# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full Org.Biomol.Chem.
_journal_coden_cambridge 0177
#TrackingRef 'PT-MKUC1_CIF.txt'
#======================================================================
_audit_creation_method SHELXL-97
_audit_creation_date 14-04-2011
#===========================================================
# 1. SUBMISSION DETAILS
#===========================================================
_publ_contact_author_name 'K. Namitharan'
_publ_contact_author_address
;
School of Chemistry
Madurai Kamaraj University
Madurai - 625 021
India
;
_publ_contact_author_email namitharan25@gmail.com
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_requested_coeditor_name ?
_publ_requested_category FO
_publ_contact_letter
;
Date 14-04-2011
Please consider this CIF submission for publication in
Organic Letters or some other journals. All authors have
seen and approved
this submission.
The CIF has passed the Chester CHECKCIF routines and gives a
satisfactory PRINTCIF file.
K. Pitchumani
;
#=====================================================================
# 3. TITLE AND AUTHER LIST
#=====================================================================
_publ_section_title
;
?
;
# The loop structure below should contain the names and addresses of
# all authors, in the required order of publication.
loop_
_publ_author_name
_publ_author_address
'K. Pitchumani'
; School of Chemistry
Madurai Kamaraj University
Madurai - 625 021
India
;
'K. Namitharan'
; School of Chemistry
Madurai Kamaraj University
Madurai - 625 021
India
;
#==========================================================
# 4. TEXT
#==========================================================
_publ_section_related_literature
;
?
;
_publ_section_abstract
;
?
;
_publ_section_comment
;
?
;
_publ_section_acknowledgements
;
KN and KP thank Dr. Babu Varghese, SAIF, IIT, Chennai, India
for the data collection.
;
_publ_section_references
;
Bruker (2004). APEX2 (Version 2.0-2) and SAINT. Bruker AXS Inc.,
Madison Wisconsin, USA.
Sheldrick, G. M. SADABS. version 2.03. University of G\"ottingen,
Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_figure_captions
;
?
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
All H atoms were fixed
geometrically and allowed to ride on their parent C atoms, with C---H
distances fixed in the range 0.93--0.97 \%A with U~iso~(H) = 1.5U~eq~(C)
for methyl H 1.2U~eq~(C) for other H atoms.
;
#============================================================================
# 5.Chemical Data
#============================================================================
data_mkuc1
_database_code_depnum_ccdc_archive 'CCDC 822410'
#TrackingRef 'PT-MKUC1_CIF.txt'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C36 H41 N3 O4 S2'
_chemical_formula_weight 643.84
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P21/c
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.8355(4)
_cell_length_b 12.6814(5)
_cell_length_c 24.4115(8)
_cell_angle_alpha 90.00
_cell_angle_beta 94.018(2)
_cell_angle_gamma 90.00
_cell_volume 3346.1(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 6946
_cell_measurement_theta_min 1.7
_cell_measurement_theta_max 26.5
_exptl_crystal_description Block
_exptl_crystal_colour 'white crystalline'
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.19
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.278
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1368
_exptl_absorpt_coefficient_mu 0.202
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.934
_exptl_absorpt_correction_T_max 0.950
_exptl_absorpt_process_details 'SADABS; Sheldrick (1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Bruker APEXII CCD area detector diffractometer'
_diffrn_measurement_method '\w and \f scans '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 32038
_diffrn_reflns_av_R_equivalents 0.0416
_diffrn_reflns_av_sigmaI/netI 0.0394
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 1.67
_diffrn_reflns_theta_max 26.53
_reflns_number_total 6946
_reflns_number_gt 4485
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEXII (BRUKER, 2004)'
_computing_cell_refinement APEXII
_computing_data_reduction 'SAINT (BRUKER, 2004)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+0.3357P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6946
_refine_ls_number_parameters 478
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0834
_refine_ls_R_factor_gt 0.0456
_refine_ls_wR_factor_ref 0.1574
_refine_ls_wR_factor_gt 0.1247
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_restrained_S_all 1.023
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0256(3) 0.9071(3) 0.14208(11) 0.0753(9) Uani 1 1 d . . .
H1A H 0.0284 0.9777 0.1280 0.113 Uiso 1 1 calc R . .
H1B H -0.0590 0.8863 0.1445 0.113 Uiso 1 1 calc R . .
H1C H 0.0649 0.8600 0.1179 0.113 Uiso 1 1 calc R . .
C2 C 0.0922(2) 0.90295(19) 0.19825(10) 0.0490(6) Uani 1 1 d . . .
C3 C 0.0266(2) 0.90251(19) 0.24471(10) 0.0514(6) Uani 1 1 d . . .
H3 H -0.0594 0.9010 0.2410 0.062 Uiso 1 1 calc R . .
C4 C 0.0862(2) 0.90428(18) 0.29638(10) 0.0471(6) Uani 1 1 d . . .
H4 H 0.0411 0.9038 0.3274 0.057 Uiso 1 1 calc R . .
C5 C 0.2143(2) 0.90680(17) 0.30147(9) 0.0397(5) Uani 1 1 d . . .
C6 C 0.2810(2) 0.90455(19) 0.25566(9) 0.0490(6) Uani 1 1 d . . .
H6 H 0.3671 0.9043 0.2592 0.059 Uiso 1 1 calc R . .
C7 C 0.2191(2) 0.9026(2) 0.20456(10) 0.0539(6) Uani 1 1 d . . .
H7 H 0.2643 0.9010 0.1735 0.065 Uiso 1 1 calc R . .
C8 C 0.2496(2) 1.10662(18) 0.39147(8) 0.0403(5) Uani 1 1 d . . .
C9 C 0.2111(2) 1.19835(18) 0.41716(8) 0.0408(5) Uani 1 1 d . . .
C11 C 0.3367(2) 1.16734(18) 0.35532(9) 0.0406(5) Uani 1 1 d . . .
C10 C 0.2892(2) 1.26187(18) 0.38717(9) 0.0410(5) Uani 1 1 d . . .
C12 C 0.3089(2) 1.16591(17) 0.29407(9) 0.0402(5) Uani 1 1 d . . .
C17 C 0.4014(2) 1.15111(19) 0.25881(10) 0.0493(6) Uani 1 1 d . . .
H12 H 0.4821 1.1400 0.2731 0.059 Uiso 1 1 calc R . .
C16 C 0.3760(3) 1.1525(2) 0.20265(10) 0.0593(7) Uani 1 1 d . . .
H13 H 0.4393 1.1431 0.1793 0.071 Uiso 1 1 calc R . .
C15 C 0.2561(3) 1.1679(2) 0.18137(10) 0.0618(7) Uani 1 1 d . . .
H14 H 0.2383 1.1686 0.1435 0.074 Uiso 1 1 calc R . .
C14 C 0.1635(3) 1.1823(2) 0.21584(10) 0.0588(7) Uani 1 1 d . . .
H15 H 0.0826 1.1929 0.2015 0.071 Uiso 1 1 calc R . .
C13 C 0.1898(2) 1.18098(19) 0.27177(9) 0.0477(6) Uani 1 1 d . . .
H16 H 0.1261 1.1904 0.2949 0.057 Uiso 1 1 calc R . .
C18 C 0.13557(19) 1.21959(18) 0.46307(8) 0.0412(5) Uani 1 1 d . . .
C19 C 0.0783(3) 1.1396(2) 0.49018(10) 0.0589(7) Uani 1 1 d . . .
H18 H 0.0832 1.0706 0.4776 0.071 Uiso 1 1 calc R . .
C20 C 0.0142(3) 1.1609(2) 0.53548(12) 0.0709(8) Uani 1 1 d . . .
H19 H -0.0240 1.1060 0.5531 0.085 Uiso 1 1 calc R . .
C21 C 0.0056(3) 1.2611(2) 0.55493(11) 0.0668(8) Uani 1 1 d . . .
H20 H -0.0369 1.2746 0.5860 0.080 Uiso 1 1 calc R . .
C22 C 0.0603(3) 1.3417(2) 0.52813(11) 0.0625(7) Uani 1 1 d . . .
H21 H 0.0540 1.4104 0.5409 0.075 Uiso 1 1 calc R . .
C23 C 0.1244(2) 1.32208(19) 0.48266(9) 0.0503(6) Uani 1 1 d . . .
H22 H 0.1606 1.3777 0.4648 0.060 Uiso 1 1 calc R . .
C24 C 0.3402(2) 1.47519(19) 0.29878(9) 0.0481(6) Uani 1 1 d . . .
C25 C 0.2759(3) 1.5686(2) 0.30466(12) 0.0637(7) Uani 1 1 d . . .
H25 H 0.2749 1.6004 0.3390 0.076 Uiso 1 1 calc R . .
C26 C 0.2141(3) 1.6140(2) 0.25975(13) 0.0692(8) Uani 1 1 d . . .
H26 H 0.1711 1.6766 0.2640 0.083 Uiso 1 1 calc R . .
C27 C 0.2142(3) 1.5687(2) 0.20824(11) 0.0611(7) Uani 1 1 d . . .
C28 C 0.2800(3) 1.4763(2) 0.20299(10) 0.0583(7) Uani 1 1 d . . .
H28 H 0.2822 1.4452 0.1686 0.070 Uiso 1 1 calc R . .
C29 C 0.3427(2) 1.42926(19) 0.24785(10) 0.0523(6) Uani 1 1 d . . .
H29 H 0.3863 1.3669 0.2436 0.063 Uiso 1 1 calc R . .
C30 C 0.1442(4) 1.6181(3) 0.15930(14) 0.0942(11) Uani 1 1 d . . .
H30A H 0.1883 1.6790 0.1478 0.141 Uiso 1 1 calc R . .
H30B H 0.0635 1.6389 0.1691 0.141 Uiso 1 1 calc R . .
H30C H 0.1362 1.5680 0.1298 0.141 Uiso 1 1 calc R . .
C31 C 0.3368(10) 0.8030(7) 0.5386(3) 0.075(3) Uani 0.465(8) 1 d P A 1
H31A H 0.3780 0.7798 0.5730 0.090 Uiso 0.465(8) 1 calc PR A 1
H31B H 0.2511 0.7807 0.5381 0.090 Uiso 0.465(8) 1 calc PR A 1
C32 C 0.342(2) 0.929(2) 0.5358(6) 0.080(4) Uani 0.465(8) 1 d P A 1
H32A H 0.4256 0.9527 0.5426 0.120 Uiso 0.465(8) 1 calc PR A 1
H32B H 0.2918 0.9586 0.5630 0.120 Uiso 0.465(8) 1 calc PR A 1
H32C H 0.3105 0.9526 0.5000 0.120 Uiso 0.465(8) 1 calc PR A 1
C33 C 0.5321(7) 0.7913(9) 0.4867(4) 0.097(3) Uani 0.465(8) 1 d P A 1
H33A H 0.5325 0.8676 0.4894 0.116 Uiso 0.465(8) 1 calc PR A 1
H33B H 0.5846 0.7641 0.5173 0.116 Uiso 0.465(8) 1 calc PR A 1
C34 C 0.583(2) 0.762(3) 0.4373(11) 0.096(7) Uani 0.465(8) 1 d P A 1
H34A H 0.5839 0.6865 0.4343 0.144 Uiso 0.465(8) 1 calc PR A 1
H34B H 0.6663 0.7882 0.4373 0.144 Uiso 0.465(8) 1 calc PR A 1
H34C H 0.5342 0.7914 0.4068 0.144 Uiso 0.465(8) 1 calc PR A 1
C35 C 0.4017(10) 0.6350(6) 0.4962(4) 0.093(3) Uani 0.465(8) 1 d P A 1
H35A H 0.4758 0.6165 0.5187 0.112 Uiso 0.465(8) 1 calc PR A 1
H35B H 0.4113 0.6074 0.4597 0.112 Uiso 0.465(8) 1 calc PR A 1
C36 C 0.2937(16) 0.5784(11) 0.5193(8) 0.163(7) Uani 0.465(8) 1 d P A 1
H36A H 0.2838 0.6028 0.5559 0.244 Uiso 0.465(8) 1 calc PR A 1
H36B H 0.3093 0.5039 0.5199 0.244 Uiso 0.465(8) 1 calc PR A 1
H36C H 0.2196 0.5926 0.4966 0.244 Uiso 0.465(8) 1 calc PR A 1
C31' C 0.4214(14) 0.8359(12) 0.5309(5) 0.154(6) Uani 0.536(8) 1 d P A 2
H31C H 0.4405 0.8040 0.5666 0.184 Uiso 0.536(8) 1 calc PR A 2
H31D H 0.4962 0.8706 0.5207 0.184 Uiso 0.536(8) 1 calc PR A 2
C32' C 0.341(3) 0.909(2) 0.5373(9) 0.150(11) Uani 0.536(8) 1 d P A 2
H32D H 0.3473 0.9619 0.5097 0.225 Uiso 0.536(8) 1 calc PR A 2
H32E H 0.3551 0.9396 0.5730 0.225 Uiso 0.536(8) 1 calc PR A 2
H32F H 0.2591 0.8785 0.5339 0.225 Uiso 0.536(8) 1 calc PR A 2
C33' C 0.5066(8) 0.6952(8) 0.4810(4) 0.102(3) Uani 0.536(8) 1 d P A 2
H33C H 0.5542 0.6835 0.5156 0.122 Uiso 0.536(8) 1 calc PR A 2
H33D H 0.4827 0.6265 0.4663 0.122 Uiso 0.536(8) 1 calc PR A 2
C34' C 0.586(2) 0.743(3) 0.4440(11) 0.111(8) Uani 0.536(8) 1 d P A 2
H34D H 0.5434 0.7501 0.4084 0.167 Uiso 0.536(8) 1 calc PR A 2
H34E H 0.6585 0.7002 0.4412 0.167 Uiso 0.536(8) 1 calc PR A 2
H34F H 0.6108 0.8118 0.4575 0.167 Uiso 0.536(8) 1 calc PR A 2
C35' C 0.3016(11) 0.6713(11) 0.5203(6) 0.171(6) Uani 0.536(8) 1 d P A 2
H35C H 0.3403 0.6409 0.5537 0.205 Uiso 0.536(8) 1 calc PR A 2
H35D H 0.2273 0.7084 0.5292 0.205 Uiso 0.536(8) 1 calc PR A 2
C36' C 0.2751(14) 0.5980(13) 0.4838(5) 0.128(5) Uani 0.536(8) 1 d P A 2
H36D H 0.1928 0.6088 0.4675 0.192 Uiso 0.536(8) 1 calc PR A 2
H36E H 0.2800 0.5301 0.5013 0.192 Uiso 0.536(8) 1 calc PR A 2
H36F H 0.3329 0.6010 0.4558 0.192 Uiso 0.536(8) 1 calc PR A 2
N1 N 0.22058(18) 1.00715(14) 0.39893(7) 0.0454(5) Uani 1 1 d . . .
N2 N 0.31055(19) 1.36373(16) 0.38982(7) 0.0501(5) Uani 1 1 d . . .
N3 N 0.3963(3) 0.7507(2) 0.49226(10) 0.0671(6) Uani 1 1 d D . .
O1 O 0.26702(17) 0.81996(13) 0.39586(7) 0.0588(5) Uani 1 1 d . . .
O2 O 0.41857(14) 0.94093(14) 0.36059(7) 0.0582(5) Uani 1 1 d . . .
O3 O 0.50390(15) 1.34026(14) 0.33765(7) 0.0613(5) Uani 1 1 d . . .
O4 O 0.46839(19) 1.49946(16) 0.39057(7) 0.0767(6) Uani 1 1 d . . .
S1 S 0.29137(5) 0.91687(5) 0.36698(2) 0.04606(18) Uani 1 1 d . . .
S2 S 0.41843(6) 1.41609(5) 0.35622(2) 0.0538(2) Uani 1 1 d . . .
H10A H 0.425(2) 1.1512(16) 0.3626(8) 0.036(6) Uiso 1 1 d . . .
H3A H 0.352(3) 0.768(2) 0.4634(8) 0.084(10) Uiso 1 1 d D . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.077(2) 0.090(2) 0.0562(17) 0.0007(16) -0.0121(14) -0.0017(17)
C2 0.0512(14) 0.0474(14) 0.0479(14) -0.0008(11) -0.0002(11) -0.0018(11)
C3 0.0368(12) 0.0539(15) 0.0630(16) -0.0038(12) 0.0011(11) -0.0023(11)
C4 0.0452(13) 0.0513(14) 0.0462(14) -0.0015(11) 0.0123(10) -0.0022(11)
C5 0.0417(12) 0.0374(12) 0.0402(12) 0.0020(9) 0.0041(9) -0.0003(9)
C6 0.0391(12) 0.0608(16) 0.0478(14) -0.0011(11) 0.0077(10) 0.0007(11)
C7 0.0541(15) 0.0672(17) 0.0419(13) -0.0031(12) 0.0133(11) -0.0005(12)
C8 0.0415(12) 0.0472(13) 0.0317(11) 0.0062(10) -0.0001(9) -0.0056(10)
C9 0.0438(12) 0.0449(13) 0.0339(11) 0.0017(10) 0.0039(9) -0.0084(10)
C11 0.0394(12) 0.0450(13) 0.0379(12) 0.0072(10) 0.0055(9) -0.0035(10)
C10 0.0420(12) 0.0479(14) 0.0329(11) 0.0031(10) 0.0011(9) -0.0088(10)
C12 0.0442(12) 0.0387(12) 0.0387(12) 0.0038(9) 0.0090(9) -0.0006(10)
C17 0.0519(14) 0.0491(14) 0.0484(14) 0.0051(11) 0.0143(11) 0.0081(11)
C16 0.0717(18) 0.0613(17) 0.0480(15) 0.0046(12) 0.0260(13) 0.0125(14)
C15 0.089(2) 0.0595(17) 0.0376(14) 0.0011(12) 0.0085(13) 0.0072(15)
C14 0.0616(16) 0.0692(18) 0.0447(15) 0.0006(12) -0.0023(12) 0.0050(13)
C13 0.0459(13) 0.0559(15) 0.0423(13) 0.0012(11) 0.0096(10) 0.0019(11)
C18 0.0410(12) 0.0501(14) 0.0324(11) 0.0003(10) 0.0025(9) -0.0082(10)
C19 0.0733(17) 0.0511(15) 0.0546(15) -0.0021(12) 0.0220(13) -0.0159(13)
C20 0.087(2) 0.0650(19) 0.0654(18) 0.0028(15) 0.0351(15) -0.0195(16)
C21 0.0734(18) 0.080(2) 0.0497(15) -0.0058(14) 0.0236(13) -0.0109(15)
C22 0.0724(18) 0.0620(17) 0.0549(16) -0.0133(13) 0.0164(13) -0.0071(14)
C23 0.0581(15) 0.0506(15) 0.0430(13) -0.0012(11) 0.0092(11) -0.0103(12)
C24 0.0559(14) 0.0426(14) 0.0476(14) 0.0027(11) 0.0168(11) -0.0138(11)
C25 0.0819(19) 0.0527(16) 0.0596(17) -0.0083(13) 0.0256(14) -0.0102(14)
C26 0.085(2) 0.0489(16) 0.077(2) 0.0046(15) 0.0269(16) 0.0089(15)
C27 0.0690(17) 0.0537(16) 0.0629(17) 0.0149(13) 0.0204(13) 0.0016(13)
C28 0.0751(18) 0.0548(16) 0.0470(15) 0.0038(12) 0.0187(12) 0.0010(14)
C29 0.0638(16) 0.0426(14) 0.0523(15) 0.0017(11) 0.0177(12) -0.0019(11)
C30 0.111(3) 0.093(2) 0.080(2) 0.027(2) 0.0163(19) 0.033(2)
C31 0.102(6) 0.076(6) 0.048(4) -0.006(3) 0.014(4) -0.005(5)
C32 0.129(11) 0.059(8) 0.054(7) -0.006(4) 0.018(6) 0.010(6)
C33 0.064(5) 0.123(8) 0.102(6) -0.048(6) -0.008(4) -0.005(5)
C34 0.072(9) 0.133(13) 0.086(11) 0.014(8) 0.024(8) 0.045(8)
C35 0.118(8) 0.073(5) 0.089(6) 0.002(4) 0.006(5) -0.005(5)
C36 0.213(16) 0.064(7) 0.219(18) -0.018(9) 0.068(14) -0.075(9)
C31' 0.174(12) 0.164(12) 0.116(8) -0.082(8) -0.040(8) 0.043(10)
C32' 0.23(2) 0.077(14) 0.148(15) -0.020(9) 0.049(14) 0.006(11)
C33' 0.100(6) 0.118(8) 0.085(5) 0.020(5) -0.005(5) 0.029(6)
C34' 0.103(11) 0.143(15) 0.083(10) -0.017(11) -0.029(8) 0.022(10)
C35' 0.129(9) 0.198(15) 0.191(14) 0.077(12) 0.047(9) 0.046(10)
C36' 0.130(9) 0.131(10) 0.125(9) -0.032(8) 0.028(7) 0.030(7)
N1 0.0574(12) 0.0418(11) 0.0376(10) 0.0047(8) 0.0086(8) -0.0066(9)
N2 0.0598(12) 0.0517(12) 0.0397(11) -0.0002(9) 0.0103(9) -0.0170(10)
N3 0.0834(18) 0.0679(16) 0.0486(14) -0.0014(12) -0.0060(12) 0.0081(14)
O1 0.0761(12) 0.0453(10) 0.0543(10) 0.0122(8) 0.0000(8) 0.0010(9)
O2 0.0461(10) 0.0661(12) 0.0615(11) 0.0033(9) -0.0025(8) 0.0004(8)
O3 0.0455(9) 0.0749(13) 0.0648(11) 0.0096(9) 0.0117(8) -0.0079(9)
O4 0.0954(15) 0.0767(13) 0.0577(11) -0.0045(10) 0.0045(10) -0.0471(11)
S1 0.0492(4) 0.0451(4) 0.0435(3) 0.0065(3) 0.0007(2) -0.0001(3)
S2 0.0566(4) 0.0587(4) 0.0466(4) 0.0024(3) 0.0077(3) -0.0242(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.505(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C7 1.374(3) . ?
C2 C3 1.380(3) . ?
C3 C4 1.376(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.374(3) . ?
C5 S1 1.756(2) . ?
C6 C7 1.375(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.316(3) . ?
C8 C9 1.399(3) . ?
C8 C11 1.543(3) . ?
C8 C10 2.019(3) . ?
C9 C10 1.410(3) . ?
C9 C18 1.458(3) . ?
C11 C12 1.504(3) . ?
C11 C10 1.537(3) . ?
C11 H10A 0.98(2) . ?
C10 N2 1.313(3) . ?
C12 C13 1.379(3) . ?
C12 C17 1.379(3) . ?
C17 C16 1.379(3) . ?
C17 H12 0.9300 . ?
C16 C15 1.378(4) . ?
C16 H13 0.9300 . ?
C15 C14 1.366(4) . ?
C15 H14 0.9300 . ?
C14 C13 1.375(3) . ?
C14 H15 0.9300 . ?
C13 H16 0.9300 . ?
C18 C19 1.382(3) . ?
C18 C23 1.393(3) . ?
C19 C20 1.373(4) . ?
C19 H18 0.9300 . ?
C20 C21 1.362(4) . ?
C20 H19 0.9300 . ?
C21 C22 1.371(4) . ?
C21 H20 0.9300 . ?
C22 C23 1.372(3) . ?
C22 H21 0.9300 . ?
C23 H22 0.9300 . ?
C24 C29 1.375(3) . ?
C24 C25 1.387(4) . ?
C24 S2 1.755(2) . ?
C25 C26 1.371(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.382(4) . ?
C27 C30 1.506(4) . ?
C28 C29 1.383(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 N3 1.495(9) . ?
C31 C32 1.61(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.41(3) . ?
C33 N3 1.574(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N3 1.472(8) . ?
C35 C36 1.514(17) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C31' C32' 1.29(3) . ?
C31' N3 1.447(10) . ?
C31' H31C 0.9700 . ?
C31' H31D 0.9700 . ?
C32' H32D 0.9600 . ?
C32' H32E 0.9600 . ?
C32' H32F 0.9600 . ?
C33' C34' 1.43(3) . ?
C33' N3 1.431(8) . ?
C33' H33C 0.9700 . ?
C33' H33D 0.9700 . ?
C34' H34D 0.9600 . ?
C34' H34E 0.9600 . ?
C34' H34F 0.9600 . ?
C35' C36' 1.305(18) . ?
C35' N3 1.623(13) . ?
C35' H35C 0.9700 . ?
C35' H35D 0.9700 . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?
N1 S1 1.610(2) . ?
N2 S2 1.617(2) . ?
N3 H3A 0.854(10) . ?
O1 S1 1.4501(17) . ?
O2 S1 1.4308(17) . ?
O3 S2 1.4305(19) . ?
O4 S2 1.4320(18) . ?
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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 118.5(2) . . ?
C7 C2 C1 121.0(2) . . ?
C3 C2 C1 120.5(2) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.1(2) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.5(2) . . ?
C6 C5 S1 119.93(17) . . ?
C4 C5 S1 119.53(17) . . ?
C5 C6 C7 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C2 C7 C6 121.5(2) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
N1 C8 C9 130.8(2) . . ?
N1 C8 C11 136.0(2) . . ?
C9 C8 C11 93.16(17) . . ?
N1 C8 C10 174.64(18) . . ?
C9 C8 C10 44.26(13) . . ?
C11 C8 C10 48.91(12) . . ?
C8 C9 C10 91.92(18) . . ?
C8 C9 C18 134.4(2) . . ?
C10 C9 C18 133.1(2) . . ?
C12 C11 C10 117.47(18) . . ?
C12 C11 C8 118.33(18) . . ?
C10 C11 C8 81.95(16) . . ?
C12 C11 H10A 107.6(12) . . ?
C10 C11 H10A 115.3(12) . . ?
C8 C11 H10A 114.7(12) . . ?
N2 C10 C9 130.3(2) . . ?
N2 C10 C11 136.7(2) . . ?
C9 C10 C11 92.95(17) . . ?
N2 C10 C8 173.67(19) . . ?
C9 C10 C8 43.82(13) . . ?
C11 C10 C8 49.14(12) . . ?
C13 C12 C17 118.3(2) . . ?
C13 C12 C11 120.5(2) . . ?
C17 C12 C11 121.2(2) . . ?
C12 C17 C16 121.0(2) . . ?
C12 C17 H12 119.5 . . ?
C16 C17 H12 119.5 . . ?
C15 C16 C17 119.6(2) . . ?
C15 C16 H13 120.2 . . ?
C17 C16 H13 120.2 . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H14 120.0 . . ?
C16 C15 H14 120.0 . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H15 120.0 . . ?
C13 C14 H15 120.0 . . ?
C14 C13 C12 121.1(2) . . ?
C14 C13 H16 119.4 . . ?
C12 C13 H16 119.4 . . ?
C19 C18 C23 117.8(2) . . ?
C19 C18 C9 121.9(2) . . ?
C23 C18 C9 120.2(2) . . ?
C20 C19 C18 120.8(3) . . ?
C20 C19 H18 119.6 . . ?
C18 C19 H18 119.6 . . ?
C21 C20 C19 121.0(3) . . ?
C21 C20 H19 119.5 . . ?
C19 C20 H19 119.5 . . ?
C20 C21 C22 119.1(3) . . ?
C20 C21 H20 120.4 . . ?
C22 C21 H20 120.4 . . ?
C21 C22 C23 120.8(3) . . ?
C21 C22 H21 119.6 . . ?
C23 C22 H21 119.6 . . ?
C22 C23 C18 120.5(2) . . ?
C22 C23 H22 119.7 . . ?
C18 C23 H22 119.7 . . ?
C29 C24 C25 119.8(2) . . ?
C29 C24 S2 120.2(2) . . ?
C25 C24 S2 120.02(19) . . ?
C26 C25 C24 119.8(3) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 121.4(3) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C28 C27 C26 118.1(3) . . ?
C28 C27 C30 120.9(3) . . ?
C26 C27 C30 121.0(3) . . ?
C27 C28 C29 121.4(2) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C24 C29 C28 119.6(2) . . ?
C24 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 C32 113.2(8) . . ?
N3 C31 H31A 108.9 . . ?
C32 C31 H31A 108.9 . . ?
N3 C31 H31B 108.9 . . ?
C32 C31 H31B 108.9 . . ?
H31A C31 H31B 107.8 . . ?
C34 C33 N3 114.4(12) . . ?
C34 C33 H33A 108.7 . . ?
N3 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
N3 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
N3 C35 C36 118.0(10) . . ?
N3 C35 H35A 107.8 . . ?
C36 C35 H35A 107.8 . . ?
N3 C35 H35B 107.8 . . ?
C36 C35 H35B 107.8 . . ?
H35A C35 H35B 107.2 . . ?
C32' C31' N3 121.0(15) . . ?
C32' C31' H31C 107.1 . . ?
N3 C31' H31C 107.1 . . ?
C32' C31' H31D 107.1 . . ?
N3 C31' H31D 107.1 . . ?
H31C C31' H31D 106.8 . . ?
C31' C32' H32D 109.5 . . ?
C31' C32' H32E 109.5 . . ?
H32D C32' H32E 109.5 . . ?
C31' C32' H32F 109.5 . . ?
H32D C32' H32F 109.5 . . ?
H32E C32' H32F 109.5 . . ?
C34' C33' N3 117.5(13) . . ?
C34' C33' H33C 107.9 . . ?
N3 C33' H33C 107.9 . . ?
C34' C33' H33D 107.9 . . ?
N3 C33' H33D 107.9 . . ?
H33C C33' H33D 107.2 . . ?
C33' C34' H34D 109.5 . . ?
C33' C34' H34E 109.5 . . ?
H34D C34' H34E 109.5 . . ?
C33' C34' H34F 109.5 . . ?
H34D C34' H34F 109.5 . . ?
H34E C34' H34F 109.5 . . ?
C36' C35' N3 105.7(13) . . ?
C36' C35' H35C 110.6 . . ?
N3 C35' H35C 110.6 . . ?
C36' C35' H35D 110.6 . . ?
N3 C35' H35D 110.6 . . ?
H35C C35' H35D 108.7 . . ?
C35' C36' H36D 109.5 . . ?
C35' C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C35' C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C8 N1 S1 119.23(16) . . ?
C10 N2 S2 120.66(17) . . ?
C33' N3 C31' 111.8(7) . . ?
C33' N3 C35 59.5(5) . . ?
C31' N3 C35 134.2(7) . . ?
C33' N3 C31 140.7(5) . . ?
C31' N3 C31 41.2(6) . . ?
C35 N3 C31 114.2(5) . . ?
C33' N3 C33 49.1(5) . . ?
C31' N3 C33 71.2(7) . . ?
C35 N3 C33 107.4(6) . . ?
C31 N3 C33 112.1(5) . . ?
C33' N3 C35' 109.7(6) . . ?
C31' N3 C35' 106.5(9) . . ?
C35 N3 C35' 51.4(6) . . ?
C31 N3 C35' 68.8(7) . . ?
C33 N3 C35' 149.5(6) . . ?
C33' N3 H3A 114(2) . . ?
C31' N3 H3A 114(2) . . ?
C35 N3 H3A 109(2) . . ?
C31 N3 H3A 105(2) . . ?
C33 N3 H3A 109(2) . . ?
C35' N3 H3A 100(2) . . ?
O2 S1 O1 116.31(11) . . ?
O2 S1 N1 113.36(10) . . ?
O1 S1 N1 104.95(10) . . ?
O2 S1 C5 108.45(10) . . ?
O1 S1 C5 106.86(10) . . ?
N1 S1 C5 106.30(10) . . ?
O3 S2 O4 117.08(12) . . ?
O3 S2 N2 113.06(11) . . ?
O4 S2 N2 105.25(11) . . ?
O3 S2 C24 108.74(11) . . ?
O4 S2 C24 107.11(12) . . ?
N2 S2 C24 104.75(11) . . ?
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
C7 C2 C3 C4 1.6(4) . . . . ?
C1 C2 C3 C4 -176.6(2) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C3 C4 C5 C6 -1.8(3) . . . . ?
C3 C4 C5 S1 176.29(18) . . . . ?
C4 C5 C6 C7 1.7(4) . . . . ?
S1 C5 C6 C7 -176.38(18) . . . . ?
C3 C2 C7 C6 -1.7(4) . . . . ?
C1 C2 C7 C6 176.5(3) . . . . ?
C5 C6 C7 C2 0.0(4) . . . . ?
N1 C8 C9 C10 177.1(2) . . . . ?
C11 C8 C9 C10 -1.11(17) . . . . ?
N1 C8 C9 C18 5.8(4) . . . . ?
C11 C8 C9 C18 -172.5(2) . . . . ?
C10 C8 C9 C18 -171.4(3) . . . . ?
N1 C8 C11 C12 66.0(3) . . . . ?
C9 C8 C11 C12 -115.9(2) . . . . ?
C10 C8 C11 C12 -116.9(2) . . . . ?
N1 C8 C11 C10 -177.1(3) . . . . ?
C9 C8 C11 C10 1.03(16) . . . . ?
C8 C9 C10 N2 -176.9(2) . . . . ?
C18 C9 C10 N2 -5.4(4) . . . . ?
C8 C9 C10 C11 1.12(17) . . . . ?
C18 C9 C10 C11 172.7(2) . . . . ?
C18 C9 C10 C8 171.5(3) . . . . ?
C12 C11 C10 N2 -65.4(3) . . . . ?
C8 C11 C10 N2 176.8(3) . . . . ?
C12 C11 C10 C9 116.8(2) . . . . ?
C8 C11 C10 C9 -1.02(16) . . . . ?
C12 C11 C10 C8 117.8(2) . . . . ?
N1 C8 C10 N2 -2(3) . . . . ?
C9 C8 C10 N2 22.0(17) . . . . ?
C11 C8 C10 N2 -159.5(17) . . . . ?
N1 C8 C10 C9 -24(2) . . . . ?
C11 C8 C10 C9 178.5(2) . . . . ?
N1 C8 C10 C11 157(2) . . . . ?
C9 C8 C10 C11 -178.5(2) . . . . ?
C10 C11 C12 C13 -51.1(3) . . . . ?
C8 C11 C12 C13 44.7(3) . . . . ?
C10 C11 C12 C17 127.9(2) . . . . ?
C8 C11 C12 C17 -136.3(2) . . . . ?
C13 C12 C17 C16 0.7(4) . . . . ?
C11 C12 C17 C16 -178.4(2) . . . . ?
C12 C17 C16 C15 -0.6(4) . . . . ?
C17 C16 C15 C14 0.3(4) . . . . ?
C16 C15 C14 C13 -0.2(4) . . . . ?
C15 C14 C13 C12 0.3(4) . . . . ?
C17 C12 C13 C14 -0.6(4) . . . . ?
C11 C12 C13 C14 178.5(2) . . . . ?
C8 C9 C18 C19 -3.4(4) . . . . ?
C10 C9 C18 C19 -171.6(2) . . . . ?
C8 C9 C18 C23 173.3(2) . . . . ?
C10 C9 C18 C23 5.2(4) . . . . ?
C23 C18 C19 C20 -1.0(4) . . . . ?
C9 C18 C19 C20 175.8(3) . . . . ?
C18 C19 C20 C21 -0.1(5) . . . . ?
C19 C20 C21 C22 1.0(5) . . . . ?
C20 C21 C22 C23 -0.8(4) . . . . ?
C21 C22 C23 C18 -0.4(4) . . . . ?
C19 C18 C23 C22 1.3(3) . . . . ?
C9 C18 C23 C22 -175.6(2) . . . . ?
C29 C24 C25 C26 0.8(4) . . . . ?
S2 C24 C25 C26 -179.4(2) . . . . ?
C24 C25 C26 C27 -0.1(4) . . . . ?
C25 C26 C27 C28 -0.7(4) . . . . ?
C25 C26 C27 C30 179.0(3) . . . . ?
C26 C27 C28 C29 0.9(4) . . . . ?
C30 C27 C28 C29 -178.8(3) . . . . ?
C25 C24 C29 C28 -0.6(4) . . . . ?
S2 C24 C29 C28 179.61(19) . . . . ?
C27 C28 C29 C24 -0.3(4) . . . . ?
C9 C8 N1 S1 -173.79(18) . . . . ?
C11 C8 N1 S1 3.7(3) . . . . ?
C10 C8 N1 S1 -151.8(19) . . . . ?
C9 C10 N2 S2 172.04(18) . . . . ?
C11 C10 N2 S2 -5.1(4) . . . . ?
C8 C10 N2 S2 152.2(16) . . . . ?
C34' C33' N3 C31' -77.9(15) . . . . ?
C34' C33' N3 C35 152.6(14) . . . . ?
C34' C33' N3 C31 -115.7(13) . . . . ?
C34' C33' N3 C33 -41.5(11) . . . . ?
C34' C33' N3 C35' 164.2(13) . . . . ?
C32' C31' N3 C33' 165(2) . . . . ?
C32' C31' N3 C35 -127(2) . . . . ?
C32' C31' N3 C31 -51.2(19) . . . . ?
C32' C31' N3 C33 137(2) . . . . ?
C32' C31' N3 C35' -75(2) . . . . ?
C36 C35 N3 C33' 172.5(13) . . . . ?
C36 C35 N3 C31' 80.9(17) . . . . ?
C36 C35 N3 C31 36.4(13) . . . . ?
C36 C35 N3 C33 161.3(11) . . . . ?
C36 C35 N3 C35' 6.4(13) . . . . ?
C32 C31 N3 C33' 104.8(13) . . . . ?
C32 C31 N3 C31' 45.2(12) . . . . ?
C32 C31 N3 C35 175.5(10) . . . . ?
C32 C31 N3 C33 53.1(12) . . . . ?
C32 C31 N3 C35' -159.7(12) . . . . ?
C34 C33 N3 C33' 53.8(17) . . . . ?
C34 C33 N3 C31' -161.8(19) . . . . ?
C34 C33 N3 C35 66.6(18) . . . . ?
C34 C33 N3 C31 -167.3(17) . . . . ?
C34 C33 N3 C35' 107(2) . . . . ?
C36' C35' N3 C33' -62.0(11) . . . . ?
C36' C35' N3 C31' 176.9(10) . . . . ?
C36' C35' N3 C35 -49.3(10) . . . . ?
C36' C35' N3 C31 160.0(12) . . . . ?
C36' C35' N3 C33 -102.2(15) . . . . ?
C8 N1 S1 O2 35.2(2) . . . . ?
C8 N1 S1 O1 163.19(16) . . . . ?
C8 N1 S1 C5 -83.81(18) . . . . ?
C6 C5 S1 O2 10.6(2) . . . . ?
C4 C5 S1 O2 -167.56(18) . . . . ?
C6 C5 S1 O1 -115.5(2) . . . . ?
C4 C5 S1 O1 66.3(2) . . . . ?
C6 C5 S1 N1 132.79(19) . . . . ?
C4 C5 S1 N1 -45.4(2) . . . . ?
C10 N2 S2 O3 -15.9(2) . . . . ?
C10 N2 S2 O4 -144.89(19) . . . . ?
C10 N2 S2 C24 102.3(2) . . . . ?
C29 C24 S2 O3 16.0(2) . . . . ?
C25 C24 S2 O3 -163.73(19) . . . . ?
C29 C24 S2 O4 143.4(2) . . . . ?
C25 C24 S2 O4 -36.3(2) . . . . ?
C29 C24 S2 N2 -105.1(2) . . . . ?
C25 C24 S2 N2 75.1(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 26.53
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.408
_refine_diff_density_min -0.331
_refine_diff_density_rms 0.056