# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
#TrackingRef '- mdbm37.cif'
_audit_update_record
;
2012-04-27 # Formatted by publCIF
;
_audit_creation_date 12-03-05
_audit_creation_method CRYSTALS_ver_14.40
_oxford_structure_analysis_title 'p21a in P2(1)/c'
_chemical_name_systematic ?
_chemical_melting_point ?
_publ_contact_author_name 'Barboiu, M.'
_publ_contact_author_address
;
Institut Europeen des Membranes,
Universite de Montpellier II,
Montpellier
France
;
_publ_section_title
# Title of paper - generally just the systematic or trivial name
;
Self-sorting of metallosupramolecular DCLs via double-level exchange:
amplification in solution and solid state modulation.
;
_publ_section_exptl_refinement
# Some potentially useful phrases are donated by Bill Clegg:
;
The H atoms were all located in a difference map, but those attached to carbon
atoms were repositioned geometrically. The H atoms were initially refined with
soft restraints on the bond lengths and angles to regularize their geometry
(C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86
O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2--1.5 times
U~eq~ of the parent atom), after which the positions were refined with
riding constraints (Cooper et al., 2010).
Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl.
Cryst. 43, 1100--1107.
;
_publ_contact_author_email barboiu@iemm.univ-montp2.fr
loop_
_publ_author_name
F.Dumitru
Y.M.Legrand
E.Petit
'A.Van der Lee'
M.Barboiu
data_1_mdbm37
_database_code_depnum_ccdc_archive 'CCDC 879235'
#TrackingRef '- mdbm37.cif'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details ?
_cell_length_a 25.4340(16)
_cell_length_b 8.3120(5)
_cell_length_c 23.7330(14)
_cell_angle_alpha 90
_cell_angle_beta 113.340(2)
_cell_angle_gamma 90
_cell_volume 4606.8(5)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/c 1 '
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0010 0.0007 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0028 0.0016 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0046 0.0029 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0077 0.0049 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.0692 0.0633 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zn 0.3321 0.8009 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C2 H2 F2 N2 O2 S2 Zn2
# Dc = 0.46 Fooo = 2158.95 Mu = 11.30 M = 318.94
# Found Formula = C44 H34.64 F6 N8 O8.64 S2 Zn1
# Dc = 1.52 FOOO = 2158.95 Mu = 7.12 M = 1057.15
_chemical_formula_sum 'C44 H34.64 F6 N8 O8.64 S2 Zn'
_chemical_formula_moiety
'C38 H28.64 N6 O2.64 Zn, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_compound_source ?
_chemical_formula_weight 1057.15
_cell_measurement_reflns_used 0
_cell_measurement_theta_min 0
_cell_measurement_theta_max 0
_cell_measurement_temperature 120
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.250
_exptl_crystal_density_diffrn 1.524
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 2158.953
_exptl_absorpt_coefficient_mu 0.712
# Sheldrick geometric approximatio 0.87 0.93
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.85
_exptl_absorpt_correction_T_max 0.93
_diffrn_measurement_device_type 'Bruker SMART'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.50915
_diffrn_measurement_method '\f scans'
_montpellier_reflns_maxres 0.701
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SMART (Siemens, 1993)'
_computing_cell_refinement 'SAINT (Siemens ,1995)'
_computing_data_reduction 'USER DEFINED DATA REDUCTION'
_computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 68831
_reflns_number_total 13674
_diffrn_reflns_av_R_equivalents 0.038
_diffrn_reflns_av_sigmaI/netI 0.0312
# Number of reflections without Friedels Law is 13674
# Number of reflections with Friedels Law is 0
# Theoretical number of reflections is about 13985
_diffrn_reflns_theta_min 0.625
_diffrn_reflns_theta_max 21.292
_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full 20.867
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_h_max 36
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_limit_l_max 33
_reflns_limit_h_min -36
_reflns_limit_h_max 33
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 33
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.89
_refine_diff_density_max 0.83
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns 11254
_refine_ls_number_restraints 32
_refine_ls_number_parameters 656
_oxford_refine_ls_R_factor_ref 0.0451
_refine_ls_wR_factor_ref 0.0401
_refine_ls_goodness_of_fit_ref 1.0501
_refine_ls_shift/su_max 0.0047480
_refine_ls_shift/su_mean 0.0000505
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 13656
_refine_ls_R_factor_all 0.0530
_refine_ls_wR_factor_all 0.0477
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 11254
_refine_ls_R_factor_gt 0.0451
_refine_ls_wR_factor_gt 0.0401
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.519 0.538 0.285
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User defined data reduction
Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J.
(2003). J. Appl. Cryst. 36, 1487--?.
Prince, E. Mathematical Techniques in Crystallography and Materials Science
Springer-Verlag, New York, 1982.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software
Package; Madison, WI.
Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector
Integration Software.; Madison, WI.
Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector
Absorption Correction;: Madison, WI.
Watkin, D. J. (1994). Acta Cryst. A50, 411--437.
Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Zn1 Zn 0.277545(5) 0.052193(15) 0.569384(6) 0.0152 1.0000 Uani . . . . . .
N2 N 0.24554(4) 0.05138(10) 0.47548(4) 0.0147 1.0000 Uani . . . . . .
C3 C 0.20439(4) 0.15658(13) 0.44358(5) 0.0157 1.0000 Uani . . . . . .
C4 C 0.18421(4) 0.26028(12) 0.48182(5) 0.0162 1.0000 Uani . . . . . .
N5 N 0.21194(4) 0.25499(11) 0.54036(4) 0.0153 1.0000 Uani . . . . . .
C6 C 0.19414(4) 0.35016(12) 0.57953(5) 0.0150 1.0000 Uani . . . . . .
C7 C 0.13628(4) 0.37778(13) 0.56780(5) 0.0168 1.0000 Uani . . . . . .
C8 C 0.12167(5) 0.47418(14) 0.60749(5) 0.0189 1.0000 Uani . . . . . .
C9 C 0.16473(5) 0.54233(13) 0.65932(5) 0.0193 1.0000 Uani D U . . . .
O10 O 0.15260(4) 0.63846(13) 0.69926(5) 0.0234 0.855(5) Uani D U P . . .
H101 H 0.1180(4) 0.650(3) 0.6873(7) 0.0468 0.855(5) Uiso D . P . . .
C11 C 0.22251(5) 0.51360(14) 0.67172(5) 0.0208 1.0000 Uani . . . . . .
C12 C 0.23697(4) 0.41681(13) 0.63205(5) 0.0185 1.0000 Uani . . . . . .
H121 H 0.2760 0.3981 0.6409 0.0236 1.0000 Uiso R . . . . .
H111 H 0.2502 0.5613 0.7069 0.0247 1.0000 Uiso R . . . . .
H81 H 0.0838 0.4952 0.6005 0.0234 1.0000 Uiso R . . . . .
H71 H 0.1080 0.3295 0.5339 0.0205 1.0000 Uiso R . . . . .
H41 H 0.1522 0.3249 0.4629 0.0195 1.0000 Uiso R . . . . .
C13 C 0.18488(5) 0.16893(14) 0.37968(5) 0.0194 1.0000 Uani . . . . . .
C14 C 0.20964(5) 0.06896(15) 0.34942(5) 0.0218 1.0000 Uani . . . . . .
C15 C 0.25241(5) -0.04017(14) 0.38306(5) 0.0199 1.0000 Uani . . . . . .
C16 C 0.26949(4) -0.04457(12) 0.44679(5) 0.0160 1.0000 Uani . . . . . .
C17 C 0.31518(4) -0.15109(13) 0.48797(5) 0.0177 1.0000 Uani . . . . . .
N18 N 0.32755(4) -0.14452(11) 0.54612(4) 0.0163 1.0000 Uani . . . . . .
C19 C 0.37353(4) -0.23904(12) 0.58726(5) 0.0166 1.0000 Uani . . . . . .
C20 C 0.37005(5) -0.29314(14) 0.64153(5) 0.0208 1.0000 Uani . . . . . .
C21 C 0.41298(5) -0.39098(15) 0.68231(6) 0.0224 1.0000 Uani . . . . . .
C22 C 0.46018(5) -0.43365(14) 0.66898(5) 0.0208 1.0000 Uani D U . . . .
O23 O 0.49960(5) -0.53843(14) 0.70873(5) 0.0246 0.815(5) Uani D U P . . .
H231 H 0.5183(9) -0.581(3) 0.6914(5) 0.0514 0.815(5) Uiso D . P . . .
C24 C 0.46512(5) -0.37457(14) 0.61620(5) 0.0210 1.0000 Uani . . . . . .
C25 C 0.42211(5) -0.27708(14) 0.57544(5) 0.0192 1.0000 Uani . . . . . .
H251 H 0.4254 -0.2378 0.5400 0.0236 1.0000 Uiso R . . . . .
H241 H 0.4980 -0.4019 0.6097 0.0242 1.0000 Uiso R . . . . .
H211 H 0.4104 -0.4293 0.7182 0.0274 1.0000 Uiso R . . . . .
H201 H 0.3389 -0.2661 0.6515 0.0251 1.0000 Uiso R . . . . .
H171 H 0.3349 -0.2197 0.4720 0.0208 1.0000 Uiso R . . . . .
H151 H 0.2707 -0.1063 0.3649 0.0249 1.0000 Uiso R . . . . .
H141 H 0.1983 0.0754 0.3084 0.0272 1.0000 Uiso R . . . . .
H131 H 0.1565 0.2397 0.3595 0.0232 1.0000 Uiso R . . . . .
N26 N 0.31196(4) 0.06815(11) 0.66349(4) 0.0190 1.0000 Uani . . . . . .
C27 C 0.36187(5) 0.14519(14) 0.69216(5) 0.0227 1.0000 Uani . . . . . .
C28 C 0.38822(5) 0.20496(14) 0.65085(6) 0.0231 1.0000 Uani . . . . . .
N29 N 0.35706(4) 0.20255(11) 0.59285(5) 0.0205 1.0000 Uani . . . . . .
C30 C 0.37736(5) 0.26712(14) 0.54988(6) 0.0212 1.0000 Uani . . . . . .
C31 C 0.33833(5) 0.35754(14) 0.50135(6) 0.0218 1.0000 Uani . . . . . .
C32 C 0.35587(5) 0.42967(14) 0.45915(6) 0.0228 1.0000 Uani . . . . . .
C33 C 0.41238(5) 0.41051(16) 0.46432(6) 0.0255 1.0000 Uani D U . . . .
O34 O 0.43127(9) 0.4702(3) 0.42928(10) 0.0265 0.439(4) Uani D U P . . .
H341 H 0.411(2) 0.546(7) 0.411(3) 0.1169 0.439(4) Uiso D . P . . .
C35 C 0.45062(5) 0.31535(17) 0.51141(6) 0.0280 1.0000 Uani . . . . . .
C36 C 0.43352(5) 0.24381(16) 0.55422(6) 0.0260 1.0000 Uani . . . . . .
H361 H 0.4581 0.1774 0.5865 0.0320 1.0000 Uiso R . . . . .
H351 H 0.4872 0.2993 0.5145 0.0337 1.0000 Uiso R . . . . .
H321 H 0.3301 0.4886 0.4286 0.0266 1.0000 Uiso R . . . . .
H311 H 0.3006 0.3721 0.5000 0.0252 1.0000 Uiso R . . . . .
H281 H 0.4264 0.2433 0.6680 0.0282 1.0000 Uiso R . . . . .
C37 C 0.38293(6) 0.17626(16) 0.75534(6) 0.0317 1.0000 Uani . . . . . .
C38 C 0.35028(7) 0.12731(18) 0.78744(6) 0.0356 1.0000 Uani . . . . . .
C39 C 0.29817(7) 0.04746(17) 0.75709(6) 0.0303 1.0000 Uani . . . . . .
C40 C 0.28053(5) 0.01997(14) 0.69403(5) 0.0209 1.0000 Uani . . . . . .
C41 C 0.22609(5) -0.05948(13) 0.65514(5) 0.0202 1.0000 Uani . . . . . .
N42 N 0.21480(4) -0.07382(11) 0.59738(4) 0.0168 1.0000 Uani . . . . . .
C43 C 0.16102(4) -0.13818(13) 0.55723(5) 0.0169 1.0000 Uani . . . . . .
C44 C 0.11015(5) -0.09834(14) 0.56401(5) 0.0206 1.0000 Uani . . . . . .
C45 C 0.05862(5) -0.16571(15) 0.52439(6) 0.0234 1.0000 Uani . . . . . .
C46 C 0.05792(5) -0.27352(14) 0.47901(6) 0.0224 1.0000 Uani D U . . . .
O47 O 0.00861(7) -0.3400(2) 0.44750(9) 0.0273 0.529(4) Uani D U P . . .
H471 H 0.0137(2) -0.430(4) 0.437(3) 0.0983 0.529(4) Uiso D . P . . .
C48 C 0.10841(5) -0.30927(14) 0.47117(5) 0.0203 1.0000 Uani . . . . . .
C49 C 0.16003(5) -0.23983(13) 0.50982(5) 0.0181 1.0000 Uani . . . . . .
H491 H 0.1945 -0.2647 0.5060 0.0223 1.0000 Uiso R . . . . .
H481 H 0.1069 -0.3798 0.4407 0.0253 1.0000 Uiso R . . . . .
H451 H 0.0243 -0.1378 0.5289 0.0279 1.0000 Uiso R . . . . .
H441 H 0.1115 -0.0269 0.5961 0.0243 1.0000 Uiso R . . . . .
H411 H 0.2007 -0.0962 0.6730 0.0240 1.0000 Uiso R . . . . .
H391 H 0.2754 0.0145 0.7786 0.0356 1.0000 Uiso R . . . . .
H381 H 0.3625 0.1465 0.8296 0.0424 1.0000 Uiso R . . . . .
H371 H 0.4170 0.2266 0.7752 0.0375 1.0000 Uiso R . . . . .
S50 S 0.016342(11) 0.31165(3) 0.354978(13) 0.0197 1.0000 Uani . . . . . .
O51 O 0.06199(4) 0.36745(12) 0.33849(6) 0.0338 1.0000 Uani . . . . . .
O52 O -0.04116(4) 0.32809(14) 0.30893(5) 0.0346 1.0000 Uani . . . . . .
O53 O 0.02212(6) 0.35879(14) 0.41613(5) 0.0400 1.0000 Uani . . . . . .
C54 C 0.02650(6) 0.09361(16) 0.36202(8) 0.0300 1.0000 Uani . . . . . .
F55 F -0.01455(4) 0.02149(10) 0.37439(4) 0.0316 1.0000 Uani . . . . . .
F56 F 0.02603(8) 0.03015(12) 0.31036(8) 0.0695 1.0000 Uani . . . . . .
F57 F 0.07648(5) 0.05713(15) 0.40755(9) 0.0721 1.0000 Uani . . . . . .
S58 S 0.383363(12) -0.20374(4) 0.336752(13) 0.0250 1.0000 Uani . . . . . .
O59 O 0.35072(6) -0.27884(12) 0.36690(5) 0.0361 1.0000 Uani . . . . . .
O60 O 0.43379(5) -0.2936(2) 0.34184(7) 0.0573 1.0000 Uani . . . . . .
O61 O 0.34983(5) -0.1383(2) 0.27742(6) 0.0568 1.0000 Uani . . . . . .
C62 C 0.41284(6) -0.02623(17) 0.38525(8) 0.0347 1.0000 Uani . . . . . .
F63 F 0.37073(5) 0.07199(12) 0.38412(7) 0.0559 1.0000 Uani . . . . . .
F64 F 0.44294(5) -0.06781(13) 0.44351(5) 0.0495 1.0000 Uani . . . . . .
F65 F 0.44768(5) 0.05769(17) 0.36670(8) 0.0706 1.0000 Uani . . . . . .
N66 N 0.21532(5) -0.43393(15) 0.41192(6) 0.0330 1.0000 Uani . . . . . .
C67 C 0.17780(5) -0.38188(15) 0.37068(6) 0.0240 1.0000 Uani . . . . . .
C68 C 0.12983(6) -0.31354(18) 0.31880(7) 0.0317 1.0000 Uani . . . . . .
H681 H 0.1412 -0.3001 0.2852 0.0481 1.0000 Uiso R . . . . .
H682 H 0.0984 -0.3855 0.3093 0.0478 1.0000 Uiso R . . . . .
H683 H 0.1191 -0.2126 0.3308 0.0482 1.0000 Uiso R . . . . .
N69 N 0.15719(8) 0.1073(2) 0.73127(8) 0.0508 1.0000 Uani . . . . . .
C70 C 0.11718(7) 0.18327(17) 0.72101(6) 0.0326 1.0000 Uani . . . . . .
C71 C 0.06666(7) 0.28095(18) 0.70946(7) 0.0349 1.0000 Uani . . . . . .
H711 H 0.0467 0.2878 0.6663 0.0523 1.0000 Uiso R . . . . .
H712 H 0.0437 0.2339 0.7281 0.0511 1.0000 Uiso R . . . . .
H713 H 0.0774 0.3878 0.7256 0.0526 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01250(6) 0.01514(6) 0.01637(6) -0.00110(4) 0.00396(4) 0.00064(4)
N2 0.0118(3) 0.0138(4) 0.0179(4) -0.0008(3) 0.0054(3) 0.0004(3)
C3 0.0120(4) 0.0153(4) 0.0188(4) -0.0008(3) 0.0048(3) 0.0008(3)
C4 0.0132(4) 0.0149(4) 0.0195(4) -0.0001(3) 0.0054(3) 0.0028(3)
N5 0.0126(3) 0.0135(4) 0.0191(4) -0.0011(3) 0.0055(3) 0.0006(3)
C6 0.0140(4) 0.0133(4) 0.0165(4) 0.0003(3) 0.0048(3) 0.0021(3)
C7 0.0136(4) 0.0174(4) 0.0188(4) 0.0000(3) 0.0059(3) -0.0001(3)
C8 0.0159(4) 0.0205(5) 0.0222(5) 0.0005(4) 0.0095(4) 0.0004(4)
C9 0.0225(5) 0.0171(4) 0.0198(4) -0.0004(4) 0.0099(4) 0.0016(4)
O10 0.0233(4) 0.0259(5) 0.0227(4) -0.0061(3) 0.0109(3) 0.0018(3)
C11 0.0199(5) 0.0194(5) 0.0199(5) -0.0031(4) 0.0045(4) 0.0014(4)
C12 0.0135(4) 0.0179(4) 0.0207(4) -0.0014(4) 0.0031(3) 0.0030(3)
C13 0.0160(4) 0.0213(5) 0.0188(4) 0.0008(4) 0.0046(4) 0.0034(4)
C14 0.0201(5) 0.0270(5) 0.0173(4) -0.0004(4) 0.0063(4) 0.0038(4)
C15 0.0183(4) 0.0221(5) 0.0205(5) -0.0022(4) 0.0091(4) 0.0023(4)
C16 0.0135(4) 0.0150(4) 0.0196(4) -0.0014(3) 0.0066(3) 0.0009(3)
C17 0.0155(4) 0.0152(4) 0.0223(5) -0.0017(4) 0.0075(4) 0.0026(3)
N18 0.0140(3) 0.0136(4) 0.0218(4) -0.0004(3) 0.0076(3) 0.0011(3)
C19 0.0151(4) 0.0136(4) 0.0208(4) -0.0009(3) 0.0067(3) 0.0023(3)
C20 0.0214(5) 0.0192(5) 0.0251(5) 0.0021(4) 0.0129(4) 0.0058(4)
C21 0.0233(5) 0.0216(5) 0.0244(5) 0.0045(4) 0.0115(4) 0.0062(4)
C22 0.0160(4) 0.0205(5) 0.0238(5) 0.0013(4) 0.0055(4) 0.0026(4)
O23 0.0182(5) 0.0264(5) 0.0271(5) 0.0048(4) 0.0067(4) 0.0071(3)
C24 0.0134(4) 0.0243(5) 0.0249(5) 0.0006(4) 0.0071(4) 0.0026(4)
C25 0.0154(4) 0.0215(5) 0.0215(5) 0.0009(4) 0.0080(4) 0.0022(4)
N26 0.0174(4) 0.0157(4) 0.0188(4) -0.0014(3) 0.0017(3) 0.0045(3)
C27 0.0180(5) 0.0172(5) 0.0232(5) -0.0009(4) -0.0023(4) 0.0050(4)
C28 0.0144(4) 0.0171(5) 0.0295(6) -0.0029(4) -0.0002(4) 0.0012(3)
N29 0.0132(4) 0.0146(4) 0.0282(5) -0.0007(3) 0.0022(3) 0.0017(3)
C30 0.0121(4) 0.0166(4) 0.0298(5) -0.0037(4) 0.0029(4) -0.0004(3)
C31 0.0130(4) 0.0183(5) 0.0305(5) -0.0017(4) 0.0048(4) -0.0001(3)
C32 0.0172(5) 0.0199(5) 0.0281(5) -0.0046(4) 0.0057(4) -0.0015(4)
C33 0.0193(5) 0.0263(5) 0.0303(6) -0.0096(5) 0.0092(4) -0.0033(4)
O34 0.0209(7) 0.0306(8) 0.0298(7) -0.0037(6) 0.0119(6) -0.0025(6)
C35 0.0144(4) 0.0327(6) 0.0352(6) -0.0091(5) 0.0078(4) 0.0003(4)
C36 0.0128(4) 0.0261(5) 0.0336(6) -0.0047(5) 0.0035(4) 0.0025(4)
C37 0.0298(6) 0.0253(6) 0.0229(5) -0.0013(4) -0.0077(5) 0.0035(5)
C38 0.0440(8) 0.0328(7) 0.0165(5) -0.0007(5) -0.0025(5) 0.0045(6)
C39 0.0385(7) 0.0300(6) 0.0168(5) 0.0033(4) 0.0050(5) 0.0064(5)
C40 0.0239(5) 0.0180(5) 0.0171(4) 0.0015(4) 0.0041(4) 0.0057(4)
C41 0.0224(5) 0.0192(5) 0.0194(5) 0.0018(4) 0.0089(4) 0.0032(4)
N42 0.0174(4) 0.0142(4) 0.0192(4) 0.0001(3) 0.0079(3) 0.0013(3)
C43 0.0170(4) 0.0162(4) 0.0186(4) 0.0016(3) 0.0083(3) -0.0002(3)
C44 0.0201(5) 0.0212(5) 0.0236(5) -0.0002(4) 0.0118(4) 0.0017(4)
C45 0.0181(5) 0.0251(5) 0.0295(5) 0.0025(4) 0.0121(4) 0.0013(4)
C46 0.0192(5) 0.0201(5) 0.0276(5) 0.0014(4) 0.0091(4) -0.0018(4)
O47 0.0193(6) 0.0270(7) 0.0313(7) -0.0051(6) 0.0053(5) -0.0036(5)
C48 0.0208(5) 0.0182(5) 0.0228(5) -0.0018(4) 0.0096(4) -0.0023(4)
C49 0.0179(4) 0.0168(4) 0.0218(5) -0.0006(4) 0.0101(4) -0.0008(3)
S50 0.01436(11) 0.01751(12) 0.02652(13) -0.00161(9) 0.00737(9) -0.00032(8)
O51 0.0293(5) 0.0226(4) 0.0602(7) 0.0103(4) 0.0291(5) 0.0024(3)
O52 0.0212(4) 0.0362(5) 0.0371(5) 0.0019(4) 0.0018(4) 0.0018(4)
O53 0.0541(7) 0.0356(6) 0.0316(5) -0.0130(4) 0.0185(5) -0.0190(5)
C54 0.0278(6) 0.0198(5) 0.0525(8) 0.0051(5) 0.0267(6) 0.0019(4)
F55 0.0336(4) 0.0251(4) 0.0450(5) -0.0065(3) 0.0250(4) -0.0114(3)
F56 0.1323(13) 0.0228(4) 0.1065(11) -0.0118(5) 0.1039(11) -0.0063(6)
F57 0.0287(5) 0.0452(6) 0.1290(13) 0.0522(7) 0.0171(6) 0.0084(4)
S58 0.01621(12) 0.04027(17) 0.01925(12) 0.00314(11) 0.00765(9) 0.00782(11)
O59 0.0551(7) 0.0213(4) 0.0427(6) -0.0004(4) 0.0310(5) -0.0034(4)
O60 0.0196(5) 0.0897(11) 0.0516(7) -0.0362(7) 0.0025(5) 0.0176(6)
O61 0.0313(6) 0.1049(13) 0.0267(5) 0.0255(7) 0.0036(4) 0.0031(7)
C62 0.0223(6) 0.0255(6) 0.0510(8) 0.0098(6) 0.0089(5) 0.0029(5)
F63 0.0331(5) 0.0216(4) 0.1036(10) -0.0042(5) 0.0171(6) 0.0059(3)
F64 0.0546(6) 0.0389(5) 0.0383(5) -0.0103(4) 0.0008(5) 0.0084(4)
F65 0.0318(5) 0.0655(8) 0.1070(12) 0.0325(8) 0.0196(6) -0.0145(5)
N66 0.0289(5) 0.0307(6) 0.0357(6) 0.0024(5) 0.0088(5) 0.0022(4)
C67 0.0256(5) 0.0213(5) 0.0271(5) -0.0001(4) 0.0124(4) -0.0017(4)
C68 0.0292(6) 0.0307(6) 0.0304(6) 0.0093(5) 0.0069(5) -0.0014(5)
N69 0.0476(8) 0.0519(9) 0.0530(9) -0.0087(7) 0.0201(7) 0.0046(7)
C70 0.0437(8) 0.0276(6) 0.0263(6) -0.0053(5) 0.0138(5) -0.0050(5)
C71 0.0465(8) 0.0273(6) 0.0311(6) 0.0007(5) 0.0155(6) 0.0009(6)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.17974(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . N2 . 2.0475(9) yes
Zn1 . N5 . 2.2781(9) yes
Zn1 . N18 . 2.2700(9) yes
Zn1 . N26 . 2.0550(10) yes
Zn1 . N29 . 2.2516(10) yes
Zn1 . N42 . 2.2194(9) yes
N2 . C3 . 1.3436(13) yes
N2 . C16 . 1.3412(13) yes
C3 . C4 . 1.4831(14) yes
C3 . C13 . 1.4000(15) yes
C4 . N5 . 1.2858(13) yes
C4 . H41 . 0.929 no
N5 . C6 . 1.4241(13) yes
C6 . C7 . 1.4040(14) yes
C6 . C12 . 1.4042(14) yes
C7 . C8 . 1.3944(15) yes
C7 . H71 . 0.931 no
C8 . C9 . 1.4020(16) yes
C8 . H81 . 0.926 no
C9 . O10 . 1.3652(14) yes
C9 . C11 . 1.4003(16) yes
O10 . H101 . 0.817(10) no
C11 . C12 . 1.3939(16) yes
C11 . H111 . 0.939 no
C12 . H121 . 0.943 no
C13 . C14 . 1.4006(16) yes
C13 . H131 . 0.906 no
C14 . C15 . 1.3982(16) yes
C14 . H141 . 0.900 no
C15 . C16 . 1.3992(15) yes
C15 . H151 . 0.929 no
C16 . C17 . 1.4798(14) yes
C17 . N18 . 1.2892(14) yes
C17 . H171 . 0.933 no
N18 . C19 . 1.4260(13) yes
C19 . C20 . 1.3997(15) yes
C19 . C25 . 1.4071(14) yes
C20 . C21 . 1.3974(15) yes
C20 . H201 . 0.939 no
C21 . C22 . 1.4029(16) yes
C21 . H211 . 0.936 no
C22 . O23 . 1.3800(15) yes
C22 . C24 . 1.3967(17) yes
O23 . H231 . 0.820(10) no
C24 . C25 . 1.3966(15) yes
C24 . H241 . 0.937 no
C25 . H251 . 0.936 no
N26 . C27 . 1.3415(15) yes
N26 . C40 . 1.3355(16) yes
C27 . C28 . 1.4759(19) yes
C27 . C37 . 1.4019(17) yes
C28 . N29 . 1.2881(16) yes
C28 . H281 . 0.947 no
N29 . C30 . 1.4184(17) yes
C30 . C31 . 1.4039(16) yes
C30 . C36 . 1.4042(15) yes
C31 . C32 . 1.3842(18) yes
C31 . H311 . 0.957 no
C32 . C33 . 1.4023(16) yes
C32 . H321 . 0.905 no
C33 . O34 . 1.219(3) yes
C33 . C35 . 1.3997(19) yes
O34 . H341 . 0.818(10) no
C35 . C36 . 1.387(2) yes
C35 . H351 . 0.914 no
C36 . H361 . 0.951 no
C37 . C38 . 1.392(2) yes
C37 . H371 . 0.907 no
C38 . C39 . 1.400(2) yes
C38 . H381 . 0.937 no
C39 . C40 . 1.4004(16) yes
C39 . H391 . 0.952 no
C40 . C41 . 1.4807(16) yes
C41 . N42 . 1.2899(14) yes
C41 . H411 . 0.952 no
N42 . C43 . 1.4256(14) yes
C43 . C44 . 1.4051(15) yes
C43 . C49 . 1.3995(15) yes
C44 . C45 . 1.3925(16) yes
C44 . H441 . 0.956 no
C45 . C46 . 1.3957(18) yes
C45 . H451 . 0.949 no
C46 . O47 . 1.302(2) yes
C46 . C48 . 1.4006(16) yes
O47 . H471 . 0.819(10) no
C48 . C49 . 1.3943(15) yes
C48 . H481 . 0.919 no
C49 . H491 . 0.939 no
S50 . O51 . 1.4410(10) yes
S50 . O52 . 1.4440(10) yes
S50 . O53 . 1.4534(11) yes
S50 . C54 . 1.8289(13) yes
C54 . F55 . 1.3334(14) yes
C54 . F56 . 1.3305(19) yes
C54 . F57 . 1.3368(19) yes
S58 . O59 . 1.4357(11) yes
S58 . O60 . 1.4472(11) yes
S58 . O61 . 1.4333(12) yes
S58 . C62 . 1.8384(17) yes
C62 . F63 . 1.3385(18) yes
C62 . F64 . 1.3337(19) yes
C62 . F65 . 1.3323(19) yes
N66 . C67 . 1.1469(18) yes
C67 . C68 . 1.4620(18) yes
C68 . H681 . 0.955 no
C68 . H682 . 0.952 no
C68 . H683 . 0.960 no
N69 . C70 . 1.139(2) yes
C70 . C71 . 1.451(2) yes
C71 . H711 . 0.948 no
C71 . H712 . 0.944 no
C71 . H713 . 0.963 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Zn1 . N5 . 75.26(3) yes
N2 . Zn1 . N18 . 75.66(3) yes
N5 . Zn1 . N18 . 150.85(3) yes
N2 . Zn1 . N26 . 176.11(4) yes
N5 . Zn1 . N26 . 103.09(3) yes
N18 . Zn1 . N26 . 105.81(4) yes
N2 . Zn1 . N29 . 101.65(4) yes
N5 . Zn1 . N29 . 98.20(3) yes
N18 . Zn1 . N29 . 85.70(3) yes
N26 . Zn1 . N29 . 75.00(4) yes
N2 . Zn1 . N42 . 107.54(3) yes
N5 . Zn1 . N42 . 84.97(3) yes
N18 . Zn1 . N42 . 105.76(3) yes
N26 . Zn1 . N42 . 75.66(4) yes
N29 . Zn1 . N42 . 150.44(4) yes
Zn1 . N2 . C3 . 119.75(7) yes
Zn1 . N2 . C16 . 119.32(7) yes
C3 . N2 . C16 . 120.66(9) yes
N2 . C3 . C4 . 114.49(9) yes
N2 . C3 . C13 . 121.39(10) yes
C4 . C3 . C13 . 124.06(9) yes
C3 . C4 . N5 . 117.82(9) yes
C3 . C4 . H41 . 119.3 no
N5 . C4 . H41 . 122.9 no
Zn1 . N5 . C4 . 111.99(7) yes
Zn1 . N5 . C6 . 126.71(7) yes
C4 . N5 . C6 . 120.41(9) yes
N5 . C6 . C7 . 122.74(9) yes
N5 . C6 . C12 . 117.59(9) yes
C7 . C6 . C12 . 119.67(9) yes
C6 . C7 . C8 . 119.93(10) yes
C6 . C7 . H71 . 119.4 no
C8 . C7 . H71 . 120.7 no
C7 . C8 . C9 . 120.02(10) yes
C7 . C8 . H81 . 121.5 no
C9 . C8 . H81 . 118.5 no
C8 . C9 . O10 . 122.20(10) yes
C8 . C9 . C11 . 120.35(10) yes
O10 . C9 . C11 . 117.44(10) yes
C9 . O10 . H101 . 109.5(3) no
C9 . C11 . C12 . 119.49(10) yes
C9 . C11 . H111 . 118.0 no
C12 . C11 . H111 . 122.5 no
C6 . C12 . C11 . 120.51(10) yes
C6 . C12 . H121 . 120.8 no
C11 . C12 . H121 . 118.7 no
C3 . C13 . C14 . 118.26(10) yes
C3 . C13 . H131 . 119.1 no
C14 . C13 . H131 . 122.7 no
C13 . C14 . C15 . 119.89(10) yes
C13 . C14 . H141 . 120.2 no
C15 . C14 . H141 . 119.9 no
C14 . C15 . C16 . 118.18(10) yes
C14 . C15 . H151 . 122.6 no
C16 . C15 . H151 . 119.2 no
C15 . C16 . N2 . 121.62(10) yes
C15 . C16 . C17 . 123.77(9) yes
N2 . C16 . C17 . 114.60(9) yes
C16 . C17 . N18 . 118.45(9) yes
C16 . C17 . H171 . 120.3 no
N18 . C17 . H171 . 121.2 no
Zn1 . N18 . C17 . 111.60(7) yes
Zn1 . N18 . C19 . 128.08(7) yes
C17 . N18 . C19 . 119.72(9) yes
N18 . C19 . C20 . 118.26(9) yes
N18 . C19 . C25 . 122.27(10) yes
C20 . C19 . C25 . 119.47(10) yes
C19 . C20 . C21 . 120.49(10) yes
C19 . C20 . H201 . 121.4 no
C21 . C20 . H201 . 118.1 no
C20 . C21 . C22 . 119.63(11) yes
C20 . C21 . H211 . 120.7 no
C22 . C21 . H211 . 119.6 no
C21 . C22 . O23 . 117.40(11) yes
C21 . C22 . C24 . 120.17(10) yes
O23 . C22 . C24 . 122.40(11) yes
C22 . O23 . H231 . 109.6(3) no
C22 . C24 . C25 . 120.08(10) yes
C22 . C24 . H241 . 117.8 no
C25 . C24 . H241 . 122.1 no
C19 . C25 . C24 . 120.06(10) yes
C19 . C25 . H251 . 119.9 no
C24 . C25 . H251 . 120.1 no
Zn1 . N26 . C27 . 119.48(9) yes
Zn1 . N26 . C40 . 118.79(8) yes
C27 . N26 . C40 . 121.15(11) yes
N26 . C27 . C28 . 114.29(10) yes
N26 . C27 . C37 . 120.94(13) yes
C28 . C27 . C37 . 124.53(12) yes
C27 . C28 . N29 . 117.10(10) yes
C27 . C28 . H281 . 119.1 no
N29 . C28 . H281 . 123.8 no
Zn1 . N29 . C28 . 112.65(9) yes
Zn1 . N29 . C30 . 125.40(7) yes
C28 . N29 . C30 . 121.15(10) yes
N29 . C30 . C31 . 116.86(10) yes
N29 . C30 . C36 . 123.00(11) yes
C31 . C30 . C36 . 120.14(12) yes
C30 . C31 . C32 . 119.97(10) yes
C30 . C31 . H311 . 118.0 no
C32 . C31 . H311 . 122.0 no
C31 . C32 . C33 . 120.04(12) yes
C31 . C32 . H321 . 118.3 no
C33 . C32 . H321 . 121.7 no
C32 . C33 . O34 . 124.16(16) yes
C32 . C33 . C35 . 119.86(12) yes
O34 . C33 . C35 . 115.97(15) yes
C33 . O34 . H341 . 109.5(3) no
C33 . C35 . C36 . 120.44(11) yes
C33 . C35 . H351 . 120.6 no
C36 . C35 . H351 . 118.9 no
C30 . C36 . C35 . 119.48(12) yes
C30 . C36 . H361 . 117.7 no
C35 . C36 . H361 . 122.8 no
C27 . C37 . C38 . 118.27(12) yes
C27 . C37 . H371 . 121.4 no
C38 . C37 . H371 . 120.3 no
C37 . C38 . C39 . 120.37(12) yes
C37 . C38 . H381 . 121.2 no
C39 . C38 . H381 . 118.4 no
C38 . C39 . C40 . 117.68(14) yes
C38 . C39 . H391 . 120.9 no
C40 . C39 . H391 . 121.4 no
C39 . C40 . N26 . 121.58(12) yes
C39 . C40 . C41 . 124.29(12) yes
N26 . C40 . C41 . 114.11(10) yes
C40 . C41 . N42 . 117.58(10) yes
C40 . C41 . H411 . 119.8 no
N42 . C41 . H411 . 122.6 no
Zn1 . N42 . C41 . 113.01(8) yes
Zn1 . N42 . C43 . 126.18(7) yes
C41 . N42 . C43 . 119.71(10) yes
N42 . C43 . C44 . 121.22(10) yes
N42 . C43 . C49 . 118.09(9) yes
C44 . C43 . C49 . 120.68(10) yes
C43 . C44 . C45 . 119.41(11) yes
C43 . C44 . H441 . 119.5 no
C45 . C44 . H441 . 121.0 no
C44 . C45 . C46 . 120.01(11) yes
C44 . C45 . H451 . 119.2 no
C46 . C45 . H451 . 120.8 no
C45 . C46 . O47 . 115.53(13) yes
C45 . C46 . C48 . 120.44(11) yes
O47 . C46 . C48 . 123.98(14) yes
C46 . O47 . H471 . 109.5(3) no
C46 . C48 . C49 . 119.92(11) yes
C46 . C48 . H481 . 118.9 no
C49 . C48 . H481 . 121.1 no
C43 . C49 . C48 . 119.42(10) yes
C43 . C49 . H491 . 119.3 no
C48 . C49 . H491 . 121.2 no
O51 . S50 . O52 . 116.57(7) yes
O51 . S50 . O53 . 114.26(7) yes
O52 . S50 . O53 . 113.68(8) yes
O51 . S50 . C54 . 104.12(6) yes
O52 . S50 . C54 . 103.12(7) yes
O53 . S50 . C54 . 102.78(7) yes
S50 . C54 . F55 . 111.78(9) yes
S50 . C54 . F56 . 111.06(10) yes
F55 . C54 . F56 . 107.62(12) yes
S50 . C54 . F57 . 110.68(11) yes
F55 . C54 . F57 . 107.27(12) yes
F56 . C54 . F57 . 108.26(15) yes
O59 . S58 . O60 . 113.73(10) yes
O59 . S58 . O61 . 114.71(8) yes
O60 . S58 . O61 . 116.14(9) yes
O59 . S58 . C62 . 102.11(7) yes
O60 . S58 . C62 . 103.52(7) yes
O61 . S58 . C62 . 104.28(9) yes
S58 . C62 . F63 . 110.64(10) yes
S58 . C62 . F64 . 111.43(10) yes
F63 . C62 . F64 . 107.76(15) yes
S58 . C62 . F65 . 111.90(14) yes
F63 . C62 . F65 . 107.80(13) yes
F64 . C62 . F65 . 107.13(13) yes
N66 . C67 . C68 . 179.05(15) yes
C67 . C68 . H681 . 108.7 no
C67 . C68 . H682 . 107.3 no
H681 . C68 . H682 . 112.3 no
C67 . C68 . H683 . 109.3 no
H681 . C68 . H683 . 111.1 no
H682 . C68 . H683 . 107.9 no
N69 . C70 . C71 . 178.66(16) yes
C70 . C71 . H711 . 107.0 no
C70 . C71 . H712 . 110.2 no
H711 . C71 . H712 . 111.5 no
C70 . C71 . H713 . 110.5 no
H711 . C71 . H713 . 108.7 no
H712 . C71 . H713 . 109.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O10 . H101 . O52 2_566 159.0(18) 0.817 1.999 2.7773(18) yes
C11 . H111 . O61 4_555 154.77(4) 0.939 2.505 3.3789(18) yes
C8 . H81 . O47 2_556 134.49(5) 0.926 2.523 3.2405(18) yes
O23 . H231 . O60 2_646 172.0(11) 0.820 1.991 2.8056(18) yes
C24 . H241 . O34 2_656 167.95(6) 0.937 2.394 3.3157(18) yes
C21 . H211 . O61 4_545 135.18(5) 0.936 2.525 3.2568(18) yes
C15 . H151 . O59 . 153.31(4) 0.929 2.475 3.3309(18) yes
C13 . H131 . O51 . 152.27(4) 0.906 2.492 3.3206(18) yes
O34 . H341 . O59 1_565 172(5) 0.818 2.075 2.8875(18) yes
O34 . H341 . O60 1_565 121.5(6) 0.818 2.363 2.8761(18) yes
C28 . H281 . O23 1_565 152.75(4) 0.947 2.503 3.3731(18) yes
O47 . H471 . O53 1_545 175(7) 0.819 1.856 2.6727(18) yes
C38 . H381 . O34 4_555 138.82(6) 0.937 2.513 3.2767(18) yes
C68 . H681 . O10 4_554 153.57(4) 0.955 2.554 3.4356(18) yes
C68 . H682 . O51 1_545 146.34(4) 0.952 2.462 3.2963(18) yes
C71 . H711 . O47 2_556 173.40(5) 0.948 2.539 3.4831(18) yes
C71 . H713 . O52 2_566 135.85(4) 0.963 2.549 3.3087(18) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/03/12 at 14:38:38
#
#LIST 12
BLOCK SCALE X'S, U'S, H(341,X'S), H(101,X'S), H(471,X'S)
CONT H(231,X'S)
EQUIV O(47,OCC) UNTIL H(471)
EQUIV O(34,OCC) UNTIL H(341)
EQUIV O(23,OCC) UNTIL H(231)
EQUIV O(10,OCC) UNTIL H(101)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 48,X'S) H ( 481,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 68,X'S) H ( 681,X'S) H ( 682,X'S) H ( 683,X'S)
RIDE C ( 71,X'S) H ( 711,X'S) H ( 712,X'S) H ( 713,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/03/12 at 14:38:38
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
A-U(IJ)'S 0.00,0.001 = C(46) TO O(47), C(33) TO O(34), C(9) TO O(10),
CONT C(22) TO O(23)
ANGLE 109.5, 0.3 = H(341) TO O(34) TO C(33)
ANGLE 109.5, 0.3 = H(101) TO O(10) TO C(9)
ANGLE 109.5, 0.3 = H(471) TO O(47) TO C(46)
ANGLE 109.5, 0.3 = H(231) TO O(23) TO C(22)
DIST 0.82, 0.01 = H(341) TO O(34)
DIST 0.82, 0.01 = H(101) TO O(10)
DIST 0.82, 0.01 = H(471) TO O(47)
DIST 0.82, 0.01 = H(231) TO O(23)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# Attachment '- vdlee46.cif'
data_1_vdlee46
_database_code_depnum_ccdc_archive 'CCDC 879236'
#TrackingRef '- vdlee46.cif'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details ?
#---------------------------------------------------------------
_cell_length_a 25.5485(11)
_cell_length_b 8.2860(3)
_cell_length_c 23.8465(11)
_cell_angle_alpha 90
_cell_angle_beta 113.144(5)
_cell_angle_gamma 90
_cell_volume 4641.9(4)
_cell_measurement_reflns_used 9410
_cell_measurement_theta_min 2.8736
_cell_measurement_theta_max 32.4240
_cell_oxdiff_length_a 23.8501(9)
_cell_oxdiff_length_b 8.2840(3)
_cell_oxdiff_length_c 25.5491(9)
_cell_oxdiff_angle_alpha 89.972(3)
_cell_oxdiff_angle_beta 113.140(3)
_cell_oxdiff_angle_gamma 89.998(3)
_cell_oxdiff_volume 4641.7(3)
_cell_oxdiff_measurement_reflns_used 9410
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c '
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_sum 'C44 H36 F6 N8 O10 S2 Zn'
_chemical_formula_moiety 'C38 H30 N6 O4 Zn, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_compound_source ?
_chemical_formula_weight 1080.34
_cell_measurement_temperature 175
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_min 0.05
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_max 0.20
_exptl_absorpt_correction_T_min 0.92163
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn 1.546
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 2208
_exptl_absorpt_coefficient_mu 0.710
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window'
_diffrn_detector_area_resol_mean 8.4205
_diffrn_measurement_device Serial
_diffrn_radiation_wavelength 0.71073
#montpellier_reflns_maxres is minimum d (highest resolution)
#where <= 2.0
#(Z. Dauter, Acta Cryst. D55, 1703-1717, 1999)
_montpellier_reflns_maxres 0.81
_montpellier_reflns_completeness_maxres 99.78
_montpellier_reflns_redundancy_maxres 7.07
#montpellier_diffrn_reflns_class_completeness_shell is completeness in shell
#montpellier_diffrn_class_reflns_cumul_completeness is cumulative
#completeness to resolution of shell
#Note: completeness percentage takes into account the fact whether
#group is centrosymmetric or not
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_I/uI
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.50 8.6 29.78 0.040 98.7 98.72
1 1.50 1.18 8.3 12.13 0.097 100.0 99.36
2 1.18 1.03 7.4 7.61 0.142 100.0 99.57
3 1.03 0.93 6.6 4.85 0.231 100.0 99.68
4 0.93 0.86 6.0 3.32 0.354 100.0 99.74
5 0.86 0.81 5.6 2.09 0.500 100.0 99.78
6 0.81 0.77 5.2 1.72 0.573 100.0 99.82
7 0.77 0.74 4.1 1.22 0.651 99.9 99.82
8 0.74 0.71 2.7 0.81 0.647 98.7 99.70
9 0.71 0.66 1.7 0.51 0.645 50.8 90.93
#End reflection statistics
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_orient_matrix_UB_11 0.0272925000
_diffrn_orient_matrix_UB_12 -0.0273244000
_diffrn_orient_matrix_UB_13 0.0030431000
_diffrn_orient_matrix_UB_21 -0.0064470000
_diffrn_orient_matrix_UB_22 0.0203637000
_diffrn_orient_matrix_UB_23 -0.0308928000
_diffrn_orient_matrix_UB_31 0.0111832000
_diffrn_orient_matrix_UB_32 0.0785490000
_diffrn_orient_matrix_UB_33 0.0090758000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 0.0000 115
#__ type_ start__ end____ width___ exp.time_
2 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 90.0000 115
#__ type_ start__ end____ width___ exp.time_
3 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 180.0000 115
#__ type_ start__ end____ width___ exp.time_
4 omega -54.00 61.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -79.0000 270.0000 115
#__ type_ start__ end____ width___ exp.time_
5 omega -111.00 10.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- -25.0000 -80.0000 100.0000 121
#__ type_ start__ end____ width___ exp.time_
6 omega -116.00 71.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- -25.0000 -10.0000 180.0000 187
#__ type_ start__ end____ width___ exp.time_
7 omega -110.00 12.00 1.0000 27.0000
omega____ theta____ kappa____ phi______ frames
- -25.0000 -80.0000 0.0000 122
;
_diffrn_measurement_method '\w scans'
_diffrn_ambient_temperature 175
_diffrn_reflns_number 87153
_reflns_number_total 15280
_diffrn_reflns_av_R_equivalents 0.140
_diffrn_reflns_av_sigmaI/netI 0.3193
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 15280
# Theoretical number of reflections is about 33595
_diffrn_reflns_theta_min 2.879
_diffrn_reflns_theta_max 32.497
_diffrn_measured_fraction_theta_max 0.909
_diffrn_reflns_theta_full 27.623
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -37
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_limit_l_max 34
_reflns_limit_h_min -38
_reflns_limit_h_max 35
_reflns_limit_k_min 0
_reflns_limit_k_max 12
_reflns_limit_l_min 0
_reflns_limit_l_max 35
_oxford_diffrn_Wilson_B_factor 1.17
_oxford_diffrn_Wilson_scale 5.15
_atom_sites_solution_primary other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.86
_refine_diff_density_max 1.46
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns 7541
_refine_ls_number_restraints 8
_refine_ls_number_parameters 652
_oxford_refine_ls_R_factor_ref 0.0720
_refine_ls_wR_factor_ref 0.0507
_refine_ls_goodness_of_fit_ref 1.0988
_refine_ls_shift/su_max 0.0011638
_refine_ls_shift/su_mean 0.0000312
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 15280
_refine_ls_R_factor_all 0.1786
_refine_ls_wR_factor_all 0.0975
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 7541
_refine_ls_R_factor_gt 0.0720
_refine_ls_wR_factor_gt 0.0507
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
3.04 -3.87 1.72 -0.742 -0.687
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
User-defined data collection reference
User defined data reduction
User defined cell refinement
Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J.
(2003). J. Appl. Cryst. 36, 1487--?.
Prince, E. Mathematical Techniques in Crystallography and Materials Science
Springer-Verlag, New York, 1982.
Watkin, D. J. (1994). Acta Cryst. A50, 411--437.
Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Zn1 Zn 0.278116(15) 0.04743(5) 0.573881(17) 0.0210 1.0000 Uani . . . . . .
N2 N 0.24690(10) 0.0461(4) 0.48071(12) 0.0206 1.0000 Uani . . . . . .
C3 C 0.20584(13) 0.1501(4) 0.44885(16) 0.0235 1.0000 Uani . . . . . .
C4 C 0.18536(13) 0.2526(4) 0.48619(15) 0.0225 1.0000 Uani . . . . . .
N5 N 0.21244(11) 0.2500(3) 0.54402(12) 0.0208 1.0000 Uani . . . . . .
C6 C 0.19476(13) 0.3462(4) 0.58318(15) 0.0218 1.0000 Uani . . . . . .
C7 C 0.13776(13) 0.3743(4) 0.57145(15) 0.0230 1.0000 Uani . . . . . .
C8 C 0.12307(13) 0.4726(4) 0.61012(15) 0.0229 1.0000 Uani . . . . . .
C9 C 0.16520(13) 0.5412(4) 0.66060(14) 0.0235 1.0000 Uani D . . . . .
O10 O 0.15327(11) 0.6391(4) 0.70013(12) 0.0350 1.0000 Uani D . . . . .
H101 H 0.1189(5) 0.652(5) 0.6881(12) 0.0528 1.0000 Uiso D . . . . .
C11 C 0.22218(14) 0.5120(4) 0.67320(16) 0.0268 1.0000 Uani . . . . . .
C12 C 0.23677(13) 0.4135(4) 0.63463(15) 0.0238 1.0000 Uani . . . . . .
H121 H 0.2749 0.3914 0.6426 0.0287 1.0000 Uiso R . . . . .
H111 H 0.2503 0.5572 0.7078 0.0319 1.0000 Uiso R . . . . .
H81 H 0.0851 0.4925 0.6025 0.0280 1.0000 Uiso R . . . . .
H71 H 0.1098 0.3268 0.5381 0.0281 1.0000 Uiso R . . . . .
H41 H 0.1534 0.3171 0.4671 0.0265 1.0000 Uiso R . . . . .
C13 C 0.18741(15) 0.1615(5) 0.38598(16) 0.0285 1.0000 Uani . . . . . .
C14 C 0.21231(15) 0.0643(5) 0.35647(16) 0.0307 1.0000 Uani . . . . . .
C15 C 0.25518(14) -0.0431(5) 0.39011(15) 0.0294 1.0000 Uani . . . . . .
C16 C 0.27142(13) -0.0485(5) 0.45243(15) 0.0238 1.0000 Uani . . . . . .
C17 C 0.31684(14) -0.1536(4) 0.49344(16) 0.0249 1.0000 Uani . . . . . .
N18 N 0.32861(11) -0.1491(3) 0.55066(13) 0.0218 1.0000 Uani . . . . . .
C19 C 0.37417(13) -0.2439(4) 0.59127(16) 0.0236 1.0000 Uani . . . . . .
C20 C 0.37085(14) -0.2991(4) 0.64506(17) 0.0281 1.0000 Uani . . . . . .
C21 C 0.41292(14) -0.3976(4) 0.68477(17) 0.0268 1.0000 Uani . . . . . .
C22 C 0.45879(13) -0.4420(4) 0.67089(15) 0.0256 1.0000 Uani D . . . . .
O23 O 0.49792(10) -0.5443(4) 0.71103(12) 0.0349 1.0000 Uani D . . . . .
H231 H 0.5205(13) -0.574(5) 0.6966(10) 0.0522 1.0000 Uiso D . . . . .
C24 C 0.46422(14) -0.3825(4) 0.61927(16) 0.0254 1.0000 Uani . . . . . .
C25 C 0.42225(14) -0.2841(5) 0.57991(16) 0.0267 1.0000 Uani . . . . . .
H251 H 0.4263 -0.2425 0.5456 0.0321 1.0000 Uiso R . . . . .
H241 H 0.4958 -0.4068 0.6113 0.0306 1.0000 Uiso R . . . . .
H211 H 0.4100 -0.4347 0.7203 0.0327 1.0000 Uiso R . . . . .
H201 H 0.3396 -0.2708 0.6537 0.0345 1.0000 Uiso R . . . . .
H171 H 0.3358 -0.2223 0.4770 0.0293 1.0000 Uiso R . . . . .
H151 H 0.2722 -0.1103 0.3708 0.0349 1.0000 Uiso R . . . . .
H141 H 0.2010 0.0712 0.3140 0.0373 1.0000 Uiso R . . . . .
H131 H 0.1593 0.2326 0.3641 0.0332 1.0000 Uiso R . . . . .
N26 N 0.31161(11) 0.0621(3) 0.66709(12) 0.0222 1.0000 Uani . . . . . .
C27 C 0.36125(14) 0.1378(4) 0.69583(16) 0.0262 1.0000 Uani . . . . . .
C28 C 0.38729(13) 0.1964(4) 0.65441(16) 0.0269 1.0000 Uani . . . . . .
N29 N 0.35645(11) 0.1975(3) 0.59756(13) 0.0237 1.0000 Uani . . . . . .
C30 C 0.37672(14) 0.2600(4) 0.55473(16) 0.0259 1.0000 Uani . . . . . .
C31 C 0.33900(13) 0.3526(4) 0.50760(17) 0.0256 1.0000 Uani . . . . . .
C32 C 0.35616(14) 0.4237(4) 0.46522(16) 0.0276 1.0000 Uani . . . . . .
C33 C 0.41189(14) 0.4025(4) 0.47032(16) 0.0253 1.0000 Uani D . . . . .
O34 O 0.43169(11) 0.4717(4) 0.43116(12) 0.0363 1.0000 Uani D . . . . .
H341 H 0.4095(11) 0.542(4) 0.4115(17) 0.0548 1.0000 Uiso D . . . . .
C35 C 0.44898(14) 0.3053(5) 0.51621(18) 0.0314 1.0000 Uani . . . . . .
C36 C 0.43172(14) 0.2340(5) 0.55835(18) 0.0305 1.0000 Uani . . . . . .
H361 H 0.4569 0.1701 0.5894 0.0368 1.0000 Uiso R . . . . .
H351 H 0.4852 0.2886 0.5179 0.0375 1.0000 Uiso R . . . . .
H321 H 0.3306 0.4845 0.4338 0.0334 1.0000 Uiso R . . . . .
H311 H 0.3027 0.3689 0.5057 0.0309 1.0000 Uiso R . . . . .
H281 H 0.4241 0.2341 0.6698 0.0321 1.0000 Uiso R . . . . .
C37 C 0.38157(16) 0.1687(5) 0.75801(17) 0.0342 1.0000 Uani . . . . . .
C38 C 0.34834(18) 0.1227(5) 0.78879(17) 0.0385 1.0000 Uani . . . . . .
C39 C 0.29674(16) 0.0458(5) 0.75906(15) 0.0327 1.0000 Uani . . . . . .
C40 C 0.27975(14) 0.0164(4) 0.69683(15) 0.0242 1.0000 Uani . . . . . .
C41 C 0.22555(14) -0.0609(4) 0.65796(15) 0.0254 1.0000 Uani . . . . . .
N42 N 0.21530(11) -0.0770(3) 0.60120(12) 0.0212 1.0000 Uani . . . . . .
C43 C 0.16226(13) -0.1399(4) 0.56126(15) 0.0230 1.0000 Uani . . . . . .
C44 C 0.11117(14) -0.0979(4) 0.56662(16) 0.0242 1.0000 Uani . . . . . .
C45 C 0.06019(14) -0.1655(5) 0.52666(17) 0.0284 1.0000 Uani . . . . . .
C46 C 0.06043(14) -0.2759(4) 0.48335(16) 0.0263 1.0000 Uani D . . . . .
O47 O 0.00954(10) -0.3442(4) 0.44792(13) 0.0380 1.0000 Uani D . . . . .
H471 H 0.0150(3) -0.434(3) 0.4371(19) 0.0567 1.0000 Uiso D . . . . .
C48 C 0.11061(14) -0.3113(4) 0.47631(15) 0.0253 1.0000 Uani . . . . . .
C49 C 0.16130(14) -0.2427(4) 0.51463(15) 0.0233 1.0000 Uani . . . . . .
H491 H 0.1949 -0.2665 0.5097 0.0281 1.0000 Uiso R . . . . .
H481 H 0.1100 -0.3814 0.4465 0.0295 1.0000 Uiso R . . . . .
H451 H 0.0261 -0.1371 0.5298 0.0337 1.0000 Uiso R . . . . .
H441 H 0.1119 -0.0262 0.5973 0.0289 1.0000 Uiso R . . . . .
H411 H 0.1999 -0.0974 0.6744 0.0302 1.0000 Uiso R . . . . .
H391 H 0.2741 0.0122 0.7796 0.0394 1.0000 Uiso R . . . . .
H381 H 0.3609 0.1443 0.8303 0.0454 1.0000 Uiso R . . . . .
H371 H 0.4171 0.2180 0.7777 0.0408 1.0000 Uiso R . . . . .
S50 S 0.01675(4) 0.30295(11) 0.35424(4) 0.0278 1.0000 Uani . . . . . .
O51 O 0.06001(12) 0.3572(4) 0.33492(15) 0.0449 1.0000 Uani . . . . . .
O52 O -0.04051(12) 0.3212(4) 0.31164(14) 0.0480 1.0000 Uani . . . . . .
O53 O 0.02558(16) 0.3499(4) 0.41550(14) 0.0548 1.0000 Uani . . . . . .
C54 C 0.02636(18) 0.0859(5) 0.3611(2) 0.0402 1.0000 Uani . . . . . .
F55 F -0.01294(11) 0.0152(3) 0.37586(12) 0.0483 1.0000 Uani . . . . . .
F56 F 0.02386(18) 0.0223(4) 0.30957(18) 0.0863 1.0000 Uani . . . . . .
F57 F 0.07642(13) 0.0476(4) 0.4036(2) 0.0910 1.0000 Uani . . . . . .
S58 S 0.38508(4) -0.19110(13) 0.33721(4) 0.0298 1.0000 Uani . . . . . .
O59 O 0.35798(12) -0.2808(3) 0.37055(14) 0.0392 1.0000 Uani . . . . . .
O60 O 0.43465(11) -0.2691(4) 0.33551(13) 0.0410 1.0000 Uani . . . . . .
O61 O 0.34686(12) -0.1217(5) 0.28154(13) 0.0549 1.0000 Uani . . . . . .
C62 C 0.41360(17) -0.0178(5) 0.3868(2) 0.0445 1.0000 Uani . . . . . .
F63 F 0.37205(12) 0.0750(3) 0.38872(15) 0.0615 1.0000 Uani . . . . . .
F64 F 0.44524(12) -0.0625(4) 0.44310(12) 0.0638 1.0000 Uani . . . . . .
F65 F 0.44581(12) 0.0723(4) 0.36714(18) 0.0795 1.0000 Uani . . . . . .
N66 N 0.21443(16) -0.4359(5) 0.41361(19) 0.0516 1.0000 Uani . . . . . .
C67 C 0.17817(18) -0.3848(5) 0.3730(2) 0.0365 1.0000 Uani . . . . . .
C68 C 0.1305(2) -0.3152(6) 0.3220(2) 0.0502 1.0000 Uani . . . . . .
H681 H 0.1422 -0.2988 0.2891 0.0754 1.0000 Uiso R . . . . .
H682 H 0.0991 -0.3885 0.3106 0.0751 1.0000 Uiso R . . . . .
H683 H 0.1200 -0.2144 0.3341 0.0755 1.0000 Uiso R . . . . .
N69 N 0.1589(2) 0.1113(7) 0.7363(2) 0.0717 1.0000 Uani . . . . . .
C70 C 0.1196(2) 0.1866(6) 0.7245(2) 0.0454 1.0000 Uani . . . . . .
C71 C 0.0694(2) 0.2861(6) 0.7102(2) 0.0512 1.0000 Uani . . . . . .
H711 H 0.0488 0.2916 0.6669 0.0772 1.0000 Uiso R . . . . .
H712 H 0.0448 0.2393 0.7282 0.0768 1.0000 Uiso R . . . . .
H713 H 0.0798 0.3930 0.7263 0.0767 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01663(15) 0.02411(19) 0.02118(17) -0.00126(18) 0.00638(13) -0.00078(17)
N2 0.0181(12) 0.0201(13) 0.0223(13) -0.0052(12) 0.0068(10) -0.0019(12)
C3 0.0187(14) 0.0241(17) 0.0278(17) 0.0016(14) 0.0095(13) 0.0021(13)
C4 0.0134(13) 0.0240(15) 0.0286(17) 0.0032(14) 0.0065(12) 0.0021(12)
N5 0.0176(12) 0.0196(13) 0.0254(14) -0.0014(11) 0.0086(11) 0.0001(10)
C6 0.0202(14) 0.0206(16) 0.0263(16) -0.0007(13) 0.0109(13) 0.0003(12)
C7 0.0193(14) 0.0240(17) 0.0229(16) -0.0021(14) 0.0053(13) -0.0058(13)
C8 0.0159(13) 0.0278(18) 0.0243(15) 0.0026(14) 0.0072(12) 0.0005(13)
C9 0.0255(15) 0.0231(16) 0.0243(15) 0.0011(15) 0.0124(13) 0.0023(15)
O10 0.0274(12) 0.0411(16) 0.0380(15) -0.0124(13) 0.0144(11) -0.0009(12)
C11 0.0219(15) 0.0263(18) 0.0270(17) -0.0028(14) 0.0041(13) 0.0007(13)
C12 0.0131(13) 0.0247(18) 0.0301(17) -0.0003(13) 0.0046(12) 0.0032(12)
C13 0.0251(16) 0.033(2) 0.0241(17) 0.0037(15) 0.0058(14) 0.0051(15)
C14 0.0305(17) 0.037(2) 0.0259(17) 0.0020(17) 0.0126(14) 0.0036(16)
C15 0.0285(16) 0.0343(19) 0.0270(16) -0.0051(17) 0.0126(13) 0.0030(17)
C16 0.0191(13) 0.0249(16) 0.0291(16) -0.0040(16) 0.0113(12) -0.0041(14)
C17 0.0230(15) 0.0222(17) 0.0311(18) -0.0067(14) 0.0125(14) 0.0008(13)
N18 0.0181(12) 0.0218(14) 0.0277(15) 0.0004(12) 0.0113(11) 0.0021(11)
C19 0.0202(15) 0.0217(16) 0.0283(17) -0.0036(14) 0.0090(13) 0.0001(13)
C20 0.0253(16) 0.0281(18) 0.038(2) -0.0004(16) 0.0206(15) 0.0012(15)
C21 0.0258(16) 0.0257(17) 0.0323(18) 0.0033(15) 0.0150(14) 0.0052(14)
C22 0.0204(14) 0.0234(17) 0.0319(17) -0.0039(16) 0.0091(13) 0.0025(14)
O23 0.0259(12) 0.0405(15) 0.0379(14) 0.0087(14) 0.0121(10) 0.0102(12)
C24 0.0188(14) 0.0270(17) 0.0334(18) -0.0038(15) 0.0135(13) -0.0011(13)
C25 0.0223(15) 0.0313(19) 0.0288(18) -0.0009(15) 0.0124(14) 0.0001(14)
N26 0.0176(12) 0.0192(14) 0.0263(14) -0.0002(12) 0.0050(10) 0.0003(11)
C27 0.0227(15) 0.0199(16) 0.0285(18) 0.0017(14) 0.0018(13) 0.0043(13)
C28 0.0142(13) 0.0237(17) 0.038(2) 0.0011(16) 0.0049(13) -0.0007(13)
N29 0.0176(12) 0.0201(14) 0.0318(15) -0.0023(12) 0.0079(11) -0.0015(11)
C30 0.0208(15) 0.0243(17) 0.0305(18) -0.0021(14) 0.0079(14) -0.0061(13)
C31 0.0168(14) 0.0195(16) 0.040(2) -0.0021(14) 0.0108(14) -0.0023(12)
C32 0.0251(16) 0.0265(19) 0.0313(18) -0.0034(15) 0.0113(14) -0.0023(14)
C33 0.0255(16) 0.0228(16) 0.0285(17) -0.0053(14) 0.0117(14) -0.0037(13)
O34 0.0293(13) 0.0471(17) 0.0381(14) 0.0041(13) 0.0193(12) -0.0033(13)
C35 0.0177(14) 0.038(2) 0.042(2) -0.0083(18) 0.0146(15) -0.0030(15)
C36 0.0191(15) 0.032(2) 0.038(2) -0.0003(16) 0.0088(14) 0.0031(14)
C37 0.0284(18) 0.031(2) 0.0301(19) 0.0025(16) -0.0032(15) -0.0004(16)
C38 0.049(2) 0.039(2) 0.0193(17) 0.0002(16) 0.0049(16) -0.0006(19)
C39 0.0427(19) 0.0320(19) 0.0209(16) 0.0026(17) 0.0099(14) 0.0021(18)
C40 0.0259(15) 0.0194(17) 0.0248(16) 0.0004(13) 0.0072(13) 0.0025(13)
C41 0.0246(15) 0.0232(17) 0.0296(17) -0.0007(15) 0.0120(13) -0.0024(14)
N42 0.0189(12) 0.0206(15) 0.0244(13) -0.0005(11) 0.0089(10) -0.0026(10)
C43 0.0215(15) 0.0202(16) 0.0270(17) 0.0019(13) 0.0091(13) -0.0032(13)
C44 0.0227(15) 0.0256(17) 0.0264(17) -0.0047(13) 0.0118(13) -0.0021(13)
C45 0.0179(14) 0.033(2) 0.0350(19) 0.0018(16) 0.0112(14) 0.0013(14)
C46 0.0234(15) 0.0279(19) 0.0239(17) 0.0004(14) 0.0052(13) -0.0048(14)
O47 0.0218(12) 0.0395(16) 0.0439(16) -0.0087(13) 0.0034(11) -0.0083(11)
C48 0.0280(16) 0.0237(17) 0.0218(16) -0.0046(14) 0.0073(13) -0.0042(14)
C49 0.0224(15) 0.0262(17) 0.0217(16) 0.0013(13) 0.0091(13) -0.0031(13)
S50 0.0235(4) 0.0261(4) 0.0341(5) -0.0026(4) 0.0116(3) 0.0000(4)
O51 0.0381(15) 0.0365(16) 0.071(2) 0.0062(15) 0.0324(15) -0.0008(13)
O52 0.0316(14) 0.0512(19) 0.0511(18) 0.0017(15) 0.0055(13) 0.0061(14)
O53 0.081(2) 0.0457(19) 0.0418(17) -0.0159(15) 0.0285(17) -0.0194(17)
C54 0.042(2) 0.031(2) 0.057(3) -0.0012(19) 0.029(2) -0.0014(17)
F55 0.0581(15) 0.0354(14) 0.0657(16) -0.0091(12) 0.0397(14) -0.0159(12)
F56 0.156(4) 0.0382(17) 0.119(3) -0.0205(18) 0.112(3) -0.0101(19)
F57 0.0480(17) 0.061(2) 0.152(3) 0.055(2) 0.026(2) 0.0136(16)
S58 0.0224(4) 0.0377(5) 0.0294(5) 0.0040(4) 0.0105(3) 0.0048(4)
O59 0.0407(15) 0.0299(15) 0.0570(18) 0.0018(13) 0.0302(14) 0.0007(12)
O60 0.0296(13) 0.0538(19) 0.0425(16) 0.0025(14) 0.0174(12) 0.0110(13)
O61 0.0361(16) 0.086(3) 0.0367(17) 0.0114(17) 0.0083(13) 0.0181(17)
C62 0.032(2) 0.032(2) 0.062(3) 0.006(2) 0.0093(19) 0.0014(17)
F63 0.0504(15) 0.0318(14) 0.096(2) -0.0072(14) 0.0227(15) 0.0105(12)
F64 0.0675(18) 0.0504(17) 0.0477(15) -0.0098(14) -0.0053(13) 0.0123(15)
F65 0.0498(17) 0.0484(19) 0.137(3) 0.0201(19) 0.0327(19) -0.0137(14)
N66 0.046(2) 0.047(2) 0.059(3) 0.002(2) 0.018(2) 0.0001(19)
C67 0.042(2) 0.029(2) 0.044(2) 0.0033(18) 0.023(2) 0.0007(18)
C68 0.052(3) 0.044(3) 0.053(3) 0.007(2) 0.018(2) -0.005(2)
N69 0.065(3) 0.077(3) 0.077(3) -0.005(3) 0.030(3) 0.014(3)
C70 0.060(3) 0.044(3) 0.034(2) -0.009(2) 0.021(2) -0.010(2)
C71 0.067(3) 0.041(3) 0.049(3) 0.003(2) 0.027(2) -0.002(2)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.4089(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . N2 . 2.044(3) yes
Zn1 . N5 . 2.281(3) yes
Zn1 . N18 . 2.277(3) yes
Zn1 . N26 . 2.048(3) yes
Zn1 . N29 . 2.232(3) yes
Zn1 . N42 . 2.210(3) yes
N2 . C3 . 1.339(4) yes
N2 . C16 . 1.339(4) yes
C3 . C4 . 1.468(5) yes
C3 . C13 . 1.387(5) yes
C4 . N5 . 1.277(4) yes
C4 . H41 . 0.932 no
N5 . C6 . 1.429(4) yes
C6 . C7 . 1.390(4) yes
C6 . C12 . 1.390(4) yes
C7 . C8 . 1.388(5) yes
C7 . H71 . 0.923 no
C8 . C9 . 1.383(5) yes
C8 . H81 . 0.930 no
C9 . O10 . 1.366(4) yes
C9 . C11 . 1.387(4) yes
O10 . H101 . 0.816(10) no
C11 . C12 . 1.385(5) yes
C11 . H111 . 0.933 no
C12 . H121 . 0.933 no
C13 . C14 . 1.379(5) yes
C13 . H131 . 0.917 no
C14 . C15 . 1.395(5) yes
C14 . H141 . 0.938 no
C15 . C16 . 1.378(4) yes
C15 . H151 . 0.932 no
C16 . C17 . 1.473(5) yes
C17 . N18 . 1.277(4) yes
C17 . H171 . 0.927 no
N18 . C19 . 1.422(4) yes
C19 . C20 . 1.396(5) yes
C19 . C25 . 1.398(4) yes
C20 . C21 . 1.385(5) yes
C20 . H201 . 0.930 no
C21 . C22 . 1.387(4) yes
C21 . H211 . 0.931 no
C22 . O23 . 1.371(4) yes
C22 . C24 . 1.383(5) yes
O23 . H231 . 0.816(10) no
C24 . C25 . 1.380(5) yes
C24 . H241 . 0.921 no
C25 . H251 . 0.929 no
N26 . C27 . 1.337(4) yes
N26 . C40 . 1.328(4) yes
C27 . C28 . 1.473(5) yes
C27 . C37 . 1.389(5) yes
C28 . N29 . 1.272(4) yes
C28 . H281 . 0.921 no
N29 . C30 . 1.413(4) yes
C30 . C31 . 1.389(5) yes
C30 . C36 . 1.390(5) yes
C31 . C32 . 1.381(5) yes
C31 . H311 . 0.921 no
C32 . C33 . 1.391(5) yes
C32 . H321 . 0.927 no
C33 . O34 . 1.352(4) yes
C33 . C35 . 1.389(5) yes
O34 . H341 . 0.819(10) no
C35 . C36 . 1.379(5) yes
C35 . H351 . 0.922 no
C36 . H361 . 0.932 no
C37 . C38 . 1.376(6) yes
C37 . H371 . 0.935 no
C38 . C39 . 1.382(6) yes
C38 . H381 . 0.930 no
C39 . C40 . 1.394(5) yes
C39 . H391 . 0.935 no
C40 . C41 . 1.476(5) yes
C41 . N42 . 1.280(4) yes
C41 . H411 . 0.936 no
N42 . C43 . 1.415(4) yes
C43 . C44 . 1.404(5) yes
C43 . C49 . 1.393(5) yes
C44 . C45 . 1.394(5) yes
C44 . H441 . 0.937 no
C45 . C46 . 1.381(5) yes
C45 . H451 . 0.933 no
C46 . O47 . 1.364(4) yes
C46 . C48 . 1.388(5) yes
O47 . H471 . 0.818(10) no
C48 . C49 . 1.380(5) yes
C48 . H481 . 0.913 no
C49 . H491 . 0.932 no
S50 . O51 . 1.427(3) yes
S50 . O52 . 1.423(3) yes
S50 . O53 . 1.441(3) yes
S50 . C54 . 1.814(4) yes
C54 . F55 . 1.323(5) yes
C54 . F56 . 1.315(5) yes
C54 . F57 . 1.321(5) yes
S58 . O59 . 1.448(3) yes
S58 . O60 . 1.437(3) yes
S58 . O61 . 1.424(3) yes
S58 . C62 . 1.821(5) yes
C62 . F63 . 1.326(5) yes
C62 . F64 . 1.319(5) yes
C62 . F65 . 1.326(5) yes
N66 . C67 . 1.128(5) yes
C67 . C68 . 1.459(6) yes
C68 . H681 . 0.953 no
C68 . H682 . 0.956 no
C68 . H683 . 0.955 no
N69 . C70 . 1.119(6) yes
C70 . C71 . 1.449(7) yes
C71 . H711 . 0.958 no
C71 . H712 . 0.967 no
C71 . H713 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Zn1 . N5 . 74.92(10) yes
N2 . Zn1 . N18 . 75.42(10) yes
N5 . Zn1 . N18 . 150.25(10) yes
N2 . Zn1 . N26 . 176.50(12) yes
N5 . Zn1 . N26 . 103.74(10) yes
N18 . Zn1 . N26 . 105.75(10) yes
N2 . Zn1 . N29 . 101.89(11) yes
N5 . Zn1 . N29 . 98.36(10) yes
N18 . Zn1 . N29 . 85.57(10) yes
N26 . Zn1 . N29 . 75.02(11) yes
N2 . Zn1 . N42 . 107.43(10) yes
N5 . Zn1 . N42 . 84.55(10) yes
N18 . Zn1 . N42 . 106.53(10) yes
N26 . Zn1 . N42 . 75.51(10) yes
N29 . Zn1 . N42 . 150.23(10) yes
Zn1 . N2 . C3 . 119.8(2) yes
Zn1 . N2 . C16 . 119.4(2) yes
C3 . N2 . C16 . 120.5(3) yes
N2 . C3 . C4 . 114.5(3) yes
N2 . C3 . C13 . 121.0(3) yes
C4 . C3 . C13 . 124.5(3) yes
C3 . C4 . N5 . 118.3(3) yes
C3 . C4 . H41 . 119.2 no
N5 . C4 . H41 . 122.5 no
Zn1 . N5 . C4 . 111.7(2) yes
Zn1 . N5 . C6 . 126.1(2) yes
C4 . N5 . C6 . 121.3(3) yes
N5 . C6 . C7 . 122.5(3) yes
N5 . C6 . C12 . 117.9(3) yes
C7 . C6 . C12 . 119.6(3) yes
C6 . C7 . C8 . 120.0(3) yes
C6 . C7 . H71 . 119.8 no
C8 . C7 . H71 . 120.2 no
C7 . C8 . C9 . 119.9(3) yes
C7 . C8 . H81 . 120.5 no
C9 . C8 . H81 . 119.6 no
C8 . C9 . O10 . 122.4(3) yes
C8 . C9 . C11 . 120.5(3) yes
O10 . C9 . C11 . 117.0(3) yes
C9 . O10 . H101 . 109.5(3) no
C9 . C11 . C12 . 119.5(3) yes
C9 . C11 . H111 . 120.0 no
C12 . C11 . H111 . 120.5 no
C6 . C12 . C11 . 120.4(3) yes
C6 . C12 . H121 . 118.9 no
C11 . C12 . H121 . 120.7 no
C3 . C13 . C14 . 118.9(3) yes
C3 . C13 . H131 . 121.1 no
C14 . C13 . H131 . 120.0 no
C13 . C14 . C15 . 119.7(3) yes
C13 . C14 . H141 . 120.4 no
C15 . C14 . H141 . 120.0 no
C14 . C15 . C16 . 118.5(3) yes
C14 . C15 . H151 . 120.8 no
C16 . C15 . H151 . 120.8 no
C15 . C16 . N2 . 121.5(3) yes
C15 . C16 . C17 . 124.1(3) yes
N2 . C16 . C17 . 114.5(3) yes
C16 . C17 . N18 . 119.0(3) yes
C16 . C17 . H171 . 119.2 no
N18 . C17 . H171 . 121.8 no
Zn1 . N18 . C17 . 111.3(2) yes
Zn1 . N18 . C19 . 128.3(2) yes
C17 . N18 . C19 . 119.8(3) yes
N18 . C19 . C20 . 118.5(3) yes
N18 . C19 . C25 . 123.1(3) yes
C20 . C19 . C25 . 118.4(3) yes
C19 . C20 . C21 . 120.7(3) yes
C19 . C20 . H201 . 119.3 no
C21 . C20 . H201 . 120.0 no
C20 . C21 . C22 . 119.7(3) yes
C20 . C21 . H211 . 119.9 no
C22 . C21 . H211 . 120.4 no
C21 . C22 . O23 . 116.8(3) yes
C21 . C22 . C24 . 120.5(3) yes
O23 . C22 . C24 . 122.7(3) yes
C22 . O23 . H231 . 109.5(3) no
C22 . C24 . C25 . 119.6(3) yes
C22 . C24 . H241 . 120.5 no
C25 . C24 . H241 . 119.9 no
C19 . C25 . C24 . 121.1(3) yes
C19 . C25 . H251 . 119.4 no
C24 . C25 . H251 . 119.5 no
Zn1 . N26 . C27 . 119.5(2) yes
Zn1 . N26 . C40 . 118.7(2) yes
C27 . N26 . C40 . 121.2(3) yes
N26 . C27 . C28 . 113.5(3) yes
N26 . C27 . C37 . 121.0(3) yes
C28 . C27 . C37 . 125.3(3) yes
C27 . C28 . N29 . 117.6(3) yes
C27 . C28 . H281 . 120.3 no
N29 . C28 . H281 . 122.1 no
Zn1 . N29 . C28 . 112.6(2) yes
Zn1 . N29 . C30 . 124.6(2) yes
C28 . N29 . C30 . 121.6(3) yes
N29 . C30 . C31 . 116.9(3) yes
N29 . C30 . C36 . 123.2(3) yes
C31 . C30 . C36 . 119.9(3) yes
C30 . C31 . C32 . 120.6(3) yes
C30 . C31 . H311 . 119.1 no
C32 . C31 . H311 . 120.3 no
C31 . C32 . C33 . 119.4(3) yes
C31 . C32 . H321 . 119.9 no
C33 . C32 . H321 . 120.8 no
C32 . C33 . O34 . 122.3(3) yes
C32 . C33 . C35 . 120.0(3) yes
O34 . C33 . C35 . 117.7(3) yes
C33 . O34 . H341 . 109.5(3) no
C33 . C35 . C36 . 120.5(3) yes
C33 . C35 . H351 . 118.9 no
C36 . C35 . H351 . 120.5 no
C30 . C36 . C35 . 119.5(3) yes
C30 . C36 . H361 . 120.2 no
C35 . C36 . H361 . 120.3 no
C27 . C37 . C38 . 117.9(3) yes
C27 . C37 . H371 . 119.9 no
C38 . C37 . H371 . 122.2 no
C37 . C38 . C39 . 121.2(4) yes
C37 . C38 . H381 . 119.1 no
C39 . C38 . H381 . 119.7 no
C38 . C39 . C40 . 117.5(3) yes
C38 . C39 . H391 . 121.9 no
C40 . C39 . H391 . 120.5 no
C39 . C40 . N26 . 121.2(3) yes
C39 . C40 . C41 . 124.6(3) yes
N26 . C40 . C41 . 114.2(3) yes
C40 . C41 . N42 . 117.4(3) yes
C40 . C41 . H411 . 121.1 no
N42 . C41 . H411 . 121.5 no
Zn1 . N42 . C41 . 113.1(2) yes
Zn1 . N42 . C43 . 126.0(2) yes
C41 . N42 . C43 . 119.6(3) yes
N42 . C43 . C44 . 121.7(3) yes
N42 . C43 . C49 . 118.3(3) yes
C44 . C43 . C49 . 119.9(3) yes
C43 . C44 . C45 . 119.4(3) yes
C43 . C44 . H441 . 119.6 no
C45 . C44 . H441 . 121.1 no
C44 . C45 . C46 . 120.0(3) yes
C44 . C45 . H451 . 119.6 no
C46 . C45 . H451 . 120.4 no
C45 . C46 . O47 . 117.0(3) yes
C45 . C46 . C48 . 120.4(3) yes
O47 . C46 . C48 . 122.6(3) yes
C46 . O47 . H471 . 109.5(3) no
C46 . C48 . C49 . 120.3(3) yes
C46 . C48 . H481 . 119.6 no
C49 . C48 . H481 . 120.2 no
C43 . C49 . C48 . 119.8(3) yes
C43 . C49 . H491 . 120.1 no
C48 . C49 . H491 . 120.1 no
O51 . S50 . O52 . 116.4(2) yes
O51 . S50 . O53 . 114.2(2) yes
O52 . S50 . O53 . 113.7(2) yes
O51 . S50 . C54 . 104.30(18) yes
O52 . S50 . C54 . 103.6(2) yes
O53 . S50 . C54 . 102.4(2) yes
S50 . C54 . F55 . 111.9(3) yes
S50 . C54 . F56 . 110.9(3) yes
F55 . C54 . F56 . 107.9(3) yes
S50 . C54 . F57 . 111.3(3) yes
F55 . C54 . F57 . 107.3(4) yes
F56 . C54 . F57 . 107.3(4) yes
O59 . S58 . O60 . 113.67(18) yes
O59 . S58 . O61 . 114.76(19) yes
O60 . S58 . O61 . 116.39(18) yes
O59 . S58 . C62 . 101.7(2) yes
O60 . S58 . C62 . 103.96(19) yes
O61 . S58 . C62 . 103.9(2) yes
S58 . C62 . F63 . 111.0(3) yes
S58 . C62 . F64 . 111.6(3) yes
F63 . C62 . F64 . 107.9(4) yes
S58 . C62 . F65 . 111.1(4) yes
F63 . C62 . F65 . 107.6(3) yes
F64 . C62 . F65 . 107.5(4) yes
N66 . C67 . C68 . 177.7(5) yes
C67 . C68 . H681 . 108.2 no
C67 . C68 . H682 . 108.6 no
H681 . C68 . H682 . 110.8 no
C67 . C68 . H683 . 109.6 no
H681 . C68 . H683 . 109.8 no
H682 . C68 . H683 . 109.8 no
N69 . C70 . C71 . 178.8(5) yes
C70 . C71 . H711 . 109.9 no
C70 . C71 . H712 . 109.7 no
H711 . C71 . H712 . 108.6 no
C70 . C71 . H713 . 110.4 no
H711 . C71 . H713 . 109.5 no
H712 . C71 . H713 . 108.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O10 . H101 . O52 2_566 161(3) 0.816 2.018 2.802(5) yes
C11 . H111 . O61 3_555 157.87(12) 0.933 2.461 3.343(5) yes
C8 . H81 . O47 2_556 136.89(10) 0.930 2.552 3.293(5) yes
O23 . H231 . O60 2_646 158(4) 0.816 2.070 2.845(5) yes
C24 . H241 . O34 2_656 168.99(10) 0.921 2.494 3.403(5) yes
C13 . H131 . O51 . 151.85(10) 0.917 2.569 3.404(5) yes
O34 . H341 . O59 1_565 175(5) 0.819 1.958 2.775(5) yes
C28 . H281 . O23 1_565 152.63(10) 0.921 2.537 3.381(5) yes
O47 . H471 . O53 1_545 176(5) 0.818 1.910 2.728(5) yes
C38 . H381 . O34 3_555 138.44(11) 0.930 2.561 3.315(5) yes
C68 . H682 . O51 1_545 146.84(13) 0.956 2.496 3.338(5) yes
C71 . H711 . O47 2_556 172.74(13) 0.958 2.589 3.542(5) yes
C71 . H712 . O51 3_555 134.15(13) 0.967 2.548 3.296(5) yes
C71 . H713 . O52 2_566 134.04(13) 0.960 2.592 3.332(5) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 06/03/12 at 15:29:08
#
#LIST 12
BLOCK SCALE X'S, U'S, H(341,X'S), H(101,X'S), H(471,X'S)
CONT H(231,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 48,X'S) H ( 481,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 68,X'S) H ( 681,X'S) H ( 682,X'S) H ( 683,X'S)
RIDE C ( 71,X'S) H ( 711,X'S) H ( 712,X'S) H ( 713,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 06/03/12 at 15:29:08
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
ANGLE 109.5, 0.3 = H(341) TO O(34) TO C(33)
ANGLE 109.5, 0.3 = H(101) TO O(10) TO C(9)
ANGLE 109.5, 0.3 = H(471) TO O(47) TO C(46)
ANGLE 109.5, 0.3 = H(231) TO O(23) TO C(22)
DIST 0.82, 0.01 = H(341) TO O(34)
DIST 0.82, 0.01 = H(101) TO O(10)
DIST 0.82, 0.01 = H(471) TO O(47)
DIST 0.82, 0.01 = H(231) TO O(23)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;