# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_170411_d_ph_a
_audit_block_doi 10.5517/ccdc.csd.cc1p2ms5
_database_code_depnum_ccdc_archive 'CCDC 1551667'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7RA10432D 2017
_audit_update_record
;
2017-05-23 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;
_audit_creation_date 2017-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C21 H18 N2 S'
_chemical_formula_sum 'C21 H18 N2 S'
_chemical_formula_weight 330.43
_chemical_melting_point ?
_chemical_oxdiff_formula 'c10 h10 n2 o8 s1'
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'
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/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 6.1982(5)
_cell_length_b 24.956(2)
_cell_length_c 10.8550(9)
_cell_angle_alpha 90
_cell_angle_beta 97.234(8)
_cell_angle_gamma 90
_cell_volume 1665.7(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2707
_cell_measurement_temperature 170
_cell_measurement_theta_max 29.3250
_cell_measurement_theta_min 3.3065
_shelx_estimated_absorpt_T_max 0.943
_shelx_estimated_absorpt_T_min 0.920
_exptl_absorpt_coefficient_mu 0.198
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.76556
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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 1.318
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 696
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.3
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0613
_diffrn_reflns_av_unetI/netI 0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 6861
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 3.313
_diffrn_ambient_temperature 170
_diffrn_detector_area_resol_mean 5.1796
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -86.00 21.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- -11.4683 -77.0000 90.0000 107
#__ type_ start__ end____ width___ exp.time_
2 omega -8.00 74.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 11.9371 38.0000 30.0000 82
;
_diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0068740000
_diffrn_orient_matrix_UB_12 0.0025616000
_diffrn_orient_matrix_UB_13 -0.0654313000
_diffrn_orient_matrix_UB_21 0.0128354000
_diffrn_orient_matrix_UB_22 0.0281544000
_diffrn_orient_matrix_UB_23 0.0063558000
_diffrn_orient_matrix_UB_31 0.1144423000
_diffrn_orient_matrix_UB_32 -0.0029921000
_diffrn_orient_matrix_UB_33 0.0036992000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2445
_reflns_number_total 3045
_reflns_odcompleteness_completeness 99.63
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.316
_refine_diff_density_min -0.281
_refine_diff_density_rms 0.060
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 219
_refine_ls_number_reflns 3045
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0741
_refine_ls_R_factor_gt 0.0592
_refine_ls_restrained_S_all 1.079
_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^)+(0.0648P)^2^+0.4976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1420
_refine_ls_wR_factor_ref 0.1526
_refine_special_details ?
_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:
C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
C15(H15), C16(H16), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_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
S1 S 0.02907(11) 0.31705(3) 0.39099(6) 0.0302(2) Uani 1 1 d . . . . .
N1 N 0.1062(3) 0.41466(9) 0.46596(19) 0.0302(5) Uani 1 1 d . . . . .
N2 N 0.1095(4) 0.10184(9) 0.4428(2) 0.0354(6) Uani 1 1 d . . . . .
C1 C -0.3596(4) 0.36027(12) 0.2645(2) 0.0349(6) Uani 1 1 d . . . . .
H1 H -0.406559 0.326525 0.230563 0.042 Uiso 1 1 calc R . . . .
C2 C -0.4855(4) 0.40549(12) 0.2404(2) 0.0370(7) Uani 1 1 d . . . . .
H2 H -0.621604 0.402730 0.189715 0.044 Uiso 1 1 calc R . . . .
C3 C -0.4168(4) 0.45528(12) 0.2893(3) 0.0382(7) Uani 1 1 d . . . . .
H3 H -0.506611 0.485818 0.271068 0.046 Uiso 1 1 calc R . . . .
C4 C -0.2207(4) 0.46082(12) 0.3636(3) 0.0363(7) Uani 1 1 d . . . . .
H4 H -0.174307 0.494816 0.396243 0.044 Uiso 1 1 calc R . . . .
C5 C -0.0917(4) 0.41539(11) 0.3897(2) 0.0285(6) Uani 1 1 d . . . . .
C6 C -0.1616(4) 0.36543(11) 0.3398(2) 0.0281(6) Uani 1 1 d . . . . .
C7 C 0.1870(4) 0.36648(11) 0.4747(2) 0.0273(6) Uani 1 1 d . . . . .
C8 C 0.4002(4) 0.35619(11) 0.5499(2) 0.0276(6) Uani 1 1 d . . . . .
C9 C 0.5182(4) 0.40153(11) 0.5943(2) 0.0317(6) Uani 1 1 d . . . . .
H9 H 0.457371 0.436053 0.576765 0.038 Uiso 1 1 calc R . . . .
C10 C 0.7207(4) 0.39735(12) 0.6631(2) 0.0364(7) Uani 1 1 d . . . . .
H10 H 0.797640 0.428640 0.692801 0.044 Uiso 1 1 calc R . . . .
C11 C 0.8105(4) 0.34709(12) 0.6883(2) 0.0358(7) Uani 1 1 d . . . . .
H11 H 0.949861 0.343772 0.735313 0.043 Uiso 1 1 calc R . . . .
C12 C 0.6972(4) 0.30190(12) 0.6451(2) 0.0326(6) Uani 1 1 d . . . . .
H12 H 0.760807 0.267669 0.662657 0.039 Uiso 1 1 calc R . . . .
C13 C 0.4910(4) 0.30515(11) 0.5762(2) 0.0279(6) Uani 1 1 d . . . . .
C14 C 0.3825(4) 0.25368(11) 0.5357(2) 0.0278(6) Uani 1 1 d . . . . .
C15 C 0.4600(4) 0.22166(11) 0.4461(2) 0.0331(6) Uani 1 1 d . . . . .
H15 H 0.577313 0.234335 0.405654 0.040 Uiso 1 1 calc R . . . .
C16 C 0.3717(4) 0.17196(11) 0.4141(2) 0.0329(6) Uani 1 1 d . . . . .
H16 H 0.428186 0.151276 0.352064 0.039 Uiso 1 1 calc R . . . .
C17 C 0.1986(4) 0.15175(11) 0.4728(2) 0.0283(6) Uani 1 1 d . . . . .
C18 C 0.1192(4) 0.18425(11) 0.5623(2) 0.0307(6) Uani 1 1 d . . . . .
H18 H 0.000029 0.172222 0.602056 0.037 Uiso 1 1 calc R . . . .
C19 C 0.2119(4) 0.23347(11) 0.5935(2) 0.0311(6) Uani 1 1 d . . . . .
H19 H 0.157408 0.254154 0.656241 0.037 Uiso 1 1 calc R . . . .
C20 C 0.2263(5) 0.06401(12) 0.3757(3) 0.0485(8) Uani 1 1 d . . . . .
H20A H 0.237011 0.077835 0.292181 0.073 Uiso 1 1 calc GR . . . .
H20B H 0.148712 0.029710 0.369447 0.073 Uiso 1 1 calc GR . . . .
H20C H 0.372696 0.058760 0.419855 0.073 Uiso 1 1 calc GR . . . .
C21 C -0.0707(5) 0.08241(12) 0.5027(3) 0.0436(7) Uani 1 1 d . . . . .
H21A H -0.020110 0.074186 0.589832 0.065 Uiso 1 1 calc GR . . . .
H21B H -0.130059 0.049921 0.460502 0.065 Uiso 1 1 calc GR . . . .
H21C H -0.184059 0.109962 0.498387 0.065 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
S1 0.0320(4) 0.0292(4) 0.0288(4) -0.0035(3) 0.0013(3) 0.0023(3)
N1 0.0257(11) 0.0299(13) 0.0346(12) -0.0005(9) 0.0020(9) -0.0002(10)
N2 0.0399(13) 0.0315(14) 0.0363(12) -0.0015(10) 0.0113(10) -0.0014(11)
C1 0.0357(15) 0.0366(17) 0.0315(14) -0.0063(12) 0.0011(11) -0.0015(13)
C2 0.0290(14) 0.0454(19) 0.0348(15) -0.0007(12) -0.0032(12) 0.0012(13)
C3 0.0360(15) 0.0354(17) 0.0415(16) 0.0040(12) -0.0015(12) 0.0051(13)
C4 0.0379(15) 0.0321(17) 0.0379(15) -0.0008(12) 0.0013(12) -0.0022(13)
C5 0.0277(13) 0.0283(15) 0.0302(13) 0.0006(11) 0.0060(11) -0.0007(11)
C6 0.0293(13) 0.0319(16) 0.0241(13) 0.0008(10) 0.0069(10) 0.0013(11)
C7 0.0284(13) 0.0305(16) 0.0244(13) -0.0011(10) 0.0087(10) -0.0030(12)
C8 0.0243(12) 0.0354(16) 0.0241(12) -0.0029(11) 0.0076(10) -0.0022(11)
C9 0.0291(14) 0.0320(16) 0.0350(14) -0.0052(11) 0.0075(11) 0.0007(12)
C10 0.0310(15) 0.0420(18) 0.0359(15) -0.0062(12) 0.0030(12) -0.0026(13)
C11 0.0267(14) 0.0461(19) 0.0346(15) -0.0031(12) 0.0038(11) 0.0003(13)
C12 0.0306(14) 0.0378(17) 0.0306(14) 0.0020(12) 0.0089(11) 0.0057(12)
C13 0.0258(13) 0.0352(16) 0.0243(13) 0.0006(11) 0.0089(10) 0.0034(12)
C14 0.0258(13) 0.0324(15) 0.0254(13) 0.0023(11) 0.0044(10) 0.0064(11)
C15 0.0283(13) 0.0370(17) 0.0355(15) 0.0041(12) 0.0098(11) 0.0016(12)
C16 0.0316(14) 0.0392(17) 0.0294(14) -0.0019(11) 0.0094(11) 0.0045(12)
C17 0.0301(13) 0.0279(15) 0.0265(13) 0.0043(10) 0.0023(10) 0.0064(11)
C18 0.0278(13) 0.0372(17) 0.0284(14) 0.0035(11) 0.0079(11) 0.0017(12)
C19 0.0296(13) 0.0342(16) 0.0302(14) -0.0003(11) 0.0070(11) 0.0037(12)
C20 0.0554(19) 0.0389(19) 0.0534(19) -0.0065(15) 0.0155(15) -0.0018(16)
C21 0.0403(16) 0.0434(19) 0.0478(18) -0.0013(14) 0.0085(13) -0.0066(14)
_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 C6 1.731(3) . ?
S1 C7 1.755(3) . ?
N1 C5 1.391(3) . ?
N1 C7 1.301(3) . ?
N2 C17 1.385(3) . ?
N2 C20 1.442(4) . ?
N2 C21 1.445(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.378(4) . ?
C1 C6 1.392(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.396(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.396(4) . ?
C5 C6 1.406(4) . ?
C7 C8 1.486(4) . ?
C8 C9 1.400(4) . ?
C8 C13 1.407(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.381(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.400(4) . ?
C13 C14 1.490(4) . ?
C14 C15 1.390(4) . ?
C14 C19 1.390(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.408(3) . ?
C17 C18 1.402(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.380(4) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
C6 S1 C7 89.40(13) . . ?
C7 N1 C5 111.0(2) . . ?
C17 N2 C20 119.8(2) . . ?
C17 N2 C21 120.3(2) . . ?
C20 N2 C21 118.3(2) . . ?
C2 C1 H1 120.9 . . ?
C2 C1 C6 118.1(3) . . ?
C6 C1 H1 120.9 . . ?
C1 C2 H2 119.4 . . ?
C1 C2 C3 121.2(3) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.5(3) . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 124.8(2) . . ?
N1 C5 C6 115.1(2) . . ?
C4 C5 C6 120.1(2) . . ?
C1 C6 S1 129.8(2) . . ?
C1 C6 C5 121.0(2) . . ?
C5 C6 S1 109.27(19) . . ?
N1 C7 S1 115.30(19) . . ?
N1 C7 C8 120.5(2) . . ?
C8 C7 S1 124.2(2) . . ?
C9 C8 C7 116.1(2) . . ?
C9 C8 C13 119.0(2) . . ?
C13 C8 C7 125.0(2) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 C8 121.7(3) . . ?
C10 C9 H9 119.2 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.4(3) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.1 . . ?
C11 C12 C13 121.7(3) . . ?
C13 C12 H12 119.1 . . ?
C8 C13 C14 124.5(2) . . ?
C12 C13 C8 118.4(3) . . ?
C12 C13 C14 117.1(2) . . ?
C15 C14 C13 121.2(2) . . ?
C19 C14 C13 121.4(2) . . ?
C19 C14 C15 117.2(3) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 122.1(2) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.5(2) . . ?
C17 C16 H16 119.7 . . ?
N2 C17 C16 121.3(2) . . ?
N2 C17 C18 121.3(2) . . ?
C18 C17 C16 117.4(3) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 120.9(2) . . ?
C19 C18 H18 119.5 . . ?
C14 C19 H19 119.0 . . ?
C18 C19 C14 121.9(2) . . ?
C18 C19 H19 119.0 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
_shelx_res_file
;
TITL 170411_D_Ph_A in P21/c #14
170411_d_ph_a.res
created by SHELXL-2016/6 at 11:38:00 on 11-Apr-2017
REM reset to P21/c #14
CELL 0.71073 6.19824 24.95626 10.85499 90 97.2345 90
ZERR 4 0.00046 0.00222 0.00088 0 0.0078 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N S
UNIT 84 72 8 4
L.S. 4
PLAN 20
SIZE 0.43 0.4 0.3
TEMP -103.15
BOND $h
htab
fmap 2
acta
SHEL 999 0.83
REM
REM
REM
WGHT 0.064800 0.497600
FVAR 7.57911
S1 4 0.029067 0.317049 0.390993 11.00000 0.03204 0.02921 =
0.02883 -0.00352 0.00129 0.00227
N1 3 0.106194 0.414664 0.465962 11.00000 0.02571 0.02989 =
0.03456 -0.00054 0.00203 -0.00017
N2 3 0.109467 0.101840 0.442790 11.00000 0.03986 0.03155 =
0.03632 -0.00151 0.01134 -0.00143
C1 1 -0.359594 0.360272 0.264468 11.00000 0.03571 0.03658 =
0.03147 -0.00627 0.00109 -0.00147
AFIX 43
H1 2 -0.406559 0.326525 0.230563 11.00000 -1.20000
AFIX 0
C2 1 -0.485517 0.405485 0.240448 11.00000 0.02905 0.04544 =
0.03476 -0.00066 -0.00321 0.00123
AFIX 43
H2 2 -0.621604 0.402730 0.189715 11.00000 -1.20000
AFIX 0
C3 1 -0.416769 0.455276 0.289306 11.00000 0.03597 0.03541 =
0.04155 0.00402 -0.00147 0.00511
AFIX 43
H3 2 -0.506611 0.485818 0.271068 11.00000 -1.20000
AFIX 0
C4 1 -0.220658 0.460820 0.363565 11.00000 0.03786 0.03215 =
0.03793 -0.00082 0.00133 -0.00222
AFIX 43
H4 2 -0.174307 0.494816 0.396243 11.00000 -1.20000
AFIX 0
C5 1 -0.091667 0.415393 0.389697 11.00000 0.02770 0.02833 =
0.03018 0.00057 0.00597 -0.00070
C6 1 -0.161607 0.365432 0.339816 11.00000 0.02927 0.03194 =
0.02410 0.00077 0.00686 0.00128
C7 1 0.186974 0.366480 0.474697 11.00000 0.02842 0.03048 =
0.02437 -0.00112 0.00872 -0.00299
C8 1 0.400227 0.356186 0.549912 11.00000 0.02435 0.03544 =
0.02412 -0.00293 0.00759 -0.00217
C9 1 0.518151 0.401531 0.594342 11.00000 0.02913 0.03198 =
0.03498 -0.00518 0.00751 0.00071
AFIX 43
H9 2 0.457371 0.436053 0.576765 11.00000 -1.20000
AFIX 0
C10 1 0.720661 0.397354 0.663096 11.00000 0.03100 0.04203 =
0.03585 -0.00623 0.00304 -0.00256
AFIX 43
H10 2 0.797640 0.428640 0.692801 11.00000 -1.20000
AFIX 0
C11 1 0.810468 0.347095 0.688328 11.00000 0.02673 0.04612 =
0.03461 -0.00312 0.00379 0.00035
AFIX 43
H11 2 0.949861 0.343772 0.735313 11.00000 -1.20000
AFIX 0
C12 1 0.697219 0.301902 0.645142 11.00000 0.03060 0.03783 =
0.03060 0.00195 0.00893 0.00570
AFIX 43
H12 2 0.760807 0.267669 0.662657 11.00000 -1.20000
AFIX 0
C13 1 0.490978 0.305147 0.576158 11.00000 0.02576 0.03519 =
0.02425 0.00063 0.00888 0.00336
C14 1 0.382475 0.253678 0.535750 11.00000 0.02579 0.03236 =
0.02544 0.00230 0.00442 0.00641
C15 1 0.459993 0.221661 0.446144 11.00000 0.02832 0.03699 =
0.03546 0.00407 0.00982 0.00159
AFIX 43
H15 2 0.577313 0.234335 0.405654 11.00000 -1.20000
AFIX 0
C16 1 0.371668 0.171957 0.414133 11.00000 0.03158 0.03918 =
0.02939 -0.00188 0.00940 0.00450
AFIX 43
H16 2 0.428186 0.151276 0.352064 11.00000 -1.20000
AFIX 0
C17 1 0.198630 0.151745 0.472782 11.00000 0.03012 0.02785 =
0.02652 0.00433 0.00228 0.00639
C18 1 0.119235 0.184246 0.562302 11.00000 0.02778 0.03715 =
0.02837 0.00353 0.00790 0.00167
AFIX 43
H18 2 0.000029 0.172222 0.602056 11.00000 -1.20000
AFIX 0
C19 1 0.211854 0.233468 0.593476 11.00000 0.02961 0.03424 =
0.03017 -0.00033 0.00698 0.00373
AFIX 43
H19 2 0.157408 0.254154 0.656241 11.00000 -1.20000
AFIX 0
C20 1 0.226333 0.064005 0.375693 11.00000 0.05543 0.03886 =
0.05335 -0.00649 0.01550 -0.00177
AFIX 137
H20A 2 0.237011 0.077835 0.292181 11.00000 -1.50000
H20B 2 0.148712 0.029710 0.369447 11.00000 -1.50000
H20C 2 0.372696 0.058760 0.419855 11.00000 -1.50000
AFIX 0
C21 1 -0.070679 0.082415 0.502696 11.00000 0.04030 0.04344 =
0.04784 -0.00127 0.00855 -0.00655
AFIX 137
H21A 2 -0.020110 0.074186 0.589832 11.00000 -1.50000
H21B 2 -0.130059 0.049921 0.460502 11.00000 -1.50000
H21C 2 -0.184059 0.109962 0.498387 11.00000 -1.50000
AFIX 0
HKLF 4
REM 170411_D_Ph_A in P21/c #14
REM R1 = 0.0592 for 2445 Fo > 4sig(Fo) and 0.0741 for all 3045 data
REM 219 parameters refined using 0 restraints
END
WGHT 0.0648 0.4955
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.316, deepest hole -0.281, 1-sigma level 0.060
Q1 1 0.1835 0.3170 0.3867 11.00000 0.05 0.32
Q2 1 -0.0728 0.3188 0.4753 11.00000 0.05 0.29
Q3 1 0.3684 0.0727 0.3401 11.00000 0.05 0.28
Q4 1 0.1413 0.3132 0.2988 11.00000 0.05 0.24
Q5 1 -0.1462 0.3213 0.3809 11.00000 0.05 0.22
Q6 1 0.3055 0.0665 0.5446 11.00000 0.05 0.22
Q7 1 0.6277 0.3053 0.5738 11.00000 0.05 0.21
Q8 1 0.2048 0.1811 0.4646 11.00000 0.05 0.21
Q9 1 0.6257 0.3949 0.5935 11.00000 0.05 0.20
Q10 1 0.0184 0.2719 0.3822 11.00000 0.05 0.20
Q11 1 0.5276 0.1431 0.2447 11.00000 0.05 0.19
Q12 1 0.7688 0.2479 0.6242 11.00000 0.05 0.19
Q13 1 0.2022 0.3917 0.4535 11.00000 0.05 0.19
Q14 1 -0.3587 0.3128 0.1207 11.00000 0.05 0.18
Q15 1 0.4523 0.3364 0.5727 11.00000 0.05 0.18
Q16 1 -0.0770 0.2077 0.4639 11.00000 0.05 0.18
Q17 1 0.9583 0.3420 0.6843 11.00000 0.05 0.18
Q18 1 0.2364 0.2638 0.6905 11.00000 0.05 0.18
Q19 1 0.3925 0.2882 0.5380 11.00000 0.05 0.18
Q20 1 -0.0017 0.4088 0.2919 11.00000 0.05 0.18
;
_shelx_res_checksum 10339
_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_180124_xiamin_4
_database_code_depnum_ccdc_archive 'CCDC 1834423'
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;
_audit_creation_date 2018-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H22 N2 S'
_chemical_formula_sum 'C27 H22 N2 S'
_chemical_formula_weight 406.52
_chemical_melting_point ?
_chemical_oxdiff_formula 'C H N O s'
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'
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/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 10.7946(7)
_cell_length_b 7.7940(6)
_cell_length_c 25.0193(18)
_cell_angle_alpha 90
_cell_angle_beta 96.088(6)
_cell_angle_gamma 90
_cell_volume 2093.1(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2160
_cell_measurement_temperature 180
_cell_measurement_theta_max 29.3824
_cell_measurement_theta_min 3.2237
_shelx_estimated_absorpt_T_max 0.941
_shelx_estimated_absorpt_T_min 0.922
_exptl_absorpt_coefficient_mu 0.171
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.93616
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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 1.290
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 856
_exptl_crystal_size_max 0.48
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.36
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0363
_diffrn_reflns_av_unetI/netI 0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 8101
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.348
_diffrn_reflns_theta_min 3.230
_diffrn_ambient_temperature 180
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -44.00 60.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -11.4683 77.0000 120.0000 104
#__ type_ start__ end____ width___ exp.time_
2 omega -17.00 59.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 11.7808 77.0000 30.0000 76
;
_diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0168847000
_diffrn_orient_matrix_UB_12 -0.0079210000
_diffrn_orient_matrix_UB_13 0.0265316000
_diffrn_orient_matrix_UB_21 -0.0176172000
_diffrn_orient_matrix_UB_22 0.0876392000
_diffrn_orient_matrix_UB_23 -0.0003153000
_diffrn_orient_matrix_UB_31 -0.0614603000
_diffrn_orient_matrix_UB_32 -0.0229779000
_diffrn_orient_matrix_UB_33 -0.0104217000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2919
_reflns_number_total 3809
_reflns_odcompleteness_completeness 99.59
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.223
_refine_diff_density_min -0.301
_refine_diff_density_rms 0.046
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 273
_refine_ls_number_reflns 3809
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0618
_refine_ls_R_factor_gt 0.0425
_refine_ls_restrained_S_all 1.016
_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^)+(0.0413P)^2^+0.4468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0926
_refine_ls_wR_factor_ref 0.1056
_refine_special_details ?
_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:
C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C13(H13),
C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_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
S1 S 0.52239(4) 0.34484(7) 0.24748(2) 0.03064(16) Uani 1 1 d . . . . .
N1 N 0.67369(14) 0.5396(2) 0.20067(6) 0.0293(4) Uani 1 1 d . . . . .
N2 N 0.32289(16) 0.0082(2) -0.11734(7) 0.0387(5) Uani 1 1 d . . . . .
C1 C 0.70627(19) 0.3600(3) 0.33649(8) 0.0336(5) Uani 1 1 d . . . . .
H1 H 0.659211 0.289524 0.357827 0.040 Uiso 1 1 calc R . . . .
C2 C 0.82103(19) 0.4247(3) 0.35647(8) 0.0364(5) Uani 1 1 d . . . . .
H2 H 0.854231 0.396680 0.392085 0.044 Uiso 1 1 calc R . . . .
C3 C 0.88882(19) 0.5300(3) 0.32552(8) 0.0381(5) Uani 1 1 d . . . . .
H3 H 0.966746 0.574376 0.340613 0.046 Uiso 1 1 calc R . . . .
C4 C 0.84549(18) 0.5711(3) 0.27360(8) 0.0359(5) Uani 1 1 d . . . . .
H4 H 0.893006 0.642227 0.252629 0.043 Uiso 1 1 calc R . . . .
C5 C 0.73001(17) 0.5064(3) 0.25211(8) 0.0284(5) Uani 1 1 d . . . . .
C6 C 0.66230(17) 0.4023(3) 0.28374(8) 0.0273(5) Uani 1 1 d . . . . .
C7 C 0.56528(17) 0.4661(2) 0.19335(7) 0.0247(4) Uani 1 1 d . . . . .
C8 C 0.47920(17) 0.4854(2) 0.14404(7) 0.0247(4) Uani 1 1 d . . . . .
C9 C 0.51959(18) 0.5697(3) 0.09994(8) 0.0285(5) Uani 1 1 d . . . . .
H9 H 0.602953 0.609850 0.101291 0.034 Uiso 1 1 calc R . . . .
C10 C 0.43765(18) 0.5946(3) 0.05412(8) 0.0308(5) Uani 1 1 d . . . . .
H10 H 0.464800 0.653072 0.024143 0.037 Uiso 1 1 calc R . . . .
C11 C 0.31611(18) 0.5347(3) 0.05177(8) 0.0300(5) Uani 1 1 d . . . . .
H11 H 0.261156 0.551546 0.019958 0.036 Uiso 1 1 calc R . . . .
C12 C 0.27356(17) 0.4505(2) 0.09533(7) 0.0254(4) Uani 1 1 d . . . . .
C13 C 0.35627(17) 0.4259(2) 0.14126(7) 0.0254(4) Uani 1 1 d . . . . .
H13 H 0.328854 0.367885 0.171251 0.031 Uiso 1 1 calc R . . . .
C14 C 0.14024(17) 0.3976(3) 0.09468(7) 0.0258(4) Uani 1 1 d . . . . .
C15 C 0.07871(17) 0.2978(2) 0.05294(7) 0.0254(4) Uani 1 1 d . . . . .
C16 C -0.04840(17) 0.2654(3) 0.05393(8) 0.0302(5) Uani 1 1 d . . . . .
H16 H -0.091052 0.198503 0.026032 0.036 Uiso 1 1 calc R . . . .
C17 C -0.11383(18) 0.3280(3) 0.09444(8) 0.0328(5) Uani 1 1 d . . . . .
H17 H -0.200587 0.306201 0.093686 0.039 Uiso 1 1 calc R . . . .
C18 C -0.05279(19) 0.4221(3) 0.13591(8) 0.0347(5) Uani 1 1 d . . . . .
H18 H -0.096758 0.463191 0.164266 0.042 Uiso 1 1 calc R . . . .
C19 C 0.07332(18) 0.4563(3) 0.13585(8) 0.0308(5) Uani 1 1 d . . . . .
H19 H 0.115091 0.521180 0.164453 0.037 Uiso 1 1 calc R . . . .
C20 C 0.14404(16) 0.2232(2) 0.00923(7) 0.0260(4) Uani 1 1 d . . . . .
C21 C 0.25433(17) 0.1304(3) 0.01888(8) 0.0289(5) Uani 1 1 d . . . . .
H21 H 0.290422 0.115715 0.054898 0.035 Uiso 1 1 calc R . . . .
C22 C 0.31270(18) 0.0591(3) -0.02209(8) 0.0311(5) Uani 1 1 d . . . . .
H22 H 0.387429 -0.004177 -0.013683 0.037 Uiso 1 1 calc R . . . .
C23 C 0.26402(18) 0.0782(3) -0.07613(8) 0.0295(5) Uani 1 1 d . . . . .
C24 C 0.15340(18) 0.1712(3) -0.08589(8) 0.0310(5) Uani 1 1 d . . . . .
H24 H 0.117479 0.187400 -0.121866 0.037 Uiso 1 1 calc R . . . .
C25 C 0.09518(17) 0.2403(3) -0.04428(7) 0.0290(5) Uani 1 1 d . . . . .
H25 H 0.019360 0.301355 -0.052423 0.035 Uiso 1 1 calc R . . . .
C26 C 0.44384(19) -0.0679(3) -0.10615(9) 0.0418(6) Uani 1 1 d . . . . .
H26A H 0.437188 -0.172963 -0.085143 0.063 Uiso 1 1 calc GR . . . .
H26B H 0.499754 0.013103 -0.085630 0.063 Uiso 1 1 calc GR . . . .
H26C H 0.477220 -0.095724 -0.140034 0.063 Uiso 1 1 calc GR . . . .
C27 C 0.2653(2) 0.0118(3) -0.17190(8) 0.0428(6) Uani 1 1 d . . . . .
H27A H 0.259026 0.130753 -0.184577 0.064 Uiso 1 1 calc GR . . . .
H27B H 0.181722 -0.038393 -0.173450 0.064 Uiso 1 1 calc GR . . . .
H27C H 0.315818 -0.054571 -0.194816 0.064 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
S1 0.0261(3) 0.0336(3) 0.0319(3) 0.0039(2) 0.0019(2) -0.0052(2)
N1 0.0232(9) 0.0344(10) 0.0304(9) -0.0024(8) 0.0032(7) -0.0027(8)
N2 0.0322(10) 0.0474(12) 0.0372(10) -0.0080(9) 0.0065(8) 0.0051(9)
C1 0.0353(12) 0.0334(12) 0.0319(11) 0.0008(10) 0.0034(9) 0.0040(10)
C2 0.0374(12) 0.0351(12) 0.0346(12) -0.0039(10) -0.0061(10) 0.0070(10)
C3 0.0281(11) 0.0438(14) 0.0403(12) -0.0076(11) -0.0053(10) -0.0005(10)
C4 0.0282(11) 0.0425(13) 0.0369(12) -0.0038(11) 0.0023(9) -0.0055(10)
C5 0.0252(10) 0.0300(11) 0.0301(11) -0.0058(9) 0.0027(8) 0.0015(9)
C6 0.0234(10) 0.0262(11) 0.0322(11) -0.0035(9) 0.0023(8) 0.0020(9)
C7 0.0243(10) 0.0225(10) 0.0282(10) -0.0032(9) 0.0070(8) 0.0001(8)
C8 0.0251(10) 0.0232(10) 0.0262(10) -0.0041(9) 0.0046(8) 0.0015(8)
C9 0.0240(10) 0.0290(11) 0.0329(11) -0.0022(9) 0.0056(8) -0.0017(9)
C10 0.0348(12) 0.0308(12) 0.0282(10) 0.0014(9) 0.0094(9) -0.0022(10)
C11 0.0325(11) 0.0314(12) 0.0256(10) -0.0015(9) 0.0012(9) -0.0020(9)
C12 0.0252(10) 0.0238(10) 0.0278(10) -0.0026(9) 0.0046(8) 0.0006(9)
C13 0.0263(10) 0.0244(10) 0.0261(10) -0.0013(9) 0.0051(8) 0.0000(9)
C14 0.0237(10) 0.0265(11) 0.0271(10) 0.0021(9) 0.0013(8) 0.0011(9)
C15 0.0215(10) 0.0258(11) 0.0284(10) 0.0034(9) 0.0003(8) 0.0020(8)
C16 0.0241(10) 0.0307(11) 0.0347(11) 0.0022(10) -0.0014(9) -0.0001(9)
C17 0.0210(10) 0.0344(12) 0.0430(12) 0.0075(10) 0.0037(9) 0.0004(9)
C18 0.0337(12) 0.0348(12) 0.0370(12) 0.0010(10) 0.0107(9) 0.0041(10)
C19 0.0304(11) 0.0318(12) 0.0304(10) -0.0004(10) 0.0034(9) -0.0002(9)
C20 0.0197(10) 0.0261(11) 0.0320(10) 0.0003(9) 0.0015(8) -0.0044(8)
C21 0.0252(10) 0.0314(11) 0.0294(10) 0.0009(9) -0.0006(8) -0.0002(9)
C22 0.0216(10) 0.0311(12) 0.0403(12) 0.0002(10) 0.0021(9) 0.0019(9)
C23 0.0267(11) 0.0263(11) 0.0360(11) -0.0032(10) 0.0053(9) -0.0030(9)
C24 0.0297(11) 0.0328(12) 0.0296(11) -0.0004(9) -0.0014(9) 0.0011(9)
C25 0.0225(10) 0.0303(11) 0.0332(11) 0.0009(10) -0.0022(8) 0.0025(9)
C26 0.0366(12) 0.0394(13) 0.0516(14) -0.0048(11) 0.0151(10) 0.0059(11)
C27 0.0440(13) 0.0500(15) 0.0363(12) -0.0005(11) 0.0136(10) 0.0027(12)
_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 C6 1.7361(19) . ?
S1 C7 1.753(2) . ?
N1 C5 1.388(2) . ?
N1 C7 1.298(2) . ?
N2 C23 1.380(3) . ?
N2 C26 1.434(3) . ?
N2 C27 1.439(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(3) . ?
C1 C6 1.394(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.398(3) . ?
C5 C6 1.393(3) . ?
C7 C8 1.471(2) . ?
C8 C9 1.393(3) . ?
C8 C13 1.400(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(3) . ?
C12 C13 1.392(2) . ?
C12 C14 1.495(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.411(3) . ?
C14 C19 1.396(3) . ?
C15 C16 1.398(3) . ?
C15 C20 1.481(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(3) . ?
C20 C25 1.392(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.376(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.405(3) . ?
C23 C24 1.396(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.381(3) . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
C6 S1 C7 88.75(9) . . ?
C7 N1 C5 110.37(16) . . ?
C23 N2 C26 119.96(17) . . ?
C23 N2 C27 120.95(17) . . ?
C26 N2 C27 119.09(18) . . ?
C2 C1 H1 121.3 . . ?
C2 C1 C6 117.3(2) . . ?
C6 C1 H1 121.3 . . ?
C1 C2 H2 119.4 . . ?
C1 C2 C3 121.29(19) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.29(19) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.7(2) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 125.03(19) . . ?
N1 C5 C6 115.51(16) . . ?
C6 C5 C4 119.45(18) . . ?
C1 C6 S1 128.59(16) . . ?
C5 C6 S1 109.46(14) . . ?
C5 C6 C1 121.94(18) . . ?
N1 C7 S1 115.90(14) . . ?
N1 C7 C8 123.56(17) . . ?
C8 C7 S1 120.51(14) . . ?
C9 C8 C7 119.29(17) . . ?
C9 C8 C13 119.42(17) . . ?
C13 C8 C7 121.25(17) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.70(18) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.36(18) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 120.98(17) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 118.39(17) . . ?
C11 C12 C14 121.26(16) . . ?
C13 C12 C14 120.23(17) . . ?
C8 C13 H13 119.4 . . ?
C12 C13 C8 121.14(18) . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C12 122.48(17) . . ?
C19 C14 C12 118.31(17) . . ?
C19 C14 C15 119.15(17) . . ?
C14 C15 C20 122.63(17) . . ?
C16 C15 C14 118.20(18) . . ?
C16 C15 C20 119.15(17) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 C15 121.82(18) . . ?
C17 C16 H16 119.1 . . ?
C16 C17 H17 120.1 . . ?
C18 C17 C16 119.87(19) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.5(2) . . ?
C19 C18 H18 120.3 . . ?
C14 C19 H19 119.3 . . ?
C18 C19 C14 121.48(19) . . ?
C18 C19 H19 119.3 . . ?
C21 C20 C15 122.77(17) . . ?
C21 C20 C25 116.49(18) . . ?
C25 C20 C15 120.73(17) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 C20 122.10(18) . . ?
C22 C21 H21 119.0 . . ?
C21 C22 H22 119.3 . . ?
C21 C22 C23 121.34(18) . . ?
C23 C22 H22 119.3 . . ?
N2 C23 C22 121.50(18) . . ?
N2 C23 C24 121.85(18) . . ?
C24 C23 C22 116.65(18) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 C23 121.31(18) . . ?
C25 C24 H24 119.3 . . ?
C20 C25 H25 118.9 . . ?
C24 C25 C20 122.10(18) . . ?
C24 C25 H25 118.9 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
_shelx_res_file
;
TITL 180124_xiamin_4 in P21/c #14
180124_xiamin_4.res
created by SHELXL-2016/6 at 12:54:11 on 24-Jan-2018
REM reset to P21/c #14
CELL 0.71073 10.7946 7.79396 25.0193 90 96.0882 90
ZERR 4 0.00065 0.00057 0.00181 0 0.0059 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N S
UNIT 108 88 8 4
L.S. 4
PLAN 15
SIZE 0.36 0.4 0.48
TEMP -93.15
BOND $H
HTAB
fmap 2
acta
SHEL 999 0.83
OMIT -4 5 10
OMIT -4 5 11
REM
REM
REM
WGHT 0.041300 0.446800
FVAR 4.40463
S1 4 0.522387 0.344845 0.247478 11.00000 0.02613 0.03361 =
0.03193 0.00388 0.00194 -0.00516
N1 3 0.673690 0.539564 0.200666 11.00000 0.02317 0.03437 =
0.03036 -0.00242 0.00316 -0.00269
N2 3 0.322893 0.008220 -0.117342 11.00000 0.03215 0.04741 =
0.03722 -0.00799 0.00650 0.00514
C1 1 0.706272 0.360011 0.336486 11.00000 0.03534 0.03338 =
0.03190 0.00077 0.00336 0.00400
AFIX 43
H1 2 0.659211 0.289524 0.357827 11.00000 -1.20000
AFIX 0
C2 1 0.821025 0.424724 0.356470 11.00000 0.03739 0.03511 =
0.03457 -0.00392 -0.00613 0.00698
AFIX 43
H2 2 0.854231 0.396680 0.392085 11.00000 -1.20000
AFIX 0
C3 1 0.888820 0.529990 0.325518 11.00000 0.02814 0.04379 =
0.04032 -0.00764 -0.00527 -0.00050
AFIX 43
H3 2 0.966746 0.574376 0.340613 11.00000 -1.20000
AFIX 0
C4 1 0.845495 0.571116 0.273598 11.00000 0.02820 0.04248 =
0.03692 -0.00380 0.00230 -0.00549
AFIX 43
H4 2 0.893006 0.642227 0.252629 11.00000 -1.20000
AFIX 0
C5 1 0.730014 0.506355 0.252109 11.00000 0.02520 0.02995 =
0.03012 -0.00583 0.00266 0.00152
C6 1 0.662305 0.402312 0.283738 11.00000 0.02340 0.02621 =
0.03223 -0.00354 0.00225 0.00202
C7 1 0.565276 0.466094 0.193351 11.00000 0.02426 0.02245 =
0.02817 -0.00319 0.00697 0.00008
C8 1 0.479199 0.485362 0.144037 11.00000 0.02506 0.02318 =
0.02620 -0.00412 0.00459 0.00149
C9 1 0.519593 0.569665 0.099945 11.00000 0.02396 0.02901 =
0.03293 -0.00216 0.00556 -0.00165
AFIX 43
H9 2 0.602953 0.609850 0.101291 11.00000 -1.20000
AFIX 0
C10 1 0.437646 0.594636 0.054120 11.00000 0.03477 0.03078 =
0.02818 0.00145 0.00935 -0.00222
AFIX 43
H10 2 0.464800 0.653072 0.024143 11.00000 -1.20000
AFIX 0
C11 1 0.316112 0.534749 0.051773 11.00000 0.03249 0.03142 =
0.02560 -0.00154 0.00117 -0.00198
AFIX 43
H11 2 0.261156 0.551546 0.019958 11.00000 -1.20000
AFIX 0
C12 1 0.273564 0.450472 0.095327 11.00000 0.02518 0.02378 =
0.02776 -0.00258 0.00458 0.00060
C13 1 0.356272 0.425946 0.141260 11.00000 0.02626 0.02440 =
0.02608 -0.00131 0.00507 0.00005
AFIX 43
H13 2 0.328854 0.367885 0.171251 11.00000 -1.20000
AFIX 0
C14 1 0.140245 0.397595 0.094682 11.00000 0.02370 0.02648 =
0.02706 0.00206 0.00129 0.00108
C15 1 0.078714 0.297789 0.052938 11.00000 0.02152 0.02585 =
0.02842 0.00344 0.00029 0.00201
C16 1 -0.048402 0.265364 0.053929 11.00000 0.02413 0.03073 =
0.03472 0.00220 -0.00138 -0.00008
AFIX 43
H16 2 -0.091052 0.198503 0.026032 11.00000 -1.20000
AFIX 0
C17 1 -0.113831 0.327990 0.094435 11.00000 0.02100 0.03441 =
0.04301 0.00747 0.00369 0.00038
AFIX 43
H17 2 -0.200587 0.306201 0.093686 11.00000 -1.20000
AFIX 0
C18 1 -0.052788 0.422136 0.135907 11.00000 0.03367 0.03483 =
0.03702 0.00095 0.01075 0.00409
AFIX 43
H18 2 -0.096758 0.463191 0.164266 11.00000 -1.20000
AFIX 0
C19 1 0.073322 0.456337 0.135847 11.00000 0.03038 0.03182 =
0.03038 -0.00041 0.00345 -0.00016
AFIX 43
H19 2 0.115091 0.521180 0.164453 11.00000 -1.20000
AFIX 0
C20 1 0.144039 0.223236 0.009232 11.00000 0.01970 0.02613 =
0.03196 0.00029 0.00148 -0.00442
C21 1 0.254327 0.130368 0.018879 11.00000 0.02516 0.03139 =
0.02941 0.00095 -0.00057 -0.00025
AFIX 43
H21 2 0.290422 0.115715 0.054898 11.00000 -1.20000
AFIX 0
C22 1 0.312702 0.059144 -0.022091 11.00000 0.02165 0.03109 =
0.04032 0.00020 0.00205 0.00194
AFIX 43
H22 2 0.387429 -0.004177 -0.013683 11.00000 -1.20000
AFIX 0
C23 1 0.264023 0.078168 -0.076127 11.00000 0.02671 0.02635 =
0.03598 -0.00316 0.00526 -0.00298
C24 1 0.153399 0.171247 -0.085886 11.00000 0.02972 0.03278 =
0.02956 -0.00042 -0.00139 0.00112
AFIX 43
H24 2 0.117479 0.187400 -0.121866 11.00000 -1.20000
AFIX 0
C25 1 0.095175 0.240283 -0.044275 11.00000 0.02247 0.03033 =
0.03325 0.00092 -0.00216 0.00246
AFIX 43
H25 2 0.019360 0.301355 -0.052423 11.00000 -1.20000
AFIX 0
C26 1 0.443840 -0.067865 -0.106151 11.00000 0.03661 0.03936 =
0.05163 -0.00484 0.01505 0.00586
AFIX 137
H26A 2 0.437188 -0.172963 -0.085143 11.00000 -1.50000
H26B 2 0.499754 0.013103 -0.085630 11.00000 -1.50000
H26C 2 0.477220 -0.095724 -0.140034 11.00000 -1.50000
AFIX 0
C27 1 0.265270 0.011786 -0.171896 11.00000 0.04397 0.05005 =
0.03626 -0.00054 0.01360 0.00268
AFIX 137
H27A 2 0.259026 0.130753 -0.184577 11.00000 -1.50000
H27B 2 0.181722 -0.038393 -0.173450 11.00000 -1.50000
H27C 2 0.315818 -0.054571 -0.194816 11.00000 -1.50000
AFIX 0
HKLF 4
REM 180124_xiamin_4 in P21/c #14
REM R1 = 0.0425 for 2919 Fo > 4sig(Fo) and 0.0618 for all 3809 data
REM 273 parameters refined using 0 restraints
END
WGHT 0.0418 0.4336
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.223, deepest hole -0.301, 1-sigma level 0.046
Q1 1 0.2284 -0.0759 -0.2130 11.00000 0.05 0.22
Q2 1 0.2068 0.4210 0.0960 11.00000 0.05 0.20
Q3 1 0.5239 0.4443 0.1613 11.00000 0.05 0.19
Q4 1 0.6970 0.3284 0.2897 11.00000 0.05 0.18
Q5 1 0.2007 0.2114 0.0081 11.00000 0.05 0.18
Q6 1 0.5259 0.2081 0.2344 11.00000 0.05 0.18
Q7 1 0.5018 -0.1259 -0.2100 11.00000 0.05 0.17
Q8 1 0.1155 0.2846 0.0288 11.00000 0.05 0.17
Q9 1 0.6629 0.4205 0.3065 11.00000 0.05 0.17
Q10 1 0.9939 0.5171 0.2389 11.00000 0.05 0.17
Q11 1 0.1129 0.3543 0.0690 11.00000 0.05 0.17
Q12 1 0.4083 0.4987 0.1489 11.00000 0.05 0.16
Q13 1 0.4145 -0.0661 -0.2490 11.00000 0.05 0.16
Q14 1 0.5591 0.3765 0.2098 11.00000 0.05 0.16
Q15 1 0.5266 0.4627 0.2215 11.00000 0.05 0.16
;
_shelx_res_checksum 86876
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_180102_xiamin180102
_database_code_depnum_ccdc_archive 'CCDC 1834425'
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;
_audit_creation_date 2018-01-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H22 N2 S'
_chemical_formula_sum 'C27 H22 N2 S'
_chemical_formula_weight 406.52
_chemical_melting_point ?
_chemical_oxdiff_formula 'c h n o s'
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'
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 7.3980(10)
_cell_length_b 14.3691(15)
_cell_length_c 20.4895(16)
_cell_angle_alpha 90
_cell_angle_beta 91.329(8)
_cell_angle_gamma 90
_cell_volume 2177.5(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 1371
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 29.3316
_cell_measurement_theta_min 2.9986
_shelx_estimated_absorpt_T_max 0.963
_shelx_estimated_absorpt_T_min 0.924
_exptl_absorpt_coefficient_mu 0.164
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.64136
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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 1.240
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 856
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.23
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0547
_diffrn_reflns_av_unetI/netI 0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 8274
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.347
_diffrn_reflns_theta_min 3.005
_diffrn_ambient_temperature 293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -89.00 13.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- -11.4683 -77.0000 -60.0000 102
#__ type_ start__ end____ width___ exp.time_
2 omega -66.00 6.00 1.0000 90.0000
omega____ theta____ kappa____ phi______ frames
- -11.4683 121.0000 24.0000 72
;
_diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0300321000
_diffrn_orient_matrix_UB_12 -0.0467748000
_diffrn_orient_matrix_UB_13 -0.0022401000
_diffrn_orient_matrix_UB_21 0.0897092000
_diffrn_orient_matrix_UB_22 -0.0146595000
_diffrn_orient_matrix_UB_23 -0.0059417000
_diffrn_orient_matrix_UB_31 0.0159126000
_diffrn_orient_matrix_UB_32 -0.0056093000
_diffrn_orient_matrix_UB_33 0.0340471000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2040
_reflns_number_total 3970
_reflns_odcompleteness_completeness 99.57
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.174
_refine_diff_density_min -0.233
_refine_diff_density_rms 0.039
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.005
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 273
_refine_ls_number_reflns 3970
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1287
_refine_ls_R_factor_gt 0.0641
_refine_ls_restrained_S_all 1.005
_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^)+(0.0726P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1472
_refine_ls_wR_factor_ref 0.1843
_refine_special_details ?
_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:
C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.32921(13) 0.26106(7) 0.31758(5) 0.0760(4) Uani 1 1 d . . . . .
N1 N 0.5910(4) 0.14803(19) 0.34919(13) 0.0710(8) Uani 1 1 d . . . . .
N2 N 1.0211(5) 0.2742(4) 0.55766(18) 0.1392(17) Uani 1 1 d . . . . .
C1 C 0.4250(8) 0.0339(3) 0.41624(19) 0.1004(15) Uani 1 1 d . . . . .
H1 H 0.527757 -0.001403 0.425505 0.120 Uiso 1 1 calc R . . . .
C2 C 0.2562(9) 0.0083(4) 0.4404(2) 0.1136(17) Uani 1 1 d . . . . .
H2 H 0.246932 -0.043904 0.466935 0.136 Uiso 1 1 calc R . . . .
C3 C 0.1060(9) 0.0593(4) 0.4254(2) 0.1127(17) Uani 1 1 d . . . . .
H3 H -0.005051 0.039197 0.440434 0.135 Uiso 1 1 calc R . . . .
C4 C 0.1119(7) 0.1396(3) 0.38881(19) 0.0975(13) Uani 1 1 d . . . . .
H4 H 0.008067 0.174556 0.380745 0.117 Uiso 1 1 calc R . . . .
C5 C 0.2771(6) 0.1669(3) 0.36424(17) 0.0732(10) Uani 1 1 d . . . . .
C6 C 0.4342(6) 0.1138(3) 0.37795(16) 0.0762(11) Uani 1 1 d . . . . .
C7 C 0.5537(5) 0.2246(2) 0.31666(14) 0.0568(8) Uani 1 1 d . . . . .
C8 C 0.6921(5) 0.2726(2) 0.27869(14) 0.0554(8) Uani 1 1 d . . . . .
C9 C 0.8244(5) 0.2198(2) 0.24906(16) 0.0672(9) Uani 1 1 d . . . . .
H9 H 0.824175 0.155675 0.255121 0.081 Uiso 1 1 calc R . . . .
C10 C 0.9543(5) 0.2581(3) 0.21150(17) 0.0775(11) Uani 1 1 d . . . . .
H10 H 1.040793 0.220624 0.192401 0.093 Uiso 1 1 calc R . . . .
C11 C 0.9563(5) 0.3535(3) 0.20201(17) 0.0806(11) Uani 1 1 d . . . . .
H11 H 1.044550 0.380614 0.176565 0.097 Uiso 1 1 calc R . . . .
C12 C 0.8271(5) 0.4080(3) 0.23045(17) 0.0720(10) Uani 1 1 d . . . . .
H12 H 0.828256 0.471973 0.223448 0.086 Uiso 1 1 calc R . . . .
C13 C 0.6948(5) 0.3698(2) 0.26942(14) 0.0580(9) Uani 1 1 d . . . . .
C14 C 0.5593(5) 0.4319(2) 0.29953(14) 0.0557(8) Uani 1 1 d . . . . .
C15 C 0.4333(5) 0.4771(2) 0.25893(17) 0.0681(10) Uani 1 1 d . . . . .
H15 H 0.443387 0.472296 0.213894 0.082 Uiso 1 1 calc R . . . .
C16 C 0.2936(5) 0.5288(2) 0.28430(19) 0.0766(11) Uani 1 1 d . . . . .
H16 H 0.209367 0.557548 0.256551 0.092 Uiso 1 1 calc R . . . .
C17 C 0.2802(5) 0.5375(2) 0.3512(2) 0.0794(11) Uani 1 1 d . . . . .
H17 H 0.185813 0.571343 0.368694 0.095 Uiso 1 1 calc R . . . .
C18 C 0.4077(5) 0.4956(2) 0.39194(17) 0.0720(10) Uani 1 1 d . . . . .
H18 H 0.399246 0.502917 0.436864 0.086 Uiso 1 1 calc R . . . .
C19 C 0.5486(5) 0.4429(2) 0.36727(15) 0.0591(8) Uani 1 1 d . . . . .
C20 C 0.6752(5) 0.3960(2) 0.41473(14) 0.0599(9) Uani 1 1 d . . . . .
C21 C 0.6114(5) 0.3405(2) 0.46321(15) 0.0642(9) Uani 1 1 d . . . . .
H21 H 0.487471 0.330555 0.465307 0.077 Uiso 1 1 calc R . . . .
C22 C 0.7233(5) 0.2988(3) 0.50894(16) 0.0744(10) Uani 1 1 d . . . . .
H22 H 0.673759 0.260290 0.540354 0.089 Uiso 1 1 calc R . . . .
C23 C 0.9073(6) 0.3129(3) 0.50913(17) 0.0857(12) Uani 1 1 d . . . . .
C24 C 0.9732(6) 0.3661(4) 0.45990(19) 0.1089(16) Uani 1 1 d . . . . .
H24 H 1.097529 0.374987 0.458068 0.131 Uiso 1 1 calc R . . . .
C25 C 0.8649(5) 0.4070(3) 0.41318(16) 0.0854(12) Uani 1 1 d . . . . .
H25 H 0.916145 0.442183 0.380294 0.102 Uiso 1 1 calc R . . . .
C26 C 1.2102(7) 0.2856(6) 0.5530(3) 0.220(4) Uani 1 1 d . . . . .
H26A H 1.246709 0.268722 0.509899 0.330 Uiso 1 1 calc GR . . . .
H26B H 1.270751 0.246475 0.584500 0.330 Uiso 1 1 calc GR . . . .
H26C H 1.241457 0.349447 0.561289 0.330 Uiso 1 1 calc GR . . . .
C27 C 0.9564(7) 0.2212(3) 0.6091(2) 0.1119(16) Uani 1 1 d . . . . .
H27A H 0.858528 0.253543 0.629096 0.168 Uiso 1 1 calc GR . . . .
H27B H 1.051945 0.211335 0.640884 0.168 Uiso 1 1 calc GR . . . .
H27C H 0.914301 0.162252 0.592822 0.168 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
S1 0.0786(7) 0.0727(6) 0.0763(7) 0.0058(5) -0.0067(5) -0.0066(5)
N1 0.094(2) 0.0630(18) 0.0563(17) 0.0009(14) 0.0027(16) 0.0039(16)
N2 0.079(3) 0.267(6) 0.071(2) 0.041(3) -0.007(2) 0.021(3)
C1 0.150(5) 0.080(3) 0.071(3) 0.010(2) 0.005(3) 0.006(3)
C2 0.159(6) 0.101(4) 0.082(3) 0.006(3) 0.026(4) -0.029(4)
C3 0.151(5) 0.111(4) 0.077(3) 0.006(3) 0.015(3) -0.037(4)
C4 0.109(4) 0.114(4) 0.070(3) -0.003(2) 0.003(2) -0.013(3)
C5 0.083(3) 0.078(3) 0.058(2) -0.0112(18) 0.009(2) -0.018(2)
C6 0.116(4) 0.064(2) 0.049(2) -0.0040(17) 0.005(2) -0.006(2)
C7 0.073(2) 0.0465(18) 0.0507(18) -0.0043(15) -0.0058(16) 0.0025(16)
C8 0.063(2) 0.0567(19) 0.0459(17) -0.0009(14) -0.0091(16) 0.0017(17)
C9 0.074(3) 0.070(2) 0.057(2) 0.0010(17) -0.0035(19) 0.0069(19)
C10 0.066(3) 0.103(3) 0.063(2) -0.002(2) -0.0010(19) 0.016(2)
C11 0.076(3) 0.099(3) 0.067(2) 0.003(2) 0.004(2) -0.008(2)
C12 0.082(3) 0.069(2) 0.065(2) 0.0019(18) 0.003(2) -0.006(2)
C13 0.069(2) 0.062(2) 0.0430(17) 0.0008(15) -0.0007(16) -0.0049(17)
C14 0.073(2) 0.0433(16) 0.0503(18) -0.0001(14) 0.0001(17) -0.0040(16)
C15 0.087(3) 0.054(2) 0.063(2) 0.0012(16) -0.004(2) 0.0007(19)
C16 0.091(3) 0.055(2) 0.083(3) 0.0121(18) -0.011(2) 0.005(2)
C17 0.089(3) 0.060(2) 0.090(3) -0.005(2) 0.007(2) 0.007(2)
C18 0.084(3) 0.066(2) 0.067(2) -0.0100(18) 0.003(2) -0.001(2)
C19 0.065(2) 0.0536(18) 0.059(2) -0.0040(15) 0.0027(17) -0.0085(17)
C20 0.067(2) 0.066(2) 0.0459(18) -0.0116(15) -0.0018(16) -0.0035(17)
C21 0.060(2) 0.075(2) 0.058(2) 0.0022(17) 0.0015(17) -0.0067(18)
C22 0.074(3) 0.093(3) 0.056(2) 0.0016(18) -0.0002(19) 0.000(2)
C23 0.071(3) 0.138(4) 0.048(2) -0.005(2) 0.000(2) 0.010(2)
C24 0.067(3) 0.198(5) 0.061(3) 0.016(3) -0.004(2) -0.014(3)
C25 0.070(3) 0.136(4) 0.050(2) 0.021(2) -0.0049(19) -0.031(2)
C26 0.071(4) 0.467(13) 0.120(5) 0.100(6) -0.014(3) 0.021(5)
C27 0.129(4) 0.101(3) 0.104(4) 0.023(3) -0.029(3) 0.005(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 C5 1.706(4) . ?
S1 C7 1.742(4) . ?
N1 C6 1.402(5) . ?
N1 C7 1.312(4) . ?
N2 C23 1.402(5) . ?
N2 C26 1.414(6) . ?
N2 C27 1.394(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.403(6) . ?
C1 C6 1.393(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.360(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.376(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.389(5) . ?
C5 C6 1.413(5) . ?
C7 C8 1.472(5) . ?
C8 C9 1.389(5) . ?
C8 C13 1.410(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.362(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.385(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.376(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(4) . ?
C13 C14 1.486(4) . ?
C14 C15 1.395(4) . ?
C14 C19 1.401(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.381(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.383(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.393(5) . ?
C19 C20 1.495(4) . ?
C20 C21 1.366(4) . ?
C20 C25 1.413(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.373(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.377(5) . ?
C23 C24 1.365(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.367(5) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 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
C5 S1 C7 89.74(18) . . ?
C7 N1 C6 110.0(3) . . ?
C23 N2 C26 119.0(4) . . ?
C27 N2 C23 122.8(4) . . ?
C27 N2 C26 118.2(4) . . ?
C2 C1 H1 121.0 . . ?
C6 C1 H1 121.0 . . ?
C6 C1 C2 118.1(5) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 C1 120.5(5) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 H3 118.7 . . ?
C2 C3 C4 122.5(5) . . ?
C4 C3 H3 118.7 . . ?
C3 C4 H4 120.9 . . ?
C3 C4 C5 118.3(5) . . ?
C5 C4 H4 120.9 . . ?
C4 C5 S1 129.8(4) . . ?
C4 C5 C6 120.1(4) . . ?
C6 C5 S1 110.1(3) . . ?
N1 C6 C5 114.3(3) . . ?
C1 C6 N1 125.3(4) . . ?
C1 C6 C5 120.4(4) . . ?
N1 C7 S1 115.8(3) . . ?
N1 C7 C8 121.4(3) . . ?
C8 C7 S1 122.7(2) . . ?
C9 C8 C7 118.7(3) . . ?
C9 C8 C13 118.0(3) . . ?
C13 C8 C7 123.2(3) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 C8 122.7(3) . . ?
C10 C9 H9 118.7 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.3(4) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 119.2 . . ?
C11 C12 C13 121.6(3) . . ?
C13 C12 H12 119.2 . . ?
C8 C13 C14 121.8(3) . . ?
C12 C13 C8 118.7(3) . . ?
C12 C13 C14 119.4(3) . . ?
C15 C14 C13 118.6(3) . . ?
C15 C14 C19 119.1(3) . . ?
C19 C14 C13 122.2(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 120.3 . . ?
C17 C16 C15 119.5(3) . . ?
C17 C16 H16 120.3 . . ?
C16 C17 H17 120.1 . . ?
C16 C17 C18 119.8(4) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 119.2 . . ?
C17 C18 C19 121.5(3) . . ?
C19 C18 H18 119.2 . . ?
C14 C19 C20 123.0(3) . . ?
C18 C19 C14 118.7(3) . . ?
C18 C19 C20 118.2(3) . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 C25 116.2(3) . . ?
C25 C20 C19 122.8(3) . . ?
C20 C21 H21 118.7 . . ?
C20 C21 C22 122.5(3) . . ?
C22 C21 H21 118.7 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.2(4) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 N2 121.4(4) . . ?
C24 C23 N2 121.8(4) . . ?
C24 C23 C22 116.8(4) . . ?
C23 C24 H24 118.5 . . ?
C23 C24 C25 123.0(4) . . ?
C25 C24 H24 118.5 . . ?
C20 C25 H25 119.9 . . ?
C24 C25 C20 120.1(3) . . ?
C24 C25 H25 119.9 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
_shelx_res_file
;
TITL 180102_xiamin180102_a.res in P2(1)/n
180102_xiamin180102.res
created by SHELXL-2016/6 at 10:52:04 on 03-Jan-2018
REM Old TITL 180102_xiamin180102 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.221, Rweak 0.271, Alpha 0.036, Orientation as input
REM Formula found by SHELXT: C28 N S
CELL 0.71073 7.398 14.3691 20.4895 90 91.329 90
ZERR 4 0.001 0.0015 0.0016 0 0.008 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N S
UNIT 108 88 8 4
L.S. 5
PLAN 20
SIZE 0.49 0.26 0.23
TEMP 20
BOND $H
htab
list 4
fmap 2
acta
SHEL 999 0.83
OMIT -2 9 8
OMIT -1 3 5
OMIT -1 1 20
REM
REM
REM
WGHT 0.072600
FVAR 0.43919
S1 4 0.329212 0.261058 0.317579 11.00000 0.07857 0.07275 =
0.07625 0.00583 -0.00669 -0.00663
N1 3 0.590952 0.148025 0.349190 11.00000 0.09372 0.06295 =
0.05628 0.00094 0.00275 0.00394
N2 3 1.021086 0.274233 0.557661 11.00000 0.07895 0.26709 =
0.07121 0.04072 -0.00707 0.02107
C1 1 0.425018 0.033936 0.416240 11.00000 0.15020 0.08020 =
0.07091 0.00959 0.00515 0.00607
AFIX 43
H1 2 0.527757 -0.001403 0.425505 11.00000 -1.20000
AFIX 0
C2 1 0.256192 0.008335 0.440425 11.00000 0.15937 0.10088 =
0.08179 0.00551 0.02618 -0.02937
AFIX 43
H2 2 0.246932 -0.043904 0.466935 11.00000 -1.20000
AFIX 0
C3 1 0.105973 0.059325 0.425400 11.00000 0.15095 0.11079 =
0.07681 0.00594 0.01461 -0.03672
AFIX 43
H3 2 -0.005051 0.039197 0.440434 11.00000 -1.20000
AFIX 0
C4 1 0.111946 0.139557 0.388807 11.00000 0.10865 0.11438 =
0.06966 -0.00261 0.00312 -0.01308
AFIX 43
H4 2 0.008067 0.174556 0.380745 11.00000 -1.20000
AFIX 0
C5 1 0.277070 0.166899 0.364235 11.00000 0.08350 0.07822 =
0.05818 -0.01116 0.00936 -0.01826
C6 1 0.434203 0.113821 0.377953 11.00000 0.11596 0.06376 =
0.04892 -0.00399 0.00524 -0.00637
C7 1 0.553734 0.224574 0.316661 11.00000 0.07283 0.04650 =
0.05067 -0.00427 -0.00585 0.00247
C8 1 0.692137 0.272592 0.278689 11.00000 0.06314 0.05666 =
0.04593 -0.00091 -0.00915 0.00168
C9 1 0.824364 0.219817 0.249061 11.00000 0.07415 0.06984 =
0.05743 0.00096 -0.00351 0.00691
AFIX 43
H9 2 0.824175 0.155675 0.255121 11.00000 -1.20000
AFIX 0
C10 1 0.954290 0.258145 0.211496 11.00000 0.06623 0.10263 =
0.06339 -0.00233 -0.00097 0.01561
AFIX 43
H10 2 1.040793 0.220624 0.192401 11.00000 -1.20000
AFIX 0
C11 1 0.956335 0.353537 0.202012 11.00000 0.07628 0.09900 =
0.06679 0.00328 0.00445 -0.00772
AFIX 43
H11 2 1.044550 0.380614 0.176565 11.00000 -1.20000
AFIX 0
C12 1 0.827098 0.408032 0.230453 11.00000 0.08213 0.06894 =
0.06492 0.00192 0.00320 -0.00567
AFIX 43
H12 2 0.828256 0.471973 0.223448 11.00000 -1.20000
AFIX 0
C13 1 0.694789 0.369811 0.269420 11.00000 0.06943 0.06152 =
0.04301 0.00085 -0.00071 -0.00487
C14 1 0.559348 0.431898 0.299528 11.00000 0.07344 0.04332 =
0.05034 -0.00014 0.00008 -0.00399
C15 1 0.433326 0.477061 0.258930 11.00000 0.08726 0.05420 =
0.06254 0.00117 -0.00375 0.00070
AFIX 43
H15 2 0.443387 0.472296 0.213894 11.00000 -1.20000
AFIX 0
C16 1 0.293554 0.528840 0.284300 11.00000 0.09141 0.05487 =
0.08278 0.01207 -0.01110 0.00543
AFIX 43
H16 2 0.209367 0.557548 0.256551 11.00000 -1.20000
AFIX 0
C17 1 0.280207 0.537496 0.351161 11.00000 0.08857 0.05980 =
0.09017 -0.00487 0.00684 0.00710
AFIX 43
H17 2 0.185813 0.571343 0.368694 11.00000 -1.20000
AFIX 0
C18 1 0.407723 0.495648 0.391937 11.00000 0.08354 0.06601 =
0.06653 -0.01003 0.00294 -0.00138
AFIX 43
H18 2 0.399246 0.502917 0.436864 11.00000 -1.20000
AFIX 0
C19 1 0.548554 0.442867 0.367274 11.00000 0.06476 0.05361 =
0.05909 -0.00399 0.00267 -0.00848
C20 1 0.675240 0.395959 0.414733 11.00000 0.06726 0.06630 =
0.04587 -0.01165 -0.00183 -0.00350
C21 1 0.611427 0.340465 0.463206 11.00000 0.05993 0.07493 =
0.05778 0.00218 0.00150 -0.00672
AFIX 43
H21 2 0.487471 0.330555 0.465307 11.00000 -1.20000
AFIX 0
C22 1 0.723261 0.298760 0.508940 11.00000 0.07432 0.09318 =
0.05575 0.00159 -0.00025 0.00035
AFIX 43
H22 2 0.673759 0.260290 0.540354 11.00000 -1.20000
AFIX 0
C23 1 0.907313 0.312867 0.509127 11.00000 0.07098 0.13811 =
0.04785 -0.00481 0.00036 0.01000
C24 1 0.973225 0.366122 0.459899 11.00000 0.06732 0.19776 =
0.06143 0.01620 -0.00393 -0.01369
AFIX 43
H24 2 1.097529 0.374987 0.458068 11.00000 -1.20000
AFIX 0
C25 1 0.864915 0.407011 0.413179 11.00000 0.06977 0.13624 =
0.04987 0.02081 -0.00495 -0.03051
AFIX 43
H25 2 0.916145 0.442183 0.380294 11.00000 -1.20000
AFIX 0
C26 1 1.210178 0.285634 0.552960 11.00000 0.07128 0.46684 =
0.12035 0.09996 -0.01407 0.02077
AFIX 137
H26A 2 1.246709 0.268722 0.509899 11.00000 -1.50000
H26B 2 1.270751 0.246475 0.584500 11.00000 -1.50000
H26C 2 1.241457 0.349447 0.561289 11.00000 -1.50000
AFIX 0
C27 1 0.956429 0.221211 0.609124 11.00000 0.12916 0.10073 =
0.10429 0.02327 -0.02872 0.00479
AFIX 137
H27A 2 0.858528 0.253543 0.629096 11.00000 -1.50000
H27B 2 1.051945 0.211335 0.640884 11.00000 -1.50000
H27C 2 0.914301 0.162252 0.592822 11.00000 -1.50000
AFIX 0
HKLF 4
REM 180102_xiamin180102_a.res in P2(1)/n
REM R1 = 0.0641 for 2040 Fo > 4sig(Fo) and 0.1287 for all 3970 data
REM 273 parameters refined using 0 restraints
END
WGHT 0.0726 0.0000
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.174, deepest hole -0.233, 1-sigma level 0.039
Q1 1 0.9794 0.2216 0.5489 11.00000 0.05 0.17
Q2 1 0.9135 0.4159 0.3952 11.00000 0.05 0.17
Q3 1 1.2393 0.2374 0.4986 11.00000 0.05 0.16
Q4 1 0.2446 0.2638 0.2598 11.00000 0.05 0.15
Q5 1 1.0082 0.3022 0.5587 11.00000 0.05 0.15
Q6 1 1.2120 0.3400 0.5869 11.00000 0.05 0.15
Q7 1 1.1213 0.1950 0.2779 11.00000 0.05 0.14
Q8 1 0.7856 0.1356 0.3590 11.00000 0.05 0.14
Q9 1 0.5696 0.4143 0.3818 11.00000 0.05 0.14
Q10 1 0.2814 0.0976 0.3871 11.00000 0.05 0.14
Q11 1 0.7429 0.2486 0.5607 11.00000 0.05 0.14
Q12 1 0.3835 0.2607 0.2611 11.00000 0.05 0.13
Q13 1 0.7491 0.3770 0.2597 11.00000 0.05 0.13
Q14 1 0.7767 0.2199 0.6130 11.00000 0.05 0.13
Q15 1 1.0857 0.2975 0.5145 11.00000 0.05 0.12
Q16 1 1.1567 0.2301 0.5518 11.00000 0.05 0.12
Q17 1 0.4565 0.1955 0.2434 11.00000 0.05 0.12
Q18 1 0.4327 0.1158 0.4143 11.00000 0.05 0.12
Q19 1 0.4446 0.2152 0.2825 11.00000 0.05 0.12
Q20 1 0.5213 0.2569 0.5512 11.00000 0.05 0.12
;
_shelx_res_checksum 60079
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_180124_xiamin_5
_database_code_depnum_ccdc_archive 'CCDC 1834424'
_audit_update_record
;
2018-04-03 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;
_audit_creation_date 2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H22 N2 S'
_chemical_formula_sum 'C27 H22 N2 S'
_chemical_formula_weight 406.52
_chemical_absolute_configuration unk
_chemical_melting_point ?
_chemical_oxdiff_formula 'C H N O s'
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'
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 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 12.2955(11)
_cell_length_b 13.9512(11)
_cell_length_c 12.4705(14)
_cell_angle_alpha 90
_cell_angle_beta 102.145(9)
_cell_angle_gamma 90
_cell_volume 2091.3(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 1996
_cell_measurement_temperature 180
_cell_measurement_theta_max 29.3394
_cell_measurement_theta_min 3.3581
_shelx_estimated_absorpt_T_max 0.967
_shelx_estimated_absorpt_T_min 0.922
_exptl_absorpt_coefficient_mu 0.171
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.87835
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light yellow'
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.291
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 856
_exptl_crystal_size_max 0.48
_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 0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 8393
_diffrn_reflns_point_group_measured_fraction_full 0.777
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.349
_diffrn_reflns_theta_min 3.365
_diffrn_ambient_temperature 180
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -37.00 64.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -11.4683 38.0000 -30.0000 101
#__ type_ start__ end____ width___ exp.time_
2 omega -38.00 39.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -11.4683 38.0000 -120.0000 77
;
_diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0282468000
_diffrn_orient_matrix_UB_12 -0.0205229000
_diffrn_orient_matrix_UB_13 -0.0384757000
_diffrn_orient_matrix_UB_21 -0.0177205000
_diffrn_orient_matrix_UB_22 0.0385669000
_diffrn_orient_matrix_UB_23 -0.0365237000
_diffrn_orient_matrix_UB_31 0.0487170000
_diffrn_orient_matrix_UB_32 0.0260207000
_diffrn_orient_matrix_UB_33 0.0237637000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.492
_reflns_Friedel_fraction_full 0.537
_reflns_Friedel_fraction_max 0.536
_reflns_number_gt 4526
_reflns_number_total 5954
_reflns_odcompleteness_completeness 99.60
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.267
_refine_diff_density_min -0.228
_refine_diff_density_rms 0.047
_refine_ls_abs_structure_details
;
Flack x determined using 1175 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.56(9)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 558
_refine_ls_number_reflns 5954
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0800
_refine_ls_R_factor_gt 0.0555
_refine_ls_restrained_S_all 1.045
_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^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1288
_refine_ls_wR_factor_ref 0.1520
_refine_special_details ?
_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. Uiso/Uaniso restraints and constraints
Uanis(N3) = Uanis(N3A)
3. Others
Sof(S2A)=Sof(N3A)=1-FVAR(1)
Sof(S2)=Sof(N3)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
C10(H10), C24(H24), C12(H12), C21(H21), C22(H22), C9(H9), C25(H25), C39(H39),
C37(H37), C16(H16), C48(H48), C13(H13), C36(H36), C19(H19), C18(H18), C49(H49),
C2(H2), C45(H45), C3(H3), C1(H1), C51(H51), C44(H44), C17(H17), C43(H43),
C46(H46), C40(H40), C52(H52), C4(H4), C30(H30), C29(H29), C31(H31), C28(H28)
4.b Idealised Me refined as rotating group:
C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C53(H53A,H53B,H53C), C54(H54A,H54B,
H54C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 1.18530(11) 0.18350(12) 0.74683(12) 0.0498(4) Uani 1 1 d . . . . .
S2 S 0.7478(2) 0.30018(17) 0.83441(18) 0.0486(9) Uani 0.776(9) 1 d . . P A 1
N1 N 1.1088(4) 0.2593(4) 0.9057(4) 0.0507(13) Uani 1 1 d . . . . .
N3 N 0.5777(7) 0.2298(7) 0.8914(8) 0.043(2) Uani 0.776(9) 1 d . . P A 1
C38 C 0.3748(4) 0.4743(3) 0.6175(4) 0.0338(12) Uani 1 1 d . . . . .
N4 N 0.6165(4) 0.8647(4) 0.8170(4) 0.0578(14) Uani 1 1 d . . . . .
N2 N 1.0982(4) 0.8528(4) 0.8220(4) 0.0542(14) Uani 1 1 d . . . . .
C10 C 0.9468(4) 0.3907(4) 0.5470(4) 0.0393(13) Uani 1 1 d . . . . .
H10 H 0.938888 0.386252 0.469703 0.047 Uiso 1 1 calc R . . . .
C24 C 0.9088(4) 0.8011(4) 0.7476(4) 0.0403(13) Uani 1 1 d . . . . .
H24 H 0.881487 0.844932 0.793951 0.048 Uiso 1 1 calc R . . . .
C8 C 1.0303(4) 0.3338(4) 0.7277(4) 0.0374(12) Uani 1 1 d . . . . .
C15 C 0.7852(4) 0.6185(4) 0.5327(5) 0.0386(13) Uani 1 1 d . . . . .
C11 C 0.8849(4) 0.4600(4) 0.5912(4) 0.0353(12) Uani 1 1 d . . . . .
C23 C 1.0234(4) 0.7963(4) 0.7527(5) 0.0416(13) Uani 1 1 d . . . . .
C14 C 0.7984(4) 0.5184(4) 0.5188(4) 0.0384(13) Uani 1 1 d . . . . .
C20 C 0.8684(4) 0.6768(4) 0.6102(4) 0.0353(11) Uani 1 1 d . . . . .
C34 C 0.6035(4) 0.2926(4) 0.8320(4) 0.0395(13) Uani 1 1 d . . . . .
C12 C 0.9011(4) 0.4652(4) 0.7048(5) 0.0425(13) Uani 1 1 d . . . . .
H12 H 0.861971 0.512400 0.736713 0.051 Uiso 1 1 calc R . . . .
C21 C 0.9831(4) 0.6701(4) 0.6140(4) 0.0385(12) Uani 1 1 d . . . . .
H21 H 1.009392 0.625041 0.568255 0.046 Uiso 1 1 calc R . . . .
C22 C 1.0584(4) 0.7276(4) 0.6829(4) 0.0396(13) Uani 1 1 d . . . . .
H22 H 1.135452 0.721127 0.683746 0.048 Uiso 1 1 calc R . . . .
C9 C 1.0188(4) 0.3291(4) 0.6144(4) 0.0397(13) Uani 1 1 d . . . . .
H9 H 1.060416 0.283454 0.583209 0.048 Uiso 1 1 calc R . . . .
C41 C 0.2934(4) 0.5318(4) 0.5359(4) 0.0403(13) Uani 1 1 d . . . . .
C25 C 0.8344(4) 0.7442(4) 0.6774(5) 0.0406(13) Uani 1 1 d . . . . .
H25 H 0.757144 0.751464 0.675176 0.049 Uiso 1 1 calc R . . . .
C39 C 0.3383(4) 0.4118(4) 0.6891(4) 0.0390(13) Uani 1 1 d . . . . .
H39 H 0.261177 0.408545 0.689363 0.047 Uiso 1 1 calc R . . . .
C35 C 0.5263(4) 0.3563(4) 0.7593(4) 0.0367(12) Uani 1 1 d . . . . .
C7 C 1.1027(4) 0.2655(4) 0.7999(4) 0.0372(12) Uani 1 1 d . . . . .
C37 C 0.4885(4) 0.4790(4) 0.6188(4) 0.0387(13) Uani 1 1 d . . . . .
H37 H 0.515268 0.523024 0.572250 0.046 Uiso 1 1 calc R . . . .
C16 C 0.6933(4) 0.6639(4) 0.4694(4) 0.0419(14) Uani 1 1 d . . . . .
H16 H 0.682236 0.730219 0.480395 0.050 Uiso 1 1 calc R . . . .
C48 C 0.4010(4) 0.6840(4) 0.7085(4) 0.0400(12) Uani 1 1 d . . . . .
H48 H 0.356801 0.638839 0.737136 0.048 Uiso 1 1 calc R . . . .
C6 C 1.2366(4) 0.1416(4) 0.8789(4) 0.0391(13) Uani 1 1 d . . . . .
C13 C 0.9723(4) 0.4037(4) 0.7725(5) 0.0405(13) Uani 1 1 d . . . . .
H13 H 0.981750 0.409131 0.849869 0.049 Uiso 1 1 calc R . . . .
C36 C 0.5631(4) 0.4193(4) 0.6881(4) 0.0376(13) Uani 1 1 d . . . . .
H36 H 0.639983 0.421785 0.686592 0.045 Uiso 1 1 calc R . . . .
C47 C 0.3902(4) 0.6897(4) 0.5957(4) 0.0378(12) Uani 1 1 d . . . . .
C19 C 0.7223(4) 0.4717(4) 0.4369(5) 0.0438(14) Uani 1 1 d . . . . .
H19 H 0.732002 0.405322 0.425004 0.053 Uiso 1 1 calc R . . . .
C50 C 0.5402(4) 0.8092(4) 0.7427(5) 0.0419(13) Uani 1 1 d . . . . .
C42 C 0.3071(4) 0.6298(4) 0.5194(5) 0.0403(13) Uani 1 1 d . . . . .
C18 C 0.6334(4) 0.5186(5) 0.3728(5) 0.0490(15) Uani 1 1 d . . . . .
H18 H 0.583567 0.484971 0.316804 0.059 Uiso 1 1 calc R . . . .
C49 C 0.4731(4) 0.7411(4) 0.7808(5) 0.0453(14) Uani 1 1 d . . . . .
H49 H 0.477600 0.734322 0.857407 0.054 Uiso 1 1 calc R . . . .
C2 C 1.3458(4) 0.0521(5) 1.0262(5) 0.0507(16) Uani 1 1 d . . . . .
H2 H 1.402647 0.006811 1.053364 0.061 Uiso 1 1 calc R . . . .
C45 C 0.1305(5) 0.5296(5) 0.3873(5) 0.0511(16) Uani 1 1 d . . . . .
H45 H 0.069185 0.495940 0.344671 0.061 Uiso 1 1 calc R . . . .
C3 C 1.2905(5) 0.0962(5) 1.0975(5) 0.0567(17) Uani 1 1 d . . . . .
H3 H 1.308328 0.079335 1.172979 0.068 Uiso 1 1 calc R . . . .
C1 C 1.3197(4) 0.0731(5) 0.9147(5) 0.0523(15) Uani 1 1 d . . . . .
H1 H 1.356816 0.042118 0.864761 0.063 Uiso 1 1 calc R . . . .
C5 C 1.1843(4) 0.1873(4) 0.9513(5) 0.0451(13) Uani 1 1 d . . . . .
C51 C 0.5295(4) 0.8166(4) 0.6296(5) 0.0467(14) Uani 1 1 d . . . . .
H51 H 0.573303 0.862020 0.600819 0.056 Uiso 1 1 calc R . . . .
C44 C 0.1485(5) 0.6247(5) 0.3672(5) 0.0555(17) Uani 1 1 d . . . . .
H44 H 0.101170 0.656078 0.307586 0.067 Uiso 1 1 calc R . . . .
C17 C 0.6172(4) 0.6148(5) 0.3904(5) 0.0470(15) Uani 1 1 d . . . . .
H17 H 0.554347 0.647252 0.348666 0.056 Uiso 1 1 calc R . . . .
C43 C 0.2347(4) 0.6754(5) 0.4326(5) 0.0497(15) Uani 1 1 d . . . . .
H43 H 0.244707 0.741390 0.418496 0.060 Uiso 1 1 calc R . . . .
C46 C 0.2039(4) 0.4843(4) 0.4712(5) 0.0443(14) Uani 1 1 d . . . . .
H46 H 0.192699 0.418433 0.485123 0.053 Uiso 1 1 calc R . . . .
C40 C 0.4121(4) 0.3540(4) 0.7602(5) 0.0434(14) Uani 1 1 d . . . . .
H40 H 0.385515 0.312706 0.809598 0.052 Uiso 1 1 calc R . . . .
C52 C 0.4555(4) 0.7585(4) 0.5581(5) 0.0441(14) Uani 1 1 d . . . . .
H52 H 0.449296 0.765904 0.481339 0.053 Uiso 1 1 calc R . . . .
C32 C 0.6677(4) 0.1770(5) 0.9539(5) 0.0488(14) Uani 1 1 d . . . . .
C26 C 1.2175(4) 0.8396(4) 0.8313(5) 0.0514(16) Uani 1 1 d . . . . .
H26A H 1.235803 0.771355 0.840406 0.077 Uiso 1 1 calc GR . . . .
H26B H 1.258149 0.875260 0.894965 0.077 Uiso 1 1 calc GR . . . .
H26C H 1.238784 0.863512 0.764665 0.077 Uiso 1 1 calc GR . . . .
C4 C 1.2099(5) 0.1639(5) 1.0622(5) 0.0620(17) Uani 1 1 d . . . . .
H4 H 1.172572 0.194203 1.112441 0.074 Uiso 1 1 calc R . . . .
C27 C 1.0611(5) 0.9158(5) 0.8990(5) 0.0553(16) Uani 1 1 d . . . . .
H27A H 1.010431 0.963956 0.858810 0.083 Uiso 1 1 calc GR . . . .
H27B H 1.125534 0.947771 0.944583 0.083 Uiso 1 1 calc GR . . . .
H27C H 1.022251 0.878283 0.945833 0.083 Uiso 1 1 calc GR . . . .
C30 C 0.7703(7) 0.0663(5) 1.0820(6) 0.0681(19) Uani 1 1 d . . . . .
H30 H 0.772102 0.018411 1.136516 0.082 Uiso 1 1 calc R . . . .
C29 C 0.8671(6) 0.0957(6) 1.0557(7) 0.076(2) Uani 1 1 d . . . . .
H29 H 0.934990 0.065899 1.089945 0.091 Uiso 1 1 calc R . . . .
C33 C 0.7667(5) 0.2081(4) 0.9274(5) 0.0522(15) Uani 1 1 d . . . . .
C53 C 0.6084(5) 0.8655(5) 0.9366(6) 0.069(2) Uani 1 1 d . . . . .
H53A H 0.537979 0.895045 0.943615 0.103 Uiso 1 1 calc GR . . . .
H53B H 0.670580 0.902274 0.979291 0.103 Uiso 1 1 calc GR . . . .
H53C H 0.611481 0.799518 0.964154 0.103 Uiso 1 1 calc GR . . . .
C31 C 0.6705(6) 0.1049(5) 1.0309(6) 0.0618(18) Uani 1 1 d . . . . .
H31 H 0.603355 0.082425 1.048226 0.074 Uiso 1 1 calc R . . . .
C28 C 0.8685(5) 0.1689(6) 0.9794(6) 0.073(2) Uani 1 1 d . . . . .
H28 H 0.936433 0.191071 0.963503 0.088 Uiso 1 1 calc R . . . .
C54 C 0.6665(5) 0.9480(5) 0.7799(6) 0.067(2) Uani 1 1 d . . . . .
H54A H 0.697291 0.931256 0.715917 0.101 Uiso 1 1 calc GR . . . .
H54B H 0.726300 0.971535 0.838793 0.101 Uiso 1 1 calc GR . . . .
H54C H 0.610137 0.998175 0.759533 0.101 Uiso 1 1 calc GR . . . .
S2A S 0.5347(11) 0.2083(8) 0.9126(9) 0.060(4) Uani 0.224(9) 1 d . . P A 2
N3A N 0.699(3) 0.2839(19) 0.843(2) 0.043(2) Uani 0.224(9) 1 d . . P 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
S1 0.0581(8) 0.0465(9) 0.0471(9) 0.0011(8) 0.0165(6) 0.0083(8)
S2 0.0435(14) 0.0500(14) 0.0530(13) 0.0114(10) 0.0120(9) -0.0003(11)
N1 0.058(3) 0.045(3) 0.049(3) 0.009(2) 0.011(2) 0.012(2)
N3 0.039(5) 0.039(5) 0.052(5) 0.000(4) 0.011(3) -0.010(4)
C38 0.044(3) 0.021(3) 0.036(3) -0.002(2) 0.007(2) -0.004(2)
N4 0.061(3) 0.046(3) 0.064(4) -0.010(3) 0.009(3) -0.013(3)
N2 0.046(3) 0.045(3) 0.070(4) -0.021(3) 0.008(2) -0.004(2)
C10 0.051(3) 0.035(3) 0.031(3) -0.001(3) 0.007(2) -0.011(3)
C24 0.043(3) 0.032(3) 0.047(3) -0.001(3) 0.011(2) 0.001(3)
C8 0.043(3) 0.030(3) 0.039(3) 0.000(2) 0.009(2) -0.008(2)
C15 0.045(3) 0.035(3) 0.038(3) 0.005(3) 0.013(2) -0.004(3)
C11 0.047(3) 0.025(3) 0.034(3) 0.002(2) 0.009(2) -0.006(2)
C23 0.051(3) 0.026(3) 0.046(3) 0.002(3) 0.007(2) 0.004(3)
C14 0.045(3) 0.039(3) 0.031(3) 0.006(3) 0.009(2) -0.004(3)
C20 0.043(3) 0.030(3) 0.034(3) 0.006(3) 0.011(2) 0.004(3)
C34 0.048(3) 0.028(3) 0.041(3) 0.006(3) 0.007(2) -0.002(3)
C12 0.052(3) 0.034(3) 0.042(3) 0.002(3) 0.011(2) -0.002(3)
C21 0.049(3) 0.027(3) 0.042(3) 0.002(3) 0.013(2) 0.004(3)
C22 0.042(3) 0.034(3) 0.043(3) 0.007(3) 0.011(2) 0.003(3)
C9 0.047(3) 0.031(3) 0.043(3) -0.005(3) 0.013(2) -0.001(3)
C41 0.049(3) 0.036(3) 0.035(3) -0.002(3) 0.008(2) 0.001(3)
C25 0.042(3) 0.033(3) 0.046(3) 0.005(3) 0.009(2) 0.003(3)
C39 0.037(3) 0.037(3) 0.044(3) -0.001(3) 0.010(2) -0.005(3)
C35 0.049(3) 0.026(3) 0.032(3) -0.001(2) 0.003(2) 0.002(2)
C7 0.042(3) 0.032(3) 0.041(3) -0.001(3) 0.016(2) -0.005(2)
C37 0.052(3) 0.028(3) 0.036(3) 0.001(2) 0.009(2) -0.004(3)
C16 0.040(3) 0.043(4) 0.043(3) 0.002(3) 0.010(2) 0.001(3)
C48 0.050(3) 0.032(3) 0.040(3) 0.004(3) 0.015(2) -0.001(3)
C6 0.041(3) 0.035(3) 0.042(3) -0.003(3) 0.012(2) -0.005(2)
C13 0.057(3) 0.027(3) 0.038(3) -0.003(3) 0.011(3) -0.002(3)
C36 0.044(3) 0.028(3) 0.041(3) 0.000(3) 0.010(2) 0.002(2)
C47 0.042(3) 0.027(3) 0.045(3) -0.001(3) 0.011(2) 0.005(3)
C19 0.051(3) 0.039(3) 0.040(3) -0.001(3) 0.008(2) -0.008(3)
C50 0.044(3) 0.029(3) 0.055(4) -0.011(3) 0.013(2) 0.002(3)
C42 0.045(3) 0.033(3) 0.043(3) 0.001(3) 0.010(2) 0.007(3)
C18 0.048(3) 0.051(4) 0.045(4) 0.001(3) 0.003(3) -0.017(3)
C49 0.051(3) 0.046(3) 0.040(3) -0.004(3) 0.010(2) -0.005(3)
C2 0.045(3) 0.038(3) 0.069(5) 0.004(3) 0.012(3) -0.003(3)
C45 0.052(3) 0.045(4) 0.050(4) -0.007(3) -0.003(3) 0.006(3)
C3 0.074(4) 0.052(4) 0.041(4) 0.006(3) 0.005(3) 0.007(3)
C1 0.052(3) 0.045(4) 0.061(4) 0.004(3) 0.017(3) -0.002(3)
C5 0.048(3) 0.037(3) 0.049(3) 0.002(3) 0.006(2) 0.001(3)
C51 0.047(3) 0.029(3) 0.066(4) 0.003(3) 0.018(3) 0.004(3)
C44 0.058(4) 0.051(4) 0.052(4) -0.008(3) -0.002(3) 0.019(3)
C17 0.041(3) 0.053(4) 0.046(4) 0.008(3) 0.007(2) -0.005(3)
C43 0.062(3) 0.037(3) 0.050(4) 0.003(3) 0.010(3) 0.008(3)
C46 0.051(3) 0.031(3) 0.049(4) -0.007(3) 0.008(3) -0.003(3)
C40 0.051(3) 0.035(3) 0.043(3) 0.006(3) 0.008(2) -0.002(3)
C52 0.052(3) 0.032(3) 0.048(4) 0.005(3) 0.013(3) 0.008(3)
C32 0.056(3) 0.039(3) 0.048(3) -0.006(3) 0.004(3) -0.003(3)
C26 0.055(3) 0.040(3) 0.057(4) -0.004(3) 0.006(3) -0.002(3)
C4 0.079(4) 0.060(4) 0.047(4) -0.004(3) 0.013(3) 0.017(4)
C27 0.064(4) 0.047(4) 0.052(4) -0.009(3) 0.007(3) -0.006(3)
C30 0.108(6) 0.043(4) 0.049(4) 0.001(3) 0.008(4) 0.006(4)
C29 0.072(5) 0.060(5) 0.083(6) -0.007(4) -0.011(4) 0.025(4)
C33 0.070(4) 0.048(4) 0.040(3) -0.001(3) 0.014(3) -0.002(3)
C53 0.071(4) 0.055(4) 0.071(5) -0.014(4) -0.007(3) -0.018(4)
C31 0.080(4) 0.046(4) 0.060(4) -0.012(4) 0.017(3) -0.014(4)
C28 0.051(4) 0.092(6) 0.077(5) -0.018(5) 0.015(3) 0.003(4)
C54 0.049(3) 0.053(4) 0.097(6) -0.024(4) 0.009(3) -0.004(3)
S2A 0.076(8) 0.043(6) 0.055(6) 0.008(4) 0.004(5) -0.006(5)
N3A 0.039(5) 0.039(5) 0.052(5) 0.000(4) 0.011(3) -0.010(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 C7 1.750(5) . ?
S1 C6 1.736(6) . ?
S2 C34 1.771(5) . ?
S2 C33 1.714(6) . ?
N1 C7 1.308(7) . ?
N1 C5 1.405(7) . ?
N3 C34 1.232(11) . ?
N3 C32 1.419(10) . ?
C38 C41 1.501(7) . ?
C38 C39 1.388(7) . ?
C38 C37 1.397(7) . ?
N4 C50 1.404(7) . ?
N4 C53 1.516(9) . ?
N4 C54 1.437(8) . ?
N2 C23 1.371(7) . ?
N2 C26 1.459(6) . ?
N2 C27 1.445(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.413(8) . ?
C10 C9 1.384(7) . ?
C24 H24 0.9500 . ?
C24 C23 1.398(7) . ?
C24 C25 1.377(7) . ?
C8 C9 1.392(7) . ?
C8 C7 1.474(7) . ?
C8 C13 1.394(7) . ?
C15 C14 1.422(8) . ?
C15 C20 1.491(7) . ?
C15 C16 1.387(7) . ?
C11 C14 1.485(7) . ?
C11 C12 1.391(7) . ?
C23 C22 1.420(8) . ?
C14 C19 1.393(7) . ?
C20 C21 1.404(7) . ?
C20 C25 1.381(8) . ?
C34 C35 1.466(7) . ?
C34 S2A 1.862(13) . ?
C34 N3A 1.16(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.380(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.380(7) . ?
C22 H22 0.9500 . ?
C9 H9 0.9500 . ?
C41 C42 1.398(8) . ?
C41 C46 1.389(8) . ?
C25 H25 0.9500 . ?
C39 H39 0.9500 . ?
C39 C40 1.386(7) . ?
C35 C36 1.391(7) . ?
C35 C40 1.407(7) . ?
C37 H37 0.9500 . ?
C37 C36 1.395(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(8) . ?
C48 H48 0.9500 . ?
C48 C47 1.387(7) . ?
C48 C49 1.377(7) . ?
C6 C1 1.402(8) . ?
C6 C5 1.371(8) . ?
C13 H13 0.9500 . ?
C36 H36 0.9500 . ?
C47 C42 1.496(7) . ?
C47 C52 1.393(8) . ?
C19 H19 0.9500 . ?
C19 C18 1.376(8) . ?
C50 C49 1.405(8) . ?
C50 C51 1.392(8) . ?
C42 C43 1.400(8) . ?
C18 H18 0.9500 . ?
C18 C17 1.382(8) . ?
C49 H49 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.373(9) . ?
C2 C1 1.390(8) . ?
C45 H45 0.9500 . ?
C45 C44 1.377(9) . ?
C45 C46 1.382(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(8) . ?
C1 H1 0.9500 . ?
C5 C4 1.391(8) . ?
C51 H51 0.9500 . ?
C51 C52 1.393(8) . ?
C44 H44 0.9500 . ?
C44 C43 1.388(8) . ?
C17 H17 0.9500 . ?
C43 H43 0.9500 . ?
C46 H46 0.9500 . ?
C40 H40 0.9500 . ?
C52 H52 0.9500 . ?
C32 C33 1.395(8) . ?
C32 C31 1.385(9) . ?
C32 S2A 1.666(14) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C4 H4 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C30 H30 0.9500 . ?
C30 C29 1.362(10) . ?
C30 C31 1.368(9) . ?
C29 H29 0.9500 . ?
C29 C28 1.398(11) . ?
C33 C28 1.395(9) . ?
C33 N3A 1.59(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C31 H31 0.9500 . ?
C28 H28 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 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
C6 S1 C7 89.2(3) . . ?
C33 S2 C34 87.7(3) . . ?
C7 N1 C5 110.4(5) . . ?
C34 N3 C32 115.4(7) . . ?
C39 C38 C41 120.8(4) . . ?
C39 C38 C37 118.7(5) . . ?
C37 C38 C41 120.4(5) . . ?
C50 N4 C53 118.7(5) . . ?
C50 N4 C54 120.4(5) . . ?
C54 N4 C53 115.6(5) . . ?
C23 N2 C26 120.6(5) . . ?
C23 N2 C27 120.3(5) . . ?
C27 N2 C26 118.5(5) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 121.1(5) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C25 C24 C23 122.0(5) . . ?
C9 C8 C7 120.6(5) . . ?
C9 C8 C13 119.2(5) . . ?
C13 C8 C7 120.1(5) . . ?
C14 C15 C20 122.3(5) . . ?
C16 C15 C14 118.6(5) . . ?
C16 C15 C20 119.1(5) . . ?
C10 C11 C14 120.9(5) . . ?
C12 C11 C10 117.4(5) . . ?
C12 C11 C14 121.4(5) . . ?
N2 C23 C24 122.5(5) . . ?
N2 C23 C22 121.6(5) . . ?
C24 C23 C22 115.9(5) . . ?
C15 C14 C11 123.3(5) . . ?
C19 C14 C15 118.2(5) . . ?
C19 C14 C11 118.3(5) . . ?
C21 C20 C15 122.2(5) . . ?
C25 C20 C15 120.7(4) . . ?
C25 C20 C21 117.0(5) . . ?
N3 C34 S2 114.6(5) . . ?
N3 C34 C35 126.0(5) . . ?
C35 C34 S2 119.3(4) . . ?
C35 C34 S2A 114.1(5) . . ?
N3A C34 C35 130.3(14) . . ?
N3A C34 S2A 115.5(14) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 C11 121.8(5) . . ?
C13 C12 H12 119.1 . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.3(5) . . ?
C22 C21 H21 119.4 . . ?
C23 C22 H22 119.2 . . ?
C21 C22 C23 121.6(5) . . ?
C21 C22 H22 119.2 . . ?
C10 C9 C8 120.2(5) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C42 C41 C38 122.6(5) . . ?
C46 C41 C38 118.2(5) . . ?
C46 C41 C42 119.2(5) . . ?
C24 C25 C20 122.2(5) . . ?
C24 C25 H25 118.9 . . ?
C20 C25 H25 118.9 . . ?
C38 C39 H39 119.3 . . ?
C40 C39 C38 121.3(5) . . ?
C40 C39 H39 119.3 . . ?
C36 C35 C34 121.5(5) . . ?
C36 C35 C40 118.6(5) . . ?
C40 C35 C34 119.9(5) . . ?
N1 C7 S1 115.1(4) . . ?
N1 C7 C8 123.9(5) . . ?
C8 C7 S1 121.0(4) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 C38 120.3(5) . . ?
C36 C37 H37 119.8 . . ?
C15 C16 H16 119.1 . . ?
C15 C16 C17 121.8(5) . . ?
C17 C16 H16 119.1 . . ?
C47 C48 H48 118.6 . . ?
C49 C48 H48 118.6 . . ?
C49 C48 C47 122.8(5) . . ?
C1 C6 S1 128.8(5) . . ?
C5 C6 S1 110.0(4) . . ?
C5 C6 C1 121.2(5) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.2(5) . . ?
C12 C13 H13 119.9 . . ?
C35 C36 C37 120.8(5) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C48 C47 C42 121.4(5) . . ?
C48 C47 C52 116.2(5) . . ?
C52 C47 C42 122.3(5) . . ?
C14 C19 H19 118.9 . . ?
C18 C19 C14 122.2(5) . . ?
C18 C19 H19 118.9 . . ?
N4 C50 C49 120.5(5) . . ?
C51 C50 N4 122.3(5) . . ?
C51 C50 C49 117.1(5) . . ?
C41 C42 C47 122.7(5) . . ?
C41 C42 C43 118.7(5) . . ?
C43 C42 C47 118.4(5) . . ?
C19 C18 H18 120.2 . . ?
C19 C18 C17 119.5(5) . . ?
C17 C18 H18 120.2 . . ?
C48 C49 C50 120.8(5) . . ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 . . ?
C3 C2 H2 119.6 . . ?
C3 C2 C1 120.8(6) . . ?
C1 C2 H2 119.6 . . ?
C44 C45 H45 120.9 . . ?
C44 C45 C46 118.3(5) . . ?
C46 C45 H45 120.9 . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.5(6) . . ?
C4 C3 H3 119.2 . . ?
C6 C1 H1 121.2 . . ?
C2 C1 C6 117.5(6) . . ?
C2 C1 H1 121.2 . . ?
C6 C5 N1 115.3(5) . . ?
C6 C5 C4 120.5(5) . . ?
C4 C5 N1 124.2(5) . . ?
C50 C51 H51 119.5 . . ?
C50 C51 C52 121.0(5) . . ?
C52 C51 H51 119.5 . . ?
C45 C44 H44 119.4 . . ?
C45 C44 C43 121.1(6) . . ?
C43 C44 H44 119.4 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.5(5) . . ?
C18 C17 H17 120.2 . . ?
C42 C43 H43 119.8 . . ?
C44 C43 C42 120.3(6) . . ?
C44 C43 H43 119.8 . . ?
C41 C46 H46 118.9 . . ?
C45 C46 C41 122.2(5) . . ?
C45 C46 H46 118.9 . . ?
C39 C40 C35 120.1(5) . . ?
C39 C40 H40 120.0 . . ?
C35 C40 H40 120.0 . . ?
C47 C52 H52 119.0 . . ?
C51 C52 C47 122.0(5) . . ?
C51 C52 H52 119.0 . . ?
C33 C32 N3 109.1(6) . . ?
C33 C32 S2A 133.9(7) . . ?
C31 C32 N3 131.3(7) . . ?
C31 C32 C33 119.6(6) . . ?
C31 C32 S2A 106.5(6) . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 C4 C5 118.5(6) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C30 H30 119.6 . . ?
C29 C30 C31 120.8(7) . . ?
C31 C30 H30 119.6 . . ?
C30 C29 H29 119.3 . . ?
C30 C29 C28 121.4(6) . . ?
C28 C29 H29 119.3 . . ?
C32 C33 S2 113.1(5) . . ?
C32 C33 C28 120.7(6) . . ?
C32 C33 N3A 90.1(13) . . ?
C28 C33 S2 126.1(5) . . ?
C28 C33 N3A 149.2(14) . . ?
N4 C53 H53A 109.5 . . ?
N4 C53 H53B 109.5 . . ?
N4 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C32 C31 H31 120.1 . . ?
C30 C31 C32 119.8(6) . . ?
C30 C31 H31 120.1 . . ?
C29 C28 H28 121.2 . . ?
C33 C28 C29 117.6(6) . . ?
C33 C28 H28 121.2 . . ?
N4 C54 H54A 109.5 . . ?
N4 C54 H54B 109.5 . . ?
N4 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C32 S2A C34 78.8(6) . . ?
C34 N3A C33 122(2) . . ?
_shelx_res_file
;
TITL 180124_xiamin_5_a.res in P2(1)
180124_xiamin_5.res
created by SHELXL-2016/6 at 11:08:29 on 25-Jan-2018
REM Old TITL 180124_xiamin_5 in P21/m #11
REM SHELXT solution in P2(1)
REM R1 0.173, Rweak 0.029, Alpha 0.001, Orientation as input
REM Flack x = 0.494 ( 0.080 ) from Parsons' quotients
REM Formula found by SHELXT: C55 N3 S2
CELL 0.71073 12.2955 13.9512 12.4705 90 102.145 90
ZERR 4 0.0011 0.0011 0.0014 0 0.009 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N S
UNIT 108 88 8 4
EADP N3 N3A
L.S. 5
PLAN 20
SIZE 0.2 0.4 0.48
TEMP -93.15
BOND $H
htab
list 4
fmap 2
acta
SHEL 999 0.83
REM
REM
REM
WGHT 0.068300
FVAR 0.36276 0.77624
S1 4 1.185302 0.183503 0.746826 11.00000 0.05812 0.04653 =
0.04711 0.00110 0.01655 0.00835
PART 1
S2 4 0.747774 0.300180 0.834414 21.00000 0.04353 0.05005 =
0.05302 0.01138 0.01195 -0.00025
PART 0
N1 3 1.108804 0.259322 0.905712 11.00000 0.05835 0.04480 =
0.04903 0.00851 0.01136 0.01202
PART 1
N3 3 0.577663 0.229760 0.891449 21.00000 0.03916 0.03947 =
0.05232 0.00012 0.01071 -0.00998
PART 0
C38 1 0.374798 0.474318 0.617537 11.00000 0.04425 0.02053 =
0.03606 -0.00232 0.00709 -0.00375
N4 3 0.616523 0.864709 0.816962 11.00000 0.06134 0.04601 =
0.06418 -0.00986 0.00917 -0.01331
N2 3 1.098212 0.852753 0.821991 11.00000 0.04588 0.04509 =
0.06998 -0.02095 0.00840 -0.00443
C10 1 0.946806 0.390681 0.546980 11.00000 0.05145 0.03456 =
0.03121 -0.00131 0.00737 -0.01115
AFIX 43
H10 2 0.938888 0.386252 0.469703 11.00000 -1.20000
AFIX 0
C24 1 0.908814 0.801104 0.747606 11.00000 0.04306 0.03204 =
0.04654 -0.00087 0.01112 0.00091
AFIX 43
H24 2 0.881487 0.844932 0.793951 11.00000 -1.20000
AFIX 0
C8 1 1.030311 0.333781 0.727715 11.00000 0.04317 0.03023 =
0.03874 -0.00043 0.00869 -0.00784
C15 1 0.785240 0.618536 0.532750 11.00000 0.04474 0.03536 =
0.03759 0.00481 0.01301 -0.00382
C11 1 0.884926 0.460038 0.591192 11.00000 0.04727 0.02461 =
0.03421 0.00155 0.00908 -0.00607
C23 1 1.023354 0.796327 0.752655 11.00000 0.05142 0.02631 =
0.04570 0.00168 0.00711 0.00365
C14 1 0.798396 0.518385 0.518775 11.00000 0.04529 0.03908 =
0.03129 0.00636 0.00925 -0.00449
C20 1 0.868382 0.676754 0.610221 11.00000 0.04276 0.02998 =
0.03442 0.00649 0.01123 0.00371
C34 1 0.603483 0.292633 0.832007 11.00000 0.04804 0.02830 =
0.04103 0.00640 0.00687 -0.00191
C12 1 0.901054 0.465231 0.704826 11.00000 0.05168 0.03449 =
0.04195 0.00196 0.01146 -0.00200
AFIX 43
H12 2 0.861971 0.512400 0.736713 11.00000 -1.20000
AFIX 0
C21 1 0.983086 0.670065 0.614016 11.00000 0.04896 0.02670 =
0.04156 0.00163 0.01328 0.00418
AFIX 43
H21 2 1.009392 0.625041 0.568255 11.00000 -1.20000
AFIX 0
C22 1 1.058370 0.727621 0.682930 11.00000 0.04227 0.03443 =
0.04283 0.00706 0.01056 0.00289
AFIX 43
H22 2 1.135452 0.721127 0.683746 11.00000 -1.20000
AFIX 0
C9 1 1.018764 0.329087 0.614383 11.00000 0.04707 0.03091 =
0.04271 -0.00484 0.01308 -0.00097
AFIX 43
H9 2 1.060416 0.283454 0.583209 11.00000 -1.20000
AFIX 0
C41 1 0.293367 0.531828 0.535911 11.00000 0.04852 0.03648 =
0.03541 -0.00168 0.00803 0.00147
C25 1 0.834410 0.744152 0.677432 11.00000 0.04242 0.03324 =
0.04605 0.00485 0.00938 0.00343
AFIX 43
H25 2 0.757144 0.751464 0.675176 11.00000 -1.20000
AFIX 0
C39 1 0.338300 0.411778 0.689111 11.00000 0.03657 0.03731 =
0.04364 -0.00107 0.00955 -0.00477
AFIX 43
H39 2 0.261177 0.408545 0.689363 11.00000 -1.20000
AFIX 0
C35 1 0.526290 0.356320 0.759289 11.00000 0.04923 0.02608 =
0.03217 -0.00141 0.00270 0.00232
C7 1 1.102715 0.265511 0.799917 11.00000 0.04245 0.03186 =
0.04064 -0.00070 0.01636 -0.00476
C37 1 0.488547 0.478995 0.618801 11.00000 0.05203 0.02788 =
0.03609 0.00066 0.00898 -0.00404
AFIX 43
H37 2 0.515268 0.523024 0.572250 11.00000 -1.20000
AFIX 0
C16 1 0.693341 0.663857 0.469397 11.00000 0.04002 0.04273 =
0.04343 0.00248 0.00978 0.00076
AFIX 43
H16 2 0.682236 0.730219 0.480395 11.00000 -1.20000
AFIX 0
C48 1 0.401026 0.684047 0.708518 11.00000 0.05045 0.03197 =
0.03967 0.00360 0.01452 -0.00102
AFIX 43
H48 2 0.356801 0.638839 0.737136 11.00000 -1.20000
AFIX 0
C6 1 1.236570 0.141576 0.878876 11.00000 0.04111 0.03525 =
0.04238 -0.00329 0.01178 -0.00487
C13 1 0.972265 0.403749 0.772513 11.00000 0.05705 0.02665 =
0.03841 -0.00275 0.01136 -0.00153
AFIX 43
H13 2 0.981750 0.409131 0.849869 11.00000 -1.20000
AFIX 0
C36 1 0.563097 0.419346 0.688066 11.00000 0.04414 0.02767 =
0.04137 0.00039 0.00971 0.00157
AFIX 43
H36 2 0.639983 0.421785 0.686592 11.00000 -1.20000
AFIX 0
C47 1 0.390175 0.689739 0.595684 11.00000 0.04192 0.02726 =
0.04511 -0.00095 0.01103 0.00548
C19 1 0.722254 0.471735 0.436935 11.00000 0.05136 0.03922 =
0.03999 -0.00052 0.00758 -0.00827
AFIX 43
H19 2 0.732002 0.405322 0.425004 11.00000 -1.20000
AFIX 0
C50 1 0.540197 0.809220 0.742676 11.00000 0.04392 0.02860 =
0.05452 -0.01106 0.01333 0.00159
C42 1 0.307130 0.629835 0.519375 11.00000 0.04524 0.03281 =
0.04301 0.00124 0.00987 0.00729
C18 1 0.633406 0.518564 0.372784 11.00000 0.04791 0.05078 =
0.04523 0.00143 0.00287 -0.01655
AFIX 43
H18 2 0.583567 0.484971 0.316804 11.00000 -1.20000
AFIX 0
C49 1 0.473137 0.741101 0.780802 11.00000 0.05062 0.04556 =
0.03976 -0.00429 0.00967 -0.00501
AFIX 43
H49 2 0.477600 0.734322 0.857407 11.00000 -1.20000
AFIX 0
C2 1 1.345843 0.052115 1.026199 11.00000 0.04485 0.03821 =
0.06882 0.00407 0.01173 -0.00334
AFIX 43
H2 2 1.402647 0.006811 1.053364 11.00000 -1.20000
AFIX 0
C45 1 0.130483 0.529557 0.387350 11.00000 0.05179 0.04532 =
0.05011 -0.00701 -0.00302 0.00554
AFIX 43
H45 2 0.069185 0.495940 0.344671 11.00000 -1.20000
AFIX 0
C3 1 1.290475 0.096160 1.097492 11.00000 0.07411 0.05187 =
0.04104 0.00583 0.00502 0.00719
AFIX 43
H3 2 1.308328 0.079335 1.172979 11.00000 -1.20000
AFIX 0
C1 1 1.319727 0.073058 0.914750 11.00000 0.05235 0.04549 =
0.06117 0.00431 0.01669 -0.00183
AFIX 43
H1 2 1.356816 0.042118 0.864761 11.00000 -1.20000
AFIX 0
C5 1 1.184293 0.187253 0.951315 11.00000 0.04754 0.03676 =
0.04928 0.00229 0.00639 0.00146
C51 1 0.529468 0.816613 0.629642 11.00000 0.04703 0.02940 =
0.06645 0.00276 0.01803 0.00379
AFIX 43
H51 2 0.573303 0.862020 0.600819 11.00000 -1.20000
AFIX 0
C44 1 0.148538 0.624661 0.367245 11.00000 0.05779 0.05067 =
0.05194 -0.00757 -0.00224 0.01890
AFIX 43
H44 2 0.101170 0.656078 0.307586 11.00000 -1.20000
AFIX 0
C17 1 0.617173 0.614846 0.390364 11.00000 0.04098 0.05292 =
0.04620 0.00777 0.00688 -0.00483
AFIX 43
H17 2 0.554347 0.647252 0.348666 11.00000 -1.20000
AFIX 0
C43 1 0.234748 0.675410 0.432640 11.00000 0.06158 0.03658 =
0.05010 0.00334 0.00956 0.00803
AFIX 43
H43 2 0.244707 0.741390 0.418496 11.00000 -1.20000
AFIX 0
C46 1 0.203867 0.484272 0.471246 11.00000 0.05126 0.03117 =
0.04918 -0.00739 0.00764 -0.00292
AFIX 43
H46 2 0.192699 0.418433 0.485123 11.00000 -1.20000
AFIX 0
C40 1 0.412087 0.353974 0.760192 11.00000 0.05121 0.03470 =
0.04338 0.00648 0.00770 -0.00233
AFIX 43
H40 2 0.385515 0.312706 0.809598 11.00000 -1.20000
AFIX 0
C52 1 0.455455 0.758469 0.558108 11.00000 0.05249 0.03244 =
0.04836 0.00534 0.01307 0.00811
AFIX 43
H52 2 0.449296 0.765904 0.481339 11.00000 -1.20000
AFIX 0
C32 1 0.667737 0.176979 0.953935 11.00000 0.05619 0.03924 =
0.04787 -0.00623 0.00418 -0.00331
C26 1 1.217524 0.839645 0.831268 11.00000 0.05487 0.04023 =
0.05674 -0.00429 0.00606 -0.00238
AFIX 137
H26A 2 1.235803 0.771355 0.840406 11.00000 -1.50000
H26B 2 1.258149 0.875260 0.894965 11.00000 -1.50000
H26C 2 1.238784 0.863512 0.764665 11.00000 -1.50000
AFIX 0
C4 1 1.209938 0.163927 1.062236 11.00000 0.07897 0.05969 =
0.04700 -0.00407 0.01252 0.01696
AFIX 43
H4 2 1.172572 0.194203 1.112441 11.00000 -1.20000
AFIX 0
C27 1 1.061125 0.915757 0.898996 11.00000 0.06433 0.04699 =
0.05239 -0.00938 0.00706 -0.00611
AFIX 137
H27A 2 1.010431 0.963956 0.858810 11.00000 -1.50000
H27B 2 1.125534 0.947771 0.944583 11.00000 -1.50000
H27C 2 1.022251 0.878283 0.945833 11.00000 -1.50000
AFIX 0
C30 1 0.770299 0.066318 1.082032 11.00000 0.10847 0.04337 =
0.04892 0.00102 0.00844 0.00561
AFIX 43
H30 2 0.772102 0.018411 1.136516 11.00000 -1.20000
AFIX 0
C29 1 0.867077 0.095719 1.055725 11.00000 0.07249 0.06026 =
0.08262 -0.00728 -0.01054 0.02464
AFIX 43
H29 2 0.934990 0.065899 1.089945 11.00000 -1.20000
AFIX 0
C33 1 0.766662 0.208101 0.927444 11.00000 0.06984 0.04765 =
0.03996 -0.00068 0.01367 -0.00227
C53 1 0.608425 0.865452 0.936575 11.00000 0.07149 0.05457 =
0.07057 -0.01352 -0.00665 -0.01765
AFIX 137
H53A 2 0.537979 0.895045 0.943615 11.00000 -1.50000
H53B 2 0.670580 0.902274 0.979291 11.00000 -1.50000
H53C 2 0.611481 0.799518 0.964154 11.00000 -1.50000
AFIX 0
C31 1 0.670539 0.104945 1.030939 11.00000 0.08017 0.04637 =
0.05974 -0.01153 0.01702 -0.01420
AFIX 43
H31 2 0.603355 0.082425 1.048226 11.00000 -1.20000
AFIX 0
C28 1 0.868510 0.168867 0.979411 11.00000 0.05109 0.09218 =
0.07684 -0.01798 0.01488 0.00346
AFIX 43
H28 2 0.936433 0.191071 0.963503 11.00000 -1.20000
AFIX 0
C54 1 0.666536 0.948039 0.779853 11.00000 0.04889 0.05293 =
0.09739 -0.02385 0.00940 -0.00367
AFIX 137
H54A 2 0.697291 0.931256 0.715917 11.00000 -1.50000
H54B 2 0.726300 0.971535 0.838793 11.00000 -1.50000
H54C 2 0.610137 0.998175 0.759533 11.00000 -1.50000
AFIX 0
PART 2
S2A 4 0.534742 0.208290 0.912581 -21.00000 0.07598 0.04307 =
0.05521 0.00781 0.00353 -0.00588
N3A 3 0.699003 0.283913 0.843353 -21.00000 0.03916 0.03947 =
0.05232 0.00012 0.01071 -0.00998
HKLF 4
REM 180124_xiamin_5_a.res in P2(1)
REM R1 = 0.0555 for 4526 Fo > 4sig(Fo) and 0.0800 for all 5954 data
REM 558 parameters refined using 1 restraints
END
WGHT 0.0683 0.0000
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, y+1/2, -z+2
HTAB C49 S2A_$1
HTAB C53 S2A_$1
HTAB C28 N1
REM Highest difference peak 0.267, deepest hole -0.228, 1-sigma level 0.047
Q1 1 0.7256 0.9868 0.8828 11.00000 0.05 0.27
Q2 1 0.6886 0.9612 0.7369 11.00000 0.05 0.22
Q3 1 0.8426 1.0554 0.8933 11.00000 0.05 0.20
Q4 1 0.8676 0.0817 0.9746 11.00000 0.05 0.20
Q5 1 0.8499 0.4064 0.8154 11.00000 0.05 0.19
Q6 1 0.6228 0.6294 0.6612 11.00000 0.05 0.19
Q7 1 0.8439 0.7149 0.6087 11.00000 0.05 0.19
Q8 1 1.0461 0.2477 0.5219 11.00000 0.05 0.19
Q9 1 0.7049 0.9564 0.9763 11.00000 0.05 0.18
Q10 1 0.7931 0.3620 0.6863 11.00000 0.05 0.18
Q11 1 0.5244 0.5002 0.2215 11.00000 0.05 0.17
Q12 1 0.5968 0.8760 0.9815 11.00000 0.05 0.17
Q13 1 1.4194 0.0851 0.8871 11.00000 0.05 0.17
Q14 1 1.3578 0.0356 0.7816 11.00000 0.05 0.17
Q15 1 1.1944 0.2512 0.6665 11.00000 0.05 0.16
Q16 1 0.1377 0.6924 0.2000 11.00000 0.05 0.16
Q17 1 1.2011 0.1946 0.9727 11.00000 0.05 0.16
Q18 1 0.8373 0.1030 0.9208 11.00000 0.05 0.16
Q19 1 0.7118 0.5815 0.2798 11.00000 0.05 0.16
Q20 1 1.0884 0.2678 0.9805 11.00000 0.05 0.16
;
_shelx_res_checksum 20740
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation Luminescent
#######################################################################
#
# 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_180504_xm0425_2
_database_code_depnum_ccdc_archive 'CCDC 1844322'
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;
_audit_creation_date 2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C27 H22 N2 S'
_chemical_formula_sum 'C27 H22 N2 S'
_chemical_formula_weight 406.52
_chemical_melting_point ?
_chemical_oxdiff_formula 'C H N O'
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'
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/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 41.697(4)
_cell_length_b 11.1157(11)
_cell_length_c 9.2068(8)
_cell_angle_alpha 90
_cell_angle_beta 93.753(6)
_cell_angle_gamma 90
_cell_volume 4258.1(7)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 2632
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 29.3412
_cell_measurement_theta_min 3.1569
_shelx_estimated_absorpt_T_max 0.978
_shelx_estimated_absorpt_T_min 0.922
_exptl_absorpt_coefficient_mu 0.168
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67695
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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 1.268
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1712
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.13
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0693
_diffrn_reflns_av_unetI/netI 0.0905
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 50
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 18819
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 3.163
_diffrn_ambient_temperature 293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 22.00 70.00 0.7500 130.0000
omega____ theta____ kappa____ phi______ frames
- 11.9371 -130.0000 142.0000 64
#__ type_ start__ end____ width___ exp.time_
2 omega -69.00 87.00 0.7500 130.0000
omega____ theta____ kappa____ phi______ frames
- 11.9371 0.0000 60.0000 208
;
_diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0170324000
_diffrn_orient_matrix_UB_12 -0.0020439000
_diffrn_orient_matrix_UB_13 -0.0068781000
_diffrn_orient_matrix_UB_21 -0.0003639000
_diffrn_orient_matrix_UB_22 0.0591261000
_diffrn_orient_matrix_UB_23 -0.0290906000
_diffrn_orient_matrix_UB_31 0.0005805000
_diffrn_orient_matrix_UB_32 -0.0239312000
_diffrn_orient_matrix_UB_33 -0.0711810000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4103
_reflns_number_total 7765
_reflns_odcompleteness_completeness 99.62
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.183
_refine_diff_density_min -0.252
_refine_diff_density_rms 0.050
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 545
_refine_ls_number_reflns 7765
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1337
_refine_ls_R_factor_gt 0.0649
_refine_ls_restrained_S_all 1.020
_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^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1275
_refine_ls_wR_factor_ref 0.1622
_refine_special_details ?
_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:
C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25),
C28(H28), C29(H29), C30(H30), C31(H31), C36(H36), C37(H37), C38(H38),
C39(H39), C42(H42), C43(H43), C44(H44), C46(H46), C48(H48), C49(H49), C51(H51),
C52(H52)
2.b Idealised Me refined as rotating group:
C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C53(H53A,H53B,H53C), C54(H54A,H54B,
H54C)
;
_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
S1 S 0.10217(2) 0.54491(9) 0.48835(9) 0.0607(3) Uani 1 1 d . . . . .
N1 N 0.04284(7) 0.4845(3) 0.4347(3) 0.0623(8) Uani 1 1 d . . . . .
N2 N 0.30311(8) 0.3538(3) 0.3652(3) 0.0733(9) Uani 1 1 d . . . . .
C1 C 0.08230(9) 0.7692(3) 0.3685(4) 0.0650(10) Uani 1 1 d . . . . .
H1 H 0.102870 0.801597 0.380596 0.078 Uiso 1 1 calc R . . . .
C2 C 0.05723(11) 0.8364(4) 0.3080(4) 0.0727(11) Uani 1 1 d . . . . .
H2 H 0.060917 0.915084 0.279043 0.087 Uiso 1 1 calc R . . . .
C3 C 0.02666(11) 0.7891(4) 0.2896(4) 0.0817(12) Uani 1 1 d . . . . .
H3 H 0.010046 0.836384 0.248634 0.098 Uiso 1 1 calc R . . . .
C4 C 0.02037(10) 0.6735(4) 0.3308(4) 0.0824(12) Uani 1 1 d . . . . .
H4 H -0.000317 0.642301 0.318239 0.099 Uiso 1 1 calc R . . . .
C5 C 0.04551(8) 0.6034(3) 0.3918(3) 0.0563(9) Uani 1 1 d . . . . .
C6 C 0.07633(8) 0.6515(3) 0.4114(3) 0.0538(9) Uani 1 1 d . . . . .
C7 C 0.07025(8) 0.4419(3) 0.4860(3) 0.0525(8) Uani 1 1 d . . . . .
C8 C 0.07376(8) 0.3141(3) 0.5309(3) 0.0542(9) Uani 1 1 d . . . . .
C9 C 0.04832(10) 0.2379(4) 0.4876(4) 0.0745(11) Uani 1 1 d . . . . .
H9 H 0.030566 0.268790 0.433662 0.089 Uiso 1 1 calc R . . . .
C10 C 0.04910(11) 0.1174(4) 0.5237(5) 0.0826(12) Uani 1 1 d . . . . .
H10 H 0.031878 0.068050 0.494126 0.099 Uiso 1 1 calc R . . . .
C11 C 0.07497(12) 0.0702(4) 0.6024(4) 0.0776(12) Uani 1 1 d . . . . .
H11 H 0.075529 -0.010969 0.626703 0.093 Uiso 1 1 calc R . . . .
C12 C 0.10041(10) 0.1451(4) 0.6455(4) 0.0717(11) Uani 1 1 d . . . . .
H12 H 0.118055 0.113068 0.699237 0.086 Uiso 1 1 calc R . . . .
C13 C 0.10028(9) 0.2664(3) 0.6107(3) 0.0558(9) Uani 1 1 d . . . . .
C14 C 0.12901(9) 0.3371(3) 0.6651(3) 0.0557(9) Uani 1 1 d . . . . .
C15 C 0.15752(8) 0.3311(3) 0.5963(3) 0.0569(9) Uani 1 1 d . . . . .
H15 H 0.158163 0.285197 0.512061 0.068 Uiso 1 1 calc R . . . .
C16 C 0.18544(9) 0.3914(3) 0.6487(3) 0.0556(9) Uani 1 1 d . . . . .
C17 C 0.18326(10) 0.4582(3) 0.7760(3) 0.0663(10) Uani 1 1 d . . . . .
H17 H 0.201294 0.499122 0.814878 0.080 Uiso 1 1 calc R . . . .
C18 C 0.15519(12) 0.4651(3) 0.8453(4) 0.0761(12) Uani 1 1 d . . . . .
H18 H 0.154569 0.510859 0.929583 0.091 Uiso 1 1 calc R . . . .
C19 C 0.12769(10) 0.4050(3) 0.7921(3) 0.0696(11) Uani 1 1 d . . . . .
H19 H 0.108782 0.409933 0.840071 0.083 Uiso 1 1 calc R . . . .
C20 C 0.21583(8) 0.3821(3) 0.5746(3) 0.0554(9) Uani 1 1 d . . . . .
C21 C 0.22162(9) 0.2899(3) 0.4778(3) 0.0606(9) Uani 1 1 d . . . . .
H21 H 0.205920 0.231363 0.460064 0.073 Uiso 1 1 calc R . . . .
C22 C 0.24943(9) 0.2817(3) 0.4075(4) 0.0622(9) Uani 1 1 d . . . . .
H22 H 0.251723 0.219111 0.342057 0.075 Uiso 1 1 calc R . . . .
C23 C 0.27449(9) 0.3642(3) 0.4308(3) 0.0593(9) Uani 1 1 d . . . . .
C24 C 0.26881(9) 0.4586(3) 0.5277(4) 0.0633(10) Uani 1 1 d . . . . .
H24 H 0.284468 0.517265 0.545504 0.076 Uiso 1 1 calc R . . . .
C25 C 0.24062(9) 0.4657(3) 0.5964(4) 0.0631(10) Uani 1 1 d . . . . .
H25 H 0.237942 0.529155 0.660374 0.076 Uiso 1 1 calc R . . . .
C26 C 0.30671(10) 0.2617(3) 0.2581(4) 0.0767(11) Uani 1 1 d . . . . .
H26A H 0.304056 0.184185 0.301607 0.115 Uiso 1 1 calc GR . . . .
H26B H 0.327739 0.267055 0.221863 0.115 Uiso 1 1 calc GR . . . .
H26C H 0.290749 0.272362 0.179161 0.115 Uiso 1 1 calc GR . . . .
C27 C 0.32689(10) 0.4475(4) 0.3798(4) 0.0840(12) Uani 1 1 d . . . . .
H27A H 0.318260 0.520205 0.336782 0.126 Uiso 1 1 calc GR . . . .
H27B H 0.345584 0.423745 0.331401 0.126 Uiso 1 1 calc GR . . . .
H27C H 0.332702 0.460995 0.481145 0.126 Uiso 1 1 calc GR . . . .
S2 S 0.41420(2) 0.71735(9) 0.01812(11) 0.0705(3) Uani 1 1 d . . . . .
N3 N 0.45492(6) 0.6150(3) -0.1411(3) 0.0616(8) Uani 1 1 d . . . . .
N4 N 0.18735(7) 0.6327(3) 0.1588(3) 0.0686(8) Uani 1 1 d . . . . .
C28 C 0.44492(11) 0.9317(4) -0.0563(4) 0.0863(12) Uani 1 1 d . . . . .
H28 H 0.431523 0.978561 -0.002502 0.104 Uiso 1 1 calc R . . . .
C29 C 0.46822(12) 0.9832(4) -0.1321(5) 0.0921(13) Uani 1 1 d . . . . .
H29 H 0.470726 1.066327 -0.129188 0.111 Uiso 1 1 calc R . . . .
C30 C 0.48841(10) 0.9150(5) -0.2136(5) 0.0863(13) Uani 1 1 d . . . . .
H30 H 0.504244 0.952576 -0.263960 0.104 Uiso 1 1 calc R . . . .
C31 C 0.48503(9) 0.7924(4) -0.2201(4) 0.0759(11) Uani 1 1 d . . . . .
H31 H 0.498396 0.746294 -0.274924 0.091 Uiso 1 1 calc R . . . .
C32 C 0.46116(8) 0.7377(3) -0.1428(3) 0.0576(9) Uani 1 1 d . . . . .
C33 C 0.44159(8) 0.8075(3) -0.0613(3) 0.0601(9) Uani 1 1 d . . . . .
C34 C 0.43092(8) 0.5925(3) -0.0634(3) 0.0539(8) Uani 1 1 d . . . . .
C35 C 0.41865(8) 0.4707(3) -0.0348(3) 0.0553(9) Uani 1 1 d . . . . .
C36 C 0.44080(9) 0.3847(4) 0.0172(4) 0.0743(11) Uani 1 1 d . . . . .
H36 H 0.462597 0.403240 0.023305 0.089 Uiso 1 1 calc R . . . .
C37 C 0.43096(11) 0.2724(4) 0.0600(5) 0.0865(12) Uani 1 1 d . . . . .
H37 H 0.446030 0.216223 0.095397 0.104 Uiso 1 1 calc R . . . .
C38 C 0.39879(11) 0.2437(4) 0.0502(5) 0.0851(12) Uani 1 1 d . . . . .
H38 H 0.392011 0.168800 0.081027 0.102 Uiso 1 1 calc R . . . .
C39 C 0.37656(9) 0.3267(3) -0.0058(4) 0.0684(10) Uani 1 1 d . . . . .
H39 H 0.354924 0.305838 -0.014199 0.082 Uiso 1 1 calc R . . . .
C40 C 0.38577(8) 0.4410(3) -0.0499(3) 0.0540(8) Uani 1 1 d . . . . .
C41 C 0.36069(8) 0.5245(3) -0.1156(3) 0.0502(8) Uani 1 1 d . . . . .
C42 C 0.36516(9) 0.5873(3) -0.2434(3) 0.0614(9) Uani 1 1 d . . . . .
H42 H 0.384161 0.578515 -0.289886 0.074 Uiso 1 1 calc R . . . .
C43 C 0.34124(9) 0.6627(3) -0.3009(4) 0.0642(10) Uani 1 1 d . . . . .
H43 H 0.344546 0.705952 -0.385005 0.077 Uiso 1 1 calc R . . . .
C44 C 0.31261(8) 0.6749(3) -0.2360(3) 0.0559(9) Uani 1 1 d . . . . .
H44 H 0.296884 0.725964 -0.277333 0.067 Uiso 1 1 calc R . . . .
C45 C 0.30674(7) 0.6118(3) -0.1087(3) 0.0458(8) Uani 1 1 d . . . . .
C46 C 0.33185(7) 0.5385(3) -0.0508(3) 0.0496(8) Uani 1 1 d . . . . .
H46 H 0.328993 0.497307 0.035358 0.059 Uiso 1 1 calc R . . . .
C47 C 0.27585(7) 0.6192(3) -0.0399(3) 0.0454(8) Uani 1 1 d . . . . .
C48 C 0.25499(8) 0.7159(3) -0.0609(3) 0.0557(9) Uani 1 1 d . . . . .
H48 H 0.260639 0.779037 -0.120448 0.067 Uiso 1 1 calc R . . . .
C49 C 0.22601(8) 0.7211(3) 0.0043(4) 0.0592(9) Uani 1 1 d . . . . .
H49 H 0.212719 0.787546 -0.012518 0.071 Uiso 1 1 calc R . . . .
C50 C 0.21627(8) 0.6291(3) 0.0948(3) 0.0526(8) Uani 1 1 d . . . . .
C51 C 0.23708(8) 0.5324(3) 0.1158(3) 0.0556(9) Uani 1 1 d . . . . .
H51 H 0.231609 0.469405 0.175894 0.067 Uiso 1 1 calc R . . . .
C52 C 0.26575(8) 0.5279(3) 0.0492(3) 0.0552(9) Uani 1 1 d . . . . .
H52 H 0.278864 0.460805 0.064694 0.066 Uiso 1 1 calc R . . . .
C53 C 0.17911(9) 0.5391(4) 0.2572(4) 0.0823(12) Uani 1 1 d . . . . .
H53A H 0.177752 0.463724 0.206322 0.123 Uiso 1 1 calc GR . . . .
H53B H 0.158748 0.556991 0.295224 0.123 Uiso 1 1 calc GR . . . .
H53C H 0.195328 0.534007 0.335965 0.123 Uiso 1 1 calc GR . . . .
C54 C 0.16581(10) 0.7328(4) 0.1379(5) 0.0952(14) Uani 1 1 d . . . . .
H54A H 0.175790 0.803879 0.179291 0.143 Uiso 1 1 calc GR . . . .
H54B H 0.146370 0.716565 0.184831 0.143 Uiso 1 1 calc GR . . . .
H54C H 0.160843 0.744951 0.035690 0.143 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
S1 0.0542(6) 0.0601(6) 0.0669(5) 0.0016(4) -0.0022(4) -0.0008(5)
N1 0.0501(19) 0.057(2) 0.0801(19) -0.0012(15) 0.0066(14) 0.0001(16)
N2 0.075(2) 0.067(2) 0.076(2) -0.0100(17) -0.0068(16) -0.0105(19)
C1 0.064(2) 0.062(3) 0.069(2) 0.0020(19) 0.0060(17) 0.001(2)
C2 0.086(3) 0.060(3) 0.072(2) 0.0051(19) 0.005(2) 0.010(2)
C3 0.074(3) 0.073(3) 0.096(3) 0.006(2) -0.012(2) 0.019(3)
C4 0.063(3) 0.072(3) 0.110(3) 0.000(2) -0.006(2) 0.008(2)
C5 0.054(2) 0.054(2) 0.060(2) -0.0029(17) 0.0003(15) 0.003(2)
C6 0.052(2) 0.059(2) 0.0503(18) -0.0033(16) 0.0022(14) 0.0015(19)
C7 0.048(2) 0.057(2) 0.0537(18) -0.0051(16) 0.0073(14) 0.0032(18)
C8 0.059(2) 0.052(2) 0.0529(18) -0.0056(17) 0.0144(16) 0.000(2)
C9 0.067(3) 0.062(3) 0.095(3) 0.000(2) 0.007(2) 0.001(2)
C10 0.082(3) 0.067(3) 0.101(3) -0.001(2) 0.027(2) -0.015(3)
C11 0.102(4) 0.061(3) 0.073(2) 0.012(2) 0.033(2) 0.007(3)
C12 0.091(3) 0.068(3) 0.058(2) 0.0059(19) 0.0160(19) 0.003(3)
C13 0.074(3) 0.050(2) 0.0445(17) 0.0006(16) 0.0157(16) 0.007(2)
C14 0.076(3) 0.047(2) 0.0421(18) -0.0016(15) -0.0079(16) 0.0099(19)
C15 0.071(2) 0.054(2) 0.0451(17) -0.0045(16) -0.0057(16) 0.007(2)
C16 0.080(3) 0.036(2) 0.0478(18) -0.0010(15) -0.0204(17) 0.0088(19)
C17 0.098(3) 0.048(2) 0.049(2) -0.0051(17) -0.0235(19) 0.013(2)
C18 0.121(4) 0.063(3) 0.0425(19) -0.0087(18) -0.015(2) 0.025(3)
C19 0.098(3) 0.062(3) 0.048(2) 0.0002(18) -0.0027(18) 0.018(2)
C20 0.066(2) 0.045(2) 0.0524(18) -0.0029(16) -0.0183(16) 0.0024(19)
C21 0.073(3) 0.043(2) 0.063(2) -0.0106(17) -0.0172(18) -0.0073(19)
C22 0.075(3) 0.050(2) 0.059(2) -0.0115(17) -0.0133(18) -0.001(2)
C23 0.072(3) 0.045(2) 0.057(2) 0.0004(17) -0.0253(18) -0.004(2)
C24 0.073(3) 0.040(2) 0.074(2) -0.0057(18) -0.0215(19) -0.005(2)
C25 0.077(3) 0.042(2) 0.067(2) -0.0112(17) -0.0239(19) -0.001(2)
C26 0.094(3) 0.065(3) 0.069(2) 0.002(2) -0.0028(19) -0.001(2)
C27 0.084(3) 0.072(3) 0.094(3) -0.003(2) -0.009(2) -0.018(3)
S2 0.0656(6) 0.0586(6) 0.0900(7) -0.0191(5) 0.0257(5) -0.0074(5)
N3 0.0487(18) 0.063(2) 0.0735(18) -0.0015(16) 0.0102(14) 0.0046(16)
N4 0.059(2) 0.072(2) 0.0747(19) 0.0001(17) 0.0004(15) 0.0097(18)
C28 0.101(3) 0.065(3) 0.094(3) -0.008(2) 0.020(2) -0.015(3)
C29 0.109(4) 0.068(3) 0.100(3) 0.003(3) 0.009(3) -0.021(3)
C30 0.074(3) 0.091(4) 0.095(3) 0.019(3) 0.008(2) -0.022(3)
C31 0.051(2) 0.090(3) 0.087(3) 0.009(2) 0.0129(18) -0.001(2)
C32 0.043(2) 0.065(3) 0.063(2) 0.0029(19) -0.0003(15) -0.0035(19)
C33 0.054(2) 0.059(3) 0.067(2) -0.0099(18) 0.0060(16) -0.008(2)
C34 0.044(2) 0.053(2) 0.065(2) -0.0113(17) -0.0002(15) 0.0035(17)
C35 0.049(2) 0.050(2) 0.066(2) -0.0095(17) 0.0014(15) -0.0001(19)
C36 0.053(2) 0.068(3) 0.102(3) -0.004(2) -0.0036(19) 0.008(2)
C37 0.069(3) 0.060(3) 0.127(3) 0.002(2) -0.014(2) 0.013(2)
C38 0.073(3) 0.054(3) 0.125(3) 0.013(2) -0.009(2) -0.001(2)
C39 0.060(2) 0.054(2) 0.090(3) 0.006(2) -0.0022(18) -0.002(2)
C40 0.056(2) 0.045(2) 0.0603(19) -0.0046(16) -0.0012(15) -0.0038(18)
C41 0.051(2) 0.041(2) 0.0570(19) -0.0017(15) -0.0051(15) -0.0064(17)
C42 0.060(2) 0.065(3) 0.059(2) 0.0015(18) 0.0014(16) -0.010(2)
C43 0.067(3) 0.067(3) 0.057(2) 0.0122(18) -0.0047(18) -0.013(2)
C44 0.063(2) 0.047(2) 0.0558(19) 0.0105(16) -0.0147(16) -0.0066(18)
C45 0.052(2) 0.0368(19) 0.0464(17) -0.0006(14) -0.0126(14) -0.0066(16)
C46 0.052(2) 0.045(2) 0.0501(17) 0.0040(15) -0.0066(15) -0.0081(17)
C47 0.048(2) 0.0357(19) 0.0509(17) -0.0002(14) -0.0113(14) -0.0022(16)
C48 0.062(2) 0.040(2) 0.063(2) 0.0073(16) -0.0117(16) 0.0013(19)
C49 0.060(2) 0.039(2) 0.077(2) 0.0004(18) -0.0138(17) 0.0087(18)
C50 0.050(2) 0.054(2) 0.0528(18) -0.0087(17) -0.0104(15) 0.0061(18)
C51 0.053(2) 0.054(2) 0.0585(19) 0.0129(16) -0.0064(15) 0.0039(19)
C52 0.051(2) 0.043(2) 0.069(2) 0.0129(17) -0.0082(16) 0.0090(17)
C53 0.069(3) 0.098(3) 0.080(3) -0.006(2) 0.0059(19) -0.010(2)
C54 0.074(3) 0.091(3) 0.121(3) -0.012(3) 0.012(2) 0.026(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 C6 1.723(3) . ?
S1 C7 1.755(3) . ?
N1 C5 1.386(4) . ?
N1 C7 1.297(4) . ?
N2 C23 1.377(4) . ?
N2 C26 1.436(4) . ?
N2 C27 1.438(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.373(5) . ?
C1 C6 1.394(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.379(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.369(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.394(5) . ?
C5 C6 1.393(4) . ?
C7 C8 1.484(5) . ?
C8 C9 1.395(5) . ?
C8 C13 1.392(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.380(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.365(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.386(5) . ?
C13 C14 1.492(5) . ?
C14 C15 1.385(5) . ?
C14 C19 1.396(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.402(4) . ?
C16 C17 1.396(4) . ?
C16 C20 1.482(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.371(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.389(4) . ?
C20 C25 1.395(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.367(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.396(5) . ?
C23 C24 1.407(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.373(5) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
S2 C33 1.718(4) . ?
S2 C34 1.745(3) . ?
N3 C32 1.389(4) . ?
N3 C34 1.292(4) . ?
N4 C50 1.377(4) . ?
N4 C53 1.436(5) . ?
N4 C54 1.435(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.359(5) . ?
C28 C33 1.389(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.389(6) . ?
C30 H30 0.9300 . ?
C30 C31 1.371(6) . ?
C31 H31 0.9300 . ?
C31 C32 1.400(5) . ?
C32 C33 1.382(5) . ?
C34 C35 1.478(5) . ?
C35 C36 1.393(5) . ?
C35 C40 1.408(4) . ?
C36 H36 0.9300 . ?
C36 C37 1.379(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.376(5) . ?
C38 H38 0.9300 . ?
C38 C39 1.383(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.396(5) . ?
C40 C41 1.496(4) . ?
C41 C42 1.390(4) . ?
C41 C46 1.386(4) . ?
C42 H42 0.9300 . ?
C42 C43 1.381(5) . ?
C43 H43 0.9300 . ?
C43 C44 1.376(5) . ?
C44 H44 0.9300 . ?
C44 C45 1.401(4) . ?
C45 C46 1.404(4) . ?
C45 C47 1.474(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.389(4) . ?
C47 C52 1.388(4) . ?
C48 H48 0.9300 . ?
C48 C49 1.386(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.396(5) . ?
C50 C51 1.387(4) . ?
C51 H51 0.9300 . ?
C51 C52 1.380(4) . ?
C52 H52 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 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
C6 S1 C7 89.44(17) . . ?
C7 N1 C5 111.5(3) . . ?
C23 N2 C26 119.6(3) . . ?
C23 N2 C27 120.7(3) . . ?
C26 N2 C27 118.6(3) . . ?
C2 C1 H1 120.6 . . ?
C2 C1 C6 118.7(4) . . ?
C6 C1 H1 120.6 . . ?
C1 C2 H2 119.5 . . ?
C1 C2 C3 121.0(4) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.9(4) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 125.1(3) . . ?
N1 C5 C6 114.8(3) . . ?
C6 C5 C4 120.0(3) . . ?
C1 C6 S1 130.1(3) . . ?
C5 C6 S1 109.6(3) . . ?
C5 C6 C1 120.3(3) . . ?
N1 C7 S1 114.6(3) . . ?
N1 C7 C8 121.3(3) . . ?
C8 C7 S1 124.1(3) . . ?
C9 C8 C7 116.3(3) . . ?
C13 C8 C7 124.9(3) . . ?
C13 C8 C9 118.8(3) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.0(4) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.0(4) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 119.1 . . ?
C13 C12 C11 121.8(4) . . ?
C13 C12 H12 119.1 . . ?
C8 C13 C14 124.7(3) . . ?
C12 C13 C8 118.9(3) . . ?
C12 C13 C14 116.4(3) . . ?
C15 C14 C13 121.1(3) . . ?
C15 C14 C19 119.4(3) . . ?
C19 C14 C13 119.4(3) . . ?
C14 C15 H15 118.7 . . ?
C14 C15 C16 122.5(3) . . ?
C16 C15 H15 118.7 . . ?
C15 C16 C20 121.6(3) . . ?
C17 C16 C15 116.4(3) . . ?
C17 C16 C20 121.9(3) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.6(4) . . ?
C18 C17 H17 119.2 . . ?
C17 C18 H18 119.3 . . ?
C17 C18 C19 121.3(3) . . ?
C19 C18 H18 119.3 . . ?
C14 C19 H19 120.7 . . ?
C18 C19 C14 118.6(4) . . ?
C18 C19 H19 120.7 . . ?
C21 C20 C16 122.4(3) . . ?
C21 C20 C25 115.2(3) . . ?
C25 C20 C16 122.4(3) . . ?
C20 C21 H21 118.6 . . ?
C22 C21 C20 122.7(3) . . ?
C22 C21 H21 118.6 . . ?
C21 C22 H22 118.9 . . ?
C21 C22 C23 122.2(3) . . ?
C23 C22 H22 118.9 . . ?
N2 C23 C22 122.7(3) . . ?
N2 C23 C24 121.8(3) . . ?
C22 C23 C24 115.5(4) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H24 119.3 . . ?
C20 C25 H25 118.5 . . ?
C24 C25 C20 122.9(3) . . ?
C24 C25 H25 118.5 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C33 S2 C34 89.14(17) . . ?
C34 N3 C32 110.4(3) . . ?
C50 N4 C53 120.1(3) . . ?
C50 N4 C54 121.6(3) . . ?
C54 N4 C53 118.2(3) . . ?
C29 C28 H28 120.8 . . ?
C29 C28 C33 118.4(4) . . ?
C33 C28 H28 120.8 . . ?
C28 C29 H29 119.1 . . ?
C28 C29 C30 121.8(4) . . ?
C30 C29 H29 119.1 . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.1(4) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.5 . . ?
C30 C31 C32 119.0(4) . . ?
C32 C31 H31 120.5 . . ?
N3 C32 C31 124.9(4) . . ?
C33 C32 N3 115.3(3) . . ?
C33 C32 C31 119.8(4) . . ?
C28 C33 S2 129.3(3) . . ?
C32 C33 S2 109.7(3) . . ?
C32 C33 C28 121.0(3) . . ?
N3 C34 S2 115.5(3) . . ?
N3 C34 C35 124.4(3) . . ?
C35 C34 S2 120.0(2) . . ?
C36 C35 C34 117.4(3) . . ?
C36 C35 C40 119.5(3) . . ?
C40 C35 C34 122.9(3) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 C35 121.1(4) . . ?
C37 C36 H36 119.5 . . ?
C36 C37 H37 120.1 . . ?
C38 C37 C36 119.9(4) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 H38 120.1 . . ?
C37 C38 C39 119.8(4) . . ?
C39 C38 H38 120.1 . . ?
C38 C39 H39 119.2 . . ?
C38 C39 C40 121.7(4) . . ?
C40 C39 H39 119.2 . . ?
C35 C40 C41 123.0(3) . . ?
C39 C40 C35 118.0(3) . . ?
C39 C40 C41 119.0(3) . . ?
C42 C41 C40 121.6(3) . . ?
C46 C41 C40 119.9(3) . . ?
C46 C41 C42 118.5(3) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 C41 119.7(3) . . ?
C43 C42 H42 120.2 . . ?
C42 C43 H43 119.4 . . ?
C44 C43 C42 121.2(3) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 H44 119.4 . . ?
C43 C44 C45 121.2(3) . . ?
C45 C44 H44 119.4 . . ?
C44 C45 C46 116.2(3) . . ?
C44 C45 C47 122.5(3) . . ?
C46 C45 C47 121.3(3) . . ?
C41 C46 C45 123.2(3) . . ?
C41 C46 H46 118.4 . . ?
C45 C46 H46 118.4 . . ?
C48 C47 C45 122.7(3) . . ?
C52 C47 C45 121.4(3) . . ?
C52 C47 C48 115.9(3) . . ?
C47 C48 H48 119.1 . . ?
C49 C48 C47 121.9(3) . . ?
C49 C48 H48 119.1 . . ?
C48 C49 H49 119.2 . . ?
C48 C49 C50 121.6(3) . . ?
C50 C49 H49 119.2 . . ?
N4 C50 C49 122.1(3) . . ?
N4 C50 C51 121.4(3) . . ?
C51 C50 C49 116.6(3) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 C50 121.2(3) . . ?
C52 C51 H51 119.4 . . ?
C47 C52 H52 118.6 . . ?
C51 C52 C47 122.8(3) . . ?
C51 C52 H52 118.6 . . ?
N4 C53 H53A 109.5 . . ?
N4 C53 H53B 109.5 . . ?
N4 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N4 C54 H54A 109.5 . . ?
N4 C54 H54B 109.5 . . ?
N4 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
_shelx_res_file
;
TITL 180504_XM0425_2 in P21/c #14
180504_xm0425_2.res
created by SHELXL-2016/6 at 10:18:54 on 07-May-2018
REM reset to P21/c #14
CELL 0.71073 41.69684 11.11572 9.20678 90 93.7525 90
ZERR 8 0.00358 0.00107 0.00075 0 0.0063 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N S
UNIT 216 176 16 8
L.S. 4
PLAN 20
SIZE 0.49 0.32 0.13
TEMP 20
BOND $h
htab
fmap 2
acta
SHEL 999 0.83
OMIT -31 8 6
OMIT 6 10 7
OMIT 8 10 7
OMIT 7 10 7
OMIT 5 10 7
OMIT 7 0 0
REM
REM
REM
WGHT 0.056100
FVAR 1.27399
S1 4 0.102172 0.544914 0.488346 11.00000 0.05422 0.06007 =
0.06689 0.00164 -0.00222 -0.00077
N1 3 0.042838 0.484466 0.434682 11.00000 0.05010 0.05698 =
0.08006 -0.00121 0.00658 0.00009
N2 3 0.303112 0.353831 0.365169 11.00000 0.07548 0.06666 =
0.07635 -0.00997 -0.00675 -0.01049
C1 1 0.082302 0.769223 0.368515 11.00000 0.06365 0.06236 =
0.06906 0.00202 0.00597 0.00136
AFIX 43
H1 2 0.102870 0.801597 0.380596 11.00000 -1.20000
AFIX 0
C2 1 0.057232 0.836419 0.308048 11.00000 0.08587 0.06033 =
0.07185 0.00506 0.00546 0.01019
AFIX 43
H2 2 0.060917 0.915084 0.279043 11.00000 -1.20000
AFIX 0
C3 1 0.026659 0.789063 0.289647 11.00000 0.07434 0.07270 =
0.09567 0.00578 -0.01181 0.01922
AFIX 43
H3 2 0.010046 0.836384 0.248634 11.00000 -1.20000
AFIX 0
C4 1 0.020373 0.673509 0.330787 11.00000 0.06345 0.07224 =
0.10984 0.00030 -0.00640 0.00826
AFIX 43
H4 2 -0.000317 0.642301 0.318239 11.00000 -1.20000
AFIX 0
C5 1 0.045509 0.603413 0.391805 11.00000 0.05433 0.05431 =
0.05978 -0.00288 0.00032 0.00268
C6 1 0.076331 0.651544 0.411446 11.00000 0.05207 0.05901 =
0.05028 -0.00332 0.00222 0.00152
C7 1 0.070251 0.441928 0.486001 11.00000 0.04764 0.05657 =
0.05374 -0.00515 0.00732 0.00323
C8 1 0.073757 0.314106 0.530939 11.00000 0.05874 0.05233 =
0.05287 -0.00559 0.01438 -0.00005
C9 1 0.048321 0.237896 0.487646 11.00000 0.06710 0.06152 =
0.09524 0.00021 0.00749 0.00053
AFIX 43
H9 2 0.030566 0.268790 0.433662 11.00000 -1.20000
AFIX 0
C10 1 0.049096 0.117414 0.523663 11.00000 0.08197 0.06722 =
0.10128 -0.00077 0.02703 -0.01454
AFIX 43
H10 2 0.031878 0.068050 0.494126 11.00000 -1.20000
AFIX 0
C11 1 0.074973 0.070239 0.602367 11.00000 0.10206 0.06098 =
0.07339 0.01250 0.03350 0.00660
AFIX 43
H11 2 0.075529 -0.010969 0.626703 11.00000 -1.20000
AFIX 0
C12 1 0.100414 0.145100 0.645505 11.00000 0.09092 0.06783 =
0.05790 0.00592 0.01595 0.00296
AFIX 43
H12 2 0.118055 0.113068 0.699237 11.00000 -1.20000
AFIX 0
C13 1 0.100279 0.266383 0.610746 11.00000 0.07387 0.05050 =
0.04449 0.00058 0.01570 0.00741
C14 1 0.129011 0.337063 0.665111 11.00000 0.07623 0.04732 =
0.04211 -0.00156 -0.00788 0.00986
C15 1 0.157516 0.331056 0.596305 11.00000 0.07052 0.05394 =
0.04507 -0.00452 -0.00568 0.00719
AFIX 43
H15 2 0.158163 0.285197 0.512061 11.00000 -1.20000
AFIX 0
C16 1 0.185439 0.391418 0.648702 11.00000 0.07983 0.03581 =
0.04779 -0.00102 -0.02042 0.00880
C17 1 0.183257 0.458225 0.776039 11.00000 0.09845 0.04766 =
0.04909 -0.00513 -0.02345 0.01256
AFIX 43
H17 2 0.201294 0.499122 0.814878 11.00000 -1.20000
AFIX 0
C18 1 0.155194 0.465062 0.845280 11.00000 0.12053 0.06252 =
0.04252 -0.00867 -0.01522 0.02537
AFIX 43
H18 2 0.154569 0.510859 0.929583 11.00000 -1.20000
AFIX 0
C19 1 0.127687 0.405008 0.792113 11.00000 0.09791 0.06167 =
0.04814 0.00020 -0.00267 0.01826
AFIX 43
H19 2 0.108782 0.409933 0.840071 11.00000 -1.20000
AFIX 0
C20 1 0.215835 0.382113 0.574582 11.00000 0.06639 0.04451 =
0.05244 -0.00290 -0.01831 0.00235
C21 1 0.221617 0.289931 0.477801 11.00000 0.07252 0.04340 =
0.06296 -0.01065 -0.01720 -0.00729
AFIX 43
H21 2 0.205920 0.231363 0.460064 11.00000 -1.20000
AFIX 0
C22 1 0.249428 0.281740 0.407547 11.00000 0.07478 0.05009 =
0.05934 -0.01147 -0.01327 -0.00150
AFIX 43
H22 2 0.251723 0.219111 0.342057 11.00000 -1.20000
AFIX 0
C23 1 0.274494 0.364183 0.430774 11.00000 0.07159 0.04516 =
0.05734 0.00036 -0.02530 -0.00403
C24 1 0.268814 0.458555 0.527662 11.00000 0.07311 0.03956 =
0.07363 -0.00571 -0.02145 -0.00488
AFIX 43
H24 2 0.284468 0.517265 0.545504 11.00000 -1.20000
AFIX 0
C25 1 0.240623 0.465729 0.596418 11.00000 0.07709 0.04201 =
0.06659 -0.01124 -0.02387 -0.00101
AFIX 43
H25 2 0.237942 0.529155 0.660374 11.00000 -1.20000
AFIX 0
C26 1 0.306712 0.261725 0.258074 11.00000 0.09432 0.06539 =
0.06921 0.00228 -0.00282 -0.00129
AFIX 137
H26A 2 0.304056 0.184185 0.301607 11.00000 -1.50000
H26B 2 0.327739 0.267055 0.221863 11.00000 -1.50000
H26C 2 0.290749 0.272362 0.179161 11.00000 -1.50000
AFIX 0
C27 1 0.326890 0.447473 0.379844 11.00000 0.08411 0.07187 =
0.09421 -0.00331 -0.00862 -0.01759
AFIX 137
H27A 2 0.318260 0.520205 0.336782 11.00000 -1.50000
H27B 2 0.345584 0.423745 0.331401 11.00000 -1.50000
H27C 2 0.332702 0.460995 0.481145 11.00000 -1.50000
AFIX 0
S2 4 0.414198 0.717351 0.018124 11.00000 0.06565 0.05864 =
0.09002 -0.01908 0.02572 -0.00742
N3 3 0.454915 0.614961 -0.141080 11.00000 0.04875 0.06332 =
0.07352 -0.00148 0.01019 0.00459
N4 3 0.187346 0.632747 0.158830 11.00000 0.05873 0.07178 =
0.07472 0.00009 0.00041 0.00973
C28 1 0.444917 0.931724 -0.056342 11.00000 0.10117 0.06543 =
0.09398 -0.00806 0.02018 -0.01473
AFIX 43
H28 2 0.431523 0.978561 -0.002502 11.00000 -1.20000
AFIX 0
C29 1 0.468222 0.983207 -0.132053 11.00000 0.10893 0.06769 =
0.09987 0.00289 0.00854 -0.02076
AFIX 43
H29 2 0.470726 1.066327 -0.129188 11.00000 -1.20000
AFIX 0
C30 1 0.488412 0.914999 -0.213638 11.00000 0.07365 0.09076 =
0.09471 0.01915 0.00755 -0.02243
AFIX 43
H30 2 0.504244 0.952576 -0.263960 11.00000 -1.20000
AFIX 0
C31 1 0.485035 0.792403 -0.220076 11.00000 0.05136 0.09033 =
0.08723 0.00919 0.01293 -0.00060
AFIX 43
H31 2 0.498396 0.746294 -0.274924 11.00000 -1.20000
AFIX 0
C32 1 0.461163 0.737711 -0.142813 11.00000 0.04345 0.06548 =
0.06333 0.00286 -0.00032 -0.00350
C33 1 0.441588 0.807453 -0.061327 11.00000 0.05421 0.05897 =
0.06748 -0.00991 0.00595 -0.00813
C34 1 0.430923 0.592516 -0.063410 11.00000 0.04378 0.05255 =
0.06503 -0.01132 -0.00018 0.00354
C35 1 0.418646 0.470673 -0.034847 11.00000 0.04919 0.05008 =
0.06644 -0.00946 0.00136 -0.00009
C36 1 0.440803 0.384666 0.017248 11.00000 0.05251 0.06769 =
0.10153 -0.00443 -0.00357 0.00812
AFIX 43
H36 2 0.462597 0.403240 0.023305 11.00000 -1.20000
AFIX 0
C37 1 0.430956 0.272432 0.059989 11.00000 0.06938 0.06015 =
0.12725 0.00166 -0.01422 0.01322
AFIX 43
H37 2 0.446030 0.216223 0.095397 11.00000 -1.20000
AFIX 0
C38 1 0.398786 0.243737 0.050162 11.00000 0.07329 0.05444 =
0.12538 0.01296 -0.00910 -0.00050
AFIX 43
H38 2 0.392011 0.168800 0.081027 11.00000 -1.20000
AFIX 0
C39 1 0.376563 0.326735 -0.005780 11.00000 0.05991 0.05376 =
0.09046 0.00592 -0.00218 -0.00227
AFIX 43
H39 2 0.354924 0.305838 -0.014199 11.00000 -1.20000
AFIX 0
C40 1 0.385774 0.441039 -0.049922 11.00000 0.05570 0.04528 =
0.06028 -0.00461 -0.00122 -0.00377
C41 1 0.360689 0.524540 -0.115626 11.00000 0.05130 0.04110 =
0.05696 -0.00173 -0.00508 -0.00638
C42 1 0.365161 0.587267 -0.243372 11.00000 0.05991 0.06493 =
0.05900 0.00148 0.00140 -0.00984
AFIX 43
H42 2 0.384161 0.578515 -0.289886 11.00000 -1.20000
AFIX 0
C43 1 0.341242 0.662651 -0.300852 11.00000 0.06706 0.06716 =
0.05731 0.01225 -0.00472 -0.01313
AFIX 43
H43 2 0.344546 0.705952 -0.385005 11.00000 -1.20000
AFIX 0
C44 1 0.312615 0.674894 -0.235955 11.00000 0.06250 0.04684 =
0.05585 0.01049 -0.01468 -0.00664
AFIX 43
H44 2 0.296884 0.725964 -0.277333 11.00000 -1.20000
AFIX 0
C45 1 0.306744 0.611813 -0.108692 11.00000 0.05213 0.03683 =
0.04642 -0.00065 -0.01256 -0.00661
C46 1 0.331853 0.538504 -0.050757 11.00000 0.05232 0.04492 =
0.05013 0.00396 -0.00664 -0.00814
AFIX 43
H46 2 0.328993 0.497307 0.035358 11.00000 -1.20000
AFIX 0
C47 1 0.275852 0.619172 -0.039929 11.00000 0.04766 0.03569 =
0.05094 -0.00020 -0.01129 -0.00218
C48 1 0.254993 0.715931 -0.060905 11.00000 0.06241 0.03999 =
0.06273 0.00735 -0.01173 0.00125
AFIX 43
H48 2 0.260639 0.779037 -0.120448 11.00000 -1.20000
AFIX 0
C49 1 0.226009 0.721133 0.004346 11.00000 0.05950 0.03866 =
0.07697 0.00043 -0.01385 0.00872
AFIX 43
H49 2 0.212719 0.787546 -0.012518 11.00000 -1.20000
AFIX 0
C50 1 0.216269 0.629096 0.094796 11.00000 0.04956 0.05369 =
0.05282 -0.00873 -0.01041 0.00615
C51 1 0.237083 0.532385 0.115794 11.00000 0.05295 0.05410 =
0.05847 0.01294 -0.00636 0.00386
AFIX 43
H51 2 0.231609 0.469405 0.175894 11.00000 -1.20000
AFIX 0
C52 1 0.265752 0.527874 0.049200 11.00000 0.05146 0.04340 =
0.06910 0.01286 -0.00823 0.00903
AFIX 43
H52 2 0.278864 0.460805 0.064694 11.00000 -1.20000
AFIX 0
C53 1 0.179111 0.539103 0.257245 11.00000 0.06910 0.09775 =
0.08012 -0.00575 0.00586 -0.01002
AFIX 137
H53A 2 0.177752 0.463724 0.206322 11.00000 -1.50000
H53B 2 0.158748 0.556991 0.295224 11.00000 -1.50000
H53C 2 0.195328 0.534007 0.335965 11.00000 -1.50000
AFIX 0
C54 1 0.165805 0.732813 0.137932 11.00000 0.07436 0.09051 =
0.12139 -0.01183 0.01233 0.02636
AFIX 137
H54A 2 0.175790 0.803879 0.179291 11.00000 -1.50000
H54B 2 0.146370 0.716565 0.184831 11.00000 -1.50000
H54C 2 0.160843 0.744951 0.035690 11.00000 -1.50000
AFIX 0
HKLF 4
REM 180504_XM0425_2 in P21/c #14
REM R1 = 0.0649 for 4103 Fo > 4sig(Fo) and 0.1337 for all 7765 data
REM 545 parameters refined using 0 restraints
END
WGHT 0.0561 0.0000
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.183, deepest hole -0.252, 1-sigma level 0.050
Q1 1 0.4214 0.6766 -0.2792 11.00000 0.05 0.18
Q2 1 0.3980 0.6071 -0.3068 11.00000 0.05 0.18
Q3 1 0.4316 0.9169 0.1617 11.00000 0.05 0.16
Q4 1 0.1110 0.7446 0.2151 11.00000 0.05 0.16
Q5 1 0.1081 -0.0841 0.6986 11.00000 0.05 0.16
Q6 1 0.4495 0.5565 -0.2511 11.00000 0.05 0.15
Q7 1 0.3774 0.7887 -0.2905 11.00000 0.05 0.15
Q8 1 0.4090 0.8826 -0.2563 11.00000 0.05 0.15
Q9 1 0.4015 0.7120 0.2534 11.00000 0.05 0.15
Q10 1 0.4381 0.5986 -0.3066 11.00000 0.05 0.15
Q11 1 0.0996 0.5954 0.6496 11.00000 0.05 0.14
Q12 1 0.0190 0.9937 0.2288 11.00000 0.05 0.14
Q13 1 0.3907 0.7031 0.1220 11.00000 0.05 0.14
Q14 1 0.1221 0.6434 0.2904 11.00000 0.05 0.14
Q15 1 0.3905 0.6945 -0.3144 11.00000 0.05 0.14
Q16 1 0.5191 0.7986 -0.3974 11.00000 0.05 0.14
Q17 1 0.4982 0.6602 -0.3186 11.00000 0.05 0.14
Q18 1 0.3985 0.7833 0.1625 11.00000 0.05 0.14
Q19 1 0.0817 0.1187 0.7050 11.00000 0.05 0.14
Q20 1 0.0894 0.6654 0.2741 11.00000 0.05 0.14
;
_shelx_res_checksum 27703
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation Luminescent