# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024
#######################################################################
#
# 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.
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data_zn9_sq
_audit_block_doi 10.5517/ccdc.csd.cc2j05tk
_database_code_depnum_ccdc_archive 'CCDC 2323878'
loop_
_audit_author_name
_audit_author_address
'Tao Ye'
;Guangxi Normal University
China
;
_audit_update_record
;
2024-11-25 deposited with the CCDC. 2024-12-06 downloaded from the CCDC.
;
_audit_creation_date 2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C60 H48 N24 O24 Zn9, 5.5[H2O]'
_chemical_formula_sum 'C60 H59 N24 O29.50 Zn9'
_chemical_formula_weight 2176.64
_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'
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'
Zn Zn 0.2839 1.4301 '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 167
_space_group_name_H-M_alt 'R -3 c'
_space_group_name_Hall '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
_cell_length_a 15.31573(19)
_cell_length_b 15.31573(19)
_cell_length_c 56.9773(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 11574.6(3)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 15234
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 28.6130
_cell_measurement_theta_min 3.4370
_shelx_estimated_absorpt_T_max 0.514
_shelx_estimated_absorpt_T_min 0.463
_exptl_absorpt_coefficient_mu 2.846
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.32515
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.874
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 6558
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.27
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0339
_diffrn_reflns_av_unetI/netI 0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 76
_diffrn_reflns_limit_l_min -76
_diffrn_reflns_number 47231
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.957
_diffrn_reflns_theta_min 3.389
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -20.00 26.00 0.50 7.50 -- 17.77 93.00 -86.00 92
2 \w -93.00 25.00 0.50 7.50 -- -19.57 -19.00 150.00 236
3 \w -88.00 2.00 0.50 7.50 -- -19.57 -57.00 0.00 180
4 \w -88.00 2.00 0.50 7.50 -- -19.57 -57.00 90.00 180
5 \w -41.00 49.00 0.50 7.50 -- -19.57 57.00 -30.00 180
6 \w -50.00 51.00 0.50 7.50 -- -19.57 77.00-150.00 202
7 \w -51.00 38.00 0.50 7.50 -- 17.77 -57.00 90.00 178
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0359290000
_diffrn_orient_matrix_UB_12 0.0386384000
_diffrn_orient_matrix_UB_13 0.0073489000
_diffrn_orient_matrix_UB_21 -0.0228213000
_diffrn_orient_matrix_UB_22 0.0296263000
_diffrn_orient_matrix_UB_23 -0.0022884000
_diffrn_orient_matrix_UB_31 -0.0323406000
_diffrn_orient_matrix_UB_32 -0.0221284000
_diffrn_orient_matrix_UB_33 0.0097815000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2822
_reflns_number_total 3247
_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 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max 1.255
_refine_diff_density_min -0.972
_refine_diff_density_rms 0.079
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 180
_refine_ls_number_reflns 3247
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0420
_refine_ls_R_factor_gt 0.0355
_refine_ls_restrained_S_all 1.039
_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^)+(0.0509P)^2^+51.9232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0976
_refine_ls_wR_factor_ref 0.1030
_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 O(H) groups
2. Restrained distances
O4-H4
0.85 with sigma of 0.01
C10-H4
1.928692 with sigma of 0.02
Zn1-H4
2.943996 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C9(H9A,H9B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4A), C5(H5)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
Zn1 Zn 0.87349(3) 0.27141(3) 0.03102(2) 0.03999(12) Uani 1 1 d D . . . .
Zn2 Zn 0.90970(3) 0.333333 0.083333 0.03198(13) Uani 1 2 d S T P . .
O1 O 0.96180(15) 0.30556(18) 0.00128(4) 0.0445(5) Uani 1 1 d . . . . .
O2 O 0.95207(19) 0.2796(3) -0.03712(4) 0.0666(8) Uani 1 1 d . . . . .
O3 O 0.96126(14) 0.29376(15) 0.05750(3) 0.0335(4) Uani 1 1 d . . . . .
O4 O 0.8538(2) 0.11884(19) 0.03502(5) 0.0600(6) Uani 1 1 d D . . . .
H4 H 0.803(2) 0.0588(9) 0.0330(6) 0.090 Uiso 1 1 d D U . . .
N1 N 0.76546(16) 0.21860(17) 0.00571(4) 0.0304(4) Uani 1 1 d . . . . .
N2 N 0.70657(16) 0.19394(17) 0.05188(4) 0.0306(4) Uani 1 1 d . . . . .
N3 N 0.54323(16) 0.12470(16) 0.04195(3) 0.0290(4) Uani 1 1 d . . . . .
N4 N 0.54997(16) 0.12621(16) 0.06595(3) 0.0290(4) Uani 1 1 d . . . . .
C1 C 0.9142(2) 0.2735(2) -0.01766(5) 0.0398(6) Uani 1 1 d . . . . .
C2 C 0.8000(2) 0.2243(2) -0.01609(4) 0.0345(5) Uani 1 1 d . . . . .
C3 C 0.7360(2) 0.1863(2) -0.03508(5) 0.0410(6) Uani 1 1 d . . . . .
H3 H 0.761338 0.192257 -0.050194 0.049 Uiso 1 1 calc R U . . .
C4 C 0.6338(2) 0.1393(3) -0.03112(5) 0.0437(7) Uani 1 1 d . . . . .
H4A H 0.589115 0.113563 -0.043677 0.052 Uiso 1 1 calc R U . . .
C5 C 0.5973(2) 0.1303(2) -0.00859(5) 0.0371(6) Uani 1 1 d . . . . .
H5 H 0.528365 0.097260 -0.005677 0.044 Uiso 1 1 calc R U . . .
C6 C 0.66651(19) 0.1721(2) 0.00968(4) 0.0307(5) Uani 1 1 d . . . . .
C7 C 0.63735(19) 0.16421(19) 0.03452(4) 0.0288(5) Uani 1 1 d . . . . .
C8 C 0.64804(19) 0.16815(19) 0.07119(4) 0.0286(5) Uani 1 1 d . . . . .
C9 C 0.9889(3) 0.2189(3) 0.06015(7) 0.0549(9) Uani 1 1 d . . . . .
H9A H 1.018286 0.224725 0.075554 0.066 Uiso 1 1 calc R U . . .
H9B H 1.039009 0.228717 0.048461 0.066 Uiso 1 1 calc R U . . .
C10 C 0.8991(3) 0.1172(3) 0.05739(7) 0.0670(11) Uani 1 1 d D . . . .
H10A H 0.918596 0.065966 0.057301 0.080 Uiso 1 1 calc R U . . .
H10B H 0.851859 0.103102 0.070149 0.080 Uiso 1 1 calc R 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
Zn1 0.03596(19) 0.0569(2) 0.02808(18) -0.00888(14) -0.00614(12) 0.02397(16)
Zn2 0.03262(17) 0.0432(3) 0.0236(2) 0.00232(16) 0.00116(8) 0.02160(13)
O1 0.0329(10) 0.0614(13) 0.0336(10) -0.0109(9) 0.0008(8) 0.0193(10)
O2 0.0447(13) 0.111(2) 0.0354(12) -0.0128(13) 0.0087(10) 0.0327(15)
O3 0.0326(9) 0.0431(10) 0.0305(9) -0.0049(8) -0.0033(7) 0.0232(8)
O4 0.0559(15) 0.0458(13) 0.0696(16) -0.0107(12) -0.0189(12) 0.0189(12)
N1 0.0297(10) 0.0359(11) 0.0242(9) -0.0042(8) 0.0000(8) 0.0154(9)
N2 0.0259(10) 0.0377(11) 0.0249(10) -0.0033(8) -0.0023(8) 0.0135(9)
N3 0.0279(10) 0.0349(11) 0.0199(9) -0.0014(8) -0.0017(7) 0.0123(8)
N4 0.0274(10) 0.0353(11) 0.0207(9) -0.0007(8) -0.0026(7) 0.0130(9)
C1 0.0363(14) 0.0513(16) 0.0308(13) -0.0064(12) 0.0048(11) 0.0212(13)
C2 0.0369(13) 0.0417(14) 0.0247(11) -0.0056(10) 0.0009(10) 0.0197(12)
C3 0.0445(15) 0.0560(18) 0.0226(12) -0.0074(11) -0.0003(11) 0.0253(14)
C4 0.0428(15) 0.0593(19) 0.0279(13) -0.0096(12) -0.0084(11) 0.0247(14)
C5 0.0316(13) 0.0481(16) 0.0302(13) -0.0062(11) -0.0048(10) 0.0190(12)
C6 0.0310(12) 0.0359(13) 0.0261(11) -0.0039(9) -0.0008(9) 0.0174(11)
C7 0.0295(12) 0.0328(12) 0.0233(11) -0.0021(9) -0.0020(9) 0.0150(10)
C8 0.0287(11) 0.0321(12) 0.0231(11) -0.0022(9) -0.0028(9) 0.0138(10)
C9 0.059(2) 0.059(2) 0.064(2) -0.0149(17) -0.0203(17) 0.0414(18)
C10 0.076(3) 0.051(2) 0.076(3) -0.0009(19) -0.018(2) 0.034(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 Zn2 3.0928(3) . ?
Zn1 O1 2.066(2) . ?
Zn1 O3 1.9341(18) . ?
Zn1 O4 2.213(3) . ?
Zn1 N1 2.033(2) . ?
Zn1 N2 2.515(2) . ?
Zn1 N3 2.325(2) 2_655 ?
Zn2 O3 1.9068(18) . ?
Zn2 O3 1.9066(18) 16_554 ?
Zn2 N4 1.991(2) 17_654 ?
Zn2 N4 1.991(2) 2_655 ?
O1 C1 1.257(4) . ?
O2 C1 1.233(3) . ?
O3 C9 1.414(4) . ?
O4 H4 0.865(9) . ?
O4 C10 1.458(4) . ?
N1 C2 1.335(3) . ?
N1 C6 1.333(3) . ?
N2 C7 1.352(3) . ?
N2 C8 1.348(3) . ?
N3 N4 1.370(3) . ?
N3 C7 1.323(3) . ?
N4 C8 1.339(3) . ?
C1 C2 1.522(4) . ?
C2 C3 1.378(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(4) . ?
C4 H4A 0.9300 . ?
C4 C5 1.379(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(4) . ?
C6 C7 1.471(3) . ?
C8 C8 1.469(5) 17_654 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.484(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 Zn2 135.94(6) . . ?
O1 Zn1 O4 94.49(10) . . ?
O1 Zn1 N2 152.84(8) . . ?
O1 Zn1 N3 106.58(9) . 2_655 ?
O3 Zn1 Zn2 36.07(5) . . ?
O3 Zn1 O1 106.62(8) . . ?
O3 Zn1 O4 79.77(9) . . ?
O3 Zn1 N1 168.29(9) . . ?
O3 Zn1 N2 99.63(7) . . ?
O3 Zn1 N3 87.08(8) . 2_655 ?
O4 Zn1 Zn2 97.67(7) . . ?
O4 Zn1 N2 83.29(9) . . ?
O4 Zn1 N3 157.68(9) . 2_655 ?
N1 Zn1 Zn2 142.29(6) . . ?
N1 Zn1 O1 79.54(8) . . ?
N1 Zn1 O4 89.92(9) . . ?
N1 Zn1 N2 73.41(8) . . ?
N1 Zn1 N3 100.87(8) . 2_655 ?
N2 Zn1 Zn2 70.92(5) . . ?
N3 Zn1 Zn2 62.04(5) 2_655 . ?
N3 Zn1 N2 81.21(7) 2_655 . ?
Zn1 Zn2 Zn1 177.03(2) . 16_554 ?
O3 Zn2 Zn1 36.68(5) 16_554 16_554 ?
O3 Zn2 Zn1 146.29(6) . 16_554 ?
O3 Zn2 Zn1 146.28(6) 16_554 . ?
O3 Zn2 Zn1 36.67(5) . . ?
O3 Zn2 O3 110.06(11) . 16_554 ?
O3 Zn2 N4 125.16(8) . 17_654 ?
O3 Zn2 N4 98.02(8) 16_554 17_654 ?
O3 Zn2 N4 98.01(8) . 2_655 ?
O3 Zn2 N4 125.17(9) 16_554 2_655 ?
N4 Zn2 Zn1 107.66(6) 17_654 . ?
N4 Zn2 Zn1 107.66(6) 2_655 16_554 ?
N4 Zn2 Zn1 70.38(6) 17_654 16_554 ?
N4 Zn2 Zn1 70.38(6) 2_655 . ?
N4 Zn2 N4 102.77(12) 2_655 17_654 ?
C1 O1 Zn1 115.27(18) . . ?
Zn2 O3 Zn1 107.26(9) . . ?
C9 O3 Zn1 113.76(18) . . ?
C9 O3 Zn2 121.0(2) . . ?
Zn1 O4 H4 133.2(19) . . ?
C10 O4 Zn1 107.0(2) . . ?
C10 O4 H4 106.4(16) . . ?
C2 N1 Zn1 114.64(18) . . ?
C6 N1 Zn1 125.03(17) . . ?
C6 N1 C2 120.0(2) . . ?
C7 N2 Zn1 104.72(15) . . ?
C8 N2 Zn1 153.46(17) . . ?
C8 N2 C7 101.8(2) . . ?
N4 N3 Zn1 109.37(15) . 3_665 ?
C7 N3 Zn1 137.67(17) . 3_665 ?
C7 N3 N4 104.83(19) . . ?
N3 N4 Zn2 115.92(15) . 3_665 ?
C8 N4 Zn2 136.35(16) . 3_665 ?
C8 N4 N3 106.72(19) . . ?
O1 C1 C2 116.2(2) . . ?
O2 C1 O1 125.7(3) . . ?
O2 C1 C2 118.1(3) . . ?
N1 C2 C1 114.0(2) . . ?
N1 C2 C3 121.9(3) . . ?
C3 C2 C1 124.1(2) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.4(3) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4A 119.9 . . ?
C3 C4 C5 120.2(3) . . ?
C5 C4 H4A 119.9 . . ?
C4 C5 H5 120.9 . . ?
C4 C5 C6 118.3(3) . . ?
C6 C5 H5 120.9 . . ?
N1 C6 C5 121.3(2) . . ?
N1 C6 C7 115.1(2) . . ?
C5 C6 C7 123.5(2) . . ?
N2 C7 C6 121.5(2) . . ?
N3 C7 N2 114.3(2) . . ?
N3 C7 C6 124.2(2) . . ?
N2 C8 C8 125.1(3) . 17_654 ?
N4 C8 N2 112.4(2) . . ?
N4 C8 C8 122.5(3) . 17_654 ?
O3 C9 H9A 109.6 . . ?
O3 C9 H9B 109.6 . . ?
O3 C9 C10 110.1(3) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
O4 C10 C9 105.9(3) . . ?
O4 C10 H10A 110.6 . . ?
O4 C10 H10B 110.6 . . ?
C9 C10 H10A 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
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
Zn1 O1 C1 O2 -174.8(3) . . . . ?
Zn1 O1 C1 C2 5.9(4) . . . . ?
Zn1 O3 C9 C10 -45.3(4) . . . . ?
Zn1 O4 C10 C9 -36.0(4) . . . . ?
Zn1 N1 C2 C1 -2.5(3) . . . . ?
Zn1 N1 C2 C3 176.1(2) . . . . ?
Zn1 N1 C6 C5 -174.2(2) . . . . ?
Zn1 N1 C6 C7 2.7(3) . . . . ?
Zn1 N2 C7 N3 -177.26(18) . . . . ?
Zn1 N2 C7 C6 5.3(3) . . . . ?
Zn1 N2 C8 N4 176.0(3) . . . . ?
Zn1 N2 C8 C8 -1.4(5) . . . 17_654 ?
Zn1 N3 N4 Zn2 16.8(2) 3_665 . . 3_665 ?
Zn1 N3 N4 C8 -153.65(16) 3_665 . . . ?
Zn1 N3 C7 N2 141.8(2) 3_665 . . . ?
Zn1 N3 C7 C6 -40.9(4) 3_665 . . . ?
Zn2 O3 C9 C10 84.6(3) . . . . ?
Zn2 N4 C8 N2 -167.86(19) 3_665 . . . ?
Zn2 N4 C8 C8 9.7(3) 3_665 . . 17_654 ?
O1 C1 C2 N1 -2.4(4) . . . . ?
O1 C1 C2 C3 179.1(3) . . . . ?
O2 C1 C2 N1 178.3(3) . . . . ?
O2 C1 C2 C3 -0.3(5) . . . . ?
O3 C9 C10 O4 53.3(4) . . . . ?
N1 C2 C3 C4 -1.5(5) . . . . ?
N1 C6 C7 N2 -5.9(4) . . . . ?
N1 C6 C7 N3 176.9(2) . . . . ?
N3 N4 C8 N2 -0.4(3) . . . . ?
N3 N4 C8 C8 177.18(13) . . . 17_654 ?
N4 N3 C7 N2 -1.3(3) . . . . ?
N4 N3 C7 C6 176.0(2) . . . . ?
C1 C2 C3 C4 176.9(3) . . . . ?
C2 N1 C6 C5 -1.1(4) . . . . ?
C2 N1 C6 C7 175.9(2) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C3 C4 C5 C6 1.6(5) . . . . ?
C4 C5 C6 N1 -0.8(4) . . . . ?
C4 C5 C6 C7 -177.5(3) . . . . ?
C5 C6 C7 N2 171.0(3) . . . . ?
C5 C6 C7 N3 -6.1(4) . . . . ?
C6 N1 C2 C1 -176.3(2) . . . . ?
C6 N1 C2 C3 2.3(4) . . . . ?
C7 N2 C8 N4 -0.4(3) . . . . ?
C7 N2 C8 C8 -177.88(14) . . . 17_654 ?
C7 N3 N4 Zn2 171.42(17) . . . 3_665 ?
C7 N3 N4 C8 1.0(3) . . . . ?
C8 N2 C7 N3 1.1(3) . . . . ?
C8 N2 C7 C6 -176.3(2) . . . . ?
_shelx_res_file
;
TITL Zn9 in R-3c #167
zn9_sq.res
created by SHELXL-2018/3 at 01:18:53 on 26-Nov-2024
REM reset to R-3c #167
CELL 0.71073 15.315732 15.315732 56.977261 90 90 120
ZERR 6 0.000188 0.000188 0.000704 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SFAC C H N O Zn
UNIT 360 354 144 177 54
DFIX 0.85 0.01 O4 H4
DANG 1.928692 0.02 C10 H4
DANG 2.943996 0.02 Zn1 H4
L.S. 5 0 10
PLAN 5
SIZE 0.27 0.28 0.32
CONF
BOND
ABIN
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.050900 51.923199
FVAR 0.99946
ZN1 5 0.873491 0.271408 0.031020 11.00000 0.03596 0.05693 =
0.02808 -0.00888 -0.00614 0.02397
ZN2 5 0.909696 0.333333 0.083333 10.50000 0.03262 0.04320 =
0.02365 0.00232 0.00116 0.02160
O1 4 0.961802 0.305555 0.001280 11.00000 0.03288 0.06138 =
0.03356 -0.01093 0.00084 0.01933
O2 4 0.952066 0.279577 -0.037120 11.00000 0.04475 0.11124 =
0.03543 -0.01283 0.00873 0.03274
O3 4 0.961258 0.293757 0.057503 11.00000 0.03257 0.04307 =
0.03054 -0.00487 -0.00328 0.02319
O4 4 0.853750 0.118838 0.035020 11.00000 0.05593 0.04578 =
0.06961 -0.01069 -0.01888 0.01891
H4 2 0.803057 0.058828 0.032980 11.00000 -1.50000
N1 3 0.765458 0.218596 0.005706 11.00000 0.02973 0.03593 =
0.02417 -0.00416 0.00005 0.01536
N2 3 0.706570 0.193939 0.051883 11.00000 0.02593 0.03771 =
0.02493 -0.00332 -0.00227 0.01345
N3 3 0.543234 0.124704 0.041953 11.00000 0.02785 0.03492 =
0.01987 -0.00142 -0.00172 0.01233
N4 3 0.549971 0.126214 0.065945 11.00000 0.02739 0.03527 =
0.02074 -0.00066 -0.00264 0.01304
C1 1 0.914169 0.273540 -0.017664 11.00000 0.03626 0.05135 =
0.03083 -0.00638 0.00485 0.02122
C2 1 0.799980 0.224331 -0.016094 11.00000 0.03692 0.04173 =
0.02469 -0.00557 0.00095 0.01966
C3 1 0.736033 0.186316 -0.035079 11.00000 0.04454 0.05597 =
0.02258 -0.00737 -0.00034 0.02530
AFIX 43
H3 2 0.761338 0.192257 -0.050194 11.00000 -1.20000
AFIX 0
C4 1 0.633753 0.139319 -0.031124 11.00000 0.04280 0.05932 =
0.02787 -0.00960 -0.00836 0.02471
AFIX 43
H4A 2 0.589115 0.113563 -0.043677 11.00000 -1.20000
AFIX 0
C5 1 0.597335 0.130345 -0.008591 11.00000 0.03163 0.04812 =
0.03024 -0.00619 -0.00476 0.01903
AFIX 43
H5 2 0.528365 0.097260 -0.005677 11.00000 -1.20000
AFIX 0
C6 1 0.666506 0.172102 0.009676 11.00000 0.03097 0.03588 =
0.02608 -0.00388 -0.00080 0.01740
C7 1 0.637349 0.164213 0.034519 11.00000 0.02948 0.03281 =
0.02329 -0.00210 -0.00196 0.01501
C8 1 0.648039 0.168150 0.071191 11.00000 0.02872 0.03213 =
0.02306 -0.00220 -0.00284 0.01377
C9 1 0.988874 0.218946 0.060153 11.00000 0.05859 0.05874 =
0.06362 -0.01487 -0.02026 0.04144
AFIX 23
H9A 2 1.018286 0.224725 0.075554 11.00000 -1.20000
H9B 2 1.039009 0.228717 0.048461 11.00000 -1.20000
AFIX 0
C10 1 0.899050 0.117221 0.057395 11.00000 0.07584 0.05120 =
0.07621 -0.00094 -0.01838 0.03354
AFIX 23
H10A 2 0.918596 0.065966 0.057301 11.00000 -1.20000
H10B 2 0.851859 0.103102 0.070149 11.00000 -1.20000
AFIX 0
HKLF 4
REM Zn9 in R-3c #167
REM wR2 = 0.1030, GooF = S = 1.036, Restrained GooF = 1.039 for all data
REM R1 = 0.0355 for 2822 Fo > 4sig(Fo) and 0.0420 for all 3247 data
REM 180 parameters refined using 3 restraints
END
WGHT 0.0509 51.9153
REM Highest difference peak 1.255, deepest hole -0.972, 1-sigma level 0.079
Q1 1 0.8699 0.2094 0.0330 11.00000 0.05 1.26
Q2 1 0.8830 0.3219 0.0188 11.00000 0.05 0.68
Q3 1 0.8612 0.1982 0.0405 11.00000 0.05 0.62
Q4 1 0.9032 0.2832 0.0794 11.00000 0.05 0.52
Q5 1 0.8748 0.3081 0.0814 11.00000 0.05 0.48
;
_shelx_res_checksum 80132
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-10 18 20 1.91 0.00
-10 18 23 -0.75 0.00
-10 18 26 -1.03 0.00
-10 18 29 -0.24 0.00
-10 18 32 0.48 0.00
-10 18 35 -1.28 0.00
-10 18 38 -2.16 0.00
-7 18 35 -1.47 0.00
-7 18 32 -0.22 0.00
-7 18 29 -0.48 0.00
-7 18 26 -2.16 0.00
-7 18 23 -2.87 0.00
-7 18 20 0.32 0.00
-7 18 17 -0.47 0.00
-7 18 14 0.09 0.00
-7 18 11 -1.68 0.00
-7 18 8 1.20 0.00
-7 18 5 0.87 0.00
-7 18 2 -1.26 0.00
-11 18 1 -0.36 0.00
-11 18 4 -1.51 0.00
-11 18 7 -2.20 0.00
-11 18 10 -0.34 0.00
-11 18 13 0.36 0.00
-11 18 16 -0.27 0.00
-11 18 19 -1.01 0.00
-11 18 22 0.47 0.00
-11 18 25 0.66 0.00
-11 18 28 -0.83 0.00
-11 18 31 -0.19 0.00
-11 18 34 -0.68 0.00
-11 18 37 -0.22 0.00
-6 18 33 -0.55 0.00
-6 18 30 -1.64 0.00
-6 18 27 -2.10 0.00
-6 18 24 -1.36 0.00
-6 18 21 -1.55 0.00
-6 18 18 -0.37 0.00
-6 18 15 -1.94 0.00
-6 18 12 1.74 0.00
-6 18 9 1.04 0.00
-6 18 6 -1.07 0.00
-6 18 3 0.04 0.00
-6 18 0 -0.30 0.00
-12 18 3 -0.94 0.00
-12 18 6 -2.84 0.00
-12 18 9 -0.93 0.00
-12 18 12 -0.18 0.00
-12 18 15 0.21 0.00
-12 18 18 -0.58 0.00
-12 18 21 0.01 0.00
-12 18 24 -0.19 0.00
-12 18 27 0.22 0.00
-12 18 30 -0.65 0.00
-12 18 33 0.64 0.00
-12 18 36 -0.33 0.00
-5 18 31 -0.43 0.00
-5 18 28 -1.38 0.00
-5 18 25 -1.73 0.00
-5 18 22 -0.67 0.00
-5 18 19 -0.47 0.00
-5 18 16 0.96 0.00
-5 18 13 -0.57 0.00
-5 18 10 0.92 0.00
-5 18 7 -0.06 0.00
-5 18 4 0.73 0.00
-5 18 1 1.04 0.00
-13 18 2 -2.33 0.00
-13 18 5 1.27 0.00
-13 18 8 0.07 0.00
-13 18 11 -0.52 0.00
-13 18 14 -1.97 0.00
-13 18 17 0.46 0.00
-13 18 20 1.52 0.00
-13 18 23 0.21 0.00
-13 18 26 -1.08 0.00
-13 18 29 0.22 0.00
-13 18 32 0.77 0.00
-4 18 32 -0.88 0.00
-4 18 29 -0.14 0.00
-4 18 26 -1.02 0.00
-4 18 23 -0.74 0.00
-4 18 20 0.98 0.00
-4 18 17 0.58 0.00
-4 18 14 1.02 0.00
-4 18 11 -0.27 0.00
-4 18 8 1.47 0.00
-4 18 5 -0.67 0.00
-4 18 2 0.02 0.00
-14 18 1 1.03 0.00
-14 18 4 -0.99 0.00
-14 18 7 0.87 0.00
-14 18 10 0.42 0.00
-14 18 13 0.84 0.00
-14 18 16 -0.68 0.00
-14 18 19 -0.46 0.00
-14 18 22 1.33 0.00
-14 18 25 0.34 0.00
-14 18 28 0.00 0.00
-14 18 31 -0.07 0.00
-3 18 27 1.63 0.00
-3 18 21 -1.23 0.00
-3 18 18 0.36 0.00
-3 18 15 1.29 0.00
-3 18 12 2.44 0.00
-3 18 9 -1.95 0.00
-3 18 6 -0.33 0.00
-3 18 3 -0.13 0.00
-3 18 0 0.76 0.00
-15 18 3 2.98 0.00
-15 18 6 -1.25 0.00
-15 18 9 -0.42 0.00
-15 18 12 1.36 0.00
-15 18 15 1.45 0.00
-15 18 18 -0.05 0.00
-15 18 21 -1.29 0.00
-15 18 24 0.89 0.00
-15 18 27 0.98 0.00
-2 18 19 -0.19 0.00
-2 18 16 1.12 0.00
-2 18 13 -0.55 0.00
-2 18 7 -1.32 0.00
-2 18 4 0.06 0.00
-2 18 1 -1.03 0.00
-16 18 2 -0.32 0.00
-16 18 5 1.16 0.00
-16 18 8 -0.97 0.00
-16 18 11 0.26 0.00
-16 18 14 1.26 0.00
-16 18 17 0.34 0.00
-16 18 20 -0.25 0.00
-16 18 23 -0.27 0.00
-17 18 1 -1.21 0.00
-17 18 4 0.61 0.00
-17 18 7 2.08 0.00
-17 18 10 -1.57 0.00
-17 18 13 -1.60 0.00
-17 18 16 1.16 0.00
-9 19 29 -1.01 0.00
-9 19 26 -0.63 0.00
-9 19 23 -0.53 0.00
-9 19 20 1.23 0.00
-9 19 17 -0.84 0.00
-9 19 14 1.09 0.00
-9 19 11 0.36 0.00
-9 19 8 1.24 0.00
-9 19 5 -1.07 0.00
-9 19 2 0.15 0.00
-10 19 1 -1.72 0.00
-10 19 4 -0.29 0.00
-10 19 7 0.46 0.00
-10 19 10 1.51 0.00
-10 19 13 -1.16 0.00
-10 19 16 0.68 0.00
-10 19 19 0.12 0.00
-10 19 22 1.55 0.00
-10 19 25 -0.19 0.00
-10 19 28 -1.07 0.00
-8 19 27 -1.38 0.00
-8 19 24 -0.33 0.00
-8 19 21 -1.81 0.00
-8 19 18 -0.19 0.00
-8 19 15 -0.87 0.00
-8 19 12 1.70 0.00
-8 19 9 -0.29 0.00
-8 19 6 -0.44 0.00
-8 19 3 1.39 0.00
-8 19 0 -0.11 0.00
-11 19 3 -0.49 0.00
-11 19 6 -1.24 0.00
-11 19 9 -2.26 0.00
-11 19 12 0.46 0.00
-11 19 15 0.55 0.00
-11 19 18 0.48 0.00
-11 19 21 -0.58 0.00
-11 19 24 0.18 0.00
-11 19 27 0.30 0.00
-7 19 28 -2.35 0.00
-7 19 25 -2.22 0.00
-7 19 22 -0.51 0.00
-7 19 19 -1.40 0.00
-7 19 16 -0.67 0.00
-7 19 13 -1.77 0.00
-7 19 10 1.43 0.00
-7 19 7 0.92 0.00
-7 19 4 -1.15 0.00
-7 19 1 1.34 0.00
-12 19 2 -1.26 0.00
-12 19 5 -1.74 0.00
-12 19 8 -1.16 0.00
-12 19 11 -0.98 0.00
-12 19 14 -0.92 0.00
-12 19 17 -0.72 0.00
-12 19 20 0.39 0.00
-12 19 23 0.95 0.00
-12 19 26 -0.68 0.00
-6 19 26 -2.26 0.00
-6 19 23 -1.61 0.00
-6 19 20 0.07 0.00
-6 19 17 -1.63 0.00
-6 19 14 0.08 0.00
-6 19 11 0.66 0.00
-6 19 8 0.57 0.00
-6 19 5 -0.81 0.00
-6 19 2 -0.42 0.00
-13 19 1 -2.15 0.00
-13 19 4 -1.92 0.00
-13 19 7 -0.48 0.00
-13 19 10 -0.34 0.00
-13 19 13 -0.41 0.00
-13 19 16 -0.96 0.00
-13 19 19 -0.58 0.00
-13 19 22 0.27 0.00
-13 19 25 0.99 0.00
-5 19 21 -0.40 0.00
-5 19 18 0.94 0.00
-5 19 15 -1.02 0.00
-5 19 12 0.66 0.00
-5 19 9 0.63 0.00
-5 19 3 -0.39 0.00
-5 19 0 -1.10 0.00
-14 19 3 0.50 0.00
-14 19 6 0.07 0.00
-14 19 9 -0.39 0.00
-14 19 12 -0.77 0.00
-14 19 15 0.46 0.00
-14 19 18 1.14 0.00
-14 19 21 -0.19 0.00
-4 19 19 0.20 0.00
-4 19 4 0.59 0.00
-4 19 1 -1.31 0.00
-15 19 2 -0.48 0.00
-15 19 5 0.95 0.00
-15 19 8 0.64 0.00
-15 19 11 0.76 0.00
-15 19 14 -0.16 0.00
-15 19 17 0.02 0.00
-15 19 20 1.85 0.00
-16 19 1 2.66 0.00
-16 19 4 -0.80 0.00
-16 19 13 1.88 0.00
-10 20 0 0.05 0.00
-10 20 3 -0.82 0.00
-10 20 6 1.12 0.00
-10 20 9 0.59 0.00
-9 20 7 0.24 0.00
-9 20 4 -0.06 0.00
-9 20 1 1.44 0.00
-11 20 2 0.28 0.00
-11 20 5 -0.07 0.00
-11 20 8 0.29 0.00
-11 20 11 -1.17 0.00
-11 20 17 0.41 0.00
-11 20 20 0.83 0.00
-8 20 5 0.68 0.00
-8 20 2 0.30 0.00
-12 20 1 -1.70 0.00
-12 20 4 -1.65 0.00
-12 20 7 -1.64 0.00
-12 20 10 0.44 0.00
-12 20 13 -0.38 0.00
-12 20 16 -0.68 0.00
-12 20 19 -0.73 0.00
-7 20 3 0.48 0.00
-7 20 0 -0.32 0.00
-13 20 3 -1.85 0.00
-13 20 6 -1.46 0.00
-13 20 9 -1.55 0.00
-13 20 12 -0.26 0.00
-13 20 18 -0.42 0.00
-6 20 1 1.64 0.00
-14 20 2 -0.60 0.00
-14 20 5 0.07 0.00
-14 20 8 -0.34 0.00
-1 2 0 104.65 0.00
0 1 2 207.39 0.00
-2 2 2 39.11 0.00
-1 2 3 -58.75 0.00
-1 1 4 117.43 0.00
0 0 6 35.13 0.00
-5 19 6 1.20 0.00
0 1 8 97.13 0.00
0 17 10 1.40 0.00
-2 18 10 0.81 0.00
-12 13 50 1.10 0.00
-11 13 51 -0.31 0.00
-11 12 52 0.21 0.00
-10 13 52 -0.38 0.00
-11 12 55 0.24 0.00
-11 11 56 0.86 0.00
-10 12 56 0.91 0.00
-10 11 57 0.22 0.00
-9 12 57 -1.33 0.00
-8 12 58 0.26 0.00
0 0 0 0.00 0.00
# SQUEEZE RESULTS (Version = 220719)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 110 33 ' '
2 0.000 0.000 0.097 40 1 ' '
3 0.000 0.439 0.250 16 7 ' '
4 0.000 0.000 0.403 40 1 ' '
5 0.000 0.000 0.500 110 33 ' '
6 0.000 0.000 0.597 40 1 ' '
7 0.000 0.560 0.750 16 7 ' '
8 0.000 0.000 0.903 40 1 ' '
9 0.106 0.773 0.083 16 7 ' '
10 0.106 0.333 0.583 16 7 ' '
11 0.333 0.667 0.167 109 33 ' '
12 0.333 0.667 0.667 109 33 ' '
13 0.227 0.333 0.083 16 7 ' '
14 0.227 0.894 0.583 16 7 ' '
15 0.333 0.667 0.264 39 1 ' '
16 0.333 0.667 0.764 39 1 ' '
17 0.333 0.667 0.070 40 1 ' '
18 0.333 0.667 0.570 40 1 ' '
19 0.333 0.227 0.417 16 7 ' '
20 0.333 0.106 0.917 16 7 ' '
21 0.439 1.000 0.250 16 7 ' '
22 0.439 0.439 0.750 17 7 ' '
23 0.667 0.333 0.333 109 33 ' '
24 0.667 0.333 0.833 109 33 ' '
25 0.560 0.561 0.250 16 7 ' '
26 0.560 0.000 0.750 16 7 ' '
27 0.666 0.333 0.430 40 1 ' '
28 0.667 0.333 0.930 40 1 ' '
29 0.667 0.333 0.236 39 1 ' '
30 0.667 0.333 0.736 39 1 ' '
31 0.666 0.894 0.083 16 7 ' '
32 0.666 0.773 0.583 16 7 ' '
33 0.773 0.106 0.417 16 7 ' '
34 0.773 0.666 0.917 16 7 ' '
35 0.894 0.666 0.417 16 7 ' '
36 0.894 0.227 0.917 16 7 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
-1 2 0 2.660
0 1 2 1.694
-2 2 2 3.154
-1 2 3 2.868
-1 1 4 2.098
0 0 6 2.145
0 1 8 3.247
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details
)
TITL Zn9 in R-3c #167
CELL 15.3157 15.3157 56.9773 90.00 90.00 120.00
SPGR R-3c
# Solvent Accessible Volume = 1422
# Electrons Found in S.A.V. = 322
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.893 0.666 0.417 ! 3.75 eA-3
C102 1.000 1.000 0.500 ! 2.39 eA-3
Q103 0.798 0.127 0.300 ! 1.41 eA-3
C104 0.105 0.052 0.994 ! 1.18 eA-3
Q105 0.339 0.437 0.856 ! 0.83 eA-3
Q106 0.691 0.565 0.077 ! 0.64 eA-3
Q107 0.562 0.607 0.416 ! 0.52 eA-3
Q108 0.330 0.498 0.375 ! 0.50 eA-3
)
;
_shelx_fab_checksum 54558
_platon_squeeze_special_details
;
A solvent mask was calculated and 336 electrons were
found in a volume of 1421\%A^3^ in 6 voids per unit cell.
This is consistent with the presence of
[5.5 H2O] per formula unit
which account for 330 electrons
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.770
_oxdiff_exptl_absorpt_empirical_full_min 0.796
#######################################################################
#
# 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_zn54-i2
_audit_block_doi 10.5517/ccdc.csd.cc2j05wm
_database_code_depnum_ccdc_archive 'CCDC 2323880'
loop_
_audit_author_name
_audit_author_address
'Tao Ye'
;Guangxi Normal University
China
;
_audit_update_record
;
2024-11-25 deposited with the CCDC. 2024-12-06 downloaded from the CCDC.
;
_audit_creation_date 2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C348 H288 N156 O118.8 Zn54, 4.8(I2), 23.5[I2]'
_chemical_formula_sum 'C348 H288 I56.60 N156 O118.80 Zn54'
_chemical_formula_weight 19268.65
_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'
I I -0.3257 6.8362 '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'
Zn Zn -1.5491 0.6778 '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 203
_space_group_name_H-M_alt 'F d -3'
_space_group_name_Hall '-F 2uv 2vw 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'-x+1/4, y, -z+1/4'
'x, -y+1/4, -z+1/4'
'z, x, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, z, x'
'-y+1/4, z, -x+1/4'
'y, -z+1/4, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'-x+1/4, y+1/2, -z+3/4'
'x, -y+3/4, -z+3/4'
'z, x+1/2, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'-y+1/4, z+1/2, -x+3/4'
'y, -z+3/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'-x+3/4, y, -z+3/4'
'x+1/2, -y+1/4, -z+3/4'
'z+1/2, x, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'-y+3/4, z, -x+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+3/4, -z+1/4'
'z+1/2, x+1/2, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y, z-1/4'
'-x, y-1/4, z-1/4'
'-z, -x, -y'
'-z, x-1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'y-1/4, -z, x-1/4'
'-y, z-1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'x-1/4, -y+1/2, z+1/4'
'-x, y+1/4, z+1/4'
'-z, -x+1/2, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-1/4, -z+1/2, x+1/4'
'-y, z+1/4, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'x+1/4, -y, z+1/4'
'-x+1/2, y-1/4, z+1/4'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'y+1/4, -z, x+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'x+1/4, -y+1/2, z-1/4'
'-x+1/2, y+1/4, z-1/4'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'y+1/4, -z+1/2, x-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, z+1/4, -x'
_cell_length_a 58.9792(3)
_cell_length_b 58.9792(3)
_cell_length_c 58.9792(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 205162(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 16437
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 66.6360
_cell_measurement_theta_min 2.4760
_shelx_estimated_absorpt_T_max 0.111
_shelx_estimated_absorpt_T_min 0.093
_exptl_absorpt_coefficient_mu 15.090
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67049
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.248
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 72306
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.26
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0423
_diffrn_reflns_av_unetI/netI 0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max 74
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 60
_diffrn_reflns_limit_k_min -35
_diffrn_reflns_limit_l_max 43
_diffrn_reflns_limit_l_min -58
_diffrn_reflns_number 63823
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.032
_diffrn_reflns_theta_min 2.485
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -28.00 27.00 0.50 30.00 -- 43.30 -19.00 90.00 110
2 \w 36.00 66.00 0.50 70.00 -- 109.26 -61.00 76.00 60
3 \w 35.00 71.00 0.50 70.00 -- 109.26 -61.00 30.00 72
4 \w -76.00 -18.00 0.50 70.00 -- -90.25 113.00 14.00 116
5 \w -39.00 -14.00 0.50 70.00 -- -90.25 45.00 30.00 50
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0015124000
_diffrn_orient_matrix_UB_12 0.0209815000
_diffrn_orient_matrix_UB_13 -0.0154550000
_diffrn_orient_matrix_UB_21 0.0221093000
_diffrn_orient_matrix_UB_22 0.0092435000
_diffrn_orient_matrix_UB_23 0.0104055000
_diffrn_orient_matrix_UB_31 0.0138440000
_diffrn_orient_matrix_UB_32 -0.0124907000
_diffrn_orient_matrix_UB_33 -0.0183159000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 10617
_reflns_number_total 16367
_reflns_odcompleteness_completeness 98.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max 0.881
_refine_diff_density_min -1.425
_refine_diff_density_rms 0.083
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.001
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 561
_refine_ls_number_reflns 16367
_refine_ls_number_restraints 95
_refine_ls_R_factor_all 0.0865
_refine_ls_R_factor_gt 0.0672
_refine_ls_restrained_S_all 1.030
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2132
_refine_ls_wR_factor_ref 0.2336
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
I2-I1 = I1-I2'
2.9 with sigma of 0.02
C18-C17 = C18-C17A
1.45 with sigma of 0.02
C18-C17 \\sim C18-C17A
with sigma of 0.02
O5-C17 \\sim O5A-C17A \\sim O6-C17 \\sim O6A-C17A
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I2') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(I3) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C17A)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(I3) = Uanis(I3')
Uanis(I2) = Uanis(I2')
Uanis(O5) = Uanis(O5A)
Uanis(C17) = Uanis(C17A)
Uanis(O6) = Uanis(O6A)
4. Others
Sof(O5A)=Sof(O6A)=Sof(C17A)=1-FVAR(1)
Sof(O5)=Sof(O6)=Sof(C17)=FVAR(1)
Fixed Sof: O9(0.9) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5)
H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5) I1(0.26666) I2(0.13333)
I2'(0.13333) I3(0.13333) I3'(0.13333)
Fixed X: C28(0.52369)
Fixed Y: C28(0.40525)
Fixed Z: C28(0.628091)
5.a Rotating group:
O10(H10A,H10B)
5.b Ternary CH refined with riding coordinates:
N13(H13)
5.c Secondary CH2 refined with riding coordinates:
C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
5.d Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C12(H12), C13(H13A), C14(H14), C19(H19), C20(H20),
C21(H21)
5.e Idealised Me refined as rotating group:
C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
Zn1 Zn 0.58704(2) 0.52402(2) 0.66482(2) 0.05696(16) Uani 1 1 d . . . . .
Zn2 Zn 0.625000 0.51635(2) 0.625000 0.05177(18) Uani 1 2 d S T P . .
Zn3 Zn 0.55502(2) 0.44761(2) 0.57937(2) 0.0787(2) Uani 1 1 d . . . . .
Zn4 Zn 0.57409(2) 0.42374(2) 0.62576(2) 0.0826(2) Uani 1 1 d . . . . .
Zn5 Zn 0.66745(2) 0.38938(2) 0.58108(2) 0.1434(4) Uani 1 1 d . . . . .
O1 O 0.59177(5) 0.55398(4) 0.72824(4) 0.0657(7) Uani 1 1 d . . . . .
O2 O 0.59088(5) 0.54946(4) 0.69070(4) 0.0609(6) Uani 1 1 d . . . . .
O3 O 0.54113(6) 0.42715(7) 0.55273(6) 0.0956(11) Uani 1 1 d . . . . .
O4 O 0.54261(7) 0.42076(8) 0.51536(6) 0.1100(13) Uani 1 1 d . . . . .
O5 O 0.6885(3) 0.3774(3) 0.5560(3) 0.156(4) Uani 0.496(14) 1 d D U P A 1
O5A O 0.6942(3) 0.3887(3) 0.5514(3) 0.156(4) Uani 0.504(14) 1 d D U P A 2
O6 O 0.6930(4) 0.3782(5) 0.5188(3) 0.212(6) Uani 0.496(14) 1 d D U P A 1
O6A O 0.6969(4) 0.3945(5) 0.5142(3) 0.212(6) Uani 0.504(14) 1 d D U P A 2
O7 O 0.60686(5) 0.53706(4) 0.64279(4) 0.0619(6) Uani 1 1 d . . . . .
O8 O 0.54969(6) 0.42743(6) 0.60419(6) 0.0921(10) Uani 1 1 d . . . . .
O9 O 0.56272(8) 0.40200(7) 0.64719(8) 0.1094(14) Uani 0.9 1 d . . P . .
O10 O 0.65881(14) 0.35449(12) 0.58947(16) 0.213(3) Uani 1 1 d . U . . .
H10A H 0.656821 0.346967 0.605631 0.320 Uiso 1 1 d R U . . .
H10B H 0.655418 0.340593 0.578572 0.320 Uiso 1 1 d R U . . .
N1 N 0.59013(5) 0.50524(5) 0.69410(5) 0.0595(7) Uani 1 1 d . . . . .
N2 N 0.59092(5) 0.48757(5) 0.65258(5) 0.0575(7) Uani 1 1 d . . . . .
N3 N 0.58259(7) 0.45240(6) 0.66562(6) 0.0733(9) Uani 1 1 d . . . . .
N4 N 0.58224(6) 0.45230(6) 0.64220(6) 0.0715(9) Uani 1 1 d . . . . .
N5 N 0.58295(5) 0.46879(6) 0.59363(6) 0.0624(8) Uani 1 1 d . . . . .
N6 N 0.60572(5) 0.49605(5) 0.60592(5) 0.0579(7) Uani 1 1 d . . . . .
N7 N 0.60707(6) 0.49653(6) 0.58267(5) 0.0638(8) Uani 1 1 d . . . . .
N8 N 0.57262(6) 0.45765(7) 0.55121(6) 0.0736(9) Uani 1 1 d . . . . .
N9 N 0.65053(12) 0.40152(11) 0.55247(10) 0.133(2) Uani 1 1 d . . . . .
N10 N 0.60048(9) 0.41578(7) 0.58354(8) 0.0947(13) Uani 1 1 d . . . . .
N11 N 0.63563(9) 0.40568(7) 0.59498(8) 0.0937(12) Uani 1 1 d . . . . .
N12 N 0.62142(11) 0.40878(8) 0.61295(9) 0.1134(17) Uani 1 1 d . . . . .
N13 N 0.53005(7) 0.47168(9) 0.58305(9) 0.0972(13) Uani 1 1 d . . . . .
H13 H 0.515069 0.464099 0.580674 0.117 Uiso 1 1 calc R U . . .
C1 C 0.59148(7) 0.54235(7) 0.71050(7) 0.0601(9) Uani 1 1 d . . . . .
C2 C 0.59158(7) 0.51681(7) 0.71372(6) 0.0641(9) Uani 1 1 d . . . . .
C3 C 0.59230(9) 0.50536(7) 0.73426(7) 0.0762(11) Uani 1 1 d . . . . .
H3 H 0.593341 0.513430 0.748162 0.091 Uiso 1 1 calc R U . . .
C4 C 0.59149(10) 0.48206(8) 0.73401(8) 0.0873(14) Uani 1 1 d . . . . .
H4 H 0.592008 0.473928 0.747906 0.105 Uiso 1 1 calc R U . . .
C5 C 0.58993(9) 0.47037(7) 0.71383(8) 0.0802(12) Uani 1 1 d . . . . .
H5 H 0.589352 0.454274 0.713630 0.096 Uiso 1 1 calc R U . . .
C6 C 0.58922(7) 0.48281(6) 0.69369(7) 0.0631(9) Uani 1 1 d . . . . .
C7 C 0.58759(7) 0.47361(7) 0.67102(7) 0.0655(10) Uani 1 1 d . . . . .
C8 C 0.58740(6) 0.47334(6) 0.63529(7) 0.0575(8) Uani 1 1 d . . . . .
C9 C 0.59128(6) 0.47949(6) 0.61167(6) 0.0569(8) Uani 1 1 d . . . . .
C10 C 0.59318(7) 0.48005(7) 0.57614(7) 0.0642(9) Uani 1 1 d . . . . .
C11 C 0.58877(8) 0.47330(8) 0.55272(8) 0.0718(11) Uani 1 1 d . . . . .
C12 C 0.59932(9) 0.48171(8) 0.53380(8) 0.0807(12) Uani 1 1 d . . . . .
H12 H 0.610307 0.493420 0.535019 0.097 Uiso 1 1 calc R U . . .
C13 C 0.59349(9) 0.47258(9) 0.51244(8) 0.0863(13) Uani 1 1 d . . . . .
H13A H 0.600894 0.477665 0.499074 0.104 Uiso 1 1 calc R U . . .
C14 C 0.57672(9) 0.45600(10) 0.51130(8) 0.0880(14) Uani 1 1 d . . . . .
H14 H 0.572373 0.449703 0.497129 0.106 Uiso 1 1 calc R U . . .
C15 C 0.56649(8) 0.44886(9) 0.53123(8) 0.0807(12) Uani 1 1 d . . . . .
C16 C 0.54852(8) 0.43094(10) 0.53327(9) 0.0878(14) Uani 1 1 d . . . . .
C17 C 0.6812(4) 0.3845(4) 0.5361(3) 0.163(5) Uani 0.496(14) 1 d D U P A 1
C17A C 0.6866(2) 0.3976(4) 0.5328(3) 0.163(5) Uani 0.504(14) 1 d D U P A 2
C18 C 0.66124(17) 0.4004(2) 0.53238(17) 0.166(4) Uani 1 1 d D . . . .
C19 C 0.6503(2) 0.40765(19) 0.51328(16) 0.162(4) Uani 1 1 d . . . . .
H19 H 0.657576 0.406328 0.498947 0.194 Uiso 1 1 calc R U . . .
C20 C 0.63102(19) 0.41598(16) 0.51456(14) 0.143(3) Uani 1 1 d . . . . .
H20 H 0.624221 0.421772 0.501152 0.172 Uiso 1 1 calc R U . . .
C21 C 0.61847(16) 0.41725(13) 0.53556(12) 0.128(2) Uani 1 1 d . . . . .
H21 H 0.603318 0.422661 0.536317 0.153 Uiso 1 1 calc R U . . .
C22 C 0.63001(13) 0.41010(11) 0.55406(11) 0.1080(19) Uani 1 1 d . . . . .
C23 C 0.62158(12) 0.41053(9) 0.57749(10) 0.0965(16) Uani 1 1 d . . . . .
C24 C 0.60056(8) 0.41459(7) 0.60703(8) 0.0708(11) Uani 1 1 d . . . . .
C25 C 0.60956(9) 0.56044(7) 0.64060(8) 0.0776(12) Uani 1 1 d . . . . .
H25A H 0.594517 0.566874 0.636862 0.093 Uiso 1 1 calc R U . . .
H25B H 0.613811 0.566412 0.655699 0.093 Uiso 1 1 calc R U . . .
C26 C 0.625000 0.56914(14) 0.625000 0.139(4) Uani 1 2 d S TU P . .
H26A H 0.634470 0.579346 0.634372 0.167 Uiso 0.5 1 calc R U P . .
H26B H 0.615530 0.579346 0.615628 0.167 Uiso 0.5 1 calc R U P . .
C27 C 0.52982(19) 0.4155(2) 0.6064(2) 0.097(3) Uani 0.5 1 d . U P B 2
H27A H 0.530112 0.403205 0.594986 0.116 Uiso 0.5 1 calc R U P B 2
H27B H 0.517315 0.425848 0.602083 0.116 Uiso 0.5 1 calc R U P B 2
C28 C 0.523690 0.405250 0.628091 0.195(9) Uani 0.5 1 d . U P B 2
H28A H 0.517927 0.417510 0.638001 0.234 Uiso 0.5 1 calc R U P B 2
H28B H 0.510860 0.394802 0.625264 0.234 Uiso 0.5 1 calc R U P B 2
C29 C 0.5407(3) 0.3927(3) 0.6409(3) 0.134(5) Uani 0.5 1 d . U P B 2
H29A H 0.533350 0.387998 0.655241 0.160 Uiso 0.5 1 calc R U P B 2
H29B H 0.543812 0.378686 0.632286 0.160 Uiso 0.5 1 calc R U P B 2
C30 C 0.53013(13) 0.48240(16) 0.60786(13) 0.143(3) Uani 1 1 d . . . . .
H30A H 0.541345 0.494640 0.608570 0.214 Uiso 1 1 calc R U . . .
H30B H 0.534032 0.470663 0.618955 0.214 Uiso 1 1 calc R U . . .
H30C H 0.515060 0.488493 0.611313 0.214 Uiso 1 1 calc R U . . .
C31 C 0.53119(16) 0.4907(2) 0.56830(18) 0.178(4) Uani 1 1 d . . . . .
H31A H 0.515956 0.494308 0.562727 0.267 Uiso 1 1 calc R U . . .
H31B H 0.541095 0.487151 0.555444 0.267 Uiso 1 1 calc R U . . .
H31C H 0.537298 0.503759 0.576563 0.267 Uiso 1 1 calc R U . . .
I1 I 0.52811(2) 0.52811(2) 0.72189(2) 0.2336(10) Uani 0.8 3 d DS T P . .
I2 I 0.52637(15) 0.48587(16) 0.7114(2) 0.260(3) Uani 0.1333 1 d D U P . .
I2' I 0.53168(16) 0.48923(16) 0.7448(2) 0.260(3) Uani 0.1333 1 d D U P . .
I3 I 0.5312(2) 0.4391(2) 0.6977(3) 0.323(4) Uani 0.1333 1 d . U P C 1
I3' I 0.5255(2) 0.4529(2) 0.6787(3) 0.323(4) Uani 0.1333 1 d . . 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
Zn1 0.0590(3) 0.0560(3) 0.0560(3) 0.0044(2) 0.0014(2) 0.0008(2)
Zn2 0.0544(4) 0.0471(3) 0.0538(4) 0.000 -0.0044(3) 0.000
Zn3 0.0663(3) 0.0973(4) 0.0726(4) -0.0113(3) -0.0122(3) -0.0166(3)
Zn4 0.0969(4) 0.0615(3) 0.0893(4) -0.0053(3) -0.0195(3) -0.0171(3)
Zn5 0.1505(9) 0.1348(8) 0.1449(8) -0.0548(7) -0.0281(7) 0.0460(7)
O1 0.0789(17) 0.0620(15) 0.0561(14) -0.0006(12) 0.0016(12) -0.0011(13)
O2 0.0725(16) 0.0535(13) 0.0568(14) 0.0024(11) 0.0031(12) 0.0003(12)
O3 0.086(2) 0.124(3) 0.077(2) -0.0175(19) -0.0207(17) -0.033(2)
O4 0.109(3) 0.135(3) 0.086(2) -0.032(2) -0.019(2) -0.038(2)
O5 0.137(5) 0.160(7) 0.169(6) -0.016(5) 0.019(4) 0.034(5)
O5A 0.137(5) 0.160(7) 0.169(6) -0.016(5) 0.019(4) 0.034(5)
O6 0.201(8) 0.261(14) 0.175(8) -0.026(10) 0.054(7) 0.019(11)
O6A 0.201(8) 0.261(14) 0.175(8) -0.026(10) 0.054(7) 0.019(11)
O7 0.0730(16) 0.0481(13) 0.0646(15) 0.0030(11) 0.0115(12) 0.0015(11)
O8 0.088(2) 0.091(2) 0.098(2) -0.0030(18) -0.0160(18) -0.0288(18)
O9 0.114(3) 0.080(2) 0.133(3) 0.023(2) -0.018(3) -0.036(2)
O10 0.224(6) 0.141(4) 0.275(7) -0.050(5) -0.033(6) 0.068(4)
N1 0.0616(17) 0.0580(17) 0.0588(17) 0.0042(14) 0.0012(14) 0.0014(14)
N2 0.0616(17) 0.0525(16) 0.0583(17) 0.0023(13) -0.0019(14) -0.0003(13)
N3 0.098(3) 0.0539(18) 0.068(2) 0.0044(15) -0.0055(18) -0.0149(17)
N4 0.081(2) 0.0591(19) 0.074(2) 0.0032(16) -0.0111(17) -0.0148(16)
N5 0.0568(17) 0.0681(19) 0.0623(18) -0.0068(15) -0.0080(14) -0.0067(14)
N6 0.0652(18) 0.0574(17) 0.0509(16) -0.0008(13) -0.0060(14) -0.0033(14)
N7 0.0689(19) 0.0631(18) 0.0594(18) 0.0001(14) -0.0112(15) -0.0014(15)
N8 0.065(2) 0.089(2) 0.067(2) -0.0110(18) -0.0189(16) -0.0018(18)
N9 0.155(6) 0.132(5) 0.111(4) -0.041(4) -0.009(4) 0.020(4)
N10 0.121(4) 0.073(2) 0.089(3) -0.017(2) -0.021(3) 0.002(2)
N11 0.111(3) 0.079(3) 0.091(3) -0.014(2) -0.008(3) 0.011(2)
N12 0.159(5) 0.069(3) 0.112(4) -0.004(2) -0.030(4) -0.006(3)
N13 0.066(2) 0.106(3) 0.119(4) 0.020(3) -0.015(2) -0.009(2)
C1 0.061(2) 0.060(2) 0.059(2) -0.0024(18) 0.0040(17) -0.0027(17)
C2 0.073(2) 0.064(2) 0.055(2) 0.0029(17) 0.0046(18) 0.0045(18)
C3 0.105(3) 0.065(2) 0.058(2) 0.0001(19) -0.003(2) 0.001(2)
C4 0.127(4) 0.072(3) 0.063(3) 0.015(2) 0.000(3) 0.001(3)
C5 0.115(4) 0.054(2) 0.071(3) 0.010(2) 0.004(2) -0.007(2)
C6 0.075(2) 0.052(2) 0.063(2) 0.0050(16) -0.0002(18) -0.0043(18)
C7 0.075(2) 0.054(2) 0.068(2) 0.0071(18) -0.0044(19) -0.0014(18)
C8 0.057(2) 0.0503(19) 0.065(2) 0.0016(17) -0.0066(16) -0.0028(15)
C9 0.0541(19) 0.0543(19) 0.062(2) -0.0041(16) -0.0090(16) -0.0011(15)
C10 0.065(2) 0.065(2) 0.063(2) -0.0054(18) -0.0184(18) -0.0025(18)
C11 0.072(3) 0.073(3) 0.070(3) -0.006(2) -0.018(2) -0.001(2)
C12 0.092(3) 0.084(3) 0.066(3) -0.005(2) -0.012(2) -0.009(2)
C13 0.097(3) 0.100(3) 0.062(3) -0.005(2) -0.012(2) -0.001(3)
C14 0.091(3) 0.106(4) 0.067(3) -0.019(3) -0.023(2) -0.007(3)
C15 0.081(3) 0.093(3) 0.068(3) -0.014(2) -0.021(2) -0.003(2)
C16 0.072(3) 0.111(4) 0.081(3) -0.021(3) -0.015(2) -0.019(3)
C17 0.164(7) 0.170(8) 0.154(7) -0.011(6) 0.012(6) 0.009(6)
C17A 0.164(7) 0.170(8) 0.154(7) -0.011(6) 0.012(6) 0.009(6)
C18 0.158(8) 0.223(11) 0.116(6) -0.065(7) -0.008(6) 0.016(7)
C19 0.177(9) 0.192(9) 0.116(7) -0.053(6) 0.015(7) 0.020(8)
C20 0.178(9) 0.150(7) 0.102(5) -0.025(5) 0.001(5) 0.000(6)
C21 0.164(7) 0.127(5) 0.092(4) -0.022(4) -0.014(4) 0.012(5)
C22 0.132(5) 0.096(4) 0.096(4) -0.033(3) -0.014(4) 0.013(4)
C23 0.123(5) 0.068(3) 0.099(4) -0.018(3) -0.020(3) 0.004(3)
C24 0.083(3) 0.054(2) 0.076(3) -0.0102(19) -0.025(2) 0.0009(19)
C25 0.101(3) 0.050(2) 0.081(3) 0.0014(19) 0.030(2) 0.005(2)
C26 0.175(7) 0.067(4) 0.175(7) 0.000 0.085(6) 0.000
C27 0.087(6) 0.104(6) 0.100(6) 0.011(5) -0.006(5) -0.035(5)
C28 0.190(11) 0.203(12) 0.193(11) 0.027(9) -0.005(9) -0.039(9)
C29 0.122(8) 0.134(8) 0.145(8) 0.025(7) -0.010(7) -0.036(7)
C30 0.112(5) 0.196(8) 0.120(5) -0.043(5) -0.021(4) 0.040(5)
C31 0.119(6) 0.239(12) 0.177(9) 0.026(8) 0.006(6) 0.027(7)
I1 0.2336(10) 0.2336(10) 0.2336(10) 0.0387(8) 0.0387(8) -0.0387(8)
I2 0.208(4) 0.255(5) 0.318(6) 0.051(5) 0.021(5) -0.013(4)
I2' 0.208(4) 0.255(5) 0.318(6) 0.051(5) 0.021(5) -0.013(4)
I3 0.290(7) 0.324(8) 0.355(9) 0.038(6) 0.022(7) -0.027(6)
I3' 0.290(7) 0.324(8) 0.355(9) 0.038(6) 0.022(7) -0.027(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.993(3) 11_566 ?
Zn1 O2 2.152(3) . ?
Zn1 O7 1.909(3) . ?
Zn1 N1 2.060(3) . ?
Zn1 N2 2.279(3) . ?
Zn2 O7 1.934(3) . ?
Zn2 O7 1.934(3) 3_656 ?
Zn2 N6 1.998(3) 3_656 ?
Zn2 N6 1.998(3) . ?
Zn3 O3 2.144(3) . ?
Zn3 O8 1.913(4) . ?
Zn3 N5 2.232(3) . ?
Zn3 N8 2.046(4) . ?
Zn3 N13 2.057(5) . ?
Zn4 O8 1.933(3) . ?
Zn4 O9 1.921(4) . ?
Zn4 N4 2.002(3) . ?
Zn4 C24 1.987(5) . ?
Zn5 O5 2.054(16) . ?
Zn5 O5A 2.356(17) . ?
Zn5 O9 1.888(5) 3_656 ?
Zn5 O10 2.177(8) . ?
Zn5 N9 2.087(7) . ?
Zn5 N11 2.262(5) . ?
O1 C1 1.251(5) . ?
O2 C1 1.241(5) . ?
O3 C16 1.247(6) . ?
O4 C16 1.264(6) . ?
O5 C17 1.317(14) . ?
O5A C17A 1.294(14) . ?
O6 C17 1.290(13) . ?
O6A C17A 1.267(13) . ?
O7 C25 1.394(5) . ?
O8 C27 1.373(10) . ?
O9 C29 1.454(14) . ?
O10 H10A 1.0577 . ?
O10 H10B 1.0605 . ?
N1 C2 1.346(5) . ?
N1 C6 1.324(5) . ?
N2 C7 1.378(5) . ?
N2 C8 1.337(5) . ?
N3 N4 1.382(5) . ?
N3 C7 1.324(5) . ?
N4 C8 1.341(5) . ?
N5 C9 1.331(5) . ?
N5 C10 1.367(5) . ?
N6 N7 1.374(4) . ?
N6 C9 1.340(5) . ?
N7 C10 1.328(5) . ?
N8 C11 1.329(6) . ?
N8 C15 1.338(5) . ?
N9 C18 1.345(11) . ?
N9 C22 1.315(9) . ?
N10 C23 1.331(8) . ?
N10 C24 1.388(6) . ?
N11 N12 1.363(7) . ?
N11 C23 1.354(7) . ?
N12 N12 1.483(10) 3_656 ?
N12 C24 1.324(7) . ?
N13 H13 1.0000 . ?
N13 C30 1.594(9) . ?
N13 C31 1.421(11) . ?
C1 C2 1.519(6) . ?
C2 C3 1.388(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.375(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.379(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.397(6) . ?
C6 C7 1.446(6) . ?
C8 C9 1.458(6) . ?
C10 C11 1.461(6) . ?
C11 C12 1.371(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.412(6) . ?
C13 H13A 0.9500 . ?
C13 C14 1.392(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(7) . ?
C15 C16 1.502(7) . ?
C17 C18 1.522(13) . ?
C17A C18 1.505(13) . ?
C18 C19 1.365(13) . ?
C19 H19 0.9500 . ?
C19 C20 1.244(12) . ?
C20 H20 0.9500 . ?
C20 C21 1.445(11) . ?
C21 H21 0.9500 . ?
C21 C22 1.354(9) . ?
C22 C23 1.469(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.392(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.461(11) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.459(16) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
I1 I2 2.569(10) . ?
I1 I2 2.569(10) 8_656 ?
I1 I2 2.569(10) 11_566 ?
I1 I2' 2.669(9) 11_566 ?
I1 I2' 2.669(9) 8_656 ?
I1 I2' 2.669(9) . ?
I2 I2' 2.504(15) 11_566 ?
I2 I3 2.889(18) . ?
I2 I3' 2.738(19) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O2 106.74(11) 11_566 . ?
O1 Zn1 N1 102.38(12) 11_566 . ?
O1 Zn1 N2 88.47(11) 11_566 . ?
O2 Zn1 N2 150.63(10) . . ?
O7 Zn1 O1 119.57(12) . 11_566 ?
O7 Zn1 O2 97.89(10) . . ?
O7 Zn1 N1 137.11(12) . . ?
O7 Zn1 N2 95.91(11) . . ?
N1 Zn1 O2 76.76(11) . . ?
N1 Zn1 N2 75.48(12) . . ?
O7 Zn2 O7 101.62(15) . 3_656 ?
O7 Zn2 N6 111.67(12) . . ?
O7 Zn2 N6 112.82(11) . 3_656 ?
O7 Zn2 N6 111.67(12) 3_656 3_656 ?
O7 Zn2 N6 112.82(11) 3_656 . ?
N6 Zn2 N6 106.40(18) . 3_656 ?
O3 Zn3 N5 150.83(14) . . ?
O8 Zn3 O3 98.51(15) . . ?
O8 Zn3 N5 100.44(13) . . ?
O8 Zn3 N8 152.21(16) . . ?
O8 Zn3 N13 103.35(18) . . ?
N8 Zn3 O3 76.21(14) . . ?
N8 Zn3 N5 76.67(13) . . ?
N8 Zn3 N13 104.44(17) . . ?
N13 Zn3 O3 101.08(18) . . ?
N13 Zn3 N5 95.88(16) . . ?
O8 Zn4 N4 113.74(15) . . ?
O8 Zn4 C24 104.47(17) . . ?
O9 Zn4 O8 104.36(17) . . ?
O9 Zn4 N4 109.07(18) . . ?
O9 Zn4 C24 117.3(2) . . ?
C24 Zn4 N4 108.00(16) . . ?
O5 Zn5 O10 88.9(6) . . ?
O5 Zn5 N9 79.9(5) . . ?
O5 Zn5 N11 155.2(5) . . ?
O9 Zn5 O5 104.4(5) 3_656 . ?
O9 Zn5 O5A 95.6(4) 3_656 . ?
O9 Zn5 O10 111.3(3) 3_656 . ?
O9 Zn5 N9 135.2(2) 3_656 . ?
O9 Zn5 N11 95.76(18) 3_656 . ?
O10 Zn5 O5A 108.0(5) . . ?
O10 Zn5 N11 97.2(3) . . ?
N9 Zn5 O5A 74.0(4) . . ?
N9 Zn5 O10 113.3(3) . . ?
N9 Zn5 N11 75.6(2) . . ?
N11 Zn5 O5A 146.2(4) . . ?
C1 O1 Zn1 118.5(2) . 8_656 ?
C1 O2 Zn1 115.8(2) . . ?
C16 O3 Zn3 116.1(3) . . ?
C17 O5 Zn5 109.6(12) . . ?
C17A O5A Zn5 113.1(11) . . ?
Zn1 O7 Zn2 116.97(12) . . ?
C25 O7 Zn1 122.1(2) . . ?
C25 O7 Zn2 120.8(2) . . ?
Zn3 O8 Zn4 116.82(16) . . ?
C27 O8 Zn3 122.1(5) . . ?
C27 O8 Zn4 121.0(5) . . ?
Zn5 O9 Zn4 119.5(2) 3_656 . ?
C29 O9 Zn4 113.3(7) . . ?
C29 O9 Zn5 125.2(6) . 3_656 ?
Zn5 O10 H10A 128.8 . . ?
Zn5 O10 H10B 129.5 . . ?
H10A O10 H10B 101.6 . . ?
C2 N1 Zn1 117.0(3) . . ?
C6 N1 Zn1 121.2(3) . . ?
C6 N1 C2 121.7(3) . . ?
C7 N2 Zn1 107.4(2) . . ?
C8 N2 Zn1 144.9(2) . . ?
C8 N2 C7 101.8(3) . . ?
C7 N3 N4 104.4(3) . . ?
N3 N4 Zn4 119.4(2) . . ?
C8 N4 Zn4 133.3(3) . . ?
C8 N4 N3 107.2(3) . . ?
C9 N5 Zn3 147.0(3) . . ?
C9 N5 C10 102.1(3) . . ?
C10 N5 Zn3 108.2(2) . . ?
N7 N6 Zn2 121.1(2) . . ?
C9 N6 Zn2 131.0(2) . . ?
C9 N6 N7 107.7(3) . . ?
C10 N7 N6 103.8(3) . . ?
C11 N8 Zn3 120.7(3) . . ?
C11 N8 C15 121.5(4) . . ?
C15 N8 Zn3 117.8(3) . . ?
C18 N9 Zn5 118.1(6) . . ?
C22 N9 Zn5 121.0(5) . . ?
C22 N9 C18 120.9(8) . . ?
C23 N10 C24 104.6(5) . . ?
N12 N11 Zn5 148.1(4) . . ?
C23 N11 Zn5 108.8(4) . . ?
C23 N11 N12 100.8(5) . . ?
N11 N12 N12 124.8(7) . 3_656 ?
C24 N12 N11 113.7(5) . . ?
C24 N12 N12 121.1(8) . 3_656 ?
Zn3 N13 H13 108.0 . . ?
C30 N13 Zn3 111.6(4) . . ?
C30 N13 H13 108.0 . . ?
C31 N13 Zn3 116.5(5) . . ?
C31 N13 H13 108.0 . . ?
C31 N13 C30 104.4(7) . . ?
O1 C1 C2 116.1(3) . . ?
O2 C1 O1 127.0(4) . . ?
O2 C1 C2 116.9(3) . . ?
N1 C2 C1 113.3(3) . . ?
N1 C2 C3 120.4(4) . . ?
C3 C2 C1 126.3(4) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.4(4) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.9 . . ?
C4 C5 C6 118.3(4) . . ?
C6 C5 H5 120.9 . . ?
N1 C6 C5 120.5(4) . . ?
N1 C6 C7 113.2(3) . . ?
C5 C6 C7 126.3(4) . . ?
N2 C7 C6 119.7(3) . . ?
N3 C7 N2 114.0(4) . . ?
N3 C7 C6 126.3(4) . . ?
N2 C8 N4 112.6(3) . . ?
N2 C8 C9 123.3(3) . . ?
N4 C8 C9 123.8(3) . . ?
N5 C9 N6 112.2(3) . . ?
N5 C9 C8 126.0(3) . . ?
N6 C9 C8 121.5(3) . . ?
N5 C10 C11 120.2(4) . . ?
N7 C10 N5 114.1(3) . . ?
N7 C10 C11 125.7(4) . . ?
N8 C11 C10 112.3(4) . . ?
N8 C11 C12 121.5(4) . . ?
C12 C11 C10 126.2(4) . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.5(5) . . ?
C13 C12 H12 120.7 . . ?
C12 C13 H13A 120.5 . . ?
C14 C13 C12 118.9(5) . . ?
C14 C13 H13A 120.5 . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.8(4) . . ?
C15 C14 H14 120.6 . . ?
N8 C15 C14 120.8(4) . . ?
N8 C15 C16 113.1(4) . . ?
C14 C15 C16 126.1(4) . . ?
O3 C16 O4 126.0(5) . . ?
O3 C16 C15 116.5(4) . . ?
O4 C16 C15 117.5(5) . . ?
O5 C17 C18 125.2(15) . . ?
O6 C17 O5 116.1(17) . . ?
O6 C17 C18 118.6(16) . . ?
O5A C17A C18 113.6(14) . . ?
O6A C17A O5A 120.7(18) . . ?
O6A C17A C18 118.6(17) . . ?
N9 C18 C17 105.4(11) . . ?
N9 C18 C17A 117.2(10) . . ?
N9 C18 C19 119.4(9) . . ?
C19 C18 C17 132.7(10) . . ?
C19 C18 C17A 121.0(12) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.3(9) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 118.6 . . ?
C19 C20 C21 122.8(10) . . ?
C21 C20 H20 118.6 . . ?
C20 C21 H21 122.7 . . ?
C22 C21 C20 114.7(8) . . ?
C22 C21 H21 122.7 . . ?
N9 C22 C21 121.7(7) . . ?
N9 C22 C23 112.6(6) . . ?
C21 C22 C23 125.6(7) . . ?
N10 C23 N11 114.7(6) . . ?
N10 C23 C22 124.9(6) . . ?
N11 C23 C22 120.4(6) . . ?
N10 C24 Zn4 122.6(4) . . ?
N12 C24 Zn4 130.8(4) . . ?
N12 C24 N10 106.2(5) . . ?
O7 C25 H25A 107.3 . . ?
O7 C25 H25B 107.3 . . ?
H25A C25 H25B 106.9 . . ?
C26 C25 O7 120.0(5) . . ?
C26 C25 H25A 107.3 . . ?
C26 C25 H25B 107.3 . . ?
C25 C26 C25 136.8(7) . 3_656 ?
C25 C26 H26A 103.0 3_656 . ?
C25 C26 H26A 103.0 . . ?
C25 C26 H26B 103.0 . . ?
C25 C26 H26B 103.0 3_656 . ?
H26A C26 H26B 105.1 . . ?
O8 C27 H27A 107.2 . . ?
O8 C27 H27B 107.2 . . ?
O8 C27 C28 120.4(8) . . ?
H27A C27 H27B 106.9 . . ?
C28 C27 H27A 107.2 . . ?
C28 C27 H27B 107.2 . . ?
C27 C28 H28A 107.4 . . ?
C27 C28 H28B 107.4 . . ?
H28A C28 H28B 107.0 . . ?
C29 C28 C27 119.6(8) . . ?
C29 C28 H28A 107.4 . . ?
C29 C28 H28B 107.4 . . ?
O9 C29 C28 123.8(10) . . ?
O9 C29 H29A 106.4 . . ?
O9 C29 H29B 106.4 . . ?
C28 C29 H29A 106.4 . . ?
C28 C29 H29B 106.4 . . ?
H29A C29 H29B 106.5 . . ?
N13 C30 H30A 109.5 . . ?
N13 C30 H30B 109.5 . . ?
N13 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N13 C31 H31A 109.5 . . ?
N13 C31 H31B 109.5 . . ?
N13 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
I2 I1 I2 101.8(3) 11_566 8_656 ?
I2 I1 I2 101.8(3) 11_566 . ?
I2 I1 I2 101.8(3) . 8_656 ?
I2 I1 I2' 45.0(3) 11_566 11_566 ?
I2 I1 I2' 57.1(3) 11_566 8_656 ?
I2 I1 I2' 105.3(3) . 8_656 ?
I2 I1 I2' 45.0(3) 8_656 8_656 ?
I2 I1 I2' 57.1(3) 8_656 . ?
I2 I1 I2' 105.3(3) 8_656 11_566 ?
I2 I1 I2' 57.1(3) . 11_566 ?
I2 I1 I2' 105.3(3) 11_566 . ?
I2 I1 I2' 45.0(3) . . ?
I2' I1 I2' 70.9(3) 11_566 . ?
I2' I1 I2' 70.9(3) 8_656 . ?
I2' I1 I2' 70.9(3) 11_566 8_656 ?
I1 I2 I3 171.8(5) . . ?
I1 I2 I3' 149.3(6) . . ?
I2' I2 I1 63.5(3) 11_566 . ?
I2' I2 I3 124.5(5) 11_566 . ?
I2' I2 I3' 115.0(5) 11_566 . ?
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
Zn1 O1 C1 O2 11.8(6) 8_656 . . . ?
Zn1 O1 C1 C2 -167.4(3) 8_656 . . . ?
Zn1 O2 C1 O1 -173.9(3) . . . . ?
Zn1 O2 C1 C2 5.4(4) . . . . ?
Zn1 O7 C25 C26 177.0(3) . . . . ?
Zn1 N1 C2 C1 -2.1(4) . . . . ?
Zn1 N1 C2 C3 176.1(3) . . . . ?
Zn1 N1 C6 C5 -176.0(3) . . . . ?
Zn1 N1 C6 C7 4.2(5) . . . . ?
Zn1 N2 C7 N3 160.8(3) . . . . ?
Zn1 N2 C7 C6 -17.9(5) . . . . ?
Zn1 N2 C8 N4 -145.8(4) . . . . ?
Zn1 N2 C8 C9 40.7(6) . . . . ?
Zn2 O7 C25 C26 1.8(6) . . . . ?
Zn2 N6 N7 C10 176.1(3) . . . . ?
Zn2 N6 C9 N5 -175.3(3) . . . . ?
Zn2 N6 C9 C8 -0.3(5) . . . . ?
Zn3 O3 C16 O4 179.8(5) . . . . ?
Zn3 O3 C16 C15 1.4(6) . . . . ?
Zn3 O8 C27 C28 -163.3(6) . . . . ?
Zn3 N5 C9 N6 -157.3(4) . . . . ?
Zn3 N5 C9 C8 28.0(7) . . . . ?
Zn3 N5 C10 N7 167.5(3) . . . . ?
Zn3 N5 C10 C11 -13.7(5) . . . . ?
Zn3 N8 C11 C10 5.3(5) . . . . ?
Zn3 N8 C11 C12 -174.0(4) . . . . ?
Zn3 N8 C15 C14 175.9(4) . . . . ?
Zn3 N8 C15 C16 -5.4(5) . . . . ?
Zn4 O8 C27 C28 18.7(13) . . . . ?
Zn4 O9 C29 C28 -30.5(17) . . . . ?
Zn4 N4 C8 N2 177.5(3) . . . . ?
Zn4 N4 C8 C9 -9.0(6) . . . . ?
Zn5 O5 C17 O6 179.9(19) . . . . ?
Zn5 O5 C17 C18 4(3) . . . . ?
Zn5 O5A C17A O6A -165.8(18) . . . . ?
Zn5 O5A C17A C18 -16(2) . . . . ?
Zn5 O9 C29 C28 165.7(9) 3_656 . . . ?
Zn5 N9 C18 C17 14.1(14) . . . . ?
Zn5 N9 C18 C17A -19.0(16) . . . . ?
Zn5 N9 C18 C19 178.3(8) . . . . ?
Zn5 N9 C22 C21 -177.4(6) . . . . ?
Zn5 N9 C22 C23 1.7(8) . . . . ?
Zn5 N11 N12 N12 31.0(8) . . . 3_656 ?
Zn5 N11 N12 C24 -156.6(5) . . . . ?
Zn5 N11 C23 N10 166.7(4) . . . . ?
Zn5 N11 C23 C22 -14.2(6) . . . . ?
O1 C1 C2 N1 177.0(3) . . . . ?
O1 C1 C2 C3 -1.0(6) . . . . ?
O2 C1 C2 N1 -2.3(5) . . . . ?
O2 C1 C2 C3 179.7(4) . . . . ?
O5 C17 C18 N9 -12(3) . . . . ?
O5 C17 C18 C19 -173.2(18) . . . . ?
O5A C17A C18 N9 23(2) . . . . ?
O5A C17A C18 C19 -174.2(15) . . . . ?
O6 C17 C18 N9 172(2) . . . . ?
O6 C17 C18 C19 11(3) . . . . ?
O6A C17A C18 N9 174.1(18) . . . . ?
O6A C17A C18 C19 -23(3) . . . . ?
O7 C25 C26 C25 -1.1(3) . . . 3_656 ?
O8 C27 C28 C29 -45.0(14) . . . . ?
N1 C2 C3 C4 -0.1(7) . . . . ?
N1 C6 C7 N2 10.8(6) . . . . ?
N1 C6 C7 N3 -167.7(4) . . . . ?
N2 C8 C9 N5 -161.7(4) . . . . ?
N2 C8 C9 N6 24.1(6) . . . . ?
N3 N4 C8 N2 -0.7(5) . . . . ?
N3 N4 C8 C9 172.7(4) . . . . ?
N4 N3 C7 N2 -0.9(5) . . . . ?
N4 N3 C7 C6 177.7(4) . . . . ?
N4 C8 C9 N5 25.5(6) . . . . ?
N4 C8 C9 N6 -148.7(4) . . . . ?
N5 C10 C11 N8 6.9(6) . . . . ?
N5 C10 C11 C12 -173.9(4) . . . . ?
N6 N7 C10 N5 -0.3(4) . . . . ?
N6 N7 C10 C11 -179.0(4) . . . . ?
N7 N6 C9 N5 0.2(4) . . . . ?
N7 N6 C9 C8 175.2(3) . . . . ?
N7 C10 C11 N8 -174.5(4) . . . . ?
N7 C10 C11 C12 4.8(7) . . . . ?
N8 C11 C12 C13 -3.1(7) . . . . ?
N8 C15 C16 O3 2.5(7) . . . . ?
N8 C15 C16 O4 -176.0(5) . . . . ?
N9 C18 C19 C20 2.5(18) . . . . ?
N9 C22 C23 N10 -171.6(6) . . . . ?
N9 C22 C23 N11 9.4(8) . . . . ?
N11 N12 C24 Zn4 -173.9(3) . . . . ?
N11 N12 C24 N10 -0.6(6) . . . . ?
N12 N11 C23 N10 -1.1(6) . . . . ?
N12 N11 C23 C22 178.1(5) . . . . ?
N12 N12 C24 Zn4 -1.3(6) 3_656 . . . ?
N12 N12 C24 N10 172.0(3) 3_656 . . . ?
C1 C2 C3 C4 177.8(5) . . . . ?
C2 N1 C6 C5 -0.5(6) . . . . ?
C2 N1 C6 C7 179.7(4) . . . . ?
C2 C3 C4 C5 -0.2(8) . . . . ?
C3 C4 C5 C6 0.1(8) . . . . ?
C4 C5 C6 N1 0.3(7) . . . . ?
C4 C5 C6 C7 -179.9(5) . . . . ?
C5 C6 C7 N2 -169.0(4) . . . . ?
C5 C6 C7 N3 12.5(8) . . . . ?
C6 N1 C2 C1 -177.7(4) . . . . ?
C6 N1 C2 C3 0.4(6) . . . . ?
C7 N2 C8 N4 0.2(4) . . . . ?
C7 N2 C8 C9 -173.3(4) . . . . ?
C7 N3 N4 Zn4 -177.6(3) . . . . ?
C7 N3 N4 C8 0.9(5) . . . . ?
C8 N2 C7 N3 0.5(5) . . . . ?
C8 N2 C7 C6 -178.2(4) . . . . ?
C9 N5 C10 N7 0.4(5) . . . . ?
C9 N5 C10 C11 179.2(4) . . . . ?
C9 N6 N7 C10 0.1(4) . . . . ?
C10 N5 C9 N6 -0.4(4) . . . . ?
C10 N5 C9 C8 -175.1(4) . . . . ?
C10 C11 C12 C13 177.7(5) . . . . ?
C11 N8 C15 C14 -0.5(7) . . . . ?
C11 N8 C15 C16 178.2(4) . . . . ?
C11 C12 C13 C14 2.3(8) . . . . ?
C12 C13 C14 C15 -0.7(8) . . . . ?
C13 C14 C15 N8 -0.2(8) . . . . ?
C13 C14 C15 C16 -178.7(5) . . . . ?
C14 C15 C16 O3 -178.9(5) . . . . ?
C14 C15 C16 O4 2.6(8) . . . . ?
C15 N8 C11 C10 -178.4(4) . . . . ?
C15 N8 C11 C12 2.3(7) . . . . ?
C17 C18 C19 C20 161.6(18) . . . . ?
C17A C18 C19 C20 -159.5(14) . . . . ?
C18 N9 C22 C21 2.7(12) . . . . ?
C18 N9 C22 C23 -178.1(7) . . . . ?
C18 C19 C20 C21 -3.9(17) . . . . ?
C19 C20 C21 C22 4.4(14) . . . . ?
C20 C21 C22 N9 -3.7(11) . . . . ?
C20 C21 C22 C23 177.2(6) . . . . ?
C21 C22 C23 N10 7.6(10) . . . . ?
C21 C22 C23 N11 -171.5(6) . . . . ?
C22 N9 C18 C17 -166.1(12) . . . . ?
C22 N9 C18 C17A 160.8(13) . . . . ?
C22 N9 C18 C19 -1.9(15) . . . . ?
C23 N10 C24 Zn4 173.9(3) . . . . ?
C23 N10 C24 N12 -0.1(5) . . . . ?
C23 N11 N12 N12 -171.3(3) . . . 3_656 ?
C23 N11 N12 C24 1.0(6) . . . . ?
C24 N10 C23 N11 0.8(6) . . . . ?
C24 N10 C23 C22 -178.3(5) . . . . ?
C27 C28 C29 O9 53.7(18) . . . . ?
_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 -0.590 -0.315 -0.763 107786.0 14043.1 '132 I2'
2 0.000 0.000 0.500 704.8 363.0 '3.5 I2'
3 0.000 0.250 0.750 704.8 363.0 '3.5 I2'
4 0.000 0.500 0.000 704.8 363.0 '3.5 I2'
5 0.000 0.750 0.250 704.8 363.0 '3.5 I2'
6 0.250 0.000 0.750 704.8 363.0 '3.5 I2'
7 0.250 0.250 0.500 704.8 363.0 '3.5 I2'
8 0.250 0.500 0.250 704.8 363.0 '3.5 I2'
9 0.250 0.750 0.000 704.8 363.0 '3.5 I2'
10 0.500 0.250 0.250 704.8 363.0 '3.5 I2'
11 0.500 0.500 0.500 704.8 363.0 '3.5 I2'
12 0.500 0.750 0.750 704.8 363.0 '3.5 I2'
13 0.500 1.000 1.000 704.8 363.0 '3.5 I2'
14 0.750 0.000 0.250 704.8 363.0 '3.5 I2'
15 0.750 0.250 0.000 704.8 363.0 '3.5 I2'
16 0.750 0.500 0.750 704.8 363.0 '3.5 I2'
17 0.750 0.750 0.500 704.8 363.0 '3.5 I2'
_smtbx_masks_void_probe_radius 1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_file
;
TITL zn54-i2_a.res in Fd-3
zn54-i2.res
created by SHELXL-2018/3 at 00:50:05 on 26-Nov-2024
REM Old TITL Zn54-I2 in Fd-3
REM SHELXT solution in Fd-3: R1 0.237, Rweak 0.023, Alpha 0.039
REM 0.376 for 482 systematic absences, Orientation as input
REM Formula found by SHELXT: C219 N48 O62 Zn27
CELL 1.54184 58.9792 58.9792 58.9792 90 90 90
ZERR 8 0.0003 0.0003 0.0003 0 0 0
LATT 4
SYMM 0.25-X,0.25-Y,+Z
SYMM 0.25-X,+Y,0.25-Z
SYMM +X,0.25-Y,0.25-Z
SYMM +Z,+X,+Y
SYMM +Z,0.25-X,0.25-Y
SYMM 0.25-Z,0.25-X,+Y
SYMM 0.25-Z,+X,0.25-Y
SYMM +Y,+Z,+X
SYMM 0.25-Y,+Z,0.25-X
SYMM +Y,0.25-Z,0.25-X
SYMM 0.25-Y,0.25-Z,+X
SFAC C H I N O Zn
UNIT 2784 2304 452.8 1248 950.4 432
EQIV $1 1.25-Z,+X,1.25-Y
EQIV $2 +Y,1.25-Z,1.25-X
EADP I3 I3'
EADP I2 I2'
ISOR 0.01 0.02 C26 C27 C28 C29 I2 I2'
ISOR 0.005 0.01 I3 O10
EADP O5 O5A
EADP C17 C17A
EADP O6 O6A
ISOR 0.01 0.02 O5 O5A C17 C17A O6 O6A
SADI C18 C17 C18 C17A
SADI O5 C17 O5A C17A O6 C17 O6A C17A
DFIX 2.9 I2 I1 I1 I2'
DFIX 1.45 C18 C17 C18 C17A
L.S. 10
PLAN 5
SIZE 0.27 0.26 0.3
TEMP -173.15
CONF
FREE I2' I2
FREE I2' I2_$1
FREE I2' I2'_$1
FREE I2' I2'_$2
list 4
MORE -1
BOND $H
ABIN
fmap 2 53
acta
OMIT 2 2 6
OMIT 2 6 16
OMIT 3 5 11
OMIT 3 9 9
OMIT 4 8 10
OMIT 5 3 11
OMIT 6 6 6
OMIT 7 3 15
REM
REM
REM
WGHT 0.163100
FVAR 0.02895 0.49572
ZN1 6 0.587036 0.524021 0.664815 11.00000 0.05895 0.05596 =
0.05598 0.00435 0.00135 0.00079
ZN2 6 0.625000 0.516346 0.625000 10.50000 0.05438 0.04709 =
0.05383 0.00000 -0.00438 0.00000
ZN3 6 0.555022 0.447612 0.579372 11.00000 0.06633 0.09731 =
0.07258 -0.01130 -0.01225 -0.01662
ZN4 6 0.574091 0.423740 0.625761 11.00000 0.09686 0.06150 =
0.08930 -0.00530 -0.01953 -0.01709
ZN5 6 0.667445 0.389383 0.581078 11.00000 0.15053 0.13476 =
0.14487 -0.05482 -0.02815 0.04604
O1 5 0.591775 0.553979 0.728238 11.00000 0.07892 0.06205 =
0.05608 -0.00061 0.00164 -0.00105
O2 5 0.590880 0.549460 0.690699 11.00000 0.07248 0.05351 =
0.05681 0.00240 0.00307 0.00026
O3 5 0.541132 0.427154 0.552726 11.00000 0.08575 0.12402 =
0.07701 -0.01755 -0.02071 -0.03253
O4 5 0.542607 0.420765 0.515356 11.00000 0.10897 0.13484 =
0.08618 -0.03205 -0.01924 -0.03779
PART 1
O5 5 0.688500 0.377439 0.556044 21.00000 0.13741 0.16050 =
0.16896 -0.01593 0.01888 0.03371
PART 2
O5A 5 0.694156 0.388698 0.551374 -21.00000 0.13741 0.16050 =
0.16896 -0.01593 0.01888 0.03371
PART 1
O6 5 0.692999 0.378220 0.518807 21.00000 0.20124 0.26107 =
0.17480 -0.02566 0.05439 0.01864
PART 2
O6A 5 0.696922 0.394534 0.514201 -21.00000 0.20124 0.26107 =
0.17480 -0.02566 0.05439 0.01864
PART 0
O7 5 0.606860 0.537062 0.642793 11.00000 0.07305 0.04810 =
0.06462 0.00296 0.01147 0.00152
O8 5 0.549687 0.427432 0.604194 11.00000 0.08813 0.09054 =
0.09751 -0.00301 -0.01599 -0.02884
O9 5 0.562716 0.402001 0.647193 10.90000 0.11444 0.08050 =
0.13314 0.02311 -0.01773 -0.03602
O10 5 0.658810 0.354485 0.589471 11.00000 0.22378 0.14093 =
0.27472 -0.05000 -0.03348 0.06755
AFIX 7
H10A 2 0.656821 0.346967 0.605631 11.00000 -1.50000
H10B 2 0.655418 0.340593 0.578572 11.00000 -1.50000
AFIX 0
N1 4 0.590134 0.505236 0.694100 11.00000 0.06156 0.05804 =
0.05880 0.00425 0.00117 0.00144
N2 4 0.590917 0.487573 0.652577 11.00000 0.06163 0.05250 =
0.05828 0.00232 -0.00194 -0.00028
N3 4 0.582592 0.452404 0.665618 11.00000 0.09763 0.05393 =
0.06835 0.00438 -0.00550 -0.01491
N4 4 0.582242 0.452304 0.642197 11.00000 0.08114 0.05905 =
0.07440 0.00324 -0.01109 -0.01483
N5 4 0.582949 0.468792 0.593632 11.00000 0.05682 0.06810 =
0.06229 -0.00684 -0.00796 -0.00669
N6 4 0.605718 0.496053 0.605919 11.00000 0.06520 0.05744 =
0.05091 -0.00079 -0.00603 -0.00333
N7 4 0.607066 0.496527 0.582674 11.00000 0.06894 0.06309 =
0.05944 0.00008 -0.01118 -0.00139
N8 4 0.572623 0.457646 0.551215 11.00000 0.06497 0.08907 =
0.06676 -0.01098 -0.01892 -0.00175
N9 4 0.650532 0.401521 0.552472 11.00000 0.15500 0.13248 =
0.11086 -0.04123 -0.00870 0.01982
N10 4 0.600478 0.415775 0.583538 11.00000 0.12122 0.07337 =
0.08945 -0.01693 -0.02059 0.00231
N11 4 0.635635 0.405678 0.594980 11.00000 0.11087 0.07891 =
0.09125 -0.01424 -0.00826 0.01116
N12 4 0.621424 0.408776 0.612948 11.00000 0.15924 0.06938 =
0.11167 -0.00437 -0.02962 -0.00626
N13 4 0.530046 0.471683 0.583053 11.00000 0.06637 0.10643 =
0.11868 0.02021 -0.01453 -0.00907
AFIX 13
H13 2 0.515069 0.464099 0.580674 11.00000 -1.20000
AFIX 0
C1 1 0.591477 0.542352 0.710498 11.00000 0.06081 0.06007 =
0.05939 -0.00238 0.00402 -0.00266
C2 1 0.591576 0.516807 0.713717 11.00000 0.07332 0.06410 =
0.05493 0.00293 0.00460 0.00448
C3 1 0.592305 0.505362 0.734259 11.00000 0.10543 0.06514 =
0.05811 0.00015 -0.00270 0.00059
AFIX 43
H3 2 0.593341 0.513430 0.748162 11.00000 -1.20000
AFIX 0
C4 1 0.591490 0.482061 0.734012 11.00000 0.12741 0.07170 =
0.06274 0.01478 -0.00044 0.00146
AFIX 43
H4 2 0.592008 0.473928 0.747906 11.00000 -1.20000
AFIX 0
C5 1 0.589931 0.470370 0.713832 11.00000 0.11533 0.05445 =
0.07091 0.01013 0.00396 -0.00718
AFIX 43
H5 2 0.589352 0.454274 0.713630 11.00000 -1.20000
AFIX 0
C6 1 0.589225 0.482806 0.693690 11.00000 0.07472 0.05198 =
0.06261 0.00497 -0.00019 -0.00435
C7 1 0.587593 0.473606 0.671016 11.00000 0.07453 0.05421 =
0.06777 0.00709 -0.00443 -0.00138
C8 1 0.587400 0.473343 0.635292 11.00000 0.05713 0.05031 =
0.06501 0.00159 -0.00659 -0.00276
C9 1 0.591283 0.479485 0.611667 11.00000 0.05412 0.05428 =
0.06239 -0.00412 -0.00902 -0.00108
C10 1 0.593176 0.480049 0.576140 11.00000 0.06474 0.06487 =
0.06305 -0.00544 -0.01843 -0.00245
C11 1 0.588767 0.473296 0.552722 11.00000 0.07166 0.07331 =
0.07039 -0.00565 -0.01828 -0.00123
C12 1 0.599318 0.481707 0.533796 11.00000 0.09194 0.08381 =
0.06632 -0.00505 -0.01237 -0.00896
AFIX 43
H12 2 0.610307 0.493420 0.535019 11.00000 -1.20000
AFIX 0
C13 1 0.593491 0.472578 0.512445 11.00000 0.09692 0.09975 =
0.06217 -0.00548 -0.01160 -0.00128
AFIX 43
H13A 2 0.600894 0.477665 0.499074 11.00000 -1.20000
AFIX 0
C14 1 0.576723 0.456004 0.511301 11.00000 0.09095 0.10594 =
0.06713 -0.01879 -0.02299 -0.00731
AFIX 43
H14 2 0.572373 0.449703 0.497129 11.00000 -1.20000
AFIX 0
C15 1 0.566487 0.448861 0.531225 11.00000 0.08123 0.09348 =
0.06753 -0.01404 -0.02075 -0.00253
C16 1 0.548516 0.430936 0.533270 11.00000 0.07175 0.11083 =
0.08094 -0.02126 -0.01538 -0.01940
PART 1
C17 1 0.681240 0.384510 0.536139 21.00000 0.16433 0.17007 =
0.15404 -0.01132 0.01236 0.00882
PART 2
C17A 1 0.686603 0.397578 0.532792 -21.00000 0.16433 0.17007 =
0.15404 -0.01132 0.01236 0.00882
PART 0
C18 1 0.661235 0.400377 0.532376 11.00000 0.15778 0.22316 =
0.11612 -0.06465 -0.00788 0.01555
C19 1 0.650349 0.407646 0.513282 11.00000 0.17661 0.19183 =
0.11642 -0.05348 0.01496 0.01957
AFIX 43
H19 2 0.657576 0.406328 0.498947 11.00000 -1.20000
AFIX 0
C20 1 0.631021 0.415985 0.514558 11.00000 0.17812 0.14966 =
0.10174 -0.02468 0.00088 0.00040
AFIX 43
H20 2 0.624221 0.421772 0.501152 11.00000 -1.20000
AFIX 0
C21 1 0.618468 0.417245 0.535555 11.00000 0.16425 0.12696 =
0.09204 -0.02217 -0.01373 0.01206
AFIX 43
H21 2 0.603318 0.422661 0.536317 11.00000 -1.20000
AFIX 0
C22 1 0.630013 0.410095 0.554056 11.00000 0.13174 0.09588 =
0.09626 -0.03305 -0.01443 0.01284
C23 1 0.621580 0.410528 0.577491 11.00000 0.12278 0.06791 =
0.09895 -0.01763 -0.02005 0.00412
C24 1 0.600558 0.414587 0.607034 11.00000 0.08285 0.05407 =
0.07561 -0.01018 -0.02453 0.00088
C25 1 0.609561 0.560436 0.640600 11.00000 0.10093 0.05040 =
0.08144 0.00143 0.03008 0.00450
AFIX 23
H25A 2 0.594517 0.566874 0.636862 11.00000 -1.20000
H25B 2 0.613811 0.566412 0.655699 11.00000 -1.20000
AFIX 0
C26 1 0.625000 0.569136 0.625000 10.50000 0.17550 0.06735 =
0.17457 0.00000 0.08461 0.00000
AFIX 23
H26A 2 0.634470 0.579346 0.634372 10.50000 -1.20000
H26B 2 0.615530 0.579346 0.615628 10.50000 -1.20000
AFIX 0
PART 2
C27 1 0.529816 0.415511 0.606398 10.50000 0.08715 0.10372 =
0.10038 0.01103 -0.00551 -0.03470
AFIX 23
H27A 2 0.530112 0.403205 0.594986 10.50000 -1.20000
H27B 2 0.517315 0.425848 0.602083 10.50000 -1.20000
AFIX 0
C28 1 10.523690 10.405250 10.628091 10.50000 0.18969 0.20291 =
0.19321 0.02662 -0.00501 -0.03931
AFIX 23
H28A 2 0.517927 0.417510 0.638001 10.50000 -1.20000
H28B 2 0.510860 0.394802 0.625264 10.50000 -1.20000
AFIX 0
C29 1 0.540738 0.392740 0.640934 10.50000 0.12186 0.13394 =
0.14503 0.02473 -0.00983 -0.03629
AFIX 23
H29A 2 0.533350 0.387998 0.655241 10.50000 -1.20000
H29B 2 0.543812 0.378686 0.632286 10.50000 -1.20000
AFIX 0
PART 0
C30 1 0.530129 0.482402 0.607862 11.00000 0.11172 0.19588 =
0.12034 -0.04331 -0.02144 0.04032
AFIX 137
H30A 2 0.541345 0.494640 0.608570 11.00000 -1.50000
H30B 2 0.534032 0.470663 0.618955 11.00000 -1.50000
H30C 2 0.515060 0.488493 0.611313 11.00000 -1.50000
AFIX 0
C31 1 0.531187 0.490701 0.568302 11.00000 0.11883 0.23858 =
0.17695 0.02583 0.00585 0.02656
AFIX 137
H31A 2 0.515956 0.494308 0.562727 11.00000 -1.50000
H31B 2 0.541095 0.487151 0.555444 11.00000 -1.50000
H31C 2 0.537298 0.503759 0.576563 11.00000 -1.50000
AFIX 0
I1 3 0.528106 0.528106 0.721894 10.26666 0.23357 0.23357 =
0.23357 0.03874 0.03874 -0.03874
I2 3 0.526372 0.485869 0.711368 10.13333 0.20779 0.25544 =
0.31778 0.05092 0.02092 -0.01278
I2' 3 0.531685 0.489228 0.744776 10.13333 0.20779 0.25544 =
0.31778 0.05092 0.02092 -0.01278
PART 1
I3 3 0.531186 0.439068 0.697715 10.13333 0.28978 0.32373 =
0.35520 0.03770 0.02202 -0.02675
PART 2
I3' 3 0.525510 0.452860 0.678737 10.13333 0.28978 0.32373 =
0.35520 0.03770 0.02202 -0.02675
HKLF 4
REM zn54-i2_a.res in Fd-3
REM wR2 = 0.2336, GooF = S = 1.001, Restrained GooF = 1.030 for all data
REM R1 = 0.0672 for 10617 Fo > 4sig(Fo) and 0.0865 for all 16367 data
REM 561 parameters refined using 95 restraints
END
WGHT 0.1631 0.0000
REM Highest difference peak 0.881, deepest hole -1.425, 1-sigma level 0.083
Q1 1 0.5282 0.5283 0.7398 11.00000 0.05 0.88
Q2 1 0.5798 0.4231 0.6800 11.00000 0.05 0.60
Q3 1 0.5182 0.5022 0.7272 11.00000 0.05 0.56
Q4 1 0.5298 0.4961 0.7147 11.00000 0.05 0.53
Q5 1 0.5249 0.4615 0.6908 11.00000 0.05 0.51
;
_shelx_res_checksum 90428
_shelx_fab_file
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36 42 38 18.4891 0.7522
36 42 40 44.8073 -0.8321
36 42 42 -17.6779 -0.2555
36 42 44 16.0379 -0.7298
36 42 46 -4.8190 -0.7533
36 42 48 -2.6882 -1.0605
36 44 36 36.4135 0.2213
36 44 38 -3.2086 -0.0268
36 44 40 25.2304 -0.5180
36 44 44 -34.2150 -0.2289
36 44 46 17.0491 -1.0928
36 46 36 21.2414 -1.4602
36 46 38 -16.4518 1.0901
36 46 40 -4.3753 -1.4667
36 46 42 -28.6421 -0.3583
36 46 44 -2.7259 -1.3445
36 48 36 -15.9900 0.2445
36 48 38 3.9441 -1.1025
36 48 40 6.7205 0.7752
36 48 42 19.5047 -0.7802
36 50 36 -23.6884 -0.6099
36 50 38 6.0764 0.8527
36 50 40 -1.2768 -1.3737
36 52 36 18.3276 -0.2365
36 52 38 22.0644 0.0686
36 54 36 -43.2800 -2.0639
37 37 37 -4.7533 -1.1118
37 39 37 -11.1957 -0.2474
37 39 39 -2.9213 -0.8250
37 39 41 -11.2996 -0.3451
37 39 43 -8.4625 -0.7026
37 41 37 9.1440 -1.0000
37 41 39 -4.3853 0.2490
37 41 41 59.6746 -0.0572
37 41 45 -13.2957 0.6153
37 41 47 35.6769 0.8656
37 41 49 6.0511 0.8269
37 43 37 -14.9336 -0.7808
37 43 39 24.9808 -0.8275
37 43 43 -19.7169 -0.6699
37 43 45 19.8283 1.6309
37 43 47 24.8096 0.6248
37 45 43 13.6964 0.9728
37 45 45 -11.6405 0.8380
37 47 39 13.3052 0.0924
37 47 41 5.4773 0.9563
37 47 43 6.2832 0.3502
37 49 37 6.5552 0.1072
37 49 39 -17.1359 -0.2124
37 49 41 17.6811 -0.0387
37 51 37 11.5615 0.5094
37 51 39 -21.4759 -1.5150
38 38 38 -6.3341 1.0234
38 40 38 -14.1333 1.6393
38 40 40 25.1817 -0.7413
38 42 38 13.1353 0.1785
38 42 40 2.2039 0.8514
38 42 44 30.5218 -0.0066
38 42 46 25.8495 -0.8475
38 42 48 -9.0189 0.9839
38 44 38 18.7055 1.5819
38 44 42 -3.2252 0.5558
38 44 44 -13.4769 -0.2451
38 44 46 -20.6844 -0.9137
38 46 40 -8.0544 0.9746
38 46 42 -6.7968 -0.3648
38 46 44 -21.4050 -0.0220
38 48 38 10.9849 1.1514
38 48 40 -4.5091 -0.5684
38 48 42 14.6381 0.4631
39 39 39 -11.7686 0.9325
39 41 39 14.2692 -0.9124
39 41 45 -4.1147 -0.0284
39 41 47 9.5265 -1.2869
39 43 43 -1.2453 0.2454
39 43 45 0.2490 -0.7958
39 45 41 -46.7148 0.2526
39 45 43 -23.6639 -0.5390
39 47 39 -20.8766 -0.6282
39 47 41 -27.8378 -1.0567
40 42 44 -9.8431 -0.0472
40 42 46 28.3984 2.1428
40 44 42 -57.8569 -0.8966
40 44 44 -1.6824 0.4989
40 46 40 -29.6424 -0.3856
40 48 40 36.5131 1.0107
41 43 43 -11.1499 -1.9112
41 45 41 -26.6125 -1.1346
42 42 42 -0.5266 -0.5569
42 44 42 21.5477 2.2801
0 0 0 0.0 0.0
;
_shelx_fab_checksum 19917
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.775
# start Validation Reply Form
_vrf_PLAT260_zn54-i2
;
PROBLEM: Large Average Ueq of Residue Including I3 0.323 Check
RESPONSE: This is due to the presence of severely disordered iodine species.
;
_vrf_PLAT420_zn54-i2
;
PROBLEM: D-H Bond Without Acceptor O10 --H10A . Please Check
RESPONSE: The solvent molecules are highly disordered, which supposed to
form hydrogen bond with water molecules have been removed
by the SQUEEZE routine.
;
# end Validation Reply Form
#######################################################################
#
# 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_20200607-hfp-ty-zn54_sq
_audit_block_doi 10.5517/ccdc.csd.cc2j05vl
_database_code_depnum_ccdc_archive 'CCDC 2323879'
loop_
_audit_author_name
_audit_author_address
'Tao Ye'
;Guangxi Normal University
China
;
_audit_update_record
;
2024-11-25 deposited with the CCDC. 2024-12-06 downloaded from the CCDC.
;
_audit_creation_date 2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C385.2 H367.2 N165.6 O108 Zn54, 16[C3H8O2], 30[C3H7NO]'
_chemical_formula_sum 'C523.20 H705.20 N195.61 O170.00 Zn54'
_chemical_formula_weight 15985.07
_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'
Zn Zn -1.5491 0.6778 '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 203
_space_group_name_H-M_alt 'F d -3'
_space_group_name_Hall '-F 2uv 2vw 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/4, -z+1/4, x'
'z, -x+1/4, -y+1/4'
'-y+1/4, z, -x+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, -z+1/4, -x+1/4'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y+1/4, -z+3/4, x+1/2'
'z, -x+3/4, -y+3/4'
'-y+1/4, z+1/2, -x+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, -z+3/4, -x+3/4'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+3/4, -z+1/4, x+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-y+3/4, z, -x+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+3/4, -z+3/4, x'
'z+1/2, -x+3/4, -y+1/4'
'-y+3/4, z+1/2, -x+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y-1/4, z-1/4, -x'
'-z, x-1/4, y-1/4'
'y-1/4, -z, x-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, z-1/4, x-1/4'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y-1/4, z+1/4, -x+1/2'
'-z, x+1/4, y+1/4'
'y-1/4, -z+1/2, x+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, z+1/4, x+1/4'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/4, z-1/4, -x+1/2'
'-z+1/2, x-1/4, y+1/4'
'y+1/4, -z, x+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, z-1/4, x+1/4'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/4, z+1/4, -x'
'-z+1/2, x+1/4, y-1/4'
'y+1/4, -z+1/2, x-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, z+1/4, x-1/4'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
_cell_length_a 58.3017(2)
_cell_length_b 58.3017(2)
_cell_length_c 58.3017(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 198173(2)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 26694
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 76.7670
_cell_measurement_theta_min 2.5040
_shelx_estimated_absorpt_T_max 0.598
_shelx_estimated_absorpt_T_min 0.539
_exptl_absorpt_coefficient_mu 1.908
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80498
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.072
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description Octahedron
_exptl_crystal_F_000 65550
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.3
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0253
_diffrn_reflns_av_unetI/netI 0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max 68
_diffrn_reflns_limit_h_min -64
_diffrn_reflns_limit_k_max 69
_diffrn_reflns_limit_k_min -52
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -64
_diffrn_reflns_number 61406
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full 67.068
_diffrn_reflns_theta_max 67.068
_diffrn_reflns_theta_min 2.514
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -39.00 18.00 0.50 30.00 -- -46.87 48.00 79.00 114
2 \w -48.00 -15.00 0.50 100.00 -- -88.50 48.00 79.00 66
3 \w -120.00 -89.00 0.50 30.00 -- -46.87-125.00-150.00 62
4 \w 44.00 69.00 0.50 100.00 -- 108.56 -61.00-150.00 50
5 \w 39.00 65.00 0.50 100.00 -- 108.56 -61.00 -30.00 52
6 \w 38.00 66.00 0.50 100.00 -- 108.56 -61.00 90.00 56
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0192307000
_diffrn_orient_matrix_UB_12 -0.0161813000
_diffrn_orient_matrix_UB_13 -0.0082583000
_diffrn_orient_matrix_UB_21 -0.0177846000
_diffrn_orient_matrix_UB_22 0.0191477000
_diffrn_orient_matrix_UB_23 0.0038267000
_diffrn_orient_matrix_UB_31 0.0036404000
_diffrn_orient_matrix_UB_32 0.0083226000
_diffrn_orient_matrix_UB_33 -0.0247897000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12642
_reflns_number_total 14575
_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 'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection 'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction 'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max 0.488
_refine_diff_density_min -0.338
_refine_diff_density_rms 0.062
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.012
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 554
_refine_ls_number_reflns 14575
_refine_ls_number_restraints 42
_refine_ls_R_factor_all 0.0434
_refine_ls_R_factor_gt 0.0390
_refine_ls_restrained_S_all 1.050
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+263.6934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1259
_refine_ls_wR_factor_ref 0.1288
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
N14-C32 = N14-C33 = N14-C33'
1.5 with sigma of 0.02
N14-C32 \\sim N14-C33' \\sim N14-C33
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C33')
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C33') = Uanis(C33)
4. Others
Fixed Sof: N14(0.8) H14(0.4) H14a(0.4) C29(0.5) H29a(0.5) H29b(0.5) C32(0.8)
H32a(0.8) H32b(0.8) H32c(0.8) C33(0.4) H33a(0.4) H33b(0.4) H33c(0.4) C33'(0.4)
H33d(0.4) H33e(0.4) H33f(0.4)
Fixed X: H28a(0.65534) H28b(0.63601)
Fixed Y: H28a(0.56641) H28b(0.56624)
Fixed Z: H28a(0.61363) H28b(0.59454)
5.a Ternary CH refined with riding coordinates:
N13(H13), N14(H14), N14(H14a)
5.b Secondary CH2 refined with riding coordinates:
C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b), C29(H29a,H29b)
5.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C12(H12), C13(H13a), C14(H14b), C19(H19), C20(H20),
C21(H21)
5.d Idealised Me refined as rotating group:
C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C33(H33a,H33b,
H33c), C33'(H33d,H33e,H33f)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
Zn1 Zn 0.58685(2) 0.52261(2) 0.66549(2) 0.04391(9) Uani 1 1 d . . . . .
Zn2 Zn 0.625000 0.51550(2) 0.625000 0.03948(10) Uani 1 2 d S T P . .
Zn3 Zn 0.55439(2) 0.44540(2) 0.58030(2) 0.05489(10) Uani 1 1 d . . . . .
Zn4 Zn 0.57469(2) 0.42091(2) 0.62663(2) 0.05398(10) Uani 1 1 d . . . . .
Zn5 Zn 0.58186(2) 0.38371(2) 0.66914(2) 0.08989(16) Uani 1 1 d . . . . .
O1 O 0.59046(3) 0.55333(3) 0.72987(3) 0.0518(4) Uani 1 1 d . . . . .
O2 O 0.59041(3) 0.54855(3) 0.69184(3) 0.0505(4) Uani 1 1 d . . . . .
O3 O 0.54095(3) 0.42334(3) 0.55433(3) 0.0655(5) Uani 1 1 d . . . . .
O4 O 0.54337(4) 0.41482(4) 0.51701(3) 0.0846(6) Uani 1 1 d . . . . .
O5 O 0.55223(7) 0.38221(10) 0.73383(7) 0.1845(19) Uani 1 1 d . U . . .
O6 O 0.55765(5) 0.37678(6) 0.69563(6) 0.1281(11) Uani 1 1 d . U . . .
O7 O 0.54919(3) 0.42589(3) 0.60605(3) 0.0616(4) Uani 1 1 d . . . . .
O8 O 0.56226(3) 0.39797(3) 0.64696(4) 0.0725(5) Uani 1 1 d . . . . .
O9 O 0.64327(3) 0.53605(2) 0.60679(3) 0.0458(3) Uani 1 1 d . . . . .
N1 N 0.59011(3) 0.50402(3) 0.69533(3) 0.0464(4) Uani 1 1 d . . . . .
N2 N 0.59076(3) 0.48567(3) 0.65363(3) 0.0431(4) Uani 1 1 d . . . . .
N3 N 0.58380(3) 0.44992(3) 0.66668(3) 0.0508(4) Uani 1 1 d . . . . .
N4 N 0.58360(3) 0.44968(3) 0.64311(3) 0.0493(4) Uani 1 1 d . . . . .
N5 N 0.58304(3) 0.46655(3) 0.59384(3) 0.0483(4) Uani 1 1 d . . . . .
N6 N 0.60543(3) 0.49483(3) 0.60608(3) 0.0437(4) Uani 1 1 d . . . . .
N7 N 0.60644(3) 0.49528(3) 0.58256(3) 0.0485(4) Uani 1 1 d . . . . .
N8 N 0.57221(3) 0.45483(4) 0.55163(3) 0.0553(5) Uani 1 1 d . . . . .
N9 N 0.59797(5) 0.39695(5) 0.69748(5) 0.0856(8) Uani 1 1 d . . . . .
N10 N 0.61415(4) 0.40129(4) 0.65484(4) 0.0625(5) Uani 1 1 d . . . . .
N11 N 0.64899(4) 0.41325(4) 0.66709(4) 0.0605(5) Uani 1 1 d . . . . .
N12 N 0.64920(4) 0.41143(3) 0.64362(4) 0.0573(5) Uani 1 1 d . . . . .
N13 N 0.52921(4) 0.47034(4) 0.58462(4) 0.0672(6) Uani 1 1 d . . . . .
H13 H 0.514139 0.462502 0.582247 0.081 Uiso 1 1 calc R U . . .
N14 N 0.58963(9) 0.35105(7) 0.66123(10) 0.1095(13) Uani 0.8 1 d D U P . .
H14 H 0.603668 0.346482 0.669958 0.131 Uiso 0.4 1 calc R U P A 1
H14A H 0.576446 0.341054 0.665748 0.131 Uiso 0.4 1 calc R U P B 2
C1 C 0.59066(4) 0.54125(4) 0.71175(4) 0.0489(5) Uani 1 1 d . . . . .
C2 C 0.59120(4) 0.51554(4) 0.71517(4) 0.0496(5) Uani 1 1 d . . . . .
C3 C 0.59206(5) 0.50409(4) 0.73610(4) 0.0560(6) Uani 1 1 d . . . . .
H3 H 0.592958 0.512365 0.750112 0.067 Uiso 1 1 calc R U . . .
C4 C 0.59157(5) 0.48044(4) 0.73600(4) 0.0604(6) Uani 1 1 d . . . . .
H4 H 0.592247 0.472251 0.750072 0.073 Uiso 1 1 calc R U . . .
C5 C 0.59009(5) 0.46858(4) 0.71544(4) 0.0567(6) Uani 1 1 d . . . . .
H5 H 0.589526 0.452293 0.715224 0.068 Uiso 1 1 calc R U . . .
C6 C 0.58946(4) 0.48106(4) 0.69518(4) 0.0480(5) Uani 1 1 d . . . . .
C7 C 0.58809(4) 0.47167(4) 0.67192(4) 0.0458(5) Uani 1 1 d . . . . .
C8 C 0.58792(3) 0.47126(4) 0.63605(4) 0.0431(5) Uani 1 1 d . . . . .
C9 C 0.59144(4) 0.47753(4) 0.61219(4) 0.0432(5) Uani 1 1 d . . . . .
C10 C 0.59297(4) 0.47809(4) 0.57624(4) 0.0489(5) Uani 1 1 d . . . . .
C11 C 0.58831(4) 0.47107(4) 0.55267(4) 0.0541(5) Uani 1 1 d . . . . .
C12 C 0.59917(5) 0.47894(5) 0.53297(4) 0.0614(6) Uani 1 1 d . . . . .
H12 H 0.610566 0.490560 0.533760 0.074 Uiso 1 1 calc R U . . .
C13 C 0.59293(5) 0.46935(5) 0.51212(5) 0.0692(7) Uani 1 1 d . . . . .
H13A H 0.599892 0.474536 0.498328 0.083 Uiso 1 1 calc R U . . .
C14 C 0.57640(5) 0.45208(5) 0.51143(5) 0.0692(7) Uani 1 1 d . . . . .
H14B H 0.572153 0.445257 0.497258 0.083 Uiso 1 1 calc R U . . .
C15 C 0.56634(5) 0.44505(5) 0.53159(4) 0.0613(6) Uani 1 1 d . . . . .
C16 C 0.54861(5) 0.42623(5) 0.53437(5) 0.0671(7) Uani 1 1 d . . . . .
C17 C 0.56343(9) 0.38424(10) 0.71558(10) 0.1285(16) Uani 1 1 d . U . . .
C18 C 0.58672(7) 0.39576(8) 0.71758(7) 0.1064(13) Uani 1 1 d . . . . .
C19 C 0.59650(8) 0.40394(8) 0.73724(7) 0.1085(14) Uani 1 1 d . . . . .
H19 H 0.588582 0.402839 0.751438 0.130 Uiso 1 1 calc R U . . .
C20 C 0.61792(7) 0.41379(7) 0.73629(6) 0.0928(11) Uani 1 1 d . . . . .
H20 H 0.624825 0.419730 0.749799 0.111 Uiso 1 1 calc R U . . .
C21 C 0.62931(6) 0.41499(6) 0.71558(5) 0.0806(9) Uani 1 1 d . . . . .
H21 H 0.644186 0.421568 0.714613 0.097 Uiso 1 1 calc R U . . .
C22 C 0.61855(5) 0.40636(5) 0.69624(5) 0.0710(7) Uani 1 1 d . . . . .
C23 C 0.62783(5) 0.40713(5) 0.67282(5) 0.0618(6) Uani 1 1 d . . . . .
C24 C 0.62824(5) 0.40448(4) 0.63705(5) 0.0591(6) Uani 1 1 d . . . . .
C25 C 0.52888(5) 0.41274(6) 0.60785(6) 0.0811(9) Uani 1 1 d . . . . .
H25A H 0.530071 0.399427 0.597377 0.097 Uiso 1 1 calc R U . . .
H25B H 0.515786 0.422219 0.602631 0.097 Uiso 1 1 calc R U . . .
C26 C 0.52404(7) 0.40442(9) 0.63082(8) 0.1178(16) Uani 1 1 d . . . . .
H26A H 0.509040 0.396502 0.630102 0.141 Uiso 1 1 calc R U . . .
H26B H 0.521850 0.418108 0.640624 0.141 Uiso 1 1 calc R U . . .
C27 C 0.53963(7) 0.38921(8) 0.64308(8) 0.1064(13) Uani 1 1 d . . . . .
H27A H 0.532703 0.385451 0.658118 0.128 Uiso 1 1 calc R U . . .
H27B H 0.540942 0.374718 0.634321 0.128 Uiso 1 1 calc R U . . .
C28 C 0.64061(5) 0.56006(4) 0.60934(5) 0.0617(7) Uani 1 1 d . . . . .
C29 C 0.63340(11) 0.56710(9) 0.63258(11) 0.0764(18) Uani 0.5 1 d . . P . .
H29A H 0.634420 0.584025 0.633436 0.092 Uiso 0.5 1 calc R U P . .
H29B H 0.644656 0.560832 0.643641 0.092 Uiso 0.5 1 calc R U P . .
C30 C 0.52888(6) 0.47965(7) 0.60839(7) 0.0971(12) Uani 1 1 d . . . . .
H30A H 0.528529 0.466941 0.619382 0.146 Uiso 1 1 calc R U . . .
H30B H 0.515222 0.489230 0.610462 0.146 Uiso 1 1 calc R U . . .
H30C H 0.542664 0.488915 0.610970 0.146 Uiso 1 1 calc R U . . .
C31 C 0.53028(8) 0.48927(9) 0.56761(9) 0.1292(18) Uani 1 1 d . . . . .
H31A H 0.543511 0.499079 0.570967 0.194 Uiso 1 1 calc R U . . .
H31B H 0.516183 0.498387 0.568481 0.194 Uiso 1 1 calc R U . . .
H31C H 0.531847 0.482841 0.552160 0.194 Uiso 1 1 calc R U . . .
C32 C 0.59370(16) 0.34812(11) 0.63850(16) 0.176(3) Uani 0.8 1 d D U P C .
H32A H 0.579513 0.350737 0.629881 0.265 Uiso 0.8 1 calc R U P . .
H32B H 0.599120 0.332448 0.635756 0.265 Uiso 0.8 1 calc R U P . .
H32C H 0.605423 0.359065 0.633454 0.265 Uiso 0.8 1 calc R U P . .
C33 C 0.6098(3) 0.3435(3) 0.6734(4) 0.216(6) Uani 0.4 1 d D . P C 2
H33A H 0.623491 0.349973 0.666147 0.325 Uiso 0.4 1 calc R U P C 2
H33B H 0.610629 0.326713 0.673000 0.325 Uiso 0.4 1 calc R U P C 2
H33C H 0.608949 0.348667 0.689391 0.325 Uiso 0.4 1 calc R U P C 2
H28A H 0.655341 0.566409 0.613630 0.260 Uiso 1 1 d . U . D 2
H28B H 0.636009 0.566240 0.594540 0.260 Uiso 1 1 d . U . E 2
C33' C 0.5715(3) 0.3349(3) 0.6662(4) 0.216(6) Uani 0.4 1 d D U P C 1
H33D H 0.578204 0.319639 0.668806 0.325 Uiso 0.4 1 calc R U P C 1
H33E H 0.560864 0.334193 0.653283 0.325 Uiso 0.4 1 calc R U P C 1
H33F H 0.563302 0.339762 0.680051 0.325 Uiso 0.4 1 calc R U P C 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.04619(16) 0.04307(16) 0.04248(16) 0.00294(11) 0.00057(11) 0.00192(12)
Zn2 0.0391(2) 0.0375(2) 0.0418(2) 0.000 -0.00329(15) 0.000
Zn3 0.04638(17) 0.0665(2) 0.05177(18) -0.00878(14) -0.00807(13) -0.00828(14)
Zn4 0.05430(19) 0.04744(18) 0.0602(2) -0.00365(13) -0.00848(14) -0.01022(13)
Zn5 0.0859(3) 0.0845(3) 0.0993(3) 0.0341(2) -0.0149(2) -0.0234(2)
O1 0.0636(10) 0.0481(8) 0.0437(8) -0.0027(7) 0.0002(7) 0.0005(7)
O2 0.0640(10) 0.0437(8) 0.0439(8) 0.0008(6) 0.0022(7) 0.0002(7)
O3 0.0538(10) 0.0842(13) 0.0583(11) -0.0144(9) -0.0095(8) -0.0158(9)
O4 0.0873(14) 0.1059(16) 0.0605(11) -0.0223(11) -0.0099(10) -0.0333(12)
O5 0.138(3) 0.289(5) 0.127(3) 0.078(3) 0.032(2) -0.045(3)
O6 0.1070(19) 0.162(3) 0.115(2) 0.0502(19) -0.0005(17) -0.0434(18)
O7 0.0501(9) 0.0718(11) 0.0628(10) -0.0032(8) -0.0089(8) -0.0164(8)
O8 0.0694(12) 0.0644(11) 0.0836(13) 0.0111(10) -0.0119(10) -0.0231(9)
O9 0.0507(8) 0.0372(7) 0.0494(8) -0.0019(6) 0.0044(6) -0.0011(6)
N1 0.0522(10) 0.0438(10) 0.0433(9) 0.0004(8) -0.0008(8) 0.0014(8)
N2 0.0423(9) 0.0425(9) 0.0445(9) -0.0007(7) -0.0036(7) 0.0008(7)
N3 0.0571(11) 0.0471(10) 0.0481(10) 0.0016(8) -0.0026(8) -0.0045(8)
N4 0.0526(11) 0.0467(10) 0.0485(10) 0.0007(8) -0.0060(8) -0.0066(8)
N5 0.0462(10) 0.0500(10) 0.0487(10) -0.0033(8) -0.0082(8) -0.0058(8)
N6 0.0422(9) 0.0467(10) 0.0422(9) 0.0012(7) -0.0055(7) -0.0018(7)
N7 0.0484(10) 0.0531(11) 0.0439(10) -0.0009(8) -0.0075(8) -0.0013(8)
N8 0.0518(11) 0.0685(13) 0.0457(10) -0.0069(9) -0.0108(8) -0.0054(9)
N9 0.0801(17) 0.0963(19) 0.0804(17) 0.0374(15) -0.0027(14) -0.0096(15)
N10 0.0645(13) 0.0541(12) 0.0688(14) 0.0105(10) -0.0067(11) -0.0043(10)
N11 0.0648(13) 0.0578(12) 0.0590(12) 0.0123(10) -0.0099(10) 0.0027(10)
N12 0.0607(12) 0.0509(11) 0.0602(12) 0.0069(9) -0.0087(10) 0.0027(9)
N13 0.0527(12) 0.0790(15) 0.0699(14) -0.0110(12) -0.0110(10) -0.0003(11)
N14 0.120(3) 0.068(2) 0.141(3) 0.028(2) -0.011(3) -0.028(2)
C1 0.0524(13) 0.0463(12) 0.0478(13) 0.0011(10) 0.0004(10) -0.0007(10)
C2 0.0558(13) 0.0484(12) 0.0445(12) -0.0013(9) 0.0003(10) 0.0013(10)
C3 0.0724(16) 0.0512(13) 0.0442(12) 0.0011(10) -0.0020(11) -0.0028(11)
C4 0.0790(17) 0.0556(14) 0.0467(13) 0.0073(11) -0.0002(12) -0.0012(12)
C5 0.0704(16) 0.0467(12) 0.0530(13) 0.0059(10) -0.0013(11) -0.0003(11)
C6 0.0537(12) 0.0437(11) 0.0467(12) 0.0024(9) -0.0019(10) -0.0012(9)
C7 0.0493(12) 0.0410(11) 0.0471(12) 0.0022(9) -0.0027(9) -0.0012(9)
C8 0.0382(10) 0.0437(11) 0.0472(11) -0.0007(9) -0.0056(9) -0.0025(8)
C9 0.0390(10) 0.0440(11) 0.0466(11) -0.0002(9) -0.0076(9) -0.0004(8)
C10 0.0459(12) 0.0552(13) 0.0455(12) -0.0020(10) -0.0085(9) -0.0023(10)
C11 0.0532(13) 0.0610(14) 0.0481(13) -0.0053(11) -0.0084(10) -0.0034(11)
C12 0.0689(16) 0.0666(16) 0.0486(13) -0.0002(11) -0.0090(12) -0.0110(13)
C13 0.0805(19) 0.0768(18) 0.0503(14) -0.0010(13) -0.0062(13) -0.0075(15)
C14 0.0726(17) 0.0849(19) 0.0502(14) -0.0108(13) -0.0125(12) -0.0094(15)
C15 0.0573(14) 0.0721(16) 0.0544(14) -0.0103(12) -0.0144(11) -0.0044(12)
C16 0.0570(15) 0.0837(19) 0.0607(16) -0.0137(14) -0.0148(12) -0.0107(13)
C17 0.108(3) 0.157(3) 0.121(3) 0.044(3) 0.020(3) -0.017(3)
C18 0.091(3) 0.139(4) 0.089(3) 0.051(3) 0.000(2) -0.010(2)
C19 0.104(3) 0.148(4) 0.074(2) 0.040(2) 0.008(2) 0.016(3)
C20 0.101(3) 0.112(3) 0.0655(19) 0.0240(18) -0.0031(18) 0.019(2)
C21 0.088(2) 0.086(2) 0.0679(19) 0.0195(16) -0.0068(16) 0.0111(17)
C22 0.0745(18) 0.0673(17) 0.0711(18) 0.0188(14) -0.0069(14) 0.0016(14)
C23 0.0659(16) 0.0554(14) 0.0640(16) 0.0116(12) -0.0084(12) 0.0008(12)
C24 0.0612(15) 0.0468(13) 0.0693(16) 0.0044(11) -0.0090(12) 0.0014(11)
C25 0.0645(17) 0.092(2) 0.087(2) 0.0053(17) -0.0126(15) -0.0324(16)
C26 0.075(2) 0.162(4) 0.116(3) 0.043(3) -0.014(2) -0.049(3)
C27 0.084(2) 0.114(3) 0.121(3) 0.032(2) -0.024(2) -0.046(2)
C28 0.0756(17) 0.0383(12) 0.0713(16) -0.0024(11) 0.0256(13) -0.0010(11)
C29 0.094(5) 0.046(3) 0.090(5) -0.019(3) 0.040(3) -0.021(3)
C30 0.0710(19) 0.119(3) 0.101(3) -0.052(2) -0.0240(18) 0.0227(19)
C31 0.111(3) 0.125(4) 0.152(4) 0.045(3) 0.031(3) 0.042(3)
C32 0.201(7) 0.079(4) 0.250(8) -0.014(5) 0.012(6) -0.022(4)
C33 0.236(10) 0.164(8) 0.249(10) 0.009(8) 0.026(8) 0.003(8)
C33' 0.236(10) 0.164(8) 0.249(10) 0.009(8) 0.026(8) 0.003(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.9903(16) 9_566 ?
Zn1 O2 2.1658(16) . ?
Zn1 O9 1.9087(15) 12_656 ?
Zn1 N1 2.0585(18) . ?
Zn1 N2 2.2736(18) . ?
Zn2 O9 1.9232(15) 12_656 ?
Zn2 O9 1.9231(15) . ?
Zn2 N6 1.9925(18) . ?
Zn2 N6 1.9926(18) 12_656 ?
Zn3 O3 2.1353(17) . ?
Zn3 O7 1.9081(19) . ?
Zn3 N5 2.2213(18) . ?
Zn3 N8 2.043(2) . ?
Zn3 N13 2.081(2) . ?
Zn4 O7 1.9323(17) . ?
Zn4 O8 1.9286(19) . ?
Zn4 N4 2.0017(19) . ?
Zn4 N12 2.005(2) 12_656 ?
Zn5 O6 2.131(3) . ?
Zn5 O8 1.915(2) . ?
Zn5 N9 2.051(3) . ?
Zn5 N10 2.300(2) . ?
Zn5 N14 2.011(5) . ?
O1 C1 1.270(3) . ?
O2 C1 1.236(3) . ?
O3 C16 1.258(3) . ?
O4 C16 1.249(3) . ?
O5 C17 1.254(6) . ?
O6 C17 1.287(6) . ?
O7 C25 1.415(3) . ?
O8 C27 1.433(4) . ?
O9 C28 1.416(3) . ?
N1 C2 1.339(3) . ?
N1 C6 1.339(3) . ?
N2 C7 1.352(3) . ?
N2 C8 1.336(3) . ?
N3 N4 1.374(3) . ?
N3 C7 1.328(3) . ?
N4 C8 1.347(3) . ?
N5 C9 1.339(3) . ?
N5 C10 1.356(3) . ?
N6 N7 1.373(3) . ?
N6 C9 1.345(3) . ?
N7 C10 1.326(3) . ?
N8 C11 1.334(3) . ?
N8 C15 1.344(3) . ?
N9 C18 1.345(5) . ?
N9 C22 1.322(4) . ?
N10 C23 1.360(4) . ?
N10 C24 1.336(4) . ?
N11 N12 1.372(3) . ?
N11 C23 1.327(4) . ?
N12 C24 1.343(3) . ?
N13 H13 1.0000 . ?
N13 C30 1.488(4) . ?
N13 C31 1.485(5) . ?
N14 H14 1.0000 . ?
N14 H14A 1.0000 . ?
N14 C32 1.357(8) . ?
N14 C33 1.443(12) . ?
N14 C33' 1.445(12) . ?
C1 C2 1.512(3) . ?
C2 C3 1.392(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(3) . ?
C6 C7 1.465(3) . ?
C8 C9 1.453(3) . ?
C10 C11 1.459(3) . ?
C11 C12 1.390(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(4) . ?
C13 H13A 0.9500 . ?
C13 C14 1.394(4) . ?
C14 H14B 0.9500 . ?
C14 C15 1.376(4) . ?
C15 C16 1.516(4) . ?
C17 C18 1.519(6) . ?
C18 C19 1.366(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.376(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.385(5) . ?
C22 C23 1.470(4) . ?
C24 C24 1.455(5) 12_656 ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.452(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.457(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.477(6) . ?
C28 C29 1.533(6) 12_656 ?
C28 H28A 0.968(3) . ?
C28 H28B 0.973(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33' H33D 0.9800 . ?
C33' H33E 0.9800 . ?
C33' H33F 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
O1 Zn1 O2 105.58(6) 9_566 . ?
O1 Zn1 N1 101.52(7) 9_566 . ?
O1 Zn1 N2 88.65(6) 9_566 . ?
O2 Zn1 N2 150.20(6) . . ?
O9 Zn1 O1 120.47(7) 12_656 9_566 ?
O9 Zn1 O2 97.93(6) 12_656 . ?
O9 Zn1 N1 137.34(7) 12_656 . ?
O9 Zn1 N2 96.94(6) 12_656 . ?
N1 Zn1 O2 76.08(6) . . ?
N1 Zn1 N2 75.47(7) . . ?
O9 Zn2 O9 102.92(9) . 12_656 ?
O9 Zn2 N6 112.85(7) . . ?
O9 Zn2 N6 112.85(7) 12_656 12_656 ?
O9 Zn2 N6 111.42(7) . 12_656 ?
O9 Zn2 N6 111.42(7) 12_656 . ?
N6 Zn2 N6 105.59(10) . 12_656 ?
O3 Zn3 N5 149.57(7) . . ?
O7 Zn3 O3 98.08(8) . . ?
O7 Zn3 N5 99.83(7) . . ?
O7 Zn3 N8 152.24(9) . . ?
O7 Zn3 N13 102.07(9) . . ?
N8 Zn3 O3 76.63(7) . . ?
N8 Zn3 N5 76.06(7) . . ?
N8 Zn3 N13 105.65(9) . . ?
N13 Zn3 O3 104.34(8) . . ?
N13 Zn3 N5 95.72(8) . . ?
O7 Zn4 N4 111.83(8) . . ?
O7 Zn4 N12 105.06(8) . 12_656 ?
O8 Zn4 O7 101.35(8) . . ?
O8 Zn4 N4 112.57(8) . . ?
O8 Zn4 N12 117.14(9) . 12_656 ?
N4 Zn4 N12 108.47(8) . 12_656 ?
O6 Zn5 N10 152.81(12) . . ?
O8 Zn5 O6 100.17(11) . . ?
O8 Zn5 N9 130.83(10) . . ?
O8 Zn5 N10 92.88(8) . . ?
O8 Zn5 N14 112.97(17) . . ?
N9 Zn5 O6 77.92(12) . . ?
N9 Zn5 N10 75.51(10) . . ?
N14 Zn5 O6 97.80(18) . . ?
N14 Zn5 N9 115.96(17) . . ?
N14 Zn5 N10 98.88(15) . . ?
C1 O1 Zn1 119.06(14) . 8_656 ?
C1 O2 Zn1 115.25(14) . . ?
C16 O3 Zn3 116.43(16) . . ?
C17 O6 Zn5 114.7(3) . . ?
Zn3 O7 Zn4 117.14(8) . . ?
C25 O7 Zn3 120.94(17) . . ?
C25 O7 Zn4 121.11(18) . . ?
Zn5 O8 Zn4 119.45(10) . . ?
C27 O8 Zn4 119.7(2) . . ?
C27 O8 Zn5 120.1(2) . . ?
Zn1 O9 Zn2 117.15(7) 12_656 . ?
C28 O9 Zn1 122.94(14) . 12_656 ?
C28 O9 Zn2 119.81(13) . . ?
C2 N1 Zn1 118.04(15) . . ?
C2 N1 C6 120.56(19) . . ?
C6 N1 Zn1 121.23(15) . . ?
C7 N2 Zn1 108.68(14) . . ?
C8 N2 Zn1 144.79(15) . . ?
C8 N2 C7 102.20(18) . . ?
C7 N3 N4 103.97(18) . . ?
N3 N4 Zn4 119.39(14) . . ?
C8 N4 Zn4 133.16(15) . . ?
C8 N4 N3 107.14(18) . . ?
C9 N5 Zn3 145.49(16) . . ?
C9 N5 C10 102.21(18) . . ?
C10 N5 Zn3 109.10(14) . . ?
N7 N6 Zn2 121.13(14) . . ?
C9 N6 Zn2 130.84(14) . . ?
C9 N6 N7 107.75(17) . . ?
C10 N7 N6 103.75(18) . . ?
C11 N8 Zn3 120.74(16) . . ?
C11 N8 C15 121.3(2) . . ?
C15 N8 Zn3 117.84(18) . . ?
C18 N9 Zn5 117.3(3) . . ?
C22 N9 Zn5 121.9(2) . . ?
C22 N9 C18 120.8(3) . . ?
C23 N10 Zn5 108.18(18) . . ?
C24 N10 Zn5 147.86(19) . . ?
C24 N10 C23 101.7(2) . . ?
C23 N11 N12 103.8(2) . . ?
N11 N12 Zn4 124.95(17) . 12_656 ?
C24 N12 Zn4 127.32(18) . 12_656 ?
C24 N12 N11 107.4(2) . . ?
Zn3 N13 H13 106.5 . . ?
C30 N13 Zn3 112.13(19) . . ?
C30 N13 H13 106.5 . . ?
C31 N13 Zn3 114.1(2) . . ?
C31 N13 H13 106.5 . . ?
C31 N13 C30 110.6(3) . . ?
Zn5 N14 H14 108.7 . . ?
Zn5 N14 H14A 108.6 . . ?
C32 N14 Zn5 112.5(4) . . ?
C32 N14 H14 108.7 . . ?
C32 N14 H14A 108.6 . . ?
C32 N14 C33 107.5(11) . . ?
C32 N14 C33' 104.1(11) . . ?
C33 N14 Zn5 111.1(9) . . ?
C33 N14 H14A 108.6 . . ?
C33' N14 Zn5 114.1(9) . . ?
C33' N14 H14 108.7 . . ?
O1 C1 C2 116.1(2) . . ?
O2 C1 O1 126.2(2) . . ?
O2 C1 C2 117.7(2) . . ?
N1 C2 C1 112.48(19) . . ?
N1 C2 C3 121.2(2) . . ?
C3 C2 C1 126.3(2) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.4(2) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.4(2) . . ?
C6 C5 H5 120.8 . . ?
N1 C6 C5 121.2(2) . . ?
N1 C6 C7 112.38(19) . . ?
C5 C6 C7 126.4(2) . . ?
N2 C7 C6 119.92(19) . . ?
N3 C7 N2 114.6(2) . . ?
N3 C7 C6 125.4(2) . . ?
N2 C8 N4 112.07(19) . . ?
N2 C8 C9 123.97(19) . . ?
N4 C8 C9 123.67(19) . . ?
N5 C9 N6 111.62(19) . . ?
N5 C9 C8 126.4(2) . . ?
N6 C9 C8 121.86(18) . . ?
N5 C10 C11 119.6(2) . . ?
N7 C10 N5 114.68(19) . . ?
N7 C10 C11 125.7(2) . . ?
N8 C11 C10 111.9(2) . . ?
N8 C11 C12 121.1(2) . . ?
C12 C11 C10 126.9(2) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 C11 118.2(3) . . ?
C13 C12 H12 120.9 . . ?
C12 C13 H13A 120.1 . . ?
C12 C13 C14 119.8(3) . . ?
C14 C13 H13A 120.1 . . ?
C13 C14 H14B 120.5 . . ?
C15 C14 C13 119.0(2) . . ?
C15 C14 H14B 120.5 . . ?
N8 C15 C14 120.5(2) . . ?
N8 C15 C16 112.8(2) . . ?
C14 C15 C16 126.7(2) . . ?
O3 C16 C15 116.0(2) . . ?
O4 C16 O3 126.3(3) . . ?
O4 C16 C15 117.7(3) . . ?
O5 C17 O6 126.7(5) . . ?
O5 C17 C18 116.2(5) . . ?
O6 C17 C18 117.0(4) . . ?
N9 C18 C17 113.1(4) . . ?
N9 C18 C19 120.6(4) . . ?
C19 C18 C17 126.3(4) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.4(4) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.6(4) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 120.8 . . ?
C20 C21 C22 118.4(4) . . ?
C22 C21 H21 120.8 . . ?
N9 C22 C21 121.2(3) . . ?
N9 C22 C23 113.4(3) . . ?
C21 C22 C23 125.4(3) . . ?
N10 C23 C22 119.5(3) . . ?
N11 C23 N10 114.7(3) . . ?
N11 C23 C22 125.7(3) . . ?
N10 C24 N12 112.3(2) . . ?
N10 C24 C24 126.2(3) . 12_656 ?
N12 C24 C24 120.8(3) . 12_656 ?
O7 C25 H25A 108.7 . . ?
O7 C25 H25B 108.7 . . ?
O7 C25 C26 114.3(3) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C25 C26 H26A 106.7 . . ?
C25 C26 H26B 106.7 . . ?
C25 C26 C27 122.3(4) . . ?
H26A C26 H26B 106.6 . . ?
C27 C26 H26A 106.7 . . ?
C27 C26 H26B 106.7 . . ?
O8 C27 C26 115.8(3) . . ?
O8 C27 H27A 108.3 . . ?
O8 C27 H27B 108.3 . . ?
C26 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
O9 C28 C29 113.7(3) . . ?
O9 C28 C29 113.4(3) . 12_656 ?
O9 C28 H28A 107.9(2) . . ?
O9 C28 H28B 107.7(2) . . ?
C29 C28 C29 52.0(5) . 12_656 ?
C29 C28 H28A 128.9(3) 12_656 . ?
C29 C28 H28A 84.8(3) . . ?
C29 C28 H28B 129.2(4) . . ?
C29 C28 H28B 85.5(3) 12_656 . ?
H28A C28 H28B 109.4(2) . . ?
C28 C29 C28 117.9(4) . 12_656 ?
C28 C29 H29A 107.8 . . ?
C28 C29 H29A 107.8 12_656 . ?
C28 C29 H29B 107.8 . . ?
C28 C29 H29B 107.8 12_656 . ?
H29A C29 H29B 107.2 . . ?
N13 C30 H30A 109.5 . . ?
N13 C30 H30B 109.5 . . ?
N13 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N13 C31 H31A 109.5 . . ?
N13 C31 H31B 109.5 . . ?
N13 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N14 C32 H32A 109.5 . . ?
N14 C32 H32B 109.5 . . ?
N14 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N14 C33 H33A 109.5 . . ?
N14 C33 H33B 109.5 . . ?
N14 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N14 C33' H33D 109.5 . . ?
N14 C33' H33E 109.5 . . ?
N14 C33' H33F 109.5 . . ?
H33D C33' H33E 109.5 . . ?
H33D C33' H33F 109.5 . . ?
H33E C33' H33F 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
Zn1 O1 C1 O2 10.0(3) 8_656 . . . ?
Zn1 O1 C1 C2 -169.84(15) 8_656 . . . ?
Zn1 O2 C1 O1 -173.09(19) . . . . ?
Zn1 O2 C1 C2 6.7(3) . . . . ?
Zn1 O9 C28 C29 148.6(3) 12_656 . . 12_656 ?
Zn1 O9 C28 C29 -154.3(3) 12_656 . . . ?
Zn1 N1 C2 C1 -2.1(3) . . . . ?
Zn1 N1 C2 C3 176.23(19) . . . . ?
Zn1 N1 C6 C5 -175.58(18) . . . . ?
Zn1 N1 C6 C7 4.4(3) . . . . ?
Zn1 N2 C7 N3 162.66(16) . . . . ?
Zn1 N2 C7 C6 -15.8(2) . . . . ?
Zn1 N2 C8 N4 -150.6(2) . . . . ?
Zn1 N2 C8 C9 35.4(4) . . . . ?
Zn2 O9 C28 C29 -27.5(4) . . . 12_656 ?
Zn2 O9 C28 C29 29.5(4) . . . . ?
Zn2 N6 N7 C10 174.34(15) . . . . ?
Zn2 N6 C9 N5 -174.05(15) . . . . ?
Zn2 N6 C9 C8 1.6(3) . . . . ?
Zn3 O3 C16 O4 178.2(3) . . . . ?
Zn3 O3 C16 C15 -0.1(3) . . . . ?
Zn3 O7 C25 C26 -162.2(3) . . . . ?
Zn3 N5 C9 N6 -154.3(2) . . . . ?
Zn3 N5 C9 C8 30.3(4) . . . . ?
Zn3 N5 C10 N7 164.53(16) . . . . ?
Zn3 N5 C10 C11 -15.5(3) . . . . ?
Zn3 N8 C11 C10 7.5(3) . . . . ?
Zn3 N8 C11 C12 -174.6(2) . . . . ?
Zn3 N8 C15 C14 174.6(2) . . . . ?
Zn3 N8 C15 C16 -6.4(3) . . . . ?
Zn4 O7 C25 C26 28.4(4) . . . . ?
Zn4 O8 C27 C26 -25.6(5) . . . . ?
Zn4 N4 C8 N2 172.79(16) . . . . ?
Zn4 N4 C8 C9 -13.2(3) . . . . ?
Zn4 N12 C24 N10 -174.53(17) 12_656 . . . ?
Zn4 N12 C24 C24 -3.8(3) 12_656 . . 12_656 ?
Zn5 O6 C17 O5 -179.6(5) . . . . ?
Zn5 O6 C17 C18 -2.6(6) . . . . ?
Zn5 O8 C27 C26 164.1(3) . . . . ?
Zn5 N9 C18 C17 0.5(5) . . . . ?
Zn5 N9 C18 C19 179.1(3) . . . . ?
Zn5 N9 C22 C21 -179.2(2) . . . . ?
Zn5 N9 C22 C23 2.4(4) . . . . ?
Zn5 N10 C23 N11 167.23(18) . . . . ?
Zn5 N10 C23 C22 -13.1(3) . . . . ?
Zn5 N10 C24 N12 -157.3(2) . . . . ?
Zn5 N10 C24 C24 32.6(4) . . . 12_656 ?
O1 C1 C2 N1 176.6(2) . . . . ?
O1 C1 C2 C3 -1.7(4) . . . . ?
O2 C1 C2 N1 -3.3(3) . . . . ?
O2 C1 C2 C3 178.4(2) . . . . ?
O5 C17 C18 N9 178.7(5) . . . . ?
O5 C17 C18 C19 0.3(8) . . . . ?
O6 C17 C18 N9 1.5(7) . . . . ?
O6 C17 C18 C19 -177.0(5) . . . . ?
O7 C25 C26 C27 -60.7(6) . . . . ?
O9 C28 C29 C28 -66.7(5) . . . 12_656 ?
N1 C2 C3 C4 -0.5(4) . . . . ?
N1 C6 C7 N2 9.0(3) . . . . ?
N1 C6 C7 N3 -169.3(2) . . . . ?
N2 C8 C9 N5 -160.0(2) . . . . ?
N2 C8 C9 N6 25.0(3) . . . . ?
N3 N4 C8 N2 -0.5(2) . . . . ?
N3 N4 C8 C9 173.51(19) . . . . ?
N4 N3 C7 N2 -0.1(3) . . . . ?
N4 N3 C7 C6 178.3(2) . . . . ?
N4 C8 C9 N5 26.7(3) . . . . ?
N4 C8 C9 N6 -148.3(2) . . . . ?
N5 C10 C11 N8 6.7(3) . . . . ?
N5 C10 C11 C12 -171.1(3) . . . . ?
N6 N7 C10 N5 0.6(3) . . . . ?
N6 N7 C10 C11 -179.4(2) . . . . ?
N7 N6 C9 N5 -0.3(2) . . . . ?
N7 N6 C9 C8 175.40(19) . . . . ?
N7 C10 C11 N8 -173.3(2) . . . . ?
N7 C10 C11 C12 8.9(4) . . . . ?
N8 C11 C12 C13 -0.4(4) . . . . ?
N8 C15 C16 O3 4.1(4) . . . . ?
N8 C15 C16 O4 -174.3(3) . . . . ?
N9 C18 C19 C20 1.0(7) . . . . ?
N9 C22 C23 N10 8.4(4) . . . . ?
N9 C22 C23 N11 -172.0(3) . . . . ?
N11 N12 C24 N10 -0.8(3) . . . . ?
N11 N12 C24 C24 169.95(16) . . . 12_656 ?
N12 N11 C23 N10 0.3(3) . . . . ?
N12 N11 C23 C22 -179.4(3) . . . . ?
C1 C2 C3 C4 177.6(2) . . . . ?
C2 N1 C6 C5 -0.5(4) . . . . ?
C2 N1 C6 C7 179.5(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C3 C4 C5 C6 0.9(4) . . . . ?
C4 C5 C6 N1 -0.4(4) . . . . ?
C4 C5 C6 C7 179.5(2) . . . . ?
C5 C6 C7 N2 -171.0(2) . . . . ?
C5 C6 C7 N3 10.7(4) . . . . ?
C6 N1 C2 C1 -177.3(2) . . . . ?
C6 N1 C2 C3 1.0(4) . . . . ?
C7 N2 C8 N4 0.4(2) . . . . ?
C7 N2 C8 C9 -173.6(2) . . . . ?
C7 N3 N4 Zn4 -174.03(15) . . . . ?
C7 N3 N4 C8 0.4(2) . . . . ?
C8 N2 C7 N3 -0.2(3) . . . . ?
C8 N2 C7 C6 -178.7(2) . . . . ?
C9 N5 C10 N7 -0.7(3) . . . . ?
C9 N5 C10 C11 179.3(2) . . . . ?
C9 N6 N7 C10 -0.2(2) . . . . ?
C10 N5 C9 N6 0.6(2) . . . . ?
C10 N5 C9 C8 -174.9(2) . . . . ?
C10 C11 C12 C13 177.2(3) . . . . ?
C11 N8 C15 C14 -1.9(4) . . . . ?
C11 N8 C15 C16 177.1(2) . . . . ?
C11 C12 C13 C14 -0.9(4) . . . . ?
C12 C13 C14 C15 0.8(5) . . . . ?
C13 C14 C15 N8 0.5(4) . . . . ?
C13 C14 C15 C16 -178.3(3) . . . . ?
C14 C15 C16 O3 -177.0(3) . . . . ?
C14 C15 C16 O4 4.6(5) . . . . ?
C15 N8 C11 C10 -176.1(2) . . . . ?
C15 N8 C11 C12 1.8(4) . . . . ?
C17 C18 C19 C20 179.4(4) . . . . ?
C18 N9 C22 C21 0.9(5) . . . . ?
C18 N9 C22 C23 -177.4(3) . . . . ?
C18 C19 C20 C21 -0.8(6) . . . . ?
C19 C20 C21 C22 0.7(5) . . . . ?
C20 C21 C22 N9 -0.8(5) . . . . ?
C20 C21 C22 C23 177.4(3) . . . . ?
C21 C22 C23 N10 -169.9(3) . . . . ?
C21 C22 C23 N11 9.8(5) . . . . ?
C22 N9 C18 C17 -179.6(4) . . . . ?
C22 N9 C18 C19 -1.1(6) . . . . ?
C23 N10 C24 N12 0.9(3) . . . . ?
C23 N10 C24 C24 -169.22(15) . . . 12_656 ?
C23 N11 N12 Zn4 174.20(17) . . . 12_656 ?
C23 N11 N12 C24 0.3(3) . . . . ?
C24 N10 C23 N11 -0.8(3) . . . . ?
C24 N10 C23 C22 178.9(2) . . . . ?
C25 C26 C27 O8 59.6(6) . . . . ?
C29 C28 C29 C28 35.3(5) 12_656 . . 12_656 ?
_shelx_res_file
;
TITL 20200607-HFP-TY-Zn54 in Fd-3 #203
20200607-hfp-ty-zn54_sq.res
created by SHELXL-2018/3 at 01:46:38 on 15-Nov-2024
REM reset to Fd-3 #203
CELL 1.54184 58.301726 58.301726 58.301726 90 90 90
ZERR 8 0.000231 0.000231 0.000231 0 0 0
LATT 4
SYMM +Z,+X,+Y
SYMM +Y,+Z,+X
SYMM 0.25-Y,0.25-Z,+X
SYMM +Z,0.25-X,0.25-Y
SYMM 0.25-Y,+Z,0.25-X
SYMM 0.25-Z,0.25-X,+Y
SYMM 0.25-Z,+X,0.25-Y
SYMM +Y,0.25-Z,0.25-X
SYMM 0.25-X,0.25-Y,+Z
SYMM +X,0.25-Y,0.25-Z
SYMM 0.25-X,+Y,0.25-Z
SFAC C H N O Zn
UNIT 4185.6 5641.6 1564.88 1360.08 432
EQIV $1 1.25-X,+Y,1.25-Z
DFIX 1.5 N14 C32 N14 C33 N14 C33'
SADI N14 C32 N14 C33' N14 C33
EADP C33' C33
ISOR 0.005 0.01 O5 C17 O6 C33' C32 N14
L.S. 20 0 174
PLAN 5
SIZE 0.37 0.3 0.32
TEMP -173.15
CONF
FREE C29 C29_$1
FREE C29 H28b
MORE -1
Bond $H
HTAB 2
ABIN
fmap 2 53
acta
SHEL 999 0.837
OMIT 0 2 22
OMIT 0 8 20
OMIT 0 12 20
OMIT 1 3 5
OMIT 2 10 10
OMIT 3 3 9
OMIT 4 12 12
OMIT 4 16 16
OMIT 5 3 11
OMIT 5 5 11
OMIT 5 7 11
OMIT 6 2 16
OMIT 6 4 12
OMIT 11 1 29
REM
REM
REM
WGHT 0.084700 263.693390
FVAR 0.06028
ZN1 5 0.586852 0.522613 0.665491 11.00000 0.04619 0.04307 =
0.04248 0.00294 0.00057 0.00192
ZN2 5 0.625000 0.515497 0.625000 10.50000 0.03907 0.03754 =
0.04183 0.00000 -0.00329 0.00000
ZN3 5 0.554393 0.445403 0.580296 11.00000 0.04638 0.06651 =
0.05177 -0.00878 -0.00807 -0.00828
ZN4 5 0.574690 0.420911 0.626634 11.00000 0.05430 0.04744 =
0.06018 -0.00365 -0.00848 -0.01022
ZN5 5 0.581858 0.383715 0.669142 11.00000 0.08589 0.08452 =
0.09926 0.03413 -0.01486 -0.02337
O1 4 0.590464 0.553330 0.729865 11.00000 0.06357 0.04815 =
0.04372 -0.00271 0.00022 0.00053
O2 4 0.590412 0.548554 0.691842 11.00000 0.06400 0.04368 =
0.04390 0.00081 0.00216 0.00016
O3 4 0.540953 0.423341 0.554333 11.00000 0.05383 0.08424 =
0.05829 -0.01444 -0.00947 -0.01580
O4 4 0.543373 0.414816 0.517015 11.00000 0.08726 0.10592 =
0.06052 -0.02230 -0.00986 -0.03326
O5 4 0.552230 0.382214 0.733827 11.00000 0.13755 0.28945 =
0.12651 0.07842 0.03183 -0.04466
O6 4 0.557648 0.376778 0.695632 11.00000 0.10699 0.16196 =
0.11546 0.05023 -0.00051 -0.04341
O7 4 0.549194 0.425891 0.606053 11.00000 0.05010 0.07183 =
0.06277 -0.00318 -0.00887 -0.01637
O8 4 0.562259 0.397965 0.646962 11.00000 0.06940 0.06445 =
0.08362 0.01114 -0.01186 -0.02313
O9 4 0.643274 0.536050 0.606790 11.00000 0.05066 0.03725 =
0.04944 -0.00192 0.00438 -0.00107
N1 3 0.590105 0.504020 0.695329 11.00000 0.05221 0.04380 =
0.04328 0.00044 -0.00077 0.00141
N2 3 0.590761 0.485671 0.653626 11.00000 0.04228 0.04253 =
0.04450 -0.00074 -0.00362 0.00075
N3 3 0.583799 0.449923 0.666679 11.00000 0.05713 0.04705 =
0.04815 0.00163 -0.00264 -0.00445
N4 3 0.583602 0.449681 0.643115 11.00000 0.05261 0.04668 =
0.04854 0.00072 -0.00596 -0.00665
N5 3 0.583044 0.466554 0.593839 11.00000 0.04616 0.04997 =
0.04868 -0.00328 -0.00817 -0.00583
N6 3 0.605430 0.494833 0.606079 11.00000 0.04225 0.04675 =
0.04216 0.00121 -0.00553 -0.00179
N7 3 0.606444 0.495278 0.582558 11.00000 0.04845 0.05310 =
0.04392 -0.00091 -0.00750 -0.00133
N8 3 0.572214 0.454832 0.551626 11.00000 0.05177 0.06849 =
0.04572 -0.00694 -0.01082 -0.00539
N9 3 0.597966 0.396948 0.697484 11.00000 0.08007 0.09634 =
0.08042 0.03737 -0.00269 -0.00963
N10 3 0.614146 0.401293 0.654839 11.00000 0.06455 0.05414 =
0.06882 0.01050 -0.00669 -0.00431
N11 3 0.648986 0.413251 0.667089 11.00000 0.06475 0.05783 =
0.05905 0.01231 -0.00994 0.00274
N12 3 0.649198 0.411426 0.643620 11.00000 0.06071 0.05094 =
0.06021 0.00692 -0.00875 0.00265
N13 3 0.529211 0.470338 0.584620 11.00000 0.05273 0.07897 =
0.06988 -0.01099 -0.01097 -0.00027
AFIX 13
H13 2 0.514139 0.462502 0.582247 11.00000 -1.20000
AFIX 0
N14 3 0.589629 0.351053 0.661229 10.80000 0.12020 0.06751 =
0.14073 0.02785 -0.01081 -0.02785
PART 1
AFIX 13
H14 2 0.603668 0.346482 0.669958 10.40000 -1.20000
AFIX 13
PART 2
H14A 2 0.576446 0.341054 0.665748 10.40000 -1.20000
AFIX 0
PART 0
C1 1 0.590663 0.541253 0.711745 11.00000 0.05239 0.04632 =
0.04785 0.00111 0.00042 -0.00069
C2 1 0.591196 0.515544 0.715167 11.00000 0.05578 0.04840 =
0.04452 -0.00128 0.00032 0.00128
C3 1 0.592057 0.504093 0.736103 11.00000 0.07243 0.05124 =
0.04421 0.00114 -0.00204 -0.00275
AFIX 43
H3 2 0.592958 0.512365 0.750112 11.00000 -1.20000
AFIX 0
C4 1 0.591569 0.480444 0.736003 11.00000 0.07905 0.05559 =
0.04666 0.00731 -0.00020 -0.00121
AFIX 43
H4 2 0.592247 0.472251 0.750072 11.00000 -1.20000
AFIX 0
C5 1 0.590093 0.468576 0.715437 11.00000 0.07038 0.04672 =
0.05304 0.00593 -0.00131 -0.00032
AFIX 43
H5 2 0.589526 0.452293 0.715224 11.00000 -1.20000
AFIX 0
C6 1 0.589463 0.481056 0.695183 11.00000 0.05365 0.04372 =
0.04669 0.00243 -0.00187 -0.00123
C7 1 0.588095 0.471673 0.671922 11.00000 0.04935 0.04099 =
0.04708 0.00222 -0.00274 -0.00120
C8 1 0.587924 0.471257 0.636046 11.00000 0.03823 0.04372 =
0.04722 -0.00073 -0.00564 -0.00248
C9 1 0.591436 0.477535 0.612189 11.00000 0.03899 0.04398 =
0.04659 -0.00020 -0.00765 -0.00037
C10 1 0.592966 0.478089 0.576242 11.00000 0.04592 0.05516 =
0.04550 -0.00200 -0.00855 -0.00231
C11 1 0.588308 0.471070 0.552671 11.00000 0.05320 0.06096 =
0.04813 -0.00528 -0.00844 -0.00343
C12 1 0.599174 0.478936 0.532967 11.00000 0.06891 0.06658 =
0.04858 -0.00022 -0.00902 -0.01105
AFIX 43
H12 2 0.610566 0.490560 0.533760 11.00000 -1.20000
AFIX 0
C13 1 0.592927 0.469348 0.512116 11.00000 0.08053 0.07681 =
0.05029 -0.00104 -0.00618 -0.00755
AFIX 43
H13A 2 0.599892 0.474536 0.498328 11.00000 -1.20000
AFIX 0
C14 1 0.576402 0.452077 0.511434 11.00000 0.07263 0.08490 =
0.05019 -0.01082 -0.01247 -0.00939
AFIX 43
H14B 2 0.572153 0.445257 0.497258 11.00000 -1.20000
AFIX 0
C15 1 0.566336 0.445053 0.531592 11.00000 0.05733 0.07215 =
0.05444 -0.01029 -0.01439 -0.00441
C16 1 0.548607 0.426229 0.534375 11.00000 0.05701 0.08369 =
0.06070 -0.01373 -0.01476 -0.01074
C17 1 0.563434 0.384244 0.715577 11.00000 0.10819 0.15678 =
0.12066 0.04393 0.01952 -0.01716
C18 1 0.586719 0.395760 0.717582 11.00000 0.09078 0.13886 =
0.08949 0.05094 -0.00034 -0.00968
C19 1 0.596500 0.403941 0.737239 11.00000 0.10373 0.14802 =
0.07376 0.03973 0.00825 0.01613
AFIX 43
H19 2 0.588582 0.402839 0.751438 11.00000 -1.20000
AFIX 0
C20 1 0.617922 0.413790 0.736287 11.00000 0.10099 0.11204 =
0.06548 0.02400 -0.00311 0.01937
AFIX 43
H20 2 0.624825 0.419730 0.749799 11.00000 -1.20000
AFIX 0
C21 1 0.629312 0.414986 0.715581 11.00000 0.08813 0.08591 =
0.06787 0.01953 -0.00684 0.01108
AFIX 43
H21 2 0.644186 0.421568 0.714613 11.00000 -1.20000
AFIX 0
C22 1 0.618551 0.406364 0.696243 11.00000 0.07452 0.06729 =
0.07112 0.01879 -0.00689 0.00158
C23 1 0.627828 0.407125 0.672817 11.00000 0.06595 0.05545 =
0.06401 0.01162 -0.00837 0.00085
C24 1 0.628239 0.404479 0.637053 11.00000 0.06117 0.04677 =
0.06925 0.00442 -0.00899 0.00135
C25 1 0.528875 0.412742 0.607847 11.00000 0.06447 0.09157 =
0.08717 0.00531 -0.01265 -0.03235
AFIX 23
H25A 2 0.530071 0.399427 0.597377 11.00000 -1.20000
H25B 2 0.515786 0.422219 0.602631 11.00000 -1.20000
AFIX 0
C26 1 0.524045 0.404418 0.630821 11.00000 0.07492 0.16201 =
0.11636 0.04327 -0.01364 -0.04872
AFIX 23
H26A 2 0.509040 0.396502 0.630102 11.00000 -1.20000
H26B 2 0.521850 0.418108 0.640624 11.00000 -1.20000
AFIX 0
C27 1 0.539632 0.389208 0.643077 11.00000 0.08430 0.11441 =
0.12059 0.03236 -0.02383 -0.04634
AFIX 23
H27A 2 0.532703 0.385451 0.658118 11.00000 -1.20000
H27B 2 0.540942 0.374718 0.634321 11.00000 -1.20000
AFIX 0
C28 1 0.640610 0.560055 0.609343 11.00000 0.07564 0.03830 =
0.07127 -0.00240 0.02556 -0.00101
C29 1 0.633399 0.567097 0.632579 10.50000 0.09364 0.04569 =
0.08988 -0.01926 0.03968 -0.02058
AFIX 23
H29A 2 0.634420 0.584025 0.633436 10.50000 -1.20000
H29B 2 0.644656 0.560832 0.643641 10.50000 -1.20000
AFIX 0
C30 1 0.528878 0.479651 0.608388 11.00000 0.07100 0.11922 =
0.10114 -0.05246 -0.02402 0.02266
AFIX 137
H30A 2 0.528529 0.466941 0.619382 11.00000 -1.50000
H30B 2 0.515222 0.489230 0.610462 11.00000 -1.50000
H30C 2 0.542664 0.488915 0.610970 11.00000 -1.50000
AFIX 0
C31 1 0.530279 0.489271 0.567611 11.00000 0.11063 0.12463 =
0.15241 0.04457 0.03079 0.04211
AFIX 137
H31A 2 0.543511 0.499079 0.570967 11.00000 -1.50000
H31B 2 0.516183 0.498387 0.568481 11.00000 -1.50000
H31C 2 0.531847 0.482841 0.552160 11.00000 -1.50000
AFIX 0
C32 1 0.593704 0.348122 0.638501 10.80000 0.20071 0.07900 =
0.24977 -0.01420 0.01182 -0.02187
AFIX 137
H32A 2 0.579513 0.350737 0.629881 10.80000 -1.50000
H32B 2 0.599120 0.332448 0.635756 10.80000 -1.50000
H32C 2 0.605423 0.359065 0.633454 10.80000 -1.50000
AFIX 0
PART 2
C33 1 0.609791 0.343496 0.673419 10.40000 0.23610 0.16365 =
0.24928 0.00884 0.02565 0.00304
AFIX 137
H33A 2 0.623491 0.349973 0.666147 10.40000 -1.50000
H33B 2 0.610629 0.326713 0.673000 10.40000 -1.50000
H33C 2 0.608949 0.348667 0.689391 10.40000 -1.50000
AFIX 0
H28A 2 10.655341 10.566409 10.613630 11.00000 -1.20000
H28B 2 10.636009 10.566240 10.594540 11.00000 -1.20000
PART 1
C33' 1 0.571545 0.334859 0.666246 10.40000 0.23610 0.16365 =
0.24928 0.00884 0.02565 0.00304
AFIX 137
H33D 2 0.578204 0.319639 0.668806 10.40000 -1.50000
H33E 2 0.560864 0.334193 0.653283 10.40000 -1.50000
H33F 2 0.563302 0.339762 0.680051 10.40000 -1.50000
AFIX 0
HKLF 4
REM 20200607-HFP-TY-Zn54 in Fd-3 #203
REM wR2 = 0.1288, GooF = S = 1.012, Restrained GooF = 1.050 for all data
REM R1 = 0.0390 for 12642 Fo > 4sig(Fo) and 0.0434 for all 14575 data
REM 554 parameters refined using 42 restraints
END
WGHT 0.0846 262.7468
REM Instructions for potential hydrogen bonds
EQIV $4 -z+1, -x+1, -y+1
HTAB N13 O4_$4
EQIV $5 -y+1, -z+1, -x+1
HTAB C14 O3_$5
HTAB C33' O6
REM Highest difference peak 0.488, deepest hole -0.338, 1-sigma level 0.062
Q1 1 0.6288 0.3409 0.6888 11.00000 0.05 0.49
Q2 1 0.5274 0.5274 0.7226 10.33333 0.05 0.48
Q3 1 0.5000 0.5000 0.5000 10.16667 0.05 0.45
Q4 1 0.5046 0.5046 0.5046 10.33333 0.05 0.33
Q5 1 0.5267 0.5163 0.7306 11.00000 0.05 0.31
;
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3 31 69 -11.29 0.00
5 31 69 -0.97 0.00
7 31 69 -1.71 0.00
9 31 69 -13.26 0.00
2 0 70 -9.54 0.00
6 0 70 15.27 0.00
10 0 70 7.36 0.00
14 0 70 11.11 0.00
18 0 70 7.87 0.00
22 0 70 -1.20 0.00
26 0 70 -16.89 0.00
30 0 70 -2.84 0.00
0 2 70 -6.92 0.00
2 2 70 5.90 0.00
4 2 70 -2.42 0.00
6 2 70 -9.05 0.00
8 2 70 -1.70 0.00
10 2 70 1.28 0.00
12 2 70 3.29 0.00
14 2 70 -2.61 0.00
16 2 70 10.22 0.00
18 2 70 -1.98 0.00
20 2 70 9.69 0.00
22 2 70 -1.66 0.00
24 2 70 5.18 0.00
26 2 70 -0.47 0.00
28 2 70 -4.69 0.00
30 2 70 -12.40 0.00
2 4 70 -11.72 0.00
4 4 70 26.52 0.00
6 4 70 -13.29 0.00
16 4 70 2.40 0.00
18 4 70 4.15 0.00
20 4 70 8.76 0.00
22 4 70 1.52 0.00
24 4 70 -11.82 0.00
26 4 70 -0.25 0.00
28 4 70 5.63 0.00
0 6 70 18.66 0.00
2 6 70 -4.99 0.00
20 6 70 -3.23 0.00
22 6 70 -5.28 0.00
24 6 70 -0.33 0.00
26 6 70 -7.00 0.00
28 6 70 1.88 0.00
2 8 70 -4.01 0.00
22 8 70 -9.31 0.00
24 8 70 -0.42 0.00
26 8 70 -6.11 0.00
28 8 70 -4.04 0.00
0 10 70 6.00 0.00
2 10 70 3.93 0.00
22 10 70 -7.34 0.00
24 10 70 3.52 0.00
26 10 70 8.51 0.00
28 10 70 8.70 0.00
20 12 70 4.44 0.00
22 12 70 -11.07 0.00
24 12 70 -5.46 0.00
26 12 70 -13.22 0.00
18 14 70 -8.61 0.00
20 14 70 -21.42 0.00
22 14 70 3.27 0.00
24 14 70 -9.72 0.00
26 14 70 2.37 0.00
6 16 70 26.83 0.00
8 16 70 -5.26 0.00
14 16 70 -1.47 0.00
16 16 70 -5.75 0.00
18 16 70 16.05 0.00
20 16 70 2.75 0.00
22 16 70 -6.56 0.00
24 16 70 7.06 0.00
10 18 70 -0.62 0.00
12 18 70 -4.20 0.00
14 18 70 -4.52 0.00
16 18 70 0.39 0.00
18 18 70 -11.16 0.00
20 18 70 6.45 0.00
22 18 70 3.01 0.00
24 18 70 -4.76 0.00
12 20 70 14.38 0.00
14 20 70 -20.67 0.00
16 20 70 -1.34 0.00
18 20 70 4.69 0.00
20 20 70 -4.50 0.00
22 20 70 11.29 0.00
0 22 70 4.76 0.00
2 22 70 6.79 0.00
4 22 70 -8.21 0.00
8 22 70 -1.67 0.00
10 22 70 -4.80 0.00
12 22 70 -2.56 0.00
14 22 70 1.05 0.00
16 22 70 -8.27 0.00
18 22 70 5.46 0.00
20 22 70 -2.65 0.00
2 24 70 10.26 0.00
4 24 70 5.27 0.00
6 24 70 6.43 0.00
8 24 70 15.96 0.00
10 24 70 -17.58 0.00
12 24 70 1.93 0.00
14 24 70 5.79 0.00
16 24 70 4.09 0.00
18 24 70 -9.92 0.00
0 26 70 -0.65 0.00
2 26 70 1.95 0.00
4 26 70 17.18 0.00
6 26 70 -12.40 0.00
8 26 70 7.89 0.00
10 26 70 2.40 0.00
12 26 70 -9.08 0.00
14 26 70 0.97 0.00
2 28 70 6.21 0.00
4 28 70 -1.49 0.00
6 28 70 -6.54 0.00
8 28 70 -8.90 0.00
10 28 70 -10.50 0.00
0 30 70 -7.45 0.00
2 30 70 5.73 0.00
1 1 71 -8.90 0.00
3 1 71 2.39 0.00
5 1 71 -4.63 0.00
7 1 71 -4.03 0.00
9 1 71 -7.44 0.00
11 1 71 3.98 0.00
13 1 71 7.53 0.00
15 1 71 -0.12 0.00
17 1 71 0.61 0.00
19 1 71 3.63 0.00
21 1 71 9.40 0.00
23 1 71 1.62 0.00
25 1 71 6.78 0.00
27 1 71 2.56 0.00
1 3 71 14.84 0.00
3 3 71 11.58 0.00
5 3 71 14.98 0.00
7 3 71 13.12 0.00
9 3 71 16.28 0.00
11 3 71 3.29 0.00
13 3 71 10.17 0.00
15 3 71 3.31 0.00
17 3 71 -5.02 0.00
19 3 71 -3.05 0.00
21 3 71 1.96 0.00
23 3 71 3.31 0.00
25 3 71 -2.43 0.00
27 3 71 2.86 0.00
1 5 71 -6.47 0.00
3 5 71 19.29 0.00
5 5 71 -6.29 0.00
7 5 71 -4.49 0.00
9 5 71 -8.17 0.00
11 5 71 1.00 0.00
13 5 71 0.19 0.00
15 5 71 -7.80 0.00
17 5 71 13.14 0.00
19 5 71 3.74 0.00
21 5 71 10.06 0.00
23 5 71 9.00 0.00
25 5 71 8.89 0.00
27 5 71 -10.05 0.00
1 7 71 -18.72 0.00
3 7 71 18.31 0.00
5 7 71 -5.66 0.00
7 7 71 6.20 0.00
9 7 71 10.03 0.00
11 7 71 -0.48 0.00
13 7 71 1.54 0.00
15 7 71 10.72 0.00
17 7 71 -10.00 0.00
19 7 71 16.19 0.00
21 7 71 -1.13 0.00
23 7 71 4.07 0.00
25 7 71 5.18 0.00
3 9 71 -0.16 0.00
5 9 71 12.73 0.00
7 9 71 -1.26 0.00
9 9 71 -10.26 0.00
11 9 71 -4.45 0.00
13 9 71 -8.47 0.00
15 9 71 -0.98 0.00
17 9 71 1.04 0.00
19 9 71 10.92 0.00
21 9 71 -4.58 0.00
23 9 71 2.27 0.00
25 9 71 3.93 0.00
3 11 71 18.44 0.00
5 11 71 20.07 0.00
7 11 71 -7.15 0.00
9 11 71 5.63 0.00
11 11 71 -20.09 0.00
13 11 71 -4.95 0.00
15 11 71 6.02 0.00
17 11 71 -6.45 0.00
19 11 71 12.97 0.00
21 11 71 -10.39 0.00
23 11 71 -4.67 0.00
25 11 71 -3.49 0.00
5 13 71 28.63 0.00
7 13 71 19.79 0.00
9 13 71 6.00 0.00
11 13 71 3.87 0.00
13 13 71 -9.70 0.00
15 13 71 -10.86 0.00
17 13 71 -21.38 0.00
19 13 71 -2.45 0.00
21 13 71 -20.04 0.00
23 13 71 0.73 0.00
7 15 71 16.90 0.00
9 15 71 -7.13 0.00
11 15 71 10.49 0.00
13 15 71 -12.35 0.00
15 15 71 18.20 0.00
17 15 71 -2.88 0.00
19 15 71 4.74 0.00
21 15 71 -3.40 0.00
23 15 71 -7.73 0.00
1 17 71 7.11 0.00
11 17 71 -8.93 0.00
13 17 71 -6.48 0.00
15 17 71 -17.29 0.00
17 17 71 -2.77 0.00
19 17 71 -3.23 0.00
21 17 71 -6.20 0.00
1 19 71 9.43 0.00
3 19 71 -0.34 0.00
5 19 71 9.39 0.00
7 19 71 10.45 0.00
9 19 71 -1.60 0.00
11 19 71 4.83 0.00
13 19 71 -8.35 0.00
15 19 71 1.86 0.00
17 19 71 -4.40 0.00
19 19 71 -0.04 0.00
1 21 71 5.33 0.00
3 21 71 4.95 0.00
5 21 71 -6.68 0.00
7 21 71 7.87 0.00
9 21 71 -21.33 0.00
11 21 71 15.65 0.00
13 21 71 -5.21 0.00
15 21 71 -3.68 0.00
17 21 71 5.37 0.00
1 23 71 -8.56 0.00
3 23 71 11.55 0.00
5 23 71 4.67 0.00
7 23 71 -9.38 0.00
9 23 71 -13.95 0.00
11 23 71 -9.61 0.00
13 23 71 -1.28 0.00
15 23 71 -20.66 0.00
1 25 71 8.42 0.00
3 25 71 -14.92 0.00
5 25 71 -6.03 0.00
7 25 71 -7.09 0.00
9 25 71 -18.06 0.00
11 25 71 -1.51 0.00
1 27 71 0.62 0.00
3 27 71 4.65 0.00
5 27 71 -8.37 0.00
0 0 72 3.96 0.00
4 0 72 6.50 0.00
8 0 72 -15.87 0.00
12 0 72 -12.55 0.00
16 0 72 -24.23 0.00
20 0 72 6.45 0.00
24 0 72 8.47 0.00
2 2 72 6.74 0.00
4 2 72 8.94 0.00
6 2 72 1.36 0.00
8 2 72 -3.41 0.00
10 2 72 2.85 0.00
12 2 72 4.86 0.00
14 2 72 -4.62 0.00
16 2 72 8.84 0.00
18 2 72 8.68 0.00
20 2 72 -4.01 0.00
22 2 72 5.10 0.00
24 2 72 -1.29 0.00
0 4 72 0.68 0.00
2 4 72 4.76 0.00
4 4 72 3.36 0.00
6 4 72 -0.76 0.00
8 4 72 8.55 0.00
10 4 72 -6.88 0.00
12 4 72 2.24 0.00
14 4 72 2.16 0.00
16 4 72 -9.17 0.00
18 4 72 -3.26 0.00
20 4 72 0.11 0.00
22 4 72 -1.92 0.00
24 4 72 7.66 0.00
2 6 72 -1.25 0.00
4 6 72 -4.81 0.00
6 6 72 -11.65 0.00
8 6 72 -1.24 0.00
10 6 72 -5.53 0.00
12 6 72 -0.20 0.00
14 6 72 -2.92 0.00
16 6 72 3.82 0.00
18 6 72 8.09 0.00
20 6 72 -6.95 0.00
22 6 72 5.22 0.00
24 6 72 4.52 0.00
0 8 72 -19.15 0.00
2 8 72 2.29 0.00
4 8 72 -4.27 0.00
6 8 72 -3.75 0.00
8 8 72 5.50 0.00
10 8 72 6.68 0.00
12 8 72 -4.82 0.00
14 8 72 9.68 0.00
16 8 72 11.79 0.00
18 8 72 4.59 0.00
20 8 72 -0.40 0.00
22 8 72 0.95 0.00
2 10 72 -10.61 0.00
4 10 72 7.69 0.00
6 10 72 -0.24 0.00
8 10 72 -4.89 0.00
10 10 72 -11.02 0.00
12 10 72 -17.34 0.00
14 10 72 -8.00 0.00
16 10 72 -6.42 0.00
18 10 72 9.01 0.00
20 10 72 -7.16 0.00
22 10 72 8.69 0.00
0 12 72 23.10 0.00
2 12 72 21.61 0.00
4 12 72 27.24 0.00
6 12 72 -2.14 0.00
8 12 72 -5.19 0.00
10 12 72 -12.35 0.00
12 12 72 -3.00 0.00
14 12 72 -5.96 0.00
16 12 72 3.70 0.00
18 12 72 1.57 0.00
20 12 72 1.70 0.00
2 14 72 -0.20 0.00
4 14 72 17.29 0.00
6 14 72 0.70 0.00
8 14 72 -3.49 0.00
10 14 72 -4.33 0.00
12 14 72 -1.66 0.00
14 14 72 -2.38 0.00
16 14 72 -11.37 0.00
18 14 72 9.11 0.00
20 14 72 -4.37 0.00
0 16 72 -12.52 0.00
2 16 72 14.45 0.00
4 16 72 -0.38 0.00
6 16 72 -1.46 0.00
8 16 72 -2.31 0.00
10 16 72 -0.08 0.00
12 16 72 -6.24 0.00
14 16 72 5.23 0.00
16 16 72 -1.85 0.00
18 16 72 3.07 0.00
2 18 72 9.32 0.00
4 18 72 1.57 0.00
6 18 72 7.83 0.00
8 18 72 1.17 0.00
10 18 72 6.63 0.00
12 18 72 5.61 0.00
14 18 72 0.83 0.00
16 18 72 3.59 0.00
0 20 72 -5.50 0.00
2 20 72 11.13 0.00
4 20 72 -0.10 0.00
6 20 72 -8.09 0.00
8 20 72 3.28 0.00
10 20 72 -5.06 0.00
12 20 72 6.80 0.00
14 20 72 5.25 0.00
2 22 72 3.74 0.00
4 22 72 -14.81 0.00
6 22 72 2.45 0.00
8 22 72 -3.79 0.00
10 22 72 4.25 0.00
0 24 72 -14.68 0.00
2 24 72 7.64 0.00
4 24 72 0.55 0.00
6 24 72 -8.34 0.00
0 0 0 0.00 0.00
# SQUEEZE RESULTS (Version = 250420)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.033 -0.008 0.250 93997 12622 ' '
2 0.499 -0.001 -0.001 582 128 ' '
3 0.750 0.000 0.250 576 126 ' '
4 0.018 -0.001 0.499 582 128 ' '
5 0.250 0.000 0.750 576 126 ' '
6 0.625 0.125 0.125 7 -1 ' '
7 0.125 0.125 0.625 7 -1 ' '
8 0.750 0.250 0.000 606 160 ' '
9 0.500 0.250 0.250 606 160 ' '
10 0.250 0.250 0.500 606 160 ' '
11 0.000 0.250 0.750 606 160 ' '
12 0.375 0.375 0.375 7 -1 ' '
13 0.875 0.375 0.875 7 -1 ' '
14 0.250 0.500 0.250 606 150 ' '
15 0.500 0.500 0.500 606 150 ' '
16 0.750 0.500 0.750 606 150 ' '
17 1.000 0.500 1.000 606 150 ' '
18 0.125 0.625 0.125 7 -1 ' '
19 0.625 0.625 0.625 7 -1 ' '
20 0.250 0.750 0.000 562 124 ' '
21 0.333 0.751 0.251 568 126 ' '
22 0.749 0.750 0.500 562 124 ' '
23 0.499 0.751 0.751 568 126 ' '
24 0.875 0.875 0.375 7 -1 ' '
25 0.375 0.875 0.875 7 -1 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 1 1.312
0 2 2 2.143
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details
)
TITL 20200607-HFP-TY-Zn54 in Fd-3 #203
CELL 58.3017 58.3017 58.3017 90.00 90.00 90.00
SPGR Fd-3
# Solvent Accessible Volume = 115446
# Electrons Found in S.A.V. = 14853
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.277 0.473 0.473 ! 3.21 eA-3
C102 0.835 0.498 0.042 ! 2.43 eA-3
C103 0.968 0.465 0.133 ! 2.32 eA-3
C104 0.667 0.199 0.080 ! 2.28 eA-3
C105 0.737 0.317 0.190 ! 2.26 eA-3
C106 0.636 0.446 0.434 ! 2.07 eA-3
C107 0.470 0.194 0.442 ! 2.02 eA-3
C108 1.000 0.500 0.000 ! 1.89 eA-3
C109 0.217 0.435 0.055 ! 1.85 eA-3
C110 0.550 0.180 0.224 ! 1.83 eA-3
C111 0.327 0.431 0.109 ! 1.78 eA-3
C112 0.828 0.481 0.042 ! 1.74 eA-3
C113 0.637 0.453 0.457 ! 1.69 eA-3
C114 0.719 0.032-0.003 ! 1.61 eA-3
C115 0.780 0.034 0.457 ! 1.58 eA-3
C116 0.710 0.193 0.082 ! 1.54 eA-3
C117 0.451 0.333 0.309 ! 1.52 eA-3
C118 0.928 0.004 0.195 ! 1.48 eA-3
C119 0.544 0.171 0.379 ! 1.48 eA-3
C120 0.456 0.300 0.354 ! 1.48 eA-3
C121 0.603 0.195 0.207 ! 1.44 eA-3
C122 0.102 0.309 0.472 ! 1.43 eA-3
C123 0.296 0.106 0.421 ! 1.43 eA-3
C124 0.673 0.084 0.394 ! 1.34 eA-3
C125 0.540 0.210 0.210 ! 1.23 eA-3
C126 0.951 0.060 0.231 ! 1.21 eA-3
C127 0.764 0.246 0.023 ! 1.06 eA-3
C128 0.643 0.308 0.339 ! 1.05 eA-3
C129 0.952 0.477 0.212 ! 1.00 eA-3
C130 0.325 0.421 0.090 ! 0.97 eA-3
C131 0.251 0.398 0.681 ! 0.96 eA-3
C132 0.751 0.398 0.181 ! 0.96 eA-3
C133 0.749 0.102 0.819 ! 0.96 eA-3
C134 0.888 0.165 0.267 ! 0.94 eA-3
C135 0.900 0.070 1.000 ! 0.93 eA-3
C136 0.759 0.086 0.452 ! 0.92 eA-3
C137 0.485 0.265 0.265 ! 0.91 eA-3
Q138 0.655 0.305 0.367 ! 0.89 eA-3
C139 0.776 0.239 0.015 ! 0.87 eA-3
C140 0.768 0.378 0.172 ! 0.85 eA-3
C141 0.389 0.457 0.681 ! 0.83 eA-3
C142 0.889 0.457 0.181 ! 0.83 eA-3
C143 0.756 0.402 0.167 ! 0.83 eA-3
C144 0.425 0.016 0.434 ! 0.77 eA-3
C145 0.234 0.017 0.352 ! 0.77 eA-3
C146 0.762 0.142 0.476 ! 0.77 eA-3
C147 0.028 0.434 0.269 ! 0.75 eA-3
C148 0.117 0.487 0.492 ! 0.74 eA-3
C149 0.254 0.115 0.301 ! 0.71 eA-3
C150 0.512 0.399 0.055 ! 0.70 eA-3
C151 0.985 0.016 0.004 ! 0.69 eA-3
C152 0.318 0.436 0.314 ! 0.65 eA-3
C153 0.189 0.020 0.339 ! 0.64 eA-3
Q154 0.342 0.039 0.132 ! 0.64 eA-3
Q155 0.232 0.024 0.365 ! 0.63 eA-3
C156 0.813 0.160 0.331 ! 0.59 eA-3
Q157 0.308 0.340 0.302 ! 0.59 eA-3
C158 0.695 0.096 0.451 ! 0.59 eA-3
C159 0.695 0.596 0.951 ! 0.59 eA-3
C160 0.013 0.436 0.273 ! 0.58 eA-3
C161 0.107 0.333 0.043 ! 0.58 eA-3
C162 0.047 0.101 0.318 ! 0.58 eA-3
C163 0.547 0.101 0.818 ! 0.58 eA-3
C164 0.684 0.951 0.897 ! 0.57 eA-3
C165 0.691 0.481 0.293 ! 0.56 eA-3
C166 0.012 0.445 0.265 ! 0.55 eA-3
C167 0.282 0.023 0.272 ! 0.54 eA-3
C168 0.476 0.196 0.016 ! 0.54 eA-3
C169 0.686 0.199 0.059 ! 0.53 eA-3
C170 0.291 0.476 0.016 ! 0.53 eA-3
Q171 0.445 0.289 0.173 ! 0.53 eA-3
C172 0.085 0.041 0.309 ! 0.53 eA-3
C173 0.570 0.204 0.447 ! 0.52 eA-3
Q174 0.356 0.465 0.394 ! 0.52 eA-3
C175 0.297 0.007 0.046 ! 0.52 eA-3
C176 0.714 0.457 0.307 ! 0.52 eA-3
C177 0.341 0.021 0.225 ! 0.51 eA-3
C178 0.608 0.404 0.212 ! 0.51 eA-3
C179 0.227 0.257 0.004 ! 0.51 eA-3
C180 0.389 0.473 0.069 ! 0.51 eA-3
)
;
_shelx_fab_checksum 69108
_platon_squeeze_special_details
;
A solvent mask was calculated and 14782 electrons were
found in a volume of 103277\%A^3^ in 7 voids per unit cell.
This is consistent with the presence of
16[C3H8O2], 30[C3H7NO] per formula unit
which account for 14976 electrons
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.746
_oxdiff_exptl_absorpt_empirical_full_min 0.812