 d D U . F 1
C7S C 0.4464(17) 0.4464(17) 0.0000 0.084(8) Uani 0.5 2 d DS TU P F 1
H7SA H 0.4276 0.3985 0.0232 0.100 Uiso 0.25 1 calc R . . F 1
H7SB H 0.3985 0.4276 -0.0232 0.100 Uiso 0.25 1 calc R . . F 1
O3S O 1.0000 1.0000 0.5000 0.21(5) Uiso 0.3334 6 d S T P . .
O7S O 0.454(3) 0.483(4) 0.0278(14) 0.136(13) Uiso 0.3333 1 d . . . G 2
O6S O 1.0000 1.0000 0.027(4) 0.25(5) Uiso 0.3333 3 d S T P . .
O4S O 0.9104(12) 0.8307(10) 0.2875(5) 0.168(5) Uiso 1 1 d . . . H 2
C1 C 0.4026(13) 0.4273(13) 0.3581(6) 0.078(5) Uani 0.654(6) 1 d . . . A 1
H1B H 0.4007 0.3914 0.3315 0.116 Uiso 0.654(6) 1 calc GR . . A 1
H1C H 0.3647 0.4523 0.3519 0.116 Uiso 0.654(6) 1 calc GR . . A 1
H1D H 0.3818 0.3905 0.3861 0.116 Uiso 0.654(6) 1 calc GR . . A 1
O5S O 0.3333 0.6667 0.288(2) 0.105(19) Uiso 0.25 3 d S T P . .
C2 C 1.059(3) 1.022(3) 0.3257(15) 0.097(12) Uiso 0.3333 1 d . . . . .
Cl1S Cl 1.027(11) 0.985(12) 0.3671(18) 0.44(4) Uiso 0.3333 1 d . . . B .
O10S O 0.3333 0.6667 0.388(4) 0.17(4) Uiso 0.25 3 d S T 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
N4A 0.036(4) 0.054(6) 0.084(6) 0.003(4) 0.011(4) 0.016(4)
N3A 0.058(5) 0.029(4) 0.069(6) 0.001(4) 0.012(4) 0.016(4)
N1A 0.051(5) 0.044(5) 0.056(4) -0.002(4) -0.007(4) 0.018(4)
N2A 0.062(5) 0.034(4) 0.079(5) 0.007(4) 0.011(4) 0.016(4)
C1A 0.053(6) 0.054(7) 0.077(6) 0.003(5) -0.003(5) 0.033(5)
C2A 0.054(6) 0.045(6) 0.072(6) 0.004(5) 0.000(5) 0.028(5)
C3A 0.038(5) 0.046(5) 0.064(6) -0.002(4) -0.009(4) 0.014(5)
C4A 0.045(5) 0.050(6) 0.082(6) 0.001(5) -0.016(4) 0.015(4)
C5A 0.090(7) 0.060(7) 0.094(6) -0.011(5) -0.037(6) 0.026(6)
C6A 0.087(8) 0.083(9) 0.167(11) -0.003(8) -0.057(7) 0.021(7)
C7A 0.059(8) 0.104(12) 0.183(11) 0.002(9) -0.039(7) 0.005(7)
C8A 0.046(6) 0.082(8) 0.169(10) 0.012(8) -0.005(6) 0.018(6)
C9A 0.048(5) 0.049(5) 0.090(6) 0.010(5) -0.007(4) 0.025(4)
C10A 0.055(6) 0.054(7) 0.083(7) 0.018(6) 0.026(6) 0.021(5)
C11A 0.064(6) 0.044(6) 0.077(7) 0.001(5) 0.008(5) 0.032(5)
C16A 0.068(7) 0.042(5) 0.066(6) 0.008(5) 0.023(5) 0.030(5)
C15A 0.080(7) 0.043(6) 0.071(7) 0.004(5) 0.027(6) 0.033(6)
C14A 0.070(7) 0.053(6) 0.070(6) 0.006(5) 0.018(5) 0.032(5)
C13A 0.068(6) 0.036(5) 0.070(6) 0.001(5) 0.021(5) 0.024(5)
C12A 0.059(6) 0.051(6) 0.067(6) 0.005(5) 0.012(5) 0.028(5)
C17A 0.068(7) 0.044(6) 0.057(6) 0.005(5) 0.011(5) 0.024(5)
C18A 0.061(6) 0.033(5) 0.061(5) -0.003(4) -0.002(4) 0.028(5)
C19A 0.052(6) 0.045(6) 0.087(7) 0.010(5) 0.023(5) 0.021(5)
C20A 0.071(7) 0.052(6) 0.078(7) 0.012(5) 0.023(6) 0.026(5)
C21A 0.063(7) 0.041(5) 0.079(7) 0.008(5) 0.005(5) 0.023(5)
C22A 0.047(6) 0.055(6) 0.091(7) 0.017(5) 0.002(5) 0.023(5)
C23A 0.045(5) 0.042(5) 0.061(5) -0.007(4) -0.003(4) 0.020(4)
C24A 0.056(6) 0.061(7) 0.059(6) 0.003(5) -0.010(5) 0.020(6)
N3B 0.089(9) 0.050(7) 0.083(7) -0.012(5) -0.003(6) 0.048(7)
N2B 0.070(8) 0.082(8) 0.069(7) 0.002(6) -0.017(6) 0.042(7)
N4B 0.052(7) 0.062(6) 0.049(6) -0.008(5) 0.003(5) 0.028(6)
N1B 0.071(8) 0.098(10) 0.058(7) -0.013(6) -0.010(6) 0.037(8)
C1B 0.075(8) 0.063(8) 0.082(7) -0.004(6) -0.010(6) 0.041(6)
C6B 0.072(8) 0.062(8) 0.067(7) 0.005(6) -0.002(6) 0.034(6)
C5B 0.077(8) 0.077(8) 0.065(7) 0.001(6) -0.008(6) 0.047(6)
C4B 0.074(8) 0.100(10) 0.060(7) 0.004(7) -0.010(6) 0.049(7)
C3B 0.068(9) 0.100(10) 0.077(8) 0.002(7) -0.013(7) 0.047(8)
C2B 0.078(9) 0.070(9) 0.082(8) 0.013(6) 0.002(6) 0.044(8)
C7B 0.084(10) 0.060(9) 0.079(7) 0.001(6) -0.008(6) 0.044(8)
C8B 0.086(9) 0.080(9) 0.079(8) 0.002(7) -0.014(7) 0.052(7)
C9B 0.065(7) 0.066(9) 0.042(7) -0.009(7) -0.001(6) 0.037(7)
C10B 0.060(7) 0.070(9) 0.037(7) -0.014(6) 0.001(6) 0.036(7)
C11B 0.064(8) 0.065(8) 0.042(8) -0.007(6) 0.005(6) 0.035(7)
C12B 0.055(9) 0.090(10) 0.092(8) -0.031(7) -0.018(7) 0.045(8)
C13B 0.17(2) 0.095(13) 0.088(9) -0.024(7) -0.008(8) 0.091(14)
C14B 0.080(10) 0.095(10) 0.068(10) -0.010(8) -0.002(8) 0.037(8)
C15B 0.085(10) 0.109(11) 0.061(10) -0.017(7) -0.010(8) 0.046(8)
C16B 0.072(9) 0.081(12) 0.067(10) -0.024(9) -0.013(8) 0.030(9)
C17B 0.085(10) 0.100(11) 0.074(10) -0.011(8) -0.018(8) 0.043(8)
C18B 0.115(13) 0.110(14) 0.063(8) -0.019(8) 0.006(9) 0.055(11)
C19B 0.072(11) 0.095(12) 0.090(9) -0.026(8) 0.004(8) 0.035(10)
Cl5S 0.188(10) 0.096(6) 0.123(6) 0.014(5) -0.027(6) 0.073(6)
C7S 0.079(14) 0.079(14) 0.076(18) 0.029(7) -0.029(7) 0.026(15)
C1 0.081(13) 0.069(11) 0.068(10) 0.017(9) 0.003(9) 0.026(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
N4A C23A 1.463(12) . ?
N4A C24A 1.272(13) . ?
N3A C17A 1.243(13) . ?
N3A C18A 1.451(12) . ?
N1A C3A 1.309(12) . ?
N1A C4A 1.452(12) . ?
N2A C9A 1.507(13) . ?
N2A C10A 1.239(13) . ?
C1A H1A 0.9500 . ?
C1A C2A 1.398(14) 3_675 ?
C1A C2A 1.375(14) . ?
C2A C1A 1.398(14) 2_765 ?
C2A C3A 1.468(14) . ?
C3A H3A 0.9500 . ?
C4A H4A 1.0000 . ?
C4A C5A 1.528(15) . ?
C4A C9A 1.529(15) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C5A C6A 1.539(19) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A C7A 1.48(2) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C7A C8A 1.51(2) . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C8A C9A 1.528(15) . ?
C9A H9A 1.0000 . ?
C10A H10A 0.9500 . ?
C10A C11A 1.509(13) . ?
C11A C16A 1.3900 . ?
C11A C12A 1.3900 . ?
C16A H16A 0.9500 . ?
C16A C15A 1.3900 . ?
C15A C14A 1.3900 . ?
C15A C24A 1.491(11) 3_675 ?
C14A H14A 0.9500 . ?
C14A C13A 1.3900 . ?
C13A C12A 1.3900 . ?
C13A C17A 1.488(11) . ?
C12A H12A 0.9500 . ?
C17A H17A 0.9500 . ?
C18A H18A 1.0000 . ?
C18A C19A 1.550(14) . ?
C18A C23A 1.534(13) . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C19A C20A 1.505(16) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C20A C21A 1.540(16) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C21A C22A 1.533(15) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C22A C23A 1.495(14) . ?
C23A H23A 1.0000 . ?
C24A C15A 1.49(2) 2_765 ?
C24A H24A 0.9500 . ?
O2S C1S 1.46(2) . ?
O2S C2S 1.42(2) . ?
O1S C3S 1.38(2) . ?
O1S C4S 1.816(15) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S C4S 1.532(19) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C2S C3S 1.42(3) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
N3C C7C 1.266(18) . ?
N3C C13C 1.478(15) . ?
N1C C12C 1.18(5) . ?
N1C C16C 1.48(2) . ?
N4C C9C 1.241(19) . ?
N4C C14C 1.479(19) . ?
N2C C8C 1.227(19) . ?
N2C C15C 1.47(2) . ?
C4C C3C 1.3900 . ?
C4C C5C 1.3900 . ?
C4C C8C 1.450(18) . ?
C3C H3C 0.9500 . ?
C3C C2C 1.3900 . ?
C2C C4S 1.3900 . ?
C2C C7C 1.49(2) . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
C4S H4S 0.9500 . ?
C4S C6C 1.3900 . ?
C6C C5C 1.3900 . ?
C6C C9C 1.495(19) . ?
C5C H5C 0.9500 . ?
C7C H7C 0.9500 . ?
C8C H8C 0.9500 . ?
C9C H9C 0.9500 . ?
C10C H10C 0.9500 . ?
C10C C11C 1.394(17) . ?
C10C C11C 1.387(17) 2_655 ?
C11C C10C 1.387(17) 3_665 ?
C11C C12C 1.56(5) . ?
C12C H12C 0.9500 . ?
C13C H13C 0.9500 . ?
C13C C14C 1.54(2) 2_655 ?
C14C C13C 1.54(2) 3_665 ?
C14C H14B 0.9900 . ?
C14C H14C 0.9900 . ?
C15C H15A 0.9900 . ?
C15C H15B 0.9900 . ?
C15C C16C 1.56(2) . ?
C16C C17C 1.38(7) . ?
C17C H17B 0.9800 . ?
C17C H17C 0.9800 . ?
C17C H17D 0.9800 . ?
N3B C7B 1.27(2) . ?
N3B C13B 1.55(3) . ?
N2B C8B 1.28(2) . ?
N2B C14B 1.37(3) . ?
N4B C11B 1.274(19) . ?
N4B C12B 1.47(2) . ?
N1B C15B 1.52(3) . ?
N1B C16B 1.24(2) . ?
C1B C6B 1.3900 . ?
C1B C2B 1.3900 . ?
C1B C7B 1.454(19) . ?
C6B H6B 0.9500 . ?
C6B C5B 1.3900 . ?
C5B C4B 1.3900 . ?
C5B C8B 1.51(2) . ?
C4B H4B 0.9500 . ?
C4B C3B 1.3900 . ?
C3B C2B 1.3900 . ?
C3B C16B 1.52(2) 3_665 ?
C2B H2B 0.9500 . ?
C7B H7B 0.9500 . ?
C8B H8B 0.9500 . ?
C9B H9B 0.9500 . ?
C9B C10B 1.39(2) . ?
C9B C10B 1.39(2) 3_665 ?
C10B C9B 1.39(2) 2_655 ?
C10B C11B 1.46(2) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.44(3) . ?
C12B C19B 1.47(3) . ?
C12B C1 1.49(3) . ?
C13B H13A 0.9900 . ?
C13B H13B 0.9900 . ?
C14B H14D 0.9900 . ?
C14B H14E 0.9900 . ?
C14B C15B 1.54(3) . ?
C15B C17B 1.48(3) . ?
C15B C18B 1.55(3) . ?
C16B C3B 1.52(5) 2_655 ?
C16B H16B 0.9500 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C17B H17G 0.9800 . ?
C18B H18B 0.9800 . ?
C18B H18C 0.9800 . ?
C18B H18D 0.9800 . ?
C19B H19C 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
Cl2S Cl2S 0.00(3) 2_765 ?
Cl2S Cl2S 0.00(3) 3_675 ?
Cl2S C2 1.44(4) 3_675 ?
Cl2S C2 1.44(4) 2_765 ?
Cl2S C2 1.44(4) . ?
Cl2S Cl1S 2.40(6) . ?
Cl4S Cl4S 1.53(3) 2_655 ?
Cl4S Cl4S 1.53(3) 3_665 ?
Cl4S C5S 1.72(3) . ?
Cl4S C5S 1.29(4) 3_665 ?
Cl4S C5S 2.03(6) 2_655 ?
Cl3S Cl3S 0.749(18) 3_665 ?
Cl3S Cl3S 0.749(18) 2_655 ?
Cl3S C5S 1.41(3) 3_665 ?
Cl3S C5S 1.76(3) . ?
Cl3S C5S 1.71(4) 2_655 ?
C5S Cl4S 2.03(6) 3_665 ?
C5S Cl3S 1.41(3) 2_655 ?
C5S Cl3S 1.71(4) 3_665 ?
C5S C5S 1.39(8) 3_665 ?
O9S O9S 1.50(14) 2_665 ?
O9S O9S 1.50(14) 3_565 ?
Cl5S C7S 1.801(18) . ?
C7S Cl5S 1.801(18) 4 ?
C7S H7SA 0.9900 . ?
C7S H7SB 0.9900 . ?
O6S O6S 1.6(2) 4 ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 Cl2S 1.44(4) 3_675 ?
C2 Cl2S 1.44(4) 2_765 ?
C2 Cl1S 1.34(11) . ?
Cl1S C2 1.54(13) 3_675 ?
Cl1S C2 1.94(7) 2_765 ?
Cl1S Cl1S 1.13(14) 3_675 ?
Cl1S Cl1S 1.13(14) 2_765 ?
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
C24A N4A C23A 114.8(9) . . ?
C17A N3A C18A 118.5(8) . . ?
C3A N1A C4A 116.4(8) . . ?
C10A N2A C9A 116.6(9) . . ?
C2A C1A H1A 119.9 3_675 . ?
C2A C1A H1A 119.9 . . ?
C2A C1A C2A 120.2(10) . 3_675 ?
C1A C2A C1A 119.7(10) . 2_765 ?
C1A C2A C3A 121.7(9) . . ?
C1A C2A C3A 118.6(9) 2_765 . ?
N1A C3A C2A 120.7(8) . . ?
N1A C3A H3A 119.7 . . ?
C2A C3A H3A 119.7 . . ?
N1A C4A H4A 109.8 . . ?
N1A C4A C5A 108.4(8) . . ?
N1A C4A C9A 108.5(8) . . ?
C5A C4A H4A 109.8 . . ?
C5A C4A C9A 110.5(9) . . ?
C9A C4A H4A 109.8 . . ?
C4A C5A H5AA 109.3 . . ?
C4A C5A H5AB 109.3 . . ?
C4A C5A C6A 111.5(11) . . ?
H5AA C5A H5AB 108.0 . . ?
C6A C5A H5AA 109.3 . . ?
C6A C5A H5AB 109.3 . . ?
C5A C6A H6AA 109.7 . . ?
C5A C6A H6AB 109.7 . . ?
H6AA C6A H6AB 108.2 . . ?
C7A C6A C5A 110.0(13) . . ?
C7A C6A H6AA 109.7 . . ?
C7A C6A H6AB 109.7 . . ?
C6A C7A H7AA 109.1 . . ?
C6A C7A H7AB 109.1 . . ?
C6A C7A C8A 112.7(15) . . ?
H7AA C7A H7AB 107.8 . . ?
C8A C7A H7AA 109.1 . . ?
C8A C7A H7AB 109.1 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A C9A 110.7(11) . . ?
H8AA C8A H8AB 108.1 . . ?
C9A C8A H8AA 109.5 . . ?
C9A C8A H8AB 109.5 . . ?
N2A C9A C4A 107.7(8) . . ?
N2A C9A C8A 111.1(9) . . ?
N2A C9A H9A 109.1 . . ?
C4A C9A H9A 109.1 . . ?
C8A C9A C4A 110.7(10) . . ?
C8A C9A H9A 109.1 . . ?
N2A C10A H10A 118.8 . . ?
N2A C10A C11A 122.4(9) . . ?
C11A C10A H10A 118.8 . . ?
C16A C11A C10A 119.2(6) . . ?
C16A C11A C12A 120.0 . . ?
C12A C11A C10A 120.8(6) . . ?
C11A C16A H16A 120.0 . . ?
C11A C16A C15A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
C16A C15A C14A 120.0 . . ?
C16A C15A C24A 121.2(6) . 3_675 ?
C14A C15A C24A 118.8(6) . 3_675 ?
C15A C14A H14A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C14A C13A C17A 121.4(6) . . ?
C12A C13A C14A 120.0 . . ?
C12A C13A C17A 118.6(6) . . ?
C11A C12A H12A 120.0 . . ?
C13A C12A C11A 120.0 . . ?
C13A C12A H12A 120.0 . . ?
N3A C17A C13A 121.6(9) . . ?
N3A C17A H17A 119.2 . . ?
C13A C17A H17A 119.2 . . ?
N3A C18A H18A 109.5 . . ?
N3A C18A C19A 109.4(7) . . ?
N3A C18A C23A 109.3(8) . . ?
C19A C18A H18A 109.5 . . ?
C23A C18A H18A 109.5 . . ?
C23A C18A C19A 109.6(8) . . ?
C18A C19A H19A 109.2 . . ?
C18A C19A H19B 109.2 . . ?
H19A C19A H19B 107.9 . . ?
C20A C19A C18A 112.0(8) . . ?
C20A C19A H19A 109.2 . . ?
C20A C19A H19B 109.2 . . ?
C19A C20A H20A 109.6 . . ?
C19A C20A H20B 109.6 . . ?
C19A C20A C21A 110.1(9) . . ?
H20A C20A H20B 108.1 . . ?
C21A C20A H20A 109.6 . . ?
C21A C20A H20B 109.6 . . ?
C20A C21A H21A 110.3 . . ?
C20A C21A H21B 110.3 . . ?
H21A C21A H21B 108.5 . . ?
C22A C21A C20A 107.2(9) . . ?
C22A C21A H21A 110.3 . . ?
C22A C21A H21B 110.3 . . ?
C21A C22A H22A 109.1 . . ?
C21A C22A H22B 109.1 . . ?
H22A C22A H22B 107.9 . . ?
C23A C22A C21A 112.4(9) . . ?
C23A C22A H22A 109.1 . . ?
C23A C22A H22B 109.1 . . ?
N4A C23A C18A 108.0(7) . . ?
N4A C23A C22A 109.5(8) . . ?
N4A C23A H23A 109.7 . . ?
C18A C23A H23A 109.7 . . ?
C22A C23A C18A 110.3(8) . . ?
C22A C23A H23A 109.7 . . ?
N4A C24A C15A 122.1(10) . 2_765 ?
N4A C24A H24A 118.9 . . ?
C15A C24A H24A 118.9 2_765 . ?
C2S O2S C1S 109.6(13) . . ?
C3S O1S C4S 109.0(12) . . ?
O2S C1S H1SA 108.1 . . ?
O2S C1S H1SB 108.1 . . ?
O2S C1S C4S 116.8(13) . . ?
H1SA C1S H1SB 107.3 . . ?
C4S C1S H1SA 108.1 . . ?
C4S C1S H1SB 108.1 . . ?
O2S C2S H2SA 109.8 . . ?
O2S C2S H2SB 109.8 . . ?
O2S C2S C3S 109.2(15) . . ?
H2SA C2S H2SB 108.3 . . ?
C3S C2S H2SA 109.8 . . ?
C3S C2S H2SB 109.8 . . ?
O1S C3S C2S 113.7(17) . . ?
O1S C3S H3SA 108.8 . . ?
O1S C3S H3SB 108.8 . . ?
C2S C3S H3SA 108.8 . . ?
C2S C3S H3SB 108.8 . . ?
H3SA C3S H3SB 107.7 . . ?
C7C N3C C13C 115(3) . . ?
C12C N1C C16C 120(4) . . ?
C9C N4C C14C 132(2) . . ?
C8C N2C C15C 119(3) . . ?
C3C C4C C5C 120.0 . . ?
C3C C4C C8C 121.6(10) . . ?
C5C C4C C8C 118.4(10) . . ?
C4C C3C H3C 120.0 . . ?
C4C C3C C2C 120.0 . . ?
C2C C3C H3C 120.0 . . ?
C3C C2C C7C 122.5(9) . . ?
C4S C2C C3C 120.0 . . ?
C4S C2C C7C 117.5(9) . . ?
O1S C4S H4SA 113.0 . . ?
O1S C4S H4SB 113.0 . . ?
C1S C4S O1S 93.8(9) . . ?
C1S C4S H4SA 113.0 . . ?
C1S C4S H4SB 113.0 . . ?
C2C C4S H4S 120.0 . . ?
H4SA C4S H4SB 110.4 . . ?
C6C C4S C2C 120.0 . . ?
C6C C4S H4S 120.0 . . ?
C4S C6C C5C 120.0 . . ?
C4S C6C C9C 120.1(9) . . ?
C5C C6C C9C 119.9(9) . . ?
C4C C5C H5C 120.0 . . ?
C6C C5C C4C 120.0 . . ?
C6C C5C H5C 120.0 . . ?
N3C C7C C2C 125(2) . . ?
N3C C7C H7C 117.5 . . ?
C2C C7C H7C 117.5 . . ?
N2C C8C C4C 118.5(19) . . ?
N2C C8C H8C 120.7 . . ?
C4C C8C H8C 120.7 . . ?
N4C C9C C6C 125.2(19) . . ?
N4C C9C H9C 117.4 . . ?
C6C C9C H9C 117.4 . . ?
C11C C10C H10C 119.8 2_655 . ?
C11C C10C H10C 119.8 . . ?
C11C C10C C11C 120.4(14) 2_655 . ?
C10C C11C C10C 119.4(14) 3_665 . ?
C10C C11C C12C 122(3) . . ?
C10C C11C C12C 118(3) 3_665 . ?
N1C C12C C11C 124(4) . . ?
N1C C12C H12C 117.8 . . ?
C11C C12C H12C 117.8 . . ?
N3C C13C H13C 127.0 . . ?
N3C C13C C14C 106.1(19) . 2_655 ?
C14C C13C H13C 127.0 2_655 . ?
N4C C14C C13C 104.8(19) . 3_665 ?
N4C C14C H14B 110.8 . . ?
N4C C14C H14C 110.8 . . ?
C13C C14C H14B 110.8 3_665 . ?
C13C C14C H14C 110.8 3_665 . ?
H14B C14C H14C 108.9 . . ?
N2C C15C H15A 111.3 . . ?
N2C C15C H15B 111.3 . . ?
N2C C15C C16C 102(3) . . ?
H15A C15C H15B 109.2 . . ?
C16C C15C H15A 111.3 . . ?
C16C C15C H15B 111.3 . . ?
N1C C16C C15C 112(3) . . ?
C17C C16C N1C 126(4) . . ?
C17C C16C C15C 110(4) . . ?
C16C C17C H17B 109.5 . . ?
C16C C17C H17C 109.5 . . ?
C16C C17C H17D 109.5 . . ?
H17B C17C H17C 109.5 . . ?
H17B C17C H17D 109.5 . . ?
H17C C17C H17D 109.5 . . ?
C7B N3B C13B 122.8(17) . . ?
C8B N2B C14B 114.7(17) . . ?
C11B N4B C12B 122.0(14) . . ?
C16B N1B C15B 124.1(17) . . ?
C6B C1B C2B 120.0 . . ?
C6B C1B C7B 121.8(10) . . ?
C2B C1B C7B 118.2(10) . . ?
C1B C6B H6B 120.0 . . ?
C1B C6B C5B 120.0 . . ?
C5B C6B H6B 120.0 . . ?
C6B C5B C8B 117.2(10) . . ?
C4B C5B C6B 120.0 . . ?
C4B C5B C8B 122.7(10) . . ?
C5B C4B H4B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C4B C3B C2B 120.0 . . ?
C4B C3B C16B 117.8(10) . 3_665 ?
C2B C3B C16B 122.2(10) . 3_665 ?
C1B C2B H2B 120.0 . . ?
C3B C2B C1B 120.0 . . ?
C3B C2B H2B 120.0 . . ?
N3B C7B C1B 120.5(15) . . ?
N3B C7B H7B 119.7 . . ?
C1B C7B H7B 119.7 . . ?
N2B C8B C5B 119.9(17) . . ?
N2B C8B H8B 120.1 . . ?
C5B C8B H8B 120.1 . . ?
C10B C9B H9B 119.4 . . ?
C10B C9B H9B 119.4 3_665 . ?
C10B C9B C10B 121.1(16) . 3_665 ?
C9B C10B C9B 118.9(16) . 2_655 ?
C9B C10B C11B 118.9(14) 2_655 . ?
C9B C10B C11B 122.3(14) . . ?
N4B C11B C10B 123.7(15) . . ?
N4B C11B H11B 118.1 . . ?
C10B C11B H11B 118.1 . . ?
N4B C12B C19B 109.1(15) . . ?
N4B C12B C1 115.1(16) . . ?
C13B C12B N4B 107.7(17) . . ?
C13B C12B C19B 103.5(18) . . ?
C13B C12B C1 104.3(19) . . ?
C19B C12B C1 116.0(16) . . ?
N3B C13B H13A 108.5 . . ?
N3B C13B H13B 108.5 . . ?
C12B C13B N3B 115.2(17) . . ?
C12B C13B H13A 108.5 . . ?
C12B C13B H13B 108.5 . . ?
H13A C13B H13B 107.5 . . ?
N2B C14B H14D 108.2 . . ?
N2B C14B H14E 108.2 . . ?
N2B C14B C15B 116(2) . . ?
H14D C14B H14E 107.3 . . ?
C15B C14B H14D 108.2 . . ?
C15B C14B H14E 108.2 . . ?
N1B C15B C14B 108.9(16) . . ?
N1B C15B C18B 110(2) . . ?
C14B C15B C18B 106(2) . . ?
C17B C15B N1B 109(2) . . ?
C17B C15B C14B 115(2) . . ?
C17B C15B C18B 107.0(17) . . ?
N1B C16B C3B 123(2) . 2_655 ?
N1B C16B H16B 118.6 . . ?
C3B C16B H16B 118.6 2_655 . ?
C15B C17B H17E 109.5 . . ?
C15B C17B H17F 109.5 . . ?
C15B C17B H17G 109.5 . . ?
H17E C17B H17F 109.5 . . ?
H17E C17B H17G 109.5 . . ?
H17F C17B H17G 109.5 . . ?
C15B C18B H18B 109.5 . . ?
C15B C18B H18C 109.5 . . ?
C15B C18B H18D 109.5 . . ?
H18B C18B H18C 109.5 . . ?
H18B C18B H18D 109.5 . . ?
H18C C18B H18D 109.5 . . ?
C12B C19B H19C 109.5 . . ?
C12B C19B H19D 109.5 . . ?
C12B C19B H19E 109.5 . . ?
H19C C19B H19D 109.5 . . ?
H19C C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
Cl2S Cl2S Cl2S 0(10) 2_765 3_675 ?
Cl2S Cl2S C2 0(10) 2_765 3_675 ?
Cl2S Cl2S C2 0(10) 3_675 2_765 ?
Cl2S Cl2S C2 0(10) 3_675 . ?
Cl2S Cl2S C2 0(10) 3_675 3_675 ?
Cl2S Cl2S C2 0(10) 2_765 2_765 ?
Cl2S Cl2S C2 0(10) 2_765 . ?
Cl2S Cl2S Cl1S 0(10) 2_765 . ?
Cl2S Cl2S Cl1S 0(10) 3_675 . ?
C2 Cl2S C2 65(3) . 3_675 ?
C2 Cl2S C2 65(3) 2_765 3_675 ?
C2 Cl2S C2 65(3) . 2_765 ?
C2 Cl2S Cl1S 29(5) . . ?
C2 Cl2S Cl1S 38(5) 3_675 . ?
C2 Cl2S Cl1S 54(3) 2_765 . ?
Cl4S Cl4S Cl4S 59.999(3) 2_655 3_665 ?
Cl4S Cl4S C5S 77(3) 3_665 . ?
Cl4S Cl4S C5S 39.5(9) 3_665 2_655 ?
Cl4S Cl4S C5S 55.7(17) 2_655 2_655 ?
Cl4S Cl4S C5S 46.2(18) 2_655 . ?
C5S Cl4S Cl4S 75(2) 3_665 3_665 ?
C5S Cl4S Cl4S 91(2) 3_665 2_655 ?
C5S Cl4S C5S 42.4(19) . 2_655 ?
C5S Cl4S C5S 42(2) 3_665 2_655 ?
C5S Cl4S C5S 52(3) 3_665 . ?
Cl3S Cl3S Cl3S 60.006(8) 3_665 2_655 ?
Cl3S Cl3S C5S 105.2(16) 3_665 3_665 ?
Cl3S Cl3S C5S 74(2) 3_665 . ?
Cl3S Cl3S C5S 81(2) 2_655 2_655 ?
Cl3S Cl3S C5S 100(3) 2_655 3_665 ?
Cl3S Cl3S C5S 54(2) 3_665 2_655 ?
Cl3S Cl3S C5S 50.5(13) 2_655 . ?
C5S Cl3S C5S 50(3) 3_665 . ?
C5S Cl3S C5S 52(3) 3_665 2_655 ?
C5S Cl3S C5S 47(3) 2_655 . ?
Cl4S C5S Cl4S 47.4(15) . 3_665 ?
Cl4S C5S Cl3S 98.9(17) . . ?
Cl3S C5S Cl4S 92(2) . 3_665 ?
Cl3S C5S Cl4S 113(3) 2_655 3_665 ?
Cl3S C5S Cl4S 90(3) 3_665 3_665 ?
Cl3S C5S Cl4S 122(2) 2_655 . ?
Cl3S C5S Cl4S 114(2) 3_665 . ?
Cl3S C5S Cl3S 25.6(10) 2_655 3_665 ?
Cl3S C5S Cl3S 24.9(7) 3_665 . ?
Cl3S C5S Cl3S 24.3(8) 2_655 . ?
C5S C5S Cl4S 57(2) 3_665 3_665 ?
C5S C5S Cl4S 47.6(17) 3_665 . ?
C5S C5S Cl3S 68(2) 3_665 3_665 ?
C5S C5S Cl3S 51.5(13) 3_665 . ?
C5S C5S Cl3S 75.4(15) 3_665 2_655 ?
O9S O9S O9S 59.999(10) 2_665 3_565 ?
Cl5S C7S Cl5S 114.4(18) 4 . ?
Cl5S C7S H7SA 108.7 . . ?
Cl5S C7S H7SA 108.7 4 . ?
Cl5S C7S H7SB 108.7 4 . ?
Cl5S C7S H7SB 108.7 . . ?
H7SA C7S H7SB 107.6 . . ?
C12B C1 H1B 109.5 . . ?
C12B C1 H1C 109.5 . . ?
C12B C1 H1D 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
Cl2S C2 Cl2S 0.000(1) 3_675 2_765 ?
Cl2S C2 Cl2S 0.000(1) . 2_765 ?
Cl2S C2 Cl2S 0.000(1) 3_675 . ?
Cl1S C2 Cl2S 120(8) . 2_765 ?
Cl1S C2 Cl2S 120(8) . 3_675 ?
Cl1S C2 Cl2S 120(8) . . ?
C2 Cl1S Cl2S 35(2) 3_675 . ?
C2 Cl1S Cl2S 31(4) . . ?
C2 Cl1S Cl2S 36.8(16) 2_765 . ?
C2 Cl1S C2 53(4) . 2_765 ?
C2 Cl1S C2 52(3) 3_675 2_765 ?
C2 Cl1S C2 65(5) . 3_675 ?
Cl1S Cl1S Cl2S 76.4(16) 2_765 . ?
Cl1S Cl1S Cl2S 76.4(16) 3_675 . ?
Cl1S Cl1S C2 103(5) 3_675 . ?
Cl1S Cl1S C2 92(9) 2_765 3_675 ?
Cl1S Cl1S C2 58(10) 3_675 3_675 ?
Cl1S Cl1S C2 77(10) 2_765 . ?
Cl1S Cl1S C2 42(4) 2_765 2_765 ?
Cl1S Cl1S C2 53(7) 3_675 2_765 ?
Cl1S Cl1S Cl1S 60.00(3) 3_675 2_765 ?
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
N3A C18A C19A C20A -175.0(9) . . . . ?
N3A C18A C23A N4A -66.1(9) . . . . ?
N3A C18A C23A C22A 174.3(8) . . . . ?
N1A C4A C5A C6A -174.1(12) . . . . ?
N1A C4A C9A N2A -64.3(10) . . . . ?
N1A C4A C9A C8A 174.0(9) . . . . ?
N2A C10A C11A C16A -177.0(8) . . . . ?
N2A C10A C11A C12A 0.6(12) . . . . ?
C1A C2A C3A N1A 2.9(15) . . . . ?
C1A C2A C3A N1A -178.0(9) 2_765 . . . ?
C2A C1A C2A C1A 2(2) 3_675 . . 2_765 ?
C2A C1A C2A C3A -179.1(6) 3_675 . . . ?
C3A N1A C4A C5A -114.6(10) . . . . ?
C3A N1A C4A C9A 125.3(9) . . . . ?
C4A N1A C3A C2A 176.4(8) . . . . ?
C4A C5A C6A C7A 55.6(18) . . . . ?
C5A C4A C9A N2A 176.9(8) . . . . ?
C5A C4A C9A C8A 55.2(12) . . . . ?
C5A C6A C7A C8A -56.8(19) . . . . ?
C6A C7A C8A C9A 58(2) . . . . ?
C7A C8A C9A N2A -175.5(13) . . . . ?
C7A C8A C9A C4A -55.8(16) . . . . ?
C9A N2A C10A C11A 178.6(8) . . . . ?
C9A C4A C5A C6A -55.3(15) . . . . ?
C10A N2A C9A C4A 123.5(9) . . . . ?
C10A N2A C9A C8A -115.1(12) . . . . ?
C10A C11A C16A C15A 177.6(7) . . . . ?
C10A C11A C12A C13A -177.6(7) . . . . ?
C11A C16A C15A C14A 0.0 . . . . ?
C11A C16A C15A C24A -178.8(8) . . . 3_675 ?
C16A C11A C12A C13A 0.0 . . . . ?
C16A C15A C14A C13A 0.0 . . . . ?
C15A C14A C13A C12A 0.0 . . . . ?
C15A C14A C13A C17A -177.6(7) . . . . ?
C14A C13A C12A C11A 0.0 . . . . ?
C14A C13A C17A N3A 5.6(12) . . . . ?
C12A C11A C16A C15A 0.0 . . . . ?
C12A C13A C17A N3A -172.0(7) . . . . ?
C17A N3A C18A C19A -118.4(10) . . . . ?
C17A N3A C18A C23A 121.7(10) . . . . ?
C17A C13A C12A C11A 177.6(7) . . . . ?
C18A N3A C17A C13A 177.3(8) . . . . ?
C18A C19A C20A C21A 58.6(12) . . . . ?
C19A C18A C23A N4A 174.1(7) . . . . ?
C19A C18A C23A C22A 54.5(10) . . . . ?
C19A C20A C21A C22A -59.2(11) . . . . ?
C20A C21A C22A C23A 60.8(11) . . . . ?
C21A C22A C23A N4A -178.3(8) . . . . ?
C21A C22A C23A C18A -59.6(11) . . . . ?
C23A N4A C24A C15A 176.0(13) . . . 2_765 ?
C23A C18A C19A C20A -55.2(11) . . . . ?
C24A N4A C23A C18A 110.9(9) . . . . ?
C24A N4A C23A C22A -129.0(9) . . . . ?
C24A C15A C14A C13A 178.8(7) 3_675 . . . ?
O2S C1S C4S O1S 59.5(14) . . . . ?
O2S C2S C3S O1S -65(2) . . . . ?
C1S O2S C2S C3S 59.3(18) . . . . ?
C2S O2S C1S C4S -68.1(17) . . . . ?
C3S O1S C4S C1S -56.8(13) . . . . ?
N2C C15C C16C N1C -66(5) . . . . ?
N2C C15C C16C C17C 79(4) . . . . ?
C4C C3C C2C C4S 0.0 . . . . ?
C4C C3C C2C C7C 180.0 . . . . ?
C3C C4C C5C C6C 0.0 . . . . ?
C3C C4C C8C N2C 0.00(5) . . . . ?
C3C C2C C4S C6C 0.0 . . . . ?
C3C C2C C7C N3C 180.00(3) . . . . ?
C2C C4S C6C C5C 0.0 . . . . ?
C2C C4S C6C C9C 180.0 . . . . ?
C4S O1S C3S C2S 64.7(18) . . . . ?
C4S C2C C7C N3C 0.00(5) . . . . ?
C4S C6C C5C C4C 0.0 . . . . ?
C4S C6C C9C N4C 180.00(3) . . . . ?
C5C C4C C3C C2C 0.0 . . . . ?
C5C C4C C8C N2C 180.00(3) . . . . ?
C5C C6C C9C N4C 0.00(5) . . . . ?
C7C N3C C13C C14C 143(2) . . . 2_655 ?
C7C C2C C4S C6C 180.0 . . . . ?
C8C N2C C15C C16C 137(2) . . . . ?
C8C C4C C3C C2C 180.0 . . . . ?
C8C C4C C5C C6C 180.0 . . . . ?
C9C N4C C14C C13C 130.9(18) . . . 3_665 ?
C9C C6C C5C C4C 180.0 . . . . ?
C10C C11C C12C N1C 15(7) 3_665 . . . ?
C10C C11C C12C N1C -171(4) . . . . ?
C11C C10C C11C C10C -6(9) 2_655 . . 3_665 ?
C11C C10C C11C C12C 180(3) 2_655 . . . ?
C12C N1C C16C C15C 120(4) . . . . ?
C12C N1C C16C C17C -18(7) . . . . ?
C13C N3C C7C C2C -176.8(18) . . . . ?
C14C N4C C9C C6C -175.5(17) . . . . ?
C15C N2C C8C C4C 170.2(19) . . . . ?
C16C N1C C12C C11C -179(4) . . . . ?
N2B C14B C15B N1B 62(3) . . . . ?
N2B C14B C15B C17B -175.6(19) . . . . ?
N2B C14B C15B C18B -57(2) . . . . ?
N4B C12B C13B N3B 60(3) . . . . ?
C1B C6B C5B C4B 0.0 . . . . ?
C1B C6B C5B C8B -177.6(12) . . . . ?
C6B C1B C2B C3B 0.0 . . . . ?
C6B C1B C7B N3B 8.7(19) . . . . ?
C6B C5B C4B C3B 0.0 . . . . ?
C6B C5B C8B N2B 170.5(12) . . . . ?
C5B C4B C3B C2B 0.0 . . . . ?
C5B C4B C3B C16B -179.9(12) . . . 3_665 ?
C4B C5B C8B N2B -7(2) . . . . ?
C4B C3B C2B C1B 0.0 . . . . ?
C2B C1B C6B C5B 0.0 . . . . ?
C2B C1B C7B N3B -174.2(12) . . . . ?
C7B N3B C13B C12B -135(2) . . . . ?
C7B C1B C6B C5B 177.1(11) . . . . ?
C7B C1B C2B C3B -177.2(11) . . . . ?
C8B N2B C14B C15B -120(2) . . . . ?
C8B C5B C4B C3B 177.5(12) . . . . ?
C9B C10B C11B N4B -178.6(12) 2_655 . . . ?
C9B C10B C11B N4B 0(2) . . . . ?
C10B C9B C10B C9B 2(3) 3_665 . . 2_655 ?
C10B C9B C10B C11B -177.3(8) 3_665 . . . ?
C11B N4B C12B C13B -129.1(18) . . . . ?
C11B N4B C12B C19B 119.2(17) . . . . ?
C11B N4B C12B C1 -13(2) . . . . ?
C12B N4B C11B C10B -175.7(13) . . . . ?
C13B N3B C7B C1B 179.3(15) . . . . ?
C14B N2B C8B C5B -178.2(17) . . . . ?
C15B N1B C16B C3B -180(2) . . . 2_655 ?
C16B N1B C15B C14B -120(2) . . . . ?
C16B N1B C15B C17B 114(2) . . . . ?
C16B N1B C15B C18B -3(3) . . . . ?
C16B C3B C2B C1B 179.8(13) 3_665 . . . ?
C19B C12B C13B N3B 176(2) . . . . ?
Cl2S Cl2S C2 Cl2S 0.0(3) 2_765 . . 3_675 ?
Cl2S Cl2S C2 Cl2S 0.0(3) 3_675 . . 2_765 ?
Cl2S Cl2S C2 Cl1S 0.0(2) 3_675 . . . ?
Cl2S Cl2S C2 Cl1S 0.0(2) 2_765 . . . ?
Cl2S C2 Cl1S Cl2S 0.000(3) 3_675 . . . ?
Cl2S C2 Cl1S Cl2S 0.000(3) 2_765 . . . ?
Cl2S C2 Cl1S C2 -47(4) 2_765 . . 2_765 ?
Cl2S C2 Cl1S C2 13(5) 2_765 . . 3_675 ?
Cl2S C2 Cl1S C2 13(5) . . . 3_675 ?
Cl2S C2 Cl1S C2 -47(4) 3_675 . . 2_765 ?
Cl2S C2 Cl1S C2 13(5) 3_675 . . 3_675 ?
Cl2S C2 Cl1S C2 -47(4) . . . 2_765 ?
Cl2S C2 Cl1S Cl1S -31(21) 3_675 . . 3_675 ?
Cl2S C2 Cl1S Cl1S -85(18) 3_675 . . 2_765 ?
Cl2S C2 Cl1S Cl1S -31(21) 2_765 . . 3_675 ?
Cl2S C2 Cl1S Cl1S -85(18) 2_765 . . 2_765 ?
Cl2S C2 Cl1S Cl1S -85(18) . . . 2_765 ?
Cl2S C2 Cl1S Cl1S -31(21) . . . 3_675 ?
Cl4S Cl4S C5S Cl4S 61(2) 2_655 . . 3_665 ?
Cl4S Cl4S C5S Cl3S 93(5) 3_665 . . 2_655 ?
Cl4S Cl4S C5S Cl3S 153(7) 2_655 . . 2_655 ?
Cl4S Cl4S C5S Cl3S 126(6) 2_655 . . 3_665 ?
Cl4S Cl4S C5S Cl3S 65(4) 3_665 . . 3_665 ?
Cl4S Cl4S C5S Cl3S 146(5) 2_655 . . . ?
Cl4S Cl4S C5S Cl3S 85(3) 3_665 . . . ?
Cl4S Cl4S C5S C5S 80(4) 3_665 . . 3_665 ?
Cl4S Cl4S C5S C5S 141(6) 2_655 . . 3_665 ?
Cl3S Cl3S C5S Cl4S -131(4) 3_665 . . . ?
Cl3S Cl3S C5S Cl4S 165(6) 2_655 . . . ?
Cl3S Cl3S C5S Cl4S -84(3) 3_665 . . 3_665 ?
Cl3S Cl3S C5S Cl4S -148(5) 2_655 . . 3_665 ?
Cl3S Cl3S C5S Cl3S 64.2(18) 3_665 . . 2_655 ?
Cl3S Cl3S C5S Cl3S -64.2(18) 2_655 . . 3_665 ?
Cl3S Cl3S C5S C5S -127(5) 3_665 . . 3_665 ?
Cl3S Cl3S C5S C5S 169(7) 2_655 . . 3_665 ?
C5S Cl4S C5S Cl4S -23(3) 2_655 . . 3_665 ?
C5S Cl4S C5S Cl4S -80(4) 3_665 . . 3_665 ?
C5S Cl4S C5S Cl3S 5(2) 3_665 . . . ?
C5S Cl4S C5S Cl3S 70(3) 2_655 . . 2_655 ?
C5S Cl4S C5S Cl3S -15.7(18) 3_665 . . 3_665 ?
C5S Cl4S C5S Cl3S 62.2(11) 2_655 . . . ?
C5S Cl4S C5S Cl3S 41.8(12) 2_655 . . 3_665 ?
C5S Cl4S C5S Cl3S 12(3) 3_665 . . 2_655 ?
C5S Cl4S C5S C5S 57.5(11) 2_655 . . 3_665 ?
C5S Cl3S C5S Cl4S -4(2) 3_665 . . . ?
C5S Cl3S C5S Cl4S -75.3(14) 2_655 . . . ?
C5S Cl3S C5S Cl4S -28(2) 2_655 . . 3_665 ?
C5S Cl3S C5S Cl4S 43(2) 3_665 . . 3_665 ?
C5S Cl3S C5S Cl3S 56(5) 2_655 . . 3_665 ?
C5S Cl3S C5S Cl3S 120(7) 2_655 . . 2_655 ?
C5S Cl3S C5S Cl3S 127(5) 3_665 . . 3_665 ?
C5S Cl3S C5S Cl3S -169(7) 3_665 . . 2_655 ?
C5S Cl3S C5S C5S -70.8(10) 2_655 . . 3_665 ?
C1 C12B C13B N3B -63(2) . . . . ?
C2 Cl2S C2 Cl2S 0(100) 3_675 . . 2_765 ?
C2 Cl2S C2 Cl2S 0(100) 2_765 . . 3_675 ?
C2 Cl2S C2 Cl2S 0(100) 2_765 . . 2_765 ?
C2 Cl2S C2 Cl2S 0(100) 3_675 . . 3_675 ?
C2 Cl2S C2 Cl1S 59(6) 2_765 . . . ?
C2 Cl2S C2 Cl1S -14(6) 3_675 . . . ?
Cl1S Cl2S C2 Cl2S 0(100) . . . 2_765 ?
Cl1S Cl2S C2 Cl2S 0(100) . . . 3_675 ?
_shelx_res_file
;
TITL thl_411_a_a.res in P321
REM Old TITL thl_411_a in P321 #150
REM SHELXT solution in P321
REM R1 0.269, Rweak 0.083, Alpha 0.015, Orientation as input
REM Flack x = -0.211 ( 0.739 ) from Parsons' quotients
REM Formula found by SHELXT: C135 N33 O20
CELL 0.71073 17.5575 17.5575 28.6921 90 90 120
ZERR 2 0.0007 0.0007 0.0012 0 0 0
LATT -1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SFAC C H Cl N O
UNIT 284.18 376.36 11 48 19.85
EQIV $1 1+Y-X,1-X,+Z
EQIV $2 1-Y,+X-Y,+Z
EQIV $3 2-Y,1+X-Y,+Z
EQIV $4 1+Y-X,2-X,+Z
DFIX 1.49 0.015 N3C_$1 C13C_$1
DFIX 1.54 0.015 C14C C13C_$1
DFIX 1.39 0.015 C11C_$1 C10C_$1 C11C_$1 C10C_$2
DFIX 1.47 0.015 N3C C13C N2C C15C N4C C14C N1C C16C
DFIX 1.54 0.015 C16C C15C
DFIX 1.74 Cl4S C5S Cl3S C5S Cl5S C7S
DFIX 1.47 0.015 C7C C2C C9C C6C C8C C4C
DFIX 1.23 0.015 N4C C9C N3C C7C N2C C8C
SADI C4S C7C C7C C3C
SADI C3C C8C C8C C5C
SADI C5C C9C C9C C4S
DANG 2.4 0.02 N4C C13C_$1
DANG 2.4 0.02 C14C N3C_$1
DANG 2.41 0.02 C10C_$1 C10C
DANG 2.41 0.02 C11C C11C_$1
DANG 2.41 0.02 C10C_$1 C10C_$2
FLAT 0.01 N3C N4C > C9C
RIGU N3B > C19B
RIGU Cl5S C7S
RIGU C4A C5A C6A C7A C8A C9A
EADP C7C N3C C13C C14C N4C C9C
L.S. 100
PLAN 0
TEMP -173.15
FREE Cl2S Cl1S_$4
FREE Cl2S Cl1S_$3
FREE C5S C5S_$2
FREE C5S Cl4S_$2
FREE C2 C2_$3
FREE C2 Cl1S_$4
FREE C2 C2_$4
FREE C2 Cl1S_$3
FREE Cl1S Cl2S_$3
FREE Cl1S Cl2S_$4
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.100000
FVAR 0.06257 0.65449
N4A 4 0.927903 0.693344 0.427929 11.00000 0.03570 0.05368 =
0.08402 0.00312 0.01060 0.01646
N3A 4 0.774797 0.713213 0.436140 11.00000 0.05797 0.02897 =
0.06870 0.00130 0.01156 0.01643
N1A 4 0.756290 0.890628 0.166399 11.00000 0.05145 0.04364 =
0.05645 -0.00246 -0.00674 0.01758
N2A 4 0.650948 0.817342 0.248444 11.00000 0.06242 0.03441 =
0.07897 0.00734 0.01137 0.01555
C1A 1 0.937087 1.025552 0.168887 11.00000 0.05266 0.05391 =
0.07737 0.00293 -0.00262 0.03273
AFIX 43
H1A 2 0.894147 1.043374 0.169484 11.00000 -1.20000
AFIX 0
C2A 1 0.911105 0.937571 0.168452 11.00000 0.05417 0.04504 =
0.07187 0.00407 -0.00044 0.02773
C3A 1 0.817830 0.869340 0.168198 11.00000 0.03789 0.04587 =
0.06411 -0.00211 -0.00877 0.01450
AFIX 43
H3A 2 0.801965 0.809107 0.169353 11.00000 -1.20000
AFIX 0
C4A 1 0.666301 0.818328 0.163481 11.00000 0.04485 0.04969 =
0.08240 0.00132 -0.01620 0.01532
AFIX 13
H4A 2 0.665306 0.761077 0.166362 11.00000 -1.20000
AFIX 0
C5A 1 0.628431 0.823046 0.116342 11.00000 0.08952 0.06044 =
0.09399 -0.01060 -0.03664 0.02612
AFIX 23
H5AA 2 0.660999 0.813050 0.091162 11.00000 -1.20000
H5AB 2 0.636343 0.882539 0.112098 11.00000 -1.20000
AFIX 0
C6A 1 0.530025 0.754142 0.112625 11.00000 0.08679 0.08328 =
0.16672 -0.00267 -0.05679 0.02137
AFIX 23
H6AA 2 0.506456 0.761353 0.082634 11.00000 -1.20000
H6AB 2 0.522326 0.694318 0.113422 11.00000 -1.20000
AFIX 0
C7A 1 0.481000 0.764801 0.151791 11.00000 0.05913 0.10399 =
0.18278 0.00179 -0.03927 0.00506
AFIX 23
H7AA 2 0.418278 0.718762 0.149550 11.00000 -1.20000
H7AB 2 0.484524 0.822685 0.149031 11.00000 -1.20000
AFIX 0
C8A 1 0.516017 0.758657 0.198764 11.00000 0.04636 0.08223 =
0.16887 0.01232 -0.00505 0.01842
AFIX 23
H8AA 2 0.508288 0.699193 0.202791 11.00000 -1.20000
H8AB 2 0.482348 0.767887 0.223620 11.00000 -1.20000
AFIX 0
C9A 1 0.613391 0.827526 0.203191 11.00000 0.04806 0.04891 =
0.08986 0.00986 -0.00742 0.02464
AFIX 13
H9A 2 0.620128 0.887515 0.201966 11.00000 -1.20000
AFIX 0
C10A 1 0.676220 0.878736 0.276656 11.00000 0.05497 0.05358 =
0.08329 0.01815 0.02560 0.02078
AFIX 43
H10A 2 0.672106 0.928915 0.268302 11.00000 -1.20000
AFIX 66
C11A 1 0.713287 0.876707 0.323791 11.00000 0.06359 0.04366 =
0.07675 0.00114 0.00776 0.03201
C16A 1 0.736499 0.946179 0.354479 11.00000 0.06806 0.04206 =
0.06642 0.00811 0.02335 0.02959
AFIX 43
H16A 2 0.731061 0.995203 0.345235 11.00000 -1.20000
AFIX 65
C15A 1 0.767668 0.943923 0.398694 11.00000 0.07959 0.04270 =
0.07067 0.00427 0.02682 0.03333
C14A 1 0.775625 0.872195 0.412220 11.00000 0.07045 0.05291 =
0.07047 0.00615 0.01816 0.03156
AFIX 43
H14A 2 0.796928 0.870654 0.442439 11.00000 -1.20000
AFIX 65
C13A 1 0.752413 0.802722 0.381533 11.00000 0.06781 0.03562 =
0.06984 0.00132 0.02096 0.02356
C12A 1 0.721244 0.804977 0.337318 11.00000 0.05882 0.05060 =
0.06704 0.00487 0.01207 0.02806
AFIX 43
H12A 2 0.705379 0.757496 0.316344 11.00000 -1.20000
AFIX 0
C17A 1 0.756796 0.723403 0.395527 11.00000 0.06783 0.04355 =
0.05697 0.00512 0.01143 0.02364
AFIX 43
H17A 2 0.745575 0.679504 0.372901 11.00000 -1.20000
AFIX 0
C18A 1 0.773986 0.632383 0.447755 11.00000 0.06129 0.03255 =
0.06056 -0.00329 -0.00218 0.02792
AFIX 13
H18A 2 0.759769 0.594840 0.419275 11.00000 -1.20000
AFIX 0
C19A 1 0.703548 0.582179 0.485719 11.00000 0.05235 0.04477 =
0.08675 0.01023 0.02311 0.02075
AFIX 23
H19A 2 0.714229 0.621818 0.512515 11.00000 -1.20000
H19B 2 0.644646 0.564627 0.472947 11.00000 -1.20000
AFIX 0
C20A 1 0.704843 0.501539 0.502311 11.00000 0.07080 0.05154 =
0.07761 0.01209 0.02348 0.02604
AFIX 23
H20A 2 0.690808 0.460060 0.476033 11.00000 -1.20000
H20B 2 0.659618 0.471731 0.526739 11.00000 -1.20000
AFIX 0
C21A 1 0.796099 0.527208 0.522094 11.00000 0.06322 0.04105 =
0.07920 0.00824 0.00501 0.02324
AFIX 23
H21A 2 0.810049 0.567370 0.548991 11.00000 -1.20000
H21B 2 0.797337 0.474151 0.532642 11.00000 -1.20000
AFIX 0
C22A 1 0.863090 0.573068 0.482865 11.00000 0.04705 0.05464 =
0.09118 0.01676 0.00181 0.02332
AFIX 23
H22A 2 0.922359 0.588535 0.494215 11.00000 -1.20000
H22B 2 0.848393 0.531827 0.456413 11.00000 -1.20000
AFIX 0
C23A 1 0.864784 0.654551 0.466179 11.00000 0.04474 0.04197 =
0.06131 -0.00679 -0.00319 0.01984
AFIX 13
H23A 2 0.882226 0.697713 0.492353 11.00000 -1.20000
AFIX 0
C24A 1 0.983400 0.774764 0.432684 11.00000 0.05592 0.06143 =
0.05934 0.00345 -0.01007 0.01979
AFIX 43
H24A 2 0.978355 0.805332 0.458743 11.00000 -1.20000
AFIX 0
PART 1
O2S 5 0.916032 0.659830 0.251406 21.00000 0.07025
O1S 5 0.767349 0.673811 0.273581 21.00000 0.07460
C1S 1 0.830695 0.580205 0.256161 21.00000 0.06913
AFIX 23
H1SA 2 0.840784 0.530060 0.260789 21.00000 -1.20000
H1SB 2 0.798596 0.570204 0.226371 21.00000 -1.20000
AFIX 0
C2S 1 0.904123 0.730371 0.236592 21.00000 0.08034
AFIX 23
H2SA 2 0.874624 0.716504 0.205837 21.00000 -1.20000
H2SB 2 0.961975 0.784642 0.233415 21.00000 -1.20000
AFIX 0
C3S 1 0.851975 0.743622 0.269919 21.00000 0.08146
AFIX 23
H3SA 2 0.880825 0.754365 0.300769 21.00000 -1.20000
H3SB 2 0.849512 0.796938 0.261279 21.00000 -1.20000
AFIX 0
PART 0
PART 2
N3C 4 0.605692 0.568610 0.313684 -21.00000 0.12110
N1C 4 0.801726 0.578222 0.048407 -21.00000 0.10552
N4C 4 0.968615 0.563934 0.316916 -21.00000 0.12110
N2C 4 0.850213 0.679821 0.132422 -21.00000 0.11158
AFIX 66
C4C 1 0.846300 0.632842 0.207822 -21.00000 0.07825
C3C 1 0.766161 0.627268 0.217707 -21.00000 0.09287
AFIX 43
H3C 2 0.737098 0.641959 0.194484 -21.00000 -1.20000
AFIX 65
C2C 1 0.728545 0.600198 0.261571 -21.00000 0.12225
PART 0
C4S 1 0.771070 0.578703 0.295549 11.00000 0.13863
PART 1
AFIX 23
H4SA 2 0.798897 0.588774 0.326654 21.00000 -1.20000
H4SB 2 0.712731 0.524499 0.295725 21.00000 -1.20000
AFIX 43
PART 0
PART 2
H4S 2 0.745361 0.560202 0.325527 -21.00000 -1.20000
AFIX 65
C6C 1 0.851210 0.584279 0.285664 -21.00000 0.09178
C5C 1 0.888825 0.611347 0.241801 -21.00000 0.09689
AFIX 43
H5C 2 0.943596 0.615157 0.235045 -21.00000 -1.20000
AFIX 0
C7C 1 0.642626 0.592881 0.274317 -21.00000 0.12110
AFIX 43
H7C 2 0.613517 0.607559 0.251115 -21.00000 -1.20000
AFIX 0
C8C 1 0.887616 0.660805 0.162484 -21.00000 0.08592
AFIX 43
H8C 2 0.942411 0.664323 0.156198 -21.00000 -1.20000
AFIX 0
C9C 1 0.897139 0.561201 0.322140 -21.00000 0.12110
AFIX 43
H9C 2 0.869360 0.542988 0.351679 -21.00000 -1.20000
AFIX 0
C10C 1 0.604659 0.360194 0.055273 -21.00000 0.10176
AFIX 43
H10C 2 0.562313 0.378662 0.057333 -21.00000 -1.20000
AFIX 0
C11C 1 0.693946 0.422730 0.053775 -21.00000 0.09752
C12C 1 0.728076 0.523378 0.055029 -21.00000 0.09666
AFIX 43
H12C 2 0.686749 0.541859 0.061576 -21.00000 -1.20000
AFIX 0
C13C 1 0.518545 0.562016 0.316798 -21.00000 0.12110
AFIX 43
H13C 2 0.501160 0.599861 0.302641 -21.00000 -1.20000
AFIX 0
C14C 1 1.019694 0.538384 0.347664 21.00000 0.12110
AFIX 23
H14B 2 0.983991 0.504339 0.374763 21.00000 -1.20000
H14C 2 1.073448 0.590993 0.359114 21.00000 -1.20000
AFIX 0
C15C 1 0.898130 0.721707 0.089131 -21.00000 0.07471
AFIX 23
H15A 2 0.949334 0.713173 0.084900 -21.00000 -1.20000
H15B 2 0.918482 0.785442 0.088908 -21.00000 -1.20000
AFIX 0
C16C 1 0.827078 0.672097 0.050924 -21.00000 0.07759
C17C 1 0.770201 0.705054 0.048533 -21.00000 0.11872
AFIX 137
H17B 2 0.734765 0.683639 0.020093 -21.00000 -1.50000
H17C 2 0.804168 0.769466 0.048012 -21.00000 -1.50000
H17D 2 0.731388 0.685399 0.075800 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
N3B 4 0.507060 0.520563 0.278254 21.00000 0.08876 0.04956 =
0.08253 -0.01205 -0.00275 0.04780
N2B 4 0.381235 0.298102 0.089909 21.00000 0.06954 0.08197 =
0.06872 0.00211 -0.01700 0.04193
N4B 4 0.562019 0.473307 0.363917 21.00000 0.05229 0.06181 =
0.04935 -0.00816 0.00305 0.02777
N1B 4 0.353359 0.117052 0.098537 21.00000 0.07137 0.09754 =
0.05822 -0.01301 -0.00987 0.03659
AFIX 66
C1B 1 0.557918 0.521723 0.201578 21.00000 0.07467 0.06278 =
0.08224 -0.00433 -0.00979 0.04056
C6B 1 0.483935 0.443310 0.188643 21.00000 0.07249 0.06238 =
0.06733 0.00451 -0.00182 0.03418
AFIX 43
H6B 2 0.437072 0.413025 0.210136 21.00000 -1.20000
AFIX 65
C5B 1 0.478520 0.409209 0.144262 21.00000 0.07665 0.07671 =
0.06507 0.00083 -0.00777 0.04697
C4B 1 0.547088 0.453521 0.112816 21.00000 0.07389 0.09957 =
0.06012 0.00406 -0.00971 0.04866
AFIX 43
H4B 2 0.543387 0.430214 0.082483 21.00000 -1.20000
AFIX 65
C3B 1 0.621071 0.531934 0.125750 21.00000 0.06774 0.09964 =
0.07722 0.00203 -0.01254 0.04731
C2B 1 0.626487 0.566036 0.170130 21.00000 0.07837 0.06952 =
0.08180 0.01251 0.00235 0.04396
AFIX 43
H2B 2 0.677051 0.619628 0.178970 21.00000 -1.20000
AFIX 0
C7B 1 0.564528 0.561792 0.246865 21.00000 0.08372 0.05968 =
0.07896 0.00148 -0.00824 0.04391
AFIX 43
H7B 2 0.612075 0.619162 0.253087 21.00000 -1.20000
AFIX 0
C8B 1 0.394875 0.325790 0.131895 21.00000 0.08620 0.07961 =
0.07868 0.00191 -0.01383 0.05220
AFIX 43
H8B 2 0.352454 0.293948 0.155317 21.00000 -1.20000
AFIX 0
C9B 1 0.696588 0.422585 0.367410 21.00000 0.06536 0.06617 =
0.04156 -0.00881 -0.00109 0.03709
AFIX 43
H9B 2 0.717228 0.483966 0.368019 21.00000 -1.20000
AFIX 0
C10B 1 0.606824 0.363786 0.366971 21.00000 0.06003 0.07020 =
0.03657 -0.01371 0.00119 0.03635
C11B 1 0.541922 0.392880 0.365357 21.00000 0.06416 0.06526 =
0.04212 -0.00712 0.00536 0.03512
AFIX 43
H11B 2 0.481368 0.349279 0.365387 21.00000 -1.20000
AFIX 0
C12B 1 0.494846 0.499873 0.365549 21.00000 0.05511 0.09026 =
0.09223 -0.03100 -0.01774 0.04534
C13B 1 0.511173 0.559359 0.327142 21.00000 0.16507 0.09513 =
0.08754 -0.02399 -0.00833 0.09135
AFIX 23
H13A 2 0.570101 0.611805 0.331333 21.00000 -1.20000
H13B 2 0.467488 0.579270 0.328475 21.00000 -1.20000
AFIX 0
C14B 1 0.301957 0.223081 0.082576 21.00000 0.08002 0.09461 =
0.06832 -0.01042 -0.00163 0.03713
AFIX 23
H14D 2 0.267462 0.237166 0.060469 21.00000 -1.20000
H14E 2 0.269443 0.206050 0.112466 21.00000 -1.20000
AFIX 0
C15B 1 0.305671 0.143055 0.063604 21.00000 0.08453 0.10881 =
0.06117 -0.01721 -0.01039 0.04601
C16B 1 0.422249 0.116212 0.089992 21.00000 0.07222 0.08076 =
0.06671 -0.02424 -0.01275 0.02959
AFIX 43
H16B 2 0.447392 0.133227 0.059804 21.00000 -1.20000
AFIX 0
C17B 1 0.219552 0.065316 0.052679 21.00000 0.08478 0.10029 =
0.07435 -0.01092 -0.01788 0.04345
AFIX 137
H17E 2 0.227598 0.015201 0.045544 21.00000 -1.50000
H17F 2 0.193652 0.078164 0.025679 21.00000 -1.50000
H17G 2 0.180293 0.051029 0.079569 21.00000 -1.50000
AFIX 0
C18B 1 0.357970 0.173327 0.017242 21.00000 0.11457 0.10955 =
0.06301 -0.01862 0.00594 0.05477
AFIX 137
H18B 2 0.409000 0.232304 0.021244 21.00000 -1.50000
H18C 2 0.319978 0.174618 -0.007398 21.00000 -1.50000
H18D 2 0.377968 0.132180 0.008596 21.00000 -1.50000
AFIX 0
C19B 1 0.509845 0.555223 0.406951 21.00000 0.07170 0.09485 =
0.08996 -0.02554 0.00416 0.03508
AFIX 137
H19C 2 0.508968 0.522868 0.434968 21.00000 -1.50000
H19D 2 0.463412 0.570555 0.409107 21.00000 -1.50000
H19E 2 0.567136 0.609076 0.404327 21.00000 -1.50000
AFIX 0
CL2S 3 1.000000 1.000000 0.286506 10.33333 0.21650
CL4S 3 0.635667 0.360548 0.159686 10.33333 0.17508
CL3S 3 0.668795 0.358949 0.249459 10.33333 0.10144
C5S 1 0.623118 0.285998 0.202239 10.33333 0.15524
O8S 5 0.333333 0.666667 0.039857 10.08333 0.20472
PART 0
PART 3
O9S 5 0.382450 0.715930 -0.006899 10.25000 0.23743
PART 0
PART 1
CL5S 3 0.460508 0.543406 0.029213 10.50000 0.18821 0.09625 =
0.12287 0.01387 -0.02731 0.07315
C7S 1 0.446386 0.446386 0.000000 10.25000 0.07885 0.07885 =
0.07600 0.02921 -0.02921 0.02631
AFIX 23
H7SA 2 0.427634 0.398539 0.023186 10.25000 -1.20000
H7SB 2 0.398535 0.427627 -0.023184 10.25000 -1.20000
AFIX 0
PART 0
O3S 5 1.000000 1.000000 0.500000 10.05556 0.21337
PART 2
O7S 5 0.453884 0.482878 0.027768 10.33333 0.13611
PART 0
O6S 5 1.000000 1.000000 0.027483 10.11111 0.24623
PART 2
O4S 5 0.910379 0.830687 0.287516 11.00000 0.16781
PART 0
PART 1
C1 1 0.402575 0.427277 0.358148 21.00000 0.08054 0.06858 =
0.06840 0.01664 0.00349 0.02602
AFIX 137
H1B 2 0.400666 0.391411 0.331517 21.00000 -1.50000
H1C 2 0.364673 0.452309 0.351923 21.00000 -1.50000
H1D 2 0.381825 0.390462 0.386147 21.00000 -1.50000
AFIX 0
PART 0
O5S 5 0.333333 0.666667 0.288224 10.08333 0.10487
C2 1 1.058507 1.022084 0.325734 10.33333 0.09738
CL1S 3 1.026871 0.984569 0.367064 10.33333 0.44267
O10S 5 0.333333 0.666667 0.387987 10.08333 0.17424
HKLF 4
REM thl_411_a_a.res in P321
REM R1 = 0.1285 for 5557 Fo > 4sig(Fo) and 0.1435 for all 6254 data
REM 595 parameters refined using 230 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 0.713, deepest hole -0.686, 1-sigma level 0.151
Q1 1 1.0391 1.0805 0.0132 11.00000 0.05 0.71
Q2 1 1.0000 1.0000 0.0551 10.33333 0.05 0.65
Q3 1 0.8568 0.8568 0.5000 10.50000 0.05 0.63
Q4 1 0.5028 0.5420 0.0225 11.00000 0.05 0.57
Q5 1 0.3572 0.6857 -0.0410 11.00000 0.05 0.55
Q6 1 0.3792 0.7664 0.0130 11.00000 0.05 0.54
Q7 1 0.4274 0.5075 0.0250 11.00000 0.05 0.53
Q8 1 0.3333 0.6667 0.4326 10.33333 0.05 0.52
Q9 1 0.5648 0.5648 0.0000 10.50000 0.05 0.51
Q10 1 0.3333 0.6667 0.3312 10.33333 0.05 0.50
Q11 1 0.4089 0.7057 0.3657 11.00000 0.05 0.50
Q12 1 1.1365 0.6146 0.3445 11.00000 0.05 0.47
Q13 1 0.3742 0.7019 0.3084 11.00000 0.05 0.47
Q14 1 1.0000 1.0000 0.4463 10.33333 0.05 0.46
Q15 1 0.6667 0.3333 0.1178 10.33333 0.05 0.46
Q16 1 0.2878 0.1786 0.0074 11.00000 0.05 0.45
Q17 1 0.0972 0.0734 0.0768 11.00000 0.05 0.43
Q18 1 0.4208 0.7150 0.3259 11.00000 0.05 0.42
Q19 1 1.0000 1.0000 0.4172 10.33333 0.05 0.41
Q20 1 0.7416 0.4157 0.5513 11.00000 0.05 0.40
;
_shelx_res_checksum 20124
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_CC2-R_1-4-dioxane
_database_code_depnum_ccdc_archive 'CCDC 1520510'
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_audit_creation_date 2015-07-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C54 H54 N12), 5.5(C4 H8 O2), 4.25(H2 O)'
_chemical_formula_sum 'C130 H160.50 N24 O15.25'
_chemical_formula_weight 2303.31
_chemical_absolute_configuration R
_chemical_melting_point ?
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 0.0100 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system cubic
_space_group_IT_number 198
_space_group_name_H-M_alt 'P 21 3'
_space_group_name_Hall 'P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
_cell_length_a 24.318(2)
_cell_length_b 24.318(2)
_cell_length_c 24.318(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 14381(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4073
_cell_measurement_temperature 100
_cell_measurement_theta_max 9.905
_cell_measurement_theta_min 2.300
_shelx_estimated_absorpt_T_max 0.997
_shelx_estimated_absorpt_T_min 0.990
_exptl_absorpt_coefficient_mu 0.066
_exptl_absorpt_correction_T_max 0.9568
_exptl_absorpt_correction_T_min 0.7928
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1759 before and 0.1032 after correction.
The Ratio of minimum to maximum transmission is 0.8286.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.064
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 4922
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0772
_diffrn_reflns_av_unetI/netI 0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 45501
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 22.500
_diffrn_reflns_theta_max 22.517
_diffrn_reflns_theta_min 1.148
_diffrn_ambient_temperature 100
_diffrn_detector 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type 'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type 'Kappa Rigaku Saturn724+'
_diffrn_measurement_method 'omega rotation'
_diffrn_radiation_collimation '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator Synchrotron
_diffrn_radiation_probe x-ray
_diffrn_radiation_type ?
_diffrn_radiation_wavelength 0.6889
_diffrn_source Synchrotron
_diffrn_source_target Cu
_diffrn_source_type 'Undulator, I19, DLS, RAL'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.847
_reflns_Friedel_fraction_full 0.996
_reflns_Friedel_fraction_max 0.996
_reflns_number_gt 5558
_reflns_number_total 6914
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'CrystalClear v2 (Rigaku)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution ?
_refine_diff_density_max 0.363
_refine_diff_density_min -0.273
_refine_diff_density_rms 0.054
_refine_ls_abs_structure_details
;
Flack x determined using 2208 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.3(10)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 609
_refine_ls_number_reflns 6914
_refine_ls_number_restraints 48
_refine_ls_R_factor_all 0.0860
_refine_ls_R_factor_gt 0.0722
_refine_ls_restrained_S_all 1.047
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1553P)^2^+0.0650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2033
_refine_ls_wR_factor_ref 0.2134
_refine_special_details ?
_olex2_refinement_description
;
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. Rigid body (RIGU) restrains
O50, O47, C48, C48, C48, C49, C49, C49
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
O44, O43, C45, C46
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C11, C10, O12, O13
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C42, O3, C41, O4
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
Sof(H5A)=Sof(H5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=1-FVAR(1)
Sof(H4A)=Sof(H4B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
Sof(H16A)=Sof(H16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
Sof(H15A)=Sof(H15B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
Sof(H22A)=Sof(H22B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(3)
Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(3)
Sof(H33A)=Sof(H33B)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(4)
Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(4)
Fixed Sof: O1(0.75) O2(0.75) C37(0.75) H37A(0.75) H37B(0.75) C38(0.75)
H38A(0.75) H38B(0.75) C39(0.75) H39A(0.75) H39B(0.75) C40(0.75) H40A(0.75)
H40B(0.75) O3(0.33333) O4(0.33333) C41(0.66667) C42(0.66667) O43(0.33333)
O44(0.33333) C45(0.66667) C46(0.66667) O47(0.25) C48(0.5) C49(0.5) O50(0.25)
O5(0.16667) O6(0.25) O7(0.25) O8(0.25) O9(0.5) C10(0.33333) C11(0.33333)
O12(0.16667) O13(0.16667)
4.a Secondary CH2 refined with riding coordinates:
C4(H4A,H4B), C5(H5A,H5B), C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B),
C23(H23A,H23B), C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B),
C39(H39A,H39B), C40(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
C1(H1), C3(H3), C7(H7), C9(H9), C1AA(H1AA), C13(H13), C14(H14), C18(H18),
C19(H19), C21(H21), C25(H25), C27(H27), C29(H29), C31(H31), C32(H32), C36(H36)
4.c Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C6B(H6BA,H6BB,H6BC), C17(H17A,H17B,H17C), C17B(H17D,H17E,
H17F), C24(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C35(H35A,H35B,H35C),
C35B(H35D,H35E,H35F)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
N1 N 0.6725(2) 0.3589(2) 0.6585(2) 0.0715(15) Uani 1 1 d . . . . .
N2 N 0.6971(2) 0.3250(2) 0.5445(2) 0.0627(13) Uani 1 1 d . . . . .
N3 N 0.95151(19) 0.2670(2) 0.49621(19) 0.0553(12) Uani 1 1 d . . . . .
N4 N 1.03079(18) 0.23784(19) 0.5826(2) 0.0541(12) Uani 1 1 d . . . . .
C1 C 0.6690(2) 0.2571(3) 0.7664(3) 0.0637(16) Uani 1 1 d . . . . .
H1 H 0.6371 0.2380 0.7544 0.076 Uiso 1 1 calc R . . . .
C2 C 0.6860(3) 0.3027(3) 0.7373(3) 0.0648(16) Uani 1 1 d . . . . .
C3 C 0.6570(3) 0.3201(3) 0.6884(3) 0.0655(17) Uani 1 1 d . . . . .
H3 H 0.6244 0.3010 0.6784 0.079 Uiso 1 1 calc R . . . .
C4 C 0.6381(3) 0.3718(3) 0.6097(3) 0.0757(19) Uani 1 1 d . . . . .
H4A H 0.6178 0.4065 0.6162 0.091 Uiso 0.673(18) 1 calc R . . A 1
H4B H 0.6109 0.3421 0.6040 0.091 Uiso 0.673(18) 1 calc R . . A 1
C5 C 0.6730(3) 0.3777(3) 0.5595(3) 0.0716(18) Uani 1 1 d . . . . .
H5A H 0.6503 0.3915 0.5287 0.086 Uiso 0.327(18) 1 calc R . . A 2
H5B H 0.7027 0.4047 0.5666 0.086 Uiso 0.327(18) 1 calc R . . A 2
C6 C 0.6348(5) 0.3991(5) 0.5156(5) 0.084(4) Uani 0.673(18) 1 d . . . A 1
H6A H 0.6561 0.4087 0.4828 0.125 Uiso 0.673(18) 1 calc GR . . A 1
H6B H 0.6157 0.4319 0.5293 0.125 Uiso 0.673(18) 1 calc GR . . A 1
H6C H 0.6078 0.3707 0.5063 0.125 Uiso 0.673(18) 1 calc GR . . A 1
C6B C 0.6093(13) 0.4245(13) 0.6076(13) 0.110(11) Uiso 0.327(18) 1 d . . . A 2
H6BA H 0.5728 0.4205 0.6243 0.165 Uiso 0.327(18) 1 calc GR . . A 2
H6BB H 0.6052 0.4360 0.5692 0.165 Uiso 0.327(18) 1 calc GR . . A 2
H6BC H 0.6304 0.4522 0.6278 0.165 Uiso 0.327(18) 1 calc GR . . A 2
C7 C 0.7478(2) 0.3244(3) 0.5335(3) 0.0593(15) Uani 1 1 d . . . . .
H7 H 0.7681 0.3576 0.5364 0.071 Uiso 1 1 calc R . . . .
C8 C 0.7765(2) 0.2740(2) 0.5164(2) 0.0521(13) Uani 1 1 d . . . . .
C9 C 0.7474(2) 0.2253(2) 0.5071(2) 0.0530(14) Uani 1 1 d . . . . .
H9 H 0.7086 0.2249 0.5112 0.064 Uiso 1 1 calc R . . . .
C0AA C 0.7742(2) 0.1788(2) 0.4923(2) 0.0525(14) Uani 1 1 d . . . . .
C1AA C 0.8313(2) 0.1780(2) 0.4864(2) 0.0547(14) Uani 1 1 d . . . . .
H1AA H 0.8497 0.1452 0.4759 0.066 Uiso 1 1 calc R . . . .
C12 C 0.8610(2) 0.2261(2) 0.4961(2) 0.0526(14) Uani 1 1 d . . . . .
C13 C 0.8325(2) 0.2737(2) 0.5110(2) 0.0543(14) Uani 1 1 d . . . . .
H13 H 0.8525 0.3066 0.5176 0.065 Uiso 1 1 calc R . . . .
C14 C 0.9214(2) 0.2253(3) 0.4896(2) 0.0561(14) Uani 1 1 d . . . . .
H14 H 0.9385 0.1915 0.4798 0.067 Uiso 1 1 calc R . . . .
C15 C 1.0097(2) 0.2612(3) 0.4869(2) 0.0592(15) Uani 1 1 d . . . . .
H15A H 1.0210 0.2852 0.4561 0.071 Uiso 0.792(16) 1 calc R . . B 1
H15B H 1.0181 0.2227 0.4768 0.071 Uiso 0.792(16) 1 calc R . . B 1
C16 C 1.0417(2) 0.2767(3) 0.5384(2) 0.0569(15) Uani 1 1 d . . . . .
H16A H 1.0816 0.2770 0.5301 0.068 Uiso 0.208(16) 1 calc R . . B 2
H16B H 1.0310 0.3142 0.5503 0.068 Uiso 0.208(16) 1 calc R . . B 2
C17 C 1.1023(3) 0.2790(3) 0.5276(3) 0.053(2) Uani 0.792(16) 1 d . . . B 1
H17A H 1.1217 0.2882 0.5617 0.079 Uiso 0.792(16) 1 calc GR . . B 1
H17B H 1.1099 0.3071 0.4997 0.079 Uiso 0.792(16) 1 calc GR . . B 1
H17C H 1.1149 0.2431 0.5142 0.079 Uiso 0.792(16) 1 calc GR . . B 1
C17B C 1.028(3) 0.271(3) 0.432(3) 0.15(2) Uiso 0.208(16) 1 d . . . B 2
H17D H 1.0388 0.2361 0.4149 0.222 Uiso 0.208(16) 1 calc GR . . B 2
H17E H 1.0599 0.2959 0.4327 0.222 Uiso 0.208(16) 1 calc GR . . B 2
H17F H 0.9984 0.2879 0.4106 0.222 Uiso 0.208(16) 1 calc GR . . B 2
C18 C 1.0176(2) 0.2582(2) 0.6283(2) 0.0536(14) Uani 1 1 d . . . . .
H18 H 1.0137 0.2970 0.6305 0.064 Uiso 1 1 calc R . . . .
N5 N 0.9158(2) 0.4163(2) 0.6163(2) 0.0600(13) Uani 1 1 d . . . . .
N6 N 0.8038(2) 0.4450(2) 0.58791(19) 0.0561(12) Uani 1 1 d . . . . .
N7 N 0.7220(2) 0.5081(2) 0.3480(2) 0.0649(13) Uani 1 1 d . . . . .
N8 N 0.8008(2) 0.4740(2) 0.2620(2) 0.0711(15) Uani 1 1 d . . . . .
C19 C 1.0161(2) 0.4190(2) 0.5058(2) 0.0554(14) Uani 1 1 d . . . . .
H19 H 1.0043 0.3870 0.4867 0.066 Uiso 1 1 calc R . . . .
C20 C 0.9871(2) 0.4370(2) 0.5519(2) 0.0522(14) Uani 1 1 d . . . . .
C21 C 0.9395(2) 0.4060(2) 0.5711(3) 0.0572(15) Uani 1 1 d . . . . .
H21 H 0.9256 0.3771 0.5488 0.069 Uiso 1 1 calc R . . . .
C22 C 0.8683(3) 0.3828(2) 0.6317(2) 0.0573(15) Uani 1 1 d . . . . .
H22A H 0.8762 0.3626 0.6662 0.069 Uiso 0.216(18) 1 calc R . . C 2
H22B H 0.8605 0.3556 0.6025 0.069 Uiso 0.216(18) 1 calc R . . C 2
C23 C 0.8194(3) 0.4197(3) 0.6397(2) 0.0612(16) Uani 1 1 d . . . . .
H23A H 0.7881 0.3979 0.6542 0.073 Uiso 0.784(18) 1 calc R . . C 1
H23B H 0.8284 0.4486 0.6669 0.073 Uiso 0.784(18) 1 calc R . . C 1
C24 C 0.8802(3) 0.3522(3) 0.6858(4) 0.064(3) Uani 0.784(18) 1 d . . . C 1
H24A H 0.9141 0.3307 0.6819 0.096 Uiso 0.784(18) 1 calc GR . . C 1
H24B H 0.8495 0.3275 0.6943 0.096 Uiso 0.784(18) 1 calc GR . . C 1
H24C H 0.8847 0.3789 0.7156 0.096 Uiso 0.784(18) 1 calc GR . . C 1
C24B C 0.797(2) 0.3816(19) 0.669(2) 0.111(16) Uiso 0.216(18) 1 d . . . C 2
H24D H 0.7613 0.3944 0.6824 0.166 Uiso 0.216(18) 1 calc GR . . C 2
H24E H 0.8209 0.3725 0.6998 0.166 Uiso 0.216(18) 1 calc GR . . C 2
H24F H 0.7915 0.3488 0.6458 0.166 Uiso 0.216(18) 1 calc GR . . C 2
C25 C 0.7975(3) 0.4956(3) 0.5870(3) 0.0636(16) Uani 1 1 d . . . . .
H25 H 0.8042 0.5162 0.6196 0.076 Uiso 1 1 calc R . . . .
C26 C 0.7798(3) 0.5247(3) 0.5368(3) 0.0661(17) Uani 1 1 d . . . . .
C27 C 0.7747(3) 0.5811(3) 0.5363(3) 0.0651(16) Uani 1 1 d . . . . .
H27 H 0.7826 0.6014 0.5688 0.078 Uiso 1 1 calc R . . . .
C28 C 0.7577(3) 0.6096(3) 0.4878(3) 0.0681(17) Uani 1 1 d . . . . .
C29 C 0.7457(3) 0.5787(3) 0.4415(3) 0.0668(17) Uani 1 1 d . . . . .
H29 H 0.7344 0.5970 0.4089 0.080 Uiso 1 1 calc R . . . .
C30 C 0.7499(3) 0.5215(3) 0.4414(3) 0.0693(18) Uani 1 1 d . . . . .
C31 C 0.7668(3) 0.4951(3) 0.4899(3) 0.0665(16) Uani 1 1 d . . . . .
H31 H 0.7694 0.4562 0.4906 0.080 Uiso 1 1 calc R . . . .
C32 C 0.7365(3) 0.4885(3) 0.3937(3) 0.0690(18) Uani 1 1 d . . . . .
H32 H 0.7388 0.4496 0.3971 0.083 Uiso 1 1 calc R . . . .
C33 C 0.7076(3) 0.4697(3) 0.3040(3) 0.0665(17) Uani 1 1 d . . . . .
H33A H 0.6679 0.4729 0.2954 0.080 Uiso 0.271(17) 1 calc R . . D 2
H33B H 0.7150 0.4315 0.3161 0.080 Uiso 0.271(17) 1 calc R . . D 2
C34 C 0.7409(3) 0.4825(3) 0.2538(3) 0.0706(18) Uani 1 1 d . . . . .
H34A H 0.7282 0.4588 0.2232 0.085 Uiso 0.729(17) 1 calc R . . D 1
H34B H 0.7343 0.5212 0.2430 0.085 Uiso 0.729(17) 1 calc R . . D 1
C35 C 0.6464(3) 0.4783(4) 0.2891(4) 0.069(3) Uani 0.729(17) 1 d . . . D 1
H35A H 0.6233 0.4679 0.3205 0.103 Uiso 0.729(17) 1 calc GR . . D 1
H35B H 0.6369 0.4553 0.2573 0.103 Uiso 0.729(17) 1 calc GR . . D 1
H35C H 0.6400 0.5170 0.2801 0.103 Uiso 0.729(17) 1 calc GR . . D 1
C35B C 0.7250(15) 0.4355(15) 0.2175(15) 0.109(12) Uiso 0.271(17) 1 d . . . D 2
H35D H 0.7570 0.4236 0.1961 0.164 Uiso 0.271(17) 1 calc GR . . D 2
H35E H 0.6956 0.4472 0.1925 0.164 Uiso 0.271(17) 1 calc GR . . D 2
H35F H 0.7118 0.4049 0.2402 0.164 Uiso 0.271(17) 1 calc GR . . D 2
C36 C 0.8316(3) 0.5142(3) 0.2529(3) 0.0647(16) Uani 1 1 d . . . . .
H36 H 0.8151 0.5480 0.2422 0.078 Uiso 1 1 calc R . . . .
O1 O 0.8129(3) 0.3762(3) 0.4229(3) 0.0838(19) Uani 0.75 1 d . . . . .
O2 O 0.8995(3) 0.3435(3) 0.3510(3) 0.0783(17) Uani 0.75 1 d . . . . .
C37 C 0.8618(5) 0.4098(4) 0.4169(5) 0.089(3) Uani 0.75 1 d . . . . .
H37A H 0.8693 0.4294 0.4518 0.107 Uiso 0.75 1 calc R . . . .
H37B H 0.8558 0.4376 0.3878 0.107 Uiso 0.75 1 calc R . . . .
C38 C 0.9097(4) 0.3744(4) 0.4022(4) 0.075(3) Uani 0.75 1 d . . . . .
H38A H 0.9428 0.3977 0.3976 0.090 Uiso 0.75 1 calc R . . . .
H38B H 0.9170 0.3483 0.4326 0.090 Uiso 0.75 1 calc R . . . .
C39 C 0.8514(4) 0.3114(4) 0.3570(5) 0.090(3) Uani 0.75 1 d . . . . .
H39A H 0.8575 0.2832 0.3857 0.108 Uiso 0.75 1 calc R . . . .
H39B H 0.8435 0.2923 0.3219 0.108 Uiso 0.75 1 calc R . . . .
C40 C 0.8024(4) 0.3468(4) 0.3728(5) 0.087(3) Uani 0.75 1 d . . . . .
H40A H 0.7947 0.3733 0.3429 0.105 Uiso 0.75 1 calc R . . . .
H40B H 0.7696 0.3232 0.3775 0.105 Uiso 0.75 1 calc R . . . .
O3 O 0.8013(13) 0.2244(6) 0.6988(14) 0.083(5) Uani 0.3333 1 d . U . . 1
O4 O 0.8743(8) 0.1633(11) 0.6560(12) 0.123(7) Uani 0.3333 1 d . U . . 2
C41 C 0.7991(6) 0.2188(6) 0.6497(6) 0.102(4) Uani 0.6667 1 d . U . . .
C42 C 0.8606(7) 0.2139(7) 0.6533(7) 0.112(4) Uani 0.6667 1 d . U . . .
O43 O 0.9224(12) 0.5295(12) 0.3898(9) 0.131(6) Uani 0.3333 1 d . U . . .
O44 O 0.9552(10) 0.5578(12) 0.3789(9) 0.126(6) Uani 0.3333 1 d . U . . .
C45 C 0.8781(9) 0.5708(10) 0.3886(9) 0.162(7) Uani 0.6667 1 d . U . . .
C46 C 0.9591(15) 0.5290(13) 0.4302(9) 0.176(8) Uani 0.6667 1 d . U . . .
O47 O 0.5583(9) 0.5583(9) 0.5583(9) 0.32(2) Uani 0.75 3 d S TU P . .
C48 C 0.621(2) 0.558(2) 0.556(3) 0.284(18) Uani 0.5 1 d . U . . .
C49 C 0.631(2) 0.564(2) 0.614(3) 0.267(17) Uani 0.5 1 d . U . . .
O50 O 0.6270(10) 0.6270(10) 0.6270(10) 0.294(19) Uani 0.75 3 d S TU P . .
O5 O 0.4238(9) 0.4238(9) 0.4238(9) 0.174(11) Uiso 0.5 3 d S T P E 1
O6 O 0.4981(11) 0.4485(12) 0.4168(11) 0.116(8) Uiso 0.25 1 d . . . F 2
O7 O 0.5089(11) 0.3788(11) 0.4554(11) 0.108(7) Uiso 0.25 1 d . . . G 3
O8 O 0.5517(12) 0.4807(12) 0.4182(12) 0.122(8) Uiso 0.25 1 d . . . H 4
O9 O 0.7278(13) 0.6917(14) 0.6362(13) 0.242(11) Uiso 0.5 1 d . . . . .
C10 C 0.754(2) 0.207(2) 0.299(2) 0.175(16) Uiso 0.3333 1 d . U . . .
C11 C 0.656(4) 0.163(4) 0.311(3) 0.22(3) Uiso 0.3333 1 d . U . . .
O12 O 0.748(3) 0.143(3) 0.312(3) 0.17(2) Uiso 0.1667 1 d . U . . .
O13 O 0.729(3) 0.204(3) 0.340(3) 0.18(2) Uiso 0.1667 1 d . U . . .
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 0.069(3) 0.065(4) 0.080(4) -0.003(3) -0.002(3) 0.020(3)
N2 0.053(3) 0.065(3) 0.070(3) 0.003(3) -0.001(2) -0.001(2)
N3 0.051(3) 0.065(3) 0.050(3) 0.002(2) 0.004(2) -0.005(2)
N4 0.047(3) 0.057(3) 0.057(3) 0.014(2) 0.007(2) -0.008(2)
C1 0.051(3) 0.072(4) 0.068(4) -0.005(3) 0.006(3) 0.012(3)
C2 0.058(4) 0.069(4) 0.068(4) -0.006(3) 0.008(3) 0.015(3)
C3 0.053(4) 0.060(4) 0.083(5) -0.009(4) 0.011(3) 0.014(3)
C4 0.063(4) 0.067(4) 0.098(5) 0.000(4) 0.000(4) 0.022(3)
C5 0.062(4) 0.058(4) 0.095(5) 0.008(3) -0.011(4) 0.013(3)
C6 0.076(7) 0.084(8) 0.091(8) 0.015(6) -0.014(6) 0.020(6)
C7 0.049(4) 0.060(4) 0.069(4) 0.010(3) -0.005(3) -0.005(3)
C8 0.055(3) 0.046(3) 0.056(3) 0.002(3) -0.005(3) -0.007(3)
C9 0.044(3) 0.060(4) 0.055(3) 0.001(3) -0.005(2) -0.002(3)
C0AA 0.048(3) 0.060(4) 0.050(3) 0.000(3) -0.005(2) -0.015(3)
C1AA 0.056(4) 0.056(3) 0.052(3) -0.002(3) 0.003(3) -0.005(3)
C12 0.050(3) 0.058(4) 0.050(3) -0.003(3) -0.003(2) -0.010(3)
C13 0.055(4) 0.050(3) 0.058(3) 0.001(3) -0.002(3) -0.011(3)
C14 0.051(3) 0.071(4) 0.047(3) 0.003(3) 0.006(2) -0.007(3)
C15 0.045(3) 0.079(4) 0.054(3) 0.012(3) 0.005(3) -0.009(3)
C16 0.044(3) 0.070(4) 0.057(3) 0.019(3) 0.000(3) -0.011(3)
C17 0.042(4) 0.060(5) 0.057(5) 0.009(3) 0.012(3) 0.000(3)
C18 0.052(3) 0.055(3) 0.054(4) 0.009(3) 0.004(3) -0.006(3)
N5 0.068(3) 0.064(3) 0.048(3) 0.011(2) -0.004(2) 0.002(3)
N6 0.061(3) 0.056(3) 0.052(3) 0.007(2) -0.001(2) -0.001(2)
N7 0.065(3) 0.066(3) 0.063(3) 0.008(3) -0.015(3) -0.001(3)
N8 0.059(3) 0.072(4) 0.082(4) 0.005(3) -0.013(3) 0.013(3)
C19 0.059(4) 0.047(3) 0.060(4) -0.001(3) -0.008(3) 0.003(3)
C20 0.053(3) 0.051(3) 0.052(3) 0.010(3) -0.007(3) 0.001(3)
C21 0.061(4) 0.052(3) 0.058(4) 0.007(3) -0.010(3) 0.006(3)
C22 0.065(4) 0.060(4) 0.047(3) 0.020(3) 0.002(3) -0.010(3)
C23 0.074(4) 0.059(4) 0.051(3) 0.016(3) 0.003(3) -0.005(3)
C24 0.048(4) 0.068(5) 0.077(6) 0.032(4) -0.003(4) 0.003(3)
C25 0.081(4) 0.054(4) 0.056(4) 0.009(3) -0.007(3) -0.008(3)
C26 0.084(4) 0.063(4) 0.051(4) 0.013(3) -0.015(3) -0.013(3)
C27 0.077(4) 0.061(4) 0.057(4) 0.005(3) -0.017(3) 0.002(3)
C28 0.081(5) 0.064(4) 0.059(4) 0.009(3) -0.015(3) -0.001(3)
C29 0.076(4) 0.060(4) 0.064(4) 0.014(3) -0.015(3) -0.003(3)
C30 0.084(5) 0.059(4) 0.065(4) 0.010(3) -0.020(3) -0.005(3)
C31 0.068(4) 0.061(4) 0.070(4) 0.009(3) -0.009(3) -0.002(3)
C32 0.068(4) 0.063(4) 0.077(5) 0.009(3) -0.021(3) -0.005(3)
C33 0.059(4) 0.074(4) 0.066(4) 0.000(3) -0.017(3) -0.004(3)
C34 0.055(4) 0.092(5) 0.064(4) 0.002(3) -0.016(3) -0.001(3)
C35 0.051(5) 0.080(6) 0.075(6) -0.010(5) -0.012(4) -0.006(4)
C36 0.068(4) 0.054(4) 0.072(4) 0.016(3) -0.012(3) 0.000(3)
O1 0.072(4) 0.068(4) 0.112(5) 0.019(4) 0.015(4) 0.005(3)
O2 0.065(4) 0.077(4) 0.093(5) 0.021(3) 0.001(3) -0.004(3)
C37 0.097(8) 0.068(6) 0.101(8) 0.028(5) 0.008(6) -0.006(6)
C38 0.062(6) 0.085(6) 0.079(6) 0.021(5) -0.008(5) -0.013(5)
C39 0.059(6) 0.077(7) 0.133(9) 0.011(6) 0.002(6) 0.005(5)
C40 0.055(5) 0.072(6) 0.135(10) 0.010(6) -0.008(6) -0.003(5)
O3 0.079(12) 0.084(10) 0.085(10) 0.017(11) 0.000(6) -0.004(12)
O4 0.083(10) 0.121(13) 0.16(2) 0.001(11) -0.005(13) -0.014(9)
C41 0.107(8) 0.107(9) 0.093(8) 0.026(7) -0.015(7) -0.010(7)
C42 0.102(8) 0.124(10) 0.112(10) 0.006(9) -0.003(7) -0.024(7)
O43 0.139(14) 0.161(16) 0.093(12) -0.048(11) 0.024(10) -0.015(11)
O44 0.124(13) 0.157(17) 0.096(11) -0.047(11) 0.027(10) 0.004(11)
C45 0.138(14) 0.214(17) 0.132(15) -0.040(14) 0.006(10) -0.008(11)
C46 0.170(18) 0.22(3) 0.142(13) -0.010(13) -0.002(14) -0.022(14)
O47 0.32(2) 0.32(2) 0.32(2) -0.073(17) -0.073(17) -0.073(17)
C48 0.31(3) 0.25(4) 0.29(3) -0.04(3) -0.06(2) -0.03(2)
C49 0.21(3) 0.29(3) 0.29(3) -0.05(2) -0.06(2) -0.04(2)
O50 0.294(19) 0.294(19) 0.294(19) -0.043(17) -0.043(17) -0.043(17)
_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 C3 1.250(9) . ?
N1 C4 1.486(9) . ?
N2 C5 1.455(8) . ?
N2 C7 1.260(7) . ?
N3 C14 1.262(8) . ?
N3 C15 1.440(8) . ?
N4 C16 1.457(7) . ?
N4 C18 1.258(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.379(9) . ?
C1 C2 1.431(9) 10_646 ?
C2 C1 1.431(9) 7_665 ?
C2 C3 1.446(10) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.494(11) . ?
C4 C6B 1.46(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.508(12) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6B H6BA 0.9800 . ?
C6B H6BB 0.9800 . ?
C6B H6BC 0.9800 . ?
C7 H7 0.9500 . ?
C7 C8 1.472(9) . ?
C8 C9 1.396(8) . ?
C8 C13 1.368(8) . ?
C9 H9 0.9500 . ?
C9 C0AA 1.354(8) . ?
C0AA C1AA 1.395(8) . ?
C0AA C18 1.480(8) 10_646 ?
C1AA H1AA 0.9500 . ?
C1AA C12 1.395(8) . ?
C12 C13 1.396(8) . ?
C12 C14 1.477(8) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.521(9) . ?
C15 C17B 1.43(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.497(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C18 C0AA 1.480(8) 7_665 ?
C18 H18 0.9500 . ?
N5 C21 1.267(8) . ?
N5 C22 1.461(8) . ?
N6 C23 1.453(7) . ?
N6 C25 1.240(8) . ?
N7 C32 1.260(8) . ?
N7 C33 1.462(9) . ?
N8 C34 1.485(8) . ?
N8 C36 1.252(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.419(9) 12_664 ?
C19 C20 1.394(8) . ?
C20 C19 1.419(9) 6_566 ?
C20 C21 1.457(8) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.502(9) . ?
C22 C24 1.538(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24B 1.28(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25 H25 0.9500 . ?
C25 C26 1.475(9) . ?
C26 C27 1.377(9) . ?
C26 C31 1.386(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.430(9) . ?
C28 C29 1.383(9) . ?
C28 C36 1.437(9) 6_566 ?
C29 H29 0.9500 . ?
C29 C30 1.394(9) . ?
C30 C31 1.404(9) . ?
C30 C32 1.449(9) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.498(10) . ?
C33 C35 1.546(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35B 1.49(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35B H35D 0.9800 . ?
C35B H35E 0.9800 . ?
C35B H35F 0.9800 . ?
C36 C28 1.437(9) 12_664 ?
C36 H36 0.9500 . ?
O1 C37 1.450(13) . ?
O1 C40 1.435(14) . ?
O2 C38 1.476(12) . ?
O2 C39 1.413(12) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.493(15) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.520(14) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
O3 O3 0.88(2) 7_665 ?
O3 O3 0.88(2) 10_646 ?
O3 C41 1.20(4) . ?
O3 C41 1.41(4) 7_665 ?
O3 C41 1.881(19) 10_646 ?
O4 O4 1.19(3) 10_646 ?
O4 O4 1.19(3) 7_665 ?
O4 C41 1.87(3) 7_665 ?
O4 C42 1.66(3) 7_665 ?
O4 C42 1.28(3) . ?
C41 O3 1.881(19) 7_665 ?
C41 O3 1.41(4) 10_646 ?
C41 O4 1.87(3) 10_646 ?
C41 C42 1.64(2) 10_646 ?
C41 C42 1.50(2) . ?
C42 O4 1.66(3) 10_646 ?
C42 C41 1.64(2) 7_665 ?
O43 O44 1.70(3) 6_566 ?
O43 O44 1.09(3) . ?
O43 C45 1.47(3) . ?
O43 C46 1.33(3) . ?
O44 O43 1.70(3) 12_664 ?
O44 C45 1.91(3) . ?
O44 C45 1.45(3) 12_664 ?
O44 C46 1.43(4) . ?
C45 O44 1.45(3) 6_566 ?
C45 C45 1.61(4) 12_664 ?
C45 C45 1.61(4) 6_566 ?
C46 C46 1.25(4) 12_664 ?
C46 C46 1.25(4) 6_566 ?
O47 C48 1.53(5) 9 ?
O47 C48 1.53(5) 5 ?
O47 C48 1.53(5) . ?
C48 C49 1.42(7) . ?
C48 C49 1.79(7) 5 ?
C49 C48 1.79(7) 9 ?
C49 O50 1.57(5) . ?
O50 C49 1.57(5) 9 ?
O50 C49 1.57(5) 5 ?
C10 C10 1.72(8) 11_556 ?
C10 C10 1.72(8) 8_645 ?
C10 O12 1.60(8) . ?
C10 O13 1.17(8) . ?
C10 O13 1.81(8) 11_556 ?
C11 C11 1.02(11) 11_556 ?
C11 C11 1.02(11) 8_645 ?
C11 O12 1.61(8) 11_556 ?
C11 O13 1.65(12) 8_645 ?
C11 O13 1.52(10) 11_556 ?
O12 C11 1.61(8) 8_645 ?
O12 O13 1.53(9) 11_556 ?
O12 O13 1.70(10) . ?
O13 C10 1.81(8) 8_645 ?
O13 C11 1.65(12) 11_556 ?
O13 C11 1.52(10) 8_645 ?
O13 O12 1.53(9) 8_645 ?
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
C3 N1 C4 117.0(6) . . ?
C7 N2 C5 117.2(5) . . ?
C14 N3 C15 118.1(5) . . ?
C18 N4 C16 116.3(5) . . ?
C2 C1 H1 118.6 10_646 . ?
C2 C1 H1 118.6 . . ?
C2 C1 C2 122.8(7) . 10_646 ?
C1 C2 C1 117.2(7) . 7_665 ?
C1 C2 C3 120.8(6) . . ?
C1 C2 C3 122.0(6) 7_665 . ?
N1 C3 C2 123.5(6) . . ?
N1 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 C5 110.7(5) . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C6B C4 N1 119.0(13) . . ?
C6B C4 C5 99.2(13) . . ?
N2 C5 C4 110.5(6) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 C6 112.0(7) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 C6 105.1(7) . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C6B H6BA 109.5 . . ?
C4 C6B H6BB 109.5 . . ?
C4 C6B H6BC 109.5 . . ?
H6BA C6B H6BB 109.5 . . ?
H6BA C6B H6BC 109.5 . . ?
H6BB C6B H6BC 109.5 . . ?
N2 C7 H7 118.9 . . ?
N2 C7 C8 122.2(6) . . ?
C8 C7 H7 118.9 . . ?
C9 C8 C7 120.7(5) . . ?
C13 C8 C7 120.3(5) . . ?
C13 C8 C9 119.0(5) . . ?
C8 C9 H9 119.8 . . ?
C0AA C9 C8 120.4(5) . . ?
C0AA C9 H9 119.8 . . ?
C9 C0AA C1AA 121.2(5) . . ?
C9 C0AA C18 118.7(5) . 10_646 ?
C1AA C0AA C18 120.2(5) . 10_646 ?
C0AA C1AA H1AA 120.4 . . ?
C0AA C1AA C12 119.1(5) . . ?
C12 C1AA H1AA 120.4 . . ?
C1AA C12 C13 118.7(5) . . ?
C1AA C12 C14 119.0(5) . . ?
C13 C12 C14 122.2(5) . . ?
C8 C13 C12 121.6(5) . . ?
C8 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
N3 C14 C12 123.5(6) . . ?
N3 C14 H14 118.3 . . ?
C12 C14 H14 118.3 . . ?
N3 C15 H15A 109.6 . . ?
N3 C15 H15B 109.6 . . ?
N3 C15 C16 110.5(5) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C17B C15 N3 116(3) . . ?
C17B C15 C16 125(3) . . ?
N4 C16 C15 110.7(5) . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
N4 C16 C17 109.4(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C17 C16 C15 111.6(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C17B H17D 109.5 . . ?
C15 C17B H17E 109.5 . . ?
C15 C17B H17F 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N4 C18 C0AA 124.3(5) . 7_665 ?
N4 C18 H18 117.8 . . ?
C0AA C18 H18 117.8 7_665 . ?
C21 N5 C22 118.2(5) . . ?
C25 N6 C23 117.9(5) . . ?
C32 N7 C33 118.1(6) . . ?
C36 N8 C34 117.1(6) . . ?
C20 C19 H19 119.7 12_664 . ?
C20 C19 H19 119.7 . . ?
C20 C19 C20 120.6(6) . 12_664 ?
C19 C20 C19 119.4(6) . 6_566 ?
C19 C20 C21 119.9(5) . . ?
C19 C20 C21 120.7(5) 6_566 . ?
N5 C21 C20 122.6(6) . . ?
N5 C21 H21 118.7 . . ?
C20 C21 H21 118.7 . . ?
N5 C22 H22A 109.9 . . ?
N5 C22 H22B 109.9 . . ?
N5 C22 C23 109.1(5) . . ?
N5 C22 C24 109.8(5) . . ?
H22A C22 H22B 108.3 . . ?
C23 C22 H22A 109.9 . . ?
C23 C22 H22B 109.9 . . ?
C23 C22 C24 109.1(5) . . ?
N6 C23 C22 110.3(5) . . ?
N6 C23 H23A 109.6 . . ?
N6 C23 H23B 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C24B C23 N6 132(2) . . ?
C24B C23 C22 89(2) . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C24B H24D 109.5 . . ?
C23 C24B H24E 109.5 . . ?
C23 C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N6 C25 H25 119.1 . . ?
N6 C25 C26 121.8(6) . . ?
C26 C25 H25 119.1 . . ?
C27 C26 C25 120.8(6) . . ?
C27 C26 C31 119.3(6) . . ?
C31 C26 C25 119.9(6) . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 121.0(6) . . ?
C28 C27 H27 119.5 . . ?
C27 C28 C36 122.2(6) . 6_566 ?
C29 C28 C27 118.1(6) . . ?
C29 C28 C36 119.8(6) . 6_566 ?
C28 C29 H29 119.1 . . ?
C28 C29 C30 121.8(6) . . ?
C30 C29 H29 119.1 . . ?
C29 C30 C31 118.4(6) . . ?
C29 C30 C32 122.6(6) . . ?
C31 C30 C32 119.0(6) . . ?
C26 C31 C30 121.4(6) . . ?
C26 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
N7 C32 C30 124.0(6) . . ?
N7 C32 H32 118.0 . . ?
C30 C32 H32 118.0 . . ?
N7 C33 H33A 109.8 . . ?
N7 C33 H33B 109.8 . . ?
N7 C33 C34 109.6(6) . . ?
N7 C33 C35 108.4(6) . . ?
H33A C33 H33B 108.2 . . ?
C34 C33 H33A 109.8 . . ?
C34 C33 H33B 109.8 . . ?
C34 C33 C35 107.5(6) . . ?
N8 C34 C33 113.0(5) . . ?
N8 C34 H34A 109.0 . . ?
N8 C34 H34B 109.0 . . ?
N8 C34 C35B 103.2(16) . . ?
C33 C34 H34A 109.0 . . ?
C33 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
C35B C34 C33 100.5(15) . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C35B H35D 109.5 . . ?
C34 C35B H35E 109.5 . . ?
C34 C35B H35F 109.5 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
N8 C36 C28 123.7(6) . 12_664 ?
N8 C36 H36 118.1 . . ?
C28 C36 H36 118.1 12_664 . ?
C40 O1 C37 109.9(8) . . ?
C39 O2 C38 109.5(8) . . ?
O1 C37 H37A 109.7 . . ?
O1 C37 H37B 109.7 . . ?
O1 C37 C38 109.8(8) . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 H37A 109.7 . . ?
C38 C37 H37B 109.7 . . ?
O2 C38 C37 111.3(8) . . ?
O2 C38 H38A 109.4 . . ?
O2 C38 H38B 109.4 . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
O2 C39 H39A 109.4 . . ?
O2 C39 H39B 109.4 . . ?
O2 C39 C40 111.2(8) . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
O1 C40 C39 110.9(9) . . ?
O1 C40 H40A 109.5 . . ?
O1 C40 H40B 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 108.0 . . ?
O3 O3 O3 59.994(8) 7_665 10_646 ?
O3 O3 C41 84(5) 10_646 . ?
O3 O3 C41 58(4) 7_665 7_665 ?
O3 O3 C41 108(4) 10_646 7_665 ?
O3 O3 C41 45(3) 7_665 10_646 ?
O3 O3 C41 128(3) 7_665 . ?
O3 O3 C41 30(2) 10_646 10_646 ?
C41 O3 C41 109.5(17) . 7_665 ?
C41 O3 C41 84.6(17) . 10_646 ?
C41 O3 C41 79.5(9) 10_646 7_665 ?
O4 O4 O4 60.001(7) 7_665 10_646 ?
O4 O4 C41 109.8(7) 10_646 7_665 ?
O4 O4 C41 93.4(17) 7_665 7_665 ?
O4 O4 C42 99(2) 10_646 7_665 ?
O4 O4 C42 50(2) 7_665 7_665 ?
O4 O4 C42 125.9(18) 7_665 . ?
O4 O4 C42 85(3) 10_646 . ?
C42 O4 C41 59.4(13) . 7_665 ?
C42 O4 C41 49.8(10) 7_665 7_665 ?
C42 O4 C42 106.0(19) . 7_665 ?
O3 C41 O3 21.6(12) . 7_665 ?
O3 C41 O3 38.5(14) . 10_646 ?
O3 C41 O3 26.4(8) 7_665 10_646 ?
O3 C41 C42 84.8(17) . . ?
O3 C41 C42 105.6(13) . 10_646 ?
O3 C41 C42 84.3(13) 7_665 10_646 ?
C42 C41 O3 109.2(15) . 10_646 ?
C42 C41 O3 73.5(12) 10_646 10_646 ?
C42 C41 O3 84.1(14) . 7_665 ?
C42 C41 O4 57.9(13) . 10_646 ?
C42 C41 O4 41.9(12) 10_646 10_646 ?
C42 C41 C42 97.0(15) . 10_646 ?
O4 C42 O4 45.4(17) . 10_646 ?
O4 C42 C41 110.0(15) . . ?
O4 C42 C41 78.7(16) . 7_665 ?
C41 C42 O4 72.3(12) . 10_646 ?
C41 C42 O4 100.1(14) 7_665 10_646 ?
C41 C42 C41 85.4(14) . 7_665 ?
O44 O43 O44 120(3) . 6_566 ?
O44 O43 C45 96(3) . . ?
O44 O43 C46 72(3) . . ?
C45 O43 O44 53.8(14) . 6_566 ?
C46 O43 O44 82(2) . 6_566 ?
C46 O43 C45 121(2) . . ?
O43 O44 O43 119(3) . 12_664 ?
O43 O44 C45 90.8(17) 12_664 . ?
O43 O44 C45 105(3) . 12_664 ?
O43 O44 C45 50(2) . . ?
O43 O44 C46 62(2) . . ?
C45 O44 O43 55.1(15) 12_664 12_664 ?
C45 O44 C45 55.0(18) 12_664 . ?
C46 O44 O43 79(2) . 12_664 ?
C46 O44 C45 118.6(18) . 12_664 ?
C46 O44 C45 92.2(19) . . ?
O43 C45 O44 34.4(13) . . ?
O43 C45 C45 113.6(12) . 6_566 ?
O43 C45 C45 81.8(18) . 12_664 ?
O44 C45 O43 71.1(17) 6_566 . ?
O44 C45 O44 92(2) 6_566 . ?
O44 C45 C45 113.7(13) 6_566 12_664 ?
O44 C45 C45 77.4(17) 6_566 6_566 ?
C45 C45 O44 92.8(11) 6_566 . ?
C45 C45 O44 47.6(13) 12_664 . ?
C45 C45 C45 60.001(4) 12_664 6_566 ?
O43 C46 O44 46.1(15) . . ?
C46 C46 O43 124.3(16) 12_664 . ?
C46 C46 O43 102(3) 6_566 . ?
C46 C46 O44 97(3) 12_664 . ?
C46 C46 O44 122.7(13) 6_566 . ?
C46 C46 C46 59.998(6) 6_566 12_664 ?
C48 O47 C48 92(4) 9 5 ?
C48 O47 C48 92(4) . 5 ?
C48 O47 C48 92(4) . 9 ?
O47 C48 C49 84(4) . 5 ?
C49 C48 O47 98(5) . . ?
C49 C48 C49 80(5) . 5 ?
C48 C49 C48 85(5) . 9 ?
C48 C49 O50 106(5) . . ?
O50 C49 C48 91(3) . 9 ?
C49 O50 C49 83(3) 9 . ?
C49 O50 C49 83(3) 5 . ?
C49 O50 C49 83(3) 9 5 ?
C10 C10 C10 59.999(7) 11_556 8_645 ?
C10 C10 O13 39(3) 11_556 11_556 ?
C10 C10 O13 83(3) 8_645 11_556 ?
O12 C10 C10 127(3) . 8_645 ?
O12 C10 C10 90(4) . 11_556 ?
O12 C10 O13 53(3) . 11_556 ?
O13 C10 C10 107(4) . 11_556 ?
O13 C10 C10 75(5) . 8_645 ?
O13 C10 O12 74(5) . . ?
O13 C10 O13 86(6) . 11_556 ?
C11 C11 C11 60.01(3) 8_645 11_556 ?
C11 C11 O12 140(5) 8_645 11_556 ?
C11 C11 O12 120(10) 11_556 11_556 ?
C11 C11 O13 64(9) 11_556 8_645 ?
C11 C11 O13 114(6) 11_556 11_556 ?
C11 C11 O13 105(8) 8_645 8_645 ?
C11 C11 O13 78(10) 8_645 11_556 ?
O12 C11 O13 56(4) 11_556 8_645 ?
O13 C11 O12 66(4) 11_556 11_556 ?
O13 C11 O13 82(5) 11_556 8_645 ?
C10 O12 C11 87(4) . 8_645 ?
C10 O12 O13 41(3) . . ?
C11 O12 O13 55(5) 8_645 . ?
O13 O12 C10 71(4) 11_556 . ?
O13 O12 C11 63(5) 11_556 8_645 ?
O13 O12 O13 80(6) 11_556 . ?
C10 O13 C10 66(5) . 8_645 ?
C10 O13 C11 124(7) . 11_556 ?
C10 O13 C11 110(7) . 8_645 ?
C10 O13 O12 121(7) . 8_645 ?
C10 O13 O12 65(5) . . ?
C11 O13 C10 79(4) 11_556 8_645 ?
C11 O13 C10 104(5) 8_645 8_645 ?
C11 O13 C11 37(5) 8_645 11_556 ?
C11 O13 O12 60(4) 8_645 . ?
C11 O13 O12 98(6) 8_645 8_645 ?
C11 O13 O12 96(5) 11_556 . ?
O12 O13 C10 116(5) . 8_645 ?
O12 O13 C10 57(3) 8_645 8_645 ?
O12 O13 C11 61(4) 8_645 11_556 ?
O12 O13 O12 155(6) 8_645 . ?
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
N1 C4 C5 N2 67.4(7) . . . . ?
N1 C4 C5 C6 -171.5(7) . . . . ?
N2 C7 C8 C9 5.5(9) . . . . ?
N2 C7 C8 C13 -172.4(6) . . . . ?
N3 C15 C16 N4 66.1(7) . . . . ?
N3 C15 C16 C17 -171.8(5) . . . . ?
C1 C2 C3 N1 -175.4(6) . . . . ?
C1 C2 C3 N1 3.7(9) 7_665 . . . ?
C2 C1 C2 C1 -1.1(12) 10_646 . . 7_665 ?
C2 C1 C2 C3 178.0(4) 10_646 . . . ?
C3 N1 C4 C5 -132.0(6) . . . . ?
C3 N1 C4 C6B 114.1(15) . . . . ?
C4 N1 C3 C2 -179.9(5) . . . . ?
C5 N2 C7 C8 -178.4(5) . . . . ?
C6B C4 C5 N2 -166.7(13) . . . . ?
C7 N2 C5 C4 -132.9(6) . . . . ?
C7 N2 C5 C6 110.2(8) . . . . ?
C7 C8 C9 C0AA -178.8(5) . . . . ?
C7 C8 C13 C12 178.5(5) . . . . ?
C8 C9 C0AA C1AA 0.5(9) . . . . ?
C8 C9 C0AA C18 -179.4(5) . . . 10_646 ?
C9 C8 C13 C12 0.6(9) . . . . ?
C9 C0AA C1AA C12 0.2(9) . . . . ?
C0AA C1AA C12 C13 -0.5(8) . . . . ?
C0AA C1AA C12 C14 -179.7(5) . . . . ?
C1AA C12 C13 C8 0.1(9) . . . . ?
C1AA C12 C14 N3 178.3(5) . . . . ?
C13 C8 C9 C0AA -0.9(8) . . . . ?
C13 C12 C14 N3 -0.9(9) . . . . ?
C14 N3 C15 C16 -121.9(6) . . . . ?
C14 N3 C15 C17B 89(3) . . . . ?
C14 C12 C13 C8 179.3(5) . . . . ?
C15 N3 C14 C12 -178.1(5) . . . . ?
C16 N4 C18 C0AA -176.8(5) . . . 7_665 ?
C17B C15 C16 N4 -148(3) . . . . ?
C18 N4 C16 C15 -129.8(6) . . . . ?
C18 N4 C16 C17 106.8(6) . . . . ?
C18 C0AA C1AA C12 -179.8(5) 10_646 . . . ?
N5 C22 C23 N6 65.6(6) . . . . ?
N5 C22 C23 C24B -159(2) . . . . ?
N6 C25 C26 C27 -177.9(7) . . . . ?
N6 C25 C26 C31 3.7(10) . . . . ?
N7 C33 C34 N8 64.3(7) . . . . ?
N7 C33 C34 C35B 173.6(16) . . . . ?
C19 C20 C21 N5 -6.3(8) 6_566 . . . ?
C19 C20 C21 N5 170.9(5) . . . . ?
C20 C19 C20 C19 -1.7(10) 12_664 . . 6_566 ?
C20 C19 C20 C21 -179.0(4) 12_664 . . . ?
C21 N5 C22 C23 -121.5(6) . . . . ?
C21 N5 C22 C24 119.0(7) . . . . ?
C22 N5 C21 C20 180.0(5) . . . . ?
C23 N6 C25 C26 -177.8(6) . . . . ?
C24 C22 C23 N6 -174.4(6) . . . . ?
C25 N6 C23 C22 -129.4(6) . . . . ?
C25 N6 C23 C24B 123(3) . . . . ?
C25 C26 C27 C28 179.9(6) . . . . ?
C25 C26 C31 C30 180.0(6) . . . . ?
C26 C27 C28 C29 0.9(10) . . . . ?
C26 C27 C28 C36 -178.9(7) . . . 6_566 ?
C27 C26 C31 C30 1.6(11) . . . . ?
C27 C28 C29 C30 0.1(11) . . . . ?
C28 C29 C30 C31 -0.2(11) . . . . ?
C28 C29 C30 C32 178.7(7) . . . . ?
C29 C30 C31 C26 -0.7(11) . . . . ?
C29 C30 C32 N7 2.6(12) . . . . ?
C31 C26 C27 C28 -1.7(11) . . . . ?
C31 C30 C32 N7 -178.4(7) . . . . ?
C32 N7 C33 C34 -126.1(7) . . . . ?
C32 N7 C33 C35 116.8(7) . . . . ?
C32 C30 C31 C26 -179.6(6) . . . . ?
C33 N7 C32 C30 -177.6(6) . . . . ?
C34 N8 C36 C28 -178.4(6) . . . 12_664 ?
C35 C33 C34 N8 -178.1(6) . . . . ?
C36 N8 C34 C33 -123.4(7) . . . . ?
C36 N8 C34 C35B 128.9(16) . . . . ?
C36 C28 C29 C30 179.9(7) 6_566 . . . ?
O1 C37 C38 O2 58.0(10) . . . . ?
O2 C39 C40 O1 -57.8(12) . . . . ?
C37 O1 C40 C39 57.6(10) . . . . ?
C38 O2 C39 C40 56.1(11) . . . . ?
C39 O2 C38 C37 -57.3(9) . . . . ?
C40 O1 C37 C38 -58.1(10) . . . . ?
O3 O3 C41 O3 -43(3) 10_646 . . 7_665 ?
O3 O3 C41 O3 43(3) 7_665 . . 10_646 ?
O3 O3 C41 C42 9(7) 7_665 . . 10_646 ?
O3 O3 C41 C42 -34(3) 10_646 . . 10_646 ?
O3 O3 C41 C42 -130(3) 10_646 . . . ?
O3 O3 C41 C42 -87(6) 7_665 . . . ?
O3 C41 C42 C41 -3.2(13) 7_665 . . 7_665 ?
O3 C41 C42 C41 18.5(12) . . . 7_665 ?
O3 C41 C42 C41 -11.7(16) 10_646 . . 7_665 ?
O4 O4 C42 O4 -47(2) 7_665 . . 10_646 ?
O4 O4 C42 C41 117(2) 10_646 . . 7_665 ?
O4 O4 C42 C41 -11(5) 7_665 . . . ?
O4 O4 C42 C41 36(3) 10_646 . . . ?
O4 O4 C42 C41 70(4) 7_665 . . 7_665 ?
O4 C41 C42 O4 -26(2) 10_646 . . . ?
O4 C41 C42 C41 -102.1(13) 10_646 . . 7_665 ?
C41 O3 C41 O3 64(5) 7_665 . . 7_665 ?
C41 O3 C41 O3 107(2) 7_665 . . 10_646 ?
C41 O3 C41 O3 30(2) 10_646 . . 10_646 ?
C41 O3 C41 O3 -13(5) 10_646 . . 7_665 ?
C41 O3 C41 C42 -100.0(10) 10_646 . . . ?
C41 O3 C41 C42 -4.1(16) 10_646 . . 10_646 ?
C41 O3 C41 C42 72.8(16) 7_665 . . 10_646 ?
C41 O3 C41 C42 -23.1(15) 7_665 . . . ?
C41 O4 C42 O4 -117(2) 7_665 . . 10_646 ?
C41 O4 C42 C41 -80.8(16) 7_665 . . . ?
C42 O4 C42 O4 -98.2(15) 7_665 . . 10_646 ?
C42 O4 C42 C41 -62.4(17) 7_665 . . . ?
C42 O4 C42 C41 18.4(12) 7_665 . . 7_665 ?
C42 C41 C42 O4 -10(2) 10_646 . . . ?
C42 C41 C42 O4 15.5(12) 10_646 . . 10_646 ?
C42 C41 C42 C41 -86.6(12) 10_646 . . 7_665 ?
O43 O44 C46 O43 132(3) 12_664 . . . ?
O43 O44 C46 C46 -132(4) . . . 12_664 ?
O43 O44 C46 C46 -1(3) 12_664 . . 12_664 ?
O43 O44 C46 C46 -74(6) . . . 6_566 ?
O43 O44 C46 C46 58(5) 12_664 . . 6_566 ?
O44 O43 O44 O43 12(6) 6_566 . . 12_664 ?
O44 O43 O44 C45 -51(3) 6_566 . . . ?
O44 O43 O44 C45 -45(4) 6_566 . . 12_664 ?
O44 O43 O44 C46 69(3) 6_566 . . . ?
O44 O43 C45 O44 123(3) 6_566 . . . ?
O44 O43 C45 O44 -123(3) . . . 6_566 ?
O44 O43 C45 C45 -5(2) . . . 12_664 ?
O44 O43 C45 C45 -57(3) . . . 6_566 ?
O44 O43 C45 C45 118.5(17) 6_566 . . 12_664 ?
O44 O43 C45 C45 66(2) 6_566 . . 6_566 ?
O44 O43 C46 O44 -125(3) 6_566 . . . ?
O44 O43 C46 C46 -63(5) 6_566 . . 12_664 ?
O44 O43 C46 C46 -1(3) 6_566 . . 6_566 ?
O44 O43 C46 C46 63(6) . . . 12_664 ?
O44 O43 C46 C46 124(4) . . . 6_566 ?
C45 O43 O44 O43 63(4) . . . 12_664 ?
C45 O43 O44 C45 6(2) . . . 12_664 ?
C45 O43 O44 C46 120.6(19) . . . . ?
C45 O43 C46 O44 -86(3) . . . . ?
C45 O43 C46 C46 38(5) . . . 6_566 ?
C45 O43 C46 C46 -23(7) . . . 12_664 ?
C45 O44 C46 O43 92(3) 12_664 . . . ?
C45 O44 C46 O43 41.2(18) . . . . ?
C45 O44 C46 C46 18(6) 12_664 . . 6_566 ?
C45 O44 C46 C46 -40(4) 12_664 . . 12_664 ?
C45 O44 C46 C46 -91(3) . . . 12_664 ?
C45 O44 C46 C46 -33(5) . . . 6_566 ?
C46 O43 O44 O43 -57(3) . . . 12_664 ?
C46 O43 O44 C45 -115(2) . . . 12_664 ?
C46 O43 O44 C45 -120.6(19) . . . . ?
C46 O43 C45 O44 73(3) . . . . ?
C46 O43 C45 O44 -51(3) . . . 6_566 ?
C46 O43 C45 C45 68(3) . . . 12_664 ?
C46 O43 C45 C45 15(4) . . . 6_566 ?
O47 C48 C49 C48 6(4) . . . 9 ?
O47 C48 C49 O50 -83(4) . . . . ?
C48 O47 C48 C49 85(3) 5 . . . ?
C48 O47 C48 C49 6(3) 5 . . 5 ?
C48 O47 C48 C49 -86(2) 9 . . 5 ?
C48 O47 C48 C49 -7(4) 9 . . . ?
C48 C49 O50 C49 85(3) . . . 9 ?
C48 C49 O50 C49 1(4) . . . 5 ?
C48 C49 O50 C49 -84(2) 9 . . 5 ?
C48 C49 O50 C49 -1(3) 9 . . 9 ?
C49 C48 C49 C48 89(3) 5 . . 9 ?
C49 C48 C49 O50 -1(4) 5 . . . ?
C10 C10 O12 C11 -21(7) 8_645 . . 8_645 ?
C10 C10 O12 C11 -73(5) 11_556 . . 8_645 ?
C10 C10 O12 O13 -56(6) 8_645 . . . ?
C10 C10 O12 O13 41(7) 8_645 . . 11_556 ?
C10 C10 O12 O13 -10(4) 11_556 . . 11_556 ?
C10 C10 O12 O13 -108(4) 11_556 . . . ?
C10 C10 O13 C10 -51(2) 11_556 . . 8_645 ?
C10 C10 O13 C11 6(8) 11_556 . . 11_556 ?
C10 C10 O13 C11 45(7) 11_556 . . 8_645 ?
C10 C10 O13 C11 97(6) 8_645 . . 8_645 ?
C10 C10 O13 C11 57(6) 8_645 . . 11_556 ?
C10 C10 O13 O12 -67(8) 11_556 . . 8_645 ?
C10 C10 O13 O12 85(5) 11_556 . . . ?
C10 C10 O13 O12 -16(7) 8_645 . . 8_645 ?
C10 C10 O13 O12 136(4) 8_645 . . . ?
C10 O12 O13 C10 44(5) . . . 8_645 ?
C10 O12 O13 C11 125(7) . . . 11_556 ?
C10 O12 O13 C11 136(7) . . . 8_645 ?
C10 O12 O13 O12 110(16) . . . 8_645 ?
C11 O12 O13 C10 -91(6) 8_645 . . 8_645 ?
C11 O12 O13 C10 -136(7) 8_645 . . . ?
C11 O12 O13 C11 -10(7) 8_645 . . 11_556 ?
C11 O12 O13 O12 -26(15) 8_645 . . 8_645 ?
O12 C10 O13 C10 -136(4) . . . 8_645 ?
O12 C10 O13 C11 -40(5) . . . 8_645 ?
O12 C10 O13 C11 -79(6) . . . 11_556 ?
O12 C10 O13 O12 -153(7) . . . 8_645 ?
O13 C10 O12 C11 35(6) . . . 8_645 ?
O13 C10 O12 C11 -63(6) 11_556 . . 8_645 ?
O13 C10 O12 O13 -98(7) 11_556 . . . ?
O13 C10 O12 O13 98(7) . . . 11_556 ?
O13 C10 O13 C10 -84(3) 11_556 . . 8_645 ?
O13 C10 O13 C11 -27(6) 11_556 . . 11_556 ?
O13 C10 O13 C11 12(5) 11_556 . . 8_645 ?
O13 C10 O13 O12 52(3) 11_556 . . . ?
O13 C10 O13 O12 -100(6) 11_556 . . 8_645 ?
O13 O12 O13 C10 -72(6) 11_556 . . . ?
O13 O12 O13 C10 -27(7) 11_556 . . 8_645 ?
O13 O12 O13 C11 54(6) 11_556 . . 11_556 ?
O13 O12 O13 C11 64(6) 11_556 . . 8_645 ?
O13 O12 O13 O12 38(18) 11_556 . . 8_645 ?
_shelx_res_file
;
TITL C54H60N12 *2.5C4H8O2 *4.75H2O in P2(1)3
CELL 0.6889 24.3179 24.3179 24.3179 90 90 90
ZERR 4 0.0022 0.0022 0.0022 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SYMM +Z,+X,+Y
SYMM 0.5+Z,0.5-X,-Y
SYMM 0.5-Z,-X,0.5+Y
SYMM -Z,0.5+X,0.5-Y
SYMM +Y,+Z,+X
SYMM -Y,0.5+Z,0.5-X
SYMM 0.5+Y,0.5-Z,-X
SYMM 0.5-Y,-Z,0.5+X
SFAC C H N O
DISP C 0.003 0.002 10.64
DISP H -0 0 0.67
DISP N 0.006 0.003 18.02
DISP O 0.01 0.006 29.59
UNIT 520 642 96 61
RIGU O50 O47 C48 C48 C48 C49 C49 C49
RIGU O44 O43 C45 C46
RIGU C11 C10 O12 O13
RIGU C42 O3 C41 O4
L.S. 50
PLAN 20
SIZE 0.15 0.1 0.05
TEMP -173.15
FREE C22 C24B
BOND $H
HTAB
MORE -1
CONF
fmap 2
acta 45
SHEL 20 0.84
OMIT 1 1 1
OMIT -1 1 1
OMIT 1 0 2
REM
REM
REM
WGHT 0.155300 0.065000
FVAR 0.05182 0.67304 0.79238 0.78424 0.72863
N1 3 0.672533 0.358913 0.658530 11.00000 0.06900 0.06542 =
0.07995 -0.00303 -0.00159 0.02041
N2 3 0.697131 0.324983 0.544475 11.00000 0.05293 0.06523 =
0.06988 0.00348 -0.00097 -0.00057
N3 3 0.951508 0.266987 0.496211 11.00000 0.05058 0.06481 =
0.05042 0.00180 0.00404 -0.00539
N4 3 1.030785 0.237839 0.582639 11.00000 0.04744 0.05732 =
0.05746 0.01362 0.00656 -0.00766
C1 1 0.668971 0.257061 0.766437 11.00000 0.05076 0.07201 =
0.06832 -0.00483 0.00581 0.01152
AFIX 43
H1 2 0.637075 0.237984 0.754400 11.00000 -1.20000
AFIX 0
C2 1 0.685968 0.302658 0.737282 11.00000 0.05767 0.06893 =
0.06793 -0.00566 0.00774 0.01534
C3 1 0.656981 0.320083 0.688378 11.00000 0.05326 0.05973 =
0.08346 -0.00889 0.01088 0.01381
AFIX 43
H3 2 0.624384 0.300999 0.678410 11.00000 -1.20000
AFIX 0
C4 1 0.638123 0.371846 0.609725 11.00000 0.06295 0.06659 =
0.09758 0.00000 -0.00028 0.02165
PART 1
AFIX 23
H4A 2 0.617780 0.406505 0.616229 21.00000 -1.20000
H4B 2 0.610913 0.342110 0.604006 21.00000 -1.20000
AFIX 0
PART 0
C5 1 0.673031 0.377656 0.559506 11.00000 0.06195 0.05762 =
0.09516 0.00812 -0.01089 0.01347
PART 2
AFIX 23
H5A 2 0.650345 0.391541 0.528685 -21.00000 -1.20000
H5B 2 0.702660 0.404667 0.566568 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C6 1 0.634792 0.399117 0.515629 21.00000 0.07628 0.08365 =
0.09105 0.01504 -0.01428 0.01964
AFIX 137
H6A 2 0.656076 0.408705 0.482779 21.00000 -1.50000
H6B 2 0.615699 0.431868 0.529298 21.00000 -1.50000
H6C 2 0.607760 0.370720 0.506306 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C6B 1 0.609263 0.424504 0.607562 -21.00000 0.10979
AFIX 137
H6BA 2 0.572825 0.420550 0.624315 -21.00000 -1.50000
H6BB 2 0.605213 0.436035 0.569161 -21.00000 -1.50000
H6BC 2 0.630396 0.452244 0.627760 -21.00000 -1.50000
AFIX 0
PART 0
C7 1 0.747783 0.324402 0.533504 11.00000 0.04915 0.05999 =
0.06869 0.01043 -0.00497 -0.00473
AFIX 43
H7 2 0.768097 0.357646 0.536389 11.00000 -1.20000
AFIX 0
C8 1 0.776537 0.273959 0.516370 11.00000 0.05469 0.04565 =
0.05603 0.00237 -0.00458 -0.00734
C9 1 0.747435 0.225336 0.507115 11.00000 0.04366 0.06012 =
0.05519 0.00077 -0.00496 -0.00171
AFIX 43
H9 2 0.708587 0.224887 0.511210 11.00000 -1.20000
AFIX 0
C0AA 1 0.774242 0.178809 0.492335 11.00000 0.04763 0.06028 =
0.04965 -0.00047 -0.00531 -0.01492
C1AA 1 0.831299 0.178022 0.486394 11.00000 0.05632 0.05610 =
0.05156 -0.00218 0.00277 -0.00465
AFIX 43
H1AA 2 0.849655 0.145179 0.475880 11.00000 -1.20000
AFIX 0
C12 1 0.861037 0.226114 0.496100 11.00000 0.04999 0.05834 =
0.04958 -0.00339 -0.00326 -0.00997
C13 1 0.832531 0.273654 0.511029 11.00000 0.05500 0.05021 =
0.05762 0.00098 -0.00228 -0.01094
AFIX 43
H13 2 0.852496 0.306576 0.517636 11.00000 -1.20000
AFIX 0
C14 1 0.921418 0.225252 0.489559 11.00000 0.05097 0.07051 =
0.04696 0.00261 0.00648 -0.00679
AFIX 43
H14 2 0.938495 0.191491 0.479829 11.00000 -1.20000
AFIX 0
C15 1 1.009700 0.261207 0.486940 11.00000 0.04470 0.07870 =
0.05434 0.01189 0.00530 -0.00888
PART 1
AFIX 23
H15A 2 1.021035 0.285224 0.456085 31.00000 -1.20000
H15B 2 1.018118 0.222701 0.476754 31.00000 -1.20000
AFIX 0
PART 0
C16 1 1.041703 0.276730 0.538412 11.00000 0.04381 0.06969 =
0.05723 0.01915 -0.00004 -0.01106
PART 2
AFIX 23
H16A 2 1.081551 0.277008 0.530080 -31.00000 -1.20000
H16B 2 1.031019 0.314176 0.550289 -31.00000 -1.20000
AFIX 0
PART 0
PART 1
C17 1 1.102267 0.278979 0.527578 31.00000 0.04183 0.05988 =
0.05664 0.00854 0.01182 -0.00024
AFIX 137
H17A 2 1.121679 0.288197 0.561670 31.00000 -1.50000
H17B 2 1.109900 0.307109 0.499748 31.00000 -1.50000
H17C 2 1.114866 0.243105 0.514224 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C17B 1 1.028150 0.271031 0.431951 -31.00000 0.14794
AFIX 137
H17D 2 1.038807 0.236099 0.414916 -31.00000 -1.50000
H17E 2 1.059882 0.295862 0.432664 -31.00000 -1.50000
H17F 2 0.998399 0.287862 0.410605 -31.00000 -1.50000
AFIX 0
PART 0
C18 1 1.017568 0.258231 0.628306 11.00000 0.05166 0.05485 =
0.05422 0.00890 0.00399 -0.00590
AFIX 43
H18 2 1.013686 0.297041 0.630517 11.00000 -1.20000
AFIX 0
N5 3 0.915771 0.416275 0.616331 11.00000 0.06756 0.06404 =
0.04847 0.01108 -0.00429 0.00217
N6 3 0.803827 0.445015 0.587905 11.00000 0.06087 0.05563 =
0.05180 0.00717 -0.00071 -0.00124
N7 3 0.722011 0.508087 0.347959 11.00000 0.06519 0.06629 =
0.06331 0.00785 -0.01476 -0.00117
N8 3 0.800766 0.474040 0.262003 11.00000 0.05918 0.07186 =
0.08217 0.00477 -0.01302 0.01335
C19 1 1.016087 0.419009 0.505782 11.00000 0.05922 0.04737 =
0.05964 -0.00098 -0.00821 0.00330
AFIX 43
H19 2 1.004305 0.386995 0.486744 11.00000 -1.20000
AFIX 0
C20 1 0.987080 0.436955 0.551859 11.00000 0.05329 0.05113 =
0.05214 0.01015 -0.00730 0.00079
C21 1 0.939461 0.406042 0.571062 11.00000 0.06083 0.05244 =
0.05844 0.00737 -0.00993 0.00573
AFIX 43
H21 2 0.925642 0.377090 0.548769 11.00000 -1.20000
AFIX 0
C22 1 0.868301 0.382822 0.631708 11.00000 0.06477 0.05990 =
0.04735 0.01985 0.00208 -0.00982
PART 2
AFIX 23
H22A 2 0.876189 0.362624 0.666163 -41.00000 -1.20000
H22B 2 0.860492 0.355612 0.602451 -41.00000 -1.20000
AFIX 0
PART 0
C23 1 0.819377 0.419662 0.639707 11.00000 0.07385 0.05853 =
0.05119 0.01608 0.00332 -0.00548
PART 1
AFIX 23
H23A 2 0.788146 0.397930 0.654188 41.00000 -1.20000
H23B 2 0.828370 0.448588 0.666907 41.00000 -1.20000
AFIX 0
C24 1 0.880211 0.352208 0.685778 41.00000 0.04756 0.06814 =
0.07729 0.03236 -0.00257 0.00332
AFIX 137
H24A 2 0.914054 0.330684 0.681854 41.00000 -1.50000
H24B 2 0.849507 0.327532 0.694287 41.00000 -1.50000
H24C 2 0.884657 0.378909 0.715634 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C24B 1 0.796937 0.381581 0.668644 -41.00000 0.11075
AFIX 137
H24D 2 0.761294 0.394403 0.682402 -41.00000 -1.50000
H24E 2 0.820869 0.372493 0.699768 -41.00000 -1.50000
H24F 2 0.791529 0.348800 0.645836 -41.00000 -1.50000
AFIX 0
PART 0
C25 1 0.797471 0.495597 0.587015 11.00000 0.08118 0.05371 =
0.05599 0.00949 -0.00735 -0.00781
AFIX 43
H25 2 0.804161 0.516154 0.619555 11.00000 -1.20000
AFIX 0
C26 1 0.779806 0.524745 0.536822 11.00000 0.08365 0.06318 =
0.05142 0.01315 -0.01526 -0.01290
C27 1 0.774705 0.581130 0.536346 11.00000 0.07694 0.06146 =
0.05698 0.00486 -0.01677 0.00240
AFIX 43
H27 2 0.782624 0.601450 0.568758 11.00000 -1.20000
AFIX 0
C28 1 0.757657 0.609555 0.487758 11.00000 0.08143 0.06360 =
0.05935 0.00882 -0.01501 -0.00126
C29 1 0.745741 0.578688 0.441508 11.00000 0.07622 0.06036 =
0.06370 0.01416 -0.01545 -0.00327
AFIX 43
H29 2 0.734425 0.596956 0.408883 11.00000 -1.20000
AFIX 0
C30 1 0.749870 0.521515 0.441425 11.00000 0.08420 0.05892 =
0.06466 0.00968 -0.02023 -0.00505
C31 1 0.766820 0.495136 0.489902 11.00000 0.06840 0.06082 =
0.07021 0.00852 -0.00885 -0.00157
AFIX 43
H31 2 0.769441 0.456164 0.490550 11.00000 -1.20000
AFIX 0
C32 1 0.736483 0.488474 0.393686 11.00000 0.06785 0.06266 =
0.07659 0.00925 -0.02123 -0.00510
AFIX 43
H32 2 0.738756 0.449621 0.397068 11.00000 -1.20000
AFIX 0
C33 1 0.707602 0.469710 0.303996 11.00000 0.05948 0.07363 =
0.06649 0.00038 -0.01668 -0.00427
PART 2
AFIX 23
H33A 2 0.667934 0.472882 0.295408 -51.00000 -1.20000
H33B 2 0.715002 0.431542 0.316070 -51.00000 -1.20000
AFIX 0
PART 0
C34 1 0.740864 0.482477 0.253768 11.00000 0.05518 0.09215 =
0.06448 0.00151 -0.01582 -0.00110
PART 1
AFIX 23
H34A 2 0.728244 0.458786 0.223160 51.00000 -1.20000
H34B 2 0.734302 0.521195 0.243035 51.00000 -1.20000
AFIX 0
C35 1 0.646372 0.478258 0.289115 51.00000 0.05136 0.07979 =
0.07488 -0.01015 -0.01160 -0.00645
AFIX 137
H35A 2 0.623340 0.467853 0.320505 51.00000 -1.50000
H35B 2 0.636940 0.455327 0.257347 51.00000 -1.50000
H35C 2 0.640031 0.517013 0.280064 51.00000 -1.50000
AFIX 0
PART 0
PART 2
C35B 1 0.724951 0.435489 0.217507 -51.00000 0.10943
AFIX 137
H35D 2 0.756954 0.423615 0.196085 -51.00000 -1.50000
H35E 2 0.695614 0.447178 0.192472 -51.00000 -1.50000
H35F 2 0.711850 0.404859 0.240183 -51.00000 -1.50000
AFIX 0
PART 0
C36 1 0.831574 0.514247 0.252890 11.00000 0.06760 0.05401 =
0.07247 0.01590 -0.01209 -0.00029
AFIX 43
H36 2 0.815101 0.548022 0.242210 11.00000 -1.20000
AFIX 0
O1 4 0.812881 0.376186 0.422879 10.75000 0.07158 0.06792 =
0.11196 0.01920 0.01461 0.00544
O2 4 0.899504 0.343502 0.351026 10.75000 0.06511 0.07680 =
0.09295 0.02099 0.00125 -0.00399
C37 1 0.861755 0.409806 0.416925 10.75000 0.09676 0.06834 =
0.10121 0.02769 0.00778 -0.00553
AFIX 23
H37A 2 0.869296 0.429357 0.451829 10.75000 -1.20000
H37B 2 0.855807 0.437628 0.387806 10.75000 -1.20000
AFIX 0
C38 1 0.909731 0.374420 0.402246 10.75000 0.06166 0.08540 =
0.07875 0.02077 -0.00797 -0.01327
AFIX 23
H38A 2 0.942773 0.397737 0.397569 10.75000 -1.20000
H38B 2 0.916992 0.348260 0.432583 10.75000 -1.20000
AFIX 0
C39 1 0.851438 0.311411 0.356983 10.75000 0.05944 0.07715 =
0.13347 0.01100 0.00220 0.00482
AFIX 23
H39A 2 0.857512 0.283170 0.385670 10.75000 -1.20000
H39B 2 0.843549 0.292255 0.321937 10.75000 -1.20000
AFIX 0
C40 1 0.802420 0.346807 0.372768 10.75000 0.05465 0.07193 =
0.13533 0.00964 -0.00773 -0.00280
AFIX 23
H40A 2 0.794662 0.373329 0.342871 10.75000 -1.20000
H40B 2 0.769603 0.323185 0.377499 10.75000 -1.20000
AFIX 0
PART 1
O3 4 0.801288 0.224400 0.698814 10.33333 0.07914 0.08389 =
0.08522 0.01702 -0.00014 -0.00372
PART 0
PART 2
O4 4 0.874347 0.163338 0.656012 10.33333 0.08292 0.12073 =
0.16430 0.00079 -0.00491 -0.01370
PART 0
C41 1 0.799137 0.218827 0.649742 10.66667 0.10726 0.10664 =
0.09253 0.02580 -0.01513 -0.01043
C42 1 0.860585 0.213879 0.653286 10.66667 0.10160 0.12389 =
0.11186 0.00574 -0.00317 -0.02412
O43 4 0.922367 0.529489 0.389774 10.33333 0.13862 0.16142 =
0.09312 -0.04830 0.02393 -0.01549
O44 4 0.955192 0.557786 0.378867 10.33333 0.12386 0.15661 =
0.09632 -0.04655 0.02669 0.00398
C45 1 0.878148 0.570775 0.388628 10.66667 0.13843 0.21398 =
0.13214 -0.03989 0.00600 -0.00789
C46 1 0.959146 0.528976 0.430158 10.66667 0.17047 0.21511 =
0.14184 -0.00990 -0.00227 -0.02232
O47 4 0.558301 0.558301 0.558301 10.25000 0.31576 0.31576 =
0.31576 -0.07281 -0.07281 -0.07281
C48 1 0.621104 0.558223 0.556466 10.50000 0.30657 0.24985 =
0.29421 -0.04211 -0.06408 -0.03363
C49 1 0.631173 0.563884 0.613900 10.50000 0.21452 0.29174 =
0.29437 -0.04676 -0.05584 -0.03909
O50 4 0.626993 0.626993 0.626993 10.25000 0.29407 0.29407 =
0.29407 -0.04277 -0.04277 -0.04277
PART 1
O5 4 0.423767 0.423767 0.423767 10.16667 0.17397
PART 0
PART 2
O6 4 0.498080 0.448509 0.416768 10.25000 0.11646
PART 0
PART 3
O7 4 0.508927 0.378764 0.455353 10.25000 0.10809
PART 0
PART 4
O8 4 0.551656 0.480672 0.418184 10.25000 0.12172
PART 0
O9 4 0.727755 0.691740 0.636229 10.50000 0.24217
C10 1 0.753812 0.207077 0.298944 10.33333 0.17453
C11 1 0.655997 0.162952 0.311463 10.33333 0.22385
O12 4 0.748216 0.142565 0.311660 10.16667 0.17428
O13 4 0.729142 0.203504 0.340254 10.16667 0.18172
HKLF 4
REM C54H60N12 *2.5C4H8O2 *4.75H2O in P2(1)3
REM R1 = 0.0722 for 5558 Fo > 4sig(Fo) and 0.0860 for all 6914 data
REM 609 parameters refined using 48 restraints
END
WGHT 0.1542 0.3411
REM Instructions for potential hydrogen bonds
HTAB C5 N6
HTAB C7 N6
EQIV $1 -y+3/2, -z+1, x-1/2
HTAB C17B N5_$1
HTAB C24B N1
EQIV $2 z+1/2, -x+3/2, -y+1
HTAB C25 O2_$2
HTAB C32 O1
HTAB C35B O9_$1
EQIV $3 -z+1, x-1/2, -y+1/2
HTAB C35B O2_$3
HTAB C38 N3
REM Highest difference peak 0.363, deepest hole -0.273, 1-sigma level 0.054
Q1 1 0.5138 0.4794 0.4563 11.00000 0.05 0.36
Q2 1 0.5175 0.5175 0.5175 10.33333 0.05 0.34
Q3 1 0.4957 0.4838 0.4085 11.00000 0.05 0.32
Q4 1 0.7696 0.2696 0.2304 10.33333 0.05 0.31
Q5 1 0.5034 0.4287 0.4383 11.00000 0.05 0.30
Q6 1 0.4713 0.4076 0.4430 11.00000 0.05 0.28
Q7 1 0.7284 0.2284 0.2716 10.33333 0.05 0.27
Q8 1 0.6024 0.5959 0.6463 11.00000 0.05 0.26
Q9 1 0.5527 0.3753 0.4638 11.00000 0.05 0.25
Q10 1 0.4104 0.4104 0.4104 10.33333 0.05 0.21
Q11 1 0.7571 0.2288 0.6328 11.00000 0.05 0.20
Q12 1 0.7518 0.1825 0.3378 11.00000 0.05 0.20
Q13 1 0.6407 0.5775 0.5724 11.00000 0.05 0.20
Q14 1 0.8263 0.3641 0.3444 11.00000 0.05 0.19
Q15 1 0.7733 0.2159 0.6123 11.00000 0.05 0.18
Q16 1 0.7514 0.7190 0.6571 11.00000 0.05 0.18
Q17 1 0.8323 0.3536 0.3644 11.00000 0.05 0.17
Q18 1 0.6804 0.1395 0.3016 11.00000 0.05 0.17
Q19 1 1.0097 0.5312 0.3968 11.00000 0.05 0.17
Q20 1 1.0893 0.4107 0.5893 10.33333 0.05 0.17
;
_shelx_res_checksum 27110
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_CC3-R_CC13-R_2-propanol
_database_code_depnum_ccdc_archive 'CCDC 1520509'
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_audit_creation_date 2015-07-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C72 H84 N12, C60 H72 N12, 6(C3 H8 O), C1 H2 Cl2, 4(H2 O)'
_chemical_formula_sum 'C151 H214 Cl2 N24 O10'
_chemical_formula_weight 2596.35
_chemical_absolute_configuration CC3-R
_chemical_melting_point ?
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'
Cl Cl 0.1484 0.1585 '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'
_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.
;
_space_group_crystal_system hexagonal
_space_group_IT_number 173
_space_group_name_H-M_alt 'P 63'
_space_group_name_Hall 'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
_cell_length_a 17.5938(7)
_cell_length_b 17.5938(7)
_cell_length_c 32.2344(13)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 8641.1(8)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9992
_cell_measurement_temperature 100
_cell_measurement_theta_max 21.762
_cell_measurement_theta_min 2.315
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.093
_exptl_absorpt_correction_T_max 0.9281
_exptl_absorpt_correction_T_min 0.6318
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1156 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.6807.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 0.998
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description hexagonal
_exptl_crystal_F_000 2804
_exptl_crystal_size_max 0.236
_exptl_crystal_size_mid 0.194
_exptl_crystal_size_min 0.078
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0532
_diffrn_reflns_av_unetI/netI 0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 37680
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full 23.150
_diffrn_reflns_theta_max 23.255
_diffrn_reflns_theta_min 1.336
_diffrn_ambient_temperature 100.0
_diffrn_detector CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type 'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation 0.3
_diffrn_radiation_monochromator Confocal
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Rotating Anode'
_diffrn_source_current 24.0
_diffrn_source_power 1.2
_diffrn_source_target Mo
_diffrn_source_type 'Rotating Anode'
_diffrn_source_voltage 50.0
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.803
_reflns_Friedel_fraction_full 0.838
_reflns_Friedel_fraction_max 0.836
_reflns_number_gt 6186
_reflns_number_total 7633
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2008)'
_computing_structure_solution ?
_refine_diff_density_max 0.587
_refine_diff_density_min -0.337
_refine_diff_density_rms 0.090
_refine_ls_abs_structure_details
;
Flack x determined using 2413 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.84(10)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 595
_refine_ls_number_reflns 7633
_refine_ls_number_restraints 74
_refine_ls_R_factor_all 0.1121
_refine_ls_R_factor_gt 0.0916
_refine_ls_restrained_S_all 1.078
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1820P)^2^+4.0227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2460
_refine_ls_wR_factor_ref 0.2709
_refine_special_details ?
_olex2_refinement_description
;
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. Shared sites
{C61, Cl3}
3. Restrained distances
Cl2-C61 = Cl3-Cl1
1.74 with sigma of 0.02
O4-C50 = O1_$8-C47_$8 = O9_$8-C53_$8 = O3_$7-C56_$7 = O2-C59
1.43 with sigma of 0.02
C51-C50 = C59-C58 = C60-C59 = C53_$8-C52_$8 = C54_$8-C53_$8 = C57_$7-C56_$7 =
C56_$7-C55_$7 = C49_$8-C47_$8 = C48_$8-C47_$8
1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C61) = Uiso(Cl3)
Uiso(C59) = Uiso(O2) = Uiso(C58) = Uiso(C60)
5. Rigid body (RIGU) restrains
N6, C13, C14, C15, C10, C12, C11, N5
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(H13A)=Sof(H13B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
Sof(H12B)=Sof(H12C)=1-FVAR(1)
Sof(H10A)=Sof(H10B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
Sof(H15B)=Sof(H15C)=FVAR(1)
Fixed Sof: O9(0.5) H9A(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5)
H53(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) O2(0.16667) C58(0.16667)
C59(0.16667) C60(0.16667) Cl1(0.16667) Cl2(0.33333) C61(0.33333) Cl3(0.16666)
O3(0.5) H3A(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5) C56(0.5) H56(0.5)
C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) O1(0.5) H1A(0.5) C47(0.5) H47(0.5)
C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
O4(0.33333) C50(0.66667) C51(0.33333) O6(0.33333) O5(0.33333) O7(0.33333)
O11(0.08333) O10(0.25)
7.a Ternary CH refined with riding coordinates:
C26(H26), C31(H31), C41(H41), C46(H46), C53(H53), C56(H56), C47(H47)
7.b Secondary CH2 refined with riding coordinates:
C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C42(H42A,
H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C10(H10A,H10B),
C13(H13A,H13B), C16(H16A,H16B)
7.c Me refined with riding coordinates:
C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C49(H49A,H49B,
H49C)
7.d Aromatic/amide H refined with riding coordinates:
C23(H23), C25(H25), C32(H32), C34(H34), C36(H36), C38(H38), C39(H39),
C40(H40), C1(H1), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C20(H20), C21(H21)
7.e Tetrahedral OH refined with riding coordinates:
O9(H9A)
7.f Idealised Me refined as rotating group:
C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C52(H52A,H52B,H52C), C48(H48A,
H48B,H48C)
7.g Idealised tetrahedral OH refined as rotating group:
O3(H3A), O1(H1A)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
N1 N 0.6183(4) 0.7232(4) 0.7236(2) 0.0514(16) Uani 1 1 d . . . . .
N2 N 0.6436(3) 0.8960(4) 0.71307(19) 0.0470(14) Uani 1 1 d . . . . .
N3 N 0.5179(4) 0.4986(4) 0.5571(2) 0.0487(15) Uani 1 1 d . . . . .
N4 N 0.4457(3) 0.5362(3) 0.48578(19) 0.0439(13) Uani 1 1 d . . . . .
C23 C 0.4217(4) 0.7289(4) 0.4922(2) 0.0410(15) Uani 1 1 d . . . . .
H23 H 0.4824 0.7717 0.4919 0.049 Uiso 1 1 calc R . . . .
C24 C 0.3967(4) 0.6404(4) 0.4924(2) 0.0387(14) Uani 1 1 d . . . . .
C25 C 0.4636(4) 0.6152(4) 0.4903(2) 0.0438(15) Uani 1 1 d . . . . .
H25 H 0.5235 0.6598 0.4924 0.053 Uiso 1 1 calc R . . . .
C26 C 0.5189(4) 0.5195(4) 0.4827(3) 0.0465(16) Uani 1 1 d . . . . .
H26 H 0.5754 0.5759 0.4862 0.056 Uiso 1 1 calc R . . . .
C27 C 0.5170(6) 0.4815(7) 0.4400(3) 0.072(3) Uani 1 1 d . . . . .
H27A H 0.4601 0.4270 0.4358 0.087 Uiso 1 1 calc R . . . .
H27B H 0.5230 0.5241 0.4183 0.087 Uiso 1 1 calc R . . . .
C28 C 0.5903(7) 0.4621(8) 0.4361(4) 0.095(3) Uani 1 1 d . . . . .
H28A H 0.5879 0.4362 0.4086 0.114 Uiso 1 1 calc R . . . .
H28B H 0.6473 0.5172 0.4386 0.114 Uiso 1 1 calc R . . . .
C29 C 0.5832(7) 0.4014(8) 0.4684(5) 0.107(5) Uani 1 1 d . . . . .
H29A H 0.6323 0.3895 0.4655 0.128 Uiso 1 1 calc R . . . .
H29B H 0.5278 0.3452 0.4645 0.128 Uiso 1 1 calc R . . . .
C30 C 0.5848(6) 0.4353(6) 0.5125(4) 0.078(3) Uani 1 1 d . . . . .
H30A H 0.5770 0.3902 0.5331 0.094 Uiso 1 1 calc R . . . .
H30B H 0.6421 0.4887 0.5178 0.094 Uiso 1 1 calc R . . . .
C31 C 0.5104(4) 0.4565(5) 0.5169(3) 0.0504(18) Uani 1 1 d . . . . .
H31 H 0.4523 0.4013 0.5147 0.060 Uiso 1 1 calc R . . . .
C32 C 0.4527(5) 0.4635(4) 0.5808(2) 0.0489(18) Uani 1 1 d . . . . .
H32 H 0.4014 0.4120 0.5717 0.059 Uiso 1 1 calc R . . . .
C33 C 0.4529(4) 0.4991(4) 0.6220(2) 0.0474(17) Uani 1 1 d . . . . .
C34 C 0.5247(4) 0.5799(5) 0.6353(3) 0.0498(18) Uani 1 1 d . . . . .
H34 H 0.5717 0.6133 0.6167 0.060 Uiso 1 1 calc R . . . .
C35 C 0.5275(4) 0.6103(5) 0.6744(2) 0.0514(18) Uani 1 1 d . . . . .
C36 C 0.4574(4) 0.5636(5) 0.7024(3) 0.0542(18) Uani 1 1 d . . . . .
H36 H 0.4588 0.5856 0.7295 0.065 Uiso 1 1 calc R . . . .
C37 C 0.3855(4) 0.4837(5) 0.6892(3) 0.0535(19) Uani 1 1 d . . . . .
C38 C 0.3835(4) 0.4524(4) 0.6496(2) 0.0484(17) Uani 1 1 d . . . . .
H38 H 0.3343 0.3984 0.6411 0.058 Uiso 1 1 calc R . . . .
C39 C 0.3158(5) 0.4335(5) 0.7200(2) 0.0511(18) Uani 1 1 d . . . . .
H39 H 0.3184 0.4599 0.7460 0.061 Uiso 1 1 calc R . . . .
C40 C 0.6060(4) 0.6924(5) 0.6865(2) 0.0477(16) Uani 1 1 d . . . . .
H40 H 0.6495 0.7241 0.6661 0.057 Uiso 1 1 calc R . . . .
C41 C 0.7016(4) 0.8016(4) 0.7324(2) 0.0443(16) Uani 1 1 d . . . . .
H41 H 0.7381 0.8201 0.7066 0.053 Uiso 1 1 calc R . . . .
C42 C 0.7492(5) 0.7801(5) 0.7660(3) 0.0541(19) Uani 1 1 d . . . . .
H42A H 0.7102 0.7551 0.7904 0.065 Uiso 1 1 calc R . . . .
H42B H 0.7624 0.7352 0.7553 0.065 Uiso 1 1 calc R . . . .
C43 C 0.8332(5) 0.8598(5) 0.7793(3) 0.061(2) Uani 1 1 d . . . . .
H43A H 0.8757 0.8794 0.7560 0.074 Uiso 1 1 calc R . . . .
H43B H 0.8588 0.8439 0.8028 0.074 Uiso 1 1 calc R . . . .
C44 C 0.8188(5) 0.9340(5) 0.7921(3) 0.069(2) Uani 1 1 d . . . . .
H44A H 0.8762 0.9868 0.7981 0.083 Uiso 1 1 calc R . . . .
H44B H 0.7833 0.9176 0.8178 0.083 Uiso 1 1 calc R . . . .
C45 C 0.7716(5) 0.9556(5) 0.7580(3) 0.058(2) Uani 1 1 d . . . . .
H45A H 0.7604 1.0024 0.7679 0.070 Uiso 1 1 calc R . . . .
H45B H 0.8098 0.9779 0.7332 0.070 Uiso 1 1 calc R . . . .
C46 C 0.6859(4) 0.8760(5) 0.7462(2) 0.0480(17) Uani 1 1 d . . . . .
H46 H 0.6464 0.8560 0.7710 0.058 Uiso 1 1 calc R . . . .
N5 N 0.7679(6) 0.7103(6) 0.6145(3) 0.093(3) Uani 1 1 d . U . . .
N6 N 0.9211(7) 0.6915(7) 0.6063(3) 0.083(2) Uani 1 1 d . U . . .
N7 N 0.6442(4) 0.8161(6) 0.4501(3) 0.074(2) Uani 1 1 d . . . . .
N8 N 0.7587(4) 0.8852(4) 0.3798(2) 0.0589(17) Uani 1 1 d . . . . .
C1 C 0.7729(5) 1.0123(9) 0.6161(3) 0.083(3) Uani 1 1 d . . . . .
H1 H 0.7893 1.0072 0.6435 0.100 Uiso 1 1 calc R . . . .
C2 C 0.7505(5) 0.9386(7) 0.5855(3) 0.078(3) Uani 1 1 d . . . . .
C3 C 0.7224(5) 0.9415(7) 0.5462(3) 0.072(2) Uani 1 1 d . . . . .
H3 H 0.7181 0.9910 0.5380 0.086 Uiso 1 1 calc R . . . .
C4 C 0.7001(5) 0.8738(8) 0.5181(3) 0.081(3) Uani 1 1 d . . . . .
C5 C 0.7060(5) 0.7996(7) 0.5303(3) 0.077(3) Uani 1 1 d . . . . .
H5 H 0.6905 0.7525 0.5114 0.092 Uiso 1 1 calc R . . . .
C6 C 0.7348(5) 0.7965(7) 0.5700(3) 0.081(3) Uani 1 1 d . . . . .
C7 C 0.7561(5) 0.8661(8) 0.5977(3) 0.084(3) Uani 1 1 d . . . . .
H7 H 0.7746 0.8633 0.6251 0.101 Uiso 1 1 calc R . . . .
C8 C 0.6694(5) 0.8794(8) 0.4759(3) 0.075(3) Uani 1 1 d . . . . .
H8 H 0.6684 0.9310 0.4680 0.090 Uiso 1 1 calc R . . . .
C9 C 0.7397(6) 0.7175(8) 0.5809(4) 0.088(3) Uani 1 1 d . . . . .
H9 H 0.7205 0.6711 0.5613 0.105 Uiso 1 1 calc R . . . .
C10 C 0.7664(9) 0.6282(9) 0.6229(5) 0.110(3) Uani 1 1 d . U . . .
H10A H 0.7518 0.5930 0.5971 0.132 Uiso 0.525(16) 1 calc R . . A 1
H10B H 0.7207 0.5939 0.6438 0.132 Uiso 0.525(16) 1 calc R . . A 1
C13 C 0.8543(9) 0.6465(8) 0.6387(4) 0.104(3) Uani 1 1 d . U . . .
H13A H 0.8702 0.6838 0.6638 0.125 Uiso 0.475(16) 1 calc R . . A 2
H13B H 0.8516 0.5907 0.6463 0.125 Uiso 0.475(16) 1 calc R . . A 2
C16 C 0.6162(5) 0.8297(7) 0.4098(3) 0.073(3) Uani 1 1 d . . . . .
H16A H 0.6271 0.8905 0.4079 0.088 Uiso 1 1 calc R . . . .
H16B H 0.5524 0.7890 0.4064 0.088 Uiso 1 1 calc R . . . .
C17 C 0.6666(5) 0.8136(5) 0.3751(3) 0.061(2) Uani 1 1 d . . . . .
C18 C 0.6491(6) 0.7203(6) 0.3778(4) 0.087(3) Uani 1 1 d . . . . .
H18A H 0.6611 0.7086 0.4060 0.130 Uiso 1 1 calc GR . . . .
H18B H 0.6871 0.7124 0.3582 0.130 Uiso 1 1 calc GR . . . .
H18C H 0.5875 0.6795 0.3709 0.130 Uiso 1 1 calc GR . . . .
C19 C 0.6360(6) 0.8308(6) 0.3336(3) 0.074(3) Uani 1 1 d . . . . .
H19A H 0.6635 0.8162 0.3109 0.110 Uiso 1 1 calc GR . . . .
H19B H 0.6527 0.8928 0.3318 0.110 Uiso 1 1 calc GR . . . .
H19C H 0.5720 0.7943 0.3315 0.110 Uiso 1 1 calc GR . . . .
C20 C 0.8183(5) 0.8673(5) 0.3868(2) 0.0523(18) Uani 1 1 d . . . . .
H20 H 0.8030 0.8078 0.3904 0.063 Uiso 1 1 calc R . . . .
C21 C 0.9373(4) 1.0254(4) 0.3895(2) 0.0445(16) Uani 1 1 d . . . . .
H21 H 0.8940 1.0427 0.3893 0.053 Uiso 1 1 calc R . . . .
C22 C 0.9111(4) 0.9363(4) 0.3896(2) 0.0456(16) Uani 1 1 d . . . . .
C14 C 0.8534(11) 0.6746(11) 0.6788(6) 0.069(4) Uani 0.525(16) 1 d . U . A 1
H14A H 0.8457 0.7260 0.6780 0.104 Uiso 0.525(16) 1 calc GR . . A 1
H14B H 0.9091 0.6902 0.6925 0.104 Uiso 0.525(16) 1 calc GR . . A 1
H14C H 0.8049 0.6273 0.6943 0.104 Uiso 0.525(16) 1 calc GR . . A 1
C15 C 0.8308(11) 0.5429(11) 0.6392(6) 0.073(5) Uani 0.525(16) 1 d . U . A 1
H15A H 0.8789 0.5390 0.6524 0.109 Uiso 0.525(16) 1 calc GR . . A 1
H15B H 0.8232 0.5210 0.6106 0.109 Uiso 0.525(16) 1 calc GR . . A 1
H15C H 0.7765 0.5074 0.6548 0.109 Uiso 0.525(16) 1 calc GR . . A 1
C11 C 0.734(2) 0.596(2) 0.6688(9) 0.117(8) Uani 0.475(16) 1 d . U . A 2
H11A H 0.6721 0.5809 0.6715 0.175 Uiso 0.475(16) 1 calc GR . . A 2
H11B H 0.7696 0.6432 0.6884 0.175 Uiso 0.475(16) 1 calc GR . . A 2
H11C H 0.7388 0.5444 0.6750 0.175 Uiso 0.475(16) 1 calc GR . . A 2
C12 C 0.7581(19) 0.5649(18) 0.5990(9) 0.105(7) Uani 0.475(16) 1 d . U . A 2
H12A H 0.8104 0.5861 0.5815 0.158 Uiso 0.475(16) 1 calc GR . . A 2
H12B H 0.7061 0.5450 0.5814 0.158 Uiso 0.475(16) 1 calc GR . . A 2
H12C H 0.7516 0.5159 0.6161 0.158 Uiso 0.475(16) 1 calc GR . . A 2
O9 O 0.606(3) 0.486(3) 0.7586(14) 0.263(18) Uiso 0.5 1 d D . . B 1
H9A H 0.5898 0.4743 0.7835 0.394 Uiso 0.5 1 calc R . . B 1
C52 C 0.4786(19) 0.368(2) 0.7577(10) 0.133(10) Uiso 0.5 1 d D . . B 1
H52A H 0.4425 0.3922 0.7480 0.200 Uiso 0.5 1 calc GR . . B 1
H52B H 0.4887 0.3777 0.7876 0.200 Uiso 0.5 1 calc GR . . B 1
H52C H 0.4482 0.3046 0.7520 0.200 Uiso 0.5 1 calc GR . . B 1
C53 C 0.5638(19) 0.411(2) 0.7357(12) 0.140(10) Uiso 0.5 1 d D . . B 1
H53 H 0.5577 0.4232 0.7059 0.168 Uiso 0.5 1 calc R . . B 1
C54 C 0.612(3) 0.362(3) 0.7409(18) 0.22(2) Uiso 0.5 1 d D . . B 1
H54A H 0.5826 0.3076 0.7246 0.324 Uiso 0.5 1 calc R . . B 1
H54B H 0.6724 0.3982 0.7312 0.324 Uiso 0.5 1 calc R . . B 1
H54C H 0.6119 0.3475 0.7702 0.324 Uiso 0.5 1 calc R . . B 1
O2 O 1.0000 1.0000 0.6081(8) 0.091(5) Uiso 0.5 3 d DS T P C 1
C58 C 0.901(4) 0.881(4) 0.669(2) 0.091(5) Uiso 0.1667 1 d D . . C 1
C59 C 0.983(4) 0.948(3) 0.6454(10) 0.091(5) Uiso 0.1667 1 d D . . C 1
C60 C 1.0000 1.0000 0.6856(12) 0.091(5) Uiso 0.5 3 d DS T P C 1
Cl1 Cl 0.3333 0.6667 0.6481(10) 0.238(11) Uiso 0.5 3 d DS T P . .
Cl2 Cl 0.4981(7) 0.7450(7) 0.5938(4) 0.111(3) Uiso 0.3333 1 d D . . . .
C61 C 0.3881(13) 0.696(2) 0.6052(9) 0.205(10) Uiso 0.3333 1 d D . . D 3
Cl3 Cl 0.3881(13) 0.696(2) 0.6052(9) 0.205(10) Uiso 0.1667 1 d D . . D 4
O3 O 0.5058(13) 0.3037(13) 0.2864(6) 0.119(5) Uiso 0.5 1 d D . . E 2
H3A H 0.4956 0.3333 0.2693 0.179 Uiso 0.5 1 calc GR . . E 2
C55 C 0.481(3) 0.404(3) 0.3266(17) 0.206(19) Uiso 0.5 1 d D . . E 2
H55A H 0.4710 0.4162 0.3553 0.309 Uiso 0.5 1 calc R . . E 2
H55B H 0.5333 0.4553 0.3155 0.309 Uiso 0.5 1 calc R . . E 2
H55C H 0.4297 0.3932 0.3096 0.309 Uiso 0.5 1 calc R . . E 2
C56 C 0.492(3) 0.323(2) 0.3256(9) 0.149(11) Uiso 0.5 1 d D . . E 2
H56 H 0.5543 0.3522 0.3356 0.179 Uiso 0.5 1 calc R . . E 2
C57 C 0.452(3) 0.252(3) 0.3575(13) 0.174(14) Uiso 0.5 1 d D . . E 2
H57A H 0.4465 0.2771 0.3839 0.261 Uiso 0.5 1 calc R . . E 2
H57B H 0.3933 0.2071 0.3482 0.261 Uiso 0.5 1 calc R . . E 2
H57C H 0.4888 0.2257 0.3615 0.261 Uiso 0.5 1 calc R . . E 2
O1 O 0.2121(9) 0.1007(10) 0.4896(5) 0.094(4) Uiso 0.5 1 d D . . F 1
H1A H 0.1888 0.0488 0.4809 0.141 Uiso 0.5 1 calc GR . . F 1
C47 C 0.3093(13) 0.1430(14) 0.4864(7) 0.106(7) Uiso 0.5 1 d D . . F 1
H47 H 0.3270 0.0983 0.4924 0.127 Uiso 0.5 1 calc R . . F 1
C48 C 0.3595(12) 0.2206(11) 0.5144(6) 0.069(4) Uiso 0.5 1 d D . . F 1
H48A H 0.3275 0.2109 0.5406 0.104 Uiso 0.5 1 calc GR . . F 1
H48B H 0.3664 0.2736 0.5009 0.104 Uiso 0.5 1 calc GR . . F 1
H48C H 0.4175 0.2279 0.5201 0.104 Uiso 0.5 1 calc GR . . F 1
C49 C 0.3387(15) 0.1783(15) 0.4432(7) 0.093(6) Uiso 0.5 1 d D . . F 1
H49A H 0.4027 0.2060 0.4413 0.139 Uiso 0.5 1 calc R . . F 1
H49B H 0.3115 0.1300 0.4231 0.139 Uiso 0.5 1 calc R . . F 1
H49C H 0.3210 0.2218 0.4369 0.139 Uiso 0.5 1 calc R . . F 1
O4 O 0.4077(17) 0.6995(16) 0.3304(8) 0.110(7) Uiso 0.3333 1 d D . . . .
C50 C 0.3653(17) 0.6510(18) 0.3696(8) 0.135(8) Uiso 0.6667 1 d D . . . .
C51 C 0.396(3) 0.592(3) 0.3804(16) 0.130(14) Uiso 0.3333 1 d D . . . .
O6 O 0.0906(19) 0.0755(17) 0.5087(8) 0.105(7) Uiso 0.3333 1 d . . . G 5
O5 O 0.9213(14) 0.9071(15) 0.5073(7) 0.086(6) Uiso 0.3333 1 d . . . H 3
O7 O 0.0302(18) 0.0564(15) 0.5012(8) 0.097(7) Uiso 0.3333 1 d . . . I 4
O11 O 0.6667 0.3333 0.2544(11) 0.051(8) Uiso 0.25 3 d S T P . .
O10 O 0.469(5) 0.526(5) 0.299(2) 0.21(3) Uiso 0.25 1 d . . . J 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 0.037(3) 0.047(3) 0.064(5) 0.009(3) -0.006(3) 0.016(3)
N2 0.040(3) 0.045(3) 0.053(4) -0.002(3) -0.007(3) 0.019(3)
N3 0.038(3) 0.048(3) 0.062(4) 0.006(3) -0.002(3) 0.022(3)
N4 0.042(3) 0.046(3) 0.048(4) 0.000(3) 0.002(3) 0.025(2)
C23 0.037(3) 0.039(3) 0.043(4) 0.000(3) 0.004(3) 0.016(3)
C24 0.041(3) 0.039(3) 0.037(4) 0.001(3) -0.001(3) 0.021(3)
C25 0.040(3) 0.040(4) 0.048(4) 0.003(3) 0.005(3) 0.017(3)
C26 0.038(3) 0.043(4) 0.059(5) -0.004(3) 0.010(3) 0.021(3)
C27 0.069(5) 0.083(6) 0.067(6) -0.010(5) 0.020(4) 0.039(5)
C28 0.086(7) 0.092(7) 0.123(10) -0.017(7) 0.025(6) 0.057(6)
C29 0.066(6) 0.106(8) 0.176(13) -0.061(9) -0.004(7) 0.064(6)
C30 0.064(5) 0.070(5) 0.121(9) -0.004(5) -0.008(5) 0.049(5)
C31 0.036(3) 0.046(4) 0.072(5) -0.011(4) -0.001(3) 0.023(3)
C32 0.047(4) 0.038(4) 0.058(5) -0.004(3) -0.012(4) 0.018(3)
C33 0.036(4) 0.039(3) 0.061(5) 0.000(3) -0.004(3) 0.014(3)
C34 0.035(3) 0.047(4) 0.058(5) 0.007(3) -0.001(3) 0.013(3)
C35 0.043(4) 0.046(4) 0.053(5) 0.002(3) -0.006(3) 0.013(3)
C36 0.044(4) 0.053(4) 0.055(5) 0.002(3) -0.002(3) 0.017(3)
C37 0.044(4) 0.042(4) 0.062(5) 0.008(4) -0.006(4) 0.013(3)
C38 0.041(4) 0.040(4) 0.054(5) -0.001(3) -0.003(3) 0.013(3)
C39 0.049(4) 0.046(4) 0.052(5) 0.003(3) -0.005(3) 0.019(3)
C40 0.042(4) 0.047(4) 0.049(5) 0.000(3) -0.010(3) 0.018(3)
C41 0.031(3) 0.045(4) 0.051(4) 0.001(3) -0.005(3) 0.015(3)
C42 0.053(4) 0.055(4) 0.057(5) -0.001(4) -0.016(4) 0.028(3)
C43 0.046(4) 0.072(5) 0.063(5) -0.001(4) -0.012(4) 0.026(4)
C44 0.058(5) 0.054(5) 0.065(6) 0.005(4) -0.032(4) 0.005(4)
C45 0.051(4) 0.046(4) 0.062(6) -0.006(3) -0.017(4) 0.013(3)
C46 0.039(4) 0.054(4) 0.046(4) 0.000(3) -0.007(3) 0.020(3)
N5 0.081(5) 0.108(6) 0.096(7) 0.037(5) 0.044(5) 0.053(5)
N6 0.113(6) 0.092(6) 0.071(5) 0.008(4) 0.007(4) 0.070(5)
N7 0.032(3) 0.096(6) 0.067(5) 0.007(5) 0.010(3) 0.012(3)
N8 0.046(4) 0.058(4) 0.064(5) 0.004(3) 0.003(3) 0.019(3)
C1 0.037(4) 0.134(10) 0.046(5) -0.007(6) 0.011(4) 0.019(5)
C2 0.041(4) 0.107(7) 0.074(7) 0.033(6) 0.020(4) 0.030(5)
C3 0.050(5) 0.107(7) 0.060(6) 0.003(5) 0.009(4) 0.040(5)
C4 0.032(4) 0.114(8) 0.081(7) 0.019(6) 0.009(4) 0.025(5)
C5 0.038(4) 0.090(7) 0.081(7) -0.001(5) -0.002(4) 0.017(4)
C6 0.031(4) 0.096(7) 0.083(8) 0.029(6) 0.004(4) 0.007(4)
C7 0.029(4) 0.122(9) 0.069(7) 0.014(6) 0.009(4) 0.013(5)
C8 0.031(4) 0.107(7) 0.077(7) 0.013(6) 0.013(4) 0.028(4)
C9 0.045(5) 0.095(7) 0.083(8) 0.023(6) 0.011(5) 0.005(5)
C10 0.114(7) 0.104(7) 0.118(8) 0.037(6) 0.050(6) 0.058(6)
C13 0.160(8) 0.113(7) 0.085(6) 0.033(5) 0.041(6) 0.103(7)
C16 0.035(4) 0.094(6) 0.070(6) 0.005(5) 0.005(4) 0.018(4)
C17 0.045(4) 0.061(5) 0.063(5) -0.001(4) -0.007(4) 0.017(4)
C18 0.061(5) 0.074(6) 0.102(8) 0.000(5) -0.018(5) 0.017(5)
C19 0.064(5) 0.071(6) 0.070(7) -0.011(5) -0.009(4) 0.023(4)
C20 0.056(4) 0.051(4) 0.046(4) 0.003(3) 0.002(3) 0.024(4)
C21 0.045(4) 0.053(4) 0.038(4) -0.003(3) -0.006(3) 0.026(3)
C22 0.043(4) 0.049(4) 0.037(4) -0.001(3) 0.002(3) 0.018(3)
C14 0.073(10) 0.059(8) 0.076(8) 0.025(6) 0.025(7) 0.033(7)
C15 0.065(9) 0.068(8) 0.095(12) 0.010(7) 0.015(8) 0.040(7)
C11 0.120(16) 0.155(19) 0.111(12) 0.056(12) 0.038(11) 0.095(15)
C12 0.125(16) 0.101(11) 0.100(12) 0.044(8) 0.030(10) 0.065(11)
_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 C40 1.285(10) . ?
N1 C41 1.452(9) . ?
N2 C39 1.272(9) 2_665 ?
N2 C46 1.444(9) . ?
N3 C31 1.469(10) . ?
N3 C32 1.252(10) . ?
N4 C25 1.271(8) . ?
N4 C26 1.462(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.398(9) 2_665 ?
C23 C24 1.391(9) . ?
C24 C23 1.398(9) 3_565 ?
C24 C25 1.453(9) . ?
C25 H25 0.9500 . ?
C26 H26 1.0000 . ?
C26 C27 1.524(12) . ?
C26 C31 1.514(11) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.495(13) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.452(19) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.537(16) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.537(10) . ?
C31 H31 1.0000 . ?
C32 H32 0.9500 . ?
C32 C33 1.469(11) . ?
C33 C34 1.417(10) . ?
C33 C38 1.398(11) . ?
C34 H34 0.9500 . ?
C34 C35 1.360(11) . ?
C35 C36 1.414(11) . ?
C35 C40 1.466(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.407(10) . ?
C37 C38 1.383(11) . ?
C37 C39 1.477(11) . ?
C38 H38 0.9500 . ?
C39 N2 1.273(9) 3_565 ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41 1.0000 . ?
C41 C42 1.528(10) . ?
C41 C46 1.533(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.503(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.508(13) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.537(11) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.505(10) . ?
C46 H46 1.0000 . ?
N5 C9 1.225(13) . ?
N5 C10 1.457(16) . ?
N6 C1 1.234(15) 2_765 ?
N6 C13 1.473(15) . ?
N7 C8 1.281(13) . ?
N7 C16 1.449(12) . ?
N8 C17 1.481(10) . ?
N8 C20 1.255(10) . ?
C1 N6 1.234(15) 3_675 ?
C1 H1 0.9500 . ?
C1 C2 1.516(16) . ?
C2 C3 1.371(14) . ?
C2 C7 1.384(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(15) . ?
C4 C5 1.416(14) . ?
C4 C8 1.486(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(14) . ?
C6 C7 1.406(17) . ?
C6 C9 1.477(17) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C13 1.501(19) . ?
C10 C11 1.59(3) . ?
C10 C12 1.30(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.39(2) . ?
C13 C15 1.655(19) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.540(13) . ?
C17 C18 1.513(13) . ?
C17 C19 1.529(13) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C22 1.472(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.395(10) . ?
C21 C22 1.383(10) 3_675 ?
C22 C21 1.383(10) 2_765 ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O9 H9A 0.8400 . ?
O9 C53 1.36(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.48(2) . ?
C53 H53 1.0000 . ?
C53 C54 1.49(3) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O2 C59 1.45(3) 3_675 ?
O2 C59 1.45(3) 2_765 ?
O2 C59 1.45(3) . ?
C58 C59 1.52(3) . ?
C59 C59 1.40(7) 3_675 ?
C59 C59 1.40(7) 2_765 ?
C59 C60 1.53(3) . ?
C60 C58 2.01(6) 2_765 ?
C60 C58 2.01(6) 3_675 ?
C60 C59 1.53(3) 2_765 ?
C60 C59 1.53(3) 3_675 ?
Cl1 C61 1.62(2) . ?
Cl1 C61 1.62(2) 3_565 ?
Cl1 C61 1.62(2) 2_665 ?
Cl1 Cl3 1.62(2) . ?
Cl1 Cl3 1.62(2) 2_665 ?
Cl1 Cl3 1.62(2) 3_565 ?
Cl2 C61 1.72(2) . ?
Cl2 Cl3 1.72(2) . ?
Cl3 Cl3 1.45(3) 2_665 ?
O3 H3A 0.8400 . ?
O3 C56 1.36(2) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C55 C56 1.54(3) . ?
C56 H56 1.0000 . ?
C56 C57 1.50(3) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
O1 H1A 0.8400 . ?
O1 C47 1.49(2) . ?
C47 H47 1.0000 . ?
C47 C48 1.50(2) . ?
C47 C49 1.51(2) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
O4 C50 1.73(3) 2_665 ?
O4 C50 1.50(2) . ?
C50 O4 1.73(4) 3_565 ?
C50 C50 1.28(4) 2_665 ?
C50 C50 1.28(4) 3_565 ?
C50 C51 1.43(3) . ?
O7 O7 1.49(4) 3 ?
O7 O7 1.49(4) 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
C40 N1 C41 117.4(6) . . ?
C39 N2 C46 117.1(6) 2_665 . ?
C32 N3 C31 117.4(6) . . ?
C25 N4 C26 117.8(5) . . ?
C24 C23 H23 119.3 2_665 . ?
C24 C23 H23 119.3 . . ?
C24 C23 C24 121.4(6) . 2_665 ?
C23 C24 C23 118.6(6) . 3_565 ?
C23 C24 C25 119.3(5) . . ?
C23 C24 C25 122.0(5) 3_565 . ?
N4 C25 C24 122.9(6) . . ?
N4 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
N4 C26 H26 109.3 . . ?
N4 C26 C27 108.7(6) . . ?
N4 C26 C31 108.8(5) . . ?
C27 C26 H26 109.3 . . ?
C31 C26 H26 109.3 . . ?
C31 C26 C27 111.4(6) . . ?
C26 C27 H27A 109.7 . . ?
C26 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 C26 110.0(9) . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
C27 C28 H28A 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C29 C28 C27 110.1(9) . . ?
C29 C28 H28A 109.7 . . ?
C29 C28 H28B 109.7 . . ?
C28 C29 H29A 108.9 . . ?
C28 C29 H29B 108.9 . . ?
C28 C29 C30 113.5(9) . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C29 C30 H30A 109.9 . . ?
C29 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
C31 C30 C29 109.0(8) . . ?
C31 C30 H30A 109.9 . . ?
C31 C30 H30B 109.9 . . ?
N3 C31 C26 108.8(5) . . ?
N3 C31 C30 109.3(7) . . ?
N3 C31 H31 109.9 . . ?
C26 C31 C30 109.1(7) . . ?
C26 C31 H31 109.9 . . ?
C30 C31 H31 109.9 . . ?
N3 C32 H32 118.9 . . ?
N3 C32 C33 122.3(6) . . ?
C33 C32 H32 118.9 . . ?
C34 C33 C32 120.8(7) . . ?
C38 C33 C32 120.7(6) . . ?
C38 C33 C34 118.4(7) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 C33 120.9(7) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 C36 120.9(7) . . ?
C34 C35 C40 117.7(7) . . ?
C36 C35 C40 121.3(7) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 C35 118.3(7) . . ?
C37 C36 H36 120.8 . . ?
C36 C37 C39 117.2(7) . . ?
C38 C37 C36 120.6(7) . . ?
C38 C37 C39 122.1(6) . . ?
C33 C38 H38 119.6 . . ?
C37 C38 C33 120.8(6) . . ?
C37 C38 H38 119.6 . . ?
N2 C39 C37 122.9(7) 3_565 . ?
N2 C39 H39 118.5 3_565 . ?
C37 C39 H39 118.5 . . ?
N1 C40 C35 122.7(7) . . ?
N1 C40 H40 118.6 . . ?
C35 C40 H40 118.6 . . ?
N1 C41 H41 109.0 . . ?
N1 C41 C42 108.7(6) . . ?
N1 C41 C46 110.0(5) . . ?
C42 C41 H41 109.0 . . ?
C42 C41 C46 111.0(6) . . ?
C46 C41 H41 109.0 . . ?
C41 C42 H42A 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C43 C42 C41 112.1(6) . . ?
C43 C42 H42A 109.2 . . ?
C43 C42 H42B 109.2 . . ?
C42 C43 H43A 109.2 . . ?
C42 C43 H43B 109.2 . . ?
C42 C43 C44 111.9(6) . . ?
H43A C43 H43B 107.9 . . ?
C44 C43 H43A 109.2 . . ?
C44 C43 H43B 109.2 . . ?
C43 C44 H44A 109.4 . . ?
C43 C44 H44B 109.4 . . ?
C43 C44 C45 111.2(7) . . ?
H44A C44 H44B 108.0 . . ?
C45 C44 H44A 109.4 . . ?
C45 C44 H44B 109.4 . . ?
C44 C45 H45A 109.4 . . ?
C44 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C46 C45 C44 111.3(6) . . ?
C46 C45 H45A 109.4 . . ?
C46 C45 H45B 109.4 . . ?
N2 C46 C41 109.1(6) . . ?
N2 C46 C45 110.9(6) . . ?
N2 C46 H46 108.9 . . ?
C41 C46 H46 108.9 . . ?
C45 C46 C41 110.1(6) . . ?
C45 C46 H46 108.9 . . ?
C9 N5 C10 117.4(12) . . ?
C1 N6 C13 117.2(11) 2_765 . ?
C8 N7 C16 115.9(9) . . ?
C20 N8 C17 120.0(7) . . ?
N6 C1 H1 119.0 3_675 . ?
N6 C1 C2 122.0(10) 3_675 . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 120.8(11) . . ?
C3 C2 C7 119.4(11) . . ?
C7 C2 C1 119.8(11) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(11) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 119.5(10) . . ?
C3 C4 C8 119.8(10) . . ?
C5 C4 C8 120.8(11) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.1(10) . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C7 119.7(11) . . ?
C5 C6 C9 116.7(11) . . ?
C7 C6 C9 123.5(10) . . ?
C2 C7 C6 120.7(10) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
N7 C8 C4 121.1(10) . . ?
N7 C8 H8 119.4 . . ?
C4 C8 H8 119.4 . . ?
N5 C9 C6 121.7(12) . . ?
N5 C9 H9 119.2 . . ?
C6 C9 H9 119.2 . . ?
N5 C10 H10A 109.6 . . ?
N5 C10 H10B 109.6 . . ?
N5 C10 C13 110.2(11) . . ?
N5 C10 C11 110.4(14) . . ?
H10A C10 H10B 108.1 . . ?
C13 C10 H10A 109.6 . . ?
C13 C10 H10B 109.6 . . ?
C13 C10 C11 85.0(14) . . ?
C12 C10 N5 132.7(17) . . ?
C12 C10 C13 92.7(16) . . ?
C12 C10 C11 112.5(18) . . ?
N6 C13 C10 109.5(10) . . ?
N6 C13 H13A 109.8 . . ?
N6 C13 H13B 109.8 . . ?
N6 C13 C15 106.9(10) . . ?
C10 C13 H13A 109.8 . . ?
C10 C13 H13B 109.8 . . ?
C10 C13 C15 96.0(12) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 N6 128.1(14) . . ?
C14 C13 C10 101.5(12) . . ?
C14 C13 C15 110.0(11) . . ?
N7 C16 H16A 109.6 . . ?
N7 C16 H16B 109.6 . . ?
N7 C16 C17 110.2(7) . . ?
H16A C16 H16B 108.1 . . ?
C17 C16 H16A 109.6 . . ?
C17 C16 H16B 109.6 . . ?
N8 C17 C16 104.8(7) . . ?
N8 C17 C18 117.4(7) . . ?
N8 C17 C19 105.4(7) . . ?
C18 C17 C16 109.5(8) . . ?
C18 C17 C19 111.3(7) . . ?
C19 C17 C16 107.9(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N8 C20 H20 119.1 . . ?
N8 C20 C22 121.7(7) . . ?
C22 C20 H20 119.1 . . ?
C22 C21 H21 119.5 3_675 . ?
C22 C21 H21 119.5 . . ?
C22 C21 C22 121.0(7) 3_675 . ?
C21 C22 C20 122.2(6) . . ?
C21 C22 C20 118.7(6) 2_765 . ?
C21 C22 C21 119.0(7) 2_765 . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C53 O9 H9A 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
O9 C53 C52 99(3) . . ?
O9 C53 H53 112.4 . . ?
O9 C53 C54 108(4) . . ?
C52 C53 H53 112.4 . . ?
C52 C53 C54 112(3) . . ?
C54 C53 H53 112.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C59 O2 C59 58(3) 2_765 3_675 ?
C59 O2 C59 58(3) . 3_675 ?
C59 O2 C59 58(3) 2_765 . ?
O2 C59 C58 136(5) . . ?
O2 C59 C60 114(3) . . ?
C58 C59 C60 83(3) . . ?
C59 C59 O2 61.1(15) 2_765 . ?
C59 C59 O2 61.1(15) 3_675 . ?
C59 C59 C58 98(6) 3_675 . ?
C59 C59 C58 144(4) 2_765 . ?
C59 C59 C59 59.998(17) 2_765 3_675 ?
C59 C59 C60 62.7(14) 3_675 . ?
C59 C59 C60 62.7(14) 2_765 . ?
C58 C60 C58 112.8(18) 2_765 3_675 ?
C59 C60 C58 48.4(17) 2_765 2_765 ?
C59 C60 C58 103(3) . 3_675 ?
C59 C60 C58 76(3) 2_765 3_675 ?
C59 C60 C58 48.4(17) 3_675 3_675 ?
C59 C60 C58 103(3) 3_675 2_765 ?
C59 C60 C58 76(3) . 2_765 ?
C59 C60 C59 55(3) . 3_675 ?
C59 C60 C59 55(3) 2_765 3_675 ?
C59 C60 C59 55(3) 2_765 . ?
C61 Cl1 C61 53.2(15) 2_665 3_565 ?
C61 Cl1 C61 53.2(15) . 3_565 ?
C61 Cl1 C61 53.2(15) 2_665 . ?
Cl3 Cl1 Cl3 53.2(15) . 3_565 ?
Cl3 Cl1 Cl3 53.2(15) 2_665 3_565 ?
Cl3 Cl1 Cl3 53.2(15) 2_665 . ?
Cl1 C61 Cl2 133.4(16) . . ?
Cl1 Cl3 Cl2 133.4(16) . . ?
Cl3 Cl3 Cl1 63.4(7) 2_665 . ?
Cl3 Cl3 Cl2 153(3) 2_665 . ?
C56 O3 H3A 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
O3 C56 C55 112(3) . . ?
O3 C56 H56 98.2 . . ?
O3 C56 C57 120(3) . . ?
C55 C56 H56 98.2 . . ?
C57 C56 C55 122(3) . . ?
C57 C56 H56 98.2 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C47 O1 H1A 109.5 . . ?
O1 C47 H47 109.0 . . ?
O1 C47 C48 114.8(17) . . ?
O1 C47 C49 110.1(17) . . ?
C48 C47 H47 109.0 . . ?
C48 C47 C49 104.9(18) . . ?
C49 C47 H47 109.0 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C50 O4 C50 46.0(16) . 2_665 ?
O4 C50 O4 75(2) . 3_565 ?
C50 C50 O4 95.4(14) 2_665 3_565 ?
C50 C50 O4 107.8(14) 3_565 . ?
C50 C50 O4 57.3(14) 3_565 3_565 ?
C50 C50 O4 77(2) 2_665 . ?
C50 C50 C50 60.001(4) 3_565 2_665 ?
C50 C50 C51 164(3) 2_665 . ?
C50 C50 C51 127(4) 3_565 . ?
C51 C50 O4 101(3) . 3_565 ?
C51 C50 O4 111(3) . . ?
O7 O7 O7 59.998(4) 2 3 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C41 C42 C43 -175.7(7) . . . . ?
N1 C41 C46 N2 -61.6(7) . . . . ?
N1 C41 C46 C45 176.4(6) . . . . ?
N3 C32 C33 C34 5.7(10) . . . . ?
N3 C32 C33 C38 -171.9(7) . . . . ?
N4 C26 C27 C28 -178.9(8) . . . . ?
N4 C26 C31 N3 -63.5(7) . . . . ?
N4 C26 C31 C30 177.4(6) . . . . ?
C23 C24 C25 N4 4.1(11) 3_565 . . . ?
C23 C24 C25 N4 -172.2(7) . . . . ?
C24 C23 C24 C23 0.8(13) 2_665 . . 3_565 ?
C24 C23 C24 C25 177.2(5) 2_665 . . . ?
C25 N4 C26 C27 -116.3(7) . . . . ?
C25 N4 C26 C31 122.2(7) . . . . ?
C26 N4 C25 C24 178.0(7) . . . . ?
C26 C27 C28 C29 57.9(12) . . . . ?
C27 C26 C31 N3 176.7(6) . . . . ?
C27 C26 C31 C30 57.6(8) . . . . ?
C27 C28 C29 C30 -58.4(12) . . . . ?
C28 C29 C30 C31 56.9(11) . . . . ?
C29 C30 C31 N3 -173.4(8) . . . . ?
C29 C30 C31 C26 -54.5(10) . . . . ?
C31 N3 C32 C33 179.3(6) . . . . ?
C31 C26 C27 C28 -59.0(9) . . . . ?
C32 N3 C31 C26 117.4(6) . . . . ?
C32 N3 C31 C30 -123.6(7) . . . . ?
C32 C33 C34 C35 -175.9(7) . . . . ?
C32 C33 C38 C37 176.8(6) . . . . ?
C33 C34 C35 C36 -2.1(11) . . . . ?
C33 C34 C35 C40 177.1(6) . . . . ?
C34 C33 C38 C37 -0.9(10) . . . . ?
C34 C35 C36 C37 1.5(11) . . . . ?
C34 C35 C40 N1 -174.3(7) . . . . ?
C35 C36 C37 C38 -0.6(11) . . . . ?
C35 C36 C37 C39 176.2(6) . . . . ?
C36 C35 C40 N1 4.9(11) . . . . ?
C36 C37 C38 C33 0.3(11) . . . . ?
C36 C37 C39 N2 -172.5(7) . . . 3_565 ?
C38 C33 C34 C35 1.8(10) . . . . ?
C38 C37 C39 N2 4.3(11) . . . 3_565 ?
C39 N2 C46 C41 116.1(7) 2_665 . . . ?
C39 N2 C46 C45 -122.4(7) 2_665 . . . ?
C39 C37 C38 C33 -176.3(7) . . . . ?
C40 N1 C41 C42 -118.9(7) . . . . ?
C40 N1 C41 C46 119.4(7) . . . . ?
C40 C35 C36 C37 -177.7(7) . . . . ?
C41 N1 C40 C35 175.7(6) . . . . ?
C41 C42 C43 C44 53.6(10) . . . . ?
C42 C41 C46 N2 178.1(6) . . . . ?
C42 C41 C46 C45 56.1(8) . . . . ?
C42 C43 C44 C45 -53.8(10) . . . . ?
C43 C44 C45 C46 56.2(10) . . . . ?
C44 C45 C46 N2 -177.8(7) . . . . ?
C44 C45 C46 C41 -57.0(9) . . . . ?
C46 C41 C42 C43 -54.6(9) . . . . ?
N5 C10 C13 N6 -63.6(13) . . . . ?
N5 C10 C13 C14 74.1(12) . . . . ?
N5 C10 C13 C15 -174.0(11) . . . . ?
N6 C1 C2 C3 -3.2(12) 3_675 . . . ?
N6 C1 C2 C7 178.6(8) 3_675 . . . ?
N7 C16 C17 N8 -66.8(9) . . . . ?
N7 C16 C17 C18 59.9(9) . . . . ?
N7 C16 C17 C19 -178.8(7) . . . . ?
N8 C20 C22 C21 7.6(12) . . . . ?
N8 C20 C22 C21 -168.0(7) . . . 2_765 ?
C1 N6 C13 C10 127.7(11) 2_765 . . . ?
C1 N6 C13 C14 4.6(18) 2_765 . . . ?
C1 N6 C13 C15 -129.3(11) 2_765 . . . ?
C1 C2 C3 C4 -178.8(7) . . . . ?
C1 C2 C7 C6 179.3(7) . . . . ?
C2 C3 C4 C5 0.3(12) . . . . ?
C2 C3 C4 C8 179.6(7) . . . . ?
C3 C2 C7 C6 1.1(12) . . . . ?
C3 C4 C5 C6 -0.5(12) . . . . ?
C3 C4 C8 N7 -176.5(7) . . . . ?
C4 C5 C6 C7 1.0(12) . . . . ?
C4 C5 C6 C9 -179.9(7) . . . . ?
C5 C4 C8 N7 2.8(11) . . . . ?
C5 C6 C7 C2 -1.3(12) . . . . ?
C5 C6 C9 N5 176.7(9) . . . . ?
C7 C2 C3 C4 -0.6(12) . . . . ?
C7 C6 C9 N5 -4.3(13) . . . . ?
C8 N7 C16 C17 126.4(8) . . . . ?
C8 C4 C5 C6 -179.8(7) . . . . ?
C9 N5 C10 C13 131.0(11) . . . . ?
C9 N5 C10 C11 -136.9(16) . . . . ?
C9 N5 C10 C12 17(3) . . . . ?
C9 C6 C7 C2 179.7(7) . . . . ?
C10 N5 C9 C6 177.4(8) . . . . ?
C16 N7 C8 C4 -179.7(6) . . . . ?
C17 N8 C20 C22 176.8(7) . . . . ?
C20 N8 C17 C16 120.0(8) . . . . ?
C20 N8 C17 C18 -1.7(12) . . . . ?
C20 N8 C17 C19 -126.3(8) . . . . ?
C22 C21 C22 C20 -176.0(5) 3_675 . . . ?
C22 C21 C22 C21 -0.4(14) 3_675 . . 2_765 ?
C11 C10 C13 N6 -173.5(15) . . . . ?
C12 C10 C13 N6 74.1(15) . . . . ?
O2 C59 C60 C58 -83(3) . . . 2_765 ?
O2 C59 C60 C58 28(5) . . . 3_675 ?
O2 C59 C60 C59 -34.2(5) . . . 2_765 ?
O2 C59 C60 C59 34.2(5) . . . 3_675 ?
C58 C59 C60 C58 -109.5(17) . . . 3_675 ?
C58 C59 C60 C58 140(3) . . . 2_765 ?
C58 C59 C60 C59 -103(6) . . . 3_675 ?
C58 C59 C60 C59 -171(6) . . . 2_765 ?
C59 O2 C59 C58 70(8) 3_675 . . . ?
C59 O2 C59 C58 140(7) 2_765 . . . ?
C59 O2 C59 C59 69.7(12) 2_765 . . 3_675 ?
C59 O2 C59 C59 -69.7(12) 3_675 . . 2_765 ?
C59 O2 C59 C60 34.8(6) 2_765 . . . ?
C59 O2 C59 C60 -34.8(6) 3_675 . . . ?
C59 C59 C60 C58 -49(3) 2_765 . . 2_765 ?
C59 C59 C60 C58 -117(4) 3_675 . . 2_765 ?
C59 C59 C60 C58 62(5) 2_765 . . 3_675 ?
C59 C59 C60 C58 -7(5) 3_675 . . 3_675 ?
C59 C59 C60 C59 68.5(10) 2_765 . . 3_675 ?
C59 C59 C60 C59 -68.5(10) 3_675 . . 2_765 ?
C61 Cl1 C61 Cl2 153(5) 2_665 . . . ?
C61 Cl1 C61 Cl2 -139(5) 3_565 . . . ?
Cl3 Cl1 Cl3 Cl2 -139(5) 3_565 . . . ?
Cl3 Cl1 Cl3 Cl2 153(5) 2_665 . . . ?
Cl3 Cl1 Cl3 Cl3 68.0(5) 3_565 . . 2_665 ?
C50 O4 C50 O4 99.5(17) 2_665 . . 3_565 ?
C50 O4 C50 C50 52.0(8) 2_665 . . 3_565 ?
C50 O4 C50 C51 -165(4) 2_665 . . . ?
_shelx_res_file
;
TITL THL_386_D6 in P6(3)
CELL 0.71073 17.5938 17.5938 32.2344 90 90 120
ZERR 2 0.0007 0.0007 0.0013 0 0 0
LATT -1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SFAC C H Cl N O
UNIT 302 428 4 48 20
EQIV $1 1+Y-X,1-X,+Z
EQIV $2 1-Y,+X-Y,+Z
EQIV $3 1-Y,1+X-Y,+Z
EQIV $4 +Y-X,1-X,+Z
EQIV $5 -2-Y,-1+X-Y,+Z
EQIV $6 -1+Y-X,-2-X,+Z
EQIV $7 5-X,5-Y,0.5+Z
EQIV $8 3+Y-X,5-X,+Z
DFIX 1.74 Cl2 C61 Cl3 Cl1
DFIX 1.43 O4 C50 O1_$8 C47_$8 O9_$8 C53_$8 O3_$7 C56_$7 O2 C59
DFIX 1.54 C51 C50 C59 C58 C60 C59 C53_$8 C52_$8 C54_$8 C53_$8 C57_$7 C56_$7 =
C56_$7 C55_$7 C49_$8 C47_$8 C48_$8 C47_$8
RIGU N6 C13 C14 C15 C10 C12 C11 N5
EADP C61 Cl3
EADP C59 O2 C58 C60
EXYZ C61 Cl3
L.S. 20
PLAN 20
TEMP -173.15
FREE C13 C12
FREE Cl3 C61_$2
FREE Cl3 C61_$1
FREE Cl3 Cl3_$2
FREE Cl3 Cl3_$1
FREE Cl3 Cl3_$4
FREE C58 C60_$5
FREE C58 C60_$6
FREE C58 C60
FREE C61 C61_$2
FREE C61 C61_$1
FREE C61 C61_$3
FREE C61 C61_$4
FREE C61 Cl3_$4
BOND
MORE -1
CONF
BOND $H
fmap 2
acta 46.3
REM
REM
REM
WGHT 0.182000 4.022700
FVAR 0.12880 0.52507
N1 4 0.618340 0.723155 0.723596 11.00000 0.03670 0.04692 =
0.06383 0.00852 -0.00622 0.01584
N2 4 0.643615 0.896039 0.713074 11.00000 0.04014 0.04532 =
0.05300 -0.00217 -0.00686 0.01937
N3 4 0.517878 0.498648 0.557148 11.00000 0.03787 0.04758 =
0.06190 0.00624 -0.00164 0.02236
N4 4 0.445672 0.536171 0.485784 11.00000 0.04177 0.04557 =
0.04823 0.00031 0.00200 0.02468
C23 1 0.421744 0.728913 0.492188 11.00000 0.03675 0.03931 =
0.04299 0.00004 0.00408 0.01599
AFIX 43
H23 2 0.482409 0.771705 0.491945 11.00000 -1.20000
AFIX 0
C24 1 0.396672 0.640370 0.492361 11.00000 0.04128 0.03900 =
0.03747 0.00059 -0.00054 0.02135
C25 1 0.463644 0.615207 0.490272 11.00000 0.03987 0.04026 =
0.04761 0.00338 0.00467 0.01733
AFIX 43
H25 2 0.523492 0.659787 0.492351 11.00000 -1.20000
AFIX 0
C26 1 0.518937 0.519453 0.482717 11.00000 0.03804 0.04298 =
0.05924 -0.00397 0.01012 0.02093
AFIX 13
H26 2 0.575415 0.575924 0.486222 11.00000 -1.20000
AFIX 0
C27 1 0.517014 0.481535 0.439951 11.00000 0.06898 0.08329 =
0.06693 -0.00985 0.02035 0.03949
AFIX 23
H27A 2 0.460129 0.426979 0.435814 11.00000 -1.20000
H27B 2 0.523010 0.524069 0.418282 11.00000 -1.20000
AFIX 0
C28 1 0.590290 0.462107 0.436128 11.00000 0.08649 0.09244 =
0.12250 -0.01684 0.02549 0.05722
AFIX 23
H28A 2 0.587883 0.436177 0.408563 11.00000 -1.20000
H28B 2 0.647290 0.517246 0.438562 11.00000 -1.20000
AFIX 0
C29 1 0.583228 0.401374 0.468430 11.00000 0.06568 0.10613 =
0.17643 -0.06063 -0.00414 0.06360
AFIX 23
H29A 2 0.632341 0.389495 0.465455 11.00000 -1.20000
H29B 2 0.527822 0.345161 0.464531 11.00000 -1.20000
AFIX 0
C30 1 0.584834 0.435322 0.512531 11.00000 0.06370 0.07019 =
0.12122 -0.00399 -0.00772 0.04908
AFIX 23
H30A 2 0.577011 0.390198 0.533112 11.00000 -1.20000
H30B 2 0.642079 0.488749 0.517802 11.00000 -1.20000
AFIX 0
C31 1 0.510388 0.456495 0.516852 11.00000 0.03587 0.04596 =
0.07241 -0.01121 -0.00145 0.02274
AFIX 13
H31 2 0.452269 0.401313 0.514749 11.00000 -1.20000
AFIX 0
C32 1 0.452728 0.463482 0.580775 11.00000 0.04682 0.03829 =
0.05756 -0.00428 -0.01220 0.01817
AFIX 43
H32 2 0.401439 0.412003 0.571719 11.00000 -1.20000
AFIX 0
C33 1 0.452852 0.499072 0.622014 11.00000 0.03624 0.03936 =
0.06060 0.00022 -0.00403 0.01450
C34 1 0.524723 0.579891 0.635334 11.00000 0.03473 0.04700 =
0.05757 0.00723 -0.00100 0.01282
AFIX 43
H34 2 0.571655 0.613292 0.616705 11.00000 -1.20000
AFIX 0
C35 1 0.527494 0.610335 0.674393 11.00000 0.04314 0.04559 =
0.05346 0.00239 -0.00566 0.01329
C36 1 0.457384 0.563615 0.702428 11.00000 0.04426 0.05337 =
0.05455 0.00240 -0.00216 0.01655
AFIX 43
H36 2 0.458783 0.585633 0.729498 11.00000 -1.20000
AFIX 0
C37 1 0.385497 0.483685 0.689211 11.00000 0.04379 0.04241 =
0.06240 0.00809 -0.00571 0.01273
C38 1 0.383473 0.452359 0.649632 11.00000 0.04070 0.04037 =
0.05377 -0.00071 -0.00281 0.01260
AFIX 43
H38 2 0.334340 0.398446 0.641109 11.00000 -1.20000
AFIX 0
C39 1 0.315811 0.433460 0.719953 11.00000 0.04860 0.04649 =
0.05158 0.00307 -0.00475 0.01879
AFIX 43
H39 2 0.318437 0.459881 0.746015 11.00000 -1.20000
AFIX 0
C40 1 0.605980 0.692367 0.686528 11.00000 0.04225 0.04660 =
0.04883 0.00000 -0.00960 0.01819
AFIX 43
H40 2 0.649502 0.724068 0.666134 11.00000 -1.20000
AFIX 0
C41 1 0.701578 0.801609 0.732363 11.00000 0.03145 0.04460 =
0.05095 0.00093 -0.00523 0.01462
AFIX 13
H41 2 0.738127 0.820059 0.706596 11.00000 -1.20000
AFIX 0
C42 1 0.749196 0.780131 0.765980 11.00000 0.05262 0.05472 =
0.05685 -0.00140 -0.01596 0.02834
AFIX 23
H42A 2 0.710172 0.755108 0.790350 11.00000 -1.20000
H42B 2 0.762409 0.735202 0.755347 11.00000 -1.20000
AFIX 0
C43 1 0.833218 0.859754 0.779263 11.00000 0.04556 0.07176 =
0.06271 -0.00065 -0.01215 0.02617
AFIX 23
H43A 2 0.875714 0.879440 0.756045 11.00000 -1.20000
H43B 2 0.858780 0.843930 0.802789 11.00000 -1.20000
AFIX 0
C44 1 0.818840 0.934043 0.792141 11.00000 0.05784 0.05391 =
0.06538 0.00495 -0.03247 0.00545
AFIX 23
H44A 2 0.876190 0.986778 0.798137 11.00000 -1.20000
H44B 2 0.783326 0.917596 0.817850 11.00000 -1.20000
AFIX 0
C45 1 0.771612 0.955623 0.757969 11.00000 0.05120 0.04625 =
0.06215 -0.00557 -0.01713 0.01310
AFIX 23
H45A 2 0.760416 1.002411 0.767852 11.00000 -1.20000
H45B 2 0.809834 0.977880 0.733192 11.00000 -1.20000
AFIX 0
C46 1 0.685921 0.875992 0.746239 11.00000 0.03919 0.05449 =
0.04558 -0.00008 -0.00722 0.01976
AFIX 13
H46 2 0.646372 0.856031 0.770997 11.00000 -1.20000
AFIX 0
N5 4 0.767878 0.710276 0.614510 11.00000 0.08122 0.10771 =
0.09604 0.03708 0.04395 0.05254
N6 4 0.921098 0.691487 0.606288 11.00000 0.11283 0.09210 =
0.07067 0.00780 0.00690 0.07017
N7 4 0.644186 0.816080 0.450058 11.00000 0.03215 0.09609 =
0.06652 0.00716 0.00989 0.01173
N8 4 0.758710 0.885219 0.379834 11.00000 0.04572 0.05756 =
0.06415 0.00397 0.00287 0.01896
C1 1 0.772871 1.012340 0.616063 11.00000 0.03678 0.13447 =
0.04621 -0.00723 0.01083 0.01907
AFIX 43
H1 2 0.789262 1.007188 0.643549 11.00000 -1.20000
AFIX 0
C2 1 0.750546 0.938553 0.585522 11.00000 0.04149 0.10719 =
0.07428 0.03261 0.01986 0.02986
C3 1 0.722437 0.941482 0.546202 11.00000 0.05005 0.10656 =
0.06015 0.00265 0.00869 0.03974
AFIX 43
H3 2 0.718129 0.991049 0.537986 11.00000 -1.20000
AFIX 0
C4 1 0.700138 0.873801 0.518127 11.00000 0.03190 0.11439 =
0.08129 0.01891 0.00882 0.02543
C5 1 0.706034 0.799557 0.530252 11.00000 0.03793 0.09036 =
0.08146 -0.00067 -0.00167 0.01720
AFIX 43
H5 2 0.690537 0.752478 0.511435 11.00000 -1.20000
AFIX 0
C6 1 0.734770 0.796475 0.570017 11.00000 0.03075 0.09644 =
0.08338 0.02890 0.00382 0.00730
C7 1 0.756119 0.866065 0.597717 11.00000 0.02939 0.12182 =
0.06893 0.01394 0.00930 0.01285
AFIX 43
H7 2 0.774567 0.863293 0.625098 11.00000 -1.20000
AFIX 0
C8 1 0.669400 0.879447 0.475915 11.00000 0.03102 0.10729 =
0.07717 0.01285 0.01332 0.02777
AFIX 43
H8 2 0.668434 0.930955 0.467969 11.00000 -1.20000
AFIX 0
C9 1 0.739677 0.717504 0.580895 11.00000 0.04521 0.09459 =
0.08335 0.02302 0.01061 0.00453
AFIX 43
H9 2 0.720465 0.671127 0.561317 11.00000 -1.20000
AFIX 0
C10 1 0.766450 0.628217 0.622874 11.00000 0.11395 0.10359 =
0.11782 0.03655 0.04971 0.05831
PART 1
AFIX 23
H10A 2 0.751833 0.592981 0.597122 21.00000 -1.20000
H10B 2 0.720694 0.593923 0.643771 21.00000 -1.20000
AFIX 0
PART 0
C13 1 0.854279 0.646476 0.638679 11.00000 0.16033 0.11274 =
0.08492 0.03319 0.04075 0.10274
PART 2
AFIX 23
H13A 2 0.870156 0.683776 0.663781 -21.00000 -1.20000
H13B 2 0.851599 0.590667 0.646282 -21.00000 -1.20000
AFIX 0
PART 0
C16 1 0.616200 0.829655 0.409834 11.00000 0.03516 0.09414 =
0.07011 0.00549 0.00482 0.01770
AFIX 23
H16A 2 0.627071 0.890458 0.407933 11.00000 -1.20000
H16B 2 0.552429 0.788968 0.406434 11.00000 -1.20000
AFIX 0
C17 1 0.666634 0.813595 0.375114 11.00000 0.04517 0.06090 =
0.06296 -0.00094 -0.00652 0.01657
C18 1 0.649057 0.720322 0.377792 11.00000 0.06071 0.07438 =
0.10165 -0.00050 -0.01829 0.01671
AFIX 137
H18A 2 0.661146 0.708588 0.406032 11.00000 -1.50000
H18B 2 0.687142 0.712440 0.358190 11.00000 -1.50000
H18C 2 0.587498 0.679516 0.370890 11.00000 -1.50000
AFIX 0
C19 1 0.635969 0.830757 0.333583 11.00000 0.06407 0.07120 =
0.07039 -0.01078 -0.00875 0.02264
AFIX 137
H19A 2 0.663491 0.816191 0.310867 11.00000 -1.50000
H19B 2 0.652747 0.892814 0.331751 11.00000 -1.50000
H19C 2 0.572012 0.794266 0.331509 11.00000 -1.50000
AFIX 0
C20 1 0.818256 0.867342 0.386788 11.00000 0.05575 0.05118 =
0.04585 0.00292 0.00156 0.02360
AFIX 43
H20 2 0.802994 0.807767 0.390358 11.00000 -1.20000
AFIX 0
C21 1 0.937260 1.025380 0.389458 11.00000 0.04519 0.05306 =
0.03772 -0.00291 -0.00591 0.02649
AFIX 43
H21 2 0.894029 1.042674 0.389325 11.00000 -1.20000
AFIX 0
C22 1 0.911132 0.936325 0.389556 11.00000 0.04311 0.04950 =
0.03694 -0.00116 0.00220 0.01776
PART 1
C14 1 0.853427 0.674580 0.678828 21.00000 0.07268 0.05869 =
0.07584 0.02513 0.02526 0.03292
AFIX 137
H14A 2 0.845724 0.726006 0.677959 21.00000 -1.50000
H14B 2 0.909088 0.690241 0.692538 21.00000 -1.50000
H14C 2 0.804868 0.627333 0.694330 21.00000 -1.50000
AFIX 0
C15 1 0.830843 0.542905 0.639167 21.00000 0.06501 0.06827 =
0.09490 0.00951 0.01475 0.04031
AFIX 137
H15A 2 0.878945 0.538970 0.652358 21.00000 -1.50000
H15B 2 0.823187 0.521018 0.610635 21.00000 -1.50000
H15C 2 0.776521 0.507402 0.654795 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C11 1 0.733603 0.596099 0.668825 -21.00000 0.12038 0.15457 =
0.11123 0.05593 0.03828 0.09514
AFIX 137
H11A 2 0.672105 0.580938 0.671451 -21.00000 -1.50000
H11B 2 0.769594 0.643174 0.688395 -21.00000 -1.50000
H11C 2 0.738835 0.544360 0.674993 -21.00000 -1.50000
AFIX 0
C12 1 0.758142 0.564902 0.598983 -21.00000 0.12490 0.10129 =
0.10019 0.04383 0.02984 0.06474
AFIX 137
H12A 2 0.810395 0.586067 0.581464 -21.00000 -1.50000
H12B 2 0.706144 0.545006 0.581401 -21.00000 -1.50000
H12C 2 0.751627 0.515940 0.616085 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
O9 5 0.605768 0.485674 0.758590 10.50000 0.26263
AFIX 83
H9A 2 0.589760 0.474318 0.783459 10.50000 -1.50000
AFIX 0
C52 1 0.478606 0.367769 0.757684 10.50000 0.13314
AFIX 137
H52A 2 0.442465 0.392241 0.748026 10.50000 -1.50000
H52B 2 0.488677 0.377702 0.787592 10.50000 -1.50000
H52C 2 0.448233 0.304596 0.752009 10.50000 -1.50000
AFIX 0
C53 1 0.563750 0.411162 0.735698 10.50000 0.13967
AFIX 13
H53 2 0.557692 0.423197 0.705922 10.50000 -1.20000
AFIX 0
C54 1 0.611772 0.361895 0.740876 10.50000 0.21577
AFIX 33
H54A 2 0.582610 0.307633 0.724591 10.50000 -1.50000
H54B 2 0.672354 0.398183 0.731203 10.50000 -1.50000
H54C 2 0.611900 0.347503 0.770237 10.50000 -1.50000
AFIX 0
O2 5 1.000000 1.000000 0.608126 10.16667 0.09094
C58 1 0.901084 0.881441 0.668505 10.16667 0.09094
C59 1 0.982562 0.947852 0.645372 10.16667 0.09094
C60 1 1.000000 1.000000 0.685586 10.16667 0.09094
PART 0
CL1 3 0.333333 0.666667 0.648112 10.16667 0.23754
CL2 3 0.498059 0.744954 0.593755 10.33333 0.11116
PART 3
C61 1 0.388122 0.695723 0.605206 10.33333 0.20472
PART 0
PART 4
CL3 3 0.388122 0.695723 0.605206 10.16666 0.20472
PART 0
PART 2
O3 5 0.505812 0.303653 0.286441 10.50000 0.11908
AFIX 147
H3A 2 0.495620 0.333346 0.269256 10.50000 -1.50000
AFIX 0
C55 1 0.480500 0.404384 0.326582 10.50000 0.20613
AFIX 33
H55A 2 0.470977 0.416225 0.355251 10.50000 -1.50000
H55B 2 0.533305 0.455302 0.315525 10.50000 -1.50000
H55C 2 0.429704 0.393176 0.309617 10.50000 -1.50000
AFIX 0
C56 1 0.492301 0.323430 0.325565 10.50000 0.14926
AFIX 13
H56 2 0.554343 0.352177 0.335607 10.50000 -1.20000
AFIX 0
C57 1 0.451720 0.252158 0.357545 10.50000 0.17374
AFIX 33
H57A 2 0.446541 0.277054 0.383875 10.50000 -1.50000
H57B 2 0.393311 0.207108 0.348204 10.50000 -1.50000
H57C 2 0.488793 0.225743 0.361452 10.50000 -1.50000
AFIX 0
PART 0
PART 1
O1 5 0.212057 0.100714 0.489634 10.50000 0.09368
AFIX 147
H1A 2 0.188804 0.048836 0.480939 10.50000 -1.50000
AFIX 0
C47 1 0.309262 0.143037 0.486359 10.50000 0.10595
AFIX 13
H47 2 0.326985 0.098287 0.492359 10.50000 -1.20000
AFIX 0
C48 1 0.359524 0.220581 0.514434 10.50000 0.06935
AFIX 137
H48A 2 0.327464 0.210869 0.540563 10.50000 -1.50000
H48B 2 0.366365 0.273570 0.500947 10.50000 -1.50000
H48C 2 0.417538 0.227901 0.520109 10.50000 -1.50000
AFIX 0
C49 1 0.338678 0.178311 0.443165 10.50000 0.09272
AFIX 33
H49A 2 0.402686 0.206011 0.441327 10.50000 -1.50000
H49B 2 0.311453 0.130047 0.423140 10.50000 -1.50000
H49C 2 0.321026 0.221818 0.436935 10.50000 -1.50000
AFIX 0
PART 0
O4 5 0.407699 0.699530 0.330425 10.33333 0.10977
C50 1 0.365305 0.651031 0.369607 10.66667 0.13516
C51 1 0.396458 0.592200 0.380358 10.33333 0.12951
PART 5
O6 5 0.090639 0.075504 0.508709 10.33333 0.10530
PART 0
PART 3
O5 5 0.921266 0.907136 0.507303 10.33333 0.08628
PART 0
PART 4
O7 5 0.030209 0.056426 0.501250 10.33333 0.09736
PART 0
O11 5 0.666667 0.333333 0.254431 10.08333 0.05078
PART 2
O10 5 0.469469 0.525503 0.299176 10.25000 0.21068
HKLF 4
REM THL_386_D6 in P6(3)
REM R1 = 0.0916 for 6186 Fo > 4sig(Fo) and 0.1121 for all 7633 data
REM 595 parameters refined using 74 restraints
END
WGHT 0.1820 4.0226
REM Highest difference peak 0.587, deepest hole -0.337, 1-sigma level 0.090
Q1 1 0.9802 0.9551 0.6683 11.00000 0.05 0.59
Q2 1 1.0205 1.0391 0.6813 11.00000 0.05 0.53
Q3 1 0.6807 0.3672 0.2662 11.00000 0.05 0.53
Q4 1 0.6566 0.4497 0.7805 11.00000 0.05 0.48
Q5 1 0.3541 0.2398 0.3876 11.00000 0.05 0.44
Q6 1 0.3280 0.2469 0.3803 11.00000 0.05 0.42
Q7 1 0.5799 0.4187 0.7555 11.00000 0.05 0.40
Q8 1 0.6261 0.4802 0.7359 11.00000 0.05 0.40
Q9 1 0.5687 0.3465 0.7779 11.00000 0.05 0.39
Q10 1 0.4418 0.1655 0.3444 11.00000 0.05 0.38
Q11 1 0.6667 0.3333 0.6884 10.33333 0.05 0.37
Q12 1 0.9787 0.9530 0.6110 11.00000 0.05 0.36
Q13 1 0.4786 0.5534 0.2786 11.00000 0.05 0.35
Q14 1 0.5436 0.2828 0.3517 11.00000 0.05 0.35
Q15 1 0.5929 0.4086 0.3180 11.00000 0.05 0.33
Q16 1 0.6667 0.3333 0.6369 10.33333 0.05 0.33
Q17 1 0.6609 0.3580 0.6076 11.00000 0.05 0.32
Q18 1 0.6360 0.4433 0.7194 11.00000 0.05 0.32
Q19 1 0.4426 0.3821 0.3403 11.00000 0.05 0.30
Q20 1 0.4024 0.1244 0.3569 11.00000 0.05 0.29
;
_shelx_res_checksum 50246
_olex2_submission_special_instructions 'No special instructions were received'