data_yb016bisf
_publ_section_related_literature ?
_publ_contact_author_name 'Yassine Beldjoudi'
_publ_contact_letter
;
Please consider this CIF for publication. I certify that this contibution is the
original work of those listed as authors; that it has not been published
before (in any language or medium) and is not being considered for publication
elsewhere; that all authors concur with and are aware of the submission; that
all workers involved in the study are listed as authors or given proper credit
in the acknowledgements; that I have obtained permission for and acknowledged
the source of any excerpts from other copyright works; and that to the best of
my knowledge the paper contains no statements which are libellous, unlawful or
in any way actionable. All coauthors have made significant scientific
contributions to the work reported, including the ideas and their execution,
and share responsibility and accountability for the results.
;
_publ_requested_category ?
_publ_requested_journal 'Acta Cryst. E'
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_contact_author_address
;
2145 Sheridan Rd, Evanston, IL 60208
;
_publ_section_title
;
Supramolecular Tessellations by a Rigid Naphthalene Diimide Triangle
;
# Loop of author details
loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
_publ_author_email
'Beldjoudi, Yassine'
;
2145 Sheridan Rd, Evanston, IL 60208
;
.
;
Yassine.Beldjoudi@northwestern.edu
;
'Stoddart, Fraser'
;
2145 Sheridan Rd, Evanston, IL 60208
;
.
;
stoddart@northwestern.edu
;
_publ_section_abstract
;
?
;
_publ_contact_author_email
'Yassine.Beldjoudi@nrthwestern.edu'
#Added by publCIF
_audit_update_record
;
2019-07-26 # Formatted by publCIF
;
_publcif_datablock.id '{05449f5a-9d32-4da0-9efc-d9b7ea75cebd}'
# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents
section
;
Chemical context
;
;
;
section
;
Structural commentary
;
;
;
section
;
Supramolecular features
;
;
;
section
;
Database survey
;
;
;
section
;
Synthesis and crystallization
;
;
;
section
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;
# publcif _publ_body_element loop end
_audit_creation_date 2019-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Bourhis, L. J., Dolomanov, O. V., Gildea, R. J., Howard, J. A. K. & Puschmann,
H. (2015). Acta Cryst. A71, 59--75.
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann,
H. (2009). J. Appl. Cryst. 42, 339--341.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C60 H42 N6 O12, C4 H3 S2.5, C6 H4 S4, 0.5(C4 H2 S3), C3 H3 S2'
_chemical_formula_sum 'C75 H53 N6 O12 S10'
_chemical_formula_weight 1550.83
_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' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567 '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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 15.8923(10)
_cell_length_b 15.9624(10)
_cell_length_c 16.7921(11)
_cell_angle_alpha 69.423(4)
_cell_angle_beta 69.340(4)
_cell_angle_gamma 70.959(4)
_cell_volume 3630.8(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 7605
_cell_measurement_temperature 103(2)
_cell_measurement_theta_max 67.239
_cell_measurement_theta_min 2.917
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.369
_exptl_absorpt_correction_T_max 0.7531
_exptl_absorpt_correction_T_min 0.4638
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1066 before and 0.0665 after correction. The Ratio of minimum to maximum transmission is 0.6159. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.419
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description 'plate'
_exptl_crystal_F_000 1602
_exptl_crystal_size_max 0.115
_exptl_crystal_size_mid 0.087
_exptl_crystal_size_min 0.072
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0419
_diffrn_reflns_av_unetI/netI 0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.895
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 15466
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full 65.114
_diffrn_reflns_theta_max 65.114
_diffrn_reflns_theta_min 2.918
_diffrn_ambient_temperature 103.26
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 10161
_reflns_number_total 11083
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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 V8.38A (?, 2016)'
_computing_data_collection 'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 1.169
_refine_diff_density_min -0.947
_refine_diff_density_rms 0.206
_refine_ls_extinction_coef 0.0249(19)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.017
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 1111
_refine_ls_number_reflns 11083
_refine_ls_number_restraints 350
_refine_ls_R_factor_all 0.2059
_refine_ls_R_factor_gt 0.1995
_refine_ls_restrained_S_all 1.012
_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^)+(0.1937P)^2^+80.1773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.4607
_refine_ls_wR_factor_ref 0.4653
_refine_special_details
'Distance restraints were imposed on the highly disordered TTF molecues and cyclohexane moeities of the NDI macrocycle. Displacement restrains where imposed on both the macrocycle and the TTF molecules. A Shelx FLAT command was imposed on the disordered TTF rings. Solvent mask was utilised in OLex2.'
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
S10-C72
1.7 with sigma of 0.02
S8A-C69A
1.71 with sigma of 0.02
C68A-S8A
1.73 with sigma of 0.02
C35-C40
1.54 with sigma of 0.02
C20-C15
1.54 with sigma of 0.02
C58-C53
1.54 with sigma of 0.02
C69A-C70A
1.33 with sigma of 0.02
C71_$1-C72_$1
1.28 with sigma of 0.02
C39-C38
1.54 with sigma of 0.01
C40-C39
1.54 with sigma of 0.01
C40-C35
1.54 with sigma of 0.01
C35-C36
1.54 with sigma of 0.01
C36-C37
1.54 with sigma of 0.01
C37-C38
1.54 with sigma of 0.01
C15-C20
1.54 with sigma of 0.01
C20-C19
1.54 with sigma of 0.01
C19-C18
1.54 with sigma of 0.01
C18-C17
1.54 with sigma of 0.01
C17-C16
1.54 with sigma of 0.01
C16-C15
1.54 with sigma of 0.01
C53-C58
1.54 with sigma of 0.01
C58-C57
1.54 with sigma of 0.01
C57-C56
1.54 with sigma of 0.01
C56-C55
1.54 with sigma of 0.01
C55-C54
1.54 with sigma of 0.01
C54-C53
1.54 with sigma of 0.01
C69B-C70B
1.3 with sigma of 0.02
C70B-S7B
1.71 with sigma of 0.02
C65-C66
1.3 with sigma of 0.02
C68B-S8B
1.71 with sigma of 0.02
C67B-C68B
1.34 with sigma of 0.02
C62-C61
1.36 with sigma of 0.01
C68B-C67B
1.36 with sigma of 0.02
S6-C67A
1.72 with sigma of 0.01
N3-C20
1.49 with sigma of 0.01
N4-C35
1.49 with sigma of 0.01
N5-C40
1.49 with sigma of 0.01
N1-C58
1.49 with sigma of 0.01
N2-C15
1.49 with sigma of 0.01
C53-C0AA
1.54 with sigma of 0.01
C40-C8AA
1.54 with sigma of 0.01
C20-C2AA
1.54 with sigma of 0.01
C74-C73
1.38 with sigma of 0.02
C76-H76
0.98 with sigma of 0.005
C75-H75
0.98 with sigma of 0.005
S11-C76
1.78 with sigma of 0.02
C54-C3AA
1.54 with sigma of 0.02
C1AA-C18
1.54 with sigma of 0.02
C1AA-C16
1.54 with sigma of 0.02
C40-C35 \\sim C36-C37 \\sim C38-C39
with sigma of 0.02
C20-C15 \\sim C20-C19 \\sim C19-C18 \\sim C18-C17 \\sim C17-C16 \\sim C16-C15
with sigma of 0.01
C20-C19 \\sim C18-C17 \\sim C16-C15
with sigma of 0.01
N2-C15 \\sim N3-C20 \\sim N4-C35 \\sim N5-C40 \\sim C53-N6 \\sim C58-N1
with sigma of 0.02
C75-H75 \\sim C76-H76
with sigma of 0.005
3. Restrained planarity
S9, S10, C71, C72
with sigma of 0.01
S5A, S6, C65, C66
with sigma of 0.01
H75, C75, H76, C76
with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N6 \\sim N5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C75 \\sim C76: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C67A) \\sim Ueq, Uanis(C67B) \\sim Ueq, Uanis(C68B) \\sim Ueq,
Uanis(C68A) \\sim Ueq, Uanis(C69B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C66) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C70A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C1DA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.1
Uanis(C69A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C70B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.1
Uanis(C4AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(C67B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C1AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C2AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C56) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C97) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C5AA) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.025
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(C50) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O11) = Uanis(O12)
5. Others
Fixed Sof: C15(0.5) H15(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5) C17(0.5)
H17A(0.5) H17B(0.5) H18A(0.5) H18B(0.5) H18C(0.5) H18D(0.5) H20(0.5) H20A(0.5)
C35(0.5) H35(0.5) H36A(0.5) H36B(0.5) H36C(0.5) H36D(0.5) C37(0.5) H37A(0.5)
H37B(0.5) C38(0.5) H38A(0.5) H38B(0.5) H39A(0.5) H39B(0.5) H39C(0.5) H39D(0.5)
H40(0.5) H40A(0.5) H53(0.5) H53A(0.5) H54C(0.5) H54D(0.5) H54A(0.5) H54B(0.5)
C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H57A(0.5) H57B(0.5)
H57C(0.5) H57D(0.5) C58(0.5) H58(0.5) S5A(0.5) S7A(0.5) S8A(0.5) C67A(0.5)
C68A(0.5) C69A(0.5) H69A(0.5) C70A(0.5) H70A(0.5) C67B(0.5) S8B(0.5) C70B(0.5)
H70B(0.5) S7B(0.5) C69B(0.5) H69B(0.5) S5B(0.5) C68B(0.5) S9(0.5) S10(0.5)
C71(0.5) H71(0.5) C72(0.5) H72(0.5) C73(0.5) C74(0.5) S11(0.5) S12(0.5)
C0AA(0.5) H0AA(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) C2AA(0.5) H2AA(0.5)
C8AA(0.5) H8AA(0.5) C76(0.5) C75(0.5) C97(0.5) H97A(0.5) H97B(0.5) C3AA(0.5)
H3AA(0.5) H3AB(0.5) C68(0.5) H68A(0.5) H68B(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5)
6.a Ternary CH refined with riding coordinates:
C15(H15), C20(H20), C20(H20A), C35(H35), C40(H40), C40(H40A), C53(H53),
C53(H53A), C58(H58), C0AA(H0AA), C2AA(H2AA), C8AA(H8AA)
6.b Secondary CH2 refined with riding coordinates:
C16(H16A,H16B), C16(H16C,H16D), C17(H17A,H17B), C18(H18A,H18B), C18(H18C,
H18D), C19(H19A,H19B), C36(H36A,H36B), C36(H36C,H36D), C37(H37A,H37B),
C38(H38A,H38B), C39(H39A,H39B), C39(H39C,H39D), C54(H54C,H54D), C54(H54A,H54B),
C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C57(H57C,H57D), C1AA(H1AA,
H1AB), C97(H97A,H97B), C3AA(H3AA,H3AB), C68(H68A,H68B), C5AA(H5AA,H5AB)
6.c Aromatic/amide H refined with riding coordinates:
C1DA(H1DA), C5BA(H5BA), C6(H6), C7(H7), C7AA(H7AA), C11(H11), C12(H12),
C26(H26), C27(H27), C32(H32), C46(H46), C47(H47), C65(H65), C66(H66),
C69A(H69A), C70A(H70A), C59(H59), C60(H60), C63(H63), C64(H64), C70B(H70B),
C69B(H69B), C71(H71), C72(H72)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary iterative
_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
C1 C 0.2418(15) 0.5850(10) 0.3761(11) 0.077(6) Uani 1 1 d . . . . .
C1DA C 0.0563(14) 0.9934(13) 0.2607(13) 0.086(5) Uani 1 1 d . U . . .
H1DA H -0.005842 0.989096 0.290585 0.103 Uiso 1 1 calc R . . A .
N1 N 0.1499(11) 0.6098(9) 0.3772(10) 0.077(4) Uani 1 1 d D . . . .
O1 O -0.0020(8) 0.6359(8) 0.4596(12) 0.110(6) Uani 1 1 d . . . . .
C2 C 0.0792(13) 0.6283(13) 0.4525(13) 0.076(5) Uani 1 1 d . U . . .
N2 N 0.2711(11) 0.6827(8) 0.7106(7) 0.069(4) Uani 1 1 d D . . . .
O2 O 0.3010(11) 0.5611(10) 0.3150(8) 0.093(4) Uani 1 1 d . . . . .
C3 C 0.1048(7) 0.6372(8) 0.5250(9) 0.051(3) Uani 1 1 d . . . . .
N3 N 0.3214(8) 0.8540(7) 0.6860(5) 0.045(2) Uani 1 1 d D . . . .
O3 O 0.1196(13) 0.7270(11) 0.7775(9) 0.128(6) Uani 1 1 d . . . . .
C4 C 0.1950(8) 0.6210(8) 0.5189(8) 0.043(3) Uani 1 1 d . . . . .
N4 N 0.3451(13) 1.1961(8) 0.2823(9) 0.079(4) Uani 1 1 d D . . . .
O4 O 0.4198(9) 0.6166(7) 0.6556(7) 0.079(4) Uani 1 1 d . . . . .
C5 C 0.2673(7) 0.5926(7) 0.4523(7) 0.034(2) Uani 1 1 d . . . . .
C5BA C 0.0823(9) 1.0718(11) 0.2472(14) 0.086(6) Uani 1 1 d . . . A -1
H5BA H 0.037374 1.120515 0.268920 0.103 Uiso 1 1 calc R . . A -1
N5 N 0.2899(9) 1.1714(6) 0.1455(8) 0.054(3) Uani 1 1 d D U . . .
O5 O 0.1776(7) 0.9343(10) 0.7406(7) 0.078(3) Uani 1 1 d . . . . .
C6 C 0.3599(8) 0.5745(8) 0.4492(8) 0.041(3) Uani 1 1 d . . . . .
H6 H 0.407000 0.554236 0.401763 0.049 Uiso 1 1 calc R . . . .
N6 N 0.1585(8) 0.7645(8) 0.2186(7) 0.055(3) Uani 1 1 d D U . . .
O6 O 0.4754(7) 0.7869(6) 0.6381(7) 0.062(3) Uani 1 1 d . . . . .
C7 C 0.3816(8) 0.5862(8) 0.5139(8) 0.043(3) Uani 1 1 d . . . . .
H7 H 0.444853 0.571049 0.513013 0.051 Uiso 1 1 calc R . . . .
C7AA C 0.1942(10) 1.1566(9) 0.5139(10) 0.056(4) Uani 1 1 d . . . . .
H7AA H 0.147578 1.212047 0.509730 0.067 Uiso 1 1 calc R . . . .
O7 O 0.2119(10) 1.2848(7) 0.3473(9) 0.089(4) Uani 1 1 d . U . . .
C4AA C 0.3143(7) 0.6202(7) 0.5837(7) 0.032(2) Uani 1 1 d . U . . .
O8 O 0.4895(11) 1.1149(9) 0.2264(7) 0.094(4) Uani 1 1 d . . . . .
C9 C 0.2224(8) 0.6356(8) 0.5836(7) 0.039(3) Uani 1 1 d . . . . .
O9 O 0.4266(7) 1.1168(8) 0.0621(8) 0.077(3) Uani 1 1 d . . . . .
C10 C 0.1508(10) 0.6713(9) 0.6554(11) 0.063(4) Uani 1 1 d . . . . .
O10 O 0.1448(8) 1.2354(7) 0.2117(7) 0.071(3) Uani 1 1 d . . . . .
C11 C 0.0634(10) 0.6863(10) 0.6568(11) 0.070(5) Uani 1 1 d . . . . .
H11 H 0.016001 0.709918 0.702230 0.084 Uiso 1 1 calc R . . . .
O11 O 0.2943(9) 0.7085(9) 0.1373(9) 0.088(3) Uani 1 1 d . . . . .
C12 C 0.0384(10) 0.6676(11) 0.5909(13) 0.076(5) Uani 1 1 d . U . . .
H12 H -0.024834 0.676839 0.594394 0.091 Uiso 1 1 calc R . . . .
O12 O 0.0121(9) 0.8231(9) 0.2938(9) 0.088(3) Uani 1 1 d . . . . .
C13 C 0.1754(13) 0.6931(14) 0.7213(10) 0.078(5) Uani 1 1 d . . . . .
C14 C 0.3415(12) 0.6326(12) 0.6525(9) 0.069(5) Uani 1 1 d . . . . .
C15 C 0.3247(14) 0.6781(10) 0.7698(9) 0.069(8) Uani 0.5 1 d D U P B 1
H15 H 0.390756 0.645884 0.749671 0.083 Uiso 0.5 1 calc R . P B 1
C16 C 0.2830(11) 0.6327(9) 0.8674(8) 0.061(4) Uani 1 1 d D . . . .
H16A H 0.221372 0.627278 0.870952 0.074 Uiso 0.5 1 calc R . P B 1
H16B H 0.321152 0.569087 0.879779 0.074 Uiso 0.5 1 calc R . P B 1
H16C H 0.320580 0.577981 0.845770 0.074 Uiso 0.5 1 calc R . P B 2
H16D H 0.223804 0.617305 0.906785 0.074 Uiso 0.5 1 calc R . P B 2
C17 C 0.2689(19) 0.6683(17) 0.9461(12) 0.063(7) Uani 0.5 1 d D U P B 1
H17A H 0.285384 0.614843 0.994811 0.076 Uiso 0.5 1 calc R . P B 1
H17B H 0.202294 0.696214 0.966649 0.076 Uiso 0.5 1 calc R . P B 1
C18 C 0.3237(13) 0.7390(12) 0.9295(10) 0.101(8) Uani 1 1 d D . . . .
H18A H 0.291905 0.774763 0.973781 0.121 Uiso 0.5 1 calc R . P B 1
H18B H 0.385730 0.705786 0.938200 0.121 Uiso 0.5 1 calc R . P B 1
H18C H 0.370259 0.739686 0.955715 0.121 Uiso 0.5 1 calc R . P B 2
H18D H 0.261698 0.759920 0.967367 0.121 Uiso 0.5 1 calc R . P B 2
C19 C 0.3352(12) 0.8060(10) 0.8368(7) 0.078(5) Uani 1 1 d D . . . .
H19A H 0.292535 0.866076 0.841868 0.093 Uiso 1 1 calc R . . . .
H19B H 0.398948 0.815225 0.815079 0.093 Uiso 1 1 calc R . . . .
C20 C 0.3176(14) 0.7771(10) 0.7674(7) 0.091(7) Uani 1 1 d D . . . .
H20 H 0.248743 0.792706 0.790064 0.109 Uiso 0.5 1 calc R . P B 1
H20A H 0.380337 0.737498 0.748444 0.109 Uiso 0.5 1 calc R . P B 2
C21 C 0.4063(7) 0.8485(7) 0.6210(7) 0.034(3) Uani 1 1 d . . . . .
C22 C 0.2478(8) 0.9297(9) 0.6808(7) 0.041(3) Uani 1 1 d . . . . .
C23 C 0.2563(9) 1.0069(8) 0.5968(8) 0.048(3) Uani 1 1 d . . . . .
C24 C 0.3383(7) 0.9967(7) 0.5282(7) 0.030(2) Uani 1 1 d . U . . .
C25 C 0.4114(10) 0.9196(8) 0.5337(8) 0.047(3) Uani 1 1 d . . . . .
C26 C 0.4894(8) 0.9118(9) 0.4655(9) 0.050(3) Uani 1 1 d . . . . .
H26 H 0.540465 0.861085 0.473295 0.060 Uiso 1 1 calc R . . . .
C27 C 0.4945(8) 0.9764(9) 0.3861(7) 0.045(3) Uani 1 1 d . . . . .
H27 H 0.547282 0.967769 0.337909 0.054 Uiso 1 1 calc R . . . .
C28 C 0.4240(9) 1.0544(9) 0.3745(8) 0.048(3) Uani 1 1 d . . . . .
C29 C 0.3427(9) 1.0679(9) 0.4471(8) 0.048(3) Uani 1 1 d . . . . .
C30 C 0.2727(8) 1.1454(9) 0.4388(8) 0.042(3) Uani 1 1 d . . . . .
C32 C 0.1863(9) 1.0865(9) 0.5929(13) 0.065(4) Uani 1 1 d . . . . .
H32 H 0.134460 1.093138 0.642358 0.078 Uiso 1 1 calc R . . . .
C33 C 0.4208(16) 1.1211(11) 0.2911(9) 0.076(5) Uani 1 1 d . . . . .
C34 C 0.2763(16) 1.2161(9) 0.3499(12) 0.080(6) Uani 1 1 d . . . . .
C35 C 0.3179(12) 1.2808(10) 0.2139(8) 0.038(5) Uani 0.5 1 d D U P C 1
H35 H 0.254838 1.314902 0.240574 0.046 Uiso 0.5 1 calc R . P C 1
C36 C 0.3843(7) 1.3451(7) 0.1798(7) 0.036(2) Uani 1 1 d D U . . .
H36A H 0.444186 1.306237 0.190521 0.043 Uiso 0.5 1 calc R . P C 1
H36B H 0.360396 1.387006 0.218436 0.043 Uiso 0.5 1 calc R . P C 1
H36C H 0.343967 1.358722 0.236129 0.043 Uiso 0.5 1 calc R . P C 2
H36D H 0.448409 1.339941 0.178813 0.043 Uiso 0.5 1 calc R . P C 2
C37 C 0.4061(18) 1.4058(16) 0.0837(10) 0.035(6) Uani 0.5 1 d D . P C 1
H37A H 0.405772 1.467679 0.084210 0.042 Uiso 0.5 1 calc R . P C 1
H37B H 0.468978 1.378776 0.051257 0.042 Uiso 0.5 1 calc R . P C 1
C38 C 0.337(2) 1.4153(13) 0.034(2) 0.052(9) Uani 0.5 1 d D U P C 1
H38A H 0.278358 1.457788 0.056148 0.062 Uiso 0.5 1 calc R . P C 1
H38B H 0.361668 1.443654 -0.029213 0.062 Uiso 0.5 1 calc R . P C 1
C39 C 0.3153(9) 1.3245(7) 0.0444(6) 0.044(3) Uani 1 1 d D . . . .
H39A H 0.254298 1.338108 0.033431 0.052 Uiso 0.5 1 calc R . P C 1
H39B H 0.362195 1.295195 -0.001079 0.052 Uiso 0.5 1 calc R . P C 1
H39C H 0.251634 1.358724 0.041284 0.052 Uiso 0.5 1 calc R . P C 2
H39D H 0.343208 1.291435 -0.002184 0.052 Uiso 0.5 1 calc R . P C 2
C40 C 0.3139(14) 1.2575(9) 0.1345(8) 0.085(5) Uani 1 1 d D . . . .
H40 H 0.381949 1.230499 0.117413 0.102 Uiso 0.5 1 calc R . P C 1
H40A H 0.254207 1.288442 0.169787 0.102 Uiso 0.5 1 calc R . P C 2
C41 C 0.3535(10) 1.1060(10) 0.1067(9) 0.052(3) Uani 1 1 d . . . . .
C42 C 0.1948(8) 1.1704(8) 0.1872(9) 0.047(3) Uani 1 1 d . . . . .
C43 C 0.1725(8) 1.0838(9) 0.2026(9) 0.048(3) Uani 1 1 d . . . . .
C44 C 0.2340(7) 1.0122(8) 0.1700(8) 0.040(3) Uani 1 1 d . . . . .
C45 C 0.3239(7) 1.0225(10) 0.1208(8) 0.047(3) Uani 1 1 d . . . . .
C46 C 0.3843(10) 0.9475(10) 0.0852(9) 0.059(4) Uani 1 1 d . U . . .
H46 H 0.444793 0.952061 0.048909 0.071 Uiso 1 1 calc R . . . .
C47 C 0.3550(10) 0.8693(9) 0.1033(9) 0.058(4) Uani 1 1 d . U . . .
H47 H 0.397237 0.820903 0.079179 0.069 Uiso 1 1 calc R . . . .
C48 C 0.2709(7) 0.8566(8) 0.1529(7) 0.033(2) Uani 1 1 d . U . . .
C49 C 0.2051(8) 0.9325(8) 0.1883(7) 0.038(3) Uani 1 1 d . U . . .
C50 C 0.1180(7) 0.9223(9) 0.2320(9) 0.049(3) Uani 1 1 d . U . . .
C51 C 0.0897(9) 0.8325(11) 0.2563(10) 0.060(4) Uani 1 1 d . U . . .
C52 C 0.2433(10) 0.7749(9) 0.1698(8) 0.050(3) Uani 1 1 d . U . . .
C53 C 0.1262(19) 0.6823(11) 0.2303(11) 0.119(10) Uani 1 1 d D . . . .
H53 H 0.188375 0.642340 0.210394 0.143 Uiso 0.5 1 calc R . P D 1
H53A H 0.064811 0.699353 0.272318 0.143 Uiso 0.5 1 calc R . P E 2
C54 C 0.0878(8) 0.6895(9) 0.1560(7) 0.044(3) Uani 1 1 d D . . . .
H54C H 0.043120 0.749590 0.145460 0.053 Uiso 0.5 1 calc R . P F 2
H54D H 0.139381 0.689803 0.101456 0.053 Uiso 0.5 1 calc R . P F 2
H54A H 0.124955 0.720499 0.098382 0.053 Uiso 0.5 1 calc R . P G 1
H54B H 0.023117 0.726006 0.165096 0.053 Uiso 0.5 1 calc R . P G 1
C55 C 0.092(2) 0.5915(11) 0.1566(15) 0.058(7) Uani 0.5 1 d D U P H 1
H55A H 0.063273 0.593822 0.112020 0.069 Uiso 0.5 1 calc R . P H 1
H55B H 0.156931 0.556298 0.142774 0.069 Uiso 0.5 1 calc R . P H 1
C56 C 0.0385(15) 0.546(2) 0.2500(15) 0.057(8) Uani 0.5 1 d D U P H 1
H56A H -0.019704 0.588446 0.271571 0.068 Uiso 0.5 1 calc R . P H 1
H56B H 0.023765 0.489594 0.250647 0.068 Uiso 0.5 1 calc R . P H 1
C57 C 0.1054(9) 0.5211(7) 0.3067(8) 0.046(3) Uani 1 1 d D . . . .
H57A H 0.169748 0.496861 0.275137 0.055 Uiso 0.5 1 calc R . P H 1
H57B H 0.087121 0.475682 0.363679 0.055 Uiso 0.5 1 calc R . P H 1
H57C H 0.045526 0.534558 0.350733 0.055 Uiso 0.5 1 calc R . P H 2
H57D H 0.140261 0.459019 0.331746 0.055 Uiso 0.5 1 calc R . P H 2
C58 C 0.0940(14) 0.6153(10) 0.3201(10) 0.053(6) Uani 0.5 1 d D U P H 1
H58 H 0.027357 0.640110 0.347378 0.063 Uiso 0.5 1 calc R . P H 1
S5A S 0.2952(7) 1.0154(6) -0.1055(12) 0.080(5) Uani 0.5 1 d . . P I 1
S6 S 0.2949(5) 1.1965(3) -0.1027(4) 0.0995(18) Uani 1 1 d D . . I 1
S7A S 0.0852(6) 1.0192(7) -0.0005(8) 0.080(3) Uani 0.5 1 d . . P I 1
S8A S 0.0695(7) 1.2013(6) 0.0144(6) 0.070(2) Uani 0.5 1 d D . P I 1
C65 C 0.3974(11) 1.0487(17) -0.1391(10) 0.086(6) Uani 1 1 d D . . I 1
H65 H 0.451705 1.004862 -0.157901 0.104 Uiso 1 1 calc R . . I 1
C66 C 0.409(3) 1.1254(19) -0.1420(14) 0.155(12) Uani 1 1 d D U . I 1
H66 H 0.466888 1.142278 -0.160881 0.187 Uiso 1 1 calc R . . I 1
C67A C 0.245(4) 1.108(3) -0.082(5) 0.10(2) Uani 0.5 1 d D U P I 1
C68A C 0.1443(15) 1.1064(14) -0.0225(16) 0.034(5) Uani 0.5 1 d D U P I 1
C69A C -0.023(2) 1.151(2) 0.071(3) 0.076(13) Uani 0.5 1 d D U P I 1
H69A H -0.081983 1.186856 0.094622 0.091 Uiso 0.5 1 calc R . P I 1
C70A C -0.010(3) 1.062(2) 0.082(3) 0.093(11) Uani 0.5 1 d D U P I 1
H70A H -0.047084 1.024437 0.129163 0.112 Uiso 0.5 1 calc R . P I 1
S1 S 0.5974(3) 0.6261(3) 0.3024(3) 0.0629(10) Uani 1 1 d . . . . .
S2 S 0.8016(3) 0.5755(3) 0.2377(2) 0.0612(10) Uani 1 1 d . . . . .
S3 S 0.6126(2) 0.6604(2) 0.4742(2) 0.0507(9) Uani 1 1 d . . . . .
S4 S 0.8150(2) 0.6184(3) 0.4096(3) 0.0590(10) Uani 1 1 d . . . . .
C59 C 0.6494(15) 0.5867(12) 0.2059(12) 0.079(5) Uani 1 1 d . . . . .
H59 H 0.613024 0.580356 0.174888 0.095 Uiso 1 1 calc R . . . .
C60 C 0.7386(13) 0.5668(11) 0.1793(12) 0.069(4) Uani 1 1 d . . . . .
H60 H 0.768894 0.547284 0.126737 0.083 Uiso 1 1 calc R . . . .
C61 C 0.7061(8) 0.6110(9) 0.3212(7) 0.048(3) Uani 1 1 d D . . . .
C62 C 0.7125(9) 0.6252(8) 0.3937(7) 0.045(3) Uani 1 1 d D . . . .
C63 C 0.6721(8) 0.6577(8) 0.5418(7) 0.041(3) Uani 1 1 d . . . . .
H63 H 0.639860 0.669968 0.597586 0.049 Uiso 1 1 calc R . . . .
C64 C 0.7661(11) 0.6379(9) 0.5159(10) 0.057(4) Uani 1 1 d . . . . .
H64 H 0.802410 0.634807 0.551701 0.069 Uiso 1 1 calc R . . . .
C67B C 0.2314(15) 1.1100(16) -0.066(2) 0.027(6) Uani 0.5 1 d D U P J 2
S8B S 0.1054(7) 1.2541(7) -0.0043(6) 0.074(2) Uani 0.5 1 d D . P J 2
C70B C -0.006(5) 1.149(4) 0.077(5) 0.17(4) Uani 0.5 1 d D U P J 2
H70B H -0.060414 1.137290 0.121811 0.210 Uiso 0.5 1 calc R . P J 2
S7B S 0.0648(7) 1.0766(10) 0.0129(8) 0.093(3) Uani 0.5 1 d D . P J 2
C69B C 0.024(3) 1.223(3) 0.057(3) 0.081(10) Uani 0.5 1 d D U P J 2
H69B H -0.017123 1.266324 0.088561 0.098 Uiso 0.5 1 calc R . P J 2
S5B S 0.310(3) 1.009(2) -0.111(3) 0.215(16) Uani 0.5 1 d . . P J 2
C68B C 0.1441(17) 1.1473(16) -0.025(2) 0.057(8) Uani 0.5 1 d D U P J 2
S9 S 0.1982(5) 0.8144(4) 0.4041(5) 0.0583(18) Uani 0.5 1 d . . P K 1
S10 S 0.2613(6) 0.9792(5) 0.3697(5) 0.0626(19) Uani 0.5 1 d D . P K 1
C71 C 0.3227(18) 0.8088(14) 0.3517(13) 0.055(6) Uani 0.5 1 d D U P K 1
H71 H 0.367197 0.756856 0.335334 0.067 Uiso 0.5 1 calc R . P K 1
C72 C 0.3398(13) 0.8850(11) 0.3409(11) 0.043(5) Uani 0.5 1 d D U P K 1
H72 H 0.402188 0.890093 0.314350 0.051 Uiso 0.5 1 calc R . P K 1
C73 C 0.076(2) 0.970(3) 0.445(3) 0.092(11) Uani 0.5 1 d D U P . .
C74 C 0.167(2) 0.931(2) 0.411(2) 0.067(8) Uani 0.5 1 d D U P K 1
S11 S -0.0098(7) 0.9148(6) 0.4898(6) 0.060(2) Uani 0.5 1 d D . P K .
S12 S 0.0446(7) 1.0849(5) 0.4564(7) 0.060(2) Uani 0.5 1 d . . P . .
C0AA C 0.1559(19) 0.5866(13) 0.2893(17) 0.051(6) Uani 0.5 1 d D U P H 2
H0AA H 0.222210 0.560919 0.261806 0.061 Uiso 0.5 1 calc R . P H 2
C1AA C 0.3346(19) 0.6432(16) 0.9280(17) 0.057(7) Uani 0.5 1 d D U P B 2
H1AA H 0.311662 0.606984 0.989284 0.069 Uiso 0.5 1 calc R . P B 2
H1AB H 0.401392 0.615828 0.907701 0.069 Uiso 0.5 1 calc R . P B 2
C2AA C 0.2606(14) 0.7080(13) 0.7885(14) 0.037(5) Uani 0.5 1 d D U P B 2
H2AA H 0.194256 0.739894 0.807897 0.044 Uiso 0.5 1 calc R . P B 2
C8AA C 0.379(2) 1.2562(17) 0.1841(17) 0.057(8) Uani 0.5 1 d D . P C 2
H8AA H 0.442435 1.222912 0.157073 0.069 Uiso 0.5 1 calc R . P C 2
C76 C -0.1007(16) 1.0142(17) 0.5099(19) 0.064(8) Uani 0.5 1 d D U P . .
C75 C -0.069(2) 1.091(2) 0.488(2) 0.068(8) Uani 0.5 1 d D U P K .
H76 H -0.158(4) 0.998(8) 0.550(5) 0.05(4) Uiso 1 1 d D . . . .
H75 H -0.121(5) 1.128(6) 0.523(5) 0.03(3) Uiso 1 1 d D . . . .
C97 C 0.088(3) 0.523(2) 0.220(2) 0.069(9) Uani 0.5 1 d . U P H 2
H97A H 0.148018 0.502074 0.179677 0.083 Uiso 0.5 1 calc R . P H 2
H97B H 0.050161 0.478266 0.235041 0.083 Uiso 0.5 1 calc R . P H 2
C3AA C 0.040(2) 0.6146(19) 0.170(2) 0.059(8) Uani 0.5 1 d D U P H 2
H3AA H 0.041301 0.610453 0.112288 0.071 Uiso 0.5 1 calc R . P H 2
H3AB H -0.025400 0.630603 0.203932 0.071 Uiso 0.5 1 calc R . P H 2
C68 C 0.362(3) 1.422(3) 0.113(3) 0.076(12) Uani 0.5 1 d . U P C 2
H68A H 0.403344 1.463824 0.097237 0.091 Uiso 0.5 1 calc R . P C 2
H68B H 0.297714 1.455591 0.132536 0.091 Uiso 0.5 1 calc R . P C 2
C5AA C 0.374(2) 1.3921(19) 0.0316(18) 0.042(7) Uani 0.5 1 d . U P C 2
H5AA H 0.440331 1.362532 0.010601 0.051 Uiso 0.5 1 calc R . P C 2
H5AB H 0.359283 1.447900 -0.015665 0.051 Uiso 0.5 1 calc R . P C 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
C1 0.145(17) 0.049(8) 0.064(10) 0.033(8) -0.076(12) -0.055(10)
C1DA 0.077(8) 0.074(8) 0.091(9) -0.037(7) 0.003(7) -0.007(7)
N1 0.092(10) 0.072(8) 0.090(10) 0.009(7) -0.077(9) -0.025(7)
O1 0.061(7) 0.068(7) 0.204(16) 0.006(9) -0.076(9) -0.020(6)
C2 0.071(8) 0.085(8) 0.085(8) -0.001(7) -0.043(7) -0.034(6)
N2 0.137(13) 0.059(7) 0.022(5) -0.013(5) 0.000(7) -0.056(8)
O2 0.144(12) 0.111(10) 0.043(6) -0.044(7) -0.005(7) -0.052(9)
C3 0.013(5) 0.037(6) 0.069(9) 0.005(6) -0.008(5) 0.012(4)
N3 0.064(7) 0.048(6) 0.023(5) -0.009(4) -0.004(5) -0.024(5)
O3 0.161(15) 0.109(11) 0.069(8) -0.045(8) 0.004(9) 0.012(10)
C4 0.030(6) 0.045(6) 0.036(6) 0.019(5) -0.011(5) -0.018(5)
N4 0.148(15) 0.050(7) 0.063(8) -0.021(7) -0.041(9) -0.034(8)
O4 0.108(9) 0.075(7) 0.083(7) 0.028(6) -0.084(7) -0.049(6)
C5 0.023(5) 0.041(6) 0.026(5) 0.013(4) -0.012(4) -0.012(4)
C5BA 0.023(7) 0.058(9) 0.139(17) -0.024(10) 0.015(8) -0.006(6)
N5 0.076(8) 0.031(5) 0.059(7) 0.010(5) -0.030(6) -0.028(5)
O5 0.043(6) 0.142(11) 0.053(6) -0.039(6) 0.022(5) -0.051(6)
C6 0.033(6) 0.046(6) 0.040(6) -0.001(5) -0.003(5) -0.023(5)
N6 0.068(6) 0.071(6) 0.049(5) -0.029(5) -0.016(5) -0.032(5)
O6 0.079(7) 0.053(5) 0.064(6) 0.008(5) -0.053(6) -0.014(5)
C7 0.023(5) 0.042(6) 0.056(7) -0.004(6) -0.012(5) -0.007(5)
C7AA 0.058(8) 0.042(7) 0.083(10) -0.026(7) -0.037(8) 0.000(6)
O7 0.142(10) 0.047(6) 0.116(9) 0.021(6) -0.118(8) -0.025(6)
C4AA 0.020(4) 0.044(5) 0.031(5) -0.002(4) -0.012(4) -0.012(4)
O8 0.170(14) 0.081(8) 0.044(6) -0.002(6) -0.013(8) -0.076(9)
C9 0.045(7) 0.052(7) 0.019(5) -0.018(5) -0.014(5) 0.002(5)
O9 0.044(6) 0.091(8) 0.093(8) 0.002(6) -0.012(5) -0.047(6)
C10 0.054(9) 0.039(7) 0.072(10) -0.001(7) 0.005(7) -0.019(6)
O10 0.092(8) 0.043(5) 0.064(6) -0.029(5) -0.001(6) -0.003(5)
C11 0.036(8) 0.055(8) 0.086(11) -0.032(8) 0.025(7) 0.003(6)
O11 0.086(6) 0.082(6) 0.086(6) -0.023(5) 0.001(5) -0.034(5)
C12 0.036(7) 0.067(9) 0.101(11) 0.022(8) -0.017(8) -0.032(7)
O12 0.086(6) 0.082(6) 0.086(6) -0.023(5) 0.001(5) -0.034(5)
C13 0.078(12) 0.106(13) 0.050(9) -0.049(9) 0.023(8) -0.034(10)
C14 0.088(11) 0.109(12) 0.031(7) 0.020(8) -0.028(7) -0.078(10)
C15 0.060(11) 0.071(11) 0.067(11) -0.004(8) -0.018(9) -0.018(9)
C16 0.083(11) 0.048(7) 0.038(7) -0.011(6) -0.012(7) -0.001(7)
C17 0.067(11) 0.063(11) 0.050(10) -0.011(8) -0.024(8) 0.001(8)
C18 0.066(11) 0.143(19) 0.057(10) 0.028(11) -0.016(9) -0.037(12)
C19 0.085(12) 0.100(13) 0.050(9) -0.046(9) -0.022(8) 0.010(10)
C20 0.155(18) 0.117(14) 0.037(8) -0.021(8) 0.016(9) -0.124(14)
C21 0.035(6) 0.036(5) 0.033(6) 0.015(5) -0.022(5) -0.021(5)
C22 0.027(6) 0.058(7) 0.030(6) -0.010(5) 0.016(5) -0.027(5)
C23 0.050(7) 0.032(6) 0.033(6) -0.001(5) 0.014(5) -0.008(5)
C24 0.023(4) 0.034(5) 0.029(5) -0.004(4) -0.002(4) -0.012(4)
C25 0.066(8) 0.027(5) 0.044(7) -0.005(5) -0.022(6) -0.003(5)
C26 0.029(6) 0.057(8) 0.056(8) -0.026(6) 0.005(6) -0.005(5)
C27 0.024(6) 0.060(7) 0.028(6) -0.018(5) 0.018(4) -0.002(5)
C28 0.039(7) 0.057(7) 0.043(7) -0.028(6) -0.002(5) 0.000(6)
C29 0.045(7) 0.051(7) 0.036(7) -0.014(6) 0.018(5) -0.026(6)
C30 0.028(6) 0.051(7) 0.048(7) -0.009(6) -0.014(5) -0.010(5)
C32 0.035(7) 0.038(7) 0.121(14) -0.038(8) -0.006(8) -0.005(5)
C33 0.154(18) 0.055(9) 0.022(7) 0.006(6) -0.020(9) -0.050(11)
C34 0.169(19) 0.020(6) 0.083(12) -0.005(7) -0.091(14) -0.008(8)
C35 0.022(10) 0.055(12) 0.029(11) -0.019(9) 0.017(8) -0.016(9)
C36 0.029(5) 0.030(5) 0.042(5) -0.008(4) -0.001(4) -0.009(4)
C37 0.046(16) 0.024(11) 0.040(14) 0.003(10) -0.015(12) -0.025(11)
C38 0.053(12) 0.045(12) 0.049(11) -0.006(8) -0.014(9) -0.008(9)
C39 0.051(7) 0.036(6) 0.028(6) -0.014(5) 0.009(5) -0.005(5)
C40 0.098(14) 0.066(10) 0.092(13) -0.007(9) -0.022(11) -0.041(10)
C41 0.050(8) 0.059(8) 0.056(8) -0.012(7) -0.024(7) -0.017(7)
C42 0.037(6) 0.027(6) 0.064(8) -0.005(6) -0.011(6) 0.000(5)
C43 0.028(6) 0.050(7) 0.056(8) -0.025(6) 0.021(5) -0.017(5)
C44 0.016(5) 0.046(6) 0.041(6) -0.018(5) 0.004(4) 0.008(4)
C45 0.018(5) 0.071(8) 0.037(6) -0.027(6) 0.009(5) 0.004(5)
C46 0.047(6) 0.054(6) 0.052(6) -0.011(5) 0.006(5) -0.004(5)
C47 0.058(7) 0.042(6) 0.055(7) -0.024(5) 0.008(5) -0.001(5)
C48 0.026(5) 0.043(5) 0.028(5) -0.019(4) -0.005(4) 0.003(4)
C49 0.040(5) 0.044(5) 0.026(5) -0.020(4) 0.010(4) -0.015(4)
C50 0.017(5) 0.059(7) 0.058(7) -0.022(6) 0.017(5) -0.017(5)
C51 0.042(6) 0.073(7) 0.074(7) -0.008(6) -0.014(5) -0.039(6)
C52 0.065(7) 0.046(6) 0.033(5) -0.011(5) 0.002(5) -0.023(5)
C53 0.27(3) 0.070(11) 0.073(11) 0.027(9) -0.098(17) -0.102(16)
C54 0.034(6) 0.067(8) 0.034(6) -0.023(6) 0.002(5) -0.018(6)
C55 0.070(16) 0.044(13) 0.069(15) -0.009(11) -0.049(13) 0.000(11)
C56 0.011(9) 0.068(14) 0.084(16) -0.010(12) -0.005(10) -0.021(10)
C57 0.051(7) 0.028(5) 0.052(7) -0.017(5) -0.007(6) 0.000(5)
C58 0.053(10) 0.054(10) 0.054(10) -0.013(8) -0.015(8) -0.017(8)
S5A 0.041(4) 0.030(4) 0.194(15) -0.058(6) -0.058(7) 0.018(3)
S6 0.152(5) 0.066(3) 0.098(4) -0.023(3) -0.037(3) -0.043(3)
S7A 0.050(5) 0.062(5) 0.114(8) -0.043(5) 0.015(4) -0.013(4)
S8A 0.069(5) 0.071(5) 0.066(5) -0.048(4) 0.011(4) -0.009(4)
C65 0.034(8) 0.148(19) 0.074(11) -0.051(12) -0.008(7) 0.000(10)
C66 0.155(15) 0.154(15) 0.162(15) -0.040(10) -0.047(10) -0.040(10)
C67A 0.10(2) 0.11(2) 0.10(3) -0.032(11) -0.029(11) -0.019(11)
C68A 0.029(9) 0.036(9) 0.034(9) -0.009(7) -0.004(7) -0.006(7)
C69A 0.069(15) 0.079(15) 0.072(15) -0.017(9) -0.016(9) -0.016(9)
C70A 0.079(14) 0.096(14) 0.096(14) -0.010(9) -0.025(9) -0.026(9)
S1 0.062(2) 0.064(2) 0.067(2) -0.0160(18) -0.0282(18) -0.0091(17)
S2 0.063(2) 0.061(2) 0.050(2) -0.0195(16) 0.0028(16) -0.0172(17)
S3 0.0425(17) 0.0558(18) 0.0413(17) -0.0177(14) 0.0030(13) -0.0057(14)
S4 0.0378(17) 0.068(2) 0.074(2) -0.0297(19) -0.0126(16) -0.0075(15)
C59 0.114(16) 0.075(11) 0.079(11) -0.015(9) -0.052(11) -0.038(10)
C60 0.077(12) 0.062(9) 0.076(11) -0.023(8) -0.021(9) -0.021(8)
C61 0.037(7) 0.063(8) 0.039(7) -0.008(6) -0.002(5) -0.022(6)
C62 0.048(7) 0.044(6) 0.040(7) -0.017(5) -0.001(5) -0.013(5)
C63 0.034(6) 0.044(6) 0.030(6) -0.012(5) 0.010(5) -0.009(5)
C64 0.069(9) 0.043(7) 0.057(8) -0.005(6) -0.031(7) -0.003(6)
C67B 0.015(9) 0.035(9) 0.021(9) -0.013(7) 0.007(6) -0.002(6)
S8B 0.071(5) 0.080(6) 0.059(5) -0.035(4) -0.001(4) -0.001(5)
C70B 0.17(4) 0.17(4) 0.17(4) -0.047(12) -0.047(12) -0.039(11)
S7B 0.055(5) 0.118(9) 0.092(7) -0.002(7) -0.005(5) -0.046(6)
C69B 0.080(13) 0.084(13) 0.074(13) -0.026(9) -0.012(9) -0.016(9)
S5B 0.28(4) 0.17(2) 0.22(3) -0.14(2) 0.00(2) -0.06(2)
C68B 0.055(11) 0.057(11) 0.056(11) -0.016(9) -0.008(8) -0.014(9)
S9 0.073(5) 0.043(3) 0.074(5) -0.003(3) -0.037(4) -0.027(3)
S10 0.085(5) 0.060(4) 0.061(4) -0.004(3) -0.035(4) -0.035(4)
C71 0.049(10) 0.049(10) 0.049(10) 0.003(8) -0.017(8) -0.001(8)
C72 0.031(8) 0.048(9) 0.055(10) -0.009(7) -0.013(7) -0.018(7)
C73 0.101(15) 0.086(14) 0.094(14) -0.030(10) -0.020(10) -0.026(9)
C74 0.068(11) 0.068(11) 0.073(12) -0.011(8) -0.023(9) -0.029(9)
S11 0.073(5) 0.063(5) 0.050(5) -0.003(4) -0.021(4) -0.029(4)
S12 0.081(6) 0.043(4) 0.069(6) 0.003(4) -0.034(5) -0.034(4)
C0AA 0.048(10) 0.057(10) 0.050(10) -0.010(8) -0.024(8) -0.009(8)
C1AA 0.061(11) 0.054(10) 0.044(10) -0.021(8) 0.004(8) -0.010(8)
C2AA 0.036(8) 0.035(8) 0.033(8) -0.001(7) -0.015(7) -0.002(7)
C8AA 0.09(2) 0.031(13) 0.037(14) 0.020(11) -0.018(16) -0.035(14)
C76 0.054(15) 0.10(2) 0.061(16) -0.005(15) -0.041(13) -0.036(15)
C75 0.064(11) 0.068(11) 0.064(11) -0.017(8) -0.011(8) -0.014(8)
C97 0.086(18) 0.082(16) 0.067(15) -0.049(13) -0.022(13) -0.024(13)
C3AA 0.030(12) 0.067(15) 0.079(16) -0.007(12) -0.011(11) -0.025(11)
C68 0.075(19) 0.072(18) 0.087(19) -0.023(14) -0.043(15) 0.000(14)
C5AA 0.046(13) 0.035(11) 0.036(12) -0.019(9) -0.006(11) 0.007(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
C1 N1 1.38(2) . ?
C1 O2 1.20(2) . ?
C1 C5 1.525(18) . ?
C1DA C5BA 1.36(3) . ?
C1DA C50 1.34(2) . ?
N1 C2 1.41(2) . ?
N1 C58 1.485(8) . ?
N1 C0AA 1.61(3) . ?
O1 C2 1.222(19) . ?
C2 C3 1.47(2) . ?
N2 C13 1.43(2) . ?
N2 C14 1.43(2) . ?
N2 C15 1.492(9) . ?
N2 C2AA 1.44(2) . ?
C3 C4 1.344(16) . ?
C3 C12 1.34(2) . ?
N3 C20 1.481(8) . ?
N3 C21 1.403(15) . ?
N3 C22 1.382(16) . ?
O3 C13 1.194(19) . ?
C4 C5 1.373(17) . ?
C4 C9 1.416(17) . ?
N4 C33 1.40(2) . ?
N4 C34 1.32(3) . ?
N4 C35 1.487(8) . ?
N4 C8AA 1.59(3) . ?
O4 C14 1.203(18) . ?
C5 C6 1.390(15) . ?
C5BA C43 1.404(18) . ?
N5 C40 1.477(8) . ?
N5 C41 1.364(19) . ?
N5 C42 1.427(17) . ?
O5 C22 1.211(14) . ?
C6 C7 1.336(18) . ?
N6 C51 1.41(2) . ?
N6 C52 1.336(17) . ?
N6 C53 1.486(12) . ?
O6 C21 1.255(14) . ?
C7 C4AA 1.412(17) . ?
C7AA C30 1.44(2) . ?
C7AA C32 1.40(2) . ?
O7 C34 1.23(2) . ?
C4AA C9 1.400(15) . ?
C4AA C14 1.460(17) . ?
O8 C33 1.24(2) . ?
C9 C10 1.471(19) . ?
O9 C41 1.168(17) . ?
C10 C11 1.32(2) . ?
C10 C13 1.47(2) . ?
O10 C42 1.188(15) . ?
C11 C12 1.45(3) . ?
O11 C52 1.270(18) . ?
O12 C51 1.203(17) . ?
C15 C16 1.536(7) . ?
C15 C20 1.534(6) . ?
C16 C17 1.535(7) . ?
C16 C1AA 1.594(18) . ?
C16 C2AA 1.50(2) . ?
C17 C18 1.537(7) . ?
C18 C19 1.534(7) . ?
C18 C1AA 1.489(18) . ?
C19 C20 1.530(7) . ?
C20 C2AA 1.521(10) . ?
C21 C25 1.500(15) . ?
C22 C23 1.510(16) . ?
C23 C24 1.409(15) . ?
C23 C32 1.388(18) . ?
C24 C25 1.390(16) . ?
C24 C29 1.431(16) . ?
C25 C26 1.365(18) . ?
C26 C27 1.363(18) . ?
C27 C28 1.384(17) . ?
C28 C29 1.447(16) . ?
C28 C33 1.437(19) . ?
C29 C30 1.371(18) . ?
C30 C34 1.518(19) . ?
C35 C36 1.537(10) . ?
C35 C40 1.531(8) . ?
C36 C37 1.546(9) . ?
C36 C8AA 1.42(3) . ?
C36 C68 1.39(4) . ?
C37 C38 1.538(10) . ?
C38 C39 1.535(9) . ?
C39 C40 1.513(9) . ?
C39 C5AA 1.56(3) . ?
C40 C8AA 1.532(10) . ?
C41 C45 1.47(2) . ?
C42 C43 1.451(17) . ?
C43 C44 1.375(16) . ?
C44 C45 1.405(16) . ?
C44 C49 1.390(17) . ?
C45 C46 1.436(18) . ?
C46 C47 1.37(2) . ?
C47 C48 1.339(18) . ?
C48 C49 1.469(15) . ?
C48 C52 1.413(17) . ?
C49 C50 1.352(15) . ?
C50 C51 1.519(18) . ?
C53 C54 1.528(9) . ?
C53 C58 1.536(9) . ?
C53 C0AA 1.527(10) . ?
C54 C55 1.541(10) . ?
C54 C3AA 1.525(17) . ?
C55 C56 1.542(10) . ?
C56 C57 1.540(10) . ?
C57 C58 1.542(10) . ?
C57 C0AA 1.41(3) . ?
C57 C97 1.57(3) . ?
S5A C65 1.72(2) . ?
S5A C67A 1.54(6) . ?
S6 C66 1.83(4) . ?
S6 C67A 1.718(10) . ?
S7A C68A 1.79(3) . ?
S7A C70A 1.78(4) . ?
S8A C68A 1.749(16) . ?
S8A C69A 1.716(19) . ?
C65 C66 1.283(18) . ?
C67A C68A 1.56(6) . ?
C69A C70A 1.33(2) . ?
S1 C59 1.77(2) . ?
S1 C61 1.789(12) . ?
S2 C60 1.692(18) . ?
S2 C61 1.758(12) . ?
S3 C62 1.761(12) . ?
S3 C63 1.697(13) . ?
S4 C62 1.704(13) . ?
S4 C64 1.772(16) . ?
C59 C60 1.29(3) . ?
C61 C62 1.357(9) . ?
C63 C64 1.360(19) . ?
C67B S5B 1.89(4) . ?
C67B C68B 1.354(14) . ?
S8B C69B 1.45(4) . ?
S8B C68B 1.726(18) . ?
C70B S7B 1.72(2) . ?
C70B C69B 1.30(2) . ?
S7B C68B 1.77(3) . ?
S9 C71 1.85(3) . ?
S9 C74 1.80(3) . ?
S10 C72 1.707(16) . ?
S10 C74 1.73(3) . ?
C71 C72 1.271(18) . ?
C73 C74 1.37(2) . ?
C73 S11 1.67(4) . ?
C73 C76 1.11(5) 2_576 ?
C74 C76 1.69(4) 2_576 ?
S11 S12 0.879(10) 2_576 ?
S11 C76 1.803(18) . ?
S11 C75 1.40(3) 2_576 ?
S12 C75 1.67(3) . ?
C76 C75 1.36(4) . ?
C97 C3AA 1.51(5) . ?
C68 C5AA 1.52(5) . ?
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
N1 C1 C5 118.4(18) . . ?
O2 C1 N1 121.0(15) . . ?
O2 C1 C5 120.5(17) . . ?
C50 C1DA C5BA 120.4(17) . . ?
C1 N1 C2 121.5(13) . . ?
C1 N1 C58 137.6(18) . . ?
C1 N1 C0AA 101.1(17) . . ?
C2 N1 C58 100.5(13) . . ?
C2 N1 C0AA 135.8(15) . . ?
N1 C2 C3 118.7(13) . . ?
O1 C2 N1 121.9(17) . . ?
O1 C2 C3 119.4(19) . . ?
C13 N2 C14 121.5(11) . . ?
C13 N2 C15 133.8(13) . . ?
C13 N2 C2AA 97.4(13) . . ?
C14 N2 C15 99.8(12) . . ?
C14 N2 C2AA 138.0(15) . . ?
C4 C3 C2 118.3(14) . . ?
C12 C3 C2 119.5(13) . . ?
C12 C3 C4 122.0(15) . . ?
C21 N3 C20 115.7(11) . . ?
C22 N3 C20 120.3(12) . . ?
C22 N3 C21 123.7(8) . . ?
C3 C4 C5 125.8(13) . . ?
C3 C4 C9 120.1(13) . . ?
C5 C4 C9 114.1(10) . . ?
C33 N4 C35 138.7(16) . . ?
C33 N4 C8AA 103.1(17) . . ?
C34 N4 C33 123.4(13) . . ?
C34 N4 C35 97.2(12) . . ?
C34 N4 C8AA 131.6(16) . . ?
C4 C5 C1 116.4(12) . . ?
C4 C5 C6 124.2(11) . . ?
C6 C5 C1 119.4(13) . . ?
C1DA C5BA C43 123.1(15) . . ?
C41 N5 C40 119.9(13) . . ?
C41 N5 C42 124.9(10) . . ?
C42 N5 C40 114.6(12) . . ?
C7 C6 C5 119.0(12) . . ?
C51 N6 C53 114.1(14) . . ?
C52 N6 C51 123.9(10) . . ?
C52 N6 C53 121.8(15) . . ?
C6 C7 C4AA 122.7(10) . . ?
C32 C7AA C30 120.5(12) . . ?
C7 C4AA C14 120.7(11) . . ?
C9 C4AA C7 115.4(10) . . ?
C9 C4AA C14 123.9(11) . . ?
C4 C9 C10 118.8(12) . . ?
C4AA C9 C4 124.5(10) . . ?
C4AA C9 C10 116.6(11) . . ?
C9 C10 C13 121.2(13) . . ?
C11 C10 C9 117.8(16) . . ?
C11 C10 C13 121.0(15) . . ?
C10 C11 C12 121.5(14) . . ?
C3 C12 C11 119.7(13) . . ?
N2 C13 C10 117.6(12) . . ?
O3 C13 N2 118.6(18) . . ?
O3 C13 C10 123(2) . . ?
N2 C14 C4AA 116.5(13) . . ?
O4 C14 N2 117.6(14) . . ?
O4 C14 C4AA 125.0(16) . . ?
N2 C15 C16 113.0(12) . . ?
N2 C15 C20 107.5(10) . . ?
C20 C15 C16 104.5(11) . . ?
C17 C16 C15 125.9(14) . . ?
C2AA C16 C1AA 122.8(14) . . ?
C16 C17 C18 116.5(16) . . ?
C19 C18 C17 113.8(16) . . ?
C1AA C18 C19 112.3(17) . . ?
C20 C19 C18 116.2(13) . . ?
N3 C20 C15 123.5(9) . . ?
N3 C20 C19 108.4(8) . . ?
N3 C20 C2AA 120.7(12) . . ?
C19 C20 C15 125.6(11) . . ?
C2AA C20 C19 124.5(13) . . ?
N3 C21 C25 118.0(10) . . ?
O6 C21 N3 119.7(9) . . ?
O6 C21 C25 122.3(11) . . ?
N3 C22 C23 117.9(9) . . ?
O5 C22 N3 121.8(12) . . ?
O5 C22 C23 120.2(12) . . ?
C24 C23 C22 117.9(10) . . ?
C32 C23 C22 118.8(12) . . ?
C32 C23 C24 123.2(11) . . ?
C23 C24 C29 117.0(10) . . ?
C25 C24 C23 123.7(10) . . ?
C25 C24 C29 119.2(10) . . ?
C24 C25 C21 117.6(11) . . ?
C26 C25 C21 120.1(11) . . ?
C26 C25 C24 122.0(11) . . ?
C27 C26 C25 120.3(11) . . ?
C26 C27 C28 121.2(10) . . ?
C27 C28 C29 119.9(12) . . ?
C27 C28 C33 124.2(13) . . ?
C33 C28 C29 115.6(13) . . ?
C24 C29 C28 117.2(11) . . ?
C30 C29 C24 121.3(10) . . ?
C30 C29 C28 121.6(12) . . ?
C7AA C30 C34 120.7(13) . . ?
C29 C30 C7AA 119.4(11) . . ?
C29 C30 C34 119.8(13) . . ?
C23 C32 C7AA 118.1(14) . . ?
N4 C33 C28 121.7(15) . . ?
O8 C33 N4 119.4(13) . . ?
O8 C33 C28 118.8(18) . . ?
N4 C34 C30 117.1(13) . . ?
O7 C34 N4 126.4(15) . . ?
O7 C34 C30 116.5(19) . . ?
N4 C35 C36 112.7(11) . . ?
N4 C35 C40 111.3(11) . . ?
C40 C35 C36 107.9(10) . . ?
C35 C36 C37 122.8(11) . . ?
C68 C36 C8AA 122(2) . . ?
C38 C37 C36 113.0(17) . . ?
C39 C38 C37 114.7(16) . . ?
C40 C39 C38 113.5(13) . . ?
C40 C39 C5AA 106.6(14) . . ?
N5 C40 C35 120.8(10) . . ?
N5 C40 C39 113.6(9) . . ?
N5 C40 C8AA 119.7(13) . . ?
C39 C40 C35 124.5(9) . . ?
C39 C40 C8AA 118.9(13) . . ?
N5 C41 C45 116.4(11) . . ?
O9 C41 N5 122.0(13) . . ?
O9 C41 C45 121.5(14) . . ?
N5 C42 C43 114.4(10) . . ?
O10 C42 N5 118.2(12) . . ?
O10 C42 C43 127.1(12) . . ?
C5BA C43 C42 120.3(12) . . ?
C44 C43 C5BA 116.0(12) . . ?
C44 C43 C42 123.5(11) . . ?
C43 C44 C45 118.4(12) . . ?
C43 C44 C49 118.7(10) . . ?
C49 C44 C45 122.8(10) . . ?
C44 C45 C41 121.4(11) . . ?
C44 C45 C46 116.3(13) . . ?
C46 C45 C41 122.3(12) . . ?
C47 C46 C45 120.3(13) . . ?
C48 C47 C46 124.4(12) . . ?
C47 C48 C49 117.6(11) . . ?
C47 C48 C52 122.7(11) . . ?
C52 C48 C49 119.7(10) . . ?
C44 C49 C48 118.5(10) . . ?
C50 C49 C44 124.0(11) . . ?
C50 C49 C48 117.4(11) . . ?
C1DA C50 C49 117.6(14) . . ?
C1DA C50 C51 119.2(13) . . ?
C49 C50 C51 123.0(12) . . ?
N6 C51 C50 114.1(10) . . ?
O12 C51 N6 121.6(13) . . ?
O12 C51 C50 123.5(15) . . ?
N6 C52 C48 121.4(11) . . ?
O11 C52 N6 115.1(12) . . ?
O11 C52 C48 123.4(12) . . ?
N6 C53 C54 114.0(9) . . ?
N6 C53 C58 124.2(11) . . ?
N6 C53 C0AA 125.0(15) . . ?
C54 C53 C58 117.1(11) . . ?
C0AA C53 C54 117.8(14) . . ?
C53 C54 C55 108.2(13) . . ?
C3AA C54 C53 116.9(15) . . ?
C56 C55 C54 107.0(18) . . ?
C57 C56 C55 103.9(15) . . ?
C56 C57 C58 101.6(15) . . ?
C0AA C57 C97 110.5(19) . . ?
N1 C58 C53 107.4(11) . . ?
N1 C58 C57 112.4(13) . . ?
C53 C58 C57 109.4(11) . . ?
C67A S5A C65 88.4(17) . . ?
C67A S6 C66 90(2) . . ?
C70A S7A C68A 93.8(14) . . ?
C69A S8A C68A 96.3(15) . . ?
C66 C65 S5A 128(2) . . ?
C65 C66 S6 107(2) . . ?
S5A C67A S6 126(4) . . ?
S5A C67A C68A 111.6(13) . . ?
C68A C67A S6 122(4) . . ?
S8A C68A S7A 111.7(13) . . ?
C67A C68A S7A 125.0(17) . . ?
C67A C68A S8A 122(2) . . ?
C70A C69A S8A 118(3) . . ?
C69A C70A S7A 113(3) . . ?
C59 S1 C61 93.3(7) . . ?
C60 S2 C61 95.5(8) . . ?
C63 S3 C62 94.3(5) . . ?
C62 S4 C64 95.4(6) . . ?
C60 C59 S1 117.5(13) . . ?
C59 C60 S2 120.2(14) . . ?
S2 C61 S1 113.4(6) . . ?
C62 C61 S1 122.4(10) . . ?
C62 C61 S2 124.2(10) . . ?
S4 C62 S3 115.7(6) . . ?
C61 C62 S3 120.9(10) . . ?
C61 C62 S4 123.2(10) . . ?
C64 C63 S3 119.8(10) . . ?
C63 C64 S4 114.2(11) . . ?
C68B C67B S5B 146(2) . . ?
C69B S8B C68B 87(2) . . ?
C69B C70B S7B 112(4) . . ?
C70B S7B C68B 87(2) . . ?
C70B C69B S8B 134(4) . . ?
C67B C68B S8B 126(2) . . ?
C67B C68B S7B 115.2(16) . . ?
S8B C68B S7B 118.5(14) . . ?
C74 S9 C71 96.8(12) . . ?
C72 S10 C74 95.9(13) . . ?
C72 C71 S9 109.5(19) . . ?
C71 C72 S10 126.1(19) . . ?
C74 C73 S11 125(3) . . ?
C76 C73 C74 85(3) 2_576 . ?
C76 C73 S11 117(4) 2_576 . ?
C73 C74 S10 129(3) . . ?
C73 C74 C76 41(2) . 2_576 ?
C76 C74 S10 100.8(19) 2_576 . ?
C73 S11 C73 81.7(15) . 2_576 ?
C73 S11 C76 95.7(16) . . ?
S12 S11 C73 119.9(18) 2_576 . ?
S12 S11 C73 49.3(13) 2_576 2_576 ?
S12 S11 C76 59.6(12) 2_576 . ?
S12 S11 C75 91.7(17) 2_576 2_576 ?
C76 S11 C73 29.2(12) . 2_576 ?
C75 S11 C73 85.1(18) 2_576 2_576 ?
C75 S11 C73 45.5(19) 2_576 . ?
C75 S11 C76 113.0(17) 2_576 . ?
C73 S12 C73 79.2(15) . 2_576 ?
C75 S12 C73 93.9(17) . . ?
C75 S12 C73 32.1(14) . 2_576 ?
C53 C0AA N1 101.8(15) . . ?
C57 C0AA N1 112.7(18) . . ?
C57 C0AA C53 117.5(17) . . ?
C18 C1AA C16 115.8(17) . . ?
N2 C2AA C16 118.1(15) . . ?
N2 C2AA C20 111.0(14) . . ?
C16 C2AA C20 106.7(13) . . ?
C36 C8AA N4 113(2) . . ?
C36 C8AA C40 114.1(15) . . ?
C40 C8AA N4 105.9(14) . . ?
S12 C76 S11 29.2(5) 2_576 . ?
C75 C76 S11 113(2) . . ?
C75 C76 S12 124(2) . 2_576 ?
C73 C75 S12 101(3) 2_576 . ?
C73 C75 C76 51(3) 2_576 . ?
C76 C75 S12 120(2) . . ?
C3AA C97 C57 116(2) . . ?
C54 C3AA C97 110(2) . . ?
C36 C68 C5AA 109(3) . . ?
C68 C5AA C39 117(3) . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.724 -0.290 -0.615 849.0 157.5 ?
2 0.125 0.045 0.121 0.2 0.0 ?
3 0.133 0.760 0.537 0.1 0.0 ?
4 0.133 0.827 0.806 0.2 -0.0 ?
5 0.209 0.036 0.483 0.2 0.1 ?
6 0.251 0.549 0.712 0.3 0.1 ?
7 0.307 0.507 0.688 0.1 0.0 ?
8 0.693 0.493 0.312 0.1 0.0 ?
9 0.749 0.451 0.288 0.3 0.1 ?
10 0.791 0.964 0.516 0.2 0.1 ?
11 0.867 0.173 0.194 0.2 -0.0 ?
12 0.867 0.240 0.463 0.1 0.0 ?
13 0.875 0.955 0.879 0.2 0.0 ?
_shelx_res_file
;
TITL
yb016bisf.res
created by SHELXL-2018/3 at 09:31:32 on 26-Jul-2019
CELL 1.54178 15.8923 15.9624 16.7921 69.4231 69.3397 70.9587
ZERR 2 0.001 0.001 0.0011 0.0041 0.004 0.004
LATT 1
SFAC C H N O S
UNIT 150 106 12 24 20
EQIV $1 -X,2-Y,1-Z
DFIX 1.7 S10 C72
DFIX 1.71 S8A C69A
DFIX 1.73 C68A S8A
DFIX 1.54 C35 C40
DFIX 1.54 C20 C15
DFIX 1.54 C58 C53
DFIX 1.33 C69A C70A
DFIX 1.28 C71_$1 C72_$1
DFIX 1.54 0.01 C39 C38
DFIX 1.54 0.01 C40 C39
DFIX 1.54 0.01 C40 C35
DFIX 1.54 0.01 C35 C36
DFIX 1.54 0.01 C36 C37
DFIX 1.54 0.01 C37 C38
DFIX 1.54 0.01 C15 C20
DFIX 1.54 0.01 C20 C19
DFIX 1.54 0.01 C19 C18
DFIX 1.54 0.01 C18 C17
DFIX 1.54 0.01 C17 C16
DFIX 1.54 0.01 C16 C15
DFIX 1.54 0.01 C53 C58
DFIX 1.54 0.01 C58 C57
DFIX 1.54 0.01 C57 C56
DFIX 1.54 0.01 C56 C55
DFIX 1.54 0.01 C55 C54
DFIX 1.54 0.01 C54 C53
DFIX 1.3 C69B C70B
DFIX 1.71 C70B S7B
DFIX 1.3 C65 C66
DFIX 1.71 C68B S8B
DFIX 1.34 C67B C68B
DFIX 1.36 0.01 C62 C61
DFIX 1.36 C68B C67B
DFIX 1.72 0.01 S6 C67A
DFIX 1.49 0.01 N3 C20
DFIX 1.49 0.01 N4 C35
DFIX 1.49 0.01 N5 C40
DFIX 1.49 0.01 N1 C58
DFIX 1.49 0.01 N2 C15
DFIX 1.54 0.01 C53 C0AA
DFIX 1.54 0.01 C40 C8AA
DFIX 1.54 0.01 C20 C2AA
DFIX 1.38 C74 C73
DFIX 0.98 0.005 C76 H76
DFIX 0.98 0.005 C75 H75
DFIX 1.78 S11 C76
DFIX 1.54 C54 C3AA
DFIX 1.54 C1AA C18
DFIX 1.54 C1AA C16
SADI C40 C35 C36 C37 C38 C39
SADI 0.01 C20 C15 C20 C19 C19 C18 C18 C17 C17 C16 C16 C15
SADI 0.01 C20 C19 C18 C17 C16 C15
SADI N2 C15 N3 C20 N4 C35 N5 C40 C53 N6 C58 N1
SADI 0.005 C75 H75 C76 H76
FLAT 0.01 S9 S10 C71 C72
FLAT 0.01 S5A S6 C65 C66
FLAT 0.02 H75 C75 H76 C76
SIMU 0.04 0.08 1.7 N6 N5
SIMU 0.04 0.08 1.7 C75 C76
ISOR 0.01 0.1 C74
ISOR 0.01 0.1 C67A C67B C68B C68A C69B
ISOR 0.01 0.1 C58
ISOR 0.01 0.1 C66
ISOR 0.01 0.1 C70A
ISOR 0.01 0.1 C17
ISOR 0.01 0.1 C48 C49 C1DA
ISOR 0.01 0.1 C69A
ISOR 0.005 0.1 C70B
ISOR 0.01 0.1 C4AA
ISOR 0.01 0.1 C71 C72
ISOR 0.01 0.1 C67B
ISOR 0.01 0.1 C1AA
ISOR 0.01 0.1 C24
ISOR 0.01 0.1 C2AA
ISOR 0.01 0.2 C73
ISOR 0.01 0.01 C36
ISOR 0.01 0.01 C2
ISOR 0.01 0.01 N6
ISOR 0.01 0.01 C52
ISOR 0.01 0.01 C0AA
ISOR 0.01 0.01 C15
ISOR 0.01 0.01 C46 C47
ISOR 0.01 0.01 C75
ISOR 0.01 0.01 C51
ISOR 0.02 0.02 C56 C3AA C97
ISOR 0.02 0.02 C12
ISOR 0.02 0.02 C35 C68
ISOR 0.01 0.01 C38
ISOR 0.02 0.02 C5AA C38
ISOR 0.025 0.025 O7
ISOR 0.02 0.02 C55 C56
ISOR 0.02 0.02 C50
EADP O11 O12
L.S. 20
PLAN 0
TEMP -169.89
CONN 3 C74
BIND C74 S10
FREE C74 H76_$1
FREE C74 H75_$1
CONN 3 C73
BIND C73 S11
BIND C73 S12
FREE C73 C75_$1
FREE S10 H76_$1
CONN 2 S7B
BIND S11 C76
FREE S12 S11_$1
FREE S12 H75
FREE S12 C76_$1
FREE H75 S9_$1
FREE H75 S11_$1
FREE C76 C74_$1
FREE C76 C73_$1
CONN 3 C75
BIND C75 S12
FREE C75 S11_$1
CONN 3 H76
FREE H76 C73_$1
ABIN
fmap 2
acta
OMIT -1 7 4
OMIT -5 0 5
OMIT 8 0 1
OMIT 8 3 0
OMIT 9 6 8
OMIT 3 3 3
OMIT -2 -1 1
OMIT 1 0 4
OMIT 0 -4 1
OMIT -10 3 6
OMIT -1 7 3
OMIT -5 -1 2
OMIT 0 -3 1
OMIT 3 0 5
OMIT -3 10 4
OMIT -3 0 2
OMIT -3 0 1
OMIT 4 -1 7
REM
REM
REM
WGHT 0.193700 80.177299
EXTI 0.024901
FVAR 0.12792
C1 1 0.241844 0.584966 0.376052 11.00000 0.14545 0.04850 =
0.06368 0.03270 -0.07559 -0.05473
C1DA 1 0.056299 0.993450 0.260700 11.00000 0.07672 0.07385 =
0.09055 -0.03712 0.00263 -0.00686
AFIX 43
H1DA 2 -0.005842 0.989096 0.290585 11.00000 -1.20000
AFIX 0
N1 3 0.149903 0.609791 0.377221 11.00000 0.09209 0.07224 =
0.08985 0.00898 -0.07707 -0.02462
O1 4 -0.001989 0.635950 0.459593 11.00000 0.06137 0.06800 =
0.20360 0.00590 -0.07599 -0.01975
C2 1 0.079224 0.628285 0.452495 11.00000 0.07074 0.08472 =
0.08452 -0.00081 -0.04310 -0.03428
N2 3 0.271085 0.682710 0.710636 11.00000 0.13718 0.05878 =
0.02215 -0.01327 -0.00036 -0.05603
O2 4 0.300955 0.561110 0.315007 11.00000 0.14427 0.11129 =
0.04326 -0.04417 -0.00509 -0.05234
C3 1 0.104803 0.637167 0.524973 11.00000 0.01308 0.03728 =
0.06884 0.00531 -0.00826 0.01165
N3 3 0.321404 0.854043 0.685978 11.00000 0.06360 0.04821 =
0.02335 -0.00862 -0.00357 -0.02428
O3 4 0.119575 0.727024 0.777544 11.00000 0.16076 0.10913 =
0.06856 -0.04493 0.00428 0.01241
C4 1 0.194989 0.621045 0.518871 11.00000 0.03016 0.04530 =
0.03574 0.01933 -0.01133 -0.01786
N4 3 0.345080 1.196104 0.282305 11.00000 0.14786 0.04979 =
0.06284 -0.02083 -0.04139 -0.03384
O4 4 0.419849 0.616559 0.655606 11.00000 0.10821 0.07520 =
0.08323 0.02816 -0.08438 -0.04852
C5 1 0.267264 0.592579 0.452310 11.00000 0.02342 0.04101 =
0.02584 0.01306 -0.01164 -0.01230
PART -1
C5BA 1 0.082334 1.071757 0.247168 11.00000 0.02333 0.05787 =
0.13866 -0.02350 0.01461 -0.00551
AFIX 43
H5BA 2 0.037374 1.120515 0.268920 11.00000 -1.20000
AFIX 0
PART 0
N5 3 0.289887 1.171437 0.145502 11.00000 0.07577 0.03071 =
0.05882 0.01029 -0.02996 -0.02810
O5 4 0.177605 0.934348 0.740633 11.00000 0.04296 0.14212 =
0.05264 -0.03948 0.02241 -0.05059
C6 1 0.359872 0.574547 0.449192 11.00000 0.03305 0.04552 =
0.04049 -0.00114 -0.00344 -0.02334
AFIX 43
H6 2 0.407000 0.554236 0.401763 11.00000 -1.20000
AFIX 0
N6 3 0.158533 0.764457 0.218571 11.00000 0.06788 0.07131 =
0.04896 -0.02930 -0.01579 -0.03237
O6 4 0.475408 0.786938 0.638092 11.00000 0.07861 0.05267 =
0.06433 0.00765 -0.05315 -0.01393
C7 1 0.381588 0.586221 0.513942 11.00000 0.02350 0.04162 =
0.05639 -0.00438 -0.01230 -0.00715
AFIX 43
H7 2 0.444853 0.571049 0.513013 11.00000 -1.20000
AFIX 0
C7AA 1 0.194224 1.156613 0.513906 11.00000 0.05847 0.04207 =
0.08262 -0.02598 -0.03684 -0.00049
AFIX 43
H7AA 2 0.147578 1.212047 0.509730 11.00000 -1.20000
AFIX 0
O7 4 0.211857 1.284787 0.347294 11.00000 0.14200 0.04729 =
0.11551 0.02080 -0.11821 -0.02483
C4AA 1 0.314297 0.620204 0.583708 11.00000 0.02037 0.04409 =
0.03145 -0.00170 -0.01167 -0.01176
O8 4 0.489519 1.114948 0.226402 11.00000 0.16960 0.08059 =
0.04394 -0.00202 -0.01323 -0.07622
C9 1 0.222435 0.635589 0.583609 11.00000 0.04549 0.05196 =
0.01925 -0.01804 -0.01371 0.00210
O9 4 0.426573 1.116809 0.062119 11.00000 0.04367 0.09082 =
0.09337 0.00226 -0.01160 -0.04736
C10 1 0.150765 0.671288 0.655352 11.00000 0.05406 0.03881 =
0.07158 -0.00089 0.00547 -0.01944
O10 4 0.144780 1.235432 0.211734 11.00000 0.09209 0.04303 =
0.06396 -0.02918 -0.00088 -0.00329
C11 1 0.063425 0.686299 0.656832 11.00000 0.03574 0.05482 =
0.08554 -0.03245 0.02506 0.00261
AFIX 43
H11 2 0.016001 0.709918 0.702230 11.00000 -1.20000
AFIX 0
O11 4 0.294321 0.708516 0.137255 11.00000 0.08642 0.08195 =
0.08559 -0.02313 0.00100 -0.03359
C12 1 0.038381 0.667595 0.590928 11.00000 0.03565 0.06736 =
0.10111 0.02153 -0.01720 -0.03190
AFIX 43
H12 2 -0.024834 0.676839 0.594394 11.00000 -1.20000
AFIX 0
O12 4 0.012074 0.823114 0.293764 11.00000 0.08642 0.08195 =
0.08559 -0.02313 0.00100 -0.03359
C13 1 0.175354 0.693082 0.721304 11.00000 0.07777 0.10632 =
0.04959 -0.04861 0.02316 -0.03449
C14 1 0.341488 0.632624 0.652516 11.00000 0.08837 0.10878 =
0.03114 0.01982 -0.02837 -0.07808
PART 1
C15 1 0.324705 0.678060 0.769843 10.50000 0.06019 0.07055 =
0.06717 -0.00443 -0.01817 -0.01764
AFIX 13
H15 2 0.390756 0.645884 0.749671 10.50000 -1.20000
AFIX 0
PART 0
C16 1 0.282997 0.632670 0.867385 11.00000 0.08337 0.04765 =
0.03796 -0.01057 -0.01209 -0.00109
PART 1
AFIX 23
H16A 2 0.221372 0.627278 0.870952 10.50000 -1.20000
H16B 2 0.321152 0.569087 0.879779 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H16C 2 0.320580 0.577981 0.845770 10.50000 -1.20000
H16D 2 0.223804 0.617305 0.906785 10.50000 -1.20000
AFIX 0
PART 0
PART 1
C17 1 0.268868 0.668261 0.946105 10.50000 0.06720 0.06347 =
0.04978 -0.01081 -0.02364 0.00097
AFIX 23
H17A 2 0.285384 0.614843 0.994811 10.50000 -1.20000
H17B 2 0.202294 0.696214 0.966649 10.50000 -1.20000
AFIX 0
PART 0
C18 1 0.323721 0.738995 0.929469 11.00000 0.06567 0.14325 =
0.05684 0.02788 -0.01604 -0.03662
PART 1
AFIX 23
H18A 2 0.291905 0.774763 0.973781 10.50000 -1.20000
H18B 2 0.385730 0.705786 0.938200 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H18C 2 0.370259 0.739686 0.955715 10.50000 -1.20000
H18D 2 0.261698 0.759920 0.967367 10.50000 -1.20000
AFIX 0
PART 0
C19 1 0.335210 0.805956 0.836810 11.00000 0.08477 0.10011 =
0.04961 -0.04560 -0.02205 0.00956
AFIX 23
H19A 2 0.292535 0.866076 0.841868 11.00000 -1.20000
H19B 2 0.398948 0.815225 0.815079 11.00000 -1.20000
AFIX 0
C20 1 0.317623 0.777051 0.767385 11.00000 0.15499 0.11732 =
0.03713 -0.02090 0.01585 -0.12356
PART 1
AFIX 13
H20 2 0.248743 0.792706 0.790064 10.50000 -1.20000
AFIX 13
PART 0
PART 2
H20A 2 0.380337 0.737498 0.748444 10.50000 -1.20000
AFIX 0
PART 0
C21 1 0.406270 0.848501 0.621007 11.00000 0.03490 0.03578 =
0.03263 0.01532 -0.02193 -0.02112
C22 1 0.247797 0.929715 0.680823 11.00000 0.02725 0.05780 =
0.02968 -0.01035 0.01579 -0.02718
C23 1 0.256305 1.006879 0.596775 11.00000 0.05027 0.03189 =
0.03304 -0.00103 0.01426 -0.00824
C24 1 0.338342 0.996683 0.528209 11.00000 0.02261 0.03394 =
0.02908 -0.00351 -0.00215 -0.01232
C25 1 0.411389 0.919639 0.533723 11.00000 0.06648 0.02678 =
0.04376 -0.00461 -0.02202 -0.00348
C26 1 0.489433 0.911804 0.465460 11.00000 0.02874 0.05668 =
0.05598 -0.02561 0.00542 -0.00465
AFIX 43
H26 2 0.540465 0.861085 0.473295 11.00000 -1.20000
AFIX 0
C27 1 0.494458 0.976434 0.386112 11.00000 0.02427 0.06016 =
0.02751 -0.01791 0.01785 -0.00216
AFIX 43
H27 2 0.547282 0.967769 0.337909 11.00000 -1.20000
AFIX 0
C28 1 0.424034 1.054421 0.374490 11.00000 0.03871 0.05725 =
0.04292 -0.02784 -0.00218 -0.00021
C29 1 0.342715 1.067896 0.447111 11.00000 0.04458 0.05128 =
0.03626 -0.01360 0.01753 -0.02628
C30 1 0.272688 1.145398 0.438805 11.00000 0.02800 0.05147 =
0.04822 -0.00913 -0.01423 -0.01013
C32 1 0.186283 1.086480 0.592853 11.00000 0.03520 0.03835 =
0.12082 -0.03843 -0.00575 -0.00545
AFIX 43
H32 2 0.134460 1.093138 0.642358 11.00000 -1.20000
AFIX 0
C33 1 0.420774 1.121143 0.291053 11.00000 0.15432 0.05508 =
0.02235 0.00581 -0.01998 -0.05038
C34 1 0.276267 1.216146 0.349866 11.00000 0.16901 0.02024 =
0.08312 -0.00522 -0.09139 -0.00826
PART 1
C35 1 0.317876 1.280781 0.213872 10.50000 0.02240 0.05472 =
0.02912 -0.01913 0.01659 -0.01555
AFIX 13
H35 2 0.254838 1.314902 0.240574 10.50000 -1.20000
AFIX 0
PART 0
C36 1 0.384301 1.345050 0.179766 11.00000 0.02938 0.02999 =
0.04155 -0.00821 -0.00126 -0.00925
PART 1
AFIX 23
H36A 2 0.444186 1.306237 0.190521 10.50000 -1.20000
H36B 2 0.360396 1.387006 0.218436 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H36C 2 0.343967 1.358722 0.236129 10.50000 -1.20000
H36D 2 0.448409 1.339941 0.178813 10.50000 -1.20000
AFIX 0
PART 0
PART 1
C37 1 0.406110 1.405754 0.083660 10.50000 0.04618 0.02355 =
0.04046 0.00333 -0.01460 -0.02538
AFIX 23
H37A 2 0.405772 1.467679 0.084210 10.50000 -1.20000
H37B 2 0.468978 1.378776 0.051257 10.50000 -1.20000
AFIX 0
C38 1 0.336817 1.415313 0.034370 10.50000 0.05334 0.04483 =
0.04925 -0.00611 -0.01446 -0.00833
AFIX 23
H38A 2 0.278358 1.457788 0.056148 10.50000 -1.20000
H38B 2 0.361668 1.443654 -0.029213 10.50000 -1.20000
AFIX 0
PART 0
C39 1 0.315257 1.324526 0.044390 11.00000 0.05058 0.03600 =
0.02835 -0.01415 0.00946 -0.00524
PART 1
AFIX 23
H39A 2 0.254298 1.338108 0.033431 10.50000 -1.20000
H39B 2 0.362195 1.295195 -0.001079 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H39C 2 0.251634 1.358724 0.041284 10.50000 -1.20000
H39D 2 0.343208 1.291435 -0.002184 10.50000 -1.20000
AFIX 0
PART 0
C40 1 0.313945 1.257466 0.134472 11.00000 0.09833 0.06572 =
0.09247 -0.00729 -0.02219 -0.04109
PART 1
AFIX 13
H40 2 0.381949 1.230499 0.117413 10.50000 -1.20000
AFIX 13
PART 0
PART 2
H40A 2 0.254207 1.288442 0.169787 10.50000 -1.20000
AFIX 0
PART 0
C41 1 0.353504 1.106022 0.106747 11.00000 0.04989 0.05855 =
0.05607 -0.01224 -0.02395 -0.01665
C42 1 0.194765 1.170362 0.187189 11.00000 0.03745 0.02740 =
0.06355 -0.00538 -0.01071 -0.00020
C43 1 0.172471 1.083772 0.202592 11.00000 0.02759 0.04986 =
0.05581 -0.02477 0.02059 -0.01665
C44 1 0.233975 1.012246 0.170038 11.00000 0.01596 0.04593 =
0.04067 -0.01781 0.00364 0.00833
C45 1 0.323863 1.022532 0.120819 11.00000 0.01849 0.07073 =
0.03733 -0.02711 0.00855 0.00356
C46 1 0.384282 0.947490 0.085201 11.00000 0.04680 0.05358 =
0.05152 -0.01116 0.00646 -0.00391
AFIX 43
H46 2 0.444793 0.952061 0.048909 11.00000 -1.20000
AFIX 0
C47 1 0.355012 0.869333 0.103347 11.00000 0.05782 0.04173 =
0.05513 -0.02435 0.00800 -0.00099
AFIX 43
H47 2 0.397237 0.820903 0.079179 11.00000 -1.20000
AFIX 0
C48 1 0.270896 0.856586 0.152852 11.00000 0.02568 0.04305 =
0.02754 -0.01856 -0.00460 0.00301
C49 1 0.205133 0.932485 0.188336 11.00000 0.04000 0.04438 =
0.02647 -0.02027 0.01047 -0.01521
C50 1 0.117978 0.922335 0.232036 11.00000 0.01711 0.05880 =
0.05755 -0.02166 0.01746 -0.01669
C51 1 0.089695 0.832479 0.256261 11.00000 0.04166 0.07267 =
0.07411 -0.00772 -0.01373 -0.03932
C52 1 0.243322 0.774892 0.169848 11.00000 0.06548 0.04554 =
0.03272 -0.01079 0.00203 -0.02298
C53 1 0.126219 0.682285 0.230313 11.00000 0.27085 0.07015 =
0.07253 0.02650 -0.09799 -0.10232
PART 1
AFIX 13
H53 2 0.188375 0.642340 0.210394 10.50000 -1.20000
AFIX 13
PART 0
PART 2
H53A 2 0.064811 0.699353 0.272318 10.50000 -1.20000
AFIX 0
PART 0
C54 1 0.087786 0.689505 0.155967 11.00000 0.03420 0.06693 =
0.03419 -0.02290 0.00247 -0.01835
PART 2
AFIX 23
H54C 2 0.043120 0.749590 0.145460 10.50000 -1.20000
H54D 2 0.139381 0.689803 0.101456 10.50000 -1.20000
AFIX 23
PART 0
PART 1
H54A 2 0.124955 0.720499 0.098382 10.50000 -1.20000
H54B 2 0.023117 0.726006 0.165096 10.50000 -1.20000
AFIX 0
C55 1 0.091944 0.591491 0.156621 10.50000 0.07039 0.04389 =
0.06875 -0.00874 -0.04900 -0.00016
AFIX 23
H55A 2 0.063273 0.593822 0.112020 10.50000 -1.20000
H55B 2 0.156931 0.556298 0.142774 10.50000 -1.20000
AFIX 0
C56 1 0.038484 0.545535 0.250015 10.50000 0.01115 0.06840 =
0.08403 -0.00955 -0.00463 -0.02051
AFIX 23
H56A 2 -0.019704 0.588446 0.271571 10.50000 -1.20000
H56B 2 0.023765 0.489594 0.250647 10.50000 -1.20000
AFIX 0
PART 0
C57 1 0.105397 0.521141 0.306683 11.00000 0.05104 0.02765 =
0.05152 -0.01729 -0.00746 -0.00048
PART 1
AFIX 23
H57A 2 0.169748 0.496861 0.275137 10.50000 -1.20000
H57B 2 0.087121 0.475682 0.363679 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H57C 2 0.045526 0.534558 0.350733 10.50000 -1.20000
H57D 2 0.140261 0.459019 0.331746 10.50000 -1.20000
AFIX 0
PART 0
PART 1
C58 1 0.094020 0.615327 0.320123 10.50000 0.05284 0.05448 =
0.05392 -0.01285 -0.01547 -0.01681
AFIX 13
H58 2 0.027357 0.640110 0.347378 10.50000 -1.20000
AFIX 0
S5A 5 0.295204 1.015356 -0.105501 10.50000 0.04123 0.03022 =
0.19361 -0.05779 -0.05751 0.01809
S6 5 0.294910 1.196456 -0.102656 11.00000 0.15204 0.06621 =
0.09836 -0.02284 -0.03727 -0.04334
S7A 5 0.085175 1.019176 -0.000462 10.50000 0.05008 0.06159 =
0.11367 -0.04312 0.01492 -0.01294
S8A 5 0.069523 1.201316 0.014434 10.50000 0.06861 0.07109 =
0.06597 -0.04809 0.01106 -0.00873
C65 1 0.397386 1.048650 -0.139104 11.00000 0.03375 0.14756 =
0.07379 -0.05066 -0.00776 -0.00045
AFIX 43
H65 2 0.451705 1.004862 -0.157901 11.00000 -1.20000
AFIX 0
C66 1 0.409449 1.125398 -0.141965 11.00000 0.15545 0.15397 =
0.16186 -0.04029 -0.04655 -0.03967
AFIX 43
H66 2 0.466888 1.142278 -0.160881 11.00000 -1.20000
AFIX 0
C67A 1 0.245138 1.107574 -0.081977 10.50000 0.10171 0.10649 =
0.10274 -0.03242 -0.02917 -0.01945
C68A 1 0.144260 1.106372 -0.022502 10.50000 0.02854 0.03586 =
0.03396 -0.00911 -0.00397 -0.00611
C69A 1 -0.022940 1.151462 0.071396 10.50000 0.06938 0.07887 =
0.07236 -0.01740 -0.01623 -0.01552
AFIX 43
H69A 2 -0.081983 1.186856 0.094622 10.50000 -1.20000
AFIX 0
C70A 1 -0.009716 1.061904 0.082160 10.50000 0.07910 0.09586 =
0.09637 -0.00958 -0.02466 -0.02595
AFIX 43
H70A 2 -0.047084 1.024437 0.129163 10.50000 -1.20000
AFIX 0
PART 0
S1 5 0.597391 0.626106 0.302407 11.00000 0.06175 0.06356 =
0.06718 -0.01597 -0.02817 -0.00911
S2 5 0.801615 0.575456 0.237661 11.00000 0.06345 0.06124 =
0.04973 -0.01953 0.00282 -0.01719
S3 5 0.612608 0.660412 0.474233 11.00000 0.04247 0.05583 =
0.04131 -0.01773 0.00299 -0.00571
S4 5 0.814960 0.618351 0.409614 11.00000 0.03775 0.06847 =
0.07409 -0.02965 -0.01258 -0.00749
C59 1 0.649381 0.586668 0.205905 11.00000 0.11355 0.07494 =
0.07896 -0.01484 -0.05168 -0.03822
AFIX 43
H59 2 0.613024 0.580356 0.174888 11.00000 -1.20000
AFIX 0
C60 1 0.738602 0.566803 0.179265 11.00000 0.07688 0.06225 =
0.07633 -0.02340 -0.02062 -0.02080
AFIX 43
H60 2 0.768894 0.547284 0.126737 11.00000 -1.20000
AFIX 0
C61 1 0.706075 0.610983 0.321237 11.00000 0.03733 0.06349 =
0.03899 -0.00767 -0.00233 -0.02244
C62 1 0.712519 0.625203 0.393741 11.00000 0.04756 0.04441 =
0.03970 -0.01733 -0.00092 -0.01273
C63 1 0.672094 0.657697 0.541825 11.00000 0.03448 0.04352 =
0.02958 -0.01205 0.01023 -0.00931
AFIX 43
H63 2 0.639860 0.669968 0.597586 11.00000 -1.20000
AFIX 0
C64 1 0.766085 0.637895 0.515904 11.00000 0.06923 0.04269 =
0.05699 -0.00452 -0.03092 -0.00326
AFIX 43
H64 2 0.802410 0.634807 0.551701 11.00000 -1.20000
AFIX 0
PART 2
C67B 1 0.231359 1.109952 -0.066105 10.50000 0.01526 0.03483 =
0.02150 -0.01339 0.00737 -0.00201
S8B 5 0.105444 1.254067 -0.004315 10.50000 0.07138 0.07953 =
0.05861 -0.03498 -0.00075 -0.00147
C70B 1 -0.005949 1.149450 0.076841 10.50000 0.17422 0.17491 =
0.17401 -0.04665 -0.04698 -0.03928
AFIX 43
H70B 2 -0.060414 1.137290 0.121811 10.50000 -1.20000
AFIX 0
S7B 5 0.064850 1.076596 0.012893 10.50000 0.05460 0.11846 =
0.09238 -0.00210 -0.00539 -0.04594
C69B 1 0.023631 1.223324 0.056585 10.50000 0.07998 0.08390 =
0.07436 -0.02571 -0.01153 -0.01610
AFIX 43
H69B 2 -0.017123 1.266324 0.088561 10.50000 -1.20000
AFIX 0
S5B 5 0.310104 1.009199 -0.110810 10.50000 0.28016 0.16724 =
0.21682 -0.13680 0.00062 -0.05855
C68B 1 0.144140 1.147268 -0.024674 10.50000 0.05456 0.05662 =
0.05631 -0.01595 -0.00833 -0.01439
PART 0
PART 1
S9 5 0.198189 0.814384 0.404097 10.50000 0.07255 0.04251 =
0.07418 -0.00292 -0.03673 -0.02669
S10 5 0.261271 0.979224 0.369728 10.50000 0.08511 0.05965 =
0.06056 -0.00365 -0.03516 -0.03532
C71 1 0.322746 0.808772 0.351706 10.50000 0.04936 0.04892 =
0.04948 0.00331 -0.01697 -0.00143
AFIX 43
H71 2 0.367197 0.756856 0.335334 10.50000 -1.20000
AFIX 0
C72 1 0.339835 0.885027 0.340929 10.50000 0.03093 0.04772 =
0.05475 -0.00917 -0.01349 -0.01809
AFIX 43
H72 2 0.402188 0.890093 0.314350 10.50000 -1.20000
AFIX 0
PART 0
C73 1 0.075512 0.970111 0.444638 10.50000 0.10095 0.08589 =
0.09388 -0.02999 -0.02029 -0.02647
PART 1
C74 1 0.166524 0.930869 0.411161 10.50000 0.06760 0.06802 =
0.07323 -0.01122 -0.02334 -0.02913
PART 0
S11 5 -0.009784 0.914835 0.489790 10.50000 0.07253 0.06298 =
0.04966 -0.00311 -0.02073 -0.02945
S12 5 0.044614 1.084889 0.456360 10.50000 0.08051 0.04308 =
0.06900 0.00297 -0.03431 -0.03389
PART 2
C0AA 1 0.155866 0.586594 0.289255 10.50000 0.04826 0.05748 =
0.05028 -0.01041 -0.02371 -0.00862
AFIX 13
H0AA 2 0.222210 0.560919 0.261806 10.50000 -1.20000
AFIX 0
C1AA 1 0.334628 0.643212 0.928039 10.50000 0.06128 0.05415 =
0.04404 -0.02054 0.00431 -0.01035
AFIX 23
H1AA 2 0.311662 0.606984 0.989284 10.50000 -1.20000
H1AB 2 0.401392 0.615828 0.907701 10.50000 -1.20000
AFIX 0
C2AA 1 0.260566 0.708027 0.788464 10.50000 0.03637 0.03453 =
0.03340 -0.00147 -0.01517 -0.00222
AFIX 13
H2AA 2 0.194256 0.739894 0.807897 10.50000 -1.20000
AFIX 0
C8AA 1 0.379040 1.256154 0.184062 10.50000 0.09466 0.03115 =
0.03660 0.02044 -0.01785 -0.03502
AFIX 13
H8AA 2 0.442435 1.222912 0.157073 10.50000 -1.20000
AFIX 0
PART 0
C76 1 -0.100663 1.014157 0.509895 10.50000 0.05442 0.10011 =
0.06082 -0.00482 -0.04119 -0.03633
C75 1 -0.069150 1.091194 0.487599 10.50000 0.06423 0.06850 =
0.06396 -0.01743 -0.01113 -0.01421
H76 2 -0.158454 0.997686 0.549805 11.00000 0.05154
H75 2 -0.121188 1.127743 0.523083 11.00000 0.03000
PART 2
C97 1 0.087728 0.523229 0.219854 10.50000 0.08643 0.08212 =
0.06718 -0.04854 -0.02175 -0.02416
AFIX 23
H97A 2 0.148018 0.502074 0.179677 10.50000 -1.20000
H97B 2 0.050161 0.478266 0.235041 10.50000 -1.20000
AFIX 0
C3AA 1 0.040020 0.614631 0.170164 10.50000 0.02975 0.06682 =
0.07904 -0.00732 -0.01110 -0.02506
AFIX 23
H3AA 2 0.041301 0.610453 0.112288 10.50000 -1.20000
H3AB 2 -0.025400 0.630603 0.203932 10.50000 -1.20000
AFIX 0
C68 1 0.362392 1.422000 0.112553 10.50000 0.07532 0.07200 =
0.08700 -0.02305 -0.04314 0.00044
AFIX 23
H68A 2 0.403344 1.463824 0.097237 10.50000 -1.20000
H68B 2 0.297714 1.455591 0.132536 10.50000 -1.20000
AFIX 0
C5AA 1 0.374335 1.392063 0.031650 10.50000 0.04604 0.03529 =
0.03634 -0.01939 -0.00613 0.00738
AFIX 23
H5AA 2 0.440331 1.362532 0.010601 10.50000 -1.20000
H5AB 2 0.359283 1.447900 -0.015665 10.50000 -1.20000
AFIX 0
HKLF 4
REM
REM wR2 = 0.465345, GooF = S = 1.01747, Restrained GooF = 1.01196 for all data
REM R1 = 0.199522 for 10161 Fo > 4sig(Fo) and 0.205901 for all 11083 data
REM 1111 parameters refined using 350 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.169, deepest hole -0.947, 1-sigma level 0.206
Q1 1 0.0178 0.8259 0.3520 11.00000 0.05 1.17
Q2 1 0.4417 1.1265 -0.2035 11.00000 0.05 0.99
Q3 1 -0.0395 0.7233 0.7049 11.00000 0.05 0.91
Q4 1 0.3723 0.5672 0.7274 11.00000 0.05 0.91
Q5 1 0.8412 0.5583 0.2794 11.00000 0.05 0.91
Q6 1 -0.0134 0.5811 0.3582 11.00000 0.05 0.88
Q7 1 0.3323 0.9069 0.3814 11.00000 0.05 0.87
Q8 1 0.6445 0.6021 0.3435 11.00000 0.05 0.86
Q9 1 0.3429 0.6619 0.9363 11.00000 0.05 0.86
Q10 1 0.8290 0.6113 0.4690 11.00000 0.05 0.83
Q11 1 0.1203 1.0156 0.2352 11.00000 0.05 0.79
Q12 1 0.3350 0.8439 0.3935 11.00000 0.05 0.79
Q13 1 0.3072 1.1159 -0.0751 11.00000 0.05 0.78
Q14 1 0.0022 0.6156 0.4106 11.00000 0.05 0.78
Q15 1 0.6634 0.7065 0.4658 11.00000 0.05 0.77
Q16 1 0.3391 0.7112 0.1317 11.00000 0.05 0.77
Q17 1 0.3987 0.8259 0.3174 11.00000 0.05 0.77
Q18 1 0.3195 0.9416 0.1467 11.00000 0.05 0.76
Q19 1 0.2761 1.1153 -0.0527 11.00000 0.05 0.76
Q20 1 0.3203 0.8368 0.4272 11.00000 0.05 0.75
;
_shelx_res_checksum 68212
_shelx_hkl_file
;
0 -3 0 181.94 9.55
0 -3 0 187.00 9.54
0 -4 0 393.50 19.63
0 -4 0 366.36 19.64
0 -5 0 154.47 8.20
0 -5 0 160.79 8.18
0 -6 0 10.65 0.67
0 -6 0 10.40 0.71
0 -7 0 17.90 1.12
0 -7 0 17.54 1.05
0 -8 0 4.51 0.58
0 -8 0 4.29 0.52
0 -9 0 0.59 0.32
0 10 0 20.23 1.15
0 -10 0 23.57 1.43
0 11 0 13.17 0.72
0 -11 0 12.89 1.07
0 12 0 6.19 0.40
0 -12 0 5.28 0.89
0 13 0 7.44 0.45
0 -13 0 5.75 0.93
0 14 0 5.23 0.38
0 15 0 0.73 0.16
0 16 0 1.55 0.17
0 17 0 1.49 0.19
-1 16 0 1.44 0.16
-1 15 0 -0.15 0.15
-1 14 0 2.48 0.28
1 -13 0 9.89 1.24
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15 5 9 5.9989 -0.0301
15 5 10 -7.1109 -0.0026
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15 5 12 5.6442 -0.0485
15 5 13 3.0994 -0.0263
15 5 14 0.6825 0.0247
15 5 15 -2.7022 0.0909
15 5 16 1.3707 0.0001
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15 6 9 -4.1873 0.0437
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15 6 11 3.5150 0.0595
15 6 12 -3.6847 0.0111
15 6 13 2.8509 -0.0961
15 6 14 1.9867 0.0327
15 6 15 5.6375 -0.0649
15 6 16 1.2549 0.1048
15 7 0 3.0198 0.1990
15 7 1 -1.6838 0.1309
15 7 2 1.2323 0.0083
15 7 3 3.8165 -0.0529
15 7 4 -1.2867 -0.1194
15 7 5 -7.7708 -0.0756
15 7 6 3.1460 0.0087
15 7 7 0.6149 -0.0093
15 7 8 4.0727 -0.0757
15 7 9 2.5317 0.0785
15 7 10 4.0299 0.0924
15 7 11 -7.3589 0.0007
15 7 12 2.3645 -0.0402
15 7 13 3.1012 0.0908
15 7 14 -2.6025 0.0449
15 7 15 -5.9866 -0.0815
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15 8 0 2.0969 0.0666
15 8 1 0.1146 0.0461
15 8 2 -6.2353 0.2265
15 8 3 -0.5301 0.0154
15 8 4 3.4147 0.0167
15 8 5 4.5343 -0.0236
15 8 6 -1.4123 0.0066
15 8 7 -2.6567 -0.1479
15 8 8 3.9645 0.0555
15 8 9 -0.0503 -0.0293
15 8 10 1.9315 0.0085
15 8 11 -2.6175 -0.0002
15 8 12 -3.1156 -0.0140
15 8 13 -3.9358 -0.0217
15 8 14 2.4196 0.0054
15 8 15 1.8852 0.0969
15 8 16 0.6717 -0.0064
15 9 0 3.6277 -0.0939
15 9 1 1.9285 -0.0519
15 9 2 -1.2550 0.1211
15 9 3 -1.0503 -0.0738
15 9 4 5.9741 0.0154
15 9 5 -3.3447 0.1076
15 9 6 -2.3024 0.0264
15 9 7 0.5798 -0.0917
15 9 8 -0.1036 0.0438
15 9 9 -0.0212 -0.1029
15 9 10 3.4937 0.0605
15 9 11 4.3583 -0.0122
15 9 12 -0.3969 0.0772
15 9 13 -1.5906 -0.0520
15 9 14 3.3771 -0.0449
15 9 15 -1.5177 -0.0248
15 9 16 -1.9562 -0.0503
15 10 1 2.3856 -0.0010
15 10 2 0.0801 -0.0218
15 10 3 -1.0306 0.0253
15 10 4 -2.3166 0.0631
15 10 5 6.8169 0.0973
15 10 6 -3.4863 -0.0348
15 10 7 0.6039 -0.0560
15 10 8 0.3393 -0.0329
15 10 9 -1.5564 0.0060
15 10 10 -4.7792 0.1283
15 10 11 2.5932 0.0146
15 10 12 -3.4091 -0.0931
15 10 13 -1.3397 -0.0099
15 10 14 -1.6117 0.0046
15 10 15 0.0206 0.0128
15 10 16 -1.3256 -0.0276
15 11 0 -0.1604 -0.0106
15 11 1 -2.9230 0.0944
15 11 2 -0.6913 0.0477
15 11 3 -0.1298 -0.0147
15 11 4 0.2510 -0.0307
15 11 5 6.1803 0.1143
15 11 6 0.1275 -0.0994
15 11 7 -0.5306 -0.0369
15 11 8 1.0199 -0.0395
15 11 9 6.1451 0.0253
15 11 10 -2.6016 -0.0078
15 11 11 0.4759 0.0706
15 11 12 3.7200 0.0738
15 11 13 0.2014 0.0519
15 11 14 -0.0267 -0.1203
15 11 15 5.8442 0.0418
15 12 0 -1.2824 -0.0530
15 12 1 2.8690 0.0055
15 12 2 0.4091 -0.0508
15 12 3 -2.7517 -0.0284
15 12 4 -6.0027 -0.0616
15 12 5 -2.2141 0.0132
15 12 6 1.4242 -0.0908
15 12 7 -6.7336 -0.0331
15 12 8 -3.9320 -0.0414
15 12 9 2.9769 0.0402
15 12 10 1.3173 0.0018
15 12 11 -2.2403 0.0740
15 12 12 1.4939 -0.0535
15 12 13 2.3667 -0.0211
15 12 14 -1.0611 0.0835
15 13 2 3.7812 0.0974
15 13 3 -1.1989 -0.0529
15 13 4 4.8760 -0.0548
15 13 5 -1.7561 0.0567
15 13 6 5.2832 -0.0373
15 13 7 6.5963 -0.1068
15 13 8 -2.3017 0.0696
15 13 9 -0.8558 -0.0155
15 13 10 3.6824 -0.0039
15 13 11 -1.7888 0.0105
15 13 12 -2.5576 0.0769
15 13 14 -1.2147 -0.0931
15 14 3 -4.7376 -0.1037
15 14 4 -0.3273 -0.0718
15 14 5 1.7992 -0.0576
15 14 6 -4.7038 0.1168
15 14 7 -2.7341 -0.1263
15 14 8 -0.1180 0.0014
15 14 9 -2.6995 -0.0255
15 14 10 -1.8318 0.0329
15 14 11 0.2204 -0.0523
15 14 12 1.1157 -0.0049
15 14 13 -0.8342 0.0793
15 15 7 1.3699 -0.0613
15 15 8 -0.2695 0.0249
15 15 9 1.0733 0.0472
15 15 10 2.1949 0.0880
15 15 11 -0.5560 0.0052
16 -3 0 -2.0841 0.0568
16 -3 1 -1.7099 0.1279
16 -3 2 -0.6628 0.1521
16 -3 3 1.3224 -0.0020
16 -3 4 0.4285 -0.0073
16 -3 5 -5.5801 -0.1640
16 -3 6 -2.7006 -0.0211
16 -3 7 -3.0045 0.0351
16 -2 0 1.7333 -0.0641
16 -2 1 -3.7076 -0.0315
16 -2 2 -2.9143 0.1596
16 -2 3 5.8858 -0.0808
16 -2 4 -1.8665 -0.0721
16 -2 5 2.1429 -0.0786
16 -2 6 2.7598 -0.0039
16 -2 7 0.3962 -0.1343
16 -2 8 -0.3375 -0.0679
16 -1 0 -0.1616 0.0371
16 -1 1 7.7614 0.0674
16 -1 2 -1.3703 0.0990
16 -1 3 -0.4869 0.1042
16 -1 4 -1.0571 -0.0113
16 -1 5 -2.0536 0.2825
16 -1 6 -0.4067 -0.0912
16 -1 7 -0.8916 0.0438
16 -1 8 0.4753 -0.0022
16 -1 10 -0.1097 -0.0172
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16 0 2 -2.3867 -0.0697
16 0 3 2.0657 0.0588
16 0 4 3.2199 0.0053
16 0 5 -3.0949 -0.1285
16 0 6 -3.5222 0.0720
16 0 7 1.0797 -0.0707
16 0 8 -4.4838 -0.0028
16 0 9 0.1667 0.0043
16 0 10 1.8327 0.1226
16 0 11 3.6036 0.0484
16 1 0 -2.5138 -0.0207
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16 1 2 2.6924 0.0514
16 1 3 -5.1543 0.0050
16 1 4 -0.3671 0.0217
16 1 5 0.2088 0.0713
16 1 6 3.3441 -0.0164
16 1 7 5.0956 -0.0940
16 1 8 2.1279 0.0274
16 1 9 -4.1983 0.0845
16 1 10 -1.6501 -0.0928
16 1 11 -1.1456 0.0650
16 1 12 2.0897 -0.0004
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16 2 2 -1.3720 -0.0555
16 2 3 -3.2904 -0.0539
16 2 4 4.2418 0.0429
16 2 5 -4.5955 0.0770
16 2 6 -4.7791 -0.0051
16 2 7 1.4692 0.0380
16 2 8 2.6190 0.0781
16 2 9 0.0258 -0.0124
16 2 10 0.3739 0.0466
16 2 11 -1.5067 -0.0472
16 2 12 -0.9739 -0.0007
16 2 13 -3.6089 0.0120
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16 3 1 0.1272 -0.0416
16 3 2 8.4230 -0.0372
16 3 3 3.8920 0.0335
16 3 4 -0.0330 -0.2368
16 3 5 4.8160 -0.0221
16 3 6 2.4996 0.0697
16 3 7 4.6875 0.0231
16 3 8 10.2965 -0.0905
16 3 9 -0.0329 -0.0341
16 3 10 -5.1982 0.1276
16 3 11 -0.4791 0.0173
16 3 12 -1.7670 -0.0054
16 3 13 2.4945 0.0148
16 3 14 -2.8087 0.1124
16 4 0 1.4833 0.1909
16 4 1 -2.6835 0.0414
16 4 2 1.0667 0.0318
16 4 3 1.7574 -0.0197
16 4 4 -1.3888 -0.0049
16 4 5 4.0708 -0.0303
16 4 6 -0.1717 0.0957
16 4 7 -5.1667 -0.0301
16 4 8 1.1969 0.0258
16 4 9 7.9788 -0.0266
16 4 10 1.1183 -0.0387
16 4 11 0.6030 0.0994
16 4 12 2.9797 0.1429
16 4 13 3.1745 -0.1146
16 4 14 -2.3569 -0.0554
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16 5 1 -0.3873 -0.0452
16 5 2 -4.3655 -0.0180
16 5 3 6.6941 -0.0116
16 5 4 -1.4698 -0.0390
16 5 5 -5.8217 0.0581
16 5 6 -1.9305 0.0438
16 5 7 -0.2804 -0.0307
16 5 8 0.3083 -0.0186
16 5 9 -5.2329 0.1319
16 5 10 -4.1649 -0.1065
16 5 11 -4.4802 0.0548
16 5 12 -3.2312 0.0166
16 5 13 -2.3913 -0.0314
16 5 14 5.2507 -0.0218
16 6 0 0.8275 0.0174
16 6 6 -2.5262 0.0500
16 6 7 5.4649 0.0820
16 6 8 -4.0972 0.0019
16 6 9 3.7323 -0.0300
16 6 11 -3.5005 0.0025
16 6 12 1.1678 0.0000
16 6 13 3.2380 -0.0015
16 6 14 5.3347 0.0520
16 6 15 -2.6458 -0.0211
16 7 2 -3.0897 0.0813
16 7 3 -7.3594 0.0684
16 7 4 0.5201 0.0094
16 7 8 1.2411 -0.0009
16 7 9 0.5743 0.0579
16 7 10 -1.2599 -0.0497
16 7 11 2.6597 0.1019
16 7 12 -4.4605 0.0296
16 7 13 -3.2040 -0.0303
16 7 14 0.0809 -0.0893
16 7 15 1.4605 0.0697
16 8 1 -1.4804 -0.0027
16 8 2 -2.4657 0.0987
16 8 3 -3.1226 -0.0354
16 8 4 1.0060 -0.0751
16 8 5 1.0748 -0.0241
16 8 6 2.3242 -0.0254
16 8 8 1.5955 -0.0438
16 8 9 -0.6346 -0.0412
16 8 10 -2.4813 -0.0118
16 8 11 1.7212 -0.0470
16 8 12 -1.8026 0.0953
16 8 13 1.2296 0.0127
16 8 14 0.3160 0.0170
16 8 15 2.5391 -0.1189
16 9 0 -1.5630 -0.0763
16 9 1 -2.0378 0.0374
16 9 2 -0.2322 0.1272
16 9 3 -0.6242 -0.0418
16 9 4 -2.8799 -0.0500
16 9 5 0.9266 0.0206
16 9 6 0.1815 0.0010
16 9 7 -6.8402 -0.0387
16 9 8 1.8574 -0.0733
16 9 9 0.3968 -0.0518
16 9 10 5.3733 0.0866
16 9 11 2.6053 0.0897
16 9 12 2.1948 0.0082
16 9 13 1.0323 0.0584
16 9 14 -1.5043 -0.0290
16 9 15 -0.0588 0.1004
16 10 0 5.1551 -0.1163
16 10 1 4.3511 -0.1317
16 10 2 -1.9466 0.1180
16 10 3 -3.6480 0.1542
16 10 4 -0.5669 0.0271
16 10 5 2.3734 0.0902
16 10 6 0.2511 0.0788
16 10 7 2.8935 -0.0033
16 10 8 0.5704 -0.0026
16 10 9 1.2834 -0.0191
16 10 10 0.8921 -0.0006
16 10 11 -3.5385 -0.0468
16 10 12 5.4430 0.0237
16 10 13 0.7726 0.0863
16 10 14 -3.7207 -0.1622
16 10 15 -0.1317 0.0135
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16 11 2 4.5405 -0.1076
16 11 3 3.0737 0.0438
16 11 4 -1.3188 0.0469
16 11 5 1.3786 -0.0112
16 11 6 5.2643 0.0667
16 11 7 0.3982 0.0301
16 11 8 -3.1565 0.0231
16 11 9 -0.0140 -0.0534
16 11 10 2.7224 0.0060
16 11 11 0.6024 0.0815
16 11 12 -0.4379 -0.0113
16 11 13 0.3591 -0.0363
16 11 14 1.7296 0.0668
16 12 2 -1.9758 0.0914
16 12 3 2.9330 -0.0171
16 12 4 0.6855 0.0249
16 12 5 -2.2681 0.0497
16 12 6 -3.3901 -0.0231
16 12 7 3.3757 -0.0344
16 12 8 -4.2925 0.0437
16 12 9 -2.5921 -0.0057
16 12 10 -1.2447 -0.0266
16 12 11 -0.9565 -0.0081
16 12 12 -2.6443 0.1549
16 12 13 2.4574 0.0011
16 13 4 0.5982 -0.0197
16 13 5 3.5723 0.0051
16 13 6 1.1376 0.0267
16 13 7 3.0390 -0.0418
16 13 8 2.0486 -0.0574
16 13 9 0.7722 0.0299
16 13 10 0.3551 0.0335
16 13 11 2.5569 -0.0130
16 13 12 -1.2267 0.0370
16 14 8 -0.8629 -0.0607
16 14 9 -2.3959 -0.0910
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17 -1 3 0.9212 0.1507
17 -1 4 1.0781 0.0634
17 -1 5 -2.4423 -0.0825
17 -1 6 -1.0447 -0.0196
17 -1 7 -3.8968 0.0420
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17 0 3 -2.1245 0.0584
17 0 4 2.1679 0.0126
17 0 5 1.1608 0.0262
17 0 6 -3.8023 -0.0004
17 0 7 4.6188 -0.1475
17 0 8 -0.5878 -0.0527
17 1 0 -2.0704 0.0381
17 1 1 -2.8048 -0.0057
17 1 2 -2.2932 -0.0883
17 1 3 -1.0966 0.0639
17 1 4 -2.3759 0.1203
17 1 5 0.1265 0.0973
17 1 6 -1.1338 -0.0029
17 1 7 0.4904 0.1016
17 1 8 -1.9152 0.0072
17 1 9 1.6647 -0.0322
17 1 10 -0.4199 0.0033
17 2 0 2.3141 -0.0064
17 2 1 0.0777 -0.0072
17 2 2 5.4540 -0.0902
17 2 3 2.0699 0.0128
17 2 4 -9.4001 0.0765
17 2 5 -0.6360 -0.1451
17 2 6 -2.2611 0.1054
17 2 7 -4.9281 0.0070
17 2 8 3.6048 0.0709
17 2 9 0.1169 -0.0802
17 2 10 -2.6278 -0.0107
17 2 11 -0.1673 0.0774
17 3 0 -2.8308 0.0721
17 3 1 -3.1514 0.0840
17 3 2 -4.0627 0.0264
17 3 3 5.7319 0.0608
17 3 4 1.0804 0.0090
17 3 5 -4.4977 0.0888
17 3 6 1.8644 -0.0437
17 3 7 -5.0352 0.0149
17 3 8 0.7750 -0.0108
17 3 9 3.3855 0.0792
17 3 10 4.8886 -0.1458
17 3 11 -0.8145 0.0225
17 3 12 1.7311 0.0695
17 4 0 2.1589 0.1336
17 4 1 5.5087 -0.0035
17 4 2 2.8788 -0.0796
17 4 3 1.3804 0.0832
17 4 4 0.7709 0.0196
17 4 5 -1.5204 0.0084
17 4 6 1.1402 0.0189
17 4 7 2.4480 0.0478
17 4 8 2.9905 -0.0070
17 4 9 -0.0537 -0.0163
17 4 10 0.7926 0.1031
17 4 11 2.7754 -0.0448
17 4 12 -3.5161 0.0562
17 5 0 -4.2646 -0.0130
17 5 1 -1.0815 -0.0162
17 5 2 -0.1301 -0.0677
17 5 3 2.0528 0.0087
17 5 4 7.8113 -0.0269
17 5 5 2.9608 -0.0726
17 5 6 -1.4711 -0.0335
17 5 7 2.7663 0.0091
17 5 8 -1.7029 0.0606
17 5 9 4.4595 -0.0857
17 5 10 2.1044 0.0058
17 5 11 -4.5265 -0.0165
17 5 12 -4.8288 0.0016
17 5 13 -2.7482 -0.0223
17 6 0 -2.2847 0.0680
17 6 1 -1.4154 0.1081
17 6 2 4.3729 -0.0014
17 6 3 -0.0823 -0.0478
17 6 4 2.1625 0.0169
17 6 5 2.5715 0.0071
17 6 6 -1.0391 0.0247
17 6 7 0.9835 -0.0161
17 6 8 3.1721 0.0515
17 6 9 -2.1926 0.0687
17 6 10 -3.5863 -0.0780
17 6 11 2.4772 -0.0939
17 6 12 -0.2745 0.1015
17 6 13 -2.3700 0.0107
17 7 0 1.1853 0.0102
17 7 1 -1.4618 0.0872
17 7 2 -0.8473 -0.0093
17 7 3 0.1308 0.0973
17 7 4 -1.4075 -0.0167
17 7 5 1.0547 -0.0697
17 7 6 -0.0640 0.0181
17 7 7 -5.2885 0.0359
17 7 8 -0.5075 0.0037
17 7 9 5.2531 0.0706
17 7 10 2.9046 -0.0191
17 7 11 -2.3111 0.0501
17 7 12 -1.7930 -0.0608
17 7 13 -1.1348 0.0739
17 8 1 -0.3173 0.0437
17 8 7 -5.4169 0.0010
17 8 8 -3.8139 -0.0337
17 8 9 1.0454 -0.0852
17 8 10 -4.5060 -0.0639
17 8 11 0.9608 0.0815
17 8 12 -2.8740 0.0048
17 8 13 -1.7466 -0.0165
17 9 8 -3.2001 -0.1168
17 9 9 -0.0283 -0.0412
17 9 10 1.5715 -0.0116
17 9 11 0.2520 -0.0173
17 9 12 -1.3971 -0.0009
17 9 13 2.8597 0.0938
17 10 3 -0.5203 0.0968
17 10 4 -4.2143 0.0156
17 10 5 1.0682 -0.0275
17 10 9 -2.0818 -0.1159
17 10 10 0.1464 -0.0116
17 10 11 -0.8407 0.0260
17 10 12 0.9220 -0.1069
17 10 13 2.0827 -0.0289
17 11 3 -0.8841 -0.0139
17 11 4 3.0747 0.0701
17 11 5 0.5339 -0.0096
17 11 6 -0.0134 0.0142
17 11 9 -0.7009 -0.0437
17 11 10 2.3734 -0.0722
17 11 11 -0.1267 -0.0561
17 11 12 0.2695 0.1177
17 12 5 -3.6903 0.0560
17 12 6 2.6105 0.0534
17 12 9 0.0045 0.0778
17 12 10 -0.2334 -0.0424
17 12 11 0.0132 -0.0550
18 2 3 -0.6389 -0.0347
18 2 4 4.0032 -0.0530
18 2 5 -2.1306 0.0862
18 2 8 -2.7760 0.0420
18 3 3 1.9918 -0.0104
18 3 4 -0.2577 0.0255
18 3 5 0.5011 0.0031
18 3 6 -1.8252 0.0230
18 3 7 -0.7216 0.0227
18 3 8 2.2173 -0.0119
18 4 2 -2.8721 -0.0119
18 4 3 -6.4687 -0.0269
18 4 4 -0.1482 0.0810
18 4 5 -0.4471 -0.0542
18 4 6 -4.3457 0.0234
18 4 7 -6.8079 -0.0538
18 4 8 -4.8372 0.0806
18 4 9 -0.8159 -0.0217
18 5 2 0.2115 0.0621
18 5 3 6.7131 -0.0239
18 5 4 3.9112 -0.0303
18 5 5 -0.1608 0.0634
18 5 6 -2.1435 -0.0438
18 5 7 -0.3665 0.0535
18 5 8 4.5605 -0.0515
18 5 9 -1.1573 0.0706
18 5 10 -3.0465 -0.0210
18 6 2 -1.8729 -0.0328
18 6 3 -2.6439 0.0808
18 6 4 -0.7814 -0.0014
18 6 5 1.2142 -0.0649
18 6 6 -1.1739 -0.0024
18 6 7 -3.1391 0.0365
18 6 8 -4.1417 0.1078
18 6 9 2.3450 -0.0506
18 6 10 4.7973 0.0841
18 6 11 -0.1094 -0.0194
18 7 3 3.4546 -0.0292
18 7 4 0.4665 -0.0098
18 7 5 4.6761 -0.0572
18 7 6 6.3833 -0.0109
18 7 7 -1.8384 -0.1208
18 7 8 -1.8615 0.0178
18 7 10 -1.2048 -0.1210
18 7 11 -1.0877 0.1308
18 8 4 3.6873 -0.0235
18 8 5 -3.4237 0.0544
18 8 6 2.0034 -0.0421
18 8 7 4.7942 -0.0059
18 8 8 -0.1406 -0.0409
18 8 10 3.5659 -0.0241
18 8 11 2.3146 -0.0629
18 9 5 -0.1724 0.0097
18 9 6 0.7336 -0.0809
18 9 7 0.7024 -0.0087
18 9 8 -2.2107 0.0715
18 9 10 -1.7869 -0.0316
18 9 11 -0.0285 0.0791
18 10 6 -4.2240 -0.0300
18 10 7 -0.5705 -0.0729
0 0 0 0.0 0.0
;
_shelx_fab_checksum 44082
_olex2_submission_special_instructions 'No special instructions were received'
loop_
# start Validation Reply Form
_vrf_PLAT029_yb016bisf
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.895 Why?
RESPONSE: We collected the data on this crystal several times and the
intensity at the high angle (< 0.95 Ang) are very week as the results
of the disorder in the lattice (disorder of both the TTF and
solvent). Although we collected the data up to 0.8 Ang, using a chiral
P1 space group, however we utilised only the data up to 0.90 Ang to
achieve a 90% completeness. We are confident in the overall structure.
;
_vrf_PLAT084_yb016bisf
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.47 Report
RESPONSE: Due to the disorder of the TTF molecules and the cyclohexane rings
of the NDI macrocycle, several atoms are restrained to be refined isotropically
which causes high R values.
;
_vrf_PLAT082_yb016bisf
;
PROBLEM: High R1 Value .................................. 0.20 Report
RESPONSE: Due to the disorder of the TTF molecules and the cyclohexane rings
of the NDI macrocycle, several atoms are restrained to be refined isotropically
which causes high R values.
;
_vrf_PLAT213_yb016bisf
;
PROBLEM: Atom C3 has ADP max/min Ratio ..... 4.2 prolat
RESPONSE: Due to the lattice disorder
;
_vrf_PLAT215_yb016bisf
;
PROBLEM: Disordered C56 has ADP max/min Ratio ..... 4.9 Note
RESPONSE: Due to the lattice disorder
;
_vrf_PLAT241_yb016bisf
;
PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of C53 Check
RESPONSE: Due to the lattice disorder
;
_vrf_PLAT340_yb016bisf
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02077 Ang.
RESPONSE: Low resolution of the collected data
;
_vrf_PLAT911_yb016bisf
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.588 1303 Report
RESPONSE: Some reflections were omitted due to non-ideal solvent
masking, the diffraction pattern displayed the presence of diffuse scattering.
;
# end Validation Reply Form