# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_rrt_i9_10
_database_code_depnum_ccdc_archive 'CCDC 1499236'
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_audit_creation_date 2016-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common 'Sulfathiazoium besilate'
_chemical_name_systematic
;
4-(1,3-thiazol-2(3H)-ylidenesulfamoyl)anilinium benzenesulfonate
;
_chemical_formula_moiety 'C9 H10 N3 O2 S2, C6 H5 O3 S'
_chemical_formula_sum 'C15 H15 N3 O5 S3'
_chemical_formula_weight 413.48
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 60
_space_group_name_H-M_alt 'P b c n'
_space_group_name_Hall '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 28.4964(13)
_cell_length_b 8.1448(3)
_cell_length_c 15.5302(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3604.5(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 5771
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 20.30
_cell_measurement_theta_min 2.60
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.444
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6736
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996) SADABS. University of Gottingen, Germany.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.524
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1712
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.5
_exptl_crystal_size_min 0.3
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1164
_diffrn_reflns_av_unetI/netI 0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max 36
_diffrn_reflns_limit_h_min -37
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 85436
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.496
_diffrn_reflns_theta_min 1.429
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2768
_reflns_number_total 4115
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.391
_refine_diff_density_min -0.561
_refine_diff_density_rms 0.085
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.102
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 354
_refine_ls_number_reflns 4115
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1032
_refine_ls_R_factor_gt 0.0537
_refine_ls_restrained_S_all 1.102
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+5.5171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0998
_refine_ls_wR_factor_ref 0.1220
_refine_special_details ?
_olex2_refinement_description
;
1. Others
Sof(H1B)=Sof(H2AA)=Sof(C0AA)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C8)=
Sof(H8)=1-FVAR(1)
Sof(H1A)=Sof(C1AA)=Sof(C2AA)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
Sof(H2)=FVAR(1)
;
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S002 S 0.32050(3) 1.17582(9) 0.63788(5) 0.02101(19) Uani 1 1 d . . . . .
S003 S 0.26432(3) 1.17845(12) 0.45103(6) 0.0393(3) Uani 1 1 d . . . . .
O004 O 0.27062(7) 1.1469(3) 0.63572(14) 0.0292(5) Uani 1 1 d . . . . .
O005 O 0.33948(8) 1.2581(3) 0.71230(14) 0.0325(6) Uani 1 1 d . . . . .
N00A N 0.33839(8) 1.2800(3) 0.55657(16) 0.0212(6) Uani 1 1 d . . . . .
N007 N 0.40941(9) 0.5126(3) 0.62919(19) 0.0193(5) Uani 1 1 d . . . . .
H00A H 0.3899(12) 0.435(4) 0.604(2) 0.025(9) Uiso 1 1 d . . . . .
H00B H 0.4099(12) 0.486(4) 0.687(3) 0.042(11) Uiso 1 1 d . . . . .
H00C H 0.4366(17) 0.513(6) 0.607(3) 0.073(16) Uiso 1 1 d . . . . .
N008 N 0.33216(10) 1.3647(4) 0.41524(18) 0.0279(6) Uani 1 1 d . . . . .
H008 H 0.3573(13) 1.416(4) 0.418(2) 0.038(11) Uiso 1 1 d . . . . .
C00C C 0.38835(10) 0.6758(3) 0.62499(17) 0.0167(6) Uani 1 1 d . . . . .
C00D C 0.34796(10) 0.9816(3) 0.62978(18) 0.0182(6) Uani 1 1 d . . . . .
C00E C 0.31569(10) 1.2776(3) 0.48202(19) 0.0206(7) Uani 1 1 d . . . . .
C00F C 0.39604(11) 0.9658(4) 0.6376(3) 0.0353(9) Uani 1 1 d . . . . .
H00F H 0.4152(13) 1.057(5) 0.643(2) 0.044(11) Uiso 1 1 d . . . . .
C00G C 0.34071(11) 0.6909(4) 0.6149(3) 0.0332(9) Uani 1 1 d . . . . .
H00G H 0.3233(12) 0.601(4) 0.606(2) 0.035(10) Uiso 1 1 d . . . . .
C00H C 0.32058(11) 0.8456(4) 0.6169(2) 0.0337(8) Uani 1 1 d . . . . .
H00H H 0.2884(13) 0.857(5) 0.617(2) 0.047(11) Uiso 1 1 d . . . . .
C00I C 0.41629(11) 0.8120(4) 0.6353(3) 0.0349(9) Uani 1 1 d . . . . .
H00I H 0.4493(13) 0.794(4) 0.642(2) 0.043(11) Uiso 1 1 d . . . . .
C00J C 0.30639(14) 1.3559(5) 0.3405(2) 0.0403(9) Uani 1 1 d . . . . .
H00J H 0.3152(13) 1.417(5) 0.290(3) 0.054(12) Uiso 1 1 d . . . . .
C00M C 0.26917(16) 1.2604(6) 0.3478(3) 0.0509(11) Uani 1 1 d . . . . .
H00M H 0.2455(16) 1.236(5) 0.313(3) 0.062(13) Uiso 1 1 d . . . . .
S001 S 0.44592(3) 0.46117(9) 0.87799(5) 0.02046(19) Uani 1 1 d . . . . .
O00B O 0.41943(9) 0.5083(4) 0.80296(15) 0.0531(8) Uani 1 1 d . . . . .
O006 O 0.49364(8) 0.5171(3) 0.87819(17) 0.0416(7) Uani 1 1 d . . . . .
O009 O 0.42035(9) 0.5096(4) 0.95374(15) 0.0514(8) Uani 1 1 d . . . . .
C1 C 0.41415(14) 0.1440(5) 0.8810(3) 0.0423(10) Uani 1 1 d . . . . .
H1A H 0.384(2) 0.191(7) 0.839(4) 0.021(16) Uiso 0.495(4) 1 d . . . A 1
H1B H 0.396(2) 0.182(7) 0.922(4) 0.010(14) Uiso 0.505(4) 1 d . . . A 2
H2AA H 0.386(3) -0.076(14) 0.875(6) 0.04(3) Uiso 0.505(4) 1 d . . . A 1
C1AA C 0.4471(2) 0.2447(9) 0.9045(5) 0.0209(15) Uani 0.495(4) 1 d . . . A 1
C2AA C 0.4105(11) -0.012(4) 0.8851(14) 0.039(5) Uani 0.495(4) 1 d . . . A 1
C5 C 0.4822(2) 0.1788(8) 0.9557(4) 0.0265(15) Uani 0.495(4) 1 d . . . A 1
H5 H 0.505(2) 0.238(7) 0.977(4) 0.013(16) Uiso 0.495(4) 1 d . . . A 1
C6 C 0.4802(3) 0.0152(9) 0.9734(5) 0.0382(19) Uani 0.495(4) 1 d . . . A 1
H6 H 0.5000 0.0000 1.0000 0.006(15) Uiso 0.990(7) 2 d S T P A 1
C7 C 0.4452(3) -0.0863(10) 0.9420(5) 0.042(2) Uani 0.495(4) 1 d . . . A 1
H7 H 0.450(2) -0.189(9) 0.957(4) 0.028(19) Uiso 0.495(4) 1 d . . . A 1
C0AA C 0.4487(2) 0.2519(8) 0.8539(5) 0.0218(14) Uani 0.505(4) 1 d . . . A 2
C2 C 0.4219(10) -0.033(4) 0.8795(19) 0.052(8) Uani 0.505(4) 1 d . . . A 2
H2 H 0.400(5) -0.116(15) 0.891(8) 0.07(4) Uiso 0.495(4) 1 d . . . A 2
C3 C 0.4861(3) 0.0272(9) 0.7791(5) 0.0293(16) Uani 0.505(4) 1 d . . . A 2
H3 H 0.5000 -0.020(11) 0.7500 0.11(4) Uiso 1.010(7) 2 d S T P A 2
C4 C 0.4834(2) 0.1940(8) 0.7978(4) 0.0242(15) Uani 0.505(4) 1 d . . . A 2
H4 H 0.5000 0.270(7) 0.7500 0.066(19) Uiso 1.010(7) 2 d S T P A 2
C8 C 0.4560(3) -0.0828(9) 0.8177(5) 0.0361(18) Uani 0.505(4) 1 d . . . A 2
H8 H 0.459(3) -0.210(13) 0.801(6) 0.10(4) Uiso 0.505(4) 1 d . . . A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S002 0.0204(4) 0.0170(4) 0.0257(4) -0.0009(3) 0.0011(3) 0.0016(3)
S003 0.0330(5) 0.0474(6) 0.0376(5) 0.0057(5) -0.0125(4) -0.0154(4)
O004 0.0190(10) 0.0283(12) 0.0403(14) 0.0047(11) 0.0077(10) 0.0046(9)
O005 0.0461(14) 0.0255(12) 0.0259(12) -0.0086(10) -0.0065(10) 0.0020(11)
N00A 0.0179(12) 0.0175(13) 0.0281(14) 0.0010(11) -0.0024(11) -0.0012(10)
N007 0.0200(13) 0.0175(14) 0.0203(14) -0.0003(11) -0.0012(12) -0.0005(11)
N008 0.0245(15) 0.0307(17) 0.0285(15) 0.0054(13) 0.0030(12) -0.0001(13)
C00C 0.0191(14) 0.0147(15) 0.0162(14) 0.0027(12) 0.0012(11) 0.0017(12)
C00D 0.0193(14) 0.0168(15) 0.0187(15) 0.0029(12) 0.0007(12) -0.0011(12)
C00E 0.0181(15) 0.0159(16) 0.0278(16) -0.0010(13) -0.0006(12) 0.0025(12)
C00F 0.0209(16) 0.0178(18) 0.067(3) 0.0006(18) -0.0144(17) -0.0075(14)
C00G 0.0202(16) 0.0157(17) 0.064(3) -0.0079(17) -0.0036(16) -0.0059(13)
C00H 0.0154(15) 0.0239(18) 0.062(2) -0.0028(17) 0.0000(16) -0.0006(14)
C00I 0.0150(15) 0.0243(18) 0.065(3) -0.0001(18) -0.0122(16) 0.0003(13)
C00J 0.046(2) 0.050(3) 0.0247(18) 0.0074(18) -0.0010(16) 0.0048(19)
C00M 0.051(3) 0.068(3) 0.034(2) 0.001(2) -0.016(2) -0.007(2)
S001 0.0190(4) 0.0203(4) 0.0221(4) -0.0013(3) 0.0021(3) -0.0005(3)
O00B 0.0530(17) 0.088(2) 0.0181(12) -0.0043(14) -0.0093(12) 0.0070(16)
O006 0.0228(12) 0.0342(14) 0.0679(19) -0.0017(13) 0.0000(12) -0.0076(11)
O009 0.0416(15) 0.092(2) 0.0206(12) 0.0034(14) 0.0119(11) 0.0269(15)
C1 0.037(2) 0.034(2) 0.055(3) -0.003(2) 0.015(2) -0.0085(18)
C1AA 0.022(3) 0.023(4) 0.019(3) 0.002(3) 0.004(3) 0.001(3)
C2AA 0.054(15) 0.028(10) 0.035(7) 0.000(5) -0.017(7) -0.003(9)
C5 0.033(4) 0.022(4) 0.025(3) 0.001(3) -0.001(3) 0.001(3)
C6 0.050(5) 0.036(5) 0.028(4) 0.008(3) -0.009(4) 0.016(4)
C7 0.078(6) 0.016(4) 0.031(4) 0.004(3) 0.010(4) 0.003(4)
C0AA 0.016(3) 0.022(4) 0.027(4) 0.005(3) -0.005(3) -0.001(3)
C2 0.046(12) 0.011(8) 0.098(15) 0.005(7) -0.015(8) -0.004(8)
C3 0.033(4) 0.027(4) 0.028(4) -0.001(3) -0.004(3) 0.009(3)
C4 0.023(3) 0.026(4) 0.023(3) 0.000(3) -0.002(3) 0.001(3)
C8 0.055(5) 0.024(4) 0.029(4) 0.001(3) -0.005(3) -0.002(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
S002 O004 1.441(2) . ?
S002 O005 1.441(2) . ?
S002 N00A 1.605(3) . ?
S002 C00D 1.769(3) . ?
S003 C00E 1.740(3) . ?
S003 C00M 1.742(4) . ?
N00A C00E 1.326(4) . ?
N007 H00A 0.92(3) . ?
N007 H00B 0.92(4) . ?
N007 H00C 0.85(5) . ?
N007 C00C 1.460(4) . ?
N008 H008 0.83(4) . ?
N008 C00E 1.341(4) . ?
N008 C00J 1.376(5) . ?
C00C C00G 1.372(4) . ?
C00C C00I 1.375(4) . ?
C00D C00F 1.382(4) . ?
C00D C00H 1.370(4) . ?
C00F H00F 0.93(4) . ?
C00F C00I 1.380(5) . ?
C00G H00G 0.90(4) . ?
C00G C00H 1.385(5) . ?
C00H H00H 0.92(4) . ?
C00I H00I 0.96(4) . ?
C00J H00J 0.96(4) . ?
C00J C00M 1.320(6) . ?
C00M H00M 0.89(4) . ?
S001 O00B 1.440(2) . ?
S001 O006 1.434(2) . ?
S001 O009 1.439(2) . ?
S001 C1AA 1.811(7) . ?
S001 C0AA 1.747(7) . ?
C1 H1A 1.13(6) . ?
C1 H1B 0.88(6) . ?
C1 C1AA 1.300(8) . ?
C1 C2AA 1.28(3) . ?
C1 C0AA 1.385(8) . ?
C1 C2 1.46(3) . ?
C1AA C5 1.385(10) . ?
C2AA H2AA 0.89(11) . ?
C2AA C7 1.46(3) . ?
C5 H5 0.87(6) . ?
C5 C6 1.362(10) . ?
C6 C6 1.422(16) 5_657 ?
C6 H6 0.711(8) . ?
C6 C7 1.382(12) . ?
C7 H7 0.88(7) . ?
C0AA C4 1.399(9) . ?
C2 H2 0.94(15) . ?
C2 C8 1.42(3) . ?
C3 C3 1.202(17) 3_656 ?
C3 H3 0.71(5) . ?
C3 C4 2.007(10) 3_656 ?
C3 C4 1.392(10) . ?
C3 C8 1.377(10) . ?
C4 C3 2.007(10) 3_656 ?
C4 C4 1.762(12) 3_656 ?
C4 H4 1.08(3) . ?
C8 H8 1.07(11) . ?
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
O004 S002 O005 117.69(14) . . ?
O004 S002 N00A 112.42(13) . . ?
O004 S002 C00D 106.77(13) . . ?
O005 S002 N00A 105.42(13) . . ?
O005 S002 C00D 107.85(13) . . ?
N00A S002 C00D 106.05(13) . . ?
C00E S003 C00M 90.57(18) . . ?
C00E N00A S002 121.6(2) . . ?
H00A N007 H00B 105(3) . . ?
H00A N007 H00C 113(4) . . ?
H00B N007 H00C 112(4) . . ?
C00C N007 H00A 110.7(19) . . ?
C00C N007 H00B 105(2) . . ?
C00C N007 H00C 111(3) . . ?
C00E N008 H008 121(3) . . ?
C00E N008 C00J 116.0(3) . . ?
C00J N008 H008 123(3) . . ?
C00G C00C N007 119.5(3) . . ?
C00G C00C C00I 121.0(3) . . ?
C00I C00C N007 119.4(3) . . ?
C00F C00D S002 121.0(2) . . ?
C00H C00D S002 118.8(2) . . ?
C00H C00D C00F 120.2(3) . . ?
N00A C00E S003 131.2(2) . . ?
N00A C00E N008 119.8(3) . . ?
N008 C00E S003 109.0(2) . . ?
C00D C00F H00F 121(2) . . ?
C00I C00F C00D 119.8(3) . . ?
C00I C00F H00F 119(2) . . ?
C00C C00G H00G 119(2) . . ?
C00C C00G C00H 119.2(3) . . ?
C00H C00G H00G 121(2) . . ?
C00D C00H C00G 120.2(3) . . ?
C00D C00H H00H 119(2) . . ?
C00G C00H H00H 120(2) . . ?
C00C C00I C00F 119.6(3) . . ?
C00C C00I H00I 117(2) . . ?
C00F C00I H00I 123(2) . . ?
N008 C00J H00J 121(2) . . ?
C00M C00J N008 112.7(4) . . ?
C00M C00J H00J 126(2) . . ?
S003 C00M H00M 114(3) . . ?
C00J C00M S003 111.7(3) . . ?
C00J C00M H00M 134(3) . . ?
O00B S001 C1AA 117.0(3) . . ?
O00B S001 C0AA 96.3(3) . . ?
O006 S001 O00B 114.46(17) . . ?
O006 S001 O009 113.04(17) . . ?
O006 S001 C1AA 106.9(2) . . ?
O006 S001 C0AA 105.5(2) . . ?
O009 S001 O00B 108.85(15) . . ?
O009 S001 C1AA 95.2(3) . . ?
O009 S001 C0AA 117.8(3) . . ?
C1AA C1 H1A 119(3) . . ?
C2AA C1 H1A 108(3) . . ?
C2AA C1 C1AA 132.3(13) . . ?
C0AA C1 H1B 115(4) . . ?
C0AA C1 C2 120.9(13) . . ?
C2 C1 H1B 117(4) . . ?
C1 C1AA S001 122.4(5) . . ?
C1 C1AA C5 116.0(6) . . ?
C5 C1AA S001 121.4(5) . . ?
C1 C2AA H2AA 130(7) . . ?
C1 C2AA C7 112.8(19) . . ?
C7 C2AA H2AA 114(7) . . ?
C1AA C5 H5 122(4) . . ?
C6 C5 C1AA 117.6(7) . . ?
C6 C5 H5 120(4) . . ?
C5 C6 C6 104.6(9) . 5_657 ?
C5 C6 H6 104.6(9) . . ?
C5 C6 C7 123.0(8) . . ?
C6 C6 H6 0.0(6) 5_657 . ?
C7 C6 C6 132.4(9) . 5_657 ?
C7 C6 H6 132.4(9) . . ?
C2AA C7 H7 132(5) . . ?
C6 C7 C2AA 117.1(14) . . ?
C6 C7 H7 111(4) . . ?
C1 C0AA S001 121.4(5) . . ?
C1 C0AA C4 118.5(6) . . ?
C4 C0AA S001 119.6(5) . . ?
C1 C2 H2 127(8) . . ?
C8 C2 C1 113(2) . . ?
C8 C2 H2 113(8) . . ?
C3 C3 H3 33(6) 3_656 . ?
C3 C3 C4 42.9(3) 3_656 3_656 ?
C3 C3 C4 101.2(4) 3_656 . ?
C3 C3 C8 137.5(5) 3_656 . ?
C4 C3 H3 75(6) 3_656 . ?
C4 C3 H3 134(7) . . ?
C4 C3 C4 59.2(5) . 3_656 ?
C8 C3 H3 106(6) . . ?
C8 C3 C4 165.8(6) . 3_656 ?
C8 C3 C4 120.6(8) . . ?
C0AA C4 C3 154.8(6) . 3_656 ?
C0AA C4 C4 154.8(5) . 3_656 ?
C0AA C4 H4 123(3) . . ?
C3 C4 C0AA 119.9(6) . . ?
C3 C4 C3 36.0(6) . 3_656 ?
C3 C4 C4 78.1(4) . 3_656 ?
C3 C4 H4 78(3) 3_656 . ?
C3 C4 H4 113(3) . . ?
C4 C4 C3 42.7(3) 3_656 3_656 ?
C4 C4 H4 35(3) 3_656 . ?
C2 C8 H8 119(5) . . ?
C3 C8 C2 122.2(14) . . ?
C3 C8 H8 119(5) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S002 N00A C00E S003 1.9(4) . . . . ?
S002 N00A C00E N008 -179.1(2) . . . . ?
S002 C00D C00F C00I 176.7(3) . . . . ?
S002 C00D C00H C00G -176.5(3) . . . . ?
O004 S002 N00A C00E -26.7(3) . . . . ?
O004 S002 C00D C00F -174.3(3) . . . . ?
O004 S002 C00D C00H 4.7(3) . . . . ?
O005 S002 N00A C00E -156.1(2) . . . . ?
O005 S002 C00D C00F -46.9(3) . . . . ?
O005 S002 C00D C00H 132.1(3) . . . . ?
N00A S002 C00D C00F 65.7(3) . . . . ?
N00A S002 C00D C00H -115.3(3) . . . . ?
N007 C00C C00G C00H 175.6(3) . . . . ?
N007 C00C C00I C00F -175.4(3) . . . . ?
N008 C00J C00M S003 0.9(5) . . . . ?
C00C C00G C00H C00D -0.7(6) . . . . ?
C00D S002 N00A C00E 89.7(3) . . . . ?
C00D C00F C00I C00C 0.3(6) . . . . ?
C00E S003 C00M C00J -1.0(4) . . . . ?
C00E N008 C00J C00M -0.2(5) . . . . ?
C00F C00D C00H C00G 2.5(5) . . . . ?
C00G C00C C00I C00F 1.5(5) . . . . ?
C00H C00D C00F C00I -2.2(6) . . . . ?
C00I C00C C00G C00H -1.3(5) . . . . ?
C00J N008 C00E S003 -0.5(4) . . . . ?
C00J N008 C00E N00A -179.7(3) . . . . ?
C00M S003 C00E N00A 179.9(3) . . . . ?
C00M S003 C00E N008 0.8(3) . . . . ?
S001 C1AA C5 C6 179.2(5) . . . . ?
S001 C0AA C4 C3 179.3(5) . . . . ?
S001 C0AA C4 C3 -166.7(9) . . . 3_656 ?
S001 C0AA C4 C4 -49.1(16) . . . 3_656 ?
O00B S001 C1AA C1 -25.1(7) . . . . ?
O00B S001 C1AA C5 158.8(5) . . . . ?
O00B S001 C0AA C1 -89.0(6) . . . . ?
O00B S001 C0AA C4 83.5(6) . . . . ?
O006 S001 C1AA C1 -154.8(5) . . . . ?
O006 S001 C1AA C5 29.0(7) . . . . ?
O006 S001 C0AA C1 153.4(5) . . . . ?
O006 S001 C0AA C4 -34.1(6) . . . . ?
O009 S001 C1AA C1 89.2(6) . . . . ?
O009 S001 C1AA C5 -87.0(6) . . . . ?
O009 S001 C0AA C1 26.2(7) . . . . ?
O009 S001 C0AA C4 -161.3(5) . . . . ?
C1 C1AA C5 C6 2.8(10) . . . . ?
C1 C2AA C7 C6 -8(3) . . . . ?
C1 C0AA C4 C3 6.0(16) . . . 3_656 ?
C1 C0AA C4 C3 -8.0(9) . . . . ?
C1 C0AA C4 C4 123.6(12) . . . 3_656 ?
C1 C2 C8 C3 15(3) . . . . ?
C1AA C1 C2AA C7 14(3) . . . . ?
C1AA C5 C6 C6 -179.7(7) . . . 5_657 ?
C1AA C5 C6 C7 0.7(11) . . . . ?
C2AA C1 C1AA S001 171.8(16) . . . . ?
C2AA C1 C1AA C5 -11.9(19) . . . . ?
C5 C6 C7 C2AA 2.2(16) . . . . ?
C6 C6 C7 C2AA -177.3(15) 5_657 . . . ?
C0AA C1 C2 C8 -25(2) . . . . ?
C2 C1 C0AA S001 -164.9(14) . . . . ?
C2 C1 C0AA C4 22.6(16) . . . . ?
C3 C3 C4 C0AA 169.9(7) 3_656 . . . ?
C3 C3 C4 C4 8.9(7) 3_656 . . 3_656 ?
C3 C3 C8 C2 -170.4(17) 3_656 . . . ?
C4 C3 C4 C0AA 161.0(8) 3_656 . . . ?
C4 C3 C4 C3 -8.9(7) 3_656 . . 3_656 ?
C4 C3 C8 C2 -87(3) 3_656 . . . ?
C4 C3 C8 C2 -1.6(17) . . . . ?
C8 C3 C4 C0AA -2.5(10) . . . . ?
C8 C3 C4 C3 -172.4(12) . . . 3_656 ?
C8 C3 C4 C4 -163.5(7) . . . 3_656 ?
_shelx_res_file
;
rrt_i9_10.res created by SHELXL-2014/7
TITL rrt_i9_10_a.res in Pbcn
REM Old TITL RRT_I9_10 in Pbcn #60
REM SHELXT solution in Pbcn
REM R1 0.193, Rweak 0.010, Alpha 0.043, Orientation as input
REM Formula found by SHELXT: C16 N3 O7 S3
CELL 0.71073 28.4964 8.1448 15.5302 90 90 90
ZERR 8 0.0013 0.0003 0.0007 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O S
UNIT 120 120 24 40 24
L.S. 4
PLAN 20
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
OMIT 4 2 0
OMIT 3 0 4
OMIT 1 0 2
REM
REM
REM
WGHT 0.036600 5.517100
FVAR 0.19078 0.49523
S002 5 0.320503 1.175820 0.637880 11.00000 0.02036 0.01699 =
0.02567 -0.00089 0.00111 0.00155
S003 5 0.264324 1.178447 0.451035 11.00000 0.03303 0.04744 =
0.03757 0.00571 -0.01249 -0.01545
O004 4 0.270618 1.146933 0.635718 11.00000 0.01898 0.02825 =
0.04033 0.00469 0.00769 0.00455
O005 4 0.339485 1.258061 0.712296 11.00000 0.04609 0.02546 =
0.02586 -0.00860 -0.00652 0.00204
N00A 3 0.338391 1.280036 0.556570 11.00000 0.01786 0.01750 =
0.02812 0.00105 -0.00245 -0.00124
N007 3 0.409415 0.512600 0.629187 11.00000 0.02000 0.01749 =
0.02027 -0.00031 -0.00118 -0.00047
H00A 2 0.389902 0.435481 0.604249 11.00000 0.02547
H00B 2 0.409912 0.486113 0.686590 11.00000 0.04164
H00C 2 0.436616 0.513228 0.606969 11.00000 0.07255
N008 3 0.332160 1.364699 0.415239 11.00000 0.02448 0.03069 =
0.02851 0.00544 0.00302 -0.00010
H008 2 0.357305 1.416205 0.418489 11.00000 0.03799
C00C 1 0.388347 0.675839 0.624992 11.00000 0.01907 0.01471 =
0.01624 0.00268 0.00120 0.00173
C00D 1 0.347955 0.981622 0.629784 11.00000 0.01929 0.01677 =
0.01868 0.00287 0.00065 -0.00106
C00E 1 0.315694 1.277598 0.482021 11.00000 0.01808 0.01588 =
0.02777 -0.00095 -0.00064 0.00253
C00F 1 0.396038 0.965829 0.637581 11.00000 0.02089 0.01783 =
0.06707 0.00061 -0.01443 -0.00750
H00F 2 0.415230 1.057269 0.642682 11.00000 0.04449
C00G 1 0.340711 0.690869 0.614858 11.00000 0.02020 0.01572 =
0.06369 -0.00786 -0.00364 -0.00586
H00G 2 0.323283 0.600670 0.605995 11.00000 0.03543
C00H 1 0.320579 0.845568 0.616884 11.00000 0.01539 0.02394 =
0.06190 -0.00285 0.00002 -0.00062
H00H 2 0.288393 0.857402 0.617340 11.00000 0.04727
C00I 1 0.416290 0.812020 0.635336 11.00000 0.01505 0.02432 =
0.06541 -0.00008 -0.01216 0.00028
H00I 2 0.449271 0.794131 0.641855 11.00000 0.04334
C00J 1 0.306388 1.355914 0.340491 11.00000 0.04613 0.05013 =
0.02474 0.00738 -0.00097 0.00484
H00J 2 0.315248 1.417393 0.290442 11.00000 0.05400
C00M 1 0.269174 1.260393 0.347842 11.00000 0.05119 0.06783 =
0.03381 0.00142 -0.01581 -0.00664
H00M 2 0.245466 1.235770 0.313040 11.00000 0.06201
S001 5 0.445917 0.461169 0.877990 11.00000 0.01897 0.02029 =
0.02211 -0.00126 0.00214 -0.00048
O00B 4 0.419435 0.508292 0.802963 11.00000 0.05296 0.08832 =
0.01808 -0.00428 -0.00929 0.00698
O006 4 0.493636 0.517056 0.878189 11.00000 0.02284 0.03421 =
0.06788 -0.00175 0.00002 -0.00762
O009 4 0.420353 0.509615 0.953736 11.00000 0.04156 0.09196 =
0.02058 0.00338 0.01188 0.02691
C1 1 0.414146 0.144000 0.881014 11.00000 0.03731 0.03449 =
0.05503 -0.00270 0.01454 -0.00848
PART 1
H1A 2 0.384337 0.191290 0.839492 21.00000 0.02148
PART 0
PART 2
H1B 2 0.396041 0.181633 0.922247 -21.00000 0.00951
PART 0
PART 1
H2AA 2 0.385870 -0.075562 0.874955 -21.00000 0.03642
C1AA 1 0.447139 0.244660 0.904532 21.00000 0.02156 0.02260 =
0.01861 0.00185 0.00436 0.00114
C2AA 1 0.410501 -0.012136 0.885079 21.00000 0.05411 0.02788 =
0.03545 0.00025 -0.01716 -0.00342
C5 1 0.482217 0.178809 0.955727 21.00000 0.03264 0.02221 =
0.02470 0.00110 -0.00072 0.00119
H5 2 0.504515 0.238208 0.977414 21.00000 0.01291
C6 1 0.480154 0.015153 0.973443 21.00000 0.04993 0.03641 =
0.02826 0.00784 -0.00886 0.01563
H6 2 0.500000 0.000000 1.000000 21.00000 0.00588
C7 1 0.445235 -0.086283 0.942030 21.00000 0.07803 0.01641 =
0.03055 0.00428 0.01021 0.00303
H7 2 0.450437 -0.189179 0.956815 21.00000 0.02783
PART 0
PART 2
C0AA 1 0.448682 0.251886 0.853871 -21.00000 0.01580 0.02244 =
0.02726 0.00500 -0.00545 -0.00100
C2 1 0.421937 -0.033068 0.879468 -21.00000 0.04619 0.01146 =
0.09788 0.00488 -0.01468 -0.00394
H2 2 0.399639 -0.115722 0.891045 21.00000 0.07329
C3 1 0.486074 0.027235 0.779060 -21.00000 0.03327 0.02653 =
0.02800 -0.00074 -0.00401 0.00947
H3 2 0.500000 -0.020091 0.750000 -21.00000 0.10686
C4 1 0.483354 0.194036 0.797799 -21.00000 0.02314 0.02622 =
0.02329 0.00003 -0.00208 0.00136
H4 2 0.500000 0.270084 0.750000 -21.00000 0.06569
C8 1 0.456044 -0.082765 0.817698 -21.00000 0.05509 0.02409 =
0.02919 0.00112 -0.00536 -0.00199
H8 2 0.458706 -0.210340 0.800760 -21.00000 0.09985
HKLF 4
REM rrt_i9_10_a.res in Pbcn
REM R1 = 0.0537 for 2768 Fo > 4sig(Fo) and 0.1032 for all 4115 data
REM 354 parameters refined using 0 restraints
END
WGHT 0.0366 5.5170
REM Highest difference peak 0.391, deepest hole -0.561, 1-sigma level 0.085
Q1 1 0.4190 0.5547 0.9752 11.00000 0.05 0.39
Q2 1 0.4287 0.4372 0.7930 11.00000 0.05 0.37
Q3 1 0.2915 1.1928 0.6398 11.00000 0.05 0.34
Q4 1 0.4094 0.7539 0.6800 11.00000 0.05 0.33
Q5 1 0.3228 1.3005 0.7336 11.00000 0.05 0.30
Q6 1 0.3353 0.9145 0.6437 11.00000 0.05 0.30
Q7 1 0.4117 0.4541 0.9971 11.00000 0.05 0.29
Q8 1 0.2911 1.2316 0.4617 11.00000 0.05 0.29
Q9 1 0.3695 0.9646 0.6249 11.00000 0.05 0.29
Q10 1 0.3366 1.1856 0.7243 11.00000 0.05 0.28
Q11 1 0.3918 0.5458 0.9484 11.00000 0.05 0.28
Q12 1 0.4997 0.5265 0.9393 11.00000 0.05 0.28
Q13 1 0.2983 0.4171 0.6023 11.00000 0.05 0.27
Q14 1 0.2876 0.8465 0.5666 11.00000 0.05 0.27
Q15 1 0.4831 0.5178 0.7514 11.00000 0.05 0.27
Q16 1 0.3601 0.0606 0.9231 11.00000 0.05 0.27
Q17 1 0.4089 0.5436 0.7858 11.00000 0.05 0.27
Q18 1 0.3729 0.1769 0.7616 11.00000 0.05 0.26
Q19 1 0.2614 1.1968 0.6214 11.00000 0.05 0.26
Q20 1 0.4090 1.0749 0.6889 11.00000 0.05 0.26
;
_shelx_res_checksum 40800
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_ee_sulfa_bf4_0m
_database_code_depnum_ccdc_archive 'CCDC 1499239'
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_audit_creation_method SHELXL-97
_chemical_name_systematic 'Sulfathiazoium tetrafluoroborate'
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C9 H10 B F4 N3 O2 S2'
_chemical_formula_weight 343.13
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/c
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 8.0557(2)
_cell_length_b 9.9422(3)
_cell_length_c 17.2090(5)
_cell_angle_alpha 90.00
_cell_angle_beta 90.5700(10)
_cell_angle_gamma 90.00
_cell_volume 1378.22(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9816
_cell_measurement_theta_min 2.37
_cell_measurement_theta_max 30.02
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.45
_exptl_crystal_size_min 0.44
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_diffrn 1.654
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 696
_exptl_absorpt_coefficient_mu 0.438
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7942
_exptl_absorpt_correction_T_max 0.8299
_exptl_absorpt_process_details 'Bruker SAINT'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(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 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 36555
_diffrn_reflns_av_R_equivalents 0.0309
_diffrn_reflns_av_sigmaI/netI 0.0154
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 2.53
_diffrn_reflns_theta_max 30.06
_reflns_number_total 4023
_reflns_number_gt 3622
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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^)+(0.0476P)^2^+0.9005P] 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 4023
_refine_ls_number_parameters 206
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0422
_refine_ls_R_factor_gt 0.0369
_refine_ls_wR_factor_ref 0.1008
_refine_ls_wR_factor_gt 0.0963
_refine_ls_goodness_of_fit_ref 1.096
_refine_ls_restrained_S_all 1.096
_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
S1 S 0.20898(4) 0.31777(4) 0.216501(18) 0.01835(9) Uani 1 1 d . . .
S2 S 0.22985(8) 0.51812(4) 0.06746(2) 0.04331(15) Uani 1 1 d . . .
O1 O 0.11296(12) 0.44110(12) 0.22023(6) 0.0261(2) Uani 1 1 d . . .
O2 O 0.15135(14) 0.20891(13) 0.26434(6) 0.0299(3) Uani 1 1 d . . .
N1 N 0.22350(14) 0.26062(12) 0.13062(6) 0.0183(2) Uani 1 1 d . . .
N2 N 0.24694(19) 0.29633(13) -0.00155(7) 0.0259(3) Uani 1 1 d . . .
N3 N 0.87665(14) 0.47488(13) 0.33905(7) 0.0181(2) Uani 1 1 d . . .
C1 C 0.41105(15) 0.36030(14) 0.24910(7) 0.0173(2) Uani 1 1 d . . .
C2 C 0.42047(17) 0.43733(17) 0.31628(9) 0.0270(3) Uani 1 1 d . . .
H2 H 0.3220 0.4658 0.3414 0.032 Uiso 1 1 calc R . .
C3 C 0.57442(18) 0.47222(17) 0.34637(9) 0.0272(3) Uani 1 1 d . . .
H3 H 0.5831 0.5234 0.3928 0.033 Uiso 1 1 calc R . .
C4 C 0.71513(15) 0.43151(14) 0.30785(8) 0.0175(2) Uani 1 1 d . . .
C5 C 0.70779(17) 0.35322(17) 0.24188(9) 0.0257(3) Uani 1 1 d . . .
H5 H 0.8066 0.3246 0.2172 0.031 Uiso 1 1 calc R . .
C6 C 0.55285(18) 0.31678(17) 0.21198(9) 0.0260(3) Uani 1 1 d . . .
H6 H 0.5446 0.2627 0.1666 0.031 Uiso 1 1 calc R . .
C7 C 0.23281(17) 0.34461(14) 0.07045(8) 0.0187(2) Uani 1 1 d . . .
C8 C 0.2564(3) 0.39114(18) -0.05980(9) 0.0385(4) Uani 1 1 d . . .
H8 H 0.2653 0.3696 -0.1134 0.046 Uiso 1 1 calc R . .
C9 C 0.2517(4) 0.51604(19) -0.03253(11) 0.0521(6) Uani 1 1 d . . .
H9 H 0.2594 0.5943 -0.0639 0.063 Uiso 1 1 calc R . .
B1 B 0.2135(2) 0.87700(16) 0.96900(9) 0.0210(3) Uani 1 1 d . . .
F11 F 0.13885(13) 0.85132(12) 0.89807(6) 0.0368(2) Uani 1 1 d . . .
F12 F 0.37545(12) 0.83359(11) 0.96791(6) 0.0356(2) Uani 1 1 d . . .
F13 F 0.20928(16) 1.01508(10) 0.98447(7) 0.0422(3) Uani 1 1 d . . .
F14 F 0.12722(13) 0.81143(9) 1.02814(5) 0.0296(2) Uani 1 1 d . . .
H31N H 0.955(3) 0.467(2) 0.3028(13) 0.032(5) Uiso 1 1 d . . .
H32N H 0.871(2) 0.558(2) 0.3537(12) 0.025(5) Uiso 1 1 d . . .
H33N H 0.901(2) 0.425(2) 0.3794(12) 0.024(5) Uiso 1 1 d . . .
H2N H 0.249(3) 0.216(3) -0.0118(13) 0.041(6) Uiso 1 1 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
S1 0.01446(15) 0.02658(18) 0.01404(15) -0.00132(11) 0.00098(10) -0.00369(11)
S2 0.0930(4) 0.01615(19) 0.0209(2) -0.00275(14) 0.0060(2) -0.0022(2)
O1 0.0187(4) 0.0379(6) 0.0217(5) -0.0058(4) 0.0022(4) 0.0059(4)
O2 0.0309(6) 0.0409(7) 0.0180(5) 0.0057(4) 0.0007(4) -0.0155(5)
N1 0.0204(5) 0.0198(5) 0.0145(5) -0.0005(4) -0.0013(4) -0.0036(4)
N2 0.0470(8) 0.0158(6) 0.0147(5) -0.0021(4) -0.0009(5) -0.0030(5)
N3 0.0156(5) 0.0228(6) 0.0159(5) -0.0030(4) -0.0008(4) -0.0006(4)
C1 0.0141(5) 0.0219(6) 0.0160(5) -0.0031(5) 0.0002(4) -0.0018(4)
C2 0.0158(6) 0.0379(8) 0.0273(7) -0.0166(6) 0.0033(5) 0.0002(5)
C3 0.0190(6) 0.0382(8) 0.0243(7) -0.0179(6) 0.0015(5) -0.0006(6)
C4 0.0149(5) 0.0204(6) 0.0171(6) -0.0033(5) -0.0003(4) -0.0013(4)
C5 0.0155(6) 0.0380(8) 0.0237(7) -0.0143(6) 0.0031(5) -0.0005(5)
C6 0.0182(6) 0.0385(8) 0.0215(6) -0.0164(6) 0.0024(5) -0.0028(6)
C7 0.0228(6) 0.0170(6) 0.0164(6) -0.0019(5) -0.0011(5) -0.0032(5)
C8 0.0766(13) 0.0235(8) 0.0156(7) 0.0014(6) 0.0015(7) -0.0034(8)
C9 0.114(2) 0.0205(8) 0.0216(8) 0.0039(6) 0.0068(10) -0.0030(10)
B1 0.0265(7) 0.0163(7) 0.0201(7) 0.0008(5) 0.0033(5) -0.0004(6)
F11 0.0381(5) 0.0479(6) 0.0243(5) 0.0020(4) -0.0069(4) -0.0046(5)
F12 0.0256(5) 0.0419(6) 0.0392(6) 0.0020(4) 0.0008(4) 0.0042(4)
F13 0.0628(7) 0.0149(4) 0.0492(7) -0.0019(4) 0.0189(5) -0.0025(4)
F14 0.0401(5) 0.0237(4) 0.0254(4) 0.0030(3) 0.0097(4) -0.0046(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.4395(11) . ?
S1 O1 1.4515(12) . ?
S1 N1 1.5888(12) . ?
S1 C1 1.7678(13) . ?
S2 C7 1.7260(14) . ?
S2 C9 1.7316(19) . ?
N1 C7 1.3328(17) . ?
N2 C7 1.3347(17) . ?
N2 C8 1.379(2) . ?
N2 H2N 0.82(3) . ?
N3 C4 1.4674(16) . ?
N3 H31N 0.89(2) . ?
N3 H32N 0.87(2) . ?
N3 H33N 0.87(2) . ?
C1 C6 1.3837(18) . ?
C1 C2 1.3883(19) . ?
C2 C3 1.3834(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.3795(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.3773(18) . ?
C5 C6 1.3933(19) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C8 C9 1.328(2) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
B1 F12 1.3742(19) . ?
B1 F11 1.3794(19) . ?
B1 F13 1.3989(18) . ?
B1 F14 1.3994(17) . ?
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
O2 S1 O1 115.77(7) . . ?
O2 S1 N1 106.88(7) . . ?
O1 S1 N1 112.79(6) . . ?
O2 S1 C1 107.43(7) . . ?
O1 S1 C1 105.86(7) . . ?
N1 S1 C1 107.74(6) . . ?
C7 S2 C9 90.93(8) . . ?
C7 N1 S1 120.25(10) . . ?
C7 N2 C8 115.78(13) . . ?
C7 N2 H2N 123.6(16) . . ?
C8 N2 H2N 120.6(16) . . ?
C4 N3 H31N 110.3(13) . . ?
C4 N3 H32N 109.9(13) . . ?
H31N N3 H32N 109.0(19) . . ?
C4 N3 H33N 108.2(13) . . ?
H31N N3 H33N 110.6(18) . . ?
H32N N3 H33N 108.8(18) . . ?
C6 C1 C2 121.23(12) . . ?
C6 C1 S1 122.72(10) . . ?
C2 C1 S1 116.02(10) . . ?
C3 C2 C1 119.43(12) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C4 C3 C2 118.98(13) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 122.22(12) . . ?
C5 C4 N3 119.89(12) . . ?
C3 C4 N3 117.89(12) . . ?
C4 C5 C6 118.84(12) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C5 119.27(13) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N1 C7 N2 120.12(13) . . ?
N1 C7 S2 130.43(10) . . ?
N2 C7 S2 109.45(10) . . ?
C9 C8 N2 112.36(15) . . ?
C9 C8 H8 123.8 . . ?
N2 C8 H8 123.8 . . ?
C8 C9 S2 111.46(13) . . ?
C8 C9 H9 124.3 . . ?
S2 C9 H9 124.3 . . ?
F12 B1 F11 109.60(13) . . ?
F12 B1 F13 109.62(13) . . ?
F11 B1 F13 109.80(13) . . ?
F12 B1 F14 110.01(13) . . ?
F11 B1 F14 109.99(13) . . ?
F13 B1 F14 107.78(12) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 30.06
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.556
_refine_diff_density_min -0.448
_refine_diff_density_rms 0.084
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_ee_sulfa_no3_0m
_database_code_depnum_ccdc_archive 'CCDC 1499238'
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_audit_creation_date 2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common 'Sulfathiazoium hydrogen dinitrate'
_chemical_name_systematic
;
4-(1,3-thiazol-2(3H)-ylidenesulfamoyl)anilinium nitrate nitric acid
;
_chemical_formula_moiety '2(C9 H10 N3 O2 S2), 2(N O3), H N O3'
_chemical_formula_sum 'C18 H21 N9 O13 S4'
_chemical_formula_weight 699.68
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.9484(4)
_cell_length_b 8.2585(2)
_cell_length_c 22.9621(6)
_cell_angle_alpha 90
_cell_angle_beta 100.8180(10)
_cell_angle_gamma 90
_cell_volume 2784.32(12)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9934
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 29.51
_cell_measurement_theta_min 2.63
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.423
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6821
_exptl_absorpt_correction_T_max 0.7460
_exptl_absorpt_process_details 'Bruker SAINT'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.669
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1440
_exptl_crystal_size_max 0.51
_exptl_crystal_size_mid 0.43
_exptl_crystal_size_min 0.18
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0461
_diffrn_reflns_av_unetI/netI 0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 67503
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 30.065
_diffrn_reflns_theta_min 1.791
_diffrn_ambient_temperature 173.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5971
_reflns_number_total 8100
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.415
_refine_diff_density_min -0.392
_refine_diff_density_rms 0.065
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 565
_refine_ls_number_reflns 8100
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0638
_refine_ls_R_factor_gt 0.0390
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+1.7483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0897
_refine_ls_wR_factor_ref 0.1022
_refine_special_details ?
_olex2_refinement_description
;
1. Others
Sof(O1AA)=Sof(O0AA)=Sof(O2AA)=1-FVAR(1)
Sof(O00H)=Sof(O00Q)=Sof(O00W)=FVAR(1)
Sof(O4AA)=Sof(O3AA)=Sof(O6)=1-FVAR(2)
Sof(O00V)=Sof(O00Y)=Sof(O018)=FVAR(2)
Sof(O1)=Sof(O2)=Sof(O4)=1-FVAR(3)
Sof(O6AA)=Sof(O7AA)=Sof(O5AA)=FVAR(3)
;
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S001 S 0.13148(3) 0.30896(5) 0.49677(2) 0.01997(10) Uani 1 1 d . . . . .
S002 S 0.32770(3) 0.67823(5) 0.68535(2) 0.02023(10) Uani 1 1 d . . . . .
S003 S 0.42112(3) 0.73805(6) 0.82372(2) 0.02831(11) Uani 1 1 d . . . . .
S004 S -0.02920(3) 0.28760(7) 0.37797(2) 0.03428(13) Uani 1 1 d . . . . .
O005 O 0.03847(9) 0.29044(16) 0.50404(6) 0.0277(3) Uani 1 1 d . . . . .
O006 O 0.29505(9) 0.59201(16) 0.63060(6) 0.0300(3) Uani 1 1 d . . . . .
O007 O 0.26518(9) 0.69654(17) 0.72555(6) 0.0299(3) Uani 1 1 d . . . . .
O008 O 0.19245(10) 0.39607(16) 0.54231(6) 0.0314(3) Uani 1 1 d . . . . .
N009 N 0.42078(10) 0.59130(18) 0.71402(6) 0.0216(3) Uani 1 1 d . . . . .
N00A N 0.53038(11) 1.66140(18) 0.53336(7) 0.0249(3) Uani 1 1 d . . . . .
N00B N 0.29406(11) -0.3510(2) 0.49479(8) 0.0246(3) Uani 1 1 d . . . . .
N00C N 0.41787(13) 1.3392(2) 0.60992(8) 0.0272(3) Uani 1 1 d . . . . .
N00D N 0.09683(11) 0.4108(2) 0.33434(7) 0.0253(3) Uani 1 1 d . . . . .
N00E N 0.14185(10) 0.39324(18) 0.43601(6) 0.0220(3) Uani 1 1 d . . . . .
N00F N 0.54636(11) 0.5800(2) 0.79018(7) 0.0257(3) Uani 1 1 d . . . . .
N00G N 0.34150(11) -0.4095(2) 0.34020(7) 0.0311(4) Uani 1 1 d . . . . .
O00H O 0.40855(12) -0.4097(2) 0.31447(8) 0.0340(5) Uani 0.824(3) 1 d . . P A 1
C00J C 0.46117(11) 0.6294(2) 0.76895(7) 0.0196(3) Uani 1 1 d . . . . .
C00L C 0.35636(11) 0.8760(2) 0.66546(7) 0.0181(3) Uani 1 1 d . . . . .
C00M C 0.17744(11) 0.1112(2) 0.49471(7) 0.0184(3) Uani 1 1 d . . . . .
C00N C 0.08008(11) 0.3678(2) 0.38750(8) 0.0203(3) Uani 1 1 d . . . . .
C00O C 0.25334(11) -0.1903(2) 0.49524(7) 0.0199(3) Uani 1 1 d . . . . .
C00P C 0.39572(12) 1.1785(2) 0.62936(7) 0.0208(3) Uani 1 1 d . . . . .
O00Q O 0.33501(16) -0.3120(2) 0.37861(8) 0.0446(6) Uani 0.824(3) 1 d . . P A 1
C00R C 0.17322(12) -0.1723(2) 0.51534(8) 0.0240(4) Uani 1 1 d . . . . .
C00S C 0.29784(13) 1.0020(2) 0.66976(9) 0.0259(4) Uani 1 1 d . . . . .
N00T N 0.29351(14) -0.8999(3) 0.30143(10) 0.0445(5) Uani 1 1 d . . . . .
C00U C 0.31765(13) 1.1557(2) 0.65136(9) 0.0257(4) Uani 1 1 d . . . . .
O00V O 0.21894(16) -0.8625(3) 0.31286(12) 0.0522(8) Uani 0.814(6) 1 d . . P B 1
O00W O 0.27905(13) -0.5100(3) 0.32237(11) 0.0540(7) Uani 0.824(3) 1 d . . P A 1
C00X C 0.13445(13) -0.0192(2) 0.51508(8) 0.0243(4) Uani 1 1 d . . . . .
O00Y O 0.34874(15) -0.7791(3) 0.29369(14) 0.0579(9) Uani 0.814(6) 1 d . . P B 1
C00Z C 0.43650(14) 0.8999(2) 0.64411(9) 0.0296(4) Uani 1 1 d . . . . .
C010 C 0.25829(14) 0.0918(2) 0.47467(10) 0.0332(5) Uani 1 1 d . . . . .
C011 C 0.29716(14) -0.0602(3) 0.47537(11) 0.0359(5) Uani 1 1 d . . . . .
C013 C 0.58223(14) 0.6265(3) 0.84767(9) 0.0317(4) Uani 1 1 d . . . . .
C014 C 0.45653(14) 1.0531(2) 0.62613(9) 0.0314(4) Uani 1 1 d . . . . .
C015 C 0.52402(15) 0.7136(3) 0.87218(9) 0.0323(4) Uani 1 1 d . . . . .
C016 C -0.04396(15) 0.3116(3) 0.30166(9) 0.0378(5) Uani 1 1 d . . . . .
C017 C 0.02813(14) 0.3792(3) 0.28649(9) 0.0332(4) Uani 1 1 d . . . . .
O018 O 0.3217(2) -1.0335(4) 0.29824(18) 0.0716(10) Uani 0.814(6) 1 d . . P B 1
H00A H 0.3551(18) -0.346(3) 0.5146(11) 0.044(7) Uiso 1 1 d . . . . .
H00Z H 0.4734(17) 0.811(3) 0.6409(11) 0.041(7) Uiso 1 1 d . . . . .
H00H H 0.5723(16) 0.525(3) 0.7677(11) 0.040(7) Uiso 1 1 d . . . . .
H00B H 0.2932(16) -0.378(3) 0.4583(11) 0.035(6) Uiso 1 1 d . . . . .
H00U H 0.2754(16) 1.246(3) 0.6514(10) 0.038(6) Uiso 1 1 d . . . . .
H00X H 0.0789(16) -0.003(3) 0.5263(10) 0.035(6) Uiso 1 1 d . . . . .
H011 H 0.3519(19) -0.071(3) 0.4646(12) 0.056(8) Uiso 1 1 d . . . . .
H013 H 0.6435(16) 0.596(3) 0.8643(10) 0.040(6) Uiso 1 1 d . . . . .
H010 H 0.2847(17) 0.183(3) 0.4601(11) 0.043(7) Uiso 1 1 d . . . . .
H015 H 0.5329(16) 0.756(3) 0.9082(11) 0.036(6) Uiso 1 1 d . . . . .
H00R H 0.1491(16) -0.261(3) 0.5308(10) 0.037(6) Uiso 1 1 d . . . . .
H014 H 0.5100(18) 1.075(3) 0.6121(11) 0.051(7) Uiso 1 1 d . . . . .
H016 H -0.0968(19) 0.284(3) 0.2777(12) 0.050(7) Uiso 1 1 d . . . . .
O1AA O 0.2679(5) -0.4177(12) 0.3628(3) 0.036(2) Uani 0.176(3) 1 d . . P A -1
O0AA O 0.3989(6) -0.3131(13) 0.3616(6) 0.058(3) Uani 0.176(3) 1 d . . P A -1
O2AA O 0.3581(9) -0.5200(15) 0.3075(5) 0.067(4) Uani 0.176(3) 1 d . . P A -1
O4AA O 0.2700(11) -0.7823(17) 0.3256(6) 0.077(5) Uani 0.186(6) 1 d . . P B -1
O3AA O 0.3602(9) -0.8694(18) 0.2672(7) 0.076(5) Uani 0.186(6) 1 d . . P B -1
O6 O 0.2678(14) -1.0371(18) 0.3009(8) 0.080(5) Uani 0.186(6) 1 d . . P B -1
O6AA O 0.4690(2) 1.6218(6) 0.56256(18) 0.0289(8) Uani 0.689(15) 1 d . . P C 1
O7AA O 0.5086(4) 1.7473(7) 0.4901(2) 0.0398(10) Uani 0.689(15) 1 d . . P C 1
H00E H 0.3784(17) 1.412(3) 0.6154(11) 0.043(7) Uiso 1 1 d . . . . .
H00C H 0.2613(18) -0.423(3) 0.5086(11) 0.046(7) Uiso 1 1 d . . . . .
H017 H 0.0354(16) 0.401(3) 0.2462(11) 0.041(7) Uiso 1 1 d . . . . .
H00S H 0.2448(16) 0.981(3) 0.6856(10) 0.036(6) Uiso 1 1 d . . . . .
H00F H 0.4705(19) 1.372(3) 0.6323(12) 0.048(7) Uiso 1 1 d . . . . .
H00G H 0.4269(19) 1.336(3) 0.5707(13) 0.056(8) Uiso 1 1 d . . . . .
H00D H 0.1466(16) 0.448(3) 0.3326(10) 0.033(6) Uiso 1 1 d . . . . .
H00Y H 0.322(3) -0.687(7) 0.312(2) 0.126(17) Uiso 1 1 d . . . . .
O5AA O 0.60863(18) 1.6150(3) 0.5513(4) 0.0473(16) Uani 0.689(15) 1 d . . P C 1
O1 O 0.6072(4) 1.6281(9) 0.5172(6) 0.032(2) Uani 0.311(15) 1 d . . P C -1
O2 O 0.5076(17) 1.6042(13) 0.5744(7) 0.074(5) Uani 0.311(15) 1 d . . P C -1
O4 O 0.4798(10) 1.749(2) 0.4960(8) 0.065(3) Uani 0.311(15) 1 d . . P C -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S001 0.0266(2) 0.01648(19) 0.01694(19) 0.00035(15) 0.00430(16) -0.00073(16)
S002 0.01922(19) 0.01781(19) 0.0227(2) 0.00088(16) 0.00135(15) -0.00231(15)
S003 0.0262(2) 0.0354(3) 0.0248(2) -0.00675(19) 0.00841(18) 0.00125(19)
S004 0.0217(2) 0.0536(3) 0.0274(2) 0.0039(2) 0.00428(18) -0.0088(2)
O005 0.0318(7) 0.0261(7) 0.0289(7) 0.0049(5) 0.0155(6) 0.0040(5)
O006 0.0329(7) 0.0214(6) 0.0305(7) -0.0029(5) -0.0073(6) -0.0050(5)
O007 0.0229(6) 0.0302(7) 0.0386(8) 0.0083(6) 0.0116(6) -0.0010(5)
O008 0.0485(9) 0.0210(6) 0.0218(6) -0.0031(5) -0.0007(6) -0.0048(6)
N009 0.0234(7) 0.0200(7) 0.0208(7) -0.0004(6) 0.0025(6) 0.0029(6)
N00A 0.0264(8) 0.0185(7) 0.0309(8) -0.0031(6) 0.0086(6) -0.0042(6)
N00B 0.0228(8) 0.0214(8) 0.0299(9) 0.0005(6) 0.0057(7) 0.0032(6)
N00C 0.0400(10) 0.0193(8) 0.0248(8) 0.0003(6) 0.0124(7) -0.0051(7)
N00D 0.0227(8) 0.0319(9) 0.0222(7) 0.0058(6) 0.0065(6) 0.0014(7)
N00E 0.0232(7) 0.0228(7) 0.0201(7) 0.0038(6) 0.0042(6) -0.0024(6)
N00F 0.0250(8) 0.0306(8) 0.0207(7) -0.0018(6) 0.0024(6) 0.0050(6)
N00G 0.0285(8) 0.0350(9) 0.0310(9) -0.0004(7) 0.0086(7) 0.0007(7)
O00H 0.0277(9) 0.0447(11) 0.0323(9) -0.0065(8) 0.0123(7) -0.0070(8)
C00J 0.0220(8) 0.0171(8) 0.0205(8) 0.0023(6) 0.0062(6) -0.0012(6)
C00L 0.0201(8) 0.0178(8) 0.0153(7) -0.0007(6) 0.0006(6) -0.0014(6)
C00M 0.0206(8) 0.0168(8) 0.0167(7) -0.0007(6) 0.0004(6) -0.0018(6)
C00N 0.0199(8) 0.0186(8) 0.0232(8) 0.0036(6) 0.0062(6) 0.0036(6)
C00O 0.0197(8) 0.0182(8) 0.0206(8) -0.0016(6) 0.0004(6) -0.0001(6)
C00P 0.0287(9) 0.0182(8) 0.0159(7) -0.0008(6) 0.0051(6) -0.0040(7)
O00Q 0.0685(16) 0.0387(11) 0.0321(10) -0.0029(8) 0.0235(10) 0.0063(10)
C00R 0.0255(9) 0.0208(8) 0.0275(9) 0.0061(7) 0.0095(7) -0.0002(7)
C00S 0.0222(8) 0.0224(9) 0.0357(10) 0.0027(8) 0.0122(8) 0.0019(7)
N00T 0.0390(11) 0.0411(12) 0.0513(12) 0.0066(10) 0.0030(9) -0.0010(9)
C00U 0.0240(9) 0.0211(9) 0.0329(10) 0.0029(7) 0.0076(7) 0.0036(7)
O00V 0.0384(13) 0.0478(14) 0.0767(17) -0.0064(12) 0.0273(11) -0.0115(11)
O00W 0.0251(10) 0.0538(13) 0.0847(17) -0.0140(12) 0.0143(10) -0.0144(9)
C00X 0.0233(9) 0.0229(9) 0.0289(9) 0.0043(7) 0.0108(7) 0.0011(7)
O00Y 0.0354(12) 0.0452(16) 0.099(2) -0.0053(15) 0.0287(13) -0.0087(10)
C00Z 0.0289(10) 0.0224(9) 0.0417(11) -0.0010(8) 0.0179(8) 0.0017(7)
C010 0.0292(10) 0.0216(9) 0.0533(13) 0.0038(9) 0.0194(9) -0.0055(8)
C011 0.0265(10) 0.0263(10) 0.0614(14) 0.0035(9) 0.0243(10) -0.0015(8)
C013 0.0286(10) 0.0391(11) 0.0245(9) 0.0006(8) -0.0027(8) 0.0025(8)
C014 0.0332(10) 0.0265(10) 0.0408(11) -0.0008(8) 0.0232(9) -0.0031(8)
C015 0.0367(11) 0.0400(12) 0.0191(9) -0.0042(8) 0.0026(8) -0.0005(9)
C016 0.0278(10) 0.0572(14) 0.0249(10) 0.0022(10) -0.0042(8) -0.0003(10)
C017 0.0363(11) 0.0416(12) 0.0201(9) 0.0053(8) 0.0015(8) 0.0063(9)
O018 0.0540(18) 0.0420(15) 0.119(3) 0.0149(15) 0.0156(19) 0.0121(14)
O1AA 0.025(4) 0.062(6) 0.024(4) -0.010(4) 0.008(3) -0.006(4)
O0AA 0.023(5) 0.049(6) 0.099(9) -0.006(6) 0.007(5) -0.010(4)
O2AA 0.085(9) 0.066(8) 0.060(7) -0.034(6) 0.042(6) -0.007(7)
O4AA 0.092(12) 0.056(8) 0.098(10) -0.009(7) 0.062(9) 0.015(8)
O3AA 0.075(8) 0.067(9) 0.100(10) -0.014(7) 0.053(7) -0.001(7)
O6 0.093(13) 0.051(8) 0.103(11) 0.022(7) 0.033(10) -0.004(9)
O6AA 0.0239(14) 0.0331(16) 0.0316(13) 0.0072(11) 0.0097(11) -0.0029(11)
O7AA 0.044(3) 0.0496(19) 0.0292(14) 0.0147(12) 0.0166(17) 0.0095(19)
O5AA 0.0240(12) 0.0376(14) 0.080(5) 0.0208(16) 0.0098(15) 0.0029(10)
O1 0.032(3) 0.030(3) 0.033(5) 0.002(3) 0.004(2) 0.009(2)
O2 0.139(14) 0.040(4) 0.064(7) 0.014(4) 0.075(9) 0.008(7)
O4 0.046(6) 0.091(7) 0.060(6) 0.022(5) 0.015(5) 0.038(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S001 O005 1.4392(14) . ?
S001 O008 1.4437(14) . ?
S001 N00E 1.5925(15) . ?
S001 C00M 1.7757(17) . ?
S002 O006 1.4475(13) . ?
S002 O007 1.4395(14) . ?
S002 N009 1.5941(15) . ?
S002 C00L 1.7699(17) . ?
S003 C00J 1.7403(17) . ?
S003 C015 1.733(2) . ?
S004 C00N 1.7380(18) . ?
S004 C016 1.736(2) . ?
N009 C00J 1.330(2) . ?
N00A O6AA 1.276(4) . ?
N00A O7AA 1.215(6) . ?
N00A O5AA 1.226(3) . ?
N00A O1 1.301(7) . ?
N00A O2 1.162(10) . ?
N00A O4 1.260(15) . ?
N00B C00O 1.461(2) . ?
N00B H00A 0.94(3) . ?
N00B H00B 0.86(2) . ?
N00B H00C 0.87(3) . ?
N00C C00P 1.458(2) . ?
N00C H00E 0.87(3) . ?
N00C H00F 0.90(3) . ?
N00C H00G 0.94(3) . ?
N00D C00N 1.339(2) . ?
N00D C017 1.381(3) . ?
N00D H00D 0.81(2) . ?
N00E C00N 1.323(2) . ?
N00F C00J 1.339(2) . ?
N00F C013 1.383(2) . ?
N00F H00H 0.84(2) . ?
N00G O00H 1.255(2) . ?
N00G O00Q 1.211(2) . ?
N00G O00W 1.259(3) . ?
N00G O1AA 1.303(8) . ?
N00G O0AA 1.206(10) . ?
N00G O2AA 1.237(10) . ?
O00H O0AA 1.373(12) . ?
O00H O2AA 1.175(13) . ?
C00L C00S 1.375(2) . ?
C00L C00Z 1.391(2) . ?
C00M C00X 1.380(2) . ?
C00M C010 1.381(3) . ?
C00O C00R 1.370(2) . ?
C00O C011 1.380(3) . ?
C00P C00U 1.369(2) . ?
C00P C014 1.389(3) . ?
O00Q O1AA 1.327(9) . ?
O00Q O0AA 1.098(10) . ?
C00R C00X 1.390(3) . ?
C00R H00R 0.92(2) . ?
C00S C00U 1.387(3) . ?
C00S H00S 0.95(2) . ?
N00T O00V 1.232(3) . ?
N00T O00Y 1.328(3) . ?
N00T O018 1.188(4) . ?
N00T O4AA 1.204(12) . ?
N00T O3AA 1.404(12) . ?
N00T O6 1.195(15) . ?
C00U H00U 0.98(2) . ?
O00V O4AA 1.012(17) . ?
O00V O6 1.662(17) . ?
O00W O1AA 1.237(8) . ?
O00W O2AA 1.293(11) . ?
C00X H00X 0.92(2) . ?
O00Y O4AA 1.499(13) . ?
O00Y O3AA 0.998(14) . ?
O00Y H00Y 0.99(5) . ?
C00Z C014 1.381(3) . ?
C00Z H00Z 0.93(3) . ?
C010 C011 1.382(3) . ?
C010 H010 0.94(3) . ?
C011 H011 0.90(3) . ?
C013 C015 1.332(3) . ?
C013 H013 0.96(2) . ?
C014 H014 0.93(3) . ?
C015 H015 0.88(2) . ?
C016 C017 1.317(3) . ?
C016 H016 0.90(3) . ?
C017 H017 0.97(2) . ?
O018 O3AA 1.683(13) . ?
O018 O6 0.819(18) . ?
O4AA H00Y 1.19(5) . ?
O6AA O2 0.61(2) . ?
O7AA O1 1.785(7) . ?
O5AA O1 0.787(6) . ?
O5AA O2 1.695(17) . ?
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
O005 S001 O008 117.46(8) . . ?
O005 S001 N00E 113.78(8) . . ?
O005 S001 C00M 107.00(8) . . ?
O008 S001 N00E 105.35(8) . . ?
O008 S001 C00M 106.42(8) . . ?
N00E S001 C00M 106.07(8) . . ?
O006 S002 N009 105.25(8) . . ?
O006 S002 C00L 106.76(8) . . ?
O007 S002 O006 117.06(9) . . ?
O007 S002 N009 113.82(8) . . ?
O007 S002 C00L 106.63(8) . . ?
N009 S002 C00L 106.70(8) . . ?
C015 S003 C00J 91.13(9) . . ?
C016 S004 C00N 91.26(10) . . ?
C00J N009 S002 119.40(12) . . ?
O6AA N00A O1 148.8(5) . . ?
O7AA N00A O6AA 118.1(3) . . ?
O7AA N00A O5AA 123.3(3) . . ?
O7AA N00A O1 90.3(4) . . ?
O7AA N00A O4 22.1(6) . . ?
O5AA N00A O6AA 118.5(3) . . ?
O5AA N00A O1 36.1(2) . . ?
O5AA N00A O4 145.2(6) . . ?
O2 N00A O6AA 28.3(12) . . ?
O2 N00A O7AA 145.8(10) . . ?
O2 N00A O5AA 90.4(10) . . ?
O2 N00A O1 123.7(8) . . ?
O2 N00A O4 123.8(8) . . ?
O4 N00A O6AA 96.1(7) . . ?
O4 N00A O1 112.1(5) . . ?
C00O N00B H00A 109.0(16) . . ?
C00O N00B H00B 107.9(16) . . ?
C00O N00B H00C 111.1(17) . . ?
H00A N00B H00B 108(2) . . ?
H00A N00B H00C 114(2) . . ?
H00B N00B H00C 106(2) . . ?
C00P N00C H00E 112.7(17) . . ?
C00P N00C H00F 108.8(17) . . ?
C00P N00C H00G 110.4(17) . . ?
H00E N00C H00F 105(2) . . ?
H00E N00C H00G 113(2) . . ?
H00F N00C H00G 107(2) . . ?
C00N N00D C017 115.88(17) . . ?
C00N N00D H00D 118.4(16) . . ?
C017 N00D H00D 125.7(16) . . ?
C00N N00E S001 120.04(12) . . ?
C00J N00F C013 115.80(17) . . ?
C00J N00F H00H 117.4(17) . . ?
C013 N00F H00H 126.8(17) . . ?
O00H N00G O00W 117.08(19) . . ?
O00H N00G O1AA 174.6(4) . . ?
O00Q N00G O00H 121.6(2) . . ?
O00Q N00G O00W 121.3(2) . . ?
O00Q N00G O1AA 63.6(4) . . ?
O00Q N00G O2AA 170.2(7) . . ?
O00W N00G O1AA 57.7(4) . . ?
O0AA N00G O00H 67.8(6) . . ?
O0AA N00G O00Q 54.0(6) . . ?
O0AA N00G O00W 174.7(6) . . ?
O0AA N00G O1AA 117.5(7) . . ?
O0AA N00G O2AA 121.7(8) . . ?
O2AA N00G O00H 56.2(6) . . ?
O2AA N00G O00W 62.4(6) . . ?
O2AA N00G O1AA 119.0(7) . . ?
N00G O00H O0AA 54.4(4) . . ?
O2AA O00H N00G 61.1(5) . . ?
O2AA O00H O0AA 113.5(6) . . ?
N009 C00J S003 130.61(14) . . ?
N009 C00J N00F 120.33(16) . . ?
N00F C00J S003 109.05(13) . . ?
C00S C00L S002 119.47(13) . . ?
C00S C00L C00Z 121.28(17) . . ?
C00Z C00L S002 119.22(13) . . ?
C00X C00M S001 120.11(13) . . ?
C00X C00M C010 120.96(17) . . ?
C010 C00M S001 118.88(13) . . ?
N00D C00N S004 108.58(13) . . ?
N00E C00N S004 131.10(13) . . ?
N00E C00N N00D 120.30(16) . . ?
C00R C00O N00B 119.51(16) . . ?
C00R C00O C011 121.76(17) . . ?
C011 C00O N00B 118.74(16) . . ?
C00U C00P N00C 119.76(16) . . ?
C00U C00P C014 121.94(17) . . ?
C014 C00P N00C 118.28(16) . . ?
N00G O00Q O1AA 61.6(4) . . ?
O0AA O00Q N00G 62.7(6) . . ?
O0AA O00Q O1AA 124.1(7) . . ?
C00O C00R C00X 119.15(17) . . ?
C00O C00R H00R 118.3(15) . . ?
C00X C00R H00R 122.4(15) . . ?
C00L C00S C00U 119.72(17) . . ?
C00L C00S H00S 118.3(15) . . ?
C00U C00S H00S 122.0(14) . . ?
O00V N00T O00Y 116.8(2) . . ?
O00V N00T O3AA 147.2(6) . . ?
O00Y N00T O3AA 42.7(6) . . ?
O018 N00T O00V 126.3(3) . . ?
O018 N00T O00Y 116.9(3) . . ?
O018 N00T O4AA 156.3(7) . . ?
O018 N00T O3AA 80.5(6) . . ?
O018 N00T O6 40.2(9) . . ?
O4AA N00T O00V 49.1(8) . . ?
O4AA N00T O00Y 72.4(8) . . ?
O4AA N00T O3AA 114.4(9) . . ?
O6 N00T O00V 86.4(9) . . ?
O6 N00T O00Y 156.5(9) . . ?
O6 N00T O4AA 130.4(11) . . ?
O6 N00T O3AA 115.2(10) . . ?
C00P C00U C00S 118.93(17) . . ?
C00P C00U H00U 119.4(14) . . ?
C00S C00U H00U 121.6(14) . . ?
N00T O00V O6 45.9(6) . . ?
O4AA O00V N00T 64.0(6) . . ?
O4AA O00V O6 106.5(9) . . ?
N00G O00W O2AA 58.0(5) . . ?
O1AA O00W N00G 63.0(4) . . ?
O1AA O00W O2AA 119.8(6) . . ?
C00M C00X C00R 119.40(16) . . ?
C00M C00X H00X 118.8(15) . . ?
C00R C00X H00X 121.7(15) . . ?
N00T O00Y O4AA 50.0(6) . . ?
N00T O00Y H00Y 102(3) . . ?
O4AA O00Y H00Y 52(3) . . ?
O3AA O00Y N00T 72.7(7) . . ?
O3AA O00Y O4AA 121.7(9) . . ?
O3AA O00Y H00Y 164(3) . . ?
C00L C00Z H00Z 118.5(15) . . ?
C014 C00Z C00L 119.01(18) . . ?
C014 C00Z H00Z 122.4(15) . . ?
C00M C010 C011 119.60(17) . . ?
C00M C010 H010 118.4(15) . . ?
C011 C010 H010 122.0(15) . . ?
C00O C011 C010 119.12(18) . . ?
C00O C011 H011 121.7(18) . . ?
C010 C011 H011 119.1(18) . . ?
N00F C013 H013 118.5(14) . . ?
C015 C013 N00F 112.71(18) . . ?
C015 C013 H013 128.8(14) . . ?
C00P C014 H014 119.1(17) . . ?
C00Z C014 C00P 119.09(17) . . ?
C00Z C014 H014 121.8(17) . . ?
S003 C015 H015 121.0(16) . . ?
C013 C015 S003 111.29(15) . . ?
C013 C015 H015 127.7(16) . . ?
S004 C016 H016 121.1(17) . . ?
C017 C016 S004 111.11(16) . . ?
C017 C016 H016 127.8(17) . . ?
N00D C017 H017 121.7(14) . . ?
C016 C017 N00D 113.14(18) . . ?
C016 C017 H017 125.1(14) . . ?
N00T O018 O3AA 55.4(5) . . ?
O6 O018 N00T 70.4(11) . . ?
O6 O018 O3AA 118.7(12) . . ?
N00G O1AA O00Q 54.8(3) . . ?
O00W O1AA N00G 59.3(4) . . ?
O00W O1AA O00Q 114.2(6) . . ?
N00G O0AA O00H 57.8(5) . . ?
O00Q O0AA N00G 63.3(5) . . ?
O00Q O0AA O00H 120.8(8) . . ?
N00G O2AA O00W 59.6(5) . . ?
O00H O2AA N00G 62.7(6) . . ?
O00H O2AA O00W 120.6(9) . . ?
N00T O4AA O00Y 57.6(5) . . ?
N00T O4AA H00Y 99(3) . . ?
O00V O4AA N00T 66.9(9) . . ?
O00V O4AA O00Y 119.3(10) . . ?
O00V O4AA H00Y 148(3) . . ?
O00Y O4AA H00Y 41(3) . . ?
N00T O3AA O018 44.1(4) . . ?
O00Y O3AA N00T 64.6(7) . . ?
O00Y O3AA O018 103.4(9) . . ?
N00T O6 O00V 47.7(6) . . ?
O018 O6 N00T 69.4(12) . . ?
O018 O6 O00V 116.7(15) . . ?
O2 O6AA N00A 65.3(12) . . ?
N00A O7AA O1 46.8(3) . . ?
N00A O5AA O2 43.3(6) . . ?
O1 O5AA N00A 77.1(6) . . ?
O1 O5AA O2 117.4(12) . . ?
N00A O1 O7AA 42.9(2) . . ?
O5AA O1 N00A 66.8(7) . . ?
O5AA O1 O7AA 106.8(7) . . ?
N00A O2 O5AA 46.4(5) . . ?
O6AA O2 N00A 86.4(17) . . ?
O6AA O2 O5AA 132.4(17) . . ?
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
S001 N00E C00N S004 15.4(2) . . . . ?
S001 N00E C00N N00D -166.74(13) . . . . ?
S001 C00M C00X C00R -177.48(14) . . . . ?
S001 C00M C010 C011 177.00(18) . . . . ?
S002 N009 C00J S003 12.6(2) . . . . ?
S002 N009 C00J N00F -168.35(13) . . . . ?
S002 C00L C00S C00U -176.68(15) . . . . ?
S002 C00L C00Z C014 177.10(16) . . . . ?
S004 C016 C017 N00D 1.0(3) . . . . ?
O005 S001 N00E C00N -33.90(17) . . . . ?
O005 S001 C00M C00X -17.20(16) . . . . ?
O005 S001 C00M C010 165.32(15) . . . . ?
O006 S002 N009 C00J -170.91(14) . . . . ?
O006 S002 C00L C00S 102.30(15) . . . . ?
O006 S002 C00L C00Z -75.83(16) . . . . ?
O007 S002 N009 C00J -41.43(16) . . . . ?
O007 S002 C00L C00S -23.56(17) . . . . ?
O007 S002 C00L C00Z 158.31(15) . . . . ?
O008 S001 N00E C00N -163.96(14) . . . . ?
O008 S001 C00M C00X 109.16(15) . . . . ?
O008 S001 C00M C010 -68.32(17) . . . . ?
N009 S002 C00L C00S -145.54(14) . . . . ?
N009 S002 C00L C00Z 36.33(16) . . . . ?
N00A O6AA O2 O5AA -6.5(16) . . . . ?
N00A O7AA O1 O5AA -21.4(7) . . . . ?
N00A O5AA O1 O7AA 15.7(4) . . . . ?
N00A O5AA O2 O6AA 9(2) . . . . ?
N00B C00O C00R C00X -179.38(17) . . . . ?
N00B C00O C011 C010 178.9(2) . . . . ?
N00C C00P C00U C00S -179.85(18) . . . . ?
N00C C00P C014 C00Z -179.72(18) . . . . ?
N00E S001 C00M C00X -138.99(14) . . . . ?
N00E S001 C00M C010 43.53(17) . . . . ?
N00F C013 C015 S003 0.7(3) . . . . ?
N00G O00H O0AA O00Q -6.2(7) . . . . ?
N00G O00H O2AA O00W 14.8(7) . . . . ?
N00G O00Q O1AA O00W -1.7(5) . . . . ?
N00G O00Q O0AA O00H 5.9(6) . . . . ?
N00G O00W O1AA O00Q 1.6(4) . . . . ?
N00G O00W O2AA O00H -15.2(7) . . . . ?
O00H N00G O00Q O1AA 178.2(5) . . . . ?
O00H N00G O00Q O0AA -6.5(7) . . . . ?
O00H N00G O00W O1AA -178.5(5) . . . . ?
O00H N00G O00W O2AA 13.7(7) . . . . ?
O00H N00G O0AA O00Q 174.1(7) . . . . ?
O00H N00G O2AA O00W -165.3(8) . . . . ?
C00J S003 C015 C013 -1.09(18) . . . . ?
C00J N00F C013 C015 0.2(3) . . . . ?
C00L S002 N009 C00J 75.90(15) . . . . ?
C00L C00S C00U C00P -0.2(3) . . . . ?
C00L C00Z C014 C00P -0.6(3) . . . . ?
C00M S001 N00E C00N 83.45(15) . . . . ?
C00M C010 C011 C00O 1.1(3) . . . . ?
C00N S004 C016 C017 -1.7(2) . . . . ?
C00N N00D C017 C016 0.5(3) . . . . ?
C00O C00R C00X C00M -0.1(3) . . . . ?
O00Q N00G O00H O0AA 5.6(6) . . . . ?
O00Q N00G O00H O2AA 168.7(8) . . . . ?
O00Q N00G O00W O1AA -1.9(5) . . . . ?
O00Q N00G O00W O2AA -169.6(7) . . . . ?
O00Q N00G O1AA O00W 178.2(5) . . . . ?
O00Q N00G O0AA O00H -174.1(7) . . . . ?
C00R C00O C011 C010 -1.3(3) . . . . ?
C00S C00L C00Z C014 -1.0(3) . . . . ?
N00T O00V O4AA O00Y 24.9(8) . . . . ?
N00T O00V O6 O018 7.8(12) . . . . ?
N00T O00Y O4AA O00V -27.3(8) . . . . ?
N00T O00Y O3AA O018 -21.6(5) . . . . ?
N00T O018 O3AA O00Y 28.5(7) . . . . ?
N00T O018 O6 O00V -6.2(10) . . . . ?
C00U C00P C014 C00Z 1.8(3) . . . . ?
O00V N00T O00Y O4AA 21.6(8) . . . . ?
O00V N00T O00Y O3AA -147.3(9) . . . . ?
O00V N00T O018 O3AA 159.1(7) . . . . ?
O00V N00T O018 O6 9.2(15) . . . . ?
O00V N00T O4AA O00Y -154.2(9) . . . . ?
O00V N00T O3AA O00Y 63.0(15) . . . . ?
O00V N00T O3AA O018 -148.0(10) . . . . ?
O00V N00T O6 O018 -172.6(12) . . . . ?
O00W N00G O00H O0AA -177.7(6) . . . . ?
O00W N00G O00H O2AA -14.7(8) . . . . ?
O00W N00G O00Q O1AA 1.8(5) . . . . ?
O00W N00G O00Q O0AA 177.1(7) . . . . ?
O00W N00G O1AA O00Q -178.2(5) . . . . ?
O00W N00G O2AA O00H 165.3(8) . . . . ?
C00X C00M C010 C011 -0.5(3) . . . . ?
O00Y N00T O00V O4AA -27.7(9) . . . . ?
O00Y N00T O00V O6 176.2(9) . . . . ?
O00Y N00T O018 O3AA -23.0(7) . . . . ?
O00Y N00T O018 O6 -173.0(14) . . . . ?
O00Y N00T O4AA O00V 154.2(9) . . . . ?
O00Y N00T O3AA O018 149.1(8) . . . . ?
O00Y N00T O6 O00V -172(2) . . . . ?
O00Y N00T O6 O018 16(3) . . . . ?
C00Z C00L C00S C00U 1.4(3) . . . . ?
C010 C00M C00X C00R -0.1(3) . . . . ?
C011 C00O C00R C00X 0.8(3) . . . . ?
C013 N00F C00J S003 -1.0(2) . . . . ?
C013 N00F C00J N009 179.78(17) . . . . ?
C014 C00P C00U C00S -1.4(3) . . . . ?
C015 S003 C00J N009 -179.73(18) . . . . ?
C015 S003 C00J N00F 1.16(14) . . . . ?
C016 S004 C00N N00D 1.84(15) . . . . ?
C016 S004 C00N N00E 179.91(19) . . . . ?
C017 N00D C00N S004 -1.7(2) . . . . ?
C017 N00D C00N N00E 180.00(17) . . . . ?
O018 N00T O00V O4AA 150.1(10) . . . . ?
O018 N00T O00V O6 -6.0(10) . . . . ?
O018 N00T O00Y O4AA -156.4(9) . . . . ?
O018 N00T O00Y O3AA 34.7(10) . . . . ?
O018 N00T O4AA O00V -88(2) . . . . ?
O018 N00T O4AA O00Y 117.4(18) . . . . ?
O018 N00T O3AA O00Y -149.1(8) . . . . ?
O018 N00T O6 O00V 172.6(12) . . . . ?
O1AA N00G O00Q O0AA 175.3(8) . . . . ?
O1AA N00G O00W O2AA -167.8(9) . . . . ?
O1AA N00G O0AA O00H -178.8(5) . . . . ?
O1AA N00G O0AA O00Q -4.7(8) . . . . ?
O1AA N00G O2AA O00H 177.1(5) . . . . ?
O1AA N00G O2AA O00W 11.8(8) . . . . ?
O1AA O00Q O0AA N00G 5.0(9) . . . . ?
O1AA O00Q O0AA O00H 10.8(15) . . . . ?
O1AA O00W O2AA N00G -12.6(9) . . . . ?
O1AA O00W O2AA O00H -27.8(15) . . . . ?
O0AA N00G O00H O2AA 163.1(10) . . . . ?
O0AA N00G O00Q O1AA -175.3(8) . . . . ?
O0AA N00G O1AA O00Q 4.3(8) . . . . ?
O0AA N00G O1AA O00W -177.5(7) . . . . ?
O0AA N00G O2AA O00H -18.5(11) . . . . ?
O0AA N00G O2AA O00W 176.3(7) . . . . ?
O0AA O00H O2AA N00G 15.0(8) . . . . ?
O0AA O00H O2AA O00W 29.7(14) . . . . ?
O0AA O00Q O1AA N00G -5.0(9) . . . . ?
O0AA O00Q O1AA O00W -6.7(12) . . . . ?
O2AA N00G O00H O0AA -163.1(10) . . . . ?
O2AA N00G O00W O1AA 167.8(9) . . . . ?
O2AA N00G O1AA O00Q 169.4(7) . . . . ?
O2AA N00G O1AA O00W -12.4(9) . . . . ?
O2AA N00G O0AA O00H 16.5(9) . . . . ?
O2AA N00G O0AA O00Q -169.4(8) . . . . ?
O2AA O00H O0AA N00G -16.1(9) . . . . ?
O2AA O00H O0AA O00Q -22.3(14) . . . . ?
O2AA O00W O1AA N00G 12.0(8) . . . . ?
O2AA O00W O1AA O00Q 13.6(11) . . . . ?
O4AA N00T O00V O6 -156.1(13) . . . . ?
O4AA N00T O00Y O3AA -168.9(12) . . . . ?
O4AA N00T O018 O3AA -131(2) . . . . ?
O4AA N00T O018 O6 79(3) . . . . ?
O4AA N00T O3AA O00Y 11.6(13) . . . . ?
O4AA N00T O3AA O018 160.7(9) . . . . ?
O4AA N00T O6 O00V 23.8(13) . . . . ?
O4AA N00T O6 O018 -148.8(12) . . . . ?
O4AA O00V O6 N00T -22.4(11) . . . . ?
O4AA O00V O6 O018 -15(2) . . . . ?
O4AA O00Y O3AA N00T -10.0(11) . . . . ?
O4AA O00Y O3AA O018 -31.5(14) . . . . ?
O3AA N00T O00V O4AA -70.3(15) . . . . ?
O3AA N00T O00V O6 133.6(16) . . . . ?
O3AA N00T O00Y O4AA 168.9(12) . . . . ?
O3AA N00T O018 O6 -149.9(16) . . . . ?
O3AA N00T O4AA O00V 146.0(8) . . . . ?
O3AA N00T O4AA O00Y -8.2(9) . . . . ?
O3AA N00T O6 O00V -154.3(8) . . . . ?
O3AA N00T O6 O018 33.1(17) . . . . ?
O3AA O00Y O4AA N00T 12.4(14) . . . . ?
O3AA O00Y O4AA O00V -14.9(19) . . . . ?
O3AA O018 O6 N00T -28.0(14) . . . . ?
O3AA O018 O6 O00V -34(2) . . . . ?
O6 N00T O00V O4AA 156.1(13) . . . . ?
O6 N00T O00Y O4AA -168(2) . . . . ?
O6 N00T O00Y O3AA 23(3) . . . . ?
O6 N00T O018 O3AA 149.9(16) . . . . ?
O6 N00T O4AA O00V -32.1(17) . . . . ?
O6 N00T O4AA O00Y 173.7(13) . . . . ?
O6 N00T O3AA O00Y -170.0(12) . . . . ?
O6 N00T O3AA O018 -20.9(12) . . . . ?
O6 O00V O4AA N00T 17.7(9) . . . . ?
O6 O00V O4AA O00Y 42.6(14) . . . . ?
O6 O018 O3AA N00T 32.6(17) . . . . ?
O6 O018 O3AA O00Y 61(2) . . . . ?
O6AA N00A O7AA O1 -166.7(4) . . . . ?
O6AA N00A O5AA O1 155.1(6) . . . . ?
O6AA N00A O5AA O2 -3.6(10) . . . . ?
O6AA N00A O1 O7AA 156.8(8) . . . . ?
O6AA N00A O1 O5AA -45.5(9) . . . . ?
O6AA N00A O2 O5AA 173.3(16) . . . . ?
O7AA N00A O6AA O2 -170.3(16) . . . . ?
O7AA N00A O5AA O1 -27.1(8) . . . . ?
O7AA N00A O5AA O2 174.2(8) . . . . ?
O7AA N00A O1 O5AA 157.6(7) . . . . ?
O7AA N00A O2 O6AA 15(3) . . . . ?
O7AA N00A O2 O5AA -171.3(12) . . . . ?
O5AA N00A O6AA O2 7.6(18) . . . . ?
O5AA N00A O7AA O1 15.6(4) . . . . ?
O5AA N00A O1 O7AA -157.6(7) . . . . ?
O5AA N00A O2 O6AA -173.3(16) . . . . ?
O1 N00A O6AA O2 36(2) . . . . ?
O1 N00A O5AA O2 -158.7(11) . . . . ?
O1 N00A O2 O6AA -158.4(11) . . . . ?
O1 N00A O2 O5AA 14.9(8) . . . . ?
O1 O5AA O2 N00A -23.5(10) . . . . ?
O1 O5AA O2 O6AA -14(3) . . . . ?
O2 N00A O7AA O1 -174.9(15) . . . . ?
O2 N00A O5AA O1 158.7(11) . . . . ?
O2 N00A O1 O7AA 176.5(11) . . . . ?
O2 N00A O1 O5AA -25.8(14) . . . . ?
O2 O5AA O1 N00A 16.3(6) . . . . ?
O2 O5AA O1 O7AA 32.0(9) . . . . ?
O4 N00A O6AA O2 -168.5(18) . . . . ?
O4 N00A O7AA O1 -171(3) . . . . ?
O4 N00A O5AA O1 -31.7(17) . . . . ?
O4 N00A O5AA O2 169.6(16) . . . . ?
O4 N00A O1 O7AA 3.5(11) . . . . ?
O4 N00A O1 O5AA 161.1(11) . . . . ?
O4 N00A O2 O6AA 14(2) . . . . ?
O4 N00A O2 O5AA -172.9(11) . . . . ?
_shelx_res_file
;
ee_sulfa_no3_0m.res created by SHELXL-2014/7
TITL ee_sulfa_no3_0m_a.res in P2(1)/n
REM Old TITL EE_sulfa_NO3_0m in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.153, Rweak 0.005, Alpha 0.028, Orientation as input
REM Formula found by SHELXT: C23 N7 O10 S4
CELL 0.71073 14.9484 8.2585 22.9621 90 100.818 90
ZERR 4 0.0004 0.0002 0.0006 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O S
UNIT 72 84 36 52 16
L.S. 4
PLAN 20
TEMP -99.95
BOND $H
LIST 6
fmap 2
MORE -1
ACTA 52
CONF
OMIT -1 0 1
OMIT 0 3 7
OMIT -7 1 5
OMIT 6 2 1
OMIT 4 1 3
REM
REM
REM
WGHT 0.045000 1.748300
FVAR 0.24087 0.82392 0.81421 0.68915
S001 5 0.131477 0.308956 0.496765 11.00000 0.02656 0.01648 =
0.01694 0.00035 0.00430 -0.00073
S002 5 0.327699 0.678233 0.685348 11.00000 0.01922 0.01781 =
0.02265 0.00088 0.00135 -0.00231
S003 5 0.421121 0.738050 0.823724 11.00000 0.02615 0.03540 =
0.02480 -0.00675 0.00841 0.00125
S004 5 -0.029204 0.287597 0.377970 11.00000 0.02171 0.05357 =
0.02744 0.00390 0.00428 -0.00881
O005 4 0.038471 0.290444 0.504044 11.00000 0.03183 0.02607 =
0.02889 0.00494 0.01555 0.00400
O006 4 0.295051 0.592013 0.630603 11.00000 0.03293 0.02138 =
0.03053 -0.00293 -0.00734 -0.00495
O007 4 0.265185 0.696539 0.725552 11.00000 0.02294 0.03023 =
0.03865 0.00829 0.01156 -0.00102
O008 4 0.192454 0.396070 0.542310 11.00000 0.04849 0.02099 =
0.02175 -0.00313 -0.00073 -0.00484
N009 3 0.420784 0.591297 0.714017 11.00000 0.02344 0.01996 =
0.02081 -0.00037 0.00248 0.00292
N00A 3 0.530377 1.661397 0.533362 11.00000 0.02637 0.01852 =
0.03091 -0.00307 0.00856 -0.00416
N00B 3 0.294062 -0.350963 0.494786 11.00000 0.02276 0.02142 =
0.02991 0.00048 0.00566 0.00321
N00C 3 0.417865 1.339164 0.609919 11.00000 0.04003 0.01933 =
0.02483 0.00031 0.01244 -0.00511
N00D 3 0.096833 0.410840 0.334340 11.00000 0.02267 0.03186 =
0.02223 0.00577 0.00648 0.00136
N00E 3 0.141847 0.393241 0.436010 11.00000 0.02316 0.02276 =
0.02012 0.00383 0.00418 -0.00245
N00F 3 0.546357 0.580044 0.790182 11.00000 0.02498 0.03062 =
0.02072 -0.00181 0.00243 0.00497
N00G 3 0.341499 -0.409521 0.340197 11.00000 0.02851 0.03498 =
0.03098 -0.00041 0.00856 0.00067
PART 1
O00H 4 0.408550 -0.409668 0.314468 21.00000 0.02766 0.04473 =
0.03230 -0.00649 0.01227 -0.00705
PART 0
C00J 1 0.461174 0.629379 0.768947 11.00000 0.02195 0.01711 =
0.02048 0.00234 0.00619 -0.00116
C00L 1 0.356355 0.875977 0.665460 11.00000 0.02007 0.01779 =
0.01529 -0.00065 0.00055 -0.00142
C00M 1 0.177437 0.111221 0.494706 11.00000 0.02061 0.01679 =
0.01669 -0.00073 0.00035 -0.00177
C00N 1 0.080079 0.367764 0.387500 11.00000 0.01986 0.01858 =
0.02320 0.00364 0.00618 0.00362
C00O 1 0.253340 -0.190293 0.495236 11.00000 0.01970 0.01821 =
0.02058 -0.00159 0.00037 -0.00008
C00P 1 0.395723 1.178473 0.629358 11.00000 0.02873 0.01821 =
0.01585 -0.00083 0.00509 -0.00399
PART 1
O00Q 4 0.335007 -0.312034 0.378609 21.00000 0.06851 0.03869 =
0.03208 -0.00290 0.02349 0.00633
PART 0
C00R 1 0.173222 -0.172334 0.515343 11.00000 0.02546 0.02081 =
0.02750 0.00607 0.00946 -0.00025
C00S 1 0.297844 1.002050 0.669762 11.00000 0.02222 0.02239 =
0.03566 0.00274 0.01220 0.00190
N00T 3 0.293507 -0.899916 0.301427 11.00000 0.03895 0.04114 =
0.05132 0.00661 0.00301 -0.00104
C00U 1 0.317649 1.155692 0.651361 11.00000 0.02401 0.02109 =
0.03293 0.00289 0.00763 0.00362
PART 1
O00V 4 0.218938 -0.862520 0.312859 31.00000 0.03843 0.04784 =
0.07666 -0.00639 0.02733 -0.01146
O00W 4 0.279051 -0.509994 0.322367 21.00000 0.02514 0.05383 =
0.08465 -0.01397 0.01430 -0.01438
PART 0
C00X 1 0.134449 -0.019225 0.515085 11.00000 0.02332 0.02290 =
0.02887 0.00435 0.01076 0.00113
PART 1
O00Y 4 0.348742 -0.779107 0.293695 31.00000 0.03536 0.04516 =
0.09937 -0.00526 0.02867 -0.00874
PART 0
C00Z 1 0.436496 0.899897 0.644111 11.00000 0.02888 0.02244 =
0.04174 -0.00102 0.01790 0.00174
C010 1 0.258295 0.091788 0.474666 11.00000 0.02922 0.02156 =
0.05329 0.00376 0.01945 -0.00549
C011 1 0.297159 -0.060180 0.475374 11.00000 0.02645 0.02627 =
0.06137 0.00352 0.02428 -0.00152
C013 1 0.582226 0.626482 0.847671 11.00000 0.02855 0.03914 =
0.02452 0.00059 -0.00274 0.00252
C014 1 0.456535 1.053088 0.626130 11.00000 0.03321 0.02647 =
0.04079 -0.00077 0.02316 -0.00310
C015 1 0.524015 0.713596 0.872180 11.00000 0.03671 0.04002 =
0.01909 -0.00425 0.00262 -0.00050
C016 1 -0.043964 0.311639 0.301662 11.00000 0.02777 0.05722 =
0.02494 0.00223 -0.00418 -0.00028
C017 1 0.028129 0.379184 0.286491 11.00000 0.03627 0.04163 =
0.02012 0.00535 0.00150 0.00633
PART 1
O018 4 0.321669 -1.033466 0.298241 31.00000 0.05399 0.04198 =
0.11872 0.01495 0.01562 0.01212
PART 0
H00A 2 0.355112 -0.346203 0.514614 11.00000 0.04391
H00Z 2 0.473406 0.810787 0.640948 11.00000 0.04092
H00H 2 0.572300 0.524997 0.767697 11.00000 0.04037
H00B 2 0.293205 -0.377509 0.458291 11.00000 0.03534
H00U 2 0.275442 1.246077 0.651405 11.00000 0.03780
H00X 2 0.078866 -0.003023 0.526335 11.00000 0.03476
H011 2 0.351940 -0.070889 0.464620 11.00000 0.05604
H013 2 0.643538 0.595880 0.864278 11.00000 0.04041
H010 2 0.284687 0.183346 0.460075 11.00000 0.04333
H015 2 0.532902 0.755507 0.908242 11.00000 0.03618
H00R 2 0.149104 -0.261439 0.530841 11.00000 0.03710
H014 2 0.510005 1.074802 0.612096 11.00000 0.05059
H016 2 -0.096797 0.283701 0.277712 11.00000 0.05029
PART -1
O1AA 4 0.267916 -0.417687 0.362808 -21.00000 0.02462 0.06191 =
0.02411 -0.00962 0.00822 -0.00552
O0AA 4 0.398908 -0.313075 0.361572 -21.00000 0.02294 0.04950 =
0.09872 -0.00623 0.00658 -0.01043
O2AA 4 0.358102 -0.520015 0.307452 -21.00000 0.08506 0.06616 =
0.05960 -0.03406 0.04193 -0.00675
O4AA 4 0.269990 -0.782257 0.325580 -31.00000 0.09228 0.05621 =
0.09837 -0.00907 0.06220 0.01546
O3AA 4 0.360176 -0.869381 0.267153 -31.00000 0.07454 0.06666 =
0.09953 -0.01373 0.05259 -0.00124
O6 4 0.267826 -1.037086 0.300902 -31.00000 0.09274 0.05064 =
0.10279 0.02197 0.03276 -0.00375
PART 0
PART 1
O6AA 4 0.469018 1.621772 0.562561 41.00000 0.02390 0.03307 =
0.03157 0.00724 0.00968 -0.00287
O7AA 4 0.508620 1.747290 0.490067 41.00000 0.04421 0.04964 =
0.02917 0.01466 0.01656 0.00951
PART 0
H00E 2 0.378378 1.411804 0.615372 11.00000 0.04312
H00C 2 0.261319 -0.423499 0.508562 11.00000 0.04616
H017 2 0.035433 0.400820 0.246240 11.00000 0.04110
H00S 2 0.244815 0.980565 0.685571 11.00000 0.03625
H00F 2 0.470482 1.371620 0.632328 11.00000 0.04821
H00G 2 0.426925 1.335581 0.570706 11.00000 0.05599
H00D 2 0.146622 0.448410 0.332594 11.00000 0.03287
H00Y 2 0.321678 -0.687336 0.311759 11.00000 0.12640
PART 1
O5AA 4 0.608628 1.615038 0.551342 41.00000 0.02396 0.03763 =
0.08024 0.02076 0.00980 0.00288
PART 0
PART -1
O1 4 0.607235 1.628124 0.517243 -41.00000 0.03238 0.03006 =
0.03329 0.00216 0.00448 0.00935
O2 4 0.507581 1.604240 0.574436 -41.00000 0.13858 0.03957 =
0.06440 0.01363 0.07458 0.00802
O4 4 0.479814 1.748969 0.495993 -41.00000 0.04559 0.09103 =
0.06012 0.02218 0.01491 0.03834
HKLF 4
REM ee_sulfa_no3_0m_a.res in P2(1)/n
REM R1 = 0.0390 for 5971 Fo > 4sig(Fo) and 0.0638 for all 8100 data
REM 565 parameters refined using 0 restraints
END
WGHT 0.0450 1.7417
REM Highest difference peak 0.415, deepest hole -0.392, 1-sigma level 0.065
Q1 1 0.3989 0.8945 0.6167 11.00000 0.05 0.41
Q2 1 0.5984 1.6945 0.5745 11.00000 0.05 0.38
Q3 1 0.3329 0.7846 0.6759 11.00000 0.05 0.38
Q4 1 0.3004 0.6885 0.7136 11.00000 0.05 0.38
Q5 1 0.0366 0.3209 0.3892 11.00000 0.05 0.38
Q6 1 0.1535 0.2062 0.4979 11.00000 0.05 0.37
Q7 1 0.5582 0.7050 0.8529 11.00000 0.05 0.37
Q8 1 0.4370 0.6658 0.7974 11.00000 0.05 0.36
Q9 1 0.4126 1.0822 0.6038 11.00000 0.05 0.35
Q10 1 0.2716 -0.1241 0.4860 11.00000 0.05 0.34
Q11 1 0.4192 1.0222 0.6009 11.00000 0.05 0.34
Q12 1 0.2067 -0.1784 0.4968 11.00000 0.05 0.33
Q13 1 0.1338 0.3678 0.4629 11.00000 0.05 0.32
Q14 1 0.0769 0.3324 0.5041 11.00000 0.05 0.32
Q15 1 0.2218 0.1235 0.4961 11.00000 0.05 0.31
Q16 1 0.4797 0.7145 0.8504 11.00000 0.05 0.31
Q17 1 0.2974 -0.5541 0.3568 11.00000 0.05 0.31
Q18 1 0.1426 -0.1014 0.5007 11.00000 0.05 0.30
Q19 1 0.3648 1.1589 0.6457 11.00000 0.05 0.30
Q20 1 0.3021 -0.9991 0.2678 11.00000 0.05 0.30
;
_shelx_res_checksum 55556
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_EE_sulf_SO4_2_0m
_database_code_depnum_ccdc_archive 'CCDC 1499240'
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic 'Sulfathiazolium Sulfate Hydrate'
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '2(C9 H10 N3 O2 S2), O4 S, O H2'
_chemical_formula_sum 'C18 H22 N6 O9 S5'
_chemical_formula_weight 626.71
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'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 17.4737(9)
_cell_length_b 11.6240(5)
_cell_length_c 11.7557(5)
_cell_angle_alpha 90
_cell_angle_beta 90.072(2)
_cell_angle_gamma 90
_cell_volume 2387.75(19)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 6312
_cell_measurement_theta_min 2.33
_cell_measurement_theta_max 30.23
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
_exptl_crystal_density_diffrn 1.743
_exptl_crystal_F_000 1296
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.468
_exptl_crystal_size_mid 0.290
_exptl_crystal_size_min 0.174
_exptl_absorpt_coefficient_mu 0.551
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6348
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_process_details
'Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany.'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 29335
_diffrn_reflns_av_unetI/netI 0.0538
_diffrn_reflns_av_R_equivalents 0.0525
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.104
_diffrn_reflns_theta_max 30.524
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 3526
_reflns_number_gt 2433
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+4.6686P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 3526
_refine_ls_number_parameters 238
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0922
_refine_ls_R_factor_gt 0.0504
_refine_ls_wR_factor_ref 0.1134
_refine_ls_wR_factor_gt 0.0961
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_restrained_S_all 1.055
_refine_ls_shift/su_max 0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.22128(16) 0.5979(3) 0.6956(2) 0.0254(5) Uani 0.5 1 d . . P A 1
N1 N 0.3141(4) 0.7566(7) 0.7366(9) 0.0200(15) Uani 0.5 1 d . . P A 1
H1N H 0.3513 0.8072 0.7296 0.024 Uiso 0.5 1 calc R U P A 1
C1 C 0.2703(5) 0.7483(8) 0.8337(7) 0.027(2) Uani 0.5 1 d . . P A 1
H1A H 0.2770 0.7959 0.8986 0.033 Uiso 0.5 1 calc R U P A 1
C2 C 0.2179(4) 0.6668(7) 0.8262(7) 0.0272(17) Uani 0.5 1 d . . P A 1
H2 H 0.1828 0.6482 0.8850 0.033 Uiso 0.5 1 calc R U P A 1
C3 C 0.2962(4) 0.6825(5) 0.6540(5) 0.0160(15) Uiso 0.5 1 d . . P A 1
S1B S 0.24036(17) 0.6151(2) 0.7220(2) 0.0251(5) Uani 0.5 1 d . . P A 2
N1B N 0.3346(4) 0.7804(7) 0.7252(8) 0.0140(13) Uani 0.5 1 d . . P A 2
H1M H 0.3699 0.8308 0.7063 0.017 Uiso 0.5 1 calc R U P A 2
C1B C 0.2984(4) 0.7824(7) 0.8298(8) 0.0239(17) Uani 0.5 1 d . . P A 2
H1B H 0.3089 0.8380 0.8870 0.029 Uiso 0.5 1 calc R U P A 2
C2B C 0.2480(5) 0.6994(7) 0.8419(7) 0.026(2) Uani 0.5 1 d . . P A 2
H2B H 0.2191 0.6873 0.9092 0.031 Uiso 0.5 1 calc R U P A 2
C3B C 0.3119(3) 0.6962(5) 0.6547(5) 0.0136(14) Uiso 0.5 1 d . . P A 2
S2 S 0.31939(4) 0.58805(5) 0.46296(5) 0.02336(15) Uani 1 1 d . . . . .
O1 O 0.33987(13) 0.63485(16) 0.35427(14) 0.0424(5) Uani 1 1 d . . . . .
O2 O 0.24306(11) 0.54455(16) 0.47850(18) 0.0401(5) Uani 1 1 d . . . . .
N2 N 0.33999(11) 0.68455(15) 0.55470(15) 0.0202(4) Uani 1 1 d . . . . .
N3 N 0.52894(13) 0.18685(16) 0.53323(18) 0.0222(4) Uani 1 1 d . . . . .
H3N H 0.580(2) 0.212(3) 0.520(3) 0.066(11) Uiso 1 1 d . . . . .
H3M H 0.5253(17) 0.153(3) 0.609(3) 0.043(8) Uiso 1 1 d . . . . .
H3L H 0.5180(17) 0.133(3) 0.476(3) 0.043(8) Uiso 1 1 d . . . . .
C4 C 0.38347(13) 0.47166(18) 0.48670(18) 0.0188(4) Uani 1 1 d . . . . .
C5 C 0.43010(14) 0.43520(18) 0.39810(18) 0.0209(5) Uani 1 1 d . . . . .
H5 H 0.4296 0.4747 0.3274 0.025 Uiso 1 1 calc R U . . .
C6 C 0.47727(13) 0.34098(18) 0.41361(18) 0.0204(5) Uani 1 1 d . . . . .
H6 H 0.5087 0.3142 0.3533 0.024 Uiso 1 1 calc R U . . .
C7 C 0.47818(13) 0.28594(17) 0.51844(18) 0.0179(4) Uani 1 1 d . . . . .
C8 C 0.43259(14) 0.32214(18) 0.60731(18) 0.0213(5) Uani 1 1 d . . . . .
H8 H 0.4343 0.2839 0.6787 0.026 Uiso 1 1 calc R U . . .
C9 C 0.38418(14) 0.41542(18) 0.59056(18) 0.0210(5) Uani 1 1 d . . . . .
H9 H 0.3516 0.4406 0.6502 0.025 Uiso 1 1 calc R U . . .
S3 S 0.5000 0.97214(6) 0.7500 0.02200(19) Uani 1 2 d S T P . .
O3 O 0.5000 1.09828(18) 0.7500 0.0291(6) Uani 1 2 d S T P B .
O4 O 0.5413(2) 0.9463(3) 0.6358(3) 0.0263(7) Uani 0.5 1 d . . P B -1
O5 O 0.5499(2) 0.9301(3) 0.8392(3) 0.0370(9) Uani 0.5 1 d . . P B -1
O6 O 0.4276(2) 0.9190(4) 0.7478(4) 0.0485(11) Uani 0.5 1 d . . P B -1
O7 O 0.3932(3) 0.9486(5) 0.9811(5) 0.0741(15) Uani 0.5 1 d . . P C -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0277(13) 0.0176(10) 0.0309(14) 0.0024(8) 0.0087(8) -0.0005(8)
N1 0.014(4) 0.019(4) 0.027(3) 0.003(3) 0.001(3) -0.005(2)
C1 0.028(6) 0.036(7) 0.017(3) -0.001(5) 0.001(4) 0.008(4)
C2 0.026(4) 0.031(4) 0.025(3) 0.011(3) 0.008(3) 0.011(3)
S1B 0.0311(14) 0.0165(9) 0.0278(13) 0.0013(7) 0.0047(8) 0.0006(8)
N1B 0.015(4) 0.012(3) 0.015(3) -0.004(2) 0.000(2) -0.003(2)
C1B 0.033(5) 0.024(4) 0.014(3) -0.003(3) 0.003(3) 0.011(3)
C2B 0.030(6) 0.024(5) 0.023(3) 0.003(4) 0.011(4) 0.009(4)
S2 0.0361(3) 0.0161(3) 0.0179(3) -0.0032(2) -0.0067(2) 0.0074(2)
O1 0.0770(15) 0.0361(10) 0.0141(9) 0.0028(7) -0.0016(8) 0.0306(10)
O2 0.0307(11) 0.0255(9) 0.0639(13) -0.0156(9) -0.0156(9) 0.0036(8)
N2 0.0279(11) 0.0131(8) 0.0197(9) -0.0023(7) 0.0006(8) 0.0006(8)
N3 0.0314(12) 0.0119(9) 0.0232(11) 0.0029(7) 0.0024(8) 0.0037(8)
C4 0.0278(12) 0.0115(9) 0.0170(11) -0.0022(8) -0.0052(8) 0.0003(9)
C5 0.0315(13) 0.0173(10) 0.0138(10) 0.0012(8) -0.0032(9) -0.0012(9)
C6 0.0292(13) 0.0172(10) 0.0147(10) -0.0021(8) -0.0001(8) 0.0018(9)
C7 0.0252(12) 0.0081(9) 0.0204(11) -0.0002(8) -0.0024(8) 0.0000(8)
C8 0.0323(13) 0.0150(10) 0.0165(11) 0.0032(8) 0.0005(9) -0.0006(9)
C9 0.0295(12) 0.0166(10) 0.0170(11) -0.0006(8) 0.0019(9) 0.0017(9)
S3 0.0330(5) 0.0099(3) 0.0231(4) 0.000 -0.0033(3) 0.000
O3 0.0568(17) 0.0118(10) 0.0186(12) 0.000 -0.0027(10) 0.000
O4 0.041(2) 0.0186(16) 0.0196(17) -0.0037(12) 0.0035(14) 0.0047(14)
O5 0.052(3) 0.037(2) 0.022(2) 0.0108(15) 0.0016(17) 0.0193(18)
O6 0.042(2) 0.051(3) 0.053(3) -0.013(2) 0.007(2) -0.028(2)
O7 0.062(4) 0.080(4) 0.080(4) 0.005(3) 0.001(3) 0.016(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
S1 C3 1.709(7) . ?
S1 C2 1.733(8) . ?
N1 C3 1.335(12) . ?
N1 C1 1.378(11) . ?
N1 H1N 0.8800 . ?
C1 C2 1.320(10) . ?
C1 H1A 0.9500 . ?
C2 H2 0.9500 . ?
C3 N2 1.397(6) . ?
S1B C2B 1.721(9) . ?
S1B C3B 1.755(7) . ?
N1B C3B 1.342(10) . ?
N1B C1B 1.383(12) . ?
N1B H1M 0.8800 . ?
C1B C2B 1.314(10) . ?
C1B H1B 0.9500 . ?
C2B H2B 0.9500 . ?
C3B N2 1.282(6) . ?
S2 O1 1.4345(19) . ?
S2 O2 1.438(2) . ?
S2 N2 1.5968(18) . ?
S2 C4 1.778(2) . ?
N3 C7 1.464(3) . ?
N3 H3N 0.96(4) . ?
N3 H3M 0.98(3) . ?
N3 H3L 0.94(3) . ?
C4 C9 1.385(3) . ?
C4 C5 1.389(3) . ?
C5 C6 1.383(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.380(3) . ?
C8 C9 1.389(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
S3 O6 1.408(4) . ?
S3 O5 1.448(3) 2_656 ?
S3 O5 1.448(3) . ?
S3 O3 1.466(2) . ?
S3 O4 1.555(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 S1 C2 90.8(3) . . ?
C3 N1 C1 115.3(6) . . ?
C3 N1 H1N 122.4 . . ?
C1 N1 H1N 122.4 . . ?
C2 C1 N1 112.4(8) . . ?
C2 C1 H1A 123.8 . . ?
N1 C1 H1A 123.8 . . ?
C1 C2 S1 111.5(7) . . ?
C1 C2 H2 124.2 . . ?
S1 C2 H2 124.2 . . ?
N1 C3 N2 117.9(5) . . ?
N1 C3 S1 110.0(5) . . ?
N2 C3 S1 132.0(4) . . ?
C2B S1B C3B 90.5(4) . . ?
C3B N1B C1B 115.2(6) . . ?
C3B N1B H1M 122.4 . . ?
C1B N1B H1M 122.4 . . ?
C2B C1B N1B 113.0(9) . . ?
C2B C1B H1B 123.5 . . ?
N1B C1B H1B 123.5 . . ?
C1B C2B S1B 112.4(8) . . ?
C1B C2B H2B 123.8 . . ?
S1B C2B H2B 123.8 . . ?
N2 C3B N1B 122.0(5) . . ?
N2 C3B S1B 129.1(4) . . ?
N1B C3B S1B 108.9(5) . . ?
O1 S2 O2 118.61(13) . . ?
O1 S2 N2 106.20(11) . . ?
O2 S2 N2 111.68(11) . . ?
O1 S2 C4 105.70(11) . . ?
O2 S2 C4 107.24(11) . . ?
N2 S2 C4 106.69(10) . . ?
C3B N2 S2 127.4(3) . . ?
C3 N2 S2 115.4(3) . . ?
C7 N3 H3N 108(2) . . ?
C7 N3 H3M 112.7(18) . . ?
H3N N3 H3M 110(3) . . ?
C7 N3 H3L 108.4(18) . . ?
H3N N3 H3L 106(3) . . ?
H3M N3 H3L 112(2) . . ?
C9 C4 C5 120.8(2) . . ?
C9 C4 S2 120.16(17) . . ?
C5 C4 S2 118.96(16) . . ?
C6 C5 C4 119.5(2) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C8 C7 C6 121.7(2) . . ?
C8 C7 N3 120.01(19) . . ?
C6 C7 N3 118.3(2) . . ?
C7 C8 C9 118.9(2) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C4 C9 C8 119.9(2) . . ?
C4 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
O6 S3 O5 45.4(2) . 2_656 ?
O6 S3 O5 113.9(2) . . ?
O5 S3 O5 140.5(3) 2_656 . ?
O6 S3 O3 116.0(2) . . ?
O5 S3 O3 109.73(16) 2_656 . ?
O5 S3 O3 109.73(16) . . ?
O6 S3 O4 108.5(2) . . ?
O5 S3 O4 65.8(2) 2_656 . ?
O5 S3 O4 106.3(2) . . ?
O3 S3 O4 101.13(12) . . ?
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
C3 N1 C1 C2 0.1(12) . . . . ?
N1 C1 C2 S1 -0.5(10) . . . . ?
C3 S1 C2 C1 0.6(7) . . . . ?
C1 N1 C3 N2 -178.2(7) . . . . ?
C1 N1 C3 S1 0.4(10) . . . . ?
C2 S1 C3 N1 -0.6(6) . . . . ?
C2 S1 C3 N2 177.8(5) . . . . ?
C3B N1B C1B C2B 0.6(13) . . . . ?
N1B C1B C2B S1B -1.6(12) . . . . ?
C3B S1B C2B C1B 1.6(8) . . . . ?
C1B N1B C3B N2 179.4(6) . . . . ?
C1B N1B C3B S1B 0.6(9) . . . . ?
C2B S1B C3B N2 -179.9(6) . . . . ?
C2B S1B C3B N1B -1.2(6) . . . . ?
N1B C3B N2 S2 179.1(5) . . . . ?
S1B C3B N2 S2 -2.4(7) . . . . ?
N1 C3 N2 S2 175.9(6) . . . . ?
S1 C3 N2 S2 -2.4(6) . . . . ?
O1 S2 N2 C3B 157.3(4) . . . . ?
O2 S2 N2 C3B 26.6(4) . . . . ?
C4 S2 N2 C3B -90.3(4) . . . . ?
O1 S2 N2 C3 152.4(3) . . . . ?
O2 S2 N2 C3 21.7(3) . . . . ?
C4 S2 N2 C3 -95.2(3) . . . . ?
O1 S2 C4 C9 173.09(19) . . . . ?
O2 S2 C4 C9 -59.5(2) . . . . ?
N2 S2 C4 C9 60.3(2) . . . . ?
O1 S2 C4 C5 -9.7(2) . . . . ?
O2 S2 C4 C5 117.76(19) . . . . ?
N2 S2 C4 C5 -122.44(18) . . . . ?
C9 C4 C5 C6 0.6(3) . . . . ?
S2 C4 C5 C6 -176.63(17) . . . . ?
C4 C5 C6 C7 -1.3(3) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
C5 C6 C7 N3 -179.6(2) . . . . ?
C6 C7 C8 C9 0.6(3) . . . . ?
N3 C7 C8 C9 -179.1(2) . . . . ?
C5 C4 C9 C8 0.7(3) . . . . ?
S2 C4 C9 C8 177.88(17) . . . . ?
C7 C8 C9 C4 -1.3(3) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1B H1M S3 0.88 2.85 3.661(6) 153.8 .
N3 H3N S2 0.96(4) 2.92(4) 3.724(2) 142(3) 5_666
N3 H3N N2 0.96(4) 2.04(4) 2.925(3) 153(3) 5_666
N3 H3M S3 0.98(3) 2.71(3) 3.603(2) 152(2) 1_545
N3 H3M O3 0.98(3) 1.83(3) 2.795(2) 169(3) 1_545
N3 H3M O4 0.98(3) 2.44(3) 3.052(4) 121(2) 1_545
N3 H3L S3 0.94(3) 2.94(3) 3.841(2) 161(2) 5_666
N3 H3L O4 0.94(3) 1.91(3) 2.801(4) 158(3) 5_666
N3 H3L O5 0.94(3) 1.86(3) 2.681(4) 146(3) 6_565
N3 H3L O7 0.94(3) 2.38(3) 2.911(6) 116(2) 6_565
C8 H8 O3 0.95 2.58 3.312(3) 133.7 1_545
C9 H9 S1 0.95 2.97 3.759(4) 141.5 .
C9 H9 S1B 0.95 2.93 3.755(4) 145.4 .
C9 H9 O1 0.95 2.56 3.249(3) 129.4 6_566
_refine_diff_density_max 0.487
_refine_diff_density_min -0.548
_refine_diff_density_rms 0.082
_shelx_res_file
;
EE_sulf_SO4_2_0m.res created by SHELXL-2014/7
TITL EE_sulf_SO4_2_0m_a.res in C2/c
REM Old TITL EE_sulf_SO4_2_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.234, Rweak 0.013, Alpha 0.044, Orientation as input
REM Formula found by SHELXT: C24 N4 O7 S5
CELL 0.71073 17.4737 11.6240 11.7557 90.000 90.072 90.000
ZERR 4.000 0.0009 0.0005 0.0005 0.000 0.002 0.000
LATT 7
SYMM -X, Y, 1/2-Z
SFAC C H N O S
UNIT 72 88 24 36 20
TEMP -99.940
ACTA
CONF
L.S. 10
BOND $H
HTAB
EQIV $1 -x+1, y, -z+3/2
HTAB N1 O5_$1
HTAB N1 O6
EQIV $2 -x+1/2, -y+3/2, -z+2
HTAB C2 O7_$2
HTAB N1B S3
EQIV $3 -x+1, -y+1, -z+1
HTAB N3 S2_$3
HTAB N3 N2_$3
EQIV $4 x, y-1, z
HTAB N3 S3_$4
HTAB N3 O3_$4
HTAB N3 O4_$4
HTAB N3 S3_$3
HTAB N3 O4_$3
EQIV $5 x, -y+1, z-1/2
HTAB N3 O5_$5
HTAB N3 O7_$5
HTAB C8 O3_$4
HTAB C9 S1
HTAB C9 S1B
EQIV $6 x, -y+1, z+1/2
HTAB C9 O1_$6
LIST 4
FMAP 2
PLAN 10
WGHT 0.042100 4.668600
FVAR 0.08034
PART 1
S1 5 0.221282 0.597885 0.695560 10.50000 0.02773 0.01762 =
0.03087 0.00244 0.00873 -0.00046
N1 3 0.314093 0.756580 0.736598 10.50000 0.01411 0.01887 =
0.02712 0.00267 0.00100 -0.00503
AFIX 43
H1N 2 0.351264 0.807153 0.729575 10.50000 -1.20000
AFIX 0
C1 1 0.270269 0.748278 0.833674 10.50000 0.02822 0.03615 =
0.01745 -0.00067 0.00118 0.00776
AFIX 43
H1A 2 0.276982 0.795864 0.898626 10.50000 -1.20000
AFIX 0
C2 1 0.217943 0.666768 0.826192 10.50000 0.02569 0.03080 =
0.02499 0.01122 0.00842 0.01125
AFIX 43
H2 2 0.182842 0.648179 0.885039 10.50000 -1.20000
AFIX 0
C3 1 0.296162 0.682476 0.653981 10.50000 0.01595
PART 2
S1B 5 0.240365 0.615081 0.722036 10.50000 0.03106 0.01654 =
0.02780 0.00131 0.00471 0.00056
N1B 3 0.334554 0.780430 0.725241 10.50000 0.01503 0.01223 =
0.01482 -0.00409 -0.00023 -0.00316
AFIX 43
H1M 2 0.369897 0.830808 0.706265 10.50000 -1.20000
AFIX 0
C1B 1 0.298421 0.782401 0.829817 10.50000 0.03341 0.02439 =
0.01384 -0.00338 0.00267 0.01132
AFIX 43
H1B 2 0.308934 0.837979 0.886989 10.50000 -1.20000
AFIX 0
C2B 1 0.248043 0.699407 0.841863 10.50000 0.03020 0.02398 =
0.02277 0.00326 0.01074 0.00927
AFIX 43
H2B 2 0.219100 0.687294 0.909160 10.50000 -1.20000
AFIX 0
C3B 1 0.311873 0.696196 0.654743 10.50000 0.01356
PART 0
S2 5 0.319393 0.588048 0.462965 11.00000 0.03610 0.01605 =
0.01791 -0.00318 -0.00668 0.00741
O1 4 0.339873 0.634849 0.354270 11.00000 0.07704 0.03609 =
0.01406 0.00278 -0.00162 0.03063
O2 4 0.243061 0.544546 0.478501 11.00000 0.03072 0.02546 =
0.06394 -0.01559 -0.01562 0.00363
N2 3 0.339987 0.684549 0.554700 11.00000 0.02787 0.01307 =
0.01966 -0.00229 0.00057 0.00062
N3 3 0.528941 0.186850 0.533231 11.00000 0.03143 0.01194 =
0.02316 0.00286 0.00240 0.00368
H3N 2 0.580449 0.211801 0.519618 11.00000 0.06605
H3M 2 0.525283 0.152893 0.608925 11.00000 0.04319
H3L 2 0.518002 0.133235 0.476017 11.00000 0.04293
C4 1 0.383469 0.471657 0.486697 11.00000 0.02780 0.01146 =
0.01705 -0.00218 -0.00518 0.00033
C5 1 0.430100 0.435204 0.398104 11.00000 0.03155 0.01726 =
0.01376 0.00124 -0.00320 -0.00120
AFIX 43
H5 2 0.429581 0.474735 0.327378 11.00000 -1.20000
AFIX 0
C6 1 0.477265 0.340982 0.413610 11.00000 0.02921 0.01721 =
0.01470 -0.00207 -0.00013 0.00184
AFIX 43
H6 2 0.508678 0.314212 0.353255 11.00000 -1.20000
AFIX 0
C7 1 0.478180 0.285940 0.518439 11.00000 0.02515 0.00814 =
0.02039 -0.00017 -0.00237 -0.00004
C8 1 0.432587 0.322142 0.607307 11.00000 0.03234 0.01498 =
0.01652 0.00316 0.00054 -0.00058
AFIX 43
H8 2 0.434284 0.283920 0.678696 11.00000 -1.20000
AFIX 0
C9 1 0.384183 0.415417 0.590557 11.00000 0.02955 0.01657 =
0.01701 -0.00057 0.00193 0.00172
AFIX 43
H9 2 0.351624 0.440592 0.650236 11.00000 -1.20000
AFIX 0
S3 5 0.500000 0.972136 0.750000 10.50000 0.03297 0.00990 =
0.02313 0.00000 -0.00334 0.00000
O3 4 0.500000 1.098276 0.750000 10.50000 0.05684 0.01176 =
0.01855 0.00000 -0.00270 0.00000
PART -1
O4 4 0.541332 0.946323 0.635780 10.50000 0.04078 0.01861 =
0.01963 -0.00373 0.00348 0.00474
O5 4 0.549907 0.930098 0.839161 10.50000 0.05210 0.03690 =
0.02213 0.01077 0.00155 0.01932
O6 4 0.427587 0.918974 0.747801 10.50000 0.04169 0.05092 =
0.05281 -0.01326 0.00731 -0.02752
O7 4 0.393224 0.948561 0.981057 10.50000 0.06246 0.07998 =
0.07980 0.00496 0.00100 0.01604
PART 0
HKLF 4
REM EE_sulf_SO4_2_0m_a.res in C2/c
REM R1 = 0.0504 for 2433 Fo > 4sig(Fo) and 0.0922 for all 3526 data
REM 238 parameters refined using 0 restraints
END
WGHT 0.0421 4.6686
REM Instructions for potential hydrogen bonds
HTAB N1 O5_$1
HTAB N1 O6
HTAB C2 O7_$2
HTAB N1B S3
HTAB N3 S2_$3
HTAB N3 N2_$3
HTAB N3 S3_$4
HTAB N3 O3_$4
HTAB N3 O4_$4
HTAB N3 S3_$3
HTAB N3 O4_$3
HTAB N3 O5_$5
HTAB N3 O7_$5
HTAB C8 O3_$4
HTAB C9 S1
HTAB C9 S1B
HTAB C9 O1_$6
REM Highest difference peak 0.487, deepest hole -0.548, 1-sigma level 0.082
Q1 1 0.3261 0.6380 0.5124 11.00000 0.05 0.49
Q2 1 0.3512 0.5329 0.4746 11.00000 0.05 0.45
Q3 1 0.4966 1.0390 0.7849 11.00000 0.05 0.42
Q4 1 0.3941 0.4407 0.5355 11.00000 0.05 0.37
Q5 1 0.4694 0.3048 0.4628 11.00000 0.05 0.33
Q6 1 0.3064 0.6047 0.3723 11.00000 0.05 0.33
Q7 1 0.5004 0.3428 0.4853 11.00000 0.05 0.32
Q8 1 0.3145 0.6794 0.6035 11.00000 0.05 0.32
Q9 1 0.5026 0.2377 0.5232 11.00000 0.05 0.31
Q10 1 0.4256 0.3587 0.3351 11.00000 0.05 0.31
;
_shelx_res_checksum 30040
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_rrt_1_2_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 1499237'
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_audit_creation_date 2016-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_common
;
N-(2-methyl-4-oxopentan-2-yl)sulfathiazoium tosylate
;
_chemical_name_systematic
'N-(2-methyl-4-oxopentan-2-yl)-4-(N-(thiazol-2(3H)-ylidene)sulfamoyl)benzenaminium 4-methylbenzenesulfonate'
_chemical_formula_moiety 'C15 H20 N3 O3 S2, C7 H7 O3 S'
_chemical_formula_sum 'C22 H27 N3 O6 S3'
_chemical_formula_weight 525.64
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.1054(4)
_cell_length_b 13.3838(3)
_cell_length_c 17.8464(4)
_cell_angle_alpha 109.9580(10)
_cell_angle_beta 92.029(2)
_cell_angle_gamma 111.5910(10)
_cell_volume 2688.99(12)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9960
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 26.14
_cell_measurement_theta_min 2.28
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.315
_exptl_absorpt_correction_T_max 0.7460
_exptl_absorpt_correction_T_min 0.6886
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996) SADABS. University of Gottingen, Germany.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.298
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1104
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0598
_diffrn_reflns_av_unetI/netI 0.0751
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 70608
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.808
_diffrn_reflns_theta_min 1.700
_diffrn_ambient_temperature 173.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8907
_reflns_number_total 13884
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.456
_refine_diff_density_min -0.463
_refine_diff_density_rms 0.077
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 715
_refine_ls_number_reflns 13884
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0978
_refine_ls_R_factor_gt 0.0496
_refine_ls_restrained_S_all 1.028
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.6118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1100
_refine_ls_wR_factor_ref 0.1382
_refine_special_details ', SQUEEZE'
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C01B(H01Z), C01C(H01V), C01G(H01G), C01H(H3AA), C01I(H4AA), C01J(H01J),
C01K(H01), C01M(H0AA), C01N(H01W), C01O(H1AA), C01R(H5AA), C01S(H6AA)
2.b Idealised Me refined as rotating group:
C01F(H01C,H01D,H01E), C01L(H01F,H01H,H01I), C01Q(H01X,H01Y,H), C01U(H2AA,HA,
HB), C01V(H01K,H01L,H01M), C01W(H7AA,HC,HD)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S001 S 0.63127(5) 0.77575(5) 0.59067(3) 0.01699(13) Uani 1 1 d . . . . .
S002 S 0.65136(5) 0.28924(5) 0.63244(3) 0.01773(13) Uani 1 1 d . . . . .
S003 S 0.82188(5) -0.11045(5) 0.21417(4) 0.01940(14) Uani 1 1 d . . . . .
S004 S 0.84159(5) 0.38191(5) 0.22434(4) 0.02052(14) Uani 1 1 d . . . . .
S005 S 0.72431(5) 0.61760(5) 0.65129(4) 0.02325(15) Uani 1 1 d . . . . .
S006 S 0.76038(6) 0.12060(5) 0.66206(4) 0.02867(16) Uani 1 1 d . . . . .
O007 O 0.55761(13) 0.68108(13) 0.61023(10) 0.0217(4) Uani 1 1 d . . . . .
O008 O 0.80151(14) -0.23083(14) 0.19871(10) 0.0249(4) Uani 1 1 d . . . . .
O009 O 0.60229(14) 0.87247(14) 0.60217(10) 0.0232(4) Uani 1 1 d . . . . .
O00A O 0.58233(14) 0.19341(14) 0.65322(10) 0.0243(4) Uani 1 1 d . . . . .
O00B O 0.62236(14) 0.38755(14) 0.65206(10) 0.0240(4) Uani 1 1 d . . . . .
O00C O 0.81250(14) 0.27017(14) 0.23177(11) 0.0268(4) Uani 1 1 d . . . . .
O00D O 0.72760(15) -0.08450(15) 0.24140(10) 0.0284(4) Uani 1 1 d . . . . .
O00E O 0.92748(15) -0.02859(16) 0.26756(11) 0.0352(5) Uani 1 1 d . . . . .
O00F O 0.93294(16) 0.47369(16) 0.28760(11) 0.0385(5) Uani 1 1 d . . . . .
O00G O 0.74437(16) 0.40802(16) 0.21703(12) 0.0349(5) Uani 1 1 d . . . . .
O00H O 0.41279(16) -0.06934(17) 0.05356(11) 0.0358(5) Uani 1 1 d . . . . .
O00I O 0.35165(16) 0.46034(16) 0.07378(11) 0.0382(5) Uani 1 1 d . . . . .
N00J N 0.66566(17) 0.58381(18) 0.24098(12) 0.0187(4) Uani 1 1 d . . . . .
N00K N 0.75744(16) 0.82821(16) 0.63733(11) 0.0184(4) Uani 1 1 d . . . . .
N00L N 0.66525(17) 0.10539(18) 0.27898(12) 0.0178(4) Uani 1 1 d . . . . .
N00M N 0.78110(16) 0.33935(16) 0.67132(11) 0.0196(4) Uani 1 1 d . . . . .
N00N N 0.90429(17) 0.79708(18) 0.68747(13) 0.0234(5) Uani 1 1 d . . . . .
N00O N 0.93586(18) 0.30198(19) 0.69428(13) 0.0242(5) Uani 1 1 d . . . . .
C00P C 0.65676(18) 0.14957(19) 0.36472(13) 0.0166(5) Uani 1 1 d . . . . .
C00Q C 0.79550(19) 0.75949(19) 0.65693(13) 0.0175(5) Uani 1 1 d . . . . .
C00R C 0.6194(2) 0.6008(2) 0.44902(14) 0.0201(5) Uani 1 1 d . . . . .
C00S C 0.62269(19) 0.1160(2) 0.48591(14) 0.0184(5) Uani 1 1 d . . . . .
C00T C 0.62765(19) 0.0734(2) 0.40461(14) 0.0191(5) Uani 1 1 d . . . . .
C00U C 0.65521(19) 0.63017(19) 0.32667(13) 0.0172(5) Uani 1 1 d . . . . .
C00V C 0.64793(18) 0.23364(19) 0.52662(13) 0.0175(5) Uani 1 1 d . . . . .
C00W C 0.6293(2) 0.5570(2) 0.36858(14) 0.0202(5) Uani 1 1 d . . . . .
C00X C 0.6812(2) 0.2670(2) 0.40429(15) 0.0208(5) Uani 1 1 d . . . . .
C00Y C 0.63832(18) 0.71736(19) 0.48649(13) 0.0164(5) Uani 1 1 d . . . . .
C00Z C 0.8253(2) 0.26651(19) 0.67603(13) 0.0189(5) Uani 1 1 d . . . . .
C010 C 0.55728(19) 0.0538(2) 0.21489(13) 0.0181(5) Uani 1 1 d . . . . .
C011 C 0.83111(19) -0.0946(2) 0.11952(14) 0.0209(5) Uani 1 1 d . . . . .
C012 C 0.6727(2) 0.7457(2) 0.36297(15) 0.0221(5) Uani 1 1 d . . . . .
C013 C 0.6764(2) 0.3093(2) 0.48593(14) 0.0201(5) Uani 1 1 d . . . . .
C014 C 0.6643(2) 0.7894(2) 0.44345(15) 0.0224(5) Uani 1 1 d . . . . .
C015 C 0.5577(2) 0.5188(2) 0.17542(13) 0.0196(5) Uani 1 1 d . . . . .
C016 C 0.8901(2) 0.3662(2) 0.13165(14) 0.0209(5) Uani 1 1 d . . . . .
C017 C 0.5940(2) 0.0040(2) 0.13482(14) 0.0216(5) Uani 1 1 d . . . . .
C018 C 0.5223(2) 0.1513(2) 0.21912(17) 0.0241(5) Uani 1 1 d . . . . .
C019 C 0.5034(2) 0.6045(2) 0.18272(16) 0.0235(5) Uani 1 1 d . . . . .
C01A C 0.4689(2) -0.0405(2) 0.23429(17) 0.0257(6) Uani 1 1 d . . . . .
C01B C 0.8611(2) 0.0155(2) 0.11795(16) 0.0263(6) Uani 1 1 d . . . . .
H01Z H 0.8780 0.0809 0.1670 0.032 Uiso 1 1 calc R . . . .
C01C C 0.9716(2) 0.2182(2) 0.69701(16) 0.0323(6) Uani 1 1 d . . . . .
H01V H 1.0480 0.2325 0.7093 0.039 Uiso 1 1 calc R . . . .
C01D C 0.3962(2) 0.5589(2) 0.12307(15) 0.0275(6) Uani 1 1 d . . . . .
C01E C 0.5043(2) -0.0718(2) 0.06038(15) 0.0255(6) Uani 1 1 d . . . . .
C01F C 0.4830(2) 0.4121(2) 0.19085(15) 0.0267(6) Uani 1 1 d . . . . .
H01C H 0.5253 0.3660 0.1936 0.040 Uiso 1 1 calc GR . . . .
H01D H 0.4183 0.3648 0.1466 0.040 Uiso 1 1 calc GR . . . .
H01E H 0.4575 0.4370 0.2423 0.040 Uiso 1 1 calc GR . . . .
C01G C 0.9337(2) 0.7157(2) 0.70295(16) 0.0286(6) Uani 1 1 d . . . . .
H01G H 1.0080 0.7305 0.7233 0.034 Uiso 1 1 calc R . . . .
C01H C 0.8138(2) 0.3031(2) 0.05973(16) 0.0333(6) Uani 1 1 d . . . . .
H3AA H 0.7363 0.2699 0.0605 0.040 Uiso 1 1 calc R . . . .
C01I C 1.0030(2) 0.4110(2) 0.13035(17) 0.0322(6) Uani 1 1 d . . . . .
H4AA H 1.0561 0.4525 0.1795 0.039 Uiso 1 1 calc R . . . .
C01J C 0.8476(2) 0.6148(2) 0.68654(16) 0.0302(6) Uani 1 1 d . . . . .
H01J H 0.8530 0.5494 0.6933 0.036 Uiso 1 1 calc R . . . .
C01K C 0.8137(2) -0.1732(3) -0.02515(16) 0.0364(7) Uani 1 1 d . . . . .
H01 H 0.7979 -0.2383 -0.0742 0.044 Uiso 1 1 calc R . . . .
C01L C 0.5991(2) 0.4859(2) 0.09576(14) 0.0277(6) Uani 1 1 d . . . . .
H01F H 0.6501 0.5566 0.0898 0.042 Uiso 1 1 calc GR . . . .
H01H H 0.5353 0.4440 0.0506 0.042 Uiso 1 1 calc GR . . . .
H01I H 0.6384 0.4361 0.0955 0.042 Uiso 1 1 calc GR . . . .
C01M C 0.8076(2) -0.1898(2) 0.04800(15) 0.0297(6) Uani 1 1 d . . . . .
H0AA H 0.7875 -0.2652 0.0487 0.036 Uiso 1 1 calc R . . . .
C01N C 0.8886(2) 0.1157(2) 0.68073(17) 0.0324(6) Uani 1 1 d . . . . .
H01W H 0.8983 0.0482 0.6795 0.039 Uiso 1 1 calc R . . . .
C01O C 0.8662(2) 0.0297(3) 0.04484(18) 0.0339(6) Uani 1 1 d . . . . .
H1AA H 0.8865 0.1052 0.0442 0.041 Uiso 1 1 calc R . . . .
C01P C 0.8422(2) -0.0644(3) -0.02783(17) 0.0366(7) Uani 1 1 d . . . . .
C01Q C 0.5365(3) -0.1523(2) -0.00633(17) 0.0388(7) Uani 1 1 d . . . . .
H01X H 0.5442 -0.2118 0.0107 0.058 Uiso 1 1 calc GR . . . .
H01Y H 0.6077 -0.1079 -0.0182 0.058 Uiso 1 1 calc GR . . . .
H H 0.4785 -0.1897 -0.0551 0.058 Uiso 1 1 calc GR . . . .
C01R C 0.8504(3) 0.2883(3) -0.01310(18) 0.0452(8) Uani 1 1 d . . . . .
H5AA H 0.7973 0.2454 -0.0623 0.054 Uiso 1 1 calc R . . . .
C01S C 1.0378(3) 0.3945(3) 0.0561(2) 0.0445(8) Uani 1 1 d . . . . .
H6AA H 1.1155 0.4251 0.0550 0.053 Uiso 1 1 calc R . . . .
C01T C 0.9626(3) 0.3347(3) -0.01615(18) 0.0441(8) Uani 1 1 d . . . . .
C01U C 0.8461(3) -0.0471(3) -0.10765(19) 0.0546(9) Uani 1 1 d . . . . .
H2AA H 0.8428 -0.1179 -0.1508 0.082 Uiso 1 1 calc GR . . . .
HA H 0.9157 0.0183 -0.1028 0.082 Uiso 1 1 calc GR . . . .
HB H 0.7823 -0.0307 -0.1209 0.082 Uiso 1 1 calc GR . . . .
C01V C 0.3472(3) 0.6447(3) 0.1283(2) 0.0558(10) Uani 1 1 d . . . . .
H01K H 0.2787 0.6076 0.0876 0.084 Uiso 1 1 calc GR . . . .
H01L H 0.4010 0.7103 0.1182 0.084 Uiso 1 1 calc GR . . . .
H01M H 0.3299 0.6729 0.1825 0.084 Uiso 1 1 calc GR . . . .
C01W C 1.0014(4) 0.3198(4) -0.0967(2) 0.0759(13) Uani 1 1 d . . . . .
H7AA H 0.9952 0.2399 -0.1232 0.114 Uiso 1 1 calc GR . . . .
HC H 1.0794 0.3741 -0.0874 0.114 Uiso 1 1 calc GR . . . .
HD H 0.9548 0.3356 -0.1314 0.114 Uiso 1 1 calc GR . . . .
H012 H 0.693(2) 0.790(2) 0.3336(16) 0.036(8) Uiso 1 1 d . . . . .
H014 H 0.684(2) 0.869(2) 0.4677(14) 0.018(6) Uiso 1 1 d . . . . .
H00X H 0.704(2) 0.321(2) 0.3767(15) 0.031(7) Uiso 1 1 d . . . . .
H00O H 0.980(2) 0.370(2) 0.6986(15) 0.026(7) Uiso 1 1 d . . . . .
H00R H 0.600(2) 0.554(2) 0.4750(14) 0.020(7) Uiso 1 1 d . . . . .
H00A H 0.708(2) 0.641(2) 0.2268(15) 0.021(7) Uiso 1 1 d . . . . .
H01A H 0.562(2) 0.677(2) 0.1791(15) 0.027(7) Uiso 1 1 d . . . . .
H00B H 0.702(2) 0.537(2) 0.2359(15) 0.027(7) Uiso 1 1 d . . . . .
H00C H 0.692(2) 0.047(2) 0.2697(15) 0.028(7) Uiso 1 1 d . . . . .
H01S H 0.401(2) -0.077(2) 0.1917(16) 0.033(7) Uiso 1 1 d . . . . .
H01B H 0.493(2) 0.631(2) 0.2366(16) 0.030(7) Uiso 1 1 d . . . . .
H01P H 0.507(2) 0.182(2) 0.2677(16) 0.023(7) Uiso 1 1 d . . . . .
H00S H 0.603(2) 0.069(2) 0.5114(14) 0.018(6) Uiso 1 1 d . . . . .
H013 H 0.694(2) 0.390(2) 0.5131(14) 0.021(6) Uiso 1 1 d . . . . .
H01N H 0.634(2) -0.041(2) 0.1407(15) 0.031(7) Uiso 1 1 d . . . . .
H01Q H 0.580(2) 0.209(2) 0.2066(15) 0.028(7) Uiso 1 1 d . . . . .
H01T H 0.494(2) -0.104(2) 0.2316(16) 0.037(8) Uiso 1 1 d . . . . .
H01O H 0.646(2) 0.067(2) 0.1209(15) 0.026(7) Uiso 1 1 d . . . . .
H00N H 0.952(2) 0.869(3) 0.6934(17) 0.037(8) Uiso 1 1 d . . . . .
H00T H 0.617(2) -0.008(2) 0.3762(15) 0.029(7) Uiso 1 1 d . . . . .
H01R H 0.452(2) 0.119(2) 0.1776(17) 0.041(8) Uiso 1 1 d . . . . .
H00W H 0.620(2) 0.481(2) 0.3437(16) 0.036(8) Uiso 1 1 d . . . . .
H00D H 0.717(2) 0.165(3) 0.2706(16) 0.037(8) Uiso 1 1 d . . . . .
H01U H 0.450(2) -0.012(2) 0.2841(18) 0.037(8) Uiso 1 1 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
S001 0.0168(3) 0.0141(3) 0.0189(3) 0.0049(2) 0.0044(2) 0.0060(2)
S002 0.0164(3) 0.0160(3) 0.0200(3) 0.0080(2) 0.0050(2) 0.0044(2)
S003 0.0197(3) 0.0155(3) 0.0233(3) 0.0086(2) 0.0041(2) 0.0062(2)
S004 0.0200(3) 0.0152(3) 0.0255(3) 0.0092(2) 0.0070(2) 0.0047(2)
S005 0.0217(3) 0.0159(3) 0.0297(3) 0.0106(3) -0.0004(3) 0.0036(2)
S006 0.0291(4) 0.0164(3) 0.0402(4) 0.0146(3) 0.0039(3) 0.0056(3)
O007 0.0192(9) 0.0191(9) 0.0259(9) 0.0099(7) 0.0082(7) 0.0051(7)
O008 0.0279(10) 0.0198(9) 0.0323(10) 0.0141(8) 0.0098(8) 0.0113(8)
O009 0.0259(9) 0.0187(9) 0.0274(9) 0.0064(7) 0.0072(7) 0.0134(8)
O00A 0.0220(9) 0.0210(9) 0.0282(9) 0.0124(7) 0.0087(7) 0.0040(7)
O00B 0.0247(9) 0.0226(9) 0.0286(9) 0.0100(7) 0.0092(7) 0.0131(8)
O00C 0.0237(9) 0.0199(9) 0.0406(11) 0.0180(8) 0.0129(8) 0.0063(8)
O00D 0.0376(11) 0.0301(10) 0.0321(10) 0.0171(8) 0.0175(8) 0.0234(9)
O00E 0.0312(11) 0.0271(10) 0.0356(11) 0.0135(9) -0.0069(9) -0.0010(8)
O00F 0.0422(12) 0.0278(10) 0.0252(10) 0.0071(8) 0.0011(9) -0.0046(9)
O00G 0.0380(11) 0.0369(11) 0.0456(12) 0.0199(9) 0.0183(9) 0.0271(10)
O00H 0.0283(11) 0.0394(11) 0.0306(10) 0.0066(9) 0.0023(8) 0.0103(9)
O00I 0.0400(12) 0.0273(11) 0.0336(11) 0.0028(9) -0.0094(9) 0.0084(9)
N00J 0.0183(11) 0.0173(10) 0.0197(10) 0.0067(8) 0.0056(8) 0.0063(9)
N00K 0.0173(10) 0.0149(10) 0.0203(10) 0.0065(8) 0.0019(8) 0.0038(8)
N00L 0.0176(10) 0.0160(10) 0.0214(10) 0.0092(8) 0.0069(8) 0.0062(9)
N00M 0.0196(10) 0.0145(10) 0.0225(10) 0.0070(8) 0.0005(8) 0.0047(8)
N00N 0.0182(11) 0.0164(11) 0.0317(12) 0.0089(9) 0.0002(9) 0.0035(9)
N00O 0.0207(11) 0.0175(11) 0.0309(12) 0.0094(9) -0.0019(9) 0.0045(9)
C00P 0.0140(11) 0.0182(11) 0.0174(11) 0.0065(9) 0.0053(9) 0.0065(9)
C00Q 0.0186(12) 0.0160(11) 0.0156(11) 0.0046(9) 0.0051(9) 0.0055(10)
C00R 0.0263(13) 0.0165(12) 0.0194(12) 0.0094(10) 0.0033(10) 0.0083(10)
C00S 0.0173(12) 0.0173(12) 0.0222(12) 0.0124(10) 0.0021(10) 0.0043(10)
C00T 0.0179(12) 0.0159(12) 0.0241(12) 0.0085(10) 0.0027(10) 0.0068(10)
C00U 0.0156(12) 0.0179(11) 0.0157(11) 0.0042(9) 0.0028(9) 0.0060(9)
C00V 0.0124(11) 0.0171(11) 0.0203(12) 0.0075(9) 0.0023(9) 0.0030(9)
C00W 0.0266(13) 0.0123(11) 0.0209(12) 0.0049(10) 0.0012(10) 0.0086(10)
C00X 0.0229(13) 0.0171(12) 0.0250(13) 0.0121(10) 0.0063(10) 0.0069(10)
C00Y 0.0142(11) 0.0167(11) 0.0164(11) 0.0049(9) 0.0015(9) 0.0058(9)
C00Z 0.0215(13) 0.0168(12) 0.0157(11) 0.0067(9) 0.0033(10) 0.0044(10)
C010 0.0170(12) 0.0179(12) 0.0176(11) 0.0063(9) 0.0047(9) 0.0053(10)
C011 0.0182(12) 0.0232(13) 0.0244(13) 0.0113(10) 0.0063(10) 0.0096(10)
C012 0.0258(14) 0.0177(12) 0.0243(13) 0.0118(10) 0.0061(11) 0.0067(10)
C013 0.0215(13) 0.0138(12) 0.0239(13) 0.0072(10) 0.0042(10) 0.0058(10)
C014 0.0281(14) 0.0125(12) 0.0249(13) 0.0071(10) 0.0038(11) 0.0066(10)
C015 0.0198(12) 0.0181(12) 0.0172(12) 0.0041(9) 0.0030(10) 0.0060(10)
C016 0.0223(13) 0.0194(12) 0.0262(13) 0.0118(10) 0.0061(10) 0.0108(10)
C017 0.0237(13) 0.0239(13) 0.0208(13) 0.0099(10) 0.0092(10) 0.0117(11)
C018 0.0238(14) 0.0252(14) 0.0248(14) 0.0081(11) 0.0065(12) 0.0126(12)
C019 0.0265(14) 0.0194(13) 0.0212(13) 0.0044(10) 0.0020(11) 0.0088(11)
C01A 0.0233(14) 0.0237(14) 0.0232(14) 0.0090(11) 0.0069(11) 0.0017(11)
C01B 0.0245(14) 0.0249(13) 0.0307(14) 0.0130(11) 0.0086(11) 0.0088(11)
C01C 0.0290(15) 0.0308(15) 0.0385(16) 0.0112(12) -0.0016(12) 0.0162(13)
C01D 0.0301(15) 0.0260(14) 0.0250(13) 0.0088(11) 0.0014(11) 0.0109(12)
C01E 0.0290(15) 0.0221(13) 0.0255(13) 0.0108(11) 0.0070(11) 0.0088(11)
C01F 0.0264(14) 0.0200(13) 0.0285(14) 0.0088(11) 0.0009(11) 0.0046(11)
C01G 0.0249(14) 0.0236(14) 0.0362(15) 0.0093(11) -0.0035(12) 0.0112(11)
C01H 0.0264(15) 0.0425(17) 0.0305(15) 0.0097(13) 0.0029(12) 0.0176(13)
C01I 0.0225(14) 0.0357(16) 0.0379(16) 0.0159(13) 0.0064(12) 0.0094(12)
C01J 0.0286(15) 0.0219(13) 0.0391(16) 0.0126(12) -0.0049(12) 0.0093(12)
C01K 0.0392(17) 0.0414(17) 0.0253(14) 0.0055(13) 0.0073(12) 0.0190(14)
C01L 0.0365(16) 0.0273(14) 0.0192(12) 0.0076(11) 0.0097(11) 0.0134(12)
C01M 0.0320(15) 0.0261(14) 0.0287(14) 0.0095(11) 0.0043(12) 0.0105(12)
C01N 0.0377(16) 0.0271(14) 0.0389(16) 0.0145(12) 0.0009(13) 0.0188(13)
C01O 0.0309(15) 0.0361(16) 0.0459(17) 0.0272(14) 0.0150(13) 0.0143(13)
C01P 0.0298(16) 0.058(2) 0.0365(16) 0.0294(15) 0.0148(13) 0.0222(15)
C01Q 0.0480(19) 0.0342(16) 0.0292(15) 0.0030(12) 0.0068(13) 0.0199(14)
C01R 0.059(2) 0.063(2) 0.0259(15) 0.0117(15) 0.0046(15) 0.0433(19)
C01S 0.0352(17) 0.055(2) 0.057(2) 0.0306(17) 0.0290(16) 0.0227(16)
C01T 0.068(2) 0.059(2) 0.0358(17) 0.0291(16) 0.0261(17) 0.0459(19)
C01U 0.053(2) 0.087(3) 0.0447(19) 0.042(2) 0.0210(17) 0.035(2)
C01V 0.055(2) 0.0434(19) 0.056(2) -0.0001(16) -0.0204(17) 0.0268(17)
C01W 0.121(4) 0.115(4) 0.055(2) 0.056(2) 0.060(2) 0.089(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
S001 O007 1.4438(16) . ?
S001 O009 1.4311(16) . ?
S001 N00K 1.6029(19) . ?
S001 C00Y 1.775(2) . ?
S002 O00A 1.4476(16) . ?
S002 O00B 1.4358(17) . ?
S002 N00M 1.607(2) . ?
S002 C00V 1.770(2) . ?
S003 O008 1.4553(16) . ?
S003 O00D 1.4583(18) . ?
S003 O00E 1.4496(18) . ?
S003 C011 1.776(2) . ?
S004 O00C 1.4556(16) . ?
S004 O00F 1.4463(19) . ?
S004 O00G 1.4524(19) . ?
S004 C016 1.766(2) . ?
S005 C00Q 1.745(2) . ?
S005 C01J 1.730(3) . ?
S006 C00Z 1.740(2) . ?
S006 C01N 1.731(3) . ?
O00H C01E 1.215(3) . ?
O00I C01D 1.208(3) . ?
N00J C00U 1.474(3) . ?
N00J C015 1.552(3) . ?
N00J H00A 0.89(3) . ?
N00J H00B 0.90(3) . ?
N00K C00Q 1.327(3) . ?
N00L C00P 1.465(3) . ?
N00L C010 1.554(3) . ?
N00L H00C 0.94(3) . ?
N00L H00D 0.90(3) . ?
N00M C00Z 1.327(3) . ?
N00N C00Q 1.346(3) . ?
N00N C01G 1.385(3) . ?
N00N H00N 0.90(3) . ?
N00O C00Z 1.336(3) . ?
N00O C01C 1.379(3) . ?
N00O H00O 0.85(3) . ?
C00P C00T 1.386(3) . ?
C00P C00X 1.388(3) . ?
C00R C00W 1.384(3) . ?
C00R C00Y 1.391(3) . ?
C00R H00R 0.88(2) . ?
C00S C00T 1.380(3) . ?
C00S C00V 1.391(3) . ?
C00S H00S 0.87(2) . ?
C00T H00T 0.99(3) . ?
C00U C00W 1.381(3) . ?
C00U C012 1.381(3) . ?
C00V C013 1.391(3) . ?
C00W H00W 0.91(3) . ?
C00X C013 1.385(3) . ?
C00X H00X 0.98(3) . ?
C00Y C014 1.385(3) . ?
C010 C017 1.534(3) . ?
C010 C018 1.515(3) . ?
C010 C01A 1.519(3) . ?
C011 C01B 1.389(3) . ?
C011 C01M 1.386(3) . ?
C012 C014 1.379(3) . ?
C012 H012 0.89(3) . ?
C013 H013 0.96(2) . ?
C014 H014 0.93(2) . ?
C015 C019 1.531(3) . ?
C015 C01F 1.527(3) . ?
C015 C01L 1.520(3) . ?
C016 C01H 1.381(3) . ?
C016 C01I 1.382(3) . ?
C017 C01E 1.506(3) . ?
C017 H01N 0.97(3) . ?
C017 H01O 0.99(3) . ?
C018 H01P 0.89(3) . ?
C018 H01Q 0.96(3) . ?
C018 H01R 1.01(3) . ?
C019 C01D 1.517(3) . ?
C019 H01A 1.02(3) . ?
C019 H01B 0.94(3) . ?
C01A H01S 0.99(3) . ?
C01A H01T 1.01(3) . ?
C01A H01U 0.92(3) . ?
C01B H01Z 0.9500 . ?
C01B C01O 1.382(4) . ?
C01C H01V 0.9500 . ?
C01C C01N 1.326(4) . ?
C01D C01V 1.488(4) . ?
C01E C01Q 1.500(4) . ?
C01F H01C 0.9800 . ?
C01F H01D 0.9800 . ?
C01F H01E 0.9800 . ?
C01G H01G 0.9500 . ?
C01G C01J 1.330(3) . ?
C01H H3AA 0.9500 . ?
C01H C01R 1.377(4) . ?
C01I H4AA 0.9500 . ?
C01I C01S 1.390(4) . ?
C01J H01J 0.9500 . ?
C01K H01 0.9500 . ?
C01K C01M 1.397(4) . ?
C01K C01P 1.382(4) . ?
C01L H01F 0.9800 . ?
C01L H01H 0.9800 . ?
C01L H01I 0.9800 . ?
C01M H0AA 0.9500 . ?
C01N H01W 0.9500 . ?
C01O H1AA 0.9500 . ?
C01O C01P 1.390(4) . ?
C01P C01U 1.519(4) . ?
C01Q H01X 0.9800 . ?
C01Q H01Y 0.9800 . ?
C01Q H 0.9800 . ?
C01R H5AA 0.9500 . ?
C01R C01T 1.381(4) . ?
C01S H6AA 0.9500 . ?
C01S C01T 1.378(4) . ?
C01T C01W 1.515(4) . ?
C01U H2AA 0.9800 . ?
C01U HA 0.9800 . ?
C01U HB 0.9800 . ?
C01V H01K 0.9800 . ?
C01V H01L 0.9800 . ?
C01V H01M 0.9800 . ?
C01W H7AA 0.9800 . ?
C01W HC 0.9800 . ?
C01W HD 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O007 S001 N00K 112.63(10) . . ?
O007 S001 C00Y 107.21(10) . . ?
O009 S001 O007 118.09(10) . . ?
O009 S001 N00K 106.61(10) . . ?
O009 S001 C00Y 106.72(10) . . ?
N00K S001 C00Y 104.63(10) . . ?
O00A S002 N00M 112.67(10) . . ?
O00A S002 C00V 107.41(10) . . ?
O00B S002 O00A 117.27(10) . . ?
O00B S002 N00M 106.46(10) . . ?
O00B S002 C00V 108.20(10) . . ?
N00M S002 C00V 103.96(10) . . ?
O008 S003 O00D 111.27(10) . . ?
O008 S003 C011 106.62(11) . . ?
O00D S003 C011 106.29(10) . . ?
O00E S003 O008 112.86(11) . . ?
O00E S003 O00D 112.88(12) . . ?
O00E S003 C011 106.36(11) . . ?
O00C S004 C016 105.51(10) . . ?
O00F S004 O00C 111.81(11) . . ?
O00F S004 O00G 113.72(12) . . ?
O00F S004 C016 106.84(11) . . ?
O00G S004 O00C 111.78(11) . . ?
O00G S004 C016 106.55(11) . . ?
C01J S005 C00Q 90.93(12) . . ?
C01N S006 C00Z 90.83(12) . . ?
C00U N00J C015 118.27(18) . . ?
C00U N00J H00A 110.3(16) . . ?
C00U N00J H00B 108.2(16) . . ?
C015 N00J H00A 104.3(16) . . ?
C015 N00J H00B 109.1(17) . . ?
H00A N00J H00B 106(2) . . ?
C00Q N00K S001 119.37(16) . . ?
C00P N00L C010 117.69(18) . . ?
C00P N00L H00C 108.7(15) . . ?
C00P N00L H00D 106.3(18) . . ?
C010 N00L H00C 106.9(16) . . ?
C010 N00L H00D 109.0(17) . . ?
H00C N00L H00D 108(2) . . ?
C00Z N00M S002 119.46(16) . . ?
C00Q N00N C01G 114.9(2) . . ?
C00Q N00N H00N 119.6(18) . . ?
C01G N00N H00N 125.3(18) . . ?
C00Z N00O C01C 115.3(2) . . ?
C00Z N00O H00O 121.2(18) . . ?
C01C N00O H00O 123.1(18) . . ?
C00T C00P N00L 118.9(2) . . ?
C00T C00P C00X 121.9(2) . . ?
C00X C00P N00L 119.2(2) . . ?
N00K C00Q S005 129.94(18) . . ?
N00K C00Q N00N 120.7(2) . . ?
N00N C00Q S005 109.33(17) . . ?
C00W C00R C00Y 119.8(2) . . ?
C00W C00R H00R 118.9(16) . . ?
C00Y C00R H00R 121.3(16) . . ?
C00T C00S C00V 120.1(2) . . ?
C00T C00S H00S 119.8(16) . . ?
C00V C00S H00S 120.1(16) . . ?
C00P C00T H00T 120.2(15) . . ?
C00S C00T C00P 118.7(2) . . ?
C00S C00T H00T 120.9(15) . . ?
C00W C00U N00J 119.0(2) . . ?
C012 C00U N00J 119.1(2) . . ?
C012 C00U C00W 121.9(2) . . ?
C00S C00V S002 119.68(17) . . ?
C013 C00V S002 119.50(18) . . ?
C013 C00V C00S 120.7(2) . . ?
C00R C00W H00W 120.8(17) . . ?
C00U C00W C00R 118.8(2) . . ?
C00U C00W H00W 120.4(17) . . ?
C00P C00X H00X 121.9(16) . . ?
C013 C00X C00P 119.1(2) . . ?
C013 C00X H00X 118.9(16) . . ?
C00R C00Y S001 120.12(17) . . ?
C014 C00Y S001 119.30(18) . . ?
C014 C00Y C00R 120.6(2) . . ?
N00M C00Z S006 129.91(18) . . ?
N00M C00Z N00O 120.7(2) . . ?
N00O C00Z S006 109.35(17) . . ?
C017 C010 N00L 103.09(18) . . ?
C018 C010 N00L 108.25(19) . . ?
C018 C010 C017 113.1(2) . . ?
C018 C010 C01A 111.9(2) . . ?
C01A C010 N00L 107.84(19) . . ?
C01A C010 C017 112.0(2) . . ?
C01B C011 S003 118.76(19) . . ?
C01M C011 S003 121.20(19) . . ?
C01M C011 C01B 120.0(2) . . ?
C00U C012 H012 117.8(18) . . ?
C014 C012 C00U 119.1(2) . . ?
C014 C012 H012 122.9(18) . . ?
C00V C013 H013 121.8(14) . . ?
C00X C013 C00V 119.4(2) . . ?
C00X C013 H013 118.7(14) . . ?
C00Y C014 H014 122.6(14) . . ?
C012 C014 C00Y 119.8(2) . . ?
C012 C014 H014 117.3(14) . . ?
C019 C015 N00J 107.08(18) . . ?
C01F C015 N00J 108.04(18) . . ?
C01F C015 C019 112.6(2) . . ?
C01L C015 N00J 104.16(19) . . ?
C01L C015 C019 112.2(2) . . ?
C01L C015 C01F 112.1(2) . . ?
C01H C016 S004 119.1(2) . . ?
C01H C016 C01I 120.0(2) . . ?
C01I C016 S004 120.84(19) . . ?
C010 C017 H01N 109.7(15) . . ?
C010 C017 H01O 110.5(15) . . ?
C01E C017 C010 117.5(2) . . ?
C01E C017 H01N 106.7(16) . . ?
C01E C017 H01O 105.3(14) . . ?
H01N C017 H01O 106(2) . . ?
C010 C018 H01P 110.9(16) . . ?
C010 C018 H01Q 109.4(16) . . ?
C010 C018 H01R 108.8(16) . . ?
H01P C018 H01Q 111(2) . . ?
H01P C018 H01R 108(2) . . ?
H01Q C018 H01R 109(2) . . ?
C015 C019 H01A 107.0(14) . . ?
C015 C019 H01B 107.0(15) . . ?
C01D C019 C015 116.0(2) . . ?
C01D C019 H01A 111.7(14) . . ?
C01D C019 H01B 111.2(16) . . ?
H01A C019 H01B 103(2) . . ?
C010 C01A H01S 108.5(15) . . ?
C010 C01A H01T 110.4(16) . . ?
C010 C01A H01U 112.3(17) . . ?
H01S C01A H01T 106(2) . . ?
H01S C01A H01U 109(2) . . ?
H01T C01A H01U 110(2) . . ?
C011 C01B H01Z 120.1 . . ?
C01O C01B C011 119.9(2) . . ?
C01O C01B H01Z 120.1 . . ?
N00O C01C H01V 123.4 . . ?
C01N C01C N00O 113.2(2) . . ?
C01N C01C H01V 123.4 . . ?
O00I C01D C019 123.8(2) . . ?
O00I C01D C01V 120.8(2) . . ?
C01V C01D C019 115.4(2) . . ?
O00H C01E C017 123.7(2) . . ?
O00H C01E C01Q 121.7(2) . . ?
C01Q C01E C017 114.6(2) . . ?
C015 C01F H01C 109.5 . . ?
C015 C01F H01D 109.5 . . ?
C015 C01F H01E 109.5 . . ?
H01C C01F H01D 109.5 . . ?
H01C C01F H01E 109.5 . . ?
H01D C01F H01E 109.5 . . ?
N00N C01G H01G 123.4 . . ?
C01J C01G N00N 113.3(2) . . ?
C01J C01G H01G 123.4 . . ?
C016 C01H H3AA 120.1 . . ?
C01R C01H C016 119.8(3) . . ?
C01R C01H H3AA 120.1 . . ?
C016 C01I H4AA 120.5 . . ?
C016 C01I C01S 119.1(3) . . ?
C01S C01I H4AA 120.5 . . ?
S005 C01J H01J 124.3 . . ?
C01G C01J S005 111.46(19) . . ?
C01G C01J H01J 124.3 . . ?
C01M C01K H01 119.2 . . ?
C01P C01K H01 119.2 . . ?
C01P C01K C01M 121.6(3) . . ?
C015 C01L H01F 109.5 . . ?
C015 C01L H01H 109.5 . . ?
C015 C01L H01I 109.5 . . ?
H01F C01L H01H 109.5 . . ?
H01F C01L H01I 109.5 . . ?
H01H C01L H01I 109.5 . . ?
C011 C01M C01K 119.1(2) . . ?
C011 C01M H0AA 120.5 . . ?
C01K C01M H0AA 120.5 . . ?
S006 C01N H01W 124.4 . . ?
C01C C01N S006 111.3(2) . . ?
C01C C01N H01W 124.4 . . ?
C01B C01O H1AA 119.4 . . ?
C01B C01O C01P 121.2(3) . . ?
C01P C01O H1AA 119.4 . . ?
C01K C01P C01O 118.2(2) . . ?
C01K C01P C01U 121.4(3) . . ?
C01O C01P C01U 120.4(3) . . ?
C01E C01Q H01X 109.5 . . ?
C01E C01Q H01Y 109.5 . . ?
C01E C01Q H 109.5 . . ?
H01X C01Q H01Y 109.5 . . ?
H01X C01Q H 109.5 . . ?
H01Y C01Q H 109.5 . . ?
C01H C01R H5AA 119.3 . . ?
C01H C01R C01T 121.4(3) . . ?
C01T C01R H5AA 119.3 . . ?
C01I C01S H6AA 119.2 . . ?
C01T C01S C01I 121.6(3) . . ?
C01T C01S H6AA 119.2 . . ?
C01R C01T C01W 120.8(3) . . ?
C01S C01T C01R 118.0(3) . . ?
C01S C01T C01W 121.1(3) . . ?
C01P C01U H2AA 109.5 . . ?
C01P C01U HA 109.5 . . ?
C01P C01U HB 109.5 . . ?
H2AA C01U HA 109.5 . . ?
H2AA C01U HB 109.5 . . ?
HA C01U HB 109.5 . . ?
C01D C01V H01K 109.5 . . ?
C01D C01V H01L 109.5 . . ?
C01D C01V H01M 109.5 . . ?
H01K C01V H01L 109.5 . . ?
H01K C01V H01M 109.5 . . ?
H01L C01V H01M 109.5 . . ?
C01T C01W H7AA 109.5 . . ?
C01T C01W HC 109.5 . . ?
C01T C01W HD 109.5 . . ?
H7AA C01W HC 109.5 . . ?
H7AA C01W HD 109.5 . . ?
HC C01W HD 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S001 N00K C00Q S005 -8.9(3) . . . . ?
S001 N00K C00Q N00N 172.18(17) . . . . ?
S001 C00Y C014 C012 178.38(19) . . . . ?
S002 N00M C00Z S006 -12.4(3) . . . . ?
S002 N00M C00Z N00O 167.94(18) . . . . ?
S002 C00V C013 C00X 175.51(18) . . . . ?
S003 C011 C01B C01O -178.4(2) . . . . ?
S003 C011 C01M C01K 178.7(2) . . . . ?
S004 C016 C01H C01R -178.9(2) . . . . ?
S004 C016 C01I C01S 178.5(2) . . . . ?
O007 S001 N00K C00Q 29.6(2) . . . . ?
O007 S001 C00Y C00R -26.2(2) . . . . ?
O007 S001 C00Y C014 154.61(18) . . . . ?
O008 S003 C011 C01B -173.87(19) . . . . ?
O008 S003 C011 C01M 7.0(2) . . . . ?
O009 S001 N00K C00Q 160.68(17) . . . . ?
O009 S001 C00Y C00R -153.65(19) . . . . ?
O009 S001 C00Y C014 27.2(2) . . . . ?
O00A S002 N00M C00Z 37.4(2) . . . . ?
O00A S002 C00V C00S -23.6(2) . . . . ?
O00A S002 C00V C013 159.84(18) . . . . ?
O00B S002 N00M C00Z 167.29(17) . . . . ?
O00B S002 C00V C00S -151.08(19) . . . . ?
O00B S002 C00V C013 32.4(2) . . . . ?
O00C S004 C016 C01H 75.0(2) . . . . ?
O00C S004 C016 C01I -101.6(2) . . . . ?
O00D S003 C011 C01B 67.3(2) . . . . ?
O00D S003 C011 C01M -111.8(2) . . . . ?
O00E S003 C011 C01B -53.2(2) . . . . ?
O00E S003 C011 C01M 127.7(2) . . . . ?
O00F S004 C016 C01H -165.9(2) . . . . ?
O00F S004 C016 C01I 17.5(2) . . . . ?
O00G S004 C016 C01H -44.0(2) . . . . ?
O00G S004 C016 C01I 139.4(2) . . . . ?
N00J C00U C00W C00R -179.9(2) . . . . ?
N00J C00U C012 C014 -179.2(2) . . . . ?
N00J C015 C019 C01D 179.4(2) . . . . ?
N00K S001 C00Y C00R 93.6(2) . . . . ?
N00K S001 C00Y C014 -85.6(2) . . . . ?
N00L C00P C00T C00S 178.3(2) . . . . ?
N00L C00P C00X C013 -178.1(2) . . . . ?
N00L C010 C017 C01E 169.6(2) . . . . ?
N00M S002 C00V C00S 96.0(2) . . . . ?
N00M S002 C00V C013 -80.5(2) . . . . ?
N00N C01G C01J S005 -0.4(3) . . . . ?
N00O C01C C01N S006 -0.6(3) . . . . ?
C00P N00L C010 C017 -173.35(19) . . . . ?
C00P N00L C010 C018 66.5(2) . . . . ?
C00P N00L C010 C01A -54.7(3) . . . . ?
C00P C00X C013 C00V 0.4(4) . . . . ?
C00Q S005 C01J C01G 1.7(2) . . . . ?
C00Q N00N C01G C01J -1.6(3) . . . . ?
C00R C00Y C014 C012 -0.8(4) . . . . ?
C00S C00V C013 C00X -1.0(4) . . . . ?
C00T C00P C00X C013 0.0(4) . . . . ?
C00T C00S C00V S002 -175.34(18) . . . . ?
C00T C00S C00V C013 1.2(4) . . . . ?
C00U N00J C015 C019 59.8(3) . . . . ?
C00U N00J C015 C01F -61.7(3) . . . . ?
C00U N00J C015 C01L 178.86(19) . . . . ?
C00U C012 C014 C00Y -0.1(4) . . . . ?
C00V S002 N00M C00Z -78.56(19) . . . . ?
C00V C00S C00T C00P -0.8(3) . . . . ?
C00W C00R C00Y S001 -177.49(18) . . . . ?
C00W C00R C00Y C014 1.7(4) . . . . ?
C00W C00U C012 C014 0.1(4) . . . . ?
C00X C00P C00T C00S 0.2(3) . . . . ?
C00Y S001 N00K C00Q -86.48(19) . . . . ?
C00Y C00R C00W C00U -1.6(4) . . . . ?
C00Z S006 C01N C01C 0.8(2) . . . . ?
C00Z N00O C01C C01N 0.0(3) . . . . ?
C010 N00L C00P C00T 87.4(3) . . . . ?
C010 N00L C00P C00X -94.5(3) . . . . ?
C010 C017 C01E O00H 22.2(4) . . . . ?
C010 C017 C01E C01Q -158.0(2) . . . . ?
C011 C01B C01O C01P -0.2(4) . . . . ?
C012 C00U C00W C00R 0.8(4) . . . . ?
C015 N00J C00U C00W 83.5(3) . . . . ?
C015 N00J C00U C012 -97.1(3) . . . . ?
C015 C019 C01D O00I 2.5(4) . . . . ?
C015 C019 C01D C01V -177.2(3) . . . . ?
C016 C01H C01R C01T 0.6(4) . . . . ?
C016 C01I C01S C01T 0.1(4) . . . . ?
C018 C010 C017 C01E -73.7(3) . . . . ?
C01A C010 C017 C01E 53.9(3) . . . . ?
C01B C011 C01M C01K -0.4(4) . . . . ?
C01B C01O C01P C01K -0.5(4) . . . . ?
C01B C01O C01P C01U 178.8(3) . . . . ?
C01C N00O C00Z S006 0.5(3) . . . . ?
C01C N00O C00Z N00M -179.7(2) . . . . ?
C01F C015 C019 C01D -62.0(3) . . . . ?
C01G N00N C00Q S005 2.8(3) . . . . ?
C01G N00N C00Q N00K -178.0(2) . . . . ?
C01H C016 C01I C01S 1.9(4) . . . . ?
C01H C01R C01T C01S 1.4(5) . . . . ?
C01H C01R C01T C01W -178.8(3) . . . . ?
C01I C016 C01H C01R -2.3(4) . . . . ?
C01I C01S C01T C01R -1.8(5) . . . . ?
C01I C01S C01T C01W 178.5(3) . . . . ?
C01J S005 C00Q N00K 178.4(2) . . . . ?
C01J S005 C00Q N00N -2.51(19) . . . . ?
C01L C015 C019 C01D 65.7(3) . . . . ?
C01M C011 C01B C01O 0.7(4) . . . . ?
C01M C01K C01P C01O 0.7(4) . . . . ?
C01M C01K C01P C01U -178.5(3) . . . . ?
C01N S006 C00Z N00M 179.6(2) . . . . ?
C01N S006 C00Z N00O -0.72(19) . . . . ?
C01P C01K C01M C011 -0.3(4) . . . . ?
_shelx_res_file
;
rrt_1_2_0m_sq.res created by SHELXL-2014/7
TITL rrt_1_2_0m_a.res in P-1
REM Old TITL RRT_1_2_0m in P-1 #2
REM SHELXT solution in P-1
REM R1 0.140, Rweak 0.008, Alpha 0.054, Orientation as input
REM Formula found by SHELXT: C44 N6 O12 S6
CELL 0.71073 13.1054 13.3838 17.8464 109.958 92.029 111.591
ZERR 4 0.0004 0.0003 0.0004 0.001 0.002 0.001
LATT 1
SFAC C H N O S
UNIT 88 108 12 24 12
L.S. 5 0 43
PLAN 20
TEMP -99.95
BOND $H
MORE -1
CONF
ABIN
fmap 2
acta 52
OMIT 1 -2 1
OMIT 0 -1 2
OMIT -6 6 1
OMIT 1 -16 17
OMIT 0 1 1
OMIT 2 -4 3
REM
REM
REM
WGHT 0.066800 0.611800
FVAR 0.31728
S001 5 0.631274 0.775747 0.590675 11.00000 0.01676 0.01407 =
0.01886 0.00489 0.00442 0.00603
S002 5 0.651362 0.289239 0.632436 11.00000 0.01635 0.01597 =
0.02002 0.00803 0.00497 0.00440
S003 5 0.821879 -0.110454 0.214169 11.00000 0.01972 0.01547 =
0.02326 0.00864 0.00412 0.00624
S004 5 0.841589 0.381914 0.224344 11.00000 0.02003 0.01520 =
0.02554 0.00919 0.00701 0.00472
S005 5 0.724306 0.617596 0.651288 11.00000 0.02167 0.01586 =
0.02972 0.01062 -0.00036 0.00361
S006 5 0.760382 0.120603 0.662057 11.00000 0.02906 0.01643 =
0.04018 0.01462 0.00388 0.00557
O007 4 0.557610 0.681081 0.610232 11.00000 0.01916 0.01910 =
0.02586 0.00991 0.00823 0.00510
O008 4 0.801514 -0.230831 0.198706 11.00000 0.02791 0.01983 =
0.03234 0.01409 0.00978 0.01130
O009 4 0.602288 0.872465 0.602167 11.00000 0.02594 0.01866 =
0.02737 0.00636 0.00720 0.01344
O00A 4 0.582334 0.193409 0.653219 11.00000 0.02205 0.02098 =
0.02822 0.01238 0.00872 0.00397
O00B 4 0.622357 0.387554 0.652061 11.00000 0.02467 0.02257 =
0.02857 0.01003 0.00920 0.01311
O00C 4 0.812504 0.270174 0.231773 11.00000 0.02368 0.01989 =
0.04057 0.01802 0.01293 0.00632
O00D 4 0.727596 -0.084498 0.241400 11.00000 0.03758 0.03006 =
0.03206 0.01708 0.01748 0.02336
O00E 4 0.927475 -0.028594 0.267555 11.00000 0.03122 0.02706 =
0.03564 0.01354 -0.00686 -0.00100
O00F 4 0.932940 0.473692 0.287599 11.00000 0.04216 0.02776 =
0.02518 0.00713 0.00113 -0.00461
O00G 4 0.744368 0.408017 0.217028 11.00000 0.03796 0.03686 =
0.04558 0.01992 0.01829 0.02707
O00H 4 0.412793 -0.069337 0.053561 11.00000 0.02826 0.03936 =
0.03056 0.00660 0.00228 0.01027
O00I 4 0.351647 0.460341 0.073776 11.00000 0.04000 0.02731 =
0.03362 0.00277 -0.00939 0.00845
N00J 3 0.665656 0.583806 0.240982 11.00000 0.01828 0.01726 =
0.01973 0.00675 0.00559 0.00635
N00K 3 0.757442 0.828206 0.637325 11.00000 0.01728 0.01486 =
0.02032 0.00648 0.00187 0.00376
N00L 3 0.665249 0.105389 0.278983 11.00000 0.01756 0.01600 =
0.02141 0.00922 0.00694 0.00624
N00M 3 0.781101 0.339352 0.671322 11.00000 0.01962 0.01446 =
0.02246 0.00702 0.00053 0.00467
N00N 3 0.904287 0.797080 0.687473 11.00000 0.01821 0.01643 =
0.03168 0.00889 0.00022 0.00353
N00O 3 0.935857 0.301980 0.694284 11.00000 0.02071 0.01753 =
0.03086 0.00939 -0.00186 0.00446
C00P 1 0.656757 0.149570 0.364724 11.00000 0.01401 0.01817 =
0.01742 0.00648 0.00528 0.00651
C00Q 1 0.795503 0.759493 0.656934 11.00000 0.01856 0.01601 =
0.01564 0.00463 0.00507 0.00555
C00R 1 0.619369 0.600797 0.449015 11.00000 0.02629 0.01650 =
0.01943 0.00942 0.00328 0.00828
C00S 1 0.622689 0.115977 0.485908 11.00000 0.01726 0.01725 =
0.02222 0.01242 0.00213 0.00430
C00T 1 0.627654 0.073366 0.404606 11.00000 0.01792 0.01588 =
0.02413 0.00848 0.00274 0.00682
C00U 1 0.655213 0.630170 0.326671 11.00000 0.01556 0.01791 =
0.01567 0.00420 0.00279 0.00605
C00V 1 0.647926 0.233643 0.526624 11.00000 0.01244 0.01711 =
0.02025 0.00745 0.00228 0.00296
C00W 1 0.629280 0.556962 0.368583 11.00000 0.02661 0.01229 =
0.02090 0.00487 0.00121 0.00857
C00X 1 0.681227 0.266980 0.404293 11.00000 0.02288 0.01708 =
0.02501 0.01208 0.00632 0.00693
C00Y 1 0.638315 0.717364 0.486490 11.00000 0.01416 0.01675 =
0.01639 0.00490 0.00148 0.00576
C00Z 1 0.825288 0.266512 0.676034 11.00000 0.02154 0.01676 =
0.01571 0.00667 0.00330 0.00443
C010 1 0.557283 0.053796 0.214889 11.00000 0.01698 0.01792 =
0.01758 0.00629 0.00474 0.00529
C011 1 0.831105 -0.094599 0.119522 11.00000 0.01818 0.02323 =
0.02443 0.01133 0.00628 0.00960
C012 1 0.672708 0.745667 0.362970 11.00000 0.02578 0.01767 =
0.02428 0.01180 0.00608 0.00673
C013 1 0.676371 0.309270 0.485927 11.00000 0.02150 0.01378 =
0.02386 0.00724 0.00422 0.00582
C014 1 0.664251 0.789421 0.443447 11.00000 0.02805 0.01254 =
0.02486 0.00709 0.00379 0.00659
C015 1 0.557704 0.518757 0.175421 11.00000 0.01979 0.01810 =
0.01717 0.00406 0.00299 0.00602
C016 1 0.890075 0.366237 0.131654 11.00000 0.02230 0.01938 =
0.02618 0.01184 0.00612 0.01081
C017 1 0.594012 0.003983 0.134825 11.00000 0.02367 0.02395 =
0.02078 0.00985 0.00919 0.01170
C018 1 0.522264 0.151314 0.219120 11.00000 0.02384 0.02517 =
0.02482 0.00810 0.00647 0.01257
C019 1 0.503449 0.604474 0.182724 11.00000 0.02648 0.01937 =
0.02121 0.00444 0.00198 0.00877
C01A 1 0.468850 -0.040518 0.234285 11.00000 0.02330 0.02365 =
0.02319 0.00903 0.00694 0.00171
C01B 1 0.861090 0.015506 0.117946 11.00000 0.02455 0.02487 =
0.03069 0.01305 0.00856 0.00879
AFIX 43
H01Z 2 0.878046 0.080902 0.167033 11.00000 -1.20000
AFIX 0
C01C 1 0.971595 0.218224 0.697009 11.00000 0.02904 0.03083 =
0.03850 0.01122 -0.00162 0.01617
AFIX 43
H01V 2 1.048015 0.232531 0.709313 11.00000 -1.20000
AFIX 0
C01D 1 0.396155 0.558857 0.123068 11.00000 0.03005 0.02603 =
0.02496 0.00883 0.00140 0.01091
C01E 1 0.504331 -0.071848 0.060376 11.00000 0.02898 0.02213 =
0.02548 0.01075 0.00698 0.00884
C01F 1 0.482988 0.412087 0.190845 11.00000 0.02641 0.02002 =
0.02855 0.00880 0.00091 0.00460
AFIX 137
H01C 2 0.525258 0.365975 0.193578 11.00000 -1.50000
H01D 2 0.418260 0.364775 0.146577 11.00000 -1.50000
H01E 2 0.457490 0.437048 0.242280 11.00000 -1.50000
AFIX 0
C01G 1 0.933699 0.715727 0.702951 11.00000 0.02488 0.02359 =
0.03618 0.00931 -0.00354 0.01115
AFIX 43
H01G 2 1.007980 0.730513 0.723265 11.00000 -1.20000
AFIX 0
C01H 1 0.813807 0.303068 0.059732 11.00000 0.02644 0.04248 =
0.03051 0.00975 0.00288 0.01764
AFIX 43
H3AA 2 0.736295 0.269850 0.060498 11.00000 -1.20000
AFIX 0
C01I 1 1.003026 0.411023 0.130352 11.00000 0.02247 0.03567 =
0.03787 0.01590 0.00643 0.00943
AFIX 43
H4AA 2 1.056115 0.452537 0.179533 11.00000 -1.20000
AFIX 0
C01J 1 0.847556 0.614812 0.686536 11.00000 0.02861 0.02193 =
0.03909 0.01258 -0.00491 0.00933
AFIX 43
H01J 2 0.853000 0.549448 0.693307 11.00000 -1.20000
AFIX 0
C01K 1 0.813719 -0.173225 -0.025154 11.00000 0.03916 0.04136 =
0.02526 0.00553 0.00735 0.01905
AFIX 43
H01 2 0.797949 -0.238305 -0.074236 11.00000 -1.20000
AFIX 0
C01L 1 0.599066 0.485948 0.095758 11.00000 0.03646 0.02733 =
0.01917 0.00755 0.00973 0.01341
AFIX 137
H01F 2 0.650149 0.556566 0.089822 11.00000 -1.50000
H01H 2 0.535339 0.443986 0.050608 11.00000 -1.50000
H01I 2 0.638371 0.436144 0.095495 11.00000 -1.50000
AFIX 0
C01M 1 0.807565 -0.189766 0.047998 11.00000 0.03204 0.02613 =
0.02870 0.00947 0.00425 0.01054
AFIX 43
H0AA 2 0.787519 -0.265217 0.048697 11.00000 -1.20000
AFIX 0
C01N 1 0.888597 0.115713 0.680731 11.00000 0.03775 0.02710 =
0.03888 0.01449 0.00090 0.01879
AFIX 43
H01W 2 0.898255 0.048242 0.679479 11.00000 -1.20000
AFIX 0
C01O 1 0.866201 0.029713 0.044838 11.00000 0.03094 0.03607 =
0.04592 0.02720 0.01500 0.01433
AFIX 43
H1AA 2 0.886495 0.105239 0.044226 11.00000 -1.20000
AFIX 0
C01P 1 0.842212 -0.064407 -0.027825 11.00000 0.02983 0.05820 =
0.03650 0.02943 0.01483 0.02225
C01Q 1 0.536479 -0.152305 -0.006329 11.00000 0.04804 0.03420 =
0.02922 0.00299 0.00676 0.01989
AFIX 137
H01X 2 0.544225 -0.211824 0.010728 11.00000 -1.50000
H01Y 2 0.607674 -0.107948 -0.018219 11.00000 -1.50000
H 2 0.478547 -0.189726 -0.055091 11.00000 -1.50000
AFIX 0
C01R 1 0.850392 0.288350 -0.013099 11.00000 0.05878 0.06347 =
0.02587 0.01166 0.00460 0.04333
AFIX 43
H5AA 2 0.797327 0.245376 -0.062276 11.00000 -1.20000
AFIX 0
C01S 1 1.037839 0.394461 0.056066 11.00000 0.03519 0.05464 =
0.05742 0.03055 0.02904 0.02267
AFIX 43
H6AA 2 1.115452 0.425073 0.055043 11.00000 -1.20000
AFIX 0
C01T 1 0.962582 0.334739 -0.016151 11.00000 0.06796 0.05858 =
0.03580 0.02913 0.02606 0.04585
C01U 1 0.846094 -0.047149 -0.107647 11.00000 0.05335 0.08735 =
0.04470 0.04190 0.02096 0.03502
AFIX 137
H2AA 2 0.842834 -0.117872 -0.150754 11.00000 -1.50000
HA 2 0.915658 0.018267 -0.102795 11.00000 -1.50000
HB 2 0.782295 -0.030707 -0.120901 11.00000 -1.50000
AFIX 0
C01V 1 0.347242 0.644748 0.128286 11.00000 0.05512 0.04340 =
0.05641 -0.00010 -0.02044 0.02680
AFIX 137
H01K 2 0.278687 0.607562 0.087586 11.00000 -1.50000
H01L 2 0.400970 0.710314 0.118195 11.00000 -1.50000
H01M 2 0.329858 0.672931 0.182513 11.00000 -1.50000
AFIX 0
C01W 1 1.001431 0.319783 -0.096653 11.00000 0.12069 0.11477 =
0.05476 0.05582 0.05966 0.08877
AFIX 137
H7AA 2 0.995167 0.239930 -0.123195 11.00000 -1.50000
HC 2 1.079430 0.374144 -0.087445 11.00000 -1.50000
HD 2 0.954833 0.335597 -0.131410 11.00000 -1.50000
AFIX 0
H012 2 0.692686 0.789539 0.333626 11.00000 0.03613
H014 2 0.683548 0.868595 0.467691 11.00000 0.01848
H00X 2 0.704247 0.321174 0.376729 11.00000 0.03058
H00O 2 0.980234 0.369549 0.698612 11.00000 0.02614
H00R 2 0.599653 0.553631 0.475049 11.00000 0.01985
H00A 2 0.708242 0.641129 0.226823 11.00000 0.02109
H01A 2 0.562431 0.676731 0.179129 11.00000 0.02653
H00B 2 0.701931 0.537248 0.235879 11.00000 0.02726
H00C 2 0.692155 0.046865 0.269719 11.00000 0.02820
H01S 2 0.401062 -0.077463 0.191711 11.00000 0.03262
H01B 2 0.492541 0.631025 0.236619 11.00000 0.03001
H01P 2 0.507274 0.182332 0.267665 11.00000 0.02322
H00S 2 0.602889 0.069051 0.511378 11.00000 0.01850
H013 2 0.694464 0.390462 0.513076 11.00000 0.02067
H01N 2 0.634377 -0.041431 0.140714 11.00000 0.03136
H01Q 2 0.580063 0.208988 0.206646 11.00000 0.02822
H01T 2 0.494378 -0.103980 0.231622 11.00000 0.03676
H01O 2 0.646154 0.067273 0.120945 11.00000 0.02581
H00N 2 0.951886 0.868680 0.693369 11.00000 0.03727
H00T 2 0.616534 -0.008419 0.376183 11.00000 0.02947
H01R 2 0.452430 0.118646 0.177584 11.00000 0.04070
H00W 2 0.619624 0.481175 0.343675 11.00000 0.03560
H00D 2 0.717047 0.165042 0.270619 11.00000 0.03663
H01U 2 0.450230 -0.011711 0.284064 11.00000 0.03657
HKLF 4
REM rrt_1_2_0m_a.res in P-1
REM R1 = 0.0496 for 8907 Fo > 4sig(Fo) and 0.0978 for all 13884 data
REM 715 parameters refined using 0 restraints
END
WGHT 0.0668 0.6118
REM Highest difference peak 0.456, deepest hole -0.463, 1-sigma level 0.077
Q1 1 0.7227 0.3152 0.6538 11.00000 0.05 0.46
Q2 1 0.6382 0.7517 0.5342 11.00000 0.05 0.42
Q3 1 0.8383 0.1277 0.6668 11.00000 0.05 0.39
Q4 1 0.6439 0.5986 0.3493 11.00000 0.05 0.38
Q5 1 0.8144 -0.2348 0.2325 11.00000 0.05 0.37
Q6 1 0.8669 0.3804 0.1688 11.00000 0.05 0.37
Q7 1 0.7592 0.7056 0.6612 11.00000 0.05 0.36
Q8 1 0.7851 0.1900 0.6560 11.00000 0.05 0.36
Q9 1 0.8284 -0.1072 0.1608 11.00000 0.05 0.36
Q10 1 0.8760 0.4900 0.2792 11.00000 0.05 0.35
Q11 1 0.6394 0.5942 0.4071 11.00000 0.05 0.34
Q12 1 0.8072 -0.1810 0.2206 11.00000 0.05 0.34
Q13 1 0.8380 0.3327 0.2365 11.00000 0.05 0.33
Q14 1 0.7059 0.7980 0.6081 11.00000 0.05 0.33
Q15 1 1.0222 0.2333 0.6170 11.00000 0.05 0.33
Q16 1 0.7923 0.4620 0.2226 11.00000 0.05 0.32
Q17 1 0.8413 -0.0553 -0.0609 11.00000 0.05 0.31
Q18 1 0.8811 0.0043 0.2786 11.00000 0.05 0.31
Q19 1 0.7832 0.8395 0.5984 11.00000 0.05 0.31
Q20 1 0.6206 0.6782 0.6291 11.00000 0.05 0.31
;
_shelx_res_checksum 94824
_shelx_fab_checksum 51563
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-8 -3 21 -0.27 0.00
-6 -3 21 0.11 0.00
-5 -3 21 0.83 0.00
-4 -3 21 1.38 0.00
-3 -3 21 1.17 0.00
-2 -3 21 0.42 0.00
-1 -3 21 -0.10 0.00
0 -3 21 -0.06 0.00
1 -3 21 0.26 0.00
2 -3 21 0.50 0.00
3 -3 21 0.60 0.00
4 -3 21 0.54 0.00
5 -3 21 0.37 0.00
6 -3 21 0.26 0.00
7 -3 21 0.20 0.00
-7 -2 21 -0.28 0.00
-6 -2 21 -0.68 0.00
-5 -2 21 -0.32 0.00
-4 -2 21 0.82 0.00
-3 -2 21 2.01 0.00
-2 -2 21 2.52 0.00
-1 -2 21 2.27 0.00
0 -2 21 1.56 0.00
1 -2 21 0.81 0.00
2 -2 21 0.39 0.00
3 -2 21 0.28 0.00
4 -2 21 0.04 0.00
5 -2 21 -0.54 0.00
6 -2 21 -1.00 0.00
-10 -1 21 -0.09 0.00
-9 -1 21 0.39 0.00
-8 -1 21 0.59 0.00
-7 -1 21 -0.10 0.00
-6 -1 21 -1.16 0.00
-5 -1 21 -1.51 0.00
-4 -1 21 -0.88 0.00
-3 -1 21 0.01 0.00
-2 -1 21 0.53 0.00
-1 -1 21 0.68 0.00
0 -1 21 0.70 0.00
1 -1 21 0.73 0.00
2 -1 21 0.77 0.00
3 -1 21 0.72 0.00
4 -1 21 0.55 0.00
-10 0 21 -1.91 0.00
-9 0 21 -1.96 0.00
-8 0 21 -1.27 0.00
-7 0 21 -0.52 0.00
-6 0 21 -0.26 0.00
-5 0 21 -0.40 0.00
-4 0 21 -0.61 0.00
-3 0 21 -0.77 0.00
-2 0 21 -0.89 0.00
-1 0 21 -0.92 0.00
0 0 21 -0.74 0.00
1 0 21 -0.25 0.00
2 0 21 0.38 0.00
-9 1 21 -0.10 0.00
-8 1 21 0.75 0.00
-7 1 21 1.14 0.00
-6 1 21 0.84 0.00
-5 1 21 0.31 0.00
-4 1 21 -0.12 0.00
-3 1 21 -0.52 0.00
-2 1 21 -1.04 0.00
-1 1 21 -1.53 0.00
0 1 21 -1.65 0.00
1 1 21 -1.18 0.00
2 1 21 -0.35 0.00
-9 2 21 -0.73 0.00
-8 2 21 -1.49 0.00
-7 2 21 -1.85 0.00
-6 2 21 -1.56 0.00
-5 2 21 -0.78 0.00
-1 2 21 -0.22 0.00
0 2 21 -0.89 0.00
1 2 21 -0.81 0.00
-8 3 21 -1.32 0.00
-7 3 21 -1.42 0.00
-6 3 21 -1.44 0.00
-5 3 21 -1.38 0.00
-4 3 21 -1.17 0.00
-2 3 21 -0.54 0.00
-1 3 21 -0.65 0.00
-5 4 21 -1.88 0.00
-4 4 21 -1.97 0.00
1 -13 22 -0.46 0.00
6 -13 22 0.98 0.00
0 -12 22 -0.55 0.00
1 -12 22 -1.29 0.00
5 -12 22 0.88 0.00
6 -12 22 0.22 0.00
-2 -11 22 0.06 0.00
-1 -11 22 0.81 0.00
0 -11 22 0.90 0.00
1 -11 22 0.58 0.00
2 -11 22 0.33 0.00
4 -11 22 0.34 0.00
5 -11 22 0.25 0.00
6 -11 22 0.11 0.00
-4 -10 22 -0.45 0.00
-3 -10 22 1.05 0.00
-2 -10 22 1.54 0.00
-1 -10 22 0.75 0.00
0 -10 22 -0.52 0.00
1 -10 22 -1.32 0.00
2 -10 22 -1.22 0.00
3 -10 22 -0.46 0.00
4 -10 22 0.20 0.00
5 -10 22 0.13 0.00
6 -10 22 -0.49 0.00
-5 -9 22 -0.70 0.00
-4 -9 22 -1.11 0.00
-3 -9 22 -1.70 0.00
-2 -9 22 -1.84 0.00
-1 -9 22 -1.30 0.00
0 -9 22 -0.45 0.00
1 -9 22 0.22 0.00
2 -9 22 0.51 0.00
3 -9 22 0.62 0.00
4 -9 22 0.92 0.00
5 -9 22 1.45 0.00
6 -9 22 1.75 0.00
-5 -8 22 -0.84 0.00
-4 -8 22 -1.14 0.00
-3 -8 22 -1.01 0.00
-2 -8 22 -0.94 0.00
-1 -8 22 -0.98 0.00
0 -8 22 -0.72 0.00
1 -8 22 -0.15 0.00
2 -8 22 0.30 0.00
3 -8 22 0.37 0.00
4 -8 22 0.21 0.00
5 -8 22 -0.02 0.00
6 -8 22 -0.28 0.00
-6 -7 22 0.74 0.00
-5 -7 22 1.42 0.00
-4 -7 22 2.13 0.00
-3 -7 22 2.08 0.00
-2 -7 22 0.88 0.00
-1 -7 22 -0.90 0.00
0 -7 22 -2.00 0.00
1 -7 22 -1.65 0.00
2 -7 22 -0.37 0.00
3 -7 22 0.64 0.00
4 -7 22 0.75 0.00
5 -7 22 0.34 0.00
-6 -6 22 -0.03 0.00
-5 -6 22 -0.47 0.00
-4 -6 22 0.07 0.00
-3 -6 22 1.23 0.00
-2 -6 22 1.79 0.00
-1 -6 22 1.31 0.00
0 -6 22 0.60 0.00
1 -6 22 0.39 0.00
2 -6 22 0.48 0.00
3 -6 22 0.44 0.00
4 -6 22 0.47 0.00
5 -6 22 0.75 0.00
-6 -5 22 -0.52 0.00
-5 -5 22 -0.37 0.00
-4 -5 22 0.12 0.00
-3 -5 22 0.79 0.00
-2 -5 22 1.11 0.00
-1 -5 22 0.76 0.00
0 -5 22 0.07 0.00
1 -5 22 -0.36 0.00
2 -5 22 -0.34 0.00
3 -5 22 -0.04 0.00
4 -5 22 0.33 0.00
5 -5 22 0.63 0.00
-6 -4 22 -0.77 0.00
-4 -4 22 -0.93 0.00
-3 -4 22 -0.31 0.00
-2 -4 22 0.70 0.00
-1 -4 22 1.41 0.00
0 -4 22 1.58 0.00
1 -4 22 1.32 0.00
2 -4 22 0.63 0.00
3 -4 22 -0.25 0.00
4 -4 22 -0.74 0.00
-5 -3 22 -0.95 0.00
-4 -3 22 -1.36 0.00
-3 -3 22 -0.99 0.00
-2 -3 22 -0.23 0.00
-1 -3 22 0.19 0.00
0 -3 22 0.04 0.00
1 -3 22 -0.36 0.00
2 -3 22 -0.68 0.00
3 -3 22 -0.77 0.00
4 -3 22 -0.60 0.00
5 -3 22 -0.33 0.00
-6 -2 22 0.60 0.00
-5 -2 22 0.10 0.00
-4 -2 22 -1.06 0.00
-3 -2 22 -2.12 0.00
-2 -2 22 -2.44 0.00
-1 -2 22 -1.99 0.00
0 -2 22 -1.13 0.00
1 -2 22 -0.35 0.00
2 -2 22 -0.00 0.00
3 -2 22 0.02 0.00
4 -2 22 0.14 0.00
-5 -1 22 1.43 0.00
-4 -1 22 0.56 0.00
-3 -1 22 -0.36 0.00
-2 -1 22 -0.82 0.00
-1 -1 22 -0.89 0.00
0 -1 22 -0.81 0.00
1 -1 22 -0.74 0.00
2 -1 22 -0.65 0.00
-4 0 22 0.60 0.00
-3 0 22 0.58 0.00
-2 0 22 0.51 0.00
-1 0 22 0.43 0.00
0 0 22 0.23 0.00
0 -11 23 -0.63 0.00
1 -11 23 -0.26 0.00
5 -11 23 0.10 0.00
-4 -10 23 -0.32 0.00
-3 -10 23 -1.32 0.00
-2 -10 23 -1.27 0.00
-1 -10 23 -0.26 0.00
0 -10 23 0.79 0.00
1 -10 23 1.17 0.00
4 -10 23 -0.08 0.00
5 -10 23 0.10 0.00
-4 -9 23 1.23 0.00
-3 -9 23 1.71 0.00
-2 -9 23 1.68 0.00
-1 -9 23 1.10 0.00
0 -9 23 0.32 0.00
1 -9 23 -0.29 0.00
2 -9 23 -0.60 0.00
3 -9 23 -0.77 0.00
4 -9 23 -1.04 0.00
5 -9 23 -1.33 0.00
-4 -8 23 0.88 0.00
-3 -8 23 0.76 0.00
-2 -8 23 0.83 0.00
-1 -8 23 0.98 0.00
0 -8 23 0.71 0.00
1 -8 23 0.05 0.00
2 -8 23 -0.47 0.00
3 -8 23 -0.53 0.00
4 -8 23 -0.36 0.00
5 -8 23 -0.16 0.00
-5 -7 23 -1.60 0.00
-4 -7 23 -2.08 0.00
-3 -7 23 -1.75 0.00
-2 -7 23 -0.48 0.00
-1 -7 23 0.99 0.00
0 -7 23 1.59 0.00
1 -7 23 0.94 0.00
2 -7 23 -0.26 0.00
3 -7 23 -0.98 0.00
4 -7 23 -0.91 0.00
-5 -6 23 0.34 0.00
-4 -6 23 -0.32 0.00
-3 -6 23 -1.30 0.00
-2 -6 23 -1.57 0.00
-1 -6 23 -0.98 0.00
0 -6 23 -0.42 0.00
1 -6 23 -0.39 0.00
2 -6 23 -0.52 0.00
3 -6 23 -0.40 0.00
4 -6 23 -0.29 0.00
-5 -5 23 0.03 0.00
-2 -5 23 -0.90 0.00
-1 -5 23 -0.42 0.00
0 -5 23 0.06 0.00
1 -5 23 0.17 0.00
2 -5 23 -0.04 0.00
3 -5 23 -0.34 0.00
-4 -4 23 0.57 0.00
-3 -4 23 -0.11 0.00
-2 -4 23 -0.98 0.00
-1 -4 23 -1.45 0.00
0 -4 23 -1.39 0.00
1 -4 23 -0.95 0.00
2 -4 23 -0.24 0.00
3 -4 23 0.44 0.00
-4 -3 23 1.10 0.00
-3 -3 23 0.69 0.00
-2 -3 23 0.10 0.00
-1 -3 23 -0.12 0.00
0 -3 23 0.12 0.00
1 -3 23 0.53 0.00
2 -3 23 0.83 0.00
3 -3 23 0.84 0.00
-3 -2 23 1.89 0.00
-2 -2 23 1.97 0.00
-1 -2 23 1.38 0.00
0 -2 23 0.55 0.00
1 -2 23 -0.06 0.00
-3 -1 23 0.64 0.00
-2 -1 23 0.90 0.00
-1 -1 23 0.82 0.00
-3 0 23 -0.21 0.00
1 -10 24 -0.76 0.00
-1 -9 24 -0.81 0.00
1 -9 24 0.32 0.00
-3 -8 24 -0.55 0.00
-1 -8 24 -0.88 0.00
0 -8 24 -0.55 0.00
1 -8 24 0.13 0.00
3 -8 24 0.58 0.00
-3 -7 24 1.15 0.00
-2 -7 24 0.10 0.00
0 -7 24 -1.01 0.00
1 -7 24 -0.28 0.00
2 -7 24 0.65 0.00
3 -7 24 1.09 0.00
-3 -6 24 1.22 0.00
0 -6 24 0.25 0.00
1 -6 24 0.35 0.00
2 -6 24 0.43 0.00
-2 -5 24 0.54 0.00
-1 -5 24 0.16 0.00
0 -5 24 -0.02 0.00
1 -5 24 0.10 0.00
2 -5 24 0.35 0.00
-2 -4 24 1.01 0.00
-1 -4 24 1.17 0.00
0 -4 24 0.93 0.00
1 -4 24 0.47 0.00
2 -4 24 -0.08 0.00
-1 -3 24 -0.11 0.00
0 -3 24 -0.34 0.00
1 0 0 68.86 0.00
-1 1 0 -4.15 0.00
-1 2 0 -20.84 0.00
4 -4 1 -4.24 0.00
0 -1 1 7.85 0.00
1 -1 1 9.96 0.00
2 -1 1 9.81 0.00
-2 0 1 -46.02 0.00
-1 0 1 -72.32 0.00
0 0 1 -77.40 0.00
1 0 1 -56.44 0.00
-1 1 1 -2.39 0.00
4 1 1 1.45 0.00
-5 2 1 -0.55 0.00
13 -15 2 0.06 0.00
14 -14 2 1.44 0.00
-3 -2 2 0.48 0.00
0 0 2 62.41 0.00
-7 3 2 3.79 0.00
11 -16 3 1.31 0.00
13 -15 3 0.00 0.00
14 -14 3 -1.32 0.00
15 -13 3 0.98 0.00
-4 -2 3 0.46 0.00
1 -1 3 11.47 0.00
9 -17 4 -0.31 0.00
13 -15 4 -0.05 0.00
14 -14 4 0.96 0.00
15 -13 4 -0.69 0.00
15 -12 4 2.24 0.00
16 -11 4 -0.22 0.00
7 -3 4 1.74 0.00
4 -2 4 2.48 0.00
7 -17 5 1.14 0.00
8 -17 5 1.15 0.00
9 -17 5 0.88 0.00
14 -14 5 -0.52 0.00
15 -13 5 0.44 0.00
14 -12 5 -2.42 0.00
15 -12 5 -2.47 0.00
15 -11 5 -0.19 0.00
16 -11 5 0.22 0.00
16 -10 5 -1.43 0.00
7 -3 5 -2.48 0.00
-5 -2 5 2.60 0.00
0 0 5 -16.01 0.00
6 -17 6 -1.10 0.00
14 -14 6 0.16 0.00
15 -13 6 -0.29 0.00
15 -12 6 2.37 0.00
14 -11 6 0.75 0.00
15 -11 6 0.23 0.00
15 -10 6 1.71 0.00
16 -10 6 1.45 0.00
16 -9 6 2.02 0.00
6 -3 6 2.62 0.00
-1 0 6 14.03 0.00
12 -16 7 0.41 0.00
13 -15 7 -0.07 0.00
14 -14 7 -0.01 0.00
15 -12 7 -1.95 0.00
14 -11 7 -0.59 0.00
15 -11 7 -0.07 0.00
13 -10 7 -0.49 0.00
14 -10 7 -1.31 0.00
15 -10 7 -1.61 0.00
16 -10 7 -1.12 0.00
15 -9 7 -1.63 0.00
16 -9 7 -1.63 0.00
2 -3 7 0.30 0.00
0 -2 7 4.75 0.00
1 -2 7 6.92 0.00
-5 0 7 -7.96 0.00
13 -15 8 0.09 0.00
14 -14 8 0.10 0.00
15 -12 8 1.35 0.00
14 -11 8 0.17 0.00
15 -11 8 -0.16 0.00
13 -10 8 0.64 0.00
14 -10 8 1.25 0.00
15 -10 8 1.27 0.00
13 -9 8 0.20 0.00
14 -9 8 0.70 0.00
15 -9 8 1.10 0.00
15 -8 8 0.79 0.00
5 -2 8 3.72 0.00
-1 0 8 10.18 0.00
-5 1 8 5.75 0.00
3 -17 9 -0.54 0.00
14 -12 9 -1.42 0.00
14 -11 9 0.26 0.00
15 -11 9 0.28 0.00
13 -10 9 -0.74 0.00
14 -10 9 -1.05 0.00
15 -10 9 -0.87 0.00
15 -9 9 -0.32 0.00
1 -2 9 5.25 0.00
14 -12 10 0.90 0.00
14 -11 10 -0.46 0.00
13 -10 10 0.70 0.00
14 -10 10 0.77 0.00
15 -10 10 0.56 0.00
14 -12 11 -0.46 0.00
14 -11 11 0.36 0.00
-2 0 11 -6.74 0.00
13 -11 12 -0.57 0.00
14 -11 12 -0.07 0.00
13 -11 14 0.01 0.00
9 -15 15 0.10 0.00
10 -14 15 -0.15 0.00
4 -16 16 0.84 0.00
5 -16 16 0.24 0.00
0 -15 16 0.85 0.00
4 -15 16 -1.64 0.00
5 -15 16 -1.02 0.00
6 -15 16 -0.07 0.00
7 -15 16 0.32 0.00
8 -15 16 0.12 0.00
5 -14 16 1.12 0.00
10 -14 16 0.53 0.00
3 -15 17 0.90 0.00
4 -15 17 1.31 0.00
5 -15 17 0.74 0.00
6 -15 17 -0.10 0.00
7 -15 17 -0.42 0.00
4 -14 17 -0.18 0.00
3 -15 18 -0.47 0.00
4 -15 18 -0.87 0.00
5 -15 18 -0.44 0.00
5 -14 18 1.02 0.00
6 -14 18 0.35 0.00
3 -14 19 1.08 0.00
4 -14 19 -0.70 0.00
5 -14 19 -1.06 0.00
5 -13 19 -0.83 0.00
3 -13 20 0.43 0.00
4 -13 20 0.83 0.00
3 -12 21 0.40 0.00
4 -12 21 -1.00 0.00
-7 -3 21 -0.23 0.00
-5 -4 22 -0.90 0.00
-6 -3 22 -0.24 0.00
-3 -5 23 -0.90 0.00
0 0 0 0.00 0.00
# SQUEEZE RESULTS (Version = 70515)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.001 0.023 0.500 283 77 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.700
-1 1 0 1.894
-1 2 0 3.250
4 -4 1 7.461
0 -1 1 1.730
1 -1 1 2.055
2 -1 1 3.353
-2 0 1 3.399
-1 0 1 1.909
0 0 1 1.235
1 0 1 2.278
-1 1 1 2.451
4 1 1 8.114
-5 2 1 7.862
-3 -2 2 6.941
0 0 2 2.471
-4 -2 3 8.557
1 -1 3 3.828
4 -2 4 7.946
0 0 5 6.187
-1 0 6 7.310
2 -3 7 8.734
0 -2 7 8.021
1 -2 7 8.235
-1 0 8 9.758
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details
)
TITL rrt_1_2_0m_a.res in P-1
CELL 13.1054 13.3838 17.8464 109.96 92.03 111.59
SPGR P-1
# Solvent Accessible Volume = 295.6
# Electrons Found in S.A.V. = 76.8
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.896 0.209 0.387 ! 4.33 eA-3
C102 0.950 0.205 0.450 ! 3.48 eA-3
C103 0.851 0.572 0.484 ! 2.61 eA-3
C104 0.045 0.381 0.503 ! 2.55 eA-3
C105 0.942 0.725 0.484 ! 2.37 eA-3
C106 0.908 0.089 0.451 ! 2.15 eA-3
C107 0.974 0.284 0.479 ! 2.10 eA-3
C108 0.999 0.469 0.506 ! 2.01 eA-3
C109 0.970 0.153 0.485 ! 1.71 eA-3
C110 0.905 0.762 0.466 ! 1.25 eA-3
C111 0.015 0.030 0.504 ! 1.12 eA-3
C112 0.984 0.115 0.441 ! 0.96 eA-3
Q113 0.719 0.171 0.282 ! 0.89 eA-3
Q114 0.873 0.050 0.406 ! 0.82 eA-3
C115 0.863 0.999 0.437 ! 0.81 eA-3
Q116 0.143 0.231 0.325 ! 0.77 eA-3
C117 0.045 0.861 0.470 ! 0.75 eA-3
C118 0.862 0.694 0.483 ! 0.75 eA-3
C119 0.977 0.333 0.449 ! 0.72 eA-3
Q120 0.625 0.592 0.405 ! 0.69 eA-3
Q121 0.970 0.988 0.407 ! 0.66 eA-3
C122 0.044 0.059 0.473 ! 0.65 eA-3
Q123 0.405 0.268 0.396 ! 0.64 eA-3
Q124 0.833 0.219 0.421 ! 0.64 eA-3
Q125 0.357 0.639 0.110 ! 0.64 eA-3
C126 0.998 0.975 0.452 ! 0.63 eA-3
Q127 0.204 0.378 0.328 ! 0.62 eA-3
Q128 0.799 0.455 0.223 ! 0.62 eA-3
C129 0.057 0.488 0.454 ! 0.61 eA-3
C130 0.044 0.948 0.468 ! 0.61 eA-3
Q131 0.936 0.447 0.281 ! 0.61 eA-3
C132 0.109 0.842 0.466 ! 0.61 eA-3
Q133 0.799 0.109 0.358 ! 0.61 eA-3
Q134 0.969 0.157 0.399 ! 0.61 eA-3
C135 0.016 0.680 0.449 ! 0.61 eA-3
Q136 0.671 0.764 0.405 ! 0.60 eA-3
Q137 0.063 0.094 0.140 ! 0.60 eA-3
Q138 0.893 0.011 0.090 ! 0.60 eA-3
Q139 0.038 0.207 0.436 ! 0.59 eA-3
Q140 0.204 0.918 0.220 ! 0.59 eA-3
Q141 0.435 0.952 0.487 ! 0.59 eA-3
Q142 0.029 0.439 0.141 ! 0.59 eA-3
Q143 0.783 0.812 0.221 ! 0.59 eA-3
Q144 0.170 0.869 0.350 ! 0.59 eA-3
Q145 0.585 1.000 0.391 ! 0.58 eA-3
Q146 0.048 0.394 0.431 ! 0.58 eA-3
Q147 0.875 0.478 0.283 ! 0.58 eA-3
Q148 0.690 0.312 0.390 ! 0.57 eA-3
Q149 0.857 0.534 0.047 ! 0.56 eA-3
Q150 0.385 0.750 0.344 ! 0.56 eA-3
Q151 0.818 0.785 0.046 ! 0.56 eA-3
Q152 0.922 0.967 0.254 ! 0.56 eA-3
Q153 0.880 0.361 0.173 ! 0.56 eA-3
Q154 0.121 0.328 0.313 ! 0.55 eA-3
Q155 0.825 0.892 0.159 ! 0.55 eA-3
C156 0.875 0.647 0.407 ! 0.54 eA-3
Q157 0.747 0.459 0.234 ! 0.54 eA-3
Q158 0.073 0.205 0.453 ! 0.54 eA-3
C159 0.063 1.000 0.482 ! 0.53 eA-3
Q160 0.405 0.648 0.063 ! 0.53 eA-3
Q161 0.326 0.676 0.147 ! 0.53 eA-3
Q162 0.234 0.124 0.161 ! 0.53 eA-3
Q163 0.781 0.263 0.198 ! 0.53 eA-3
Q164 0.410 0.890 0.154 ! 0.53 eA-3
Q165 0.408 0.707 0.156 ! 0.52 eA-3
Q166 0.183 0.847 0.471 ! 0.52 eA-3
Q167 0.591 0.098 0.439 ! 0.52 eA-3
Q168 0.954 0.212 0.272 ! 0.52 eA-3
Q169 0.063 0.198 0.389 ! 0.52 eA-3
Q170 0.628 0.601 0.342 ! 0.52 eA-3
Q171 0.517 0.662 0.174 ! 0.52 eA-3
Q172 0.358 0.637 0.377 ! 0.52 eA-3
Q173 0.608 0.922 0.136 ! 0.52 eA-3
Q174 0.252 0.309 0.340 ! 0.51 eA-3
Q175 0.828 0.253 0.232 ! 0.51 eA-3
Q176 0.191 0.077 0.172 ! 0.51 eA-3
Q177 0.169 0.968 0.112 ! 0.51 eA-3
Q178 0.985 0.054 0.246 ! 0.51 eA-3
Q179 0.608 0.531 0.204 ! 0.51 eA-3
Q180 0.035 0.203 0.120 ! 0.51 eA-3
Q181 0.657 0.795 0.479 ! 0.51 eA-3
Q182 0.874 0.984 0.286 ! 0.51 eA-3
Q183 0.200 0.153 0.358 ! 0.50 eA-3
Q184 0.191 0.685 0.343 ! 0.50 eA-3
Q185 0.046 0.720 0.374 ! 0.50 eA-3
Q186 0.955 0.573 0.419 ! 0.50 eA-3
Q187 0.161 0.734 0.031 ! 0.50 eA-3
Q188 0.861 0.357 0.092 ! 0.50 eA-3
Q189 0.563 0.330 0.032 ! 0.50 eA-3
)
;
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'