# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019
#######################################################################
#
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1891649'
loop_
_audit_author_name
_audit_author_address
'Antonio C. Doriguetto'
;Federal University of Alfenas, Institute of Chemistry, Alfenas-MG
Brazil
;
_audit_update_record
;
2019-01-17 deposited with the CCDC. 2019-06-05 downloaded from the CCDC.
;
_audit_creation_date 2019-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
loop_
_audit_author_email
doriguetto@unifal-mg.edu.br
crisbrizoti@yahoo.com.br
_chemical_name_common ?
_chemical_name_systematic 'Sulfamethoxazole bromide'
_chemical_formula_moiety 'C10 H12 N3 O3 S, Br'
_chemical_formula_sum 'C10 H12 Br N3 O3 S'
_chemical_formula_weight 334.19
_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'
Br Br -0.2901 2.4595 '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 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
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 14.2076(8)
_cell_length_b 12.7070(6)
_cell_length_c 15.2817(9)
_cell_angle_alpha 90
_cell_angle_beta 92.703(5)
_cell_angle_gamma 90
_cell_volume 2755.8(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 11830
_cell_measurement_temperature 294(2)
_cell_measurement_theta_max 28.9350
_cell_measurement_theta_min 3.8030
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.138
_exptl_absorpt_correction_T_max 0.534
_exptl_absorpt_correction_T_min 0.242
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.552
_oxdiff_exptl_absorpt_empirical_full_max 4.187
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.611
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1344
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0456
_diffrn_reflns_av_unetI/netI 0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 23577
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.612
_diffrn_reflns_theta_min 3.376
_diffrn_ambient_temperature 294.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type SuperNova
_diffrn_measurement_method ?
_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 2907
_reflns_number_total 3886
_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 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.779
_refine_diff_density_min -0.699
_refine_diff_density_rms 0.078
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 165
_refine_ls_number_reflns 3596
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0536
_refine_ls_R_factor_gt 0.0370
_refine_ls_restrained_S_all 1.029
_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^)+(0.0395P)^2^+4.5754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0826
_refine_ls_wR_factor_ref 0.0908
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups, All N(H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
N1(H1), C3(H3), C5(H5), C8(H8), C6(H6), C2(H2)
2.b Idealised Me refined as rotating group:
N2(H2A,H2B,H2C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens geom
_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
Br1 Br 0.53562(2) 0.65491(2) 0.59396(2) 0.04136(10) Uani 1 1 d . . . . .
S1 S 0.74915(4) 0.27942(4) 0.62708(4) 0.02939(14) Uani 1 1 d . . . . .
O2 O 0.68657(13) 0.31959(13) 0.55980(10) 0.0340(4) Uani 1 1 d . . . . .
O1 O 0.75912(15) 0.16873(13) 0.63932(12) 0.0414(4) Uani 1 1 d . . . . .
O3 O 0.86551(15) 0.59176(16) 0.57693(16) 0.0575(6) Uani 1 1 d . . . . .
N2 N 0.64960(15) 0.48931(16) 0.95812(13) 0.0336(5) Uani 1 1 d . . . . .
H2A H 0.614507 0.545755 0.945294 0.040 Uiso 1 1 calc GR . . . .
H2B H 0.702575 0.509084 0.986918 0.040 Uiso 1 1 calc GR . . . .
H2C H 0.617786 0.445711 0.991431 0.040 Uiso 1 1 calc GR . . . .
N1 N 0.85513(16) 0.32089(17) 0.61316(15) 0.0378(5) Uani 1 1 d . . . . .
H1 H 0.899439 0.274881 0.611954 0.045 Uiso 1 1 calc R . . . .
N3 N 0.81807(18) 0.49491(18) 0.57282(18) 0.0496(6) Uani 1 1 d . . . . .
C4 C 0.67249(18) 0.43568(17) 0.87706(15) 0.0296(5) Uani 1 1 d . . . . .
C3 C 0.7365(2) 0.3548(2) 0.88100(17) 0.0432(7) Uani 1 1 d . . . . .
H3 H 0.764157 0.333626 0.934500 0.052 Uiso 1 1 calc R . . . .
C1 C 0.71764(18) 0.33867(17) 0.72582(15) 0.0292(5) Uani 1 1 d . . . . .
C5 C 0.63008(19) 0.4687(2) 0.79959(16) 0.0370(6) Uani 1 1 d . . . . .
H5 H 0.586304 0.523139 0.798770 0.044 Uiso 1 1 calc R . . . .
C7 C 0.87910(18) 0.4261(2) 0.60302(16) 0.0341(5) Uani 1 1 d . . . . .
C8 C 0.9656(2) 0.4723(3) 0.6252(2) 0.0554(8) Uani 1 1 d . . . . .
H8 H 1.020112 0.439183 0.647123 0.066 Uiso 1 1 calc R . . . .
C6 C 0.65309(19) 0.4202(2) 0.72274(16) 0.0364(6) Uani 1 1 d . . . . .
H6 H 0.625479 0.442023 0.669419 0.044 Uiso 1 1 calc R . . . .
C2 C 0.7593(2) 0.3049(2) 0.80418(17) 0.0430(7) Uani 1 1 d . . . . .
H2 H 0.802106 0.249509 0.805450 0.052 Uiso 1 1 calc R . . . .
C9 C 0.9535(2) 0.5747(3) 0.6082(2) 0.0577(8) Uani 1 1 d . . . . .
C10 C 1.0134(4) 0.6703(4) 0.6185(4) 0.1017(18) Uani 1 1 d . . . . .
H10A H 1.014584 0.706586 0.563493 0.153 Uiso 1 1 calc GR . . . .
H10B H 1.076268 0.650071 0.637147 0.153 Uiso 1 1 calc GR . . . .
H10C H 0.987937 0.715868 0.661580 0.153 Uiso 1 1 calc GR . . . .
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
Br1 0.02995(16) 0.04020(16) 0.05433(18) -0.00285(11) 0.00638(12) 0.00165(10)
S1 0.0317(3) 0.0267(3) 0.0301(3) -0.0038(2) 0.0041(2) 0.0025(2)
O2 0.0354(10) 0.0372(9) 0.0292(8) -0.0030(7) -0.0008(7) -0.0007(7)
O1 0.0541(13) 0.0273(9) 0.0434(10) -0.0037(7) 0.0071(9) 0.0057(8)
O3 0.0475(13) 0.0432(12) 0.0806(15) 0.0138(10) -0.0090(11) -0.0145(10)
N2 0.0351(12) 0.0342(11) 0.0319(10) -0.0053(8) 0.0059(9) -0.0026(9)
N1 0.0273(12) 0.0366(11) 0.0499(13) -0.0033(9) 0.0061(10) 0.0070(9)
N3 0.0380(14) 0.0358(12) 0.0742(17) 0.0052(11) -0.0066(12) -0.0072(10)
C4 0.0333(13) 0.0273(11) 0.0286(11) -0.0034(8) 0.0075(9) -0.0029(9)
C3 0.0574(19) 0.0441(15) 0.0274(12) 0.0013(10) -0.0043(12) 0.0150(13)
C1 0.0304(13) 0.0287(11) 0.0285(11) -0.0023(8) 0.0041(9) 0.0034(9)
C5 0.0383(15) 0.0362(13) 0.0367(13) -0.0044(10) 0.0039(11) 0.0116(11)
C7 0.0268(12) 0.0411(13) 0.0348(12) -0.0002(10) 0.0054(10) -0.0018(10)
C8 0.0303(15) 0.068(2) 0.067(2) 0.0141(16) -0.0042(14) -0.0101(14)
C6 0.0401(15) 0.0396(13) 0.0291(12) -0.0010(9) -0.0018(10) 0.0118(11)
C2 0.0530(18) 0.0412(14) 0.0345(13) -0.0010(11) -0.0010(12) 0.0219(13)
C9 0.0465(19) 0.067(2) 0.0594(19) 0.0149(15) -0.0036(15) -0.0234(16)
C10 0.086(3) 0.093(3) 0.123(4) 0.034(3) -0.031(3) -0.060(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 O2 1.4220(18) . ?
S1 O1 1.4251(18) . ?
S1 N1 1.619(2) . ?
S1 C1 1.763(2) . ?
O3 N3 1.403(3) . ?
O3 C9 1.334(4) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.464(3) . ?
N1 H1 0.8600 . ?
N1 C7 1.390(3) . ?
N3 C7 1.301(4) . ?
C4 C3 1.372(4) . ?
C4 C5 1.369(3) . ?
C3 H3 0.9300 . ?
C3 C2 1.386(4) . ?
C1 C6 1.383(3) . ?
C1 C2 1.379(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(3) . ?
C7 C8 1.390(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.337(5) . ?
C6 H6 0.9300 . ?
C2 H2 0.9300 . ?
C9 C10 1.487(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
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 120.26(12) . . ?
O2 S1 N1 110.00(11) . . ?
O2 S1 C1 106.87(11) . . ?
O1 S1 N1 104.56(12) . . ?
O1 S1 C1 109.68(11) . . ?
N1 S1 C1 104.41(12) . . ?
C9 O3 N3 108.3(2) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
S1 N1 H1 117.9 . . ?
C7 N1 S1 124.20(18) . . ?
C7 N1 H1 117.9 . . ?
C7 N3 O3 105.2(2) . . ?
C3 C4 N2 119.0(2) . . ?
C5 C4 N2 118.9(2) . . ?
C5 C4 C3 122.1(2) . . ?
C4 C3 H3 120.4 . . ?
C4 C3 C2 119.1(2) . . ?
C2 C3 H3 120.4 . . ?
C6 C1 S1 119.05(18) . . ?
C2 C1 S1 119.64(18) . . ?
C2 C1 C6 121.3(2) . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.1(2) . . ?
C6 C5 H5 120.4 . . ?
N3 C7 N1 121.6(2) . . ?
N3 C7 C8 111.7(3) . . ?
C8 C7 N1 126.7(3) . . ?
C7 C8 H8 127.5 . . ?
C9 C8 C7 105.0(3) . . ?
C9 C8 H8 127.5 . . ?
C1 C6 H6 120.3 . . ?
C5 C6 C1 119.3(2) . . ?
C5 C6 H6 120.3 . . ?
C3 C2 H2 120.5 . . ?
C1 C2 C3 119.1(2) . . ?
C1 C2 H2 120.5 . . ?
O3 C9 C8 109.7(3) . . ?
O3 C9 C10 115.3(3) . . ?
C8 C9 C10 134.9(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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
S1 N1 C7 N3 -25.3(4) . . . . ?
S1 N1 C7 C8 152.3(3) . . . . ?
S1 C1 C6 C5 -178.3(2) . . . . ?
S1 C1 C2 C3 177.6(2) . . . . ?
O2 S1 N1 C7 52.8(2) . . . . ?
O2 S1 C1 C6 -9.3(2) . . . . ?
O2 S1 C1 C2 172.3(2) . . . . ?
O1 S1 N1 C7 -176.8(2) . . . . ?
O1 S1 C1 C6 -141.2(2) . . . . ?
O1 S1 C1 C2 40.4(3) . . . . ?
O3 N3 C7 N1 176.5(2) . . . . ?
O3 N3 C7 C8 -1.3(3) . . . . ?
N2 C4 C3 C2 -179.0(3) . . . . ?
N2 C4 C5 C6 178.4(2) . . . . ?
N1 S1 C1 C6 107.2(2) . . . . ?
N1 S1 C1 C2 -71.2(2) . . . . ?
N1 C7 C8 C9 -176.6(3) . . . . ?
N3 O3 C9 C8 -0.4(4) . . . . ?
N3 O3 C9 C10 -178.8(3) . . . . ?
N3 C7 C8 C9 1.1(4) . . . . ?
C4 C3 C2 C1 0.5(5) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C3 C4 C5 C6 -0.9(4) . . . . ?
C1 S1 N1 C7 -61.5(2) . . . . ?
C5 C4 C3 C2 0.2(4) . . . . ?
C7 C8 C9 O3 -0.4(4) . . . . ?
C7 C8 C9 C10 177.6(5) . . . . ?
C6 C1 C2 C3 -0.7(4) . . . . ?
C2 C1 C6 C5 0.1(4) . . . . ?
C9 O3 N3 C7 1.1(3) . . . . ?
_iucr_refine_instructions_details
;
TITL SIR92 run in space group C 1 2/c 1
shelx.res
created by SHELXL-2017/1 at 16:57:42 on 17-Jan-2019
CELL 0.71073 14.2076 12.707 15.2817 90 92.703 90
ZERR 9 0.0008 0.0006 0.0009 0 0.005 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O S Br
UNIT 90 108 27 27 9 9
L.S. 10
PLAN 25
TEMP 21
BOND $H
CONF
fmap 2
ACTA
MERG 2
REM
REM
REM
WGHT 0.039500 4.575400
FVAR 2.15012
BR1 6 0.535618 0.654915 0.593964 11.00000 0.02995 0.04020 =
0.05433 -0.00285 0.00638 0.00165
S1 5 0.749155 0.279423 0.627082 11.00000 0.03167 0.02668 =
0.03007 -0.00384 0.00405 0.00247
O2 4 0.686565 0.319586 0.559803 11.00000 0.03536 0.03720 =
0.02924 -0.00299 -0.00082 -0.00071
O1 4 0.759115 0.168729 0.639322 11.00000 0.05406 0.02725 =
0.04341 -0.00366 0.00706 0.00571
O3 4 0.865513 0.591760 0.576934 11.00000 0.04746 0.04316 =
0.08060 0.01383 -0.00899 -0.01448
N2 3 0.649597 0.489315 0.958120 11.00000 0.03512 0.03422 =
0.03186 -0.00531 0.00587 -0.00259
AFIX 137
H2A 2 0.614507 0.545755 0.945294 11.00000 -1.20000
H2B 2 0.702575 0.509084 0.986918 11.00000 -1.20000
H2C 2 0.617786 0.445711 0.991431 11.00000 -1.20000
AFIX 0
N1 3 0.855125 0.320889 0.613157 11.00000 0.02725 0.03655 =
0.04985 -0.00330 0.00608 0.00704
AFIX 43
H1 2 0.899439 0.274881 0.611954 11.00000 -1.20000
AFIX 0
N3 3 0.818068 0.494915 0.572815 11.00000 0.03802 0.03585 =
0.07419 0.00515 -0.00664 -0.00716
C4 1 0.672494 0.435685 0.877058 11.00000 0.03335 0.02730 =
0.02863 -0.00341 0.00749 -0.00291
C3 1 0.736478 0.354753 0.880996 11.00000 0.05744 0.04413 =
0.02739 0.00130 -0.00433 0.01497
AFIX 43
H3 2 0.764157 0.333626 0.934500 11.00000 -1.20000
AFIX 0
C1 1 0.717640 0.338666 0.725817 11.00000 0.03045 0.02874 =
0.02854 -0.00229 0.00410 0.00338
C5 1 0.630078 0.468691 0.799586 11.00000 0.03833 0.03618 =
0.03668 -0.00435 0.00385 0.01162
AFIX 43
H5 2 0.586304 0.523139 0.798770 11.00000 -1.20000
AFIX 0
C7 1 0.879097 0.426092 0.603020 11.00000 0.02682 0.04105 =
0.03481 -0.00022 0.00542 -0.00179
C8 1 0.965598 0.472318 0.625202 11.00000 0.03032 0.06850 =
0.06675 0.01407 -0.00417 -0.01006
AFIX 43
H8 2 1.020112 0.439183 0.647123 11.00000 -1.20000
AFIX 0
C6 1 0.653091 0.420159 0.722741 11.00000 0.04014 0.03957 =
0.02909 -0.00098 -0.00181 0.01183
AFIX 43
H6 2 0.625479 0.442023 0.669419 11.00000 -1.20000
AFIX 0
C2 1 0.759301 0.304921 0.804176 11.00000 0.05296 0.04119 =
0.03452 -0.00096 -0.00105 0.02188
AFIX 43
H2 2 0.802106 0.249509 0.805450 11.00000 -1.20000
AFIX 0
C9 1 0.953460 0.574748 0.608198 11.00000 0.04651 0.06667 =
0.05942 0.01487 -0.00357 -0.02335
C10 1 1.013368 0.670279 0.618519 11.00000 0.08568 0.09282 =
0.12320 0.03428 -0.03109 -0.06025
AFIX 137
H10A 2 1.014584 0.706586 0.563493 11.00000 -1.50000
H10B 2 1.076268 0.650071 0.637147 11.00000 -1.50000
H10C 2 0.987937 0.715868 0.661580 11.00000 -1.50000
AFIX 0
HKLF 4
REM SIR92 run in space group C 1 2/c 1
REM R1 = 0.0370 for 2907 Fo > 4sig(Fo) and 0.0536 for all 3596 data
REM 165 parameters refined using 0 restraints
END
WGHT 0.0395 4.5755
REM Highest difference peak 0.779, deepest hole -0.699, 1-sigma level 0.078
Q1 1 0.5303 0.6967 0.5597 11.00000 0.05 0.78
Q2 1 0.5255 0.5962 0.5700 11.00000 0.05 0.49
Q3 1 0.5878 0.6529 0.5887 11.00000 0.05 0.35
Q4 1 0.5771 0.6250 0.5358 11.00000 0.05 0.32
Q5 1 0.5437 0.7044 0.6436 11.00000 0.05 0.31
Q6 1 0.7242 0.4198 0.8723 11.00000 0.05 0.29
Q7 1 0.7340 0.3134 0.6803 11.00000 0.05 0.29
Q8 1 0.4843 0.7167 0.6175 11.00000 0.05 0.28
Q9 1 0.5896 0.5759 0.7686 11.00000 0.05 0.28
Q10 1 0.7977 0.3534 0.9896 11.00000 0.05 0.28
Q11 1 0.6601 0.4558 0.7660 11.00000 0.05 0.27
Q12 1 0.6559 0.3609 0.7369 11.00000 0.05 0.27
Q13 1 0.6505 0.2429 0.6169 11.00000 0.05 0.26
Q14 1 0.4495 0.6629 0.5633 11.00000 0.05 0.26
Q15 1 0.7350 0.3132 0.5726 11.00000 0.05 0.26
Q16 1 0.5805 0.6892 0.5324 11.00000 0.05 0.26
Q17 1 0.6868 0.3848 0.7308 11.00000 0.05 0.25
Q18 1 0.4968 0.6231 0.6646 11.00000 0.05 0.24
Q19 1 0.7467 0.3425 0.8391 11.00000 0.05 0.24
Q20 1 1.0000 0.2656 0.7500 10.50000 0.05 0.24
Q21 1 0.8282 0.3000 0.7834 11.00000 0.05 0.24
Q22 1 0.6268 0.6319 0.6378 11.00000 0.05 0.24
Q23 1 0.5335 0.6822 0.6330 11.00000 0.05 0.24
Q24 1 0.7002 0.3715 0.5914 11.00000 0.05 0.24
Q25 1 0.6705 0.2768 0.6032 11.00000 0.05 0.24
REM The information below was added by Olex2.
REM
REM R1 = 0.0370 for 2907 Fo > 4sig(Fo) and 0.0536 for all 24085 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.78, deepest hole -0.70
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0536
REM R1_gt = 0.0370
REM wR_ref = 0.0908
REM GOOF = 1.029
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 24085
REM Reflections_gt = 2907
REM Parameters = n/a
REM Hole = -0.70
REM Peak = 0.78
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_smxno32med
_database_code_depnum_ccdc_archive 'CCDC 1891650'
loop_
_audit_author_name
_audit_author_address
'Antonio C. Doriguetto'
;Federal University of Alfenas, Institute of Chemistry, Alfenas-MG
Brazil
;
_audit_update_record
;
2019-01-17 deposited with the CCDC. 2019-06-05 downloaded from the CCDC.
;
_audit_creation_date 2019-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
loop_
_audit_author_email
crisbrizoti@yahoo.com.br
doriguetto@unifal-mg.edu.br
_chemical_name_common ?
_chemical_name_systematic 'Sulfamethoxazole nitrate'
_chemical_formula_moiety 'C10 H12 N3 O3 S, N O3'
_chemical_formula_sum 'C10 H12 N4 O6 S'
_chemical_formula_weight 316.30
_chemical_absolute_configuration unk
_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 4
_space_group_name_H-M_alt 'P 21'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 5.3927(4)
_cell_length_b 31.353(2)
_cell_length_c 7.8011(6)
_cell_angle_alpha 90
_cell_angle_beta 99.399(8)
_cell_angle_gamma 90
_cell_volume 1301.28(17)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 8978
_cell_measurement_temperature 292.44(11)
_cell_measurement_theta_max 29.3490
_cell_measurement_theta_min 3.8620
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.285
_exptl_absorpt_correction_T_max 0.972
_exptl_absorpt_correction_T_min 0.966
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.615
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 656
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0314
_diffrn_reflns_av_unetI/netI 0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 43
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 17077
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.758
_diffrn_reflns_theta_min 3.287
_diffrn_ambient_environment air
_diffrn_ambient_temperature 292.44(11)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.5847
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -13.00 86.00 0.75 6.78 -- 11.26 38.00 90.00 132
2 \w -17.00 82.75 0.75 6.78 -- 11.26 57.00 -30.00 133
3 \w -21.00 87.00 0.75 6.78 -- 11.26 77.00 -90.00 144
4 \w -65.00 43.00 0.75 6.78 -- 11.26 -77.00 150.00 144
5 \w -20.00 45.25 0.75 6.78 -- 11.26 -99.00 -30.00 87
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0133548000
_diffrn_orient_matrix_UB_12 0.0069750000
_diffrn_orient_matrix_UB_13 -0.0870353000
_diffrn_orient_matrix_UB_21 0.0042819000
_diffrn_orient_matrix_UB_22 0.0214332000
_diffrn_orient_matrix_UB_23 0.0283458000
_diffrn_orient_matrix_UB_31 0.1319909000
_diffrn_orient_matrix_UB_32 0.0000193000
_diffrn_orient_matrix_UB_33 0.0051535000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.825
_reflns_Friedel_fraction_full 0.982
_reflns_Friedel_fraction_max 0.775
_reflns_number_gt 5606
_reflns_number_total 7433
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.764
_refine_diff_density_min -0.270
_refine_diff_density_rms 0.064
_refine_ls_abs_structure_details
;
Flack x determined using 2197 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.17(4)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 383
_refine_ls_number_reflns 6269
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0565
_refine_ls_R_factor_gt 0.0503
_refine_ls_restrained_S_all 1.075
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.3669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1307
_refine_ls_wR_factor_ref 0.1364
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups, All N(H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
3.a Riding coordinates:
N1(H1)
3.b Aromatic/amide H refined with riding coordinates:
C2'(H2'), N1'(H1'), C5'(H5'), C6(H6), C5(H5), C2(H2), C6'(H6'), C8(H8),
C3(H3), C3'(H3'), C8'(H8')
3.c Idealised Me refined as rotating group:
N2(H2A,H2B,H2C), N2'(H2'A,H2'B,H2'C), C10(H10A,H10B,H10C), C10'(H10D,H10E,H10F)
;
_atom_sites_solution_hydrogens mixed
_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
S1 S 0.77351(19) 0.33156(3) 0.69408(13) 0.0320(2) Uani 1 1 d . . . . .
S1' S 0.64815(19) 0.03232(3) 1.21251(13) 0.0317(2) Uani 1 1 d . . . . .
O2 O 1.0143(6) 0.35137(11) 0.7176(4) 0.0414(8) Uani 1 1 d . . . . .
O2' O 0.8887(6) 0.01248(11) 1.2381(5) 0.0414(7) Uani 1 1 d . . . . .
O3 O 0.4317(6) 0.45893(13) 0.4127(5) 0.0489(9) Uani 1 1 d . . . . .
O1' O 0.5713(7) 0.05852(11) 1.3425(4) 0.0469(8) Uani 1 1 d . . . . .
C1 C 0.7415(8) 0.30233(13) 0.4996(5) 0.0288(8) Uani 1 1 d . . . . .
O3' O 0.3082(6) -0.09554(13) 0.9294(5) 0.0500(9) Uani 1 1 d . . . . .
N2 N 0.6729(8) 0.22882(13) 0.0487(5) 0.0404(9) Uani 1 1 d . . . . .
H2A H 0.516208 0.229892 -0.008602 0.049 Uiso 1 1 calc GR . . . .
H2B H 0.711579 0.202006 0.079746 0.049 Uiso 1 1 calc GR . . . .
H2C H 0.778254 0.238282 -0.019428 0.049 Uiso 1 1 calc GR . . . .
C2' C 0.4357(9) 0.09262(14) 0.9878(6) 0.0391(10) Uani 1 1 d . . . . .
H2' H 0.327075 0.097423 1.066914 0.047 Uiso 1 1 calc R . . . .
O1 O 0.7004(7) 0.30487(12) 0.8246(4) 0.0479(8) Uani 1 1 d . . . . .
C1' C 0.6208(8) 0.06198(12) 1.0191(5) 0.0278(8) Uani 1 1 d . . . . .
O5' O 0.7606(7) 0.15491(12) 0.2517(5) 0.0519(9) Uani 1 1 d . . . . .
N1 N 0.5625(7) 0.36855(12) 0.6671(5) 0.0371(9) Uani 1 1 d . . . . .
H1 H 0.416781 0.357013 0.640060 0.045 Uiso 1 1 d R . . . .
N2' N 0.5579(8) 0.13399(12) 0.5648(5) 0.0403(9) Uani 1 1 d . . . . .
H2'A H 0.399358 0.133894 0.510554 0.048 Uiso 1 1 calc GR . . . .
H2'B H 0.656814 0.123046 0.495143 0.048 Uiso 1 1 calc GR . . . .
H2'C H 0.605214 0.160642 0.592462 0.048 Uiso 1 1 calc GR . . . .
N4' N 0.9871(8) 0.14772(12) 0.2967(6) 0.0420(9) Uani 1 1 d . . . . .
C7 C 0.5729(7) 0.40524(14) 0.5640(5) 0.0314(9) Uani 1 1 d . . . . .
C9' C 0.5595(8) -0.09802(15) 0.9556(6) 0.0348(9) Uani 1 1 d . . . . .
C4 C 0.6939(8) 0.25554(13) 0.2039(5) 0.0319(9) Uani 1 1 d . . . . .
O6' O 1.1449(9) 0.16370(19) 0.2240(7) 0.0754(14) Uani 1 1 d . . . . .
N1' N 0.4358(7) -0.00490(12) 1.1809(5) 0.0357(8) Uani 1 1 d . . . . .
H1' H 0.305588 -0.001918 1.230462 0.043 Uiso 1 1 calc R . . . .
N4 N 0.0835(9) 0.21483(13) 0.7653(6) 0.0483(11) Uani 1 1 d . U . . .
C5' C 0.7587(9) 0.07750(16) 0.7512(6) 0.0405(10) Uani 1 1 d . . . . .
H5' H 0.864763 0.072392 0.670625 0.049 Uiso 1 1 calc R . . . .
C6 C 0.9011(8) 0.31015(15) 0.3821(6) 0.0353(9) Uani 1 1 d . . . . .
H6 H 1.024002 0.331147 0.404063 0.042 Uiso 1 1 calc R . . . .
C7' C 0.4482(8) -0.04111(14) 1.0803(5) 0.0318(8) Uani 1 1 d . . . . .
C4' C 0.5781(8) 0.10852(13) 0.7217(6) 0.0329(9) Uani 1 1 d . . . . .
C5 C 0.8760(8) 0.28625(15) 0.2302(6) 0.0363(9) Uani 1 1 d . . . . .
H5 H 0.980532 0.291031 0.148456 0.044 Uiso 1 1 calc R . . . .
O5 O -0.1321(10) 0.20085(16) 0.7401(6) 0.0727(13) Uani 1 1 d . . . . .
C2 C 0.5568(9) 0.27174(14) 0.4697(6) 0.0355(10) Uani 1 1 d . . . . .
H2 H 0.450036 0.267106 0.550145 0.043 Uiso 1 1 calc R . . . .
C6' C 0.7808(9) 0.05386(16) 0.9028(6) 0.0398(10) Uani 1 1 d . . . . .
H6' H 0.902711 0.032722 0.925741 0.048 Uiso 1 1 calc R . . . .
N3' N 0.2376(7) -0.05829(14) 1.0089(6) 0.0465(10) Uani 1 1 d . . . . .
C8 C 0.7816(8) 0.42893(15) 0.5334(6) 0.0361(9) Uani 1 1 d . . . . .
H8 H 0.950804 0.423006 0.570747 0.043 Uiso 1 1 calc R . . . .
C9 C 0.6824(8) 0.46172(15) 0.4389(6) 0.0369(9) Uani 1 1 d . . . . .
O4 O 0.1483(8) 0.23626(15) 0.9012(6) 0.0664(11) Uani 1 1 d . . . . .
C3 C 0.5316(9) 0.24798(15) 0.3189(6) 0.0381(10) Uani 1 1 d . . . . .
H3 H 0.407180 0.227276 0.295731 0.046 Uiso 1 1 calc R . . . .
C3' C 0.4155(10) 0.11593(16) 0.8369(7) 0.0426(11) Uani 1 1 d . . . . .
H3' H 0.291723 0.136718 0.812807 0.051 Uiso 1 1 calc R . . . .
C10 C 0.7917(11) 0.49996(18) 0.3662(7) 0.0496(12) Uani 1 1 d . . . . .
H10A H 0.778141 0.524096 0.439826 0.074 Uiso 1 1 calc GR . . . .
H10B H 0.701829 0.505662 0.251807 0.074 Uiso 1 1 calc GR . . . .
H10C H 0.965429 0.494786 0.360012 0.074 Uiso 1 1 calc GR . . . .
O4' O 1.0478(8) 0.12338(15) 0.4241(7) 0.0706(13) Uani 1 1 d . . . . .
C8' C 0.6587(8) -0.06470(14) 1.0499(6) 0.0346(9) Uani 1 1 d . . . . .
H8' H 0.827689 -0.058543 1.086752 0.041 Uiso 1 1 calc R . . . .
C10' C 0.6695(11) -0.13587(17) 0.8849(7) 0.0469(12) Uani 1 1 d . . . . .
H10D H 0.596716 -0.139441 0.764976 0.070 Uiso 1 1 calc GR . . . .
H10E H 0.635436 -0.160676 0.949353 0.070 Uiso 1 1 calc GR . . . .
H10F H 0.847860 -0.132151 0.894264 0.070 Uiso 1 1 calc GR . . . .
N3 N 0.3629(8) 0.42195(15) 0.4952(6) 0.0494(11) Uani 1 1 d . . . . .
O6 O 0.2330(13) 0.20808(18) 0.6664(9) 0.109(3) Uani 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 0.0372(5) 0.0331(5) 0.0255(5) -0.0017(4) 0.0043(4) -0.0015(4)
S1' 0.0360(5) 0.0324(5) 0.0266(5) 0.0021(4) 0.0049(4) 0.0001(4)
O2 0.0382(17) 0.0444(18) 0.0394(18) -0.0054(15) 0.0001(14) -0.0024(14)
O2' 0.0354(16) 0.0467(18) 0.0392(18) 0.0083(15) -0.0023(14) -0.0008(14)
O3 0.0359(17) 0.059(2) 0.050(2) 0.0138(19) 0.0012(15) 0.0087(16)
O1' 0.066(2) 0.0425(17) 0.0332(17) -0.0044(14) 0.0119(16) 0.0010(16)
C1 0.032(2) 0.0280(18) 0.0253(19) 0.0014(15) 0.0015(16) 0.0017(15)
O3' 0.0346(16) 0.059(2) 0.053(2) -0.0162(18) -0.0018(16) -0.0058(16)
N2 0.052(2) 0.0364(19) 0.032(2) -0.0058(16) 0.0049(18) 0.0022(17)
C2' 0.046(3) 0.039(2) 0.035(2) 0.0021(19) 0.014(2) 0.0099(19)
O1 0.068(2) 0.0465(18) 0.0302(16) 0.0048(15) 0.0108(16) -0.0046(17)
C1' 0.034(2) 0.0240(17) 0.0249(19) -0.0011(15) 0.0042(16) -0.0035(15)
O5' 0.0407(19) 0.053(2) 0.060(2) 0.0076(18) 0.0012(17) -0.0015(15)
N1 0.0334(19) 0.0348(19) 0.045(2) -0.0067(16) 0.0133(17) -0.0024(15)
N2' 0.056(2) 0.0355(19) 0.0287(19) 0.0032(16) 0.0033(18) -0.0049(17)
N4' 0.045(2) 0.0297(18) 0.052(2) -0.0031(17) 0.009(2) -0.0046(16)
C7 0.031(2) 0.035(2) 0.029(2) -0.0091(17) 0.0054(17) -0.0001(17)
C9' 0.038(2) 0.039(2) 0.029(2) 0.0034(18) 0.0095(19) -0.0019(19)
C4 0.039(2) 0.032(2) 0.024(2) -0.0029(16) 0.0041(18) 0.0024(17)
O6' 0.061(3) 0.080(3) 0.093(4) 0.000(3) 0.034(3) -0.018(2)
N1' 0.0341(18) 0.0336(18) 0.043(2) 0.0059(16) 0.0164(17) -0.0007(15)
N4 0.058(3) 0.035(2) 0.056(3) 0.0085(19) 0.023(2) 0.0063(19)
C5' 0.044(2) 0.048(3) 0.032(2) 0.003(2) 0.015(2) 0.005(2)
C6 0.038(2) 0.037(2) 0.033(2) -0.0015(18) 0.0104(18) -0.0111(18)
C7' 0.031(2) 0.037(2) 0.029(2) 0.0064(17) 0.0087(17) 0.0001(17)
C4' 0.041(2) 0.0276(19) 0.030(2) 0.0018(16) 0.0029(18) -0.0067(17)
C5 0.037(2) 0.044(2) 0.030(2) -0.0008(19) 0.0104(18) -0.0057(19)
O5 0.072(3) 0.080(3) 0.068(3) -0.022(3) 0.015(2) -0.028(2)
C2 0.039(2) 0.037(2) 0.034(2) -0.0013(18) 0.0148(19) -0.0064(18)
C6' 0.038(2) 0.044(3) 0.038(3) 0.007(2) 0.011(2) 0.0092(19)
N3' 0.0285(18) 0.056(3) 0.053(3) -0.012(2) 0.0002(18) 0.0018(17)
C8 0.028(2) 0.039(2) 0.040(2) 0.0031(19) 0.0043(19) 0.0020(18)
C9 0.038(2) 0.039(2) 0.035(2) -0.0019(19) 0.0070(19) 0.0033(19)
O4 0.056(2) 0.070(3) 0.070(3) -0.014(2) 0.000(2) -0.002(2)
C3 0.043(2) 0.034(2) 0.038(3) -0.0047(19) 0.008(2) -0.0093(19)
C3' 0.051(3) 0.036(2) 0.043(3) 0.008(2) 0.011(2) 0.015(2)
C10 0.058(3) 0.047(3) 0.043(3) 0.007(2) 0.008(3) -0.002(2)
O4' 0.059(3) 0.065(3) 0.082(3) 0.025(2) -0.005(2) 0.000(2)
C8' 0.029(2) 0.037(2) 0.038(2) 0.0007(19) 0.0066(19) -0.0033(17)
C10' 0.055(3) 0.045(3) 0.042(3) -0.012(2) 0.010(2) 0.000(2)
N3 0.032(2) 0.058(3) 0.057(3) 0.011(2) 0.004(2) -0.0006(19)
O6 0.143(5) 0.063(3) 0.152(6) 0.007(3) 0.115(5) 0.012(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 O2 1.424(4) . ?
S1 C1 1.756(4) . ?
S1 O1 1.422(3) . ?
S1 N1 1.614(4) . ?
S1' O2' 1.423(4) . ?
S1' O1' 1.419(3) . ?
S1' C1' 1.758(4) . ?
S1' N1' 1.625(4) . ?
O3 C9 1.337(6) . ?
O3 N3 1.405(6) . ?
C1 C6 1.378(6) . ?
C1 C2 1.375(6) . ?
O3' C9' 1.339(6) . ?
O3' N3' 1.404(6) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.461(5) . ?
C2' H2' 0.9300 . ?
C2' C1' 1.378(6) . ?
C2' C3' 1.375(7) . ?
C1' C6' 1.374(6) . ?
O5' N4' 1.235(6) . ?
N1 H1 0.8597 . ?
N1 C7 1.410(6) . ?
N2' H2'A 0.8900 . ?
N2' H2'B 0.8900 . ?
N2' H2'C 0.8900 . ?
N2' C4' 1.451(6) . ?
N4' O6' 1.206(6) . ?
N4' O4' 1.254(6) . ?
C7 C8 1.401(6) . ?
C7 N3 1.283(6) . ?
C9' C8' 1.338(6) . ?
C9' C10' 1.473(7) . ?
C4 C5 1.366(6) . ?
C4 C3 1.372(6) . ?
N1' H1' 0.8600 . ?
N1' C7' 1.388(6) . ?
N4 O5 1.228(6) . ?
N4 O4 1.256(6) . ?
N4 O6 1.221(6) . ?
C5' H5' 0.9300 . ?
C5' C4' 1.369(6) . ?
C5' C6' 1.385(6) . ?
C6 H6 0.9300 . ?
C6 C5 1.389(6) . ?
C7' N3' 1.297(6) . ?
C7' C8' 1.407(6) . ?
C4' C3' 1.374(7) . ?
C5 H5 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.380(6) . ?
C6' H6' 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.326(6) . ?
C9 C10 1.489(7) . ?
C3 H3 0.9300 . ?
C3' H3' 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C8' H8' 0.9300 . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?
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 C1 107.3(2) . . ?
O2 S1 N1 108.2(2) . . ?
O1 S1 O2 121.2(2) . . ?
O1 S1 C1 108.2(2) . . ?
O1 S1 N1 104.1(2) . . ?
N1 S1 C1 107.1(2) . . ?
O2' S1' C1' 107.3(2) . . ?
O2' S1' N1' 108.1(2) . . ?
O1' S1' O2' 121.3(2) . . ?
O1' S1' C1' 108.3(2) . . ?
O1' S1' N1' 104.1(2) . . ?
N1' S1' C1' 107.0(2) . . ?
C9 O3 N3 108.7(4) . . ?
C6 C1 S1 119.9(3) . . ?
C2 C1 S1 118.5(3) . . ?
C2 C1 C6 121.6(4) . . ?
C9' O3' N3' 108.8(4) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
C1' C2' H2' 120.8 . . ?
C3' C2' H2' 120.8 . . ?
C3' C2' C1' 118.4(4) . . ?
C2' C1' S1' 118.5(3) . . ?
C6' C1' S1' 119.7(3) . . ?
C6' C1' C2' 121.8(4) . . ?
S1 N1 H1 109.0 . . ?
C7 N1 S1 124.6(3) . . ?
C7 N1 H1 108.9 . . ?
H2'A N2' H2'B 109.5 . . ?
H2'A N2' H2'C 109.5 . . ?
H2'B N2' H2'C 109.5 . . ?
C4' N2' H2'A 109.5 . . ?
C4' N2' H2'B 109.5 . . ?
C4' N2' H2'C 109.5 . . ?
O5' N4' O4' 117.0(4) . . ?
O6' N4' O5' 122.1(5) . . ?
O6' N4' O4' 120.8(5) . . ?
C8 C7 N1 129.6(4) . . ?
N3 C7 N1 117.2(4) . . ?
N3 C7 C8 113.0(4) . . ?
O3' C9' C10' 116.7(4) . . ?
C8' C9' O3' 110.0(4) . . ?
C8' C9' C10' 133.3(4) . . ?
C5 C4 N2 119.0(4) . . ?
C5 C4 C3 122.9(4) . . ?
C3 C4 N2 118.1(4) . . ?
S1' N1' H1' 117.4 . . ?
C7' N1' S1' 125.1(3) . . ?
C7' N1' H1' 117.4 . . ?
O5 N4 O4 116.8(5) . . ?
O6 N4 O5 122.9(6) . . ?
O6 N4 O4 120.3(6) . . ?
C4' C5' H5' 120.6 . . ?
C4' C5' C6' 118.9(4) . . ?
C6' C5' H5' 120.6 . . ?
C1 C6 H6 120.4 . . ?
C1 C6 C5 119.1(4) . . ?
C5 C6 H6 120.4 . . ?
N1' C7' C8' 129.8(4) . . ?
N3' C7' N1' 117.6(4) . . ?
N3' C7' C8' 112.5(4) . . ?
C5' C4' N2' 119.1(4) . . ?
C5' C4' C3' 121.5(4) . . ?
C3' C4' N2' 119.4(4) . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.3(4) . . ?
C3 C2 H2 120.4 . . ?
C1' C6' C5' 119.3(4) . . ?
C1' C6' H6' 120.4 . . ?
C5' C6' H6' 120.4 . . ?
C7' N3' O3' 104.7(4) . . ?
C7 C8 H8 128.0 . . ?
C9 C8 C7 104.1(4) . . ?
C9 C8 H8 128.0 . . ?
O3 C9 C10 116.6(4) . . ?
C8 C9 O3 109.9(4) . . ?
C8 C9 C10 133.4(5) . . ?
C4 C3 C2 118.6(4) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0(4) . . ?
C4' C3' H3' 120.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9' C8' C7' 104.0(4) . . ?
C9' C8' H8' 128.0 . . ?
C7' C8' H8' 128.0 . . ?
C9' C10' H10D 109.5 . . ?
C9' C10' H10E 109.5 . . ?
C9' C10' H10F 109.5 . . ?
H10D C10' H10E 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
C7 N3 O3 104.3(4) . . ?
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
_geom_hbond_publ_flag
N2' H2'B O1' 0.89 2.35 2.941(5) 123.5 1_554 yes
N1' H1' O2' 0.86 2.30 3.103(5) 154.8 1_455 yes
C8 H8 O2 0.93 2.52 2.994(6) 112.0 . yes
C8' H8' O2' 0.93 2.52 2.992(6) 112.0 . yes
C8' H8' N3' 0.93 2.39 3.196(6) 145.5 1_655 yes
C10' H10F O3' 0.96 2.71 3.632(6) 161.8 1_655 yes
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
S1 C1 C6 C5 178.9(3) . . . . ?
S1 C1 C2 C3 -178.9(4) . . . . ?
S1 N1 C7 C8 -33.7(7) . . . . ?
S1 N1 C7 N3 151.5(4) . . . . ?
S1' C1' C6' C5' -179.7(4) . . . . ?
S1' N1' C7' N3' -152.4(4) . . . . ?
S1' N1' C7' C8' 32.0(7) . . . . ?
O2 S1 C1 C6 -16.1(4) . . . . ?
O2 S1 C1 C2 163.4(4) . . . . ?
O2 S1 N1 C7 42.1(4) . . . . ?
O2' S1' C1' C2' -163.6(3) . . . . ?
O2' S1' C1' C6' 17.2(4) . . . . ?
O2' S1' N1' C7' -41.3(4) . . . . ?
O1' S1' C1' C2' -31.1(4) . . . . ?
O1' S1' C1' C6' 149.7(4) . . . . ?
O1' S1' N1' C7' -171.5(4) . . . . ?
C1 S1 N1 C7 -73.2(4) . . . . ?
C1 C6 C5 C4 -0.4(7) . . . . ?
C1 C2 C3 C4 0.5(7) . . . . ?
O3' C9' C8' C7' 0.0(5) . . . . ?
N2 C4 C5 C6 -177.2(4) . . . . ?
N2 C4 C3 C2 177.2(4) . . . . ?
C2' C1' C6' C5' 1.0(7) . . . . ?
O1 S1 C1 C6 -148.4(4) . . . . ?
O1 S1 C1 C2 31.1(4) . . . . ?
O1 S1 N1 C7 172.3(4) . . . . ?
C1' S1' N1' C7' 74.0(4) . . . . ?
C1' C2' C3' C4' -0.2(8) . . . . ?
N1 S1 C1 C6 99.9(4) . . . . ?
N1 S1 C1 C2 -80.6(4) . . . . ?
N1 C7 C8 C9 -175.2(4) . . . . ?
N1 C7 N3 O3 175.8(4) . . . . ?
N2' C4' C3' C2' -178.7(4) . . . . ?
C7 C8 C9 O3 0.2(5) . . . . ?
C7 C8 C9 C10 177.5(5) . . . . ?
C9' O3' N3' C7' -1.1(5) . . . . ?
N1' S1' C1' C2' 80.6(4) . . . . ?
N1' S1' C1' C6' -98.7(4) . . . . ?
N1' C7' N3' O3' -175.2(4) . . . . ?
N1' C7' C8' C9' 175.1(4) . . . . ?
C5' C4' C3' C2' 1.5(8) . . . . ?
C6 C1 C2 C3 0.5(7) . . . . ?
C4' C5' C6' C1' 0.3(7) . . . . ?
C5 C4 C3 C2 -1.5(8) . . . . ?
C2 C1 C6 C5 -0.6(7) . . . . ?
C6' C5' C4' N2' 178.7(4) . . . . ?
C6' C5' C4' C3' -1.6(7) . . . . ?
N3' O3' C9' C8' 0.7(6) . . . . ?
N3' O3' C9' C10' 178.5(4) . . . . ?
N3' C7' C8' C9' -0.7(5) . . . . ?
C8 C7 N3 O3 0.2(6) . . . . ?
C9 O3 N3 C7 -0.1(5) . . . . ?
C3 C4 C5 C6 1.5(7) . . . . ?
C3' C2' C1' S1' 179.7(4) . . . . ?
C3' C2' C1' C6' -1.1(7) . . . . ?
C8' C7' N3' O3' 1.1(5) . . . . ?
C10' C9' C8' C7' -177.3(5) . . . . ?
N3 O3 C9 C8 0.0(6) . . . . ?
N3 O3 C9 C10 -177.9(4) . . . . ?
N3 C7 C8 C9 -0.2(6) . . . . ?
_iucr_refine_instructions_details
;
TITL SIR2014 run in space group P 21
smxno32med.res
created by SHELXL-2017/1 at 19:33:55 on 17-Jan-2019
CELL 0.71073 5.3927 31.3529 7.8011 90 99.399 90
ZERR 2 0.0004 0.0021 0.0006 0 0.008 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O S
UNIT 40 48 16 24 4
EQIV $1 1+X,+Y,+Z
EQIV $2 +X,+Y,-1+Z
EQIV $3 -1+X,+Y,+Z
SIMU N4
L.S. 10
PLAN 25
HTAB N2' O1'_$2
HTAB N2' O5
HTAB N1' O2'_$3
HTAB C8' N3'_$1
HTAB C8 O2
HTAB C8' O2'
HTAB C10' O3'_$1
BOND $H
CONF
fmap 2
acta
MERG 2
REM
REM
REM
WGHT 0.073400 0.366900
FVAR 6.94632
S1 5 0.773511 0.331559 0.694085 11.00000 0.03717 0.03311 =
0.02548 -0.00170 0.00432 -0.00151
S1' 5 0.648148 0.032321 1.212508 11.00000 0.03605 0.03237 =
0.02658 0.00215 0.00493 0.00006
O2 4 1.014282 0.351368 0.717569 11.00000 0.03821 0.04439 =
0.03940 -0.00537 0.00011 -0.00240
O2' 4 0.888750 0.012480 1.238062 11.00000 0.03536 0.04672 =
0.03916 0.00835 -0.00229 -0.00076
O3 4 0.431741 0.458934 0.412697 11.00000 0.03586 0.05925 =
0.04956 0.01384 0.00121 0.00870
O1' 4 0.571329 0.058520 1.342530 11.00000 0.06626 0.04248 =
0.03325 -0.00443 0.01194 0.00098
C1 1 0.741485 0.302334 0.499622 11.00000 0.03202 0.02800 =
0.02535 0.00136 0.00147 0.00166
O3' 4 0.308210 -0.095538 0.929354 11.00000 0.03460 0.05921 =
0.05328 -0.01616 -0.00183 -0.00580
N2 3 0.672935 0.228818 0.048743 11.00000 0.05216 0.03638 =
0.03206 -0.00584 0.00490 0.00215
AFIX 137
H2A 2 0.516208 0.229892 -0.008602 11.00000 -1.20000
H2B 2 0.711579 0.202006 0.079746 11.00000 -1.20000
H2C 2 0.778254 0.238282 -0.019428 11.00000 -1.20000
AFIX 0
C2' 1 0.435737 0.092623 0.987814 11.00000 0.04642 0.03858 =
0.03465 0.00206 0.01357 0.00985
AFIX 43
H2' 2 0.327075 0.097423 1.066914 11.00000 -1.20000
AFIX 0
O1 4 0.700405 0.304871 0.824587 11.00000 0.06798 0.04654 =
0.03019 0.00476 0.01076 -0.00464
C1' 1 0.620817 0.061979 1.019136 11.00000 0.03429 0.02398 =
0.02489 -0.00109 0.00417 -0.00353
O5' 4 0.760629 0.154908 0.251707 11.00000 0.04065 0.05281 =
0.05982 0.00762 0.00116 -0.00149
N1 3 0.562541 0.368553 0.667060 11.00000 0.03339 0.03484 =
0.04537 -0.00672 0.01326 -0.00243
AFIX 3
H1 2 0.416781 0.357013 0.640060 11.00000 -1.20000
AFIX 0
N2' 3 0.557919 0.133986 0.564810 11.00000 0.05563 0.03548 =
0.02874 0.00321 0.00333 -0.00494
AFIX 137
H2'A 2 0.399358 0.133894 0.510554 11.00000 -1.20000
H2'B 2 0.656814 0.123046 0.495143 11.00000 -1.20000
H2'C 2 0.605214 0.160642 0.592462 11.00000 -1.20000
AFIX 0
N4' 3 0.987070 0.147719 0.296677 11.00000 0.04475 0.02975 =
0.05194 -0.00311 0.00897 -0.00460
C7 1 0.572898 0.405237 0.563969 11.00000 0.03091 0.03492 =
0.02855 -0.00915 0.00541 -0.00012
C9' 1 0.559474 -0.098021 0.955593 11.00000 0.03757 0.03923 =
0.02907 0.00341 0.00954 -0.00191
C4 1 0.693893 0.255538 0.203931 11.00000 0.03926 0.03178 =
0.02433 -0.00287 0.00408 0.00244
O6' 4 1.144944 0.163704 0.223983 11.00000 0.06092 0.07951 =
0.09315 0.00041 0.03446 -0.01818
N1' 3 0.435803 -0.004895 1.180949 11.00000 0.03406 0.03362 =
0.04284 0.00587 0.01639 -0.00070
AFIX 43
H1' 2 0.305588 -0.001918 1.230462 11.00000 -1.20000
AFIX 0
N4 3 0.083504 0.214827 0.765257 11.00000 0.05828 0.03530 =
0.05607 0.00847 0.02305 0.00629
C5' 1 0.758699 0.077501 0.751160 11.00000 0.04443 0.04773 =
0.03219 0.00303 0.01493 0.00473
AFIX 43
H5' 2 0.864763 0.072392 0.670625 11.00000 -1.20000
AFIX 0
C6 1 0.901105 0.310150 0.382051 11.00000 0.03765 0.03655 =
0.03320 -0.00149 0.01039 -0.01113
AFIX 43
H6 2 1.024002 0.331147 0.404063 11.00000 -1.20000
AFIX 0
C7' 1 0.448150 -0.041111 1.080337 11.00000 0.03064 0.03743 =
0.02867 0.00640 0.00868 0.00012
C4' 1 0.578087 0.108516 0.721734 11.00000 0.04053 0.02762 =
0.02957 0.00180 0.00290 -0.00675
C5 1 0.875961 0.286247 0.230225 11.00000 0.03690 0.04375 =
0.03004 -0.00080 0.01043 -0.00572
AFIX 43
H5 2 0.980532 0.291031 0.148456 11.00000 -1.20000
AFIX 0
O5 4 -0.132140 0.200854 0.740098 11.00000 0.07217 0.07971 =
0.06762 -0.02244 0.01543 -0.02802
C2 1 0.556814 0.271739 0.469667 11.00000 0.03869 0.03658 =
0.03423 -0.00129 0.01476 -0.00643
AFIX 43
H2 2 0.450036 0.267106 0.550145 11.00000 -1.20000
AFIX 0
C6' 1 0.780841 0.053864 0.902829 11.00000 0.03845 0.04416 =
0.03826 0.00747 0.01088 0.00921
AFIX 43
H6' 2 0.902711 0.032722 0.925741 11.00000 -1.20000
AFIX 0
N3' 3 0.237618 -0.058286 1.008850 11.00000 0.02850 0.05596 =
0.05278 -0.01159 0.00022 0.00179
C8 1 0.781623 0.428925 0.533388 11.00000 0.02836 0.03910 =
0.04031 0.00313 0.00431 0.00202
AFIX 43
H8 2 0.950804 0.423006 0.570747 11.00000 -1.20000
AFIX 0
C9 1 0.682414 0.461717 0.438940 11.00000 0.03788 0.03862 =
0.03461 -0.00191 0.00705 0.00326
O4 4 0.148324 0.236255 0.901152 11.00000 0.05579 0.06992 =
0.06981 -0.01428 -0.00046 -0.00170
C3 1 0.531611 0.247984 0.318927 11.00000 0.04262 0.03377 =
0.03839 -0.00473 0.00794 -0.00927
AFIX 43
H3 2 0.407180 0.227276 0.295731 11.00000 -1.20000
AFIX 0
C3' 1 0.415507 0.115927 0.836928 11.00000 0.05065 0.03573 =
0.04270 0.00755 0.01100 0.01463
AFIX 43
H3' 2 0.291723 0.136718 0.812807 11.00000 -1.20000
AFIX 0
C10 1 0.791651 0.499961 0.366187 11.00000 0.05839 0.04740 =
0.04291 0.00739 0.00828 -0.00207
AFIX 137
H10A 2 0.778141 0.524096 0.439826 11.00000 -1.50000
H10B 2 0.701829 0.505662 0.251807 11.00000 -1.50000
H10C 2 0.965429 0.494786 0.360012 11.00000 -1.50000
AFIX 0
O4' 4 1.047846 0.123379 0.424134 11.00000 0.05886 0.06537 =
0.08198 0.02510 -0.00514 -0.00042
C8' 1 0.658691 -0.064696 1.049879 11.00000 0.02892 0.03676 =
0.03843 0.00073 0.00665 -0.00328
AFIX 43
H8' 2 0.827689 -0.058543 1.086752 11.00000 -1.20000
AFIX 0
C10' 1 0.669452 -0.135869 0.884887 11.00000 0.05497 0.04467 =
0.04197 -0.01209 0.01041 -0.00006
AFIX 137
H10D 2 0.596716 -0.139441 0.764976 11.00000 -1.50000
H10E 2 0.635436 -0.160676 0.949353 11.00000 -1.50000
H10F 2 0.847860 -0.132151 0.894264 11.00000 -1.50000
AFIX 0
N3 3 0.362916 0.421951 0.495151 11.00000 0.03197 0.05812 =
0.05703 0.01137 0.00394 -0.00056
O6 4 0.232967 0.208081 0.666424 11.00000 0.14334 0.06291 =
0.15184 0.00732 0.11522 0.01158
HKLF 4
REM SIR2014 run in space group P 21
REM R1 = 0.0503 for 5606 Fo > 4sig(Fo) and 0.0565 for all 6269 data
REM 383 parameters refined using 1 restraints
END
WGHT 0.0734 0.3669
REM Highest difference peak 0.764, deepest hole -0.270, 1-sigma level 0.064
Q1 1 0.2873 0.3308 0.6968 11.00000 0.05 0.76
Q2 1 0.1920 0.0317 1.2135 11.00000 0.05 0.74
Q3 1 0.3498 0.0173 1.2386 11.00000 0.05 0.32
Q4 1 0.4692 0.3507 0.7180 11.00000 0.05 0.31
Q5 1 0.1315 0.0619 1.0232 11.00000 0.05 0.30
Q6 1 0.9528 0.3325 0.6992 11.00000 0.05 0.28
Q7 1 0.0677 0.1094 0.7183 11.00000 0.05 0.28
Q8 1 0.5094 0.1490 0.2860 11.00000 0.05 0.28
Q9 1 1.0856 0.4610 0.4043 11.00000 0.05 0.26
Q10 1 -0.0812 0.2095 0.6592 11.00000 0.05 0.26
Q11 1 0.2819 0.0011 1.1714 11.00000 0.05 0.25
Q12 1 0.2472 0.3016 0.4960 11.00000 0.05 0.25
Q13 1 0.9440 0.5088 0.4431 11.00000 0.05 0.25
Q14 1 0.8113 0.0309 1.2273 11.00000 0.05 0.25
Q15 1 0.9198 0.4187 0.5039 11.00000 0.05 0.24
Q16 1 0.9883 0.3019 0.8421 11.00000 0.05 0.23
Q17 1 1.0354 0.1336 0.5721 11.00000 0.05 0.23
Q18 1 0.1895 0.2518 0.2202 11.00000 0.05 0.23
Q19 1 0.2388 0.4294 0.5454 11.00000 0.05 0.23
Q20 1 0.8104 -0.0539 1.0280 11.00000 0.05 0.23
Q21 1 0.3601 0.3080 0.8170 11.00000 0.05 0.23
Q22 1 0.0705 0.2297 1.0461 11.00000 0.05 0.22
Q23 1 0.1247 -0.0650 1.0540 11.00000 0.05 0.22
Q24 1 0.8678 -0.0071 1.1659 11.00000 0.05 0.22
Q25 1 0.9439 -0.1011 0.9228 11.00000 0.05 0.22
REM The information below was added by Olex2.
REM
REM R1 = 0.0503 for 5606 Fo > 4sig(Fo) and 0.0565 for all 17143 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.76, deepest hole -0.27
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0565
REM R1_gt = 0.0503
REM wR_ref = 0.1364
REM GOOF = 1.075
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 17143
REM Reflections_gt = 5606
REM Parameters = n/a
REM Hole = -0.27
REM Peak = 0.76
REM Flack = 0.17(4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.631