# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# 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_s4613a
_database_code_depnum_ccdc_archive 'CCDC 1812198'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_audit_creation_date 2017-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C15 H27 In O6 S6'
_chemical_formula_sum 'C15 H27 In O6 S6'
_chemical_formula_weight 610.54
_chemical_melting_point ?
_chemical_oxdiff_formula InS4O8C30H20
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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.6588(10)
_cell_length_b 11.3293(5)
_cell_length_c 26.0649(11)
_cell_angle_alpha 90
_cell_angle_beta 114.445(6)
_cell_angle_gamma 90
_cell_volume 5016.0(5)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 4614
_cell_measurement_temperature 150.01(10)
_cell_measurement_theta_max 27.9590
_cell_measurement_theta_min 3.6190
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.468
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.66229
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.617
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 2480
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.08
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0270
_diffrn_reflns_av_unetI/netI 0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 10603
_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 26.372
_diffrn_reflns_theta_min 3.276
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -7.00 90.00 1.00 10.00 -- 18.86 37.00 -60.00 97
2 \w 36.00 95.00 1.00 10.00 -- 18.86 178.00-120.00 59
3 \w -46.00 -8.00 1.00 10.00 -- 18.86 -57.00 -60.00 38
4 \w -81.00 -46.00 1.00 10.00 -- -17.77-178.00 -30.00 35
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0342162000
_diffrn_orient_matrix_UB_12 0.0356365000
_diffrn_orient_matrix_UB_13 0.0118970000
_diffrn_orient_matrix_UB_21 -0.0173071000
_diffrn_orient_matrix_UB_22 0.0417273000
_diffrn_orient_matrix_UB_23 -0.0219943000
_diffrn_orient_matrix_UB_31 -0.0165499000
_diffrn_orient_matrix_UB_32 0.0301532000
_diffrn_orient_matrix_UB_33 0.0163701000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4260
_reflns_number_total 5144
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.609
_refine_diff_density_min -0.505
_refine_diff_density_rms 0.088
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 312
_refine_ls_number_reflns 5144
_refine_ls_number_restraints 19
_refine_ls_R_factor_all 0.0526
_refine_ls_R_factor_gt 0.0394
_refine_ls_restrained_S_all 1.057
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+6.8790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0752
_refine_ls_wR_factor_ref 0.0806
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
C13-C12 \\sim C13A-C12 \\sim C15A-C14A \\sim C15-C14
with sigma of 0.002
O6A-C14A \\sim O6-C14 \\sim O6A-C13A \\sim O6-C13
with sigma of 0.002
C5-C4A \\sim C5-C4
with sigma of 0.002
O2A-C4A \\sim O2-C4 \\sim O2-C3 \\sim O2A-C3
with sigma of 0.002
3. Others
Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(O6A)=Sof(C14A)=
Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
Sof(O6)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H12A)=
Sof(H12B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
Sof(H3BC)=Sof(H3BD)=Sof(H5BD)=Sof(H5BE)=Sof(H5BF)=Sof(O2A)=Sof(C4A)=Sof(H4AA)=
Sof(H4AB)=1-FVAR(2)
Sof(O2)=Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H5AA)=Sof(H5AB)=
Sof(H5AC)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C13(H13A,H13B), C14(H14A,H14B),
C12(H12A,H12B), C12(H12C,H12D), C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD),
C4(H4A,H4B), C13A(H13C,H13D), C14A(H14C,H14D), C4A(H4AA,H4AB)
4.b Me refined with riding coordinates:
C5(H5AA,H5AB,H5AC), C5(H5BD,H5BE,H5BF)
4.c Idealised Me refined as rotating group:
C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F)
;
_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
In1 In 0.82751(2) 0.32465(2) 0.72772(2) 0.02916(8) Uani 1 1 d . . . . .
S3 S 0.87539(6) 0.29439(9) 0.83483(4) 0.0386(2) Uani 1 1 d . . . . .
S4 S 0.93339(5) 0.48018(8) 0.78103(4) 0.0313(2) Uani 1 1 d . . . . .
S5 S 0.90521(5) 0.16665(8) 0.70192(4) 0.0348(2) Uani 1 1 d . . . . .
S6 S 0.82643(5) 0.37090(8) 0.62876(4) 0.0309(2) Uani 1 1 d . . . . .
S1 S 0.69857(5) 0.20843(8) 0.68545(4) 0.0327(2) Uani 1 1 d . . . . .
S2 S 0.70653(5) 0.46449(8) 0.71344(4) 0.0341(2) Uani 1 1 d . . . . .
O3 O 0.97014(14) 0.4592(2) 0.88992(9) 0.0319(6) Uani 1 1 d . . . . .
O4 O 1.11045(16) 0.5226(2) 0.98593(10) 0.0446(7) Uani 1 1 d . . . . .
O6 O 0.8646(6) 0.0807(4) 0.5019(3) 0.054(3) Uani 0.544(12) 1 d D . P A 1
O5 O 0.90420(15) 0.1995(2) 0.60494(10) 0.0339(6) Uani 1 1 d . . . . .
O1 O 0.57742(14) 0.3364(2) 0.66254(11) 0.0377(6) Uani 1 1 d . . . . .
O2 O 0.4133(3) 0.3009(3) 0.6312(2) 0.0372(17) Uani 0.548(9) 1 d D . P B 1
C6 C 0.9302(2) 0.4176(3) 0.83872(14) 0.0285(8) Uani 1 1 d . . . . .
C7 C 1.0138(2) 0.5692(3) 0.89525(15) 0.0356(9) Uani 1 1 d . . . . .
H7A H 0.9780 0.6323 0.8727 0.043 Uiso 1 1 calc R . . . .
H7B H 1.0555 0.5578 0.8815 0.043 Uiso 1 1 calc R . . . .
C8 C 1.0498(2) 0.6026(3) 0.95645(16) 0.0432(10) Uani 1 1 d . . . . .
H8A H 1.0712 0.6837 0.9609 0.052 Uiso 1 1 calc R . . . .
H8B H 1.0093 0.6003 0.9717 0.052 Uiso 1 1 calc R . . . .
C9 C 1.1597(3) 0.5591(5) 1.04032(17) 0.0610(13) Uani 1 1 d . . . . .
H9A H 1.1287 0.5698 1.0629 0.073 Uiso 1 1 calc R . . . .
H9B H 1.1842 0.6357 1.0387 0.073 Uiso 1 1 calc R . . . .
C10 C 1.2223(3) 0.4683(5) 1.06735(19) 0.0764(16) Uani 1 1 d . . . . .
H10A H 1.2532 0.4585 1.0450 0.115 Uiso 1 1 calc GR . . . .
H10B H 1.1978 0.3929 1.0692 0.115 Uiso 1 1 calc GR . . . .
H10C H 1.2570 0.4939 1.1055 0.115 Uiso 1 1 calc GR . . . .
C13 C 0.9060(8) 0.1879(7) 0.5107(4) 0.064(4) Uani 0.544(12) 1 d D . P A 1
H13A H 0.8914 0.2311 0.4748 0.076 Uiso 0.544(12) 1 calc R . P A 1
H13B H 0.9635 0.1739 0.5276 0.076 Uiso 0.544(12) 1 calc R . P A 1
C14 C 0.8736(11) 0.0113(12) 0.4602(4) 0.075(7) Uani 0.544(12) 1 d D . P A 1
H14A H 0.9299 -0.0072 0.4714 0.091 Uiso 0.544(12) 1 calc R . P A 1
H14B H 0.8540 0.0547 0.4240 0.091 Uiso 0.544(12) 1 calc R . P A 1
C12 C 0.8820(3) 0.2561(3) 0.55048(16) 0.0433(10) Uani 1 1 d D . . . .
H12A H 0.9065 0.3353 0.5564 0.052 Uiso 0.544(12) 1 calc R . P A 1
H12B H 0.8242 0.2670 0.5329 0.052 Uiso 0.544(12) 1 calc R . P A 1
H12C H 0.8905 0.3425 0.5542 0.052 Uiso 0.456(12) 1 calc R . P A 2
H12D H 0.8266 0.2395 0.5249 0.052 Uiso 0.456(12) 1 calc R . P A 2
C11 C 0.87977(19) 0.2446(3) 0.64160(14) 0.0279(8) Uani 1 1 d . . . . .
C15 C 0.8275(12) -0.1006(14) 0.4537(9) 0.118(9) Uani 0.544(12) 1 d D . P A 1
H15A H 0.8362 -0.1528 0.4269 0.177 Uiso 0.544(12) 1 calc GR . P A 1
H15B H 0.7714 -0.0818 0.4398 0.177 Uiso 0.544(12) 1 calc GR . P A 1
H15C H 0.8449 -0.1402 0.4903 0.177 Uiso 0.544(12) 1 calc GR . P A 1
C1 C 0.6552(2) 0.3401(3) 0.68582(14) 0.0300(8) Uani 1 1 d . . . . .
C2 C 0.5310(2) 0.4392(3) 0.66261(18) 0.0443(10) Uani 1 1 d . . . . .
H2A H 0.5473 0.5082 0.6467 0.053 Uiso 1 1 calc R . . . .
H2B H 0.5385 0.4585 0.7016 0.053 Uiso 1 1 calc R . . . .
C3 C 0.4484(2) 0.4105(3) 0.62808(17) 0.0426(10) Uani 1 1 d D . . . .
H3AA H 0.4167 0.4726 0.6356 0.051 Uiso 0.548(9) 1 calc R . P B 1
H3AB H 0.4403 0.4203 0.5883 0.051 Uiso 0.548(9) 1 calc R . P B 1
H3BC H 0.4138 0.4805 0.6210 0.051 Uiso 0.452(9) 1 calc R . P B 2
H3BD H 0.4410 0.3738 0.5918 0.051 Uiso 0.452(9) 1 calc R . P B 2
C4 C 0.3952(5) 0.2975(7) 0.6791(3) 0.048(3) Uani 0.548(9) 1 d D . P B 1
H4A H 0.3722 0.3742 0.6826 0.058 Uiso 0.548(9) 1 calc R . P B 1
H4B H 0.4444 0.2862 0.7134 0.058 Uiso 0.548(9) 1 calc R . P B 1
C5 C 0.3411(3) 0.2048(4) 0.6758(2) 0.0638(14) Uani 1 1 d D . . . .
H5AA H 0.3305 0.2061 0.7096 0.096 Uiso 0.548(9) 1 calc R . P B 1
H5AB H 0.2918 0.2165 0.6423 0.096 Uiso 0.548(9) 1 calc R . P B 1
H5AC H 0.3641 0.1285 0.6731 0.096 Uiso 0.548(9) 1 calc R . P B 1
H5BD H 0.2844 0.1924 0.6631 0.096 Uiso 0.452(9) 1 calc R . P B 2
H5BE H 0.3647 0.1352 0.6666 0.096 Uiso 0.452(9) 1 calc R . P B 2
H5BF H 0.3652 0.2175 0.7166 0.096 Uiso 0.452(9) 1 calc R . P B 2
C13A C 0.9385(6) 0.1968(6) 0.5311(5) 0.048(4) Uani 0.456(12) 1 d D . P A 2
H13C H 0.9360 0.2391 0.4972 0.058 Uiso 0.456(12) 1 calc R . P A 2
H13D H 0.9923 0.2081 0.5608 0.058 Uiso 0.456(12) 1 calc R . P A 2
O6A O 0.9287(6) 0.0757(5) 0.5181(3) 0.042(3) Uani 0.456(12) 1 d D . P A 2
C14A C 0.8837(15) 0.0521(14) 0.4607(4) 0.053(5) Uani 0.456(12) 1 d D . P A 2
H14C H 0.9143 0.0719 0.4387 0.064 Uiso 0.456(12) 1 calc R . P A 2
H14D H 0.8353 0.1009 0.4466 0.064 Uiso 0.456(12) 1 calc R . P A 2
C15A C 0.8621(11) -0.0765(15) 0.4538(9) 0.050(4) Uani 0.456(12) 1 d D . P A 2
H15D H 0.8445 -0.0987 0.4141 0.075 Uiso 0.456(12) 1 calc GR . P A 2
H15E H 0.8195 -0.0908 0.4658 0.075 Uiso 0.456(12) 1 calc GR . P A 2
H15F H 0.9081 -0.1238 0.4769 0.075 Uiso 0.456(12) 1 calc GR . P A 2
O2A O 0.4361(3) 0.3283(6) 0.6651(3) 0.042(2) Uani 0.452(9) 1 d D . P B 2
C4A C 0.3544(4) 0.3062(8) 0.6481(5) 0.061(4) Uani 0.452(9) 1 d D . P B 2
H4AA H 0.3292 0.2937 0.6068 0.074 Uiso 0.452(9) 1 calc R . P B 2
H4AB H 0.3297 0.3760 0.6569 0.074 Uiso 0.452(9) 1 calc R . P B 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
In1 0.02703(14) 0.03039(15) 0.02881(13) -0.00415(11) 0.01031(10) -0.00294(11)
S3 0.0470(6) 0.0370(5) 0.0307(5) -0.0025(4) 0.0150(4) -0.0151(4)
S4 0.0295(5) 0.0329(5) 0.0318(4) -0.0020(4) 0.0130(4) -0.0062(4)
S5 0.0341(5) 0.0348(5) 0.0272(4) 0.0011(4) 0.0045(4) 0.0107(4)
S6 0.0317(5) 0.0260(4) 0.0344(5) 0.0035(4) 0.0131(4) 0.0028(4)
S1 0.0302(5) 0.0232(4) 0.0452(5) -0.0041(4) 0.0162(4) -0.0029(4)
S2 0.0294(5) 0.0264(5) 0.0447(5) -0.0094(4) 0.0136(4) -0.0045(4)
O3 0.0349(14) 0.0281(13) 0.0278(12) -0.0055(10) 0.0081(11) -0.0046(11)
O4 0.0457(17) 0.0403(15) 0.0331(14) -0.0080(12) 0.0016(12) 0.0086(13)
O6 0.101(8) 0.030(3) 0.036(3) -0.005(2) 0.031(4) 0.008(3)
O5 0.0379(15) 0.0299(14) 0.0384(14) -0.0043(11) 0.0202(12) -0.0009(11)
O1 0.0264(13) 0.0257(13) 0.0578(17) -0.0085(12) 0.0141(12) -0.0030(11)
O2 0.026(3) 0.025(3) 0.057(4) -0.009(2) 0.014(3) -0.006(2)
C6 0.0271(18) 0.0281(18) 0.0300(17) 0.0002(15) 0.0116(15) 0.0008(15)
C7 0.033(2) 0.0208(17) 0.041(2) -0.0034(16) 0.0030(17) 0.0015(15)
C8 0.041(2) 0.031(2) 0.046(2) -0.0168(18) 0.0063(18) 0.0042(18)
C9 0.048(3) 0.083(4) 0.041(2) -0.016(2) 0.007(2) -0.005(3)
C10 0.062(3) 0.099(4) 0.044(3) 0.015(3) -0.002(2) 0.004(3)
C13 0.092(9) 0.079(9) 0.028(6) -0.002(5) 0.033(6) 0.012(7)
C14 0.088(14) 0.075(15) 0.038(7) -0.008(6) 0.001(6) 0.045(12)
C12 0.066(3) 0.031(2) 0.043(2) -0.0020(18) 0.033(2) -0.013(2)
C11 0.0201(17) 0.0268(18) 0.0331(18) -0.0073(15) 0.0075(14) -0.0040(14)
C15 0.16(2) 0.057(10) 0.074(10) -0.026(8) -0.014(13) 0.042(11)
C1 0.0272(19) 0.0281(18) 0.0357(19) 0.0017(16) 0.0141(15) -0.0019(15)
C2 0.035(2) 0.029(2) 0.065(3) -0.0109(19) 0.017(2) 0.0031(17)
C3 0.033(2) 0.032(2) 0.059(3) 0.005(2) 0.0146(19) 0.0026(17)
C4 0.055(7) 0.033(5) 0.046(5) -0.001(4) 0.011(4) 0.012(5)
C5 0.059(3) 0.050(3) 0.096(4) -0.010(3) 0.047(3) -0.009(2)
C13A 0.095(10) 0.031(6) 0.028(6) -0.010(4) 0.035(7) -0.016(6)
O6A 0.062(7) 0.037(4) 0.029(3) 0.001(3) 0.020(4) -0.001(3)
C14A 0.069(9) 0.025(7) 0.042(8) 0.000(5) -0.001(6) -0.003(6)
C15A 0.065(10) 0.042(8) 0.040(7) -0.010(6) 0.017(7) -0.012(7)
O2A 0.026(4) 0.023(3) 0.068(6) 0.004(4) 0.012(4) -0.006(3)
C4A 0.047(7) 0.062(7) 0.082(9) 0.038(7) 0.034(7) 0.021(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 S3 2.5780(9) . ?
In1 S4 2.5820(9) . ?
In1 S5 2.5622(10) . ?
In1 S6 2.6239(9) . ?
In1 S1 2.5576(9) . ?
In1 S2 2.6549(10) . ?
S3 C6 1.709(4) . ?
S4 C6 1.685(3) . ?
S5 C11 1.691(4) . ?
S6 C11 1.695(3) . ?
S1 C1 1.699(4) . ?
S2 C1 1.689(4) . ?
O3 C6 1.317(4) . ?
O3 C7 1.463(4) . ?
O4 C8 1.404(4) . ?
O4 C9 1.396(4) . ?
O6 C13 1.406(6) . ?
O6 C14 1.406(6) . ?
O5 C12 1.453(4) . ?
O5 C11 1.320(4) . ?
O1 C1 1.321(4) . ?
O1 C2 1.453(4) . ?
O2 C3 1.421(4) . ?
O2 C4 1.424(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.501(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.497(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.502(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.502(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C12 C13A 1.502(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.464(5) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 O2A 1.426(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.434(7) . ?
C5 H5AA 0.9800 . ?
C5 H5AB 0.9800 . ?
C5 H5AC 0.9800 . ?
C5 H5BD 0.9800 . ?
C5 H5BE 0.9800 . ?
C5 H5BF 0.9800 . ?
C5 C4A 1.431(7) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A O6A 1.406(6) . ?
O6A C14A 1.406(6) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C14A C15A 1.502(6) . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
O2A C4A 1.423(4) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
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
S3 In1 S4 70.29(3) . . ?
S3 In1 S6 161.69(3) . . ?
S3 In1 S2 97.16(3) . . ?
S4 In1 S6 94.91(3) . . ?
S4 In1 S2 94.88(3) . . ?
S5 In1 S3 102.19(3) . . ?
S5 In1 S4 103.18(3) . . ?
S5 In1 S6 69.91(3) . . ?
S5 In1 S2 157.03(3) . . ?
S6 In1 S2 94.75(3) . . ?
S1 In1 S3 103.93(3) . . ?
S1 In1 S4 163.14(3) . . ?
S1 In1 S5 93.49(3) . . ?
S1 In1 S6 93.21(3) . . ?
S1 In1 S2 69.71(3) . . ?
C6 S3 In1 83.47(12) . . ?
C6 S4 In1 83.79(12) . . ?
C11 S5 In1 84.69(12) . . ?
C11 S6 In1 82.67(12) . . ?
C1 S1 In1 84.90(12) . . ?
C1 S2 In1 82.03(12) . . ?
C6 O3 C7 117.4(3) . . ?
C9 O4 C8 114.1(3) . . ?
C14 O6 C13 112.1(9) . . ?
C11 O5 C12 119.5(3) . . ?
C1 O1 C2 121.1(3) . . ?
C3 O2 C4 110.8(4) . . ?
S4 C6 S3 122.1(2) . . ?
O3 C6 S3 115.2(2) . . ?
O3 C6 S4 122.7(3) . . ?
O3 C7 H7A 110.2 . . ?
O3 C7 H7B 110.2 . . ?
O3 C7 C8 107.6(3) . . ?
H7A C7 H7B 108.5 . . ?
C8 C7 H7A 110.2 . . ?
C8 C7 H7B 110.2 . . ?
O4 C8 C7 108.9(3) . . ?
O4 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O4 C9 H9A 109.8 . . ?
O4 C9 H9B 109.8 . . ?
O4 C9 C10 109.4(4) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O6 C13 H13A 110.8 . . ?
O6 C13 H13B 110.8 . . ?
O6 C13 C12 104.9(5) . . ?
H13A C13 H13B 108.8 . . ?
C12 C13 H13A 110.8 . . ?
C12 C13 H13B 110.8 . . ?
O6 C14 H14A 110.0 . . ?
O6 C14 H14B 110.0 . . ?
O6 C14 C15 108.3(12) . . ?
H14A C14 H14B 108.4 . . ?
C15 C14 H14A 110.0 . . ?
C15 C14 H14B 110.0 . . ?
O5 C12 C13 113.7(5) . . ?
O5 C12 H12A 108.8 . . ?
O5 C12 H12B 108.8 . . ?
O5 C12 H12C 111.8 . . ?
O5 C12 H12D 111.8 . . ?
O5 C12 C13A 100.1(5) . . ?
C13 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
H12C C12 H12D 109.5 . . ?
C13A C12 H12C 111.8 . . ?
C13A C12 H12D 111.8 . . ?
S5 C11 S6 122.7(2) . . ?
O5 C11 S5 115.0(2) . . ?
O5 C11 S6 122.3(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
S2 C1 S1 123.2(2) . . ?
O1 C1 S1 113.9(2) . . ?
O1 C1 S2 123.0(3) . . ?
O1 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
O1 C2 C3 107.3(3) . . ?
H2A C2 H2B 108.5 . . ?
C3 C2 H2A 110.3 . . ?
C3 C2 H2B 110.3 . . ?
O2 C3 C2 123.5(4) . . ?
O2 C3 H3AA 106.5 . . ?
O2 C3 H3AB 106.5 . . ?
C2 C3 H3AA 106.5 . . ?
C2 C3 H3AB 106.5 . . ?
C2 C3 H3BC 112.0 . . ?
C2 C3 H3BD 112.0 . . ?
H3AA C3 H3AB 106.5 . . ?
H3BC C3 H3BD 109.7 . . ?
O2A C3 C2 98.7(4) . . ?
O2A C3 H3BC 112.0 . . ?
O2A C3 H3BD 112.0 . . ?
O2 C4 H4A 109.1 . . ?
O2 C4 H4B 109.1 . . ?
O2 C4 C5 112.6(5) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C4 C5 H5AA 109.5 . . ?
C4 C5 H5AB 109.5 . . ?
C4 C5 H5AC 109.5 . . ?
H5AA C5 H5AB 109.5 . . ?
H5AA C5 H5AC 109.5 . . ?
H5AB C5 H5AC 109.5 . . ?
H5BD C5 H5BE 109.5 . . ?
H5BD C5 H5BF 109.5 . . ?
H5BE C5 H5BF 109.5 . . ?
C4A C5 H5BD 109.5 . . ?
C4A C5 H5BE 109.5 . . ?
C4A C5 H5BF 109.5 . . ?
C12 C13A H13C 107.7 . . ?
C12 C13A H13D 107.7 . . ?
H13C C13A H13D 107.1 . . ?
O6A C13A C12 118.6(7) . . ?
O6A C13A H13C 107.7 . . ?
O6A C13A H13D 107.7 . . ?
C14A O6A C13A 113.8(9) . . ?
O6A C14A H14C 109.9 . . ?
O6A C14A H14D 109.9 . . ?
O6A C14A C15A 109.0(13) . . ?
H14C C14A H14D 108.3 . . ?
C15A C14A H14C 109.9 . . ?
C15A C14A H14D 109.9 . . ?
C14A C15A H15D 109.5 . . ?
C14A C15A H15E 109.5 . . ?
C14A C15A H15F 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C4A O2A C3 110.9(4) . . ?
C5 C4A H4AA 109.3 . . ?
C5 C4A H4AB 109.3 . . ?
O2A C4A C5 111.8(5) . . ?
O2A C4A H4AA 109.3 . . ?
O2A C4A H4AB 109.3 . . ?
H4AA C4A H4AB 107.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
In1 S3 C6 S4 -5.6(2) . . . . ?
In1 S3 C6 O3 174.9(3) . . . . ?
In1 S4 C6 S3 5.6(2) . . . . ?
In1 S4 C6 O3 -174.9(3) . . . . ?
In1 S5 C11 S6 1.53(19) . . . . ?
In1 S5 C11 O5 -178.1(2) . . . . ?
In1 S6 C11 S5 -1.50(19) . . . . ?
In1 S6 C11 O5 178.1(3) . . . . ?
In1 S1 C1 S2 -4.2(2) . . . . ?
In1 S1 C1 O1 175.8(3) . . . . ?
In1 S2 C1 S1 4.1(2) . . . . ?
In1 S2 C1 O1 -175.9(3) . . . . ?
O3 C7 C8 O4 70.3(4) . . . . ?
O6 C13 C12 O5 62.4(9) . . . . ?
O5 C12 C13A O6A 68.1(9) . . . . ?
O1 C2 C3 O2 43.6(6) . . . . ?
O1 C2 C3 O2A 71.1(5) . . . . ?
C6 O3 C7 C8 176.4(3) . . . . ?
C7 O3 C6 S3 -176.0(2) . . . . ?
C7 O3 C6 S4 4.6(4) . . . . ?
C8 O4 C9 C10 -179.4(4) . . . . ?
C9 O4 C8 C7 166.3(4) . . . . ?
C13 O6 C14 C15 -179.9(11) . . . . ?
C14 O6 C13 C12 173.2(10) . . . . ?
C12 O5 C11 S5 176.8(3) . . . . ?
C12 O5 C11 S6 -2.9(4) . . . . ?
C12 C13A O6A C14A 94.1(18) . . . . ?
C11 O5 C12 C13 -173.4(6) . . . . ?
C11 O5 C12 C13A 165.7(5) . . . . ?
C1 O1 C2 C3 173.3(3) . . . . ?
C2 O1 C1 S1 175.9(3) . . . . ?
C2 O1 C1 S2 -4.0(5) . . . . ?
C2 C3 O2A C4A 166.0(8) . . . . ?
C3 O2 C4 C5 163.8(5) . . . . ?
C3 O2A C4A C5 166.2(7) . . . . ?
C4 O2 C3 C2 78.3(7) . . . . ?
C13A O6A C14A C15A -167.6(15) . . . . ?
_shelx_res_file
;
TITL s4613a C 1 2/c 1 R = 0.05
CELL 0.71073 18.6588 11.3293 26.0649 90 114.445 90
ZERR 8 0.001 0.0005 0.0011 0 0.006 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H In O S
UNIT 120 216 8 48 48
SADI 0.002 C13 C12 C13A C12 C15A C14A C15 C14
SADI 0.002 O6A C14A O6 C14 O6A C13A O6 C13
SADI 0.002 C5 C4A C5 C4
SADI 0.002 O2A C4A O2 C4 O2 C3 O2A C3
L.S. 20
PLAN -20
TEMP -123
BOND $H
CONF
fmap 2
acta
SHEL 100 0.8
REM
REM
REM
WGHT 0.029000 6.879000
FVAR 1.80460 0.54414 0.54775
IN1 3 0.827505 0.324646 0.727720 11.00000 0.02703 0.03039 =
0.02881 -0.00415 0.01031 -0.00294
S3 5 0.875393 0.294388 0.834835 11.00000 0.04695 0.03702 =
0.03069 -0.00252 0.01502 -0.01514
S4 5 0.933385 0.480176 0.781034 11.00000 0.02952 0.03291 =
0.03175 -0.00201 0.01303 -0.00622
S5 5 0.905211 0.166653 0.701923 11.00000 0.03406 0.03484 =
0.02724 0.00111 0.00448 0.01071
S6 5 0.826428 0.370895 0.628764 11.00000 0.03174 0.02599 =
0.03437 0.00345 0.01307 0.00281
S1 5 0.698574 0.208429 0.685445 11.00000 0.03024 0.02318 =
0.04518 -0.00409 0.01622 -0.00290
S2 5 0.706528 0.464487 0.713443 11.00000 0.02939 0.02641 =
0.04473 -0.00939 0.01364 -0.00447
O3 4 0.970144 0.459233 0.889922 11.00000 0.03487 0.02809 =
0.02779 -0.00548 0.00814 -0.00458
O4 4 1.110454 0.522602 0.985932 11.00000 0.04570 0.04030 =
0.03305 -0.00805 0.00163 0.00856
PART 1
O6 4 0.864617 0.080739 0.501875 21.00000 0.10061 0.02968 =
0.03560 -0.00491 0.03086 0.00825
PART 0
O5 4 0.904200 0.199501 0.604936 11.00000 0.03787 0.02994 =
0.03836 -0.00428 0.02015 -0.00089
O1 4 0.577420 0.336372 0.662542 11.00000 0.02638 0.02575 =
0.05779 -0.00852 0.01410 -0.00297
PART 1
O2 4 0.413329 0.300922 0.631162 31.00000 0.02568 0.02499 =
0.05739 -0.00873 0.01377 -0.00577
PART 0
C6 1 0.930244 0.417611 0.838723 11.00000 0.02711 0.02806 =
0.03004 0.00016 0.01164 0.00082
C7 1 1.013844 0.569167 0.895253 11.00000 0.03313 0.02079 =
0.04056 -0.00337 0.00298 0.00146
AFIX 23
H7A 2 0.977965 0.632285 0.872655 11.00000 -1.20000
H7B 2 1.055494 0.557823 0.881483 11.00000 -1.20000
AFIX 0
C8 1 1.049812 0.602552 0.956452 11.00000 0.04076 0.03114 =
0.04597 -0.01678 0.00633 0.00419
AFIX 23
H8A 2 1.071200 0.683727 0.960927 11.00000 -1.20000
H8B 2 1.009262 0.600323 0.971705 11.00000 -1.20000
AFIX 0
C9 1 1.159734 0.559132 1.040318 11.00000 0.04756 0.08297 =
0.04104 -0.01636 0.00691 -0.00512
AFIX 23
H9A 2 1.128673 0.569767 1.062921 11.00000 -1.20000
H9B 2 1.184250 0.635736 1.038708 11.00000 -1.20000
AFIX 0
C10 1 1.222344 0.468256 1.067351 11.00000 0.06194 0.09911 =
0.04417 0.01523 -0.00193 0.00431
AFIX 137
H10A 2 1.253188 0.458547 1.044996 11.00000 -1.50000
H10B 2 1.197801 0.392853 1.069227 11.00000 -1.50000
H10C 2 1.257038 0.493864 1.105531 11.00000 -1.50000
AFIX 0
PART 1
C13 1 0.905995 0.187931 0.510713 21.00000 0.09218 0.07881 =
0.02773 -0.00172 0.03262 0.01243
AFIX 23
H13A 2 0.891373 0.231149 0.474775 21.00000 -1.20000
H13B 2 0.963515 0.173852 0.527556 21.00000 -1.20000
AFIX 0
C14 1 0.873614 0.011316 0.460235 21.00000 0.08818 0.07527 =
0.03793 -0.00776 0.00096 0.04509
AFIX 23
H14A 2 0.929941 -0.007226 0.471425 21.00000 -1.20000
H14B 2 0.853956 0.054695 0.424031 21.00000 -1.20000
AFIX 0
PART 0
C12 1 0.882041 0.256121 0.550484 11.00000 0.06584 0.03128 =
0.04304 -0.00199 0.03284 -0.01258
PART 1
AFIX 23
H12A 2 0.906547 0.335340 0.556355 21.00000 -1.20000
H12B 2 0.824216 0.266998 0.532880 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H12C 2 0.890498 0.342532 0.554240 -21.00000 -1.20000
H12D 2 0.826588 0.239523 0.524858 -21.00000 -1.20000
AFIX 0
PART 0
C11 1 0.879768 0.244639 0.641602 11.00000 0.02015 0.02677 =
0.03310 -0.00726 0.00748 -0.00403
PART 1
C15 1 0.827522 -0.100588 0.453746 21.00000 0.15921 0.05714 =
0.07444 -0.02631 -0.01401 0.04196
AFIX 137
H15A 2 0.836226 -0.152779 0.426882 21.00000 -1.50000
H15B 2 0.771351 -0.081828 0.439775 21.00000 -1.50000
H15C 2 0.844911 -0.140185 0.490346 21.00000 -1.50000
AFIX 0
PART 0
C1 1 0.655169 0.340101 0.685822 11.00000 0.02723 0.02807 =
0.03570 0.00168 0.01409 -0.00191
C2 1 0.530980 0.439233 0.662613 11.00000 0.03471 0.02883 =
0.06532 -0.01094 0.01656 0.00312
AFIX 23
H2A 2 0.547298 0.508249 0.646719 11.00000 -1.20000
H2B 2 0.538522 0.458460 0.701571 11.00000 -1.20000
AFIX 0
C3 1 0.448375 0.410500 0.628079 11.00000 0.03272 0.03161 =
0.05898 0.00534 0.01461 0.00263
PART 1
AFIX 23
H3AA 2 0.416674 0.472637 0.635610 31.00000 -1.20000
H3AB 2 0.440350 0.420296 0.588323 31.00000 -1.20000
AFIX 23
PART 0
PART 2
H3BC 2 0.413833 0.480504 0.621015 -31.00000 -1.20000
H3BD 2 0.441045 0.373804 0.591769 -31.00000 -1.20000
AFIX 0
PART 0
PART 1
C4 1 0.395187 0.297494 0.679103 31.00000 0.05536 0.03331 =
0.04587 -0.00150 0.01069 0.01193
AFIX 23
H4A 2 0.372175 0.374182 0.682615 31.00000 -1.20000
H4B 2 0.444441 0.286184 0.713396 31.00000 -1.20000
AFIX 0
PART 0
C5 1 0.341114 0.204834 0.675785 11.00000 0.05948 0.05020 =
0.09625 -0.01020 0.04667 -0.00859
PART 1
AFIX 33
H5AA 2 0.330536 0.206145 0.709608 31.00000 -1.50000
H5AB 2 0.291783 0.216512 0.642346 31.00000 -1.50000
H5AC 2 0.364058 0.128503 0.673132 31.00000 -1.50000
AFIX 33
PART 0
PART 2
H5BD 2 0.284365 0.192437 0.663085 -31.00000 -1.50000
H5BE 2 0.364670 0.135209 0.666573 -31.00000 -1.50000
H5BF 2 0.365190 0.217459 0.716642 -31.00000 -1.50000
AFIX 0
C13A 1 0.938493 0.196762 0.531123 -21.00000 0.09482 0.03093 =
0.02817 -0.00991 0.03516 -0.01585
AFIX 23
H13C 2 0.936026 0.239054 0.497194 -21.00000 -1.20000
H13D 2 0.992269 0.208094 0.560846 -21.00000 -1.20000
AFIX 0
O6A 4 0.928690 0.075717 0.518135 -21.00000 0.06155 0.03685 =
0.02944 0.00076 0.01958 -0.00119
C14A 1 0.883652 0.052081 0.460734 -21.00000 0.06883 0.02467 =
0.04232 0.00050 -0.00148 -0.00276
AFIX 23
H14C 2 0.914315 0.071908 0.438687 -21.00000 -1.20000
H14D 2 0.835334 0.100944 0.446635 -21.00000 -1.20000
AFIX 0
C15A 1 0.862082 -0.076473 0.453759 -21.00000 0.06510 0.04156 =
0.03998 -0.00983 0.01746 -0.01171
AFIX 137
H15D 2 0.844484 -0.098739 0.414072 -21.00000 -1.50000
H15E 2 0.819547 -0.090756 0.465791 -21.00000 -1.50000
H15F 2 0.908138 -0.123806 0.476863 -21.00000 -1.50000
AFIX 0
O2A 4 0.436123 0.328282 0.665079 -31.00000 0.02569 0.02308 =
0.06849 0.00385 0.01184 -0.00550
C4A 1 0.354424 0.306162 0.648124 -31.00000 0.04743 0.06186 =
0.08162 0.03758 0.03379 0.02149
AFIX 23
H4AA 2 0.329160 0.293734 0.606841 -31.00000 -1.20000
H4AB 2 0.329680 0.376024 0.656934 -31.00000 -1.20000
AFIX 0
HKLF 4
REM s4613a C 1 2/c 1 R = 0.05
REM R1 = 0.0394 for 4260 Fo > 4sig(Fo) and 0.0526 for all 5144 data
REM 312 parameters refined using 19 restraints
END
WGHT 0.0290 6.8722
REM Highest difference peak 0.609, deepest hole -0.505, 1-sigma level 0.088
Q1 1 0.6788 0.2763 0.6799 11.00000 0.05 0.61
Q2 1 0.8631 0.3986 0.7346 11.00000 0.05 0.58
Q3 1 0.7952 0.2508 0.7191 11.00000 0.05 0.55
Q4 1 0.7891 0.3803 0.7198 11.00000 0.05 0.54
Q5 1 0.8558 0.2361 0.7377 11.00000 0.05 0.45
Q6 1 0.8467 0.3065 0.6287 11.00000 0.05 0.44
Q7 1 0.9222 0.2137 0.6854 11.00000 0.05 0.42
Q8 1 0.8247 0.3219 0.6903 11.00000 0.05 0.41
Q9 1 0.6774 0.3962 0.7106 11.00000 0.05 0.40
Q10 1 0.8387 0.3508 0.8246 11.00000 0.05 0.39
Q11 1 0.8925 0.3798 0.8365 11.00000 0.05 0.38
Q12 1 0.8996 0.4178 0.7792 11.00000 0.05 0.36
Q13 1 0.9590 0.4179 0.8069 11.00000 0.05 0.35
Q14 1 0.9051 0.2817 0.8779 11.00000 0.05 0.35
Q15 1 1.0836 0.5429 1.0047 11.00000 0.05 0.34
Q16 1 0.9409 0.3238 0.7881 11.00000 0.05 0.34
Q17 1 0.9496 0.2442 0.6217 11.00000 0.05 0.34
Q18 1 0.8020 0.3216 0.6457 11.00000 0.05 0.34
Q19 1 0.9024 0.2380 0.7870 11.00000 0.05 0.34
Q20 1 0.7395 0.2599 0.6960 11.00000 0.05 0.34
;
_shelx_res_checksum 76081
_olex2_date_sample_data_collection 2017-02-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.665
#######################################################################
#
# 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_s4796l
_database_code_depnum_ccdc_archive 'CCDC 1812202'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_audit_creation_date 2017-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C7 H13 K O2 S2'
_chemical_formula_sum 'C7 H13 K O2 S2'
_chemical_formula_weight 232.39
_chemical_absolute_configuration ad
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 9
_space_group_name_H-M_alt 'C 1 c 1'
_space_group_name_Hall 'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a 8.6583(2)
_cell_length_b 18.7658(4)
_cell_length_c 6.6572(2)
_cell_angle_alpha 90
_cell_angle_beta 95.538(2)
_cell_angle_gamma 90
_cell_volume 1076.61(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6962
_cell_measurement_temperature 149.9(3)
_cell_measurement_theta_max 26.3060
_cell_measurement_theta_min 2.1780
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.842
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.40834
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.434
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 488
_exptl_crystal_size_max 0.421
_exptl_crystal_size_mid 0.072
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0267
_diffrn_reflns_av_unetI/netI 0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 9921
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.368
_diffrn_reflns_theta_min 2.171
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 149.9(3)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -17.00 48.00 1.00 1.00 -- 16.40 60.00 -60.00 65
2 \w 53.00 106.00 1.00 1.00 -- 16.40 60.00 -60.00 53
3 \w -45.00 106.00 1.00 1.00 -- 16.40 57.00-180.00 151
4 \w -60.00 28.00 1.00 1.00 -- 16.40 57.00 90.00 88
5 \w 33.00 106.00 1.00 1.00 -- 16.40 57.00 90.00 73
6 \w -70.00 102.00 1.00 1.00 -- 16.40 60.00 -30.00 172
7 \w -66.00 47.00 1.00 1.00 -- 16.40 60.00-150.00 113
8 \w 51.00 106.00 1.00 1.00 -- 16.40 60.00-150.00 55
9 \w -42.00 106.00 1.00 1.00 -- 16.40 60.00 60.00 148
10 \w -50.00 -21.00 1.00 1.00 -- 16.40 60.00 -60.00 29
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0414229000
_diffrn_orient_matrix_UB_12 -0.0315056000
_diffrn_orient_matrix_UB_13 0.0295437000
_diffrn_orient_matrix_UB_21 -0.0702653000
_diffrn_orient_matrix_UB_22 -0.0196746000
_diffrn_orient_matrix_UB_23 -0.0108114000
_diffrn_orient_matrix_UB_31 0.0110659000
_diffrn_orient_matrix_UB_32 -0.0070177000
_diffrn_orient_matrix_UB_33 -0.1022987000
_diffrn_oxdiff_ac3_digest_frames
;
013ef6d86a4aab218d794348ecbdbc452200947bd73
;
_diffrn_oxdiff_ac3_digest_hkl
;
01783813457d52b01e154e351ce9f5bf8fa19f
;
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.990
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 1.000
_reflns_number_gt 2145
_reflns_number_total 2184
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.319
_refine_diff_density_min -0.196
_refine_diff_density_rms 0.049
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.11(11)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.158
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 113
_refine_ls_number_reflns 2184
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0551
_refine_ls_R_factor_gt 0.0548
_refine_ls_restrained_S_all 1.157
_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^)+(0.1146P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1416
_refine_ls_wR_factor_ref 0.1419
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.89(11)
0.11(11)
2. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_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
K1 K 0.98015(13) 0.42345(6) 0.29736(16) 0.0213(3) Uani 1 1 d . . . . .
S2 S 0.71604(15) 0.44444(7) 0.9278(2) 0.0212(4) Uani 1 1 d . . . . .
S1 S 1.01957(15) 0.40237(7) 0.78083(19) 0.0204(4) Uani 1 1 d . . . . .
O2 O 0.2942(5) 0.3992(2) 0.2943(7) 0.0216(9) Uani 1 1 d . . . . .
O1 O 0.7553(4) 0.3777(2) 0.5859(6) 0.0169(8) Uani 1 1 d . . . . .
C4 C 0.3748(6) 0.3317(3) 0.2849(9) 0.0204(11) Uani 1 1 d . . . . .
C3 C 0.5490(7) 0.3394(3) 0.3501(9) 0.0183(10) Uani 1 1 d . . . . .
H3A H 0.596236 0.292483 0.352052 0.022 Uiso 1 1 calc R . . . .
H3B H 0.595611 0.367619 0.249847 0.022 Uiso 1 1 calc R . . . .
C5 C 0.3483(7) 0.4545(3) 0.1731(10) 0.0242(12) Uani 1 1 d . . . . .
H5A H 0.343976 0.438812 0.035392 0.036 Uiso 1 1 calc GR . . . .
H5B H 0.453398 0.466235 0.220630 0.036 Uiso 1 1 calc GR . . . .
H5C H 0.283898 0.495874 0.181254 0.036 Uiso 1 1 calc GR . . . .
C2 C 0.5865(6) 0.3736(3) 0.5545(8) 0.0184(11) Uani 1 1 d . . . . .
H2A H 0.541307 0.420848 0.556737 0.022 Uiso 1 1 calc R . . . .
H2B H 0.546260 0.345026 0.659055 0.022 Uiso 1 1 calc R . . . .
C6 C 0.3542(7) 0.3010(3) 0.0712(9) 0.0247(13) Uani 1 1 d . . . . .
H6A H 0.246184 0.301632 0.022299 0.037 Uiso 1 1 calc GR . . . .
H6B H 0.391669 0.252831 0.073118 0.037 Uiso 1 1 calc GR . . . .
H6C H 0.411713 0.329251 -0.015883 0.037 Uiso 1 1 calc GR . . . .
C1 C 0.8222(7) 0.4071(3) 0.7581(8) 0.0158(10) Uani 1 1 d . . . . .
C7 C 0.2936(7) 0.2837(3) 0.4307(10) 0.0283(14) Uani 1 1 d . . . . .
H7A H 0.294326 0.306903 0.559351 0.042 Uiso 1 1 calc GR . . . .
H7B H 0.347669 0.239110 0.447026 0.042 Uiso 1 1 calc GR . . . .
H7C H 0.188402 0.275293 0.376611 0.042 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
K1 0.0176(6) 0.0269(6) 0.0190(6) 0.0008(5) -0.0003(5) 0.0021(4)
S2 0.0187(7) 0.0283(7) 0.0163(7) -0.0042(5) 0.0007(5) 0.0020(5)
S1 0.0127(6) 0.0270(6) 0.0206(7) -0.0002(5) -0.0023(5) 0.0007(5)
O2 0.0185(19) 0.0192(19) 0.027(2) 0.0016(16) 0.0024(17) 0.0016(14)
O1 0.0127(16) 0.0196(17) 0.018(2) -0.0026(15) -0.0018(14) 0.0007(13)
C4 0.017(3) 0.020(2) 0.024(3) -0.003(2) -0.001(2) 0.001(2)
C3 0.015(2) 0.019(2) 0.020(3) -0.002(2) -0.0023(19) 0.0013(19)
C5 0.022(3) 0.023(3) 0.028(3) 0.004(2) -0.001(3) -0.003(2)
C2 0.012(2) 0.024(3) 0.019(3) -0.004(2) -0.003(2) 0.0007(19)
C6 0.024(3) 0.024(3) 0.025(3) -0.006(2) -0.005(2) 0.001(2)
C1 0.015(2) 0.015(2) 0.017(3) 0.0030(18) -0.002(2) -0.0004(18)
C7 0.025(3) 0.024(3) 0.036(4) 0.002(2) 0.001(3) -0.003(2)
_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
K1 K1 4.3972(15) 2_565 ?
K1 K1 4.3972(15) 2_564 ?
K1 S2 3.5375(17) 2_564 ?
K1 S2 3.2172(17) 1_554 ?
K1 S1 3.5105(18) 1_554 ?
K1 S1 3.2896(18) 2_564 ?
K1 S1 3.2280(17) . ?
K1 O2 2.759(4) 1_655 ?
K1 O1 2.990(4) . ?
K1 C5 3.419(6) 1_655 ?
K1 C1 3.490(6) . ?
K1 C1 3.461(5) 2_564 ?
S2 C1 1.677(6) . ?
S1 C1 1.703(6) . ?
O2 C4 1.451(7) . ?
O2 C5 1.422(7) . ?
O1 C2 1.458(6) . ?
O1 C1 1.351(7) . ?
C4 C3 1.536(7) . ?
C4 C6 1.529(8) . ?
C4 C7 1.542(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.511(7) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 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
K1 K1 K1 98.40(5) 2_564 2_565 ?
S2 K1 K1 77.00(4) 2_564 2_564 ?
S2 K1 K1 52.63(3) 1_554 2_564 ?
S2 K1 K1 116.54(4) 1_554 2_565 ?
S2 K1 K1 46.29(3) 2_564 2_565 ?
S2 K1 S2 70.93(4) 1_554 2_564 ?
S2 K1 S1 85.48(4) 1_554 2_564 ?
S2 K1 S1 140.93(5) 1_554 . ?
S2 K1 S1 52.69(4) 1_554 1_554 ?
S2 K1 C5 113.85(11) 1_554 1_655 ?
S2 K1 C1 111.89(10) 1_554 . ?
S2 K1 C1 65.37(10) 1_554 2_564 ?
S1 K1 K1 48.17(2) . 2_565 ?
S1 K1 K1 47.55(2) 1_554 2_564 ?
S1 K1 K1 145.31(5) 1_554 2_565 ?
S1 K1 K1 145.80(5) . 2_564 ?
S1 K1 K1 46.98(4) 2_564 2_564 ?
S1 K1 K1 51.94(4) 2_564 2_565 ?
S1 K1 S2 51.93(3) 2_564 2_564 ?
S1 K1 S2 116.47(4) 1_554 2_564 ?
S1 K1 S2 81.36(4) . 2_564 ?
S1 K1 S1 162.16(6) . 1_554 ?
S1 K1 S1 93.38(5) 2_564 1_554 ?
S1 K1 S1 98.85(5) . 2_564 ?
S1 K1 C5 104.53(12) . 1_655 ?
S1 K1 C5 73.76(10) 2_564 1_655 ?
S1 K1 C1 29.09(10) 2_564 2_564 ?
S1 K1 C1 29.04(9) . . ?
S1 K1 C1 101.00(10) . 2_564 ?
S1 K1 C1 99.64(9) 2_564 . ?
O2 K1 K1 100.68(9) 1_655 2_565 ?
O2 K1 K1 91.74(9) 1_655 2_564 ?
O2 K1 S2 130.01(10) 1_655 1_554 ?
O2 K1 S2 141.11(9) 1_655 2_564 ?
O2 K1 S1 77.60(10) 1_655 1_554 ?
O2 K1 S1 93.33(9) 1_655 2_564 ?
O2 K1 S1 88.72(10) 1_655 . ?
O2 K1 O1 131.34(12) 1_655 . ?
O2 K1 C5 23.66(13) 1_655 1_655 ?
O2 K1 C1 117.51(13) 1_655 . ?
O2 K1 C1 122.24(13) 1_655 2_564 ?
O1 K1 K1 136.19(8) . 2_564 ?
O1 K1 K1 69.75(7) . 2_565 ?
O1 K1 S2 93.88(8) . 1_554 ?
O1 K1 S2 64.36(8) . 2_564 ?
O1 K1 S1 112.52(8) . 2_564 ?
O1 K1 S1 48.46(8) . . ?
O1 K1 S1 136.71(9) . 1_554 ?
O1 K1 C5 152.17(14) . 1_655 ?
O1 K1 C1 22.41(12) . . ?
O1 K1 C1 92.03(12) . 2_564 ?
C5 K1 K1 98.04(11) 1_655 2_565 ?
C5 K1 K1 68.73(10) 1_655 2_564 ?
C5 K1 S2 125.42(11) 1_655 2_564 ?
C5 K1 S1 66.49(12) 1_655 1_554 ?
C5 K1 C1 132.93(15) 1_655 . ?
C5 K1 C1 101.29(14) 1_655 2_564 ?
C1 K1 K1 50.47(8) . 2_565 ?
C1 K1 K1 55.11(10) 2_564 2_565 ?
C1 K1 K1 51.06(10) 2_564 2_564 ?
C1 K1 K1 138.70(9) . 2_564 ?
C1 K1 S2 61.86(9) . 2_564 ?
C1 K1 S2 27.70(10) 2_564 2_564 ?
C1 K1 S1 159.11(10) . 1_554 ?
C1 K1 S1 96.01(10) 2_564 1_554 ?
C1 K1 C1 87.80(14) 2_564 . ?
K1 S2 K1 81.08(4) 1_556 2_565 ?
C1 S2 K1 73.62(18) . 2_565 ?
C1 S2 K1 93.9(2) . 1_556 ?
K1 S1 K1 84.85(4) . 2_565 ?
K1 S1 K1 162.16(6) . 1_556 ?
K1 S1 K1 80.51(4) 2_565 1_556 ?
C1 S1 K1 81.06(17) . 2_565 ?
C1 S1 K1 83.7(2) . 1_556 ?
C1 S1 K1 84.05(19) . . ?
C4 O2 K1 128.5(3) . 1_455 ?
C5 O2 K1 105.2(3) . 1_455 ?
C5 O2 C4 115.3(5) . . ?
C2 O1 K1 128.9(3) . . ?
C1 O1 K1 100.1(3) . . ?
C1 O1 C2 119.0(4) . . ?
O2 C4 C3 111.6(4) . . ?
O2 C4 C6 110.9(5) . . ?
O2 C4 C7 103.4(5) . . ?
C3 C4 C7 111.8(5) . . ?
C6 C4 C3 108.8(5) . . ?
C6 C4 C7 110.3(5) . . ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C2 C3 C4 114.5(5) . . ?
C2 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
K1 C5 H5A 103.2 1_455 . ?
K1 C5 H5B 146.7 1_455 . ?
K1 C5 H5C 64.2 1_455 . ?
O2 C5 K1 51.1(3) . 1_455 ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
O2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 C2 C3 106.1(4) . . ?
O1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C3 C2 H2A 110.5 . . ?
C3 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
K1 C1 K1 78.47(11) 2_565 . ?
S2 C1 K1 78.68(18) . 2_565 ?
S2 C1 K1 147.4(2) . . ?
S2 C1 S1 124.9(3) . . ?
S1 C1 K1 69.86(17) . 2_565 ?
S1 C1 K1 66.91(18) . . ?
O1 C1 K1 125.0(3) . 2_565 ?
O1 C1 K1 57.5(3) . . ?
O1 C1 S2 121.6(4) . . ?
O1 C1 S1 113.5(4) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
_shelx_res_file
;
TITL s4796l_a.res in Cc
s4796l.res
created by SHELXL-2016/6 at 16:00:04 on 06-Jun-2017
REM Old TITL s4796l_a.res in Cc
REM SHELXT solution in Cc
REM R1 0.066, Rweak 0.028, Alpha 0.001, Orientation as input
REM Flack x = 0.204 ( 0.106 ) from Parsons' quotients
REM Formula found by SHELXT: C7 O2 K3
CELL 0.71073 8.6583 18.7658 6.6572 90 95.538 90
ZERR 4 0.0002 0.0004 0.0002 0 0.002 0
LATT -7
SYMM +X,-Y,0.5+Z
SFAC C H K O S
UNIT 28 52 4 8 8
L.S. 16
PLAN 20
BOND $H
list 4
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.114600
BASF 0.10558
FVAR 0.67889
K1 3 0.980150 0.423446 0.297358 11.00000 0.01758 0.02692 =
0.01900 0.00084 -0.00029 0.00210
S2 5 0.716039 0.444435 0.927832 11.00000 0.01872 0.02827 =
0.01628 -0.00418 0.00074 0.00198
S1 5 1.019571 0.402366 0.780832 11.00000 0.01272 0.02700 =
0.02065 -0.00021 -0.00234 0.00074
O2 4 0.294226 0.399191 0.294349 11.00000 0.01853 0.01923 =
0.02718 0.00163 0.00238 0.00162
O1 4 0.755300 0.377664 0.585947 11.00000 0.01274 0.01965 =
0.01765 -0.00256 -0.00179 0.00066
C4 1 0.374760 0.331658 0.284857 11.00000 0.01671 0.01958 =
0.02436 -0.00250 -0.00081 0.00100
C3 1 0.549002 0.339380 0.350079 11.00000 0.01508 0.01892 =
0.02012 -0.00185 -0.00229 0.00126
AFIX 23
H3A 2 0.596236 0.292483 0.352052 11.00000 -1.20000
H3B 2 0.595611 0.367619 0.249847 11.00000 -1.20000
AFIX 0
C5 1 0.348263 0.454522 0.173055 11.00000 0.02180 0.02269 =
0.02766 0.00377 -0.00057 -0.00319
AFIX 137
H5A 2 0.343976 0.438812 0.035392 11.00000 -1.50000
H5B 2 0.453398 0.466235 0.220630 11.00000 -1.50000
H5C 2 0.283898 0.495874 0.181254 11.00000 -1.50000
AFIX 0
C2 1 0.586538 0.373599 0.554454 11.00000 0.01196 0.02384 =
0.01856 -0.00436 -0.00306 0.00065
AFIX 23
H2A 2 0.541307 0.420848 0.556737 11.00000 -1.20000
H2B 2 0.546260 0.345026 0.659055 11.00000 -1.20000
AFIX 0
C6 1 0.354167 0.300992 0.071233 11.00000 0.02396 0.02369 =
0.02498 -0.00642 -0.00506 0.00149
AFIX 137
H6A 2 0.246184 0.301632 0.022299 11.00000 -1.50000
H6B 2 0.391669 0.252831 0.073118 11.00000 -1.50000
H6C 2 0.411713 0.329251 -0.015883 11.00000 -1.50000
AFIX 0
C1 1 0.822192 0.407111 0.758105 11.00000 0.01466 0.01504 =
0.01709 0.00299 -0.00191 -0.00037
C7 1 0.293636 0.283718 0.430723 11.00000 0.02534 0.02365 =
0.03559 0.00246 0.00122 -0.00267
AFIX 137
H7A 2 0.294326 0.306903 0.559351 11.00000 -1.50000
H7B 2 0.347669 0.239110 0.447026 11.00000 -1.50000
H7C 2 0.188402 0.275293 0.376611 11.00000 -1.50000
AFIX 0
HKLF 4
REM s4796l_a.res in Cc
REM R1 = 0.0548 for 2145 Fo > 4sig(Fo) and 0.0551 for all 2184 data
REM 113 parameters refined using 2 restraints
END
WGHT 0.1146 0.0000
REM Highest difference peak 0.319, deepest hole -0.196, 1-sigma level 0.049
Q1 1 0.2608 0.3494 0.3736 11.00000 0.05 0.31
Q2 1 1.0799 0.4247 0.4301 11.00000 0.05 0.21
Q3 1 0.7983 0.4427 1.0773 11.00000 0.05 0.20
Q4 1 0.7500 0.3737 0.7026 11.00000 0.05 0.20
Q5 1 0.4834 0.3321 0.3212 11.00000 0.05 0.19
Q6 1 0.9162 0.3897 0.7825 11.00000 0.05 0.19
Q7 1 0.6128 0.4430 0.7853 11.00000 0.05 0.19
Q8 1 0.9159 0.4008 0.6494 11.00000 0.05 0.19
Q9 1 1.1233 0.4102 0.9291 11.00000 0.05 0.17
Q10 1 0.9058 0.4162 0.1497 11.00000 0.05 0.17
Q11 1 0.7755 0.4096 0.8325 11.00000 0.05 0.17
Q12 1 0.7130 0.3401 0.2183 11.00000 0.05 0.16
Q13 1 0.6731 0.3652 0.5897 11.00000 0.05 0.16
Q14 1 0.6310 0.4067 0.9339 11.00000 0.05 0.16
Q15 1 0.9976 0.4391 0.9001 11.00000 0.05 0.15
Q16 1 0.8012 0.4757 0.9612 11.00000 0.05 0.15
Q17 1 1.0826 0.4345 0.2890 11.00000 0.05 0.15
Q18 1 0.3533 0.3508 0.2835 11.00000 0.05 0.15
Q19 1 0.9168 0.4289 0.7564 11.00000 0.05 0.15
Q20 1 1.0905 0.4407 0.7093 11.00000 0.05 0.15
;
_shelx_res_checksum 38626
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.961
_oxdiff_exptl_absorpt_empirical_full_min 0.510
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.89(11)
2 0.11(11)
#######################################################################
#
# 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_s4596na
_database_code_depnum_ccdc_archive 'CCDC 1812201'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C15 H27 In O3 S6'
_chemical_formula_weight 562.54
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'
_cell_length_a 19.7328(5)
_cell_length_b 9.9324(3)
_cell_length_c 23.6448(6)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4634.2(2)
_cell_formula_units_Z 8
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 4635
_cell_measurement_theta_min 4.48
_cell_measurement_theta_max 72.13
_exptl_crystal_description block
_exptl_crystal_colour white
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.613
_exptl_crystal_F_000 2288
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.210
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.060
_exptl_absorpt_coefficient_mu 13.309
_shelx_estimated_absorpt_T_min 0.166
_shelx_estimated_absorpt_T_max 0.502
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.408208
_exptl_absorpt_correction_T_max 0.502
_exptl_absorpt_process_details SADABS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 26580
_diffrn_reflns_av_unetI/netI 0.0465
_diffrn_reflns_av_R_equivalents 0.0760
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 4.359
_diffrn_reflns_theta_max 72.183
_diffrn_reflns_theta_full 67.679
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 4549
_reflns_number_gt 3788
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+10.8065P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 4549
_refine_ls_number_parameters 232
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0478
_refine_ls_R_factor_gt 0.0374
_refine_ls_wR_factor_ref 0.0911
_refine_ls_wR_factor_gt 0.0861
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.94079(2) 0.10047(3) 0.72840(2) 0.01369(9) Uani 1 1 d . . . . .
S1 S 0.89126(6) 0.02366(12) 0.63297(5) 0.0269(2) Uani 1 1 d . . . . .
S2 S 0.96116(5) 0.28651(10) 0.65132(4) 0.0186(2) Uani 1 1 d . . . . .
S3 S 1.02987(5) 0.19183(9) 0.80029(4) 0.01414(19) Uani 1 1 d . . . . .
S4 S 1.05727(5) -0.01059(9) 0.71098(4) 0.0150(2) Uani 1 1 d . . . . .
S5 S 0.83592(5) 0.20842(9) 0.77766(4) 0.0172(2) Uani 1 1 d . . . . .
S6 S 0.87830(5) -0.07901(9) 0.78752(5) 0.0187(2) Uani 1 1 d . . . . .
O1 O 0.91276(19) 0.1862(4) 0.55351(14) 0.0320(8) Uani 1 1 d . . . . .
O2 O 1.14934(15) 0.0805(3) 0.77674(12) 0.0180(6) Uani 1 1 d . . . . .
O3 O 0.77638(15) 0.0206(3) 0.84036(12) 0.0176(6) Uani 1 1 d . . . . .
C1 C 0.9226(2) 0.1729(5) 0.60842(19) 0.0230(9) Uani 1 1 d . . . . .
C2 C 0.9387(3) 0.3041(5) 0.5267(2) 0.0337(11) Uani 1 1 d . . . . .
H2A H 0.9881 0.3119 0.5334 0.040 Uiso 1 1 calc R U . . .
H2B H 0.9163 0.3855 0.5420 0.040 Uiso 1 1 calc R U . . .
C3 C 0.9241(3) 0.2898(6) 0.4633(2) 0.0368(12) Uani 1 1 d . . . . .
H3 H 0.8747 0.2694 0.4588 0.044 Uiso 1 1 calc R U . . .
C4 C 0.9624(4) 0.1785(6) 0.4385(2) 0.0486(16) Uani 1 1 d . . . . .
H4A H 0.9515 0.1713 0.3981 0.073 Uiso 1 1 calc R U . . .
H4B H 0.9504 0.0944 0.4576 0.073 Uiso 1 1 calc R U . . .
H4C H 1.0111 0.1955 0.4430 0.073 Uiso 1 1 calc R U . . .
C5 C 0.9380(3) 0.4240(6) 0.4352(2) 0.0434(14) Uani 1 1 d . . . . .
H5A H 0.9865 0.4439 0.4373 0.065 Uiso 1 1 calc R U . . .
H5B H 0.9125 0.4949 0.4547 0.065 Uiso 1 1 calc R U . . .
H5C H 0.9239 0.4200 0.3955 0.065 Uiso 1 1 calc R U . . .
C6 C 1.0843(2) 0.0885(4) 0.76505(16) 0.0145(8) Uani 1 1 d . . . . .
C7 C 1.1768(2) 0.1530(4) 0.82533(17) 0.0167(8) Uani 1 1 d . . . . .
H7A H 1.1546 0.2421 0.8284 0.020 Uiso 1 1 calc R U . . .
H7B H 1.2260 0.1679 0.8199 0.020 Uiso 1 1 calc R U . . .
C8 C 1.1652(2) 0.0738(4) 0.87954(18) 0.0181(8) Uani 1 1 d . . . . .
H8 H 1.1156 0.0544 0.8829 0.022 Uiso 1 1 calc R U . . .
C9 C 1.1862(3) 0.1602(5) 0.9298(2) 0.0292(11) Uani 1 1 d . . . . .
H9A H 1.1744 0.1139 0.9650 0.044 Uiso 1 1 calc R U . . .
H9B H 1.1626 0.2469 0.9280 0.044 Uiso 1 1 calc R U . . .
H9C H 1.2353 0.1755 0.9285 0.044 Uiso 1 1 calc R U . . .
C10 C 1.2030(2) -0.0595(4) 0.8786(2) 0.0279(10) Uani 1 1 d . . . . .
H10A H 1.2519 -0.0425 0.8782 0.042 Uiso 1 1 calc R U . . .
H10B H 1.1903 -0.1102 0.8446 0.042 Uiso 1 1 calc R U . . .
H10C H 1.1912 -0.1119 0.9123 0.042 Uiso 1 1 calc R U . . .
C11 C 0.8253(2) 0.0507(4) 0.80424(17) 0.0161(8) Uani 1 1 d . . . . .
C12 C 0.7292(2) 0.1259(4) 0.85794(18) 0.0167(8) Uani 1 1 d . . . . .
H12A H 0.7007 0.1541 0.8256 0.020 Uiso 1 1 calc R U . . .
H12B H 0.7545 0.2053 0.8719 0.020 Uiso 1 1 calc R U . . .
C13 C 0.6852(2) 0.0683(4) 0.90482(17) 0.0171(8) Uani 1 1 d . . . . .
H13 H 0.6615 -0.0132 0.8899 0.021 Uiso 1 1 calc R U . . .
C14 C 0.7271(3) 0.0268(6) 0.9559(2) 0.0374(13) Uani 1 1 d . . . . .
H14A H 0.7599 -0.0423 0.9446 0.056 Uiso 1 1 calc R U . . .
H14B H 0.6971 -0.0096 0.9852 0.056 Uiso 1 1 calc R U . . .
H14C H 0.7512 0.1054 0.9708 0.056 Uiso 1 1 calc R U . . .
C15 C 0.6321(2) 0.1725(4) 0.92053(19) 0.0234(9) Uani 1 1 d . . . . .
H15A H 0.6545 0.2549 0.9335 0.035 Uiso 1 1 calc R U . . .
H15B H 0.6033 0.1370 0.9508 0.035 Uiso 1 1 calc R U . . .
H15C H 0.6041 0.1930 0.8873 0.035 Uiso 1 1 calc R U . . .
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
In1 0.01294(15) 0.01384(13) 0.01428(14) 0.00005(9) -0.00014(10) -0.00051(10)
S1 0.0240(6) 0.0306(5) 0.0263(5) -0.0094(5) -0.0060(4) -0.0040(5)
S2 0.0198(5) 0.0179(4) 0.0180(4) 0.0051(4) 0.0015(4) 0.0031(4)
S3 0.0153(5) 0.0119(4) 0.0153(4) -0.0024(3) -0.0001(4) 0.0014(3)
S4 0.0172(5) 0.0110(4) 0.0168(5) -0.0033(3) 0.0005(4) 0.0008(3)
S5 0.0176(5) 0.0116(4) 0.0223(5) 0.0022(4) 0.0026(4) 0.0011(4)
S6 0.0191(5) 0.0101(4) 0.0270(5) -0.0008(4) 0.0059(4) 0.0007(4)
O1 0.040(2) 0.0356(18) 0.0207(16) 0.0032(14) -0.0003(15) 0.0012(16)
O2 0.0128(14) 0.0213(14) 0.0199(14) -0.0007(12) 0.0008(12) -0.0026(11)
O3 0.0194(15) 0.0124(12) 0.0210(14) 0.0028(11) 0.0053(12) 0.0018(11)
C1 0.022(2) 0.029(2) 0.018(2) -0.0025(17) -0.0008(17) 0.0075(18)
C2 0.038(3) 0.028(2) 0.035(3) -0.008(2) 0.002(2) 0.001(2)
C3 0.032(3) 0.051(3) 0.027(2) 0.009(2) -0.008(2) -0.013(2)
C4 0.071(5) 0.045(3) 0.029(3) -0.002(2) 0.007(3) -0.016(3)
C5 0.055(4) 0.047(3) 0.029(3) 0.003(2) -0.006(3) 0.016(3)
C6 0.016(2) 0.0119(17) 0.0156(19) 0.0054(14) 0.0018(15) -0.0011(15)
C7 0.0130(19) 0.0184(18) 0.0188(19) 0.0016(15) -0.0032(16) -0.0051(15)
C8 0.015(2) 0.0158(18) 0.023(2) 0.0034(16) -0.0043(16) -0.0019(16)
C9 0.043(3) 0.023(2) 0.022(2) 0.0049(18) -0.014(2) -0.005(2)
C10 0.020(2) 0.018(2) 0.046(3) 0.007(2) -0.008(2) 0.0013(17)
C11 0.020(2) 0.0132(17) 0.0152(18) -0.0023(15) 0.0011(16) -0.0020(15)
C12 0.014(2) 0.0155(18) 0.020(2) 0.0000(16) 0.0041(16) 0.0045(15)
C13 0.017(2) 0.0172(18) 0.0168(19) 0.0002(15) 0.0035(16) 0.0009(16)
C14 0.037(3) 0.053(3) 0.022(2) 0.011(2) 0.000(2) 0.020(3)
C15 0.021(2) 0.027(2) 0.023(2) 0.0019(18) 0.0015(18) 0.0066(18)
_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
In1 S1 2.5745(11) . ?
In1 S6 2.5793(10) . ?
In1 S4 2.5824(10) . ?
In1 S5 2.6055(10) . ?
In1 S3 2.6082(10) . ?
In1 S2 2.6263(10) . ?
S1 C1 1.708(5) . ?
S2 C1 1.697(5) . ?
S3 C6 1.704(4) . ?
S4 C6 1.699(4) . ?
S5 C11 1.701(4) . ?
S6 C11 1.706(4) . ?
O1 C1 1.319(5) . ?
O1 C2 1.426(6) . ?
O2 C6 1.315(5) . ?
O2 C7 1.460(5) . ?
O3 C11 1.323(5) . ?
O3 C12 1.460(5) . ?
C2 C3 1.534(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.463(9) . ?
C3 C5 1.514(8) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 C8 1.521(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C10 1.520(6) . ?
C8 C9 1.523(6) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 C13 1.520(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C15 1.519(6) . ?
C13 C14 1.520(6) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
S1 In1 S6 95.09(4) . . ?
S1 In1 S4 94.10(4) . . ?
S6 In1 S4 102.52(3) . . ?
S1 In1 S5 102.25(4) . . ?
S6 In1 S5 70.27(3) . . ?
S4 In1 S5 162.54(3) . . ?
S1 In1 S3 158.45(4) . . ?
S6 In1 S3 102.09(3) . . ?
S4 In1 S3 69.68(3) . . ?
S5 In1 S3 95.78(3) . . ?
S1 In1 S2 70.03(4) . . ?
S6 In1 S2 159.31(4) . . ?
S4 In1 S2 93.08(3) . . ?
S5 In1 S2 98.18(3) . . ?
S3 In1 S2 95.99(3) . . ?
C1 S1 In1 84.45(15) . . ?
C1 S2 In1 83.02(16) . . ?
C6 S3 In1 84.06(14) . . ?
C6 S4 In1 84.96(14) . . ?
C11 S5 In1 83.37(15) . . ?
C11 S6 In1 84.09(14) . . ?
C1 O1 C2 117.8(4) . . ?
C6 O2 C7 119.8(3) . . ?
C11 O3 C12 119.1(3) . . ?
O1 C1 S2 126.0(4) . . ?
O1 C1 S1 111.6(3) . . ?
S2 C1 S1 122.4(3) . . ?
O1 C2 C3 106.9(4) . . ?
O1 C2 H2A 110.4 . . ?
C3 C2 H2A 110.4 . . ?
O1 C2 H2B 110.4 . . ?
C3 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C4 C3 C5 113.3(5) . . ?
C4 C3 C2 111.4(5) . . ?
C5 C3 C2 108.2(5) . . ?
C4 C3 H3 107.9 . . ?
C5 C3 H3 107.9 . . ?
C2 C3 H3 107.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C6 S4 115.4(3) . . ?
O2 C6 S3 123.3(3) . . ?
S4 C6 S3 121.3(2) . . ?
O2 C7 C8 110.6(3) . . ?
O2 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C10 C8 C7 111.4(4) . . ?
C10 C8 C9 111.7(4) . . ?
C7 C8 C9 108.9(3) . . ?
C10 C8 H8 108.3 . . ?
C7 C8 H8 108.3 . . ?
C9 C8 H8 108.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C11 S5 122.5(3) . . ?
O3 C11 S6 115.2(3) . . ?
S5 C11 S6 122.3(2) . . ?
O3 C12 C13 107.6(3) . . ?
O3 C12 H12A 110.2 . . ?
C13 C12 H12A 110.2 . . ?
O3 C12 H12B 110.2 . . ?
C13 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C15 C13 C12 108.5(3) . . ?
C15 C13 C14 111.5(4) . . ?
C12 C13 C14 111.7(4) . . ?
C15 C13 H13 108.4 . . ?
C12 C13 H13 108.4 . . ?
C14 C13 H13 108.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S2 2.4(6) . . . . ?
C2 O1 C1 S1 -177.6(3) . . . . ?
In1 S2 C1 O1 -177.1(4) . . . . ?
In1 S2 C1 S1 2.9(3) . . . . ?
In1 S1 C1 O1 177.1(3) . . . . ?
In1 S1 C1 S2 -3.0(3) . . . . ?
C1 O1 C2 C3 176.8(4) . . . . ?
O1 C2 C3 C4 -66.1(6) . . . . ?
O1 C2 C3 C5 168.8(4) . . . . ?
C7 O2 C6 S4 -175.0(3) . . . . ?
C7 O2 C6 S3 5.8(5) . . . . ?
In1 S4 C6 O2 -177.2(3) . . . . ?
In1 S4 C6 S3 1.9(2) . . . . ?
In1 S3 C6 O2 177.2(3) . . . . ?
In1 S3 C6 S4 -1.9(2) . . . . ?
C6 O2 C7 C8 82.0(4) . . . . ?
O2 C7 C8 C10 63.6(4) . . . . ?
O2 C7 C8 C9 -172.8(4) . . . . ?
C12 O3 C11 S5 0.5(5) . . . . ?
C12 O3 C11 S6 178.9(3) . . . . ?
In1 S5 C11 O3 177.3(4) . . . . ?
In1 S5 C11 S6 -1.0(2) . . . . ?
In1 S6 C11 O3 -177.4(3) . . . . ?
In1 S6 C11 S5 1.1(2) . . . . ?
C11 O3 C12 C13 -172.5(3) . . . . ?
O3 C12 C13 C15 -175.6(3) . . . . ?
O3 C12 C13 C14 61.2(5) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C8 H8 S3 1.00 2.92 3.467(4) 115.1 .
C8 H8 S3 1.00 2.92 3.467(4) 115.1 .
_refine_diff_density_max 1.619
_refine_diff_density_min -1.184
_refine_diff_density_rms 0.117
_shelx_res_file
;
s4596na.res created by SHELXL-2014/7
TITL s4596na in Pbca
CELL 1.54178 19.7328 9.9324 23.6448 90.000 90.000 90.000
ZERR 8.00 0.0005 0.0003 0.0006 0.000 0.000 0.000
LATT 1
SYMM x+1/2, -y+1/2, -z
SYMM -x, y+1/2, -z+1/2
SYMM -x+1/2, -y, z+1/2
SFAC C H O S In
UNIT 120 216 24 48 8
L.S. 16
ACTA
BOND $H
FMAP 2
PLAN 0
HTAB C8 S3
HTAB
CONF
SIZE 0.060 0.120 0.210
HTAB C8 S3
TEMP -173.000
WGHT 0.037400 10.806499
FVAR 0.05151
IN1 5 0.940791 0.100467 0.728397 11.00000 0.01294 0.01384 =
0.01428 0.00005 -0.00014 -0.00051
S1 4 0.891262 0.023656 0.632973 11.00000 0.02396 0.03057 =
0.02631 -0.00940 -0.00602 -0.00402
S2 4 0.961156 0.286508 0.651321 11.00000 0.01979 0.01790 =
0.01800 0.00509 0.00153 0.00307
S3 4 1.029869 0.191829 0.800287 11.00000 0.01527 0.01190 =
0.01526 -0.00241 -0.00009 0.00145
S4 4 1.057267 -0.010595 0.710983 11.00000 0.01717 0.01104 =
0.01677 -0.00329 0.00052 0.00082
S5 4 0.835918 0.208415 0.777657 11.00000 0.01755 0.01161 =
0.02233 0.00220 0.00259 0.00105
S6 4 0.878296 -0.079009 0.787518 11.00000 0.01906 0.01011 =
0.02696 -0.00082 0.00591 0.00068
O1 3 0.912759 0.186212 0.553514 11.00000 0.03967 0.03563 =
0.02074 0.00316 -0.00031 0.00117
O2 3 1.149340 0.080486 0.776743 11.00000 0.01275 0.02134 =
0.01986 -0.00067 0.00079 -0.00257
O3 3 0.776384 0.020566 0.840360 11.00000 0.01939 0.01241 =
0.02096 0.00277 0.00532 0.00181
C1 1 0.922604 0.172908 0.608417 11.00000 0.02181 0.02891 =
0.01836 -0.00252 -0.00083 0.00748
C2 1 0.938741 0.304088 0.526741 11.00000 0.03818 0.02837 =
0.03461 -0.00824 0.00181 0.00052
AFIX 23
H2A 2 0.988126 0.311870 0.533359 11.00000 -1.20000
H2B 2 0.916310 0.385492 0.542015 11.00000 -1.20000
AFIX 0
C3 1 0.924055 0.289796 0.463328 11.00000 0.03243 0.05101 =
0.02684 0.00883 -0.00783 -0.01313
AFIX 13
H3 2 0.874728 0.269404 0.458786 11.00000 -1.20000
AFIX 0
C4 1 0.962424 0.178546 0.438466 11.00000 0.07144 0.04513 =
0.02922 -0.00181 0.00743 -0.01589
AFIX 137
H4A 2 0.951538 0.171256 0.398144 11.00000 -1.50000
H4B 2 0.950389 0.094371 0.457615 11.00000 -1.50000
H4C 2 1.011050 0.195480 0.442984 11.00000 -1.50000
AFIX 0
C5 1 0.937968 0.423991 0.435241 11.00000 0.05470 0.04681 =
0.02863 0.00340 -0.00631 0.01602
AFIX 137
H5A 2 0.986543 0.443931 0.437308 11.00000 -1.50000
H5B 2 0.912481 0.494873 0.454705 11.00000 -1.50000
H5C 2 0.923883 0.420017 0.395531 11.00000 -1.50000
AFIX 0
C6 1 1.084308 0.088479 0.765047 11.00000 0.01586 0.01192 =
0.01557 0.00542 0.00176 -0.00105
C7 1 1.176793 0.153032 0.825330 11.00000 0.01296 0.01839 =
0.01877 0.00155 -0.00320 -0.00508
AFIX 23
H7A 2 1.154585 0.242112 0.828390 11.00000 -1.20000
H7B 2 1.225970 0.167863 0.819860 11.00000 -1.20000
AFIX 0
C8 1 1.165215 0.073800 0.879540 11.00000 0.01510 0.01582 =
0.02349 0.00340 -0.00434 -0.00187
AFIX 13
H8 2 1.115650 0.054401 0.882888 11.00000 -1.20000
AFIX 0
C9 1 1.186227 0.160233 0.929755 11.00000 0.04263 0.02306 =
0.02178 0.00486 -0.01415 -0.00458
AFIX 137
H9A 2 1.174363 0.113938 0.964992 11.00000 -1.50000
H9B 2 1.162569 0.246891 0.928047 11.00000 -1.50000
H9C 2 1.235271 0.175498 0.928544 11.00000 -1.50000
AFIX 0
C10 1 1.203021 -0.059548 0.878599 11.00000 0.01981 0.01815 =
0.04578 0.00705 -0.00829 0.00128
AFIX 137
H10A 2 1.251939 -0.042543 0.878226 11.00000 -1.50000
H10B 2 1.190301 -0.110174 0.844645 11.00000 -1.50000
H10C 2 1.191192 -0.111884 0.912319 11.00000 -1.50000
AFIX 0
C11 1 0.825257 0.050715 0.804240 11.00000 0.01995 0.01325 =
0.01517 -0.00228 0.00106 -0.00199
C12 1 0.729237 0.125863 0.857940 11.00000 0.01432 0.01550 =
0.02019 -0.00003 0.00407 0.00451
AFIX 23
H12A 2 0.700733 0.154117 0.825593 11.00000 -1.20000
H12B 2 0.754495 0.205344 0.871869 11.00000 -1.20000
AFIX 0
C13 1 0.685188 0.068326 0.904821 11.00000 0.01735 0.01723 =
0.01677 0.00016 0.00349 0.00092
AFIX 13
H13 2 0.661451 -0.013223 0.889896 11.00000 -1.20000
AFIX 0
C14 1 0.727077 0.026766 0.955883 11.00000 0.03664 0.05330 =
0.02218 0.01097 0.00006 0.01973
AFIX 137
H14A 2 0.759890 -0.042270 0.944617 11.00000 -1.50000
H14B 2 0.697097 -0.009576 0.985189 11.00000 -1.50000
H14C 2 0.751244 0.105353 0.970759 11.00000 -1.50000
AFIX 0
C15 1 0.632070 0.172547 0.920527 11.00000 0.02077 0.02669 =
0.02259 0.00187 0.00150 0.00659
AFIX 137
H15A 2 0.654540 0.254897 0.933549 11.00000 -1.50000
H15B 2 0.603270 0.137015 0.950815 11.00000 -1.50000
H15C 2 0.604137 0.192959 0.887347 11.00000 -1.50000
AFIX 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM s4596na in Pbca
REM R1 = 0.0374 for 3788 Fo > 4sig(Fo) and 0.0478 for all 4549 data
REM 232 parameters refined using 0 restraints
END
WGHT 0.0372 10.8848
REM Instructions for potential hydrogen bonds
HTAB C8 S3
REM Highest difference peak 1.619, deepest hole -1.184, 1-sigma level 0.117
Q1 1 0.9400 0.2624 0.5588 11.00000 0.05 1.62
Q2 1 0.9000 0.0801 0.6123 11.00000 0.05 1.40
Q3 1 0.9081 0.1811 0.5065 11.00000 0.05 1.09
Q4 1 1.0121 0.2340 0.4555 11.00000 0.05 0.98
Q5 1 0.9398 0.0987 0.7659 11.00000 0.05 0.81
Q6 1 0.9401 0.0973 0.6896 11.00000 0.05 0.80
Q7 1 0.9157 0.3631 0.4472 11.00000 0.05 0.54
Q8 1 0.9411 0.2421 0.6087 11.00000 0.05 0.53
Q9 1 0.8761 -0.0753 0.7514 11.00000 0.05 0.41
Q10 1 0.9001 0.2251 0.6435 11.00000 0.05 0.40
Q11 1 0.7040 0.0354 0.9303 11.00000 0.05 0.40
Q12 1 0.9896 0.5561 0.3730 11.00000 0.05 0.40
Q13 1 0.9784 0.3263 0.6702 11.00000 0.05 0.40
Q14 1 0.8471 0.2006 0.7412 11.00000 0.05 0.37
Q15 1 0.9059 -0.1966 0.7601 11.00000 0.05 0.36
Q16 1 0.8703 -0.0189 0.6798 11.00000 0.05 0.35
Q17 1 1.1171 0.3419 0.8191 11.00000 0.05 0.35
Q18 1 0.9107 -0.1066 0.7513 11.00000 0.05 0.35
Q19 1 1.0255 0.1827 0.8402 11.00000 0.05 0.35
Q20 1 0.9217 -0.0244 0.7640 11.00000 0.05 0.35
;
_shelx_res_checksum 80338
#######################################################################
#
# 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_s4599ma
_database_code_depnum_ccdc_archive 'CCDC 1812203'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C12 H21 In O6 S6'
_chemical_formula_weight 568.47
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.2235(4)
_cell_length_b 11.1426(4)
_cell_length_c 15.9305(5)
_cell_angle_alpha 90
_cell_angle_beta 92.748(2)
_cell_angle_gamma 90
_cell_volume 2167.26(13)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 5178
_cell_measurement_theta_min 4.46
_cell_measurement_theta_max 72.12
_exptl_crystal_description block
_exptl_crystal_colour white
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.742
_exptl_crystal_F_000 1144
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.220
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_min 0.040
_exptl_absorpt_coefficient_mu 14.347
_shelx_estimated_absorpt_T_min 0.144
_shelx_estimated_absorpt_T_max 0.598
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.493017
_exptl_absorpt_correction_T_max 0.598
_exptl_absorpt_process_details SADABS
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 15315
_diffrn_reflns_av_unetI/netI 0.0361
_diffrn_reflns_av_R_equivalents 0.0412
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 4.457
_diffrn_reflns_theta_max 72.206
_diffrn_reflns_theta_full 67.679
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total 4231
_reflns_number_gt 3707
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 4231
_refine_ls_number_parameters 229
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0294
_refine_ls_R_factor_gt 0.0233
_refine_ls_wR_factor_ref 0.0520
_refine_ls_wR_factor_gt 0.0503
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_restrained_S_all 1.015
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8677(2) 0.6842(2) 0.06965(14) 0.0128(4) Uani 1 1 d . . . . .
C2 C 0.8282(2) 0.5070(2) 0.14627(15) 0.0154(5) Uani 1 1 d . . . . .
H2A H 0.7676 0.4813 0.1068 0.019 Uiso 1 1 calc R U . . .
H2B H 0.7967 0.5515 0.1932 0.019 Uiso 1 1 calc R U . . .
C3 C 0.8907(2) 0.3997(2) 0.17926(16) 0.0186(5) Uani 1 1 d . . . . .
H3A H 0.8394 0.3388 0.1998 0.022 Uiso 1 1 calc R U . . .
H3B H 0.9322 0.3632 0.1339 0.022 Uiso 1 1 calc R U . . .
C4 C 1.0220(3) 0.3392(3) 0.2839(2) 0.0326(7) Uani 1 1 d . . . . .
H4A H 0.9697 0.2809 0.3047 0.049 Uiso 1 1 calc R U . . .
H4B H 1.0695 0.3684 0.3308 0.049 Uiso 1 1 calc R U . . .
H4C H 1.0668 0.3006 0.2422 0.049 Uiso 1 1 calc R U . . .
C5 C 0.71722(19) 1.0966(2) 0.10886(14) 0.0116(4) Uani 1 1 d . . . . .
C6 C 0.5717(2) 1.2053(2) 0.17040(16) 0.0159(5) Uani 1 1 d . . . . .
H6A H 0.5333 1.1394 0.1985 0.019 Uiso 1 1 calc R U . . .
H6B H 0.5367 1.2172 0.1137 0.019 Uiso 1 1 calc R U . . .
C7 C 0.5662(2) 1.3188(3) 0.22095(16) 0.0189(5) Uani 1 1 d . . . . .
H7A H 0.4900 1.3319 0.2372 0.023 Uiso 1 1 calc R U . . .
H7B H 0.6130 1.3103 0.2731 0.023 Uiso 1 1 calc R U . . .
C8 C 0.5142(3) 1.4781(3) 0.1313(2) 0.0351(8) Uani 1 1 d . . . . .
H8A H 0.4717 1.4198 0.0971 0.053 Uiso 1 1 calc R U . . .
H8B H 0.5435 1.5398 0.0947 0.053 Uiso 1 1 calc R U . . .
H8C H 0.4667 1.5158 0.1715 0.053 Uiso 1 1 calc R U . . .
C9 C 0.77020(19) 0.9526(2) -0.18940(15) 0.0132(5) Uani 1 1 d . . . . .
C10 C 0.6786(2) 0.9132(2) -0.32287(15) 0.0156(5) Uani 1 1 d . . . . .
H10A H 0.6040 0.9177 -0.3015 0.019 Uiso 1 1 calc R U . . .
H10B H 0.7012 0.8279 -0.3244 0.019 Uiso 1 1 calc R U . . .
C11 C 0.6805(2) 0.9681(3) -0.40950(15) 0.0170(5) Uani 1 1 d . . . . .
H11A H 0.6219 0.9310 -0.4458 0.020 Uiso 1 1 calc R U . . .
H11B H 0.6641 1.0549 -0.4053 0.020 Uiso 1 1 calc R U . . .
C12 C 0.8039(3) 0.8333(3) -0.46926(17) 0.0242(6) Uani 1 1 d . . . . .
H12A H 0.8238 0.7881 -0.4180 0.036 Uiso 1 1 calc R U . . .
H12B H 0.8646 0.8308 -0.5072 0.036 Uiso 1 1 calc R U . . .
H12C H 0.7386 0.7974 -0.4972 0.036 Uiso 1 1 calc R U . . .
In1 In 0.80162(2) 0.91659(2) -0.00658(2) 0.01148(5) Uani 1 1 d . . . . .
O1 O 0.90498(14) 0.58349(17) 0.10290(11) 0.0148(3) Uani 1 1 d . . . . .
O2 O 0.96394(17) 0.43746(18) 0.24601(12) 0.0222(4) Uani 1 1 d . . . . .
O3 O 0.68802(14) 1.17608(17) 0.16429(11) 0.0139(3) Uani 1 1 d . . . . .
O4 O 0.60133(16) 1.41898(19) 0.17517(14) 0.0241(4) Uani 1 1 d . . . . .
O5 O 0.75560(15) 0.98247(17) -0.26905(11) 0.0155(4) Uani 1 1 d . . . . .
O6 O 0.78154(15) 0.95404(18) -0.44821(11) 0.0194(4) Uani 1 1 d . . . . .
S1 S 0.95982(5) 0.76418(5) 0.01428(4) 0.01349(12) Uani 1 1 d . . . . .
S2 S 0.73733(5) 0.73346(5) 0.08061(4) 0.01457(12) Uani 1 1 d . . . . .
S3 S 0.62796(5) 1.03502(6) 0.03630(4) 0.01409(12) Uani 1 1 d . . . . .
S4 S 0.85399(5) 1.06017(5) 0.11517(3) 0.01291(12) Uani 1 1 d . . . . .
S5 S 0.85408(5) 1.04709(6) -0.13131(3) 0.01445(12) Uani 1 1 d . . . . .
S6 S 0.71154(5) 0.83005(6) -0.14708(3) 0.01451(12) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0160(11) 0.0127(12) 0.0094(9) -0.0011(9) -0.0014(9) -0.0014(9)
C2 0.0161(12) 0.0144(13) 0.0159(11) 0.0008(9) 0.0021(10) -0.0051(9)
C3 0.0241(13) 0.0129(13) 0.0189(11) 0.0010(10) 0.0023(10) -0.0025(10)
C4 0.0290(16) 0.0279(17) 0.0406(17) 0.0154(14) -0.0001(14) 0.0073(12)
C5 0.0125(11) 0.0125(12) 0.0099(9) 0.0029(9) 0.0013(8) -0.0002(8)
C6 0.0115(12) 0.0171(13) 0.0195(11) 0.0004(10) 0.0052(9) 0.0014(9)
C7 0.0216(13) 0.0178(14) 0.0176(11) -0.0013(10) 0.0058(10) 0.0013(10)
C8 0.0272(16) 0.0339(19) 0.0445(18) 0.0161(15) 0.0061(14) 0.0110(13)
C9 0.0122(11) 0.0144(12) 0.0132(10) -0.0010(9) 0.0026(9) 0.0019(9)
C10 0.0151(12) 0.0195(13) 0.0121(10) -0.0023(10) -0.0006(9) -0.0045(9)
C11 0.0176(12) 0.0215(14) 0.0117(10) -0.0014(10) -0.0018(9) -0.0005(10)
C12 0.0323(15) 0.0228(15) 0.0183(12) -0.0020(11) 0.0075(11) 0.0026(11)
In1 0.01342(8) 0.01128(9) 0.00977(7) -0.00045(6) 0.00078(5) 0.00042(6)
O1 0.0142(8) 0.0141(9) 0.0161(8) 0.0015(7) 0.0018(7) -0.0004(7)
O2 0.0251(10) 0.0160(10) 0.0246(9) 0.0046(8) -0.0062(8) 0.0008(7)
O3 0.0107(8) 0.0160(9) 0.0152(8) -0.0028(7) 0.0009(6) -0.0008(6)
O4 0.0200(10) 0.0171(10) 0.0356(11) 0.0018(9) 0.0057(8) 0.0004(7)
O5 0.0182(9) 0.0176(10) 0.0107(7) -0.0007(7) 0.0004(7) -0.0039(7)
O6 0.0234(10) 0.0200(10) 0.0152(8) -0.0029(7) 0.0052(7) -0.0068(7)
S1 0.0126(3) 0.0126(3) 0.0156(3) 0.0010(2) 0.0031(2) -0.00065(19)
S2 0.0122(3) 0.0149(3) 0.0169(3) 0.0021(2) 0.0036(2) 0.0005(2)
S3 0.0116(3) 0.0158(3) 0.0147(2) -0.0036(2) -0.0013(2) -0.0003(2)
S4 0.0106(3) 0.0142(3) 0.0139(2) -0.0018(2) -0.0006(2) 0.00029(19)
S5 0.0170(3) 0.0146(3) 0.0117(2) -0.0003(2) 0.0002(2) -0.0049(2)
S6 0.0170(3) 0.0146(3) 0.0119(2) -0.0004(2) 0.0004(2) -0.0041(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.313(3) . ?
C1 S2 1.703(3) . ?
C1 S1 1.713(2) . ?
C2 O1 1.465(3) . ?
C2 C3 1.500(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O2 1.421(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O2 1.423(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 O3 1.312(3) . ?
C5 S3 1.696(2) . ?
C5 S4 1.719(2) . ?
C6 O3 1.466(3) . ?
C6 C7 1.502(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O4 1.412(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O4 1.409(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 O5 1.316(3) . ?
C9 S6 1.697(3) . ?
C9 S5 1.711(3) . ?
C10 O5 1.462(3) . ?
C10 C11 1.511(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 O6 1.415(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O6 1.416(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
In1 S5 2.5683(6) . ?
In1 S4 2.5713(6) . ?
In1 S1 2.5830(6) . ?
In1 S2 2.6106(6) . ?
In1 S3 2.6179(6) . ?
In1 S6 2.6299(6) . ?
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
O1 C1 S2 122.85(19) . . ?
O1 C1 S1 115.37(18) . . ?
S2 C1 S1 121.77(15) . . ?
O1 C2 C3 107.6(2) . . ?
O1 C2 H2A 110.2 . . ?
C3 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
C3 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O2 C3 C2 108.6(2) . . ?
O2 C3 H3A 110.0 . . ?
C2 C3 H3A 110.0 . . ?
O2 C3 H3B 110.0 . . ?
C2 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 S3 123.02(18) . . ?
O3 C5 S4 114.54(17) . . ?
S3 C5 S4 122.44(15) . . ?
O3 C6 C7 106.9(2) . . ?
O3 C6 H6A 110.3 . . ?
C7 C6 H6A 110.3 . . ?
O3 C6 H6B 110.3 . . ?
C7 C6 H6B 110.3 . . ?
H6A C6 H6B 108.6 . . ?
O4 C7 C6 111.5(2) . . ?
O4 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
O4 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
O4 C8 H8A 109.5 . . ?
O4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O5 C9 S6 123.13(19) . . ?
O5 C9 S5 114.58(18) . . ?
S6 C9 S5 122.29(15) . . ?
O5 C10 C11 106.5(2) . . ?
O5 C10 H10A 110.4 . . ?
C11 C10 H10A 110.4 . . ?
O5 C10 H10B 110.4 . . ?
C11 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
O6 C11 C10 113.9(2) . . ?
O6 C11 H11A 108.8 . . ?
C10 C11 H11A 108.8 . . ?
O6 C11 H11B 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
S5 In1 S4 99.725(19) . . ?
S5 In1 S1 104.989(19) . . ?
S4 In1 S1 98.876(19) . . ?
S5 In1 S2 161.24(2) . . ?
S4 In1 S2 98.942(19) . . ?
S1 In1 S2 70.143(19) . . ?
S5 In1 S3 98.75(2) . . ?
S4 In1 S3 70.440(18) . . ?
S1 In1 S3 155.406(19) . . ?
S2 In1 S3 89.234(19) . . ?
S5 In1 S6 70.059(19) . . ?
S4 In1 S6 161.63(2) . . ?
S1 In1 S6 98.55(2) . . ?
S2 In1 S6 92.397(19) . . ?
S3 In1 S6 95.464(19) . . ?
C1 O1 C2 118.0(2) . . ?
C3 O2 C4 111.9(2) . . ?
C5 O3 C6 119.37(19) . . ?
C8 O4 C7 112.6(2) . . ?
C9 O5 C10 119.04(19) . . ?
C11 O6 C12 113.0(2) . . ?
C1 S1 In1 84.37(9) . . ?
C1 S2 In1 83.70(9) . . ?
C5 S3 In1 83.03(9) . . ?
C5 S4 In1 84.07(8) . . ?
C9 S5 In1 84.52(9) . . ?
C9 S6 In1 82.85(9) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 O2 69.9(3) . . . . ?
O3 C6 C7 O4 71.3(3) . . . . ?
O5 C10 C11 O6 66.4(3) . . . . ?
S2 C1 O1 C2 4.3(3) . . . . ?
S1 C1 O1 C2 -176.00(16) . . . . ?
C3 C2 O1 C1 -179.2(2) . . . . ?
C2 C3 O2 C4 176.7(2) . . . . ?
S3 C5 O3 C6 6.3(3) . . . . ?
S4 C5 O3 C6 -174.00(17) . . . . ?
C7 C6 O3 C5 -165.4(2) . . . . ?
C6 C7 O4 C8 92.6(3) . . . . ?
S6 C9 O5 C10 5.0(3) . . . . ?
S5 C9 O5 C10 -175.25(17) . . . . ?
C11 C10 O5 C9 -179.6(2) . . . . ?
C10 C11 O6 C12 68.0(3) . . . . ?
O1 C1 S1 In1 -178.48(18) . . . . ?
S2 C1 S1 In1 1.25(13) . . . . ?
O1 C1 S2 In1 178.5(2) . . . . ?
S1 C1 S2 In1 -1.24(13) . . . . ?
O3 C5 S3 In1 -178.8(2) . . . . ?
S4 C5 S3 In1 1.57(14) . . . . ?
O3 C5 S4 In1 178.73(18) . . . . ?
S3 C5 S4 In1 -1.60(14) . . . . ?
O5 C9 S5 In1 175.02(18) . . . . ?
S6 C9 S5 In1 -5.26(14) . . . . ?
O5 C9 S6 In1 -175.1(2) . . . . ?
S5 C9 S6 In1 5.16(14) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11A S1 0.99 2.99 3.891(3) 151.9 4_575
C10 H10A O2 0.99 2.50 3.337(3) 142.5 4_575
C7 H7B S2 0.99 3.02 3.992(3) 168.4 2_655
C6 H6A O2 0.99 2.42 3.305(3) 149.0 2_655
C3 H3A O3 0.99 2.63 3.514(3) 148.2 1_545
C2 H2A O6 0.99 2.59 3.420(3) 141.8 2_644
C2 H2A O4 0.99 2.45 2.998(3) 114.3 1_545
_refine_diff_density_max 0.534
_refine_diff_density_min -0.334
_refine_diff_density_rms 0.083
_shelx_res_file
;
s4599ma.res created by SHELXL-2014/7
TITL s4599ma in P2(1)/n
CELL 1.54178 12.2235 11.1426 15.9305 90.000 92.748 90.000
ZERR 4.00 0.0004 0.0004 0.0005 0.000 0.002 0.000
LATT 1
SYMM -x+1/2, y+1/2, -z+1/2
SFAC C H O S In
UNIT 48 84 24 24 4
L.S. 16
ACTA
BOND $H
FMAP 2
PLAN 0
HTAB C11 S1_$4
HTAB C10 O2_$4
EQIV $4 x-1/2, -y+3/2, z-1/2
HTAB C7 S2_$3
HTAB C6 O2_$3
EQIV $3 -x+3/2, y+1/2, -z+1/2
HTAB C3 O3_$1
HTAB C2 O6_$2
EQIV $2 -x+3/2, y-1/2, -z-1/2
HTAB C2 O4_$1
EQIV $1 x, y-1, z
HTAB
CONF
SIZE .04 .13 .22
TEMP -173.000
WGHT 0.024200
FVAR 0.10491
C1 1 0.867719 0.684194 0.069653 11.00000 0.01601 0.01271 =
0.00940 -0.00113 -0.00138 -0.00144
C2 1 0.828211 0.506964 0.146273 11.00000 0.01612 0.01440 =
0.01595 0.00078 0.00214 -0.00506
AFIX 23
H2A 2 0.767626 0.481326 0.106838 11.00000 -1.20000
H2B 2 0.796693 0.551503 0.193156 11.00000 -1.20000
AFIX 0
C3 1 0.890686 0.399682 0.179264 11.00000 0.02407 0.01288 =
0.01891 0.00099 0.00234 -0.00251
AFIX 23
H3A 2 0.839373 0.338839 0.199832 11.00000 -1.20000
H3B 2 0.932166 0.363166 0.133897 11.00000 -1.20000
AFIX 0
C4 1 1.021983 0.339211 0.283888 11.00000 0.02896 0.02792 =
0.04061 0.01538 -0.00010 0.00729
AFIX 137
H4A 2 0.969706 0.280933 0.304712 11.00000 -1.50000
H4B 2 1.069455 0.368396 0.330844 11.00000 -1.50000
H4C 2 1.066765 0.300643 0.242192 11.00000 -1.50000
AFIX 0
C5 1 0.717225 1.096624 0.108856 11.00000 0.01249 0.01253 =
0.00995 0.00294 0.00132 -0.00016
C6 1 0.571728 1.205276 0.170396 11.00000 0.01152 0.01708 =
0.01947 0.00045 0.00523 0.00135
AFIX 23
H6A 2 0.533331 1.139368 0.198493 11.00000 -1.20000
H6B 2 0.536696 1.217217 0.113687 11.00000 -1.20000
AFIX 0
C7 1 0.566243 1.318754 0.220955 11.00000 0.02163 0.01777 =
0.01764 -0.00132 0.00581 0.00135
AFIX 23
H7A 2 0.489982 1.331885 0.237161 11.00000 -1.20000
H7B 2 0.613029 1.310316 0.273088 11.00000 -1.20000
AFIX 0
C8 1 0.514155 1.478083 0.131296 11.00000 0.02721 0.03394 =
0.04449 0.01607 0.00607 0.01102
AFIX 137
H8A 2 0.471719 1.419791 0.097113 11.00000 -1.50000
H8B 2 0.543465 1.539771 0.094717 11.00000 -1.50000
H8C 2 0.466663 1.515784 0.171549 11.00000 -1.50000
AFIX 0
C9 1 0.770201 0.952568 -0.189398 11.00000 0.01222 0.01438 =
0.01324 -0.00098 0.00257 0.00191
C10 1 0.678622 0.913198 -0.322870 11.00000 0.01505 0.01952 =
0.01214 -0.00228 -0.00063 -0.00447
AFIX 23
H10A 2 0.604019 0.917655 -0.301467 11.00000 -1.20000
H10B 2 0.701205 0.827935 -0.324448 11.00000 -1.20000
AFIX 0
C11 1 0.680520 0.968122 -0.409499 11.00000 0.01757 0.02153 =
0.01166 -0.00140 -0.00183 -0.00047
AFIX 23
H11A 2 0.621851 0.930995 -0.445800 11.00000 -1.20000
H11B 2 0.664065 1.054852 -0.405317 11.00000 -1.20000
AFIX 0
C12 1 0.803855 0.833272 -0.469257 11.00000 0.03230 0.02275 =
0.01829 -0.00196 0.00752 0.00260
AFIX 137
H12A 2 0.823780 0.788130 -0.417984 11.00000 -1.50000
H12B 2 0.864638 0.830751 -0.507158 11.00000 -1.50000
H12C 2 0.738585 0.797380 -0.497187 11.00000 -1.50000
AFIX 0
IN1 5 0.801623 0.916586 -0.006575 11.00000 0.01342 0.01128 =
0.00977 -0.00045 0.00078 0.00042
O1 3 0.904979 0.583488 0.102903 11.00000 0.01423 0.01411 =
0.01606 0.00146 0.00177 -0.00038
O2 3 0.963937 0.437456 0.246015 11.00000 0.02514 0.01603 =
0.02462 0.00465 -0.00623 0.00082
O3 3 0.688021 1.176080 0.164288 11.00000 0.01066 0.01598 =
0.01519 -0.00281 0.00085 -0.00079
O4 3 0.601329 1.418983 0.175166 11.00000 0.02002 0.01714 =
0.03560 0.00177 0.00571 0.00042
O5 3 0.755599 0.982466 -0.269053 11.00000 0.01821 0.01763 =
0.01069 -0.00074 0.00039 -0.00390
O6 3 0.781540 0.954042 -0.448212 11.00000 0.02338 0.01998 =
0.01517 -0.00289 0.00519 -0.00684
S1 4 0.959823 0.764180 0.014282 11.00000 0.01256 0.01257 =
0.01557 0.00097 0.00306 -0.00065
S2 4 0.737325 0.733462 0.080612 11.00000 0.01220 0.01494 =
0.01686 0.00210 0.00356 0.00052
S3 4 0.627958 1.035020 0.036297 11.00000 0.01164 0.01577 =
0.01470 -0.00360 -0.00127 -0.00031
S4 4 0.853987 1.060169 0.115169 11.00000 0.01055 0.01415 =
0.01393 -0.00177 -0.00060 0.00029
S5 4 0.854076 1.047090 -0.131308 11.00000 0.01698 0.01462 =
0.01172 -0.00027 0.00024 -0.00488
S6 4 0.711542 0.830050 -0.147085 11.00000 0.01705 0.01457 =
0.01189 -0.00038 0.00041 -0.00412
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM s4599ma in P2(1)/n
REM R1 = 0.0233 for 3707 Fo > 4sig(Fo) and 0.0294 for all 4231 data
REM 229 parameters refined using 0 restraints
END
WGHT 0.0242 0.0000
REM Instructions for potential hydrogen bonds
HTAB C2 O4_$1
HTAB C2 O6_$2
HTAB C3 O3_$1
HTAB C6 O2_$3
HTAB C7 S2_$3
HTAB C10 O2_$4
HTAB C11 S1_$4
REM Highest difference peak 0.534, deepest hole -0.334, 1-sigma level 0.083
Q1 1 0.5632 1.3988 0.1295 11.00000 0.05 0.53
Q2 1 0.5440 1.5369 0.1657 11.00000 0.05 0.46
Q3 1 0.8356 0.9635 -0.0758 11.00000 0.05 0.41
Q4 1 0.7956 0.8408 -0.0023 11.00000 0.05 0.38
Q5 1 0.6715 0.9354 -0.3651 11.00000 0.05 0.36
Q6 1 0.8772 1.0648 0.0590 11.00000 0.05 0.35
Q7 1 0.6414 0.9553 0.0397 11.00000 0.05 0.35
Q8 1 0.6251 0.9406 -0.0405 11.00000 0.05 0.34
Q9 1 0.9764 0.5027 0.2474 11.00000 0.05 0.34
Q10 1 0.8621 0.9693 0.1134 11.00000 0.05 0.33
Q11 1 0.8275 1.0463 -0.0819 11.00000 0.05 0.32
Q12 1 0.4324 1.4838 0.1645 11.00000 0.05 0.31
Q13 1 0.7954 1.0012 0.0011 11.00000 0.05 0.29
Q14 1 0.9057 1.1243 0.1046 11.00000 0.05 0.29
Q15 1 0.9805 0.9073 -0.0189 11.00000 0.05 0.28
Q16 1 0.7163 0.7753 0.0223 11.00000 0.05 0.28
Q17 1 0.9601 0.9806 0.0182 11.00000 0.05 0.28
Q18 1 0.5575 1.2587 0.2048 11.00000 0.05 0.28
Q19 1 0.7835 1.0756 0.0940 11.00000 0.05 0.27
Q20 1 0.7363 0.9745 -0.2224 11.00000 0.05 0.27
;
_shelx_res_checksum 460
#######################################################################
#
# 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_s5023r
_database_code_depnum_ccdc_archive 'CCDC 1812199'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_audit_creation_date 2017-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '1.07(C14.01 H25.23 In0.93 O5.61 S5.61)'
_chemical_formula_sum 'C15 H27 In O6 S6'
_chemical_formula_weight 610.55
_chemical_melting_point ?
_chemical_oxdiff_formula InS6O6C10H12
_chemical_oxdiff_usercomment uhrs9?
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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_H-M_alt 'R -3'
_space_group_name_Hall '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
_cell_length_a 18.9024(5)
_cell_length_b 18.9024(5)
_cell_length_c 11.8583(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 3669.3(2)
_cell_formula_units_Z 5.99994
_cell_measurement_reflns_used 9348
_cell_measurement_temperature 150
_cell_measurement_theta_max 29.7510
_cell_measurement_theta_min 2.1170
_shelx_estimated_absorpt_T_max 0.864
_shelx_estimated_absorpt_T_min 0.705
_exptl_absorpt_coefficient_mu 1.505
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.73890
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.658
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1860
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0304
_diffrn_reflns_av_unetI/netI 0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 18510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.127
_diffrn_reflns_theta_min 2.121
_diffrn_ambient_temperature 150
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 29.00 68.00 1.00 2.00 -- -7.80 23.00-122.00 39
2 \w -96.00 43.00 1.00 2.00 -- -7.80 -23.00 72.00 139
3 \w 20.00 46.00 1.00 2.00 -- 5.00 57.00-120.00 26
4 \w -2.00 44.00 1.00 2.00 -- 5.00 76.00-150.00 46
5 \w 54.00 79.00 1.00 2.00 -- 5.00 76.00-150.00 25
6 \w -96.00 26.00 1.00 2.00 -- -7.80 -57.00 0.00 122
7 \w -88.00 -1.00 1.00 2.00 -- -7.80 -57.00 -90.00 87
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0186662000
_diffrn_orient_matrix_UB_12 0.0120847000
_diffrn_orient_matrix_UB_13 0.0418273000
_diffrn_orient_matrix_UB_21 0.0232314000
_diffrn_orient_matrix_UB_22 -0.0056899000
_diffrn_orient_matrix_UB_23 0.0422474000
_diffrn_orient_matrix_UB_31 0.0314197000
_diffrn_orient_matrix_UB_32 0.0412304000
_diffrn_orient_matrix_UB_33 -0.0066215000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 1917
_reflns_number_total 2183
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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 0.538
_refine_diff_density_min -0.398
_refine_diff_density_rms 0.063
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.127
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 167
_refine_ls_number_reflns 2183
_refine_ls_number_restraints 139
_refine_ls_R_factor_all 0.0340
_refine_ls_R_factor_gt 0.0286
_refine_ls_restrained_S_all 1.113
_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^)+(0.0212P)^2^+10.7099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0647
_refine_ls_wR_factor_ref 0.0661
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
O5A-C7A
2.4 with sigma of 0.02
C10A-C6A = C7A-C6A
1.54 with sigma of 0.02
C6A-C4A
2.4 with sigma of 0.02
C6A-O8A
2.4 with sigma of 0.02
O8A-C7A = O8A-C9A
1.45 with sigma of 0.02
C10A-C7A
2.4 with sigma of 0.02
S3A-C4A \\sim S3-C4
with sigma of 0.002
S2A-C4A \\sim S2-C4
with sigma of 0.002
O5A-C4A \\sim O5-C4
with sigma of 0.002
O8-C7 \\sim O8-C9
with sigma of 0.002
C10-C6 \\sim C7-C6
with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C10A \\sim C9: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C9A \\sim C9: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(In1A) = Uanis(In1)
Uanis(C10A) = Uanis(C9A)
4. Rigid body (RIGU) restrains
In1A, S3A, S2A, C4A, O5A
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
In1, S3, S2, O5, O8, C4, C6, C7, C9, C10
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
In1A, S3A, S2A, C4A, O5A, C6A, C7A, C10A, O8A, C9A
with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
Sof(S3A)=Sof(S2A)=Sof(C4A)=Sof(O5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=
Sof(H7AB)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(O8A)=Sof(C9A)=Sof(H9AA)=
Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
Sof(In1A)=0.33333*(1-FVAR(2))
Sof(In1)=0.33333*FVAR(2)
Sof(S3)=Sof(S2)=Sof(O5)=Sof(O8)=Sof(C4)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7A)=
Sof(H7B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=
Sof(H10C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
C6(H6), C6A(H6A)
6.b Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C7A(H7AA,H7AB)
6.c Me refined with riding coordinates:
C9A(H9AA,H9AB,H9AC)
6.d Idealised Me refined as rotating group:
C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
;
_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
In1 In 0.6667 0.3333 0.58324(6) 0.03043(11) Uani 0.9343(18) 3 d S TU P A 1
S3 S 0.54722(4) 0.32808(4) 0.70307(7) 0.03407(17) Uani 0.9343(18) 1 d D U . A 1
S2 S 0.59947(4) 0.40253(4) 0.47500(6) 0.03573(18) Uani 0.9343(18) 1 d D U . A 1
O5 O 0.48728(10) 0.40778(11) 0.58792(14) 0.0357(4) Uani 0.9343(18) 1 d D U . A
1
O8 O 0.31314(10) 0.30759(9) 0.58917(15) 0.0316(4) Uani 0.9343(18) 1 d D U . A 1
C4 C 0.53909(14) 0.38049(14) 0.5922(2) 0.0299(5) Uani 0.9343(18) 1 d D U . A 1
C6 C 0.43854(12) 0.40333(14) 0.6877(2) 0.0325(5) Uani 0.9343(18) 1 d D U . A 1
H6 H 0.4327 0.3590 0.7396 0.039 Uiso 0.9343(18) 1 calc R . . A 1
C7 C 0.35610(12) 0.38429(13) 0.64355(19) 0.0283(5) Uani 0.9343(18) 1 d D U . A
1
H7A H 0.3227 0.3854 0.7072 0.034 Uiso 0.9343(18) 1 calc R . . A 1
H7B H 0.3636 0.4275 0.5897 0.034 Uiso 0.9343(18) 1 calc R . . A 1
C9 C 0.27318(19) 0.24136(16) 0.6652(2) 0.0484(7) Uani 0.9343(18) 1 d D U . A 1
H9A H 0.2407 0.1907 0.6226 0.073 Uiso 0.9343(18) 1 calc GR . . A 1
H9B H 0.2372 0.2507 0.7147 0.073 Uiso 0.9343(18) 1 calc GR . . A 1
H9C H 0.3140 0.2368 0.7107 0.073 Uiso 0.9343(18) 1 calc GR . . A 1
C10 C 0.48053(17) 0.48446(16) 0.7475(3) 0.0428(7) Uani 0.9343(18) 1 d D U . A 1
H10A H 0.5341 0.4955 0.7744 0.064 Uiso 0.9343(18) 1 calc GR . . A 1
H10B H 0.4472 0.4830 0.8118 0.064 Uiso 0.9343(18) 1 calc GR . . A 1
H10C H 0.4875 0.5276 0.6952 0.064 Uiso 0.9343(18) 1 calc GR . . A 1
In1A In 0.6768(9) 0.3351(17) 0.6224(8) 0.03043(11) Uani 0.0219(6) 1 d . U . A 2
S3A S 0.5483(5) 0.3033(6) 0.7516(9) 0.035(2) Uani 0.0657(18) 1 d D U . A 2
S2A S 0.5797(6) 0.4032(6) 0.5411(8) 0.037(2) Uani 0.0657(18) 1 d D U . A 2
C4A C 0.5254(12) 0.3586(14) 0.6612(14) 0.028(5) Uani 0.0657(18) 1 d D U . A 2
O5A O 0.4634(11) 0.3660(14) 0.6966(19) 0.036(4) Uani 0.0657(18) 1 d D U . A 2
C6A C 0.3940(14) 0.3494(16) 0.672(3) 0.050(5) Uani 0.0657(18) 1 d D U . A 2
H6A H 0.3699 0.3340 0.7496 0.060 Uiso 0.0657(18) 1 calc R . . A 2
C7A C 0.388(2) 0.4285(18) 0.658(5) 0.067(6) Uani 0.0657(18) 1 d D U . A 2
H7AA H 0.3767 0.4363 0.5793 0.080 Uiso 0.0657(18) 1 calc R . . A 2
H7AB H 0.3451 0.4272 0.7078 0.080 Uiso 0.0657(18) 1 calc R . . A 2
C10A C 0.321(3) 0.285(2) 0.608(5) 0.051(3) Uani 0.0657(18) 1 d D U . A 2
H10D H 0.3387 0.2793 0.5320 0.076 Uiso 0.0657(18) 1 calc GR . . A 2
H10E H 0.2800 0.3021 0.6011 0.076 Uiso 0.0657(18) 1 calc GR . . A 2
H10F H 0.2978 0.2330 0.6475 0.076 Uiso 0.0657(18) 1 calc GR . . A 2
O8A O 0.471(2) 0.4936(17) 0.694(3) 0.064(6) Uani 0.0657(18) 1 d D U . A 2
C9A C 0.454(3) 0.531(3) 0.787(3) 0.051(3) Uani 0.0657(18) 1 d D U . A 2
H9AA H 0.5051 0.5758 0.8176 0.076 Uiso 0.0657(18) 1 calc R . . A 2
H9AB H 0.4197 0.5536 0.7606 0.076 Uiso 0.0657(18) 1 calc R . . A 2
H9AC H 0.4248 0.4908 0.8461 0.076 Uiso 0.0657(18) 1 calc R . . 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
In1 0.02139(12) 0.02139(12) 0.0485(3) 0.000 0.000 0.01069(6)
S3 0.0293(3) 0.0362(3) 0.0408(4) 0.0091(3) 0.0038(3) 0.0194(3)
S2 0.0350(3) 0.0389(3) 0.0399(4) 0.0071(3) 0.0080(3) 0.0235(3)
O5 0.0318(9) 0.0460(10) 0.0376(9) 0.0083(7) 0.0043(7) 0.0258(8)
O8 0.0308(8) 0.0285(9) 0.0284(9) -0.0018(7) -0.0016(7) 0.0095(7)
C4 0.0237(11) 0.0283(11) 0.0379(13) 0.0009(10) -0.0002(10) 0.0130(9)
C6 0.0262(11) 0.0348(12) 0.0372(12) -0.0020(10) 0.0010(9) 0.0159(10)
C7 0.0261(10) 0.0261(11) 0.0336(12) -0.0021(9) -0.0011(9) 0.0137(9)
C9 0.0503(16) 0.0355(14) 0.0415(15) 0.0041(11) -0.0001(12) 0.0081(12)
C10 0.0300(13) 0.0378(14) 0.0490(16) -0.0080(12) -0.0036(12) 0.0082(11)
In1A 0.02139(12) 0.02139(12) 0.0485(3) 0.000 0.000 0.01069(6)
S3A 0.034(4) 0.036(4) 0.036(4) 0.013(3) 0.002(3) 0.019(3)
S2A 0.046(5) 0.049(5) 0.032(5) 0.013(4) 0.014(4) 0.035(4)
C4A 0.033(6) 0.027(10) 0.023(6) 0.003(6) 0.000(5) 0.015(7)
O5A 0.039(5) 0.036(7) 0.033(7) 0.004(5) 0.005(4) 0.020(5)
C6A 0.043(5) 0.054(6) 0.055(11) -0.008(6) -0.003(5) 0.026(4)
C7A 0.063(8) 0.055(6) 0.087(13) -0.015(7) -0.023(8) 0.034(6)
C10A 0.050(4) 0.041(4) 0.048(4) 0.004(4) -0.003(4) 0.013(3)
O8A 0.063(8) 0.065(8) 0.057(8) -0.011(7) -0.010(6) 0.027(6)
C9A 0.050(4) 0.041(4) 0.048(4) 0.004(4) -0.003(4) 0.013(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
In1 S3 2.6274(7) 3_665 ?
In1 S3 2.6274(7) 2_655 ?
In1 S3 2.6274(7) . ?
In1 S2 2.5755(7) 3_665 ?
In1 S2 2.5755(7) . ?
In1 S2 2.5755(7) 2_655 ?
S3 C4 1.699(3) . ?
S2 C4 1.712(3) . ?
O5 C4 1.317(3) . ?
O5 C6 1.476(3) . ?
O8 C7 1.414(2) . ?
O8 C9 1.416(2) . ?
C6 H6 1.0000 . ?
C6 C7 1.507(2) . ?
C6 C10 1.506(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
In1A In1A 0.31(2) 2_655 ?
In1A In1A 0.31(2) 3_665 ?
In1A S3A 2.673(13) . ?
In1A S3A 2.45(2) 2_655 ?
In1A S3A 2.48(2) 3_665 ?
In1A S2A 2.77(3) 2_655 ?
In1A S2A 2.598(17) 3_665 ?
In1A S2A 2.88(2) . ?
S3A In1A 2.48(2) 2_655 ?
S3A In1A 2.45(2) 3_665 ?
S3A C4A 1.698(3) . ?
S2A In1A 2.77(3) 3_665 ?
S2A In1A 2.598(17) 2_655 ?
S2A C4A 1.711(3) . ?
C4A O5A 1.316(3) . ?
O5A C6A 1.22(2) . ?
C6A H6A 1.0000 . ?
C6A C7A 1.565(18) . ?
C6A C10A 1.511(19) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C7A O8A 1.497(19) . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
O8A C9A 1.44(2) . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 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
S3 In1 S3 93.51(2) 3_665 . ?
S3 In1 S3 93.51(2) 2_655 3_665 ?
S3 In1 S3 93.51(2) 2_655 . ?
S2 In1 S3 156.58(2) . 2_655 ?
S2 In1 S3 103.59(2) 2_655 . ?
S2 In1 S3 69.88(2) 3_665 3_665 ?
S2 In1 S3 69.88(2) 2_655 2_655 ?
S2 In1 S3 156.58(2) 2_655 3_665 ?
S2 In1 S3 103.59(2) . 3_665 ?
S2 In1 S3 156.58(2) 3_665 . ?
S2 In1 S3 103.59(2) 3_665 2_655 ?
S2 In1 S3 69.88(2) . . ?
S2 In1 S2 97.32(2) 3_665 . ?
S2 In1 S2 97.32(2) 2_655 3_665 ?
S2 In1 S2 97.32(2) 2_655 . ?
C4 S3 In1 83.45(9) . . ?
C4 S2 In1 84.83(8) . . ?
C4 O5 C6 120.81(19) . . ?
C7 O8 C9 113.30(19) . . ?
S3 C4 S2 121.77(14) . . ?
O5 C4 S3 124.1(2) . . ?
O5 C4 S2 114.16(18) . . ?
O5 C6 H6 110.2 . . ?
O5 C6 C7 106.04(17) . . ?
O5 C6 C10 108.86(19) . . ?
C7 C6 H6 110.2 . . ?
C10 C6 H6 110.2 . . ?
C10 C6 C7 111.2(2) . . ?
O8 C7 C6 113.48(18) . . ?
O8 C7 H7A 108.9 . . ?
O8 C7 H7B 108.9 . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
O8 C9 H9A 109.5 . . ?
O8 C9 H9B 109.5 . . ?
O8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
In1A In1A In1A 60.01(4) 2_655 3_665 ?
In1A In1A S3A 90(8) 3_665 2_655 ?
In1A In1A S3A 127(6) 3_665 3_665 ?
In1A In1A S3A 47(5) 2_655 . ?
In1A In1A S3A 42(4) 3_665 . ?
In1A In1A S3A 83(8) 2_655 3_665 ?
In1A In1A S3A 133(5) 2_655 2_655 ?
In1A In1A S2A 158(2) 3_665 3_665 ?
In1A In1A S2A 53(8) 3_665 2_655 ?
In1A In1A S2A 109(9) 2_655 2_655 ?
In1A In1A S2A 65(8) 3_665 . ?
In1A In1A S2A 19.8(17) 2_655 . ?
In1A In1A S2A 121(9) 2_655 3_665 ?
S3A In1A S3A 90.1(5) 2_655 3_665 ?
S3A In1A S3A 85.6(5) 2_655 . ?
S3A In1A S3A 85.2(5) 3_665 . ?
S3A In1A S2A 69.9(8) 2_655 2_655 ?
S3A In1A S2A 72.6(6) 3_665 3_665 ?
S3A In1A S2A 90.8(7) . 2_655 ?
S3A In1A S2A 100.1(5) 2_655 3_665 ?
S3A In1A S2A 159.9(8) 3_665 2_655 ?
S3A In1A S2A 150.5(6) 2_655 . ?
S3A In1A S2A 92.3(9) 3_665 . ?
S3A In1A S2A 65.3(4) . . ?
S2A In1A S3A 157.0(11) 3_665 . ?
S2A In1A S2A 104.0(5) 2_655 . ?
S2A In1A S2A 112.2(6) 3_665 2_655 ?
S2A In1A S2A 108.6(8) 3_665 . ?
In1A S3A In1A 5.2(5) 2_655 . ?
In1A S3A In1A 7.1(5) 3_665 2_655 ?
In1A S3A In1A 4.8(5) 3_665 . ?
C4A S3A In1A 83.8(6) . 2_655 ?
C4A S3A In1A 88.2(8) . 3_665 ?
C4A S3A In1A 89.0(7) . . ?
In1A S2A In1A 5.8(5) 3_665 . ?
In1A S2A In1A 2.3(2) 2_655 . ?
In1A S2A In1A 5.4(7) 2_655 3_665 ?
C4A S2A In1A 79.8(7) . 2_655 ?
C4A S2A In1A 82.0(6) . . ?
C4A S2A In1A 78.1(6) . 3_665 ?
S3A C4A S2A 123.6(8) . . ?
O5A C4A S3A 112.3(12) . . ?
O5A C4A S2A 124.0(12) . . ?
C6A O5A C4A 143(3) . . ?
O5A C6A H6A 97.7 . . ?
O5A C6A C7A 111.2(18) . . ?
O5A C6A C10A 139(3) . . ?
C7A C6A H6A 97.7 . . ?
C10A C6A H6A 97.7 . . ?
C10A C6A C7A 103.9(16) . . ?
C6A C7A H7AA 111.4 . . ?
C6A C7A H7AB 111.4 . . ?
H7AA C7A H7AB 109.3 . . ?
O8A C7A C6A 101.9(14) . . ?
O8A C7A H7AA 111.4 . . ?
O8A C7A H7AB 111.4 . . ?
C6A C10A H10D 109.5 . . ?
C6A C10A H10E 109.5 . . ?
C6A C10A H10F 109.5 . . ?
H10D C10A H10E 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
C9A O8A C7A 102(3) . . ?
O8A C9A H9AA 109.5 . . ?
O8A C9A H9AB 109.5 . . ?
O8A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
In1 S3 C4 S2 2.64(14) . . . . ?
In1 S3 C4 O5 -177.1(2) . . . . ?
In1 S2 C4 S3 -2.69(14) . . . . ?
In1 S2 C4 O5 177.10(18) . . . . ?
O5 C6 C7 O8 63.4(2) . . . . ?
C4 O5 C6 C7 -143.2(2) . . . . ?
C4 O5 C6 C10 97.0(3) . . . . ?
C6 O5 C4 S3 7.8(3) . . . . ?
C6 O5 C4 S2 -171.99(15) . . . . ?
C9 O8 C7 C6 80.7(3) . . . . ?
C10 C6 C7 O8 -178.4(2) . . . . ?
In1A S3A C4A S2A 1.9(19) . . . . ?
In1A S3A C4A S2A -2.8(18) 3_665 . . . ?
In1A S3A C4A S2A 2.8(18) 2_655 . . . ?
In1A S3A C4A O5A -175(2) . . . . ?
In1A S3A C4A O5A -175(2) 2_655 . . . ?
In1A S3A C4A O5A 180(2) 3_665 . . . ?
In1A S2A C4A S3A -1.8(18) . . . . ?
In1A S2A C4A S3A -2.7(17) 2_655 . . . ?
In1A S2A C4A S3A 2.6(17) 3_665 . . . ?
In1A S2A C4A O5A 174(3) 2_655 . . . ?
In1A S2A C4A O5A 180(3) 3_665 . . . ?
In1A S2A C4A O5A 175(3) . . . . ?
S3A C4A O5A C6A -118(4) . . . . ?
S2A C4A O5A C6A 65(5) . . . . ?
C4A O5A C6A C7A -119(4) . . . . ?
C4A O5A C6A C10A 28(8) . . . . ?
O5A C6A C7A O8A -6(5) . . . . ?
C6A C7A O8A C9A -121(4) . . . . ?
C10A C6A C7A O8A -165(4) . . . . ?
_shelx_res_file
;
TITL s5023r R -3 :h R = 0.05
CELL 0.71073 18.9024 18.9024 11.8583 90 90 120
ZERR 5.99994 0.0005 0.0005 0.0004 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H In O S
UNIT 90 162 6 36 36
DFIX 2.4 O5A C7A
DFIX 1.54 C10A C6A C7A C6A
DFIX 2.4 C6A C4A
DFIX 2.4 C6A O8A
DFIX 1.45 O8A C7A O8A C9A
DFIX 2.4 C10A C7A
SADI 0.002 S3A C4A S3 C4
SADI 0.002 S2A C4A S2 C4
SADI 0.002 O5A C4A O5 C4
SADI 0.002 O8 C7 O8 C9
SADI 0.002 C10 C6 C7 C6
SIMU C10
SIMU 0.002 0.004 2 C10A C9
SIMU 0.002 0.004 2 C9A C9
RIGU In1A S3A S2A C4A O5A
RIGU In1 S3 S2 O5 O8 C4 C6 C7 C9 C10
RIGU 0.002 0.002 In1A S3A S2A C4A O5A C6A C7A C10A O8A C9A
EADP In1A In1
EADP C10A C9A
L.S. 25
PLAN -20
SIZE 0.25 0.22 0.1
TEMP -123.15
BOND $H
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.021200 10.709900
FVAR 0.17998 0.93429
PART 1
IN1 3 0.666667 0.333333 0.583236 20.33333 0.02139 0.02139 =
0.04852 0.00000 0.00000 0.01069
S3 5 0.547220 0.328083 0.703075 21.00000 0.02932 0.03616 =
0.04077 0.00905 0.00383 0.01940
S2 5 0.599475 0.402535 0.474997 21.00000 0.03501 0.03890 =
0.03993 0.00711 0.00799 0.02346
O5 4 0.487278 0.407783 0.587923 21.00000 0.03182 0.04601 =
0.03761 0.00826 0.00433 0.02582
O8 4 0.313144 0.307590 0.589175 21.00000 0.03082 0.02851 =
0.02837 -0.00184 -0.00164 0.00947
C4 1 0.539092 0.380485 0.592192 21.00000 0.02366 0.02831 =
0.03790 0.00089 -0.00020 0.01304
C6 1 0.438542 0.403329 0.687718 21.00000 0.02622 0.03484 =
0.03720 -0.00199 0.00101 0.01587
AFIX 13
H6 2 0.432666 0.358982 0.739571 21.00000 -1.20000
AFIX 0
C7 1 0.356103 0.384293 0.643547 21.00000 0.02611 0.02609 =
0.03358 -0.00215 -0.00110 0.01370
AFIX 23
H7A 2 0.322743 0.385378 0.707163 21.00000 -1.20000
H7B 2 0.363571 0.427503 0.589660 21.00000 -1.20000
AFIX 0
C9 1 0.273183 0.241357 0.665156 21.00000 0.05026 0.03547 =
0.04153 0.00407 -0.00006 0.00809
AFIX 137
H9A 2 0.240733 0.190685 0.622634 21.00000 -1.50000
H9B 2 0.237177 0.250733 0.714700 21.00000 -1.50000
H9C 2 0.313974 0.236802 0.710731 21.00000 -1.50000
AFIX 0
C10 1 0.480534 0.484462 0.747496 21.00000 0.02996 0.03777 =
0.04897 -0.00797 -0.00365 0.00815
AFIX 137
H10A 2 0.534144 0.495549 0.774423 21.00000 -1.50000
H10B 2 0.447242 0.482994 0.811779 21.00000 -1.50000
H10C 2 0.487546 0.527648 0.695195 21.00000 -1.50000
AFIX 0
PART 0
PART 2
IN1A 3 0.676804 0.335094 0.622439 -20.33333 0.02139 0.02139 =
0.04852 0.00000 0.00000 0.01069
S3A 5 0.548318 0.303293 0.751568 -21.00000 0.03402 0.03555 =
0.03564 0.01254 0.00230 0.01850
S2A 5 0.579689 0.403208 0.541052 -21.00000 0.04600 0.04878 =
0.03183 0.01296 0.01383 0.03538
C4A 1 0.525393 0.358604 0.661181 -21.00000 0.03315 0.02741 =
0.02263 0.00307 0.00029 0.01510
O5A 4 0.463407 0.365960 0.696570 -21.00000 0.03873 0.03574 =
0.03346 0.00390 0.00476 0.01957
C6A 1 0.394004 0.349358 0.672316 -21.00000 0.04278 0.05401 =
0.05514 -0.00805 -0.00320 0.02619
AFIX 13
H6A 2 0.369909 0.333988 0.749627 -21.00000 -1.20000
AFIX 0
C7A 1 0.387966 0.428527 0.658489 -21.00000 0.06323 0.05501 =
0.08697 -0.01476 -0.02315 0.03350
AFIX 23
H7AA 2 0.376673 0.436268 0.579296 -21.00000 -1.20000
H7AB 2 0.345091 0.427248 0.707827 -21.00000 -1.20000
AFIX 0
C10A 1 0.321235 0.285341 0.607532 -21.00000 0.05030 0.04113 =
0.04789 0.00407 -0.00268 0.01349
AFIX 137
H10D 2 0.338654 0.279339 0.532023 -21.00000 -1.50000
H10E 2 0.280024 0.302121 0.601059 -21.00000 -1.50000
H10F 2 0.297821 0.233032 0.647488 -21.00000 -1.50000
AFIX 0
O8A 4 0.471401 0.493622 0.694428 -21.00000 0.06261 0.06549 =
0.05723 -0.01068 -0.00964 0.02733
C9A 1 0.453876 0.531476 0.787041 -21.00000 0.05030 0.04113 =
0.04789 0.00407 -0.00268 0.01349
AFIX 33
H9AA 2 0.505119 0.575826 0.817611 -21.00000 -1.50000
H9AB 2 0.419724 0.553620 0.760609 -21.00000 -1.50000
H9AC 2 0.424832 0.490797 0.846065 -21.00000 -1.50000
AFIX 0
HKLF 4
REM s5023r R -3 :h R = 0.05
REM R1 = 0.0286 for 1917 Fo > 4sig(Fo) and 0.0340 for all 2183 data
REM 167 parameters refined using 139 restraints
END
WGHT 0.0212 10.7035
REM Highest difference peak 0.538, deepest hole -0.398, 1-sigma level 0.063
Q1 1 0.4440 0.4282 0.6241 11.00000 0.05 0.54
Q2 1 0.7794 0.4209 0.4870 11.00000 0.05 0.51
Q3 1 0.4520 0.3499 0.5753 11.00000 0.05 0.46
Q4 1 0.7898 0.3671 0.5205 11.00000 0.05 0.45
Q5 1 0.3277 0.2680 0.6524 11.00000 0.05 0.40
Q6 1 0.5154 0.3028 0.6498 11.00000 0.05 0.39
Q7 1 0.4533 0.4435 0.7201 11.00000 0.05 0.28
Q8 1 0.3959 0.4018 0.6835 11.00000 0.05 0.28
Q9 1 0.6819 0.3091 0.5508 11.00000 0.05 0.27
Q10 1 0.6236 0.2900 0.6059 11.00000 0.05 0.25
Q11 1 0.4839 0.4157 0.5252 11.00000 0.05 0.24
Q12 1 0.3570 0.3331 0.6776 11.00000 0.05 0.22
Q13 1 0.3508 0.2995 0.5741 11.00000 0.05 0.21
Q14 1 0.6222 0.2575 0.5164 11.00000 0.05 0.21
Q15 1 0.6209 0.2600 0.4555 11.00000 0.05 0.20
Q16 1 0.4700 0.8307 0.0757 11.00000 0.05 0.19
Q17 1 0.5247 0.3393 0.5781 11.00000 0.05 0.19
Q18 1 0.5566 0.4135 0.4361 11.00000 0.05 0.19
Q19 1 0.2355 0.2192 0.7481 11.00000 0.05 0.18
Q20 1 0.3501 0.3464 0.6151 11.00000 0.05 0.18
;
_shelx_res_checksum 42803
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.690
#######################################################################
#
# 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_s4712r
_database_code_depnum_ccdc_archive 'CCDC 1812204'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_audit_creation_date 2017-04-20
_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 'C12 H21 In O3 S6'
_chemical_formula_sum 'C12 H21 In O3 S6'
_chemical_formula_weight 520.47
_chemical_melting_point ?
_chemical_oxdiff_formula InS4C10H10O2
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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/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 12.6914(11)
_cell_length_b 16.4263(9)
_cell_length_c 10.4553(8)
_cell_angle_alpha 90
_cell_angle_beta 113.465(10)
_cell_angle_gamma 90
_cell_volume 1999.4(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4152
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 28.8560
_cell_measurement_theta_min 3.2530
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.815
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.43401
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.21a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.729
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 21 1 0.1530
-7 -21 -1 0.1530
-5 -4 14 0.1100
5 4 -14 0.1100
-16 8 1 0.0235
16 -8 -1 0.0015
_exptl_crystal_size_max 0.323
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.025
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.9998 21.0020 0.9992 0.9850 -0.2583 0.0087
-6.9998 -21.0020 -0.9992 -0.9850 0.2583 -0.0087
-4.9997 -4.0024 14.0001 -0.0495 0.0061 0.9693
4.9997 4.0024 -14.0001 0.0495 -0.0061 -0.9693
-16.0011 8.0008 1.0000 0.1478 0.9926 -0.0990
16.0011 -8.0008 -1.0000 -0.1478 -0.9926 0.0990
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0426
_diffrn_reflns_av_unetI/netI 0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 11553
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 26.371
_diffrn_reflns_theta_min 2.144
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -22.00 44.00 1.00 2.00 -- -5.10 -19.00 -90.00 66
2 \w -47.00 23.00 1.00 2.00 -- -5.10 -57.00 30.00 70
3 \w -94.00 -35.00 1.00 2.00 -- -5.10 -19.00 -90.00 59
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0126152000
_diffrn_orient_matrix_UB_12 0.0420760000
_diffrn_orient_matrix_UB_13 0.0129964000
_diffrn_orient_matrix_UB_21 -0.0590494000
_diffrn_orient_matrix_UB_22 0.0082534000
_diffrn_orient_matrix_UB_23 -0.0182935000
_diffrn_orient_matrix_UB_31 0.0078209000
_diffrn_orient_matrix_UB_32 -0.0055431000
_diffrn_orient_matrix_UB_33 0.0704469000
_diffrn_oxdiff_ac3_digest_frames
;
010f9fa70e24c2ec72f05ed76a1ca9d8810019549d0
;
_diffrn_oxdiff_ac3_digest_hkl
;
0132770fa682e092cbfb9b9d65feb7ced3c3ff
;
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3457
_reflns_number_total 4029
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.333
_refine_diff_density_min -1.223
_refine_diff_density_rms 0.111
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 202
_refine_ls_number_reflns 4029
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0382
_refine_ls_R_factor_gt 0.0315
_refine_ls_restrained_S_all 1.056
_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^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0777
_refine_ls_wR_factor_ref 0.0802
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C19(H19A,H19B), C20(H20A,H20B), C12(H12A,H12B), C5(H5A,H5B), C6(H6A,H6B),
C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
C21(H21A,H21B,H21C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;
_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
In1 In 0.27088(2) 0.49139(2) 0.74851(2) 0.01625(9) Uani 1 1 d . . . . .
S8 S 0.25234(6) 0.57509(5) 0.52846(7) 0.01771(17) Uani 1 1 d . . . . .
S15 S 0.07672(6) 0.53378(5) 0.75344(7) 0.01908(17) Uani 1 1 d . . . . .
S22 S 0.20215(7) 0.35220(5) 0.62403(7) 0.01874(17) Uani 1 1 d . . . . .
S9 S 0.30133(6) 0.61049(5) 0.92593(7) 0.01847(17) Uani 1 1 d . . . . .
S2 S 0.47063(7) 0.51015(5) 0.74249(8) 0.01879(17) Uani 1 1 d . . . . .
S16 S 0.32718(7) 0.37700(5) 0.93051(7) 0.01873(17) Uani 1 1 d . . . . .
O11 O 0.10064(17) 0.64476(13) 0.93638(19) 0.0177(4) Uani 1 1 d . . . . .
O18 O 0.25853(17) 0.23756(13) 0.81908(19) 0.0183(4) Uani 1 1 d . . . . .
O4 O 0.46197(16) 0.59817(14) 0.53738(19) 0.0188(4) Uani 1 1 d . . . . .
C17 C 0.2607(2) 0.31520(19) 0.7898(3) 0.0169(6) Uani 1 1 d . . . . .
C10 C 0.1574(2) 0.60051(18) 0.8791(3) 0.0164(6) Uani 1 1 d . . . . .
C3 C 0.3976(3) 0.56439(19) 0.5945(3) 0.0180(6) Uani 1 1 d . . . . .
C19 C 0.2079(3) 0.17835(19) 0.7062(3) 0.0196(6) Uani 1 1 d . . . . .
H19A H 0.245400 0.181498 0.641595 0.023 Uiso 1 1 calc R . . . .
H19B H 0.126725 0.189388 0.655417 0.023 Uiso 1 1 calc R . . . .
C20 C 0.2248(3) 0.0951(2) 0.7719(3) 0.0218(7) Uani 1 1 d . . . . .
H20A H 0.184705 0.092105 0.833773 0.026 Uiso 1 1 calc R . . . .
H20B H 0.305858 0.086119 0.827041 0.026 Uiso 1 1 calc R . . . .
C12 C 0.1663(3) 0.7020(2) 1.0474(3) 0.0193(6) Uani 1 1 d . . . . .
H12A H 0.206138 0.740874 1.012677 0.023 Uiso 1 1 calc R . . . .
H12B H 0.222994 0.672762 1.124923 0.023 Uiso 1 1 calc R . . . .
C5 C 0.4109(3) 0.6465(2) 0.4095(3) 0.0197(6) Uani 1 1 d . . . . .
H5A H 0.351207 0.681805 0.414133 0.024 Uiso 1 1 calc R . . . .
H5B H 0.377445 0.611221 0.329026 0.024 Uiso 1 1 calc R . . . .
C6 C 0.5062(3) 0.6960(2) 0.3991(3) 0.0205(7) Uani 1 1 d . . . . .
H6A H 0.568916 0.660164 0.405946 0.025 Uiso 1 1 calc R . . . .
H6B H 0.534533 0.733823 0.476732 0.025 Uiso 1 1 calc R . . . .
C13 C 0.0842(3) 0.7457(2) 1.0947(3) 0.0235(7) Uani 1 1 d . . . . .
H13A H 0.025050 0.770986 1.014330 0.028 Uiso 1 1 calc R . . . .
H13B H 0.125515 0.788794 1.158334 0.028 Uiso 1 1 calc R . . . .
C21 C 0.1797(3) 0.0293(2) 0.6612(3) 0.0232(7) Uani 1 1 d . . . . .
H21A H 0.100535 0.040017 0.603269 0.035 Uiso 1 1 calc GR . . . .
H21B H 0.186075 -0.022731 0.705369 0.035 Uiso 1 1 calc GR . . . .
H21C H 0.223838 0.029195 0.605053 0.035 Uiso 1 1 calc GR . . . .
C7 C 0.4677(3) 0.7435(2) 0.2630(3) 0.0225(7) Uani 1 1 d . . . . .
H7A H 0.446177 0.706170 0.186179 0.034 Uiso 1 1 calc GR . . . .
H7B H 0.529704 0.777227 0.263553 0.034 Uiso 1 1 calc GR . . . .
H7C H 0.403131 0.777077 0.253546 0.034 Uiso 1 1 calc GR . . . .
C14 C 0.0267(3) 0.6920(2) 1.1667(3) 0.0299(8) Uani 1 1 d . . . . .
H14A H -0.016441 0.649981 1.103835 0.045 Uiso 1 1 calc GR . . . .
H14B H -0.023966 0.724410 1.193675 0.045 Uiso 1 1 calc GR . . . .
H14C H 0.084310 0.667686 1.248046 0.045 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
In1 0.02434(14) 0.01042(13) 0.01788(13) 0.00010(7) 0.01253(10) 0.00012(8)
S8 0.0222(4) 0.0147(4) 0.0186(4) 0.0019(3) 0.0107(3) 0.0006(3)
S15 0.0228(4) 0.0164(4) 0.0206(4) -0.0040(3) 0.0113(3) -0.0015(3)
S22 0.0288(4) 0.0136(4) 0.0152(3) -0.0001(3) 0.0102(3) -0.0028(3)
S9 0.0220(4) 0.0149(4) 0.0210(4) -0.0027(3) 0.0112(3) -0.0010(3)
S2 0.0233(4) 0.0162(4) 0.0197(4) 0.0029(3) 0.0115(3) 0.0021(3)
S16 0.0295(4) 0.0115(4) 0.0155(3) -0.0008(3) 0.0093(3) -0.0002(3)
O11 0.0221(11) 0.0144(12) 0.0189(10) -0.0037(8) 0.0105(8) -0.0001(9)
O18 0.0275(11) 0.0112(11) 0.0158(10) -0.0008(8) 0.0082(8) -0.0014(9)
O4 0.0206(11) 0.0183(12) 0.0196(10) 0.0047(9) 0.0101(8) 0.0015(9)
C17 0.0212(15) 0.0149(16) 0.0197(14) -0.0007(12) 0.0137(12) 0.0009(12)
C10 0.0264(16) 0.0102(15) 0.0154(13) 0.0037(11) 0.0112(12) 0.0012(12)
C3 0.0272(16) 0.0102(16) 0.0204(14) -0.0032(11) 0.0135(12) 0.0007(12)
C19 0.0283(17) 0.0139(17) 0.0180(14) -0.0039(12) 0.0107(13) -0.0023(13)
C20 0.0293(17) 0.0140(17) 0.0215(15) 0.0000(12) 0.0095(13) -0.0015(13)
C12 0.0214(16) 0.0158(16) 0.0195(14) -0.0058(12) 0.0068(12) -0.0022(12)
C5 0.0263(16) 0.0173(17) 0.0178(14) 0.0035(12) 0.0114(12) 0.0018(13)
C6 0.0270(17) 0.0176(17) 0.0196(15) 0.0022(12) 0.0121(13) -0.0022(13)
C13 0.0244(16) 0.0202(18) 0.0254(16) -0.0083(13) 0.0096(13) 0.0008(13)
C21 0.0329(18) 0.0144(17) 0.0271(16) -0.0022(13) 0.0169(14) -0.0023(14)
C7 0.0269(17) 0.0208(18) 0.0217(15) 0.0024(13) 0.0116(13) -0.0043(14)
C14 0.0320(19) 0.037(2) 0.0238(16) -0.0089(14) 0.0145(14) -0.0013(16)
_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
In1 S8 2.6091(7) . ?
In1 S15 2.5809(8) . ?
In1 S22 2.6035(8) . ?
In1 S9 2.6166(8) . ?
In1 S2 2.5793(8) . ?
In1 S16 2.5650(8) . ?
S8 C3 1.700(3) . ?
S15 C10 1.704(3) . ?
S22 C17 1.703(3) . ?
S9 C10 1.701(3) . ?
S2 C3 1.705(3) . ?
S16 C17 1.708(3) . ?
O11 C10 1.322(3) . ?
O11 C12 1.468(3) . ?
O18 C17 1.314(4) . ?
O18 C19 1.466(3) . ?
O4 C3 1.312(3) . ?
O4 C5 1.466(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.507(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.519(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.502(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.496(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.522(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.521(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 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
S8 In1 S9 99.62(2) . . ?
S15 In1 S8 97.11(3) . . ?
S15 In1 S22 96.57(3) . . ?
S15 In1 S9 69.93(2) . . ?
S22 In1 S8 97.31(2) . . ?
S22 In1 S9 159.47(2) . . ?
S2 In1 S8 70.12(2) . . ?
S2 In1 S15 157.48(3) . . ?
S2 In1 S22 103.28(3) . . ?
S2 In1 S9 93.37(3) . . ?
S16 In1 S8 160.19(3) . . ?
S16 In1 S15 99.73(3) . . ?
S16 In1 S22 70.51(2) . . ?
S16 In1 S9 95.91(3) . . ?
S16 In1 S2 96.86(3) . . ?
C3 S8 In1 83.40(10) . . ?
C10 S15 In1 84.47(10) . . ?
C17 S22 In1 83.17(11) . . ?
C10 S9 In1 83.42(10) . . ?
C3 S2 In1 84.26(10) . . ?
C17 S16 In1 84.27(10) . . ?
C10 O11 C12 118.0(2) . . ?
C17 O18 C19 120.0(2) . . ?
C3 O4 C5 121.0(2) . . ?
S22 C17 S16 122.02(19) . . ?
O18 C17 S22 122.8(2) . . ?
O18 C17 S16 115.1(2) . . ?
S9 C10 S15 122.05(17) . . ?
O11 C10 S15 115.7(2) . . ?
O11 C10 S9 122.2(2) . . ?
S8 C3 S2 122.16(17) . . ?
O4 C3 S8 122.9(2) . . ?
O4 C3 S2 115.0(2) . . ?
O18 C19 H19A 110.2 . . ?
O18 C19 H19B 110.2 . . ?
O18 C19 C20 107.3(2) . . ?
H19A C19 H19B 108.5 . . ?
C20 C19 H19A 110.2 . . ?
C20 C19 H19B 110.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 C21 110.8(2) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
O11 C12 H12A 110.0 . . ?
O11 C12 H12B 110.0 . . ?
O11 C12 C13 108.5(2) . . ?
H12A C12 H12B 108.4 . . ?
C13 C12 H12A 110.0 . . ?
C13 C12 H12B 110.0 . . ?
O4 C5 H5A 110.4 . . ?
O4 C5 H5B 110.4 . . ?
O4 C5 C6 106.5(2) . . ?
H5A C5 H5B 108.6 . . ?
C6 C5 H5A 110.4 . . ?
C6 C5 H5B 110.4 . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C5 C6 C7 112.3(2) . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C12 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
C12 C13 C14 114.7(3) . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
In1 S8 C3 S2 2.32(17) . . . . ?
In1 S8 C3 O4 -176.4(3) . . . . ?
In1 S15 C10 S9 3.63(16) . . . . ?
In1 S15 C10 O11 -177.3(2) . . . . ?
In1 S22 C17 S16 -1.43(16) . . . . ?
In1 S22 C17 O18 178.7(2) . . . . ?
In1 S9 C10 S15 -3.59(16) . . . . ?
In1 S9 C10 O11 177.4(2) . . . . ?
In1 S2 C3 S8 -2.34(17) . . . . ?
In1 S2 C3 O4 176.5(2) . . . . ?
In1 S16 C17 S22 1.45(16) . . . . ?
In1 S16 C17 O18 -178.6(2) . . . . ?
O11 C12 C13 C14 66.3(3) . . . . ?
O18 C19 C20 C21 -177.3(2) . . . . ?
O4 C5 C6 C7 174.4(2) . . . . ?
C17 O18 C19 C20 176.6(2) . . . . ?
C10 O11 C12 C13 179.3(2) . . . . ?
C3 O4 C5 C6 162.6(3) . . . . ?
C19 O18 C17 S22 2.4(4) . . . . ?
C19 O18 C17 S16 -177.52(19) . . . . ?
C12 O11 C10 S15 178.70(19) . . . . ?
C12 O11 C10 S9 -2.2(3) . . . . ?
C5 O4 C3 S8 -1.3(4) . . . . ?
C5 O4 C3 S2 179.9(2) . . . . ?
_shelx_res_file
;
TITL s4712r_a.res in P2(1)/c
s4712r.res
created by SHELXL-2016/6 at 11:42:31 on 20-Apr-2017
REM Old TITL s4712r in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.078, Rweak 0.002, Alpha 0.029, Orientation as input
REM Formula found by SHELXT: C12 O3 S6 In
CELL 0.71073 12.691426 16.426263 10.455328 90 113.4646 90
ZERR 4 0.001071 0.000915 0.000844 0 0.0098 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H In O S
UNIT 48 84 4 12 24
L.S. 4
PLAN 11
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
SHEL 9999 0.8
REM
REM
REM
WGHT 0.038300
FVAR 1.08354
IN1 3 0.270882 0.491390 0.748515 11.00000 0.02434 0.01042 =
0.01788 0.00010 0.01253 0.00012
S8 5 0.252338 0.575088 0.528463 11.00000 0.02224 0.01471 =
0.01862 0.00193 0.01072 0.00062
S15 5 0.076716 0.533784 0.753439 11.00000 0.02278 0.01644 =
0.02055 -0.00397 0.01129 -0.00149
S22 5 0.202153 0.352202 0.624033 11.00000 0.02880 0.01360 =
0.01518 -0.00007 0.01018 -0.00279
S9 5 0.301333 0.610491 0.925926 11.00000 0.02199 0.01486 =
0.02103 -0.00272 0.01117 -0.00099
S2 5 0.470632 0.510151 0.742490 11.00000 0.02328 0.01616 =
0.01969 0.00286 0.01148 0.00207
S16 5 0.327177 0.376996 0.930508 11.00000 0.02950 0.01153 =
0.01546 -0.00077 0.00925 -0.00019
O11 4 0.100638 0.644760 0.936381 11.00000 0.02214 0.01435 =
0.01894 -0.00374 0.01050 -0.00015
O18 4 0.258535 0.237564 0.819081 11.00000 0.02748 0.01122 =
0.01584 -0.00083 0.00819 -0.00141
O4 4 0.461972 0.598174 0.537381 11.00000 0.02056 0.01826 =
0.01958 0.00467 0.01011 0.00152
C17 1 0.260742 0.315195 0.789772 11.00000 0.02117 0.01491 =
0.01974 -0.00073 0.01368 0.00089
C10 1 0.157377 0.600513 0.879096 11.00000 0.02641 0.01017 =
0.01540 0.00365 0.01118 0.00115
C3 1 0.397573 0.564388 0.594461 11.00000 0.02721 0.01020 =
0.02035 -0.00324 0.01354 0.00069
C19 1 0.207918 0.178348 0.706189 11.00000 0.02825 0.01387 =
0.01805 -0.00390 0.01073 -0.00227
AFIX 23
H19A 2 0.245400 0.181498 0.641595 11.00000 -1.20000
H19B 2 0.126725 0.189388 0.655417 11.00000 -1.20000
AFIX 0
C20 1 0.224761 0.095107 0.771919 11.00000 0.02929 0.01397 =
0.02150 0.00000 0.00948 -0.00147
AFIX 23
H20A 2 0.184705 0.092105 0.833773 11.00000 -1.20000
H20B 2 0.305858 0.086119 0.827041 11.00000 -1.20000
AFIX 0
C12 1 0.166316 0.702007 1.047395 11.00000 0.02143 0.01582 =
0.01945 -0.00577 0.00683 -0.00216
AFIX 23
H12A 2 0.206138 0.740874 1.012677 11.00000 -1.20000
H12B 2 0.222994 0.672762 1.124923 11.00000 -1.20000
AFIX 0
C5 1 0.410909 0.646544 0.409537 11.00000 0.02632 0.01733 =
0.01781 0.00352 0.01141 0.00179
AFIX 23
H5A 2 0.351207 0.681805 0.414133 11.00000 -1.20000
H5B 2 0.377445 0.611221 0.329026 11.00000 -1.20000
AFIX 0
C6 1 0.506177 0.696030 0.399114 11.00000 0.02696 0.01762 =
0.01964 0.00218 0.01213 -0.00218
AFIX 23
H6A 2 0.568916 0.660164 0.405946 11.00000 -1.20000
H6B 2 0.534533 0.733823 0.476732 11.00000 -1.20000
AFIX 0
C13 1 0.084241 0.745675 1.094728 11.00000 0.02441 0.02024 =
0.02541 -0.00835 0.00961 0.00079
AFIX 23
H13A 2 0.025050 0.770986 1.014330 11.00000 -1.20000
H13B 2 0.125515 0.788794 1.158334 11.00000 -1.20000
AFIX 0
C21 1 0.179654 0.029349 0.661222 11.00000 0.03286 0.01438 =
0.02705 -0.00222 0.01686 -0.00228
AFIX 137
H21A 2 0.100535 0.040017 0.603269 11.00000 -1.50000
H21B 2 0.186075 -0.022731 0.705369 11.00000 -1.50000
H21C 2 0.223838 0.029195 0.605053 11.00000 -1.50000
AFIX 0
C7 1 0.467748 0.743511 0.263028 11.00000 0.02686 0.02079 =
0.02166 0.00244 0.01162 -0.00431
AFIX 137
H7A 2 0.446177 0.706170 0.186179 11.00000 -1.50000
H7B 2 0.529704 0.777227 0.263553 11.00000 -1.50000
H7C 2 0.403131 0.777077 0.253546 11.00000 -1.50000
AFIX 0
C14 1 0.026731 0.691986 1.166710 11.00000 0.03199 0.03705 =
0.02385 -0.00890 0.01452 -0.00127
AFIX 137
H14A 2 -0.016441 0.649981 1.103835 11.00000 -1.50000
H14B 2 -0.023966 0.724410 1.193675 11.00000 -1.50000
H14C 2 0.084310 0.667686 1.248046 11.00000 -1.50000
AFIX 0
HKLF 4
REM s4712r_a.res in P2(1)/c
REM R1 = 0.0315 for 3457 Fo > 4sig(Fo) and 0.0382 for all 4029 data
REM 202 parameters refined using 0 restraints
END
WGHT 0.0383 0.0000
REM Highest difference peak 1.333, deepest hole -1.223, 1-sigma level 0.111
Q1 1 0.1971 0.4871 0.7169 11.00000 0.05 1.33
Q2 1 0.3463 0.4873 0.7786 11.00000 0.05 1.10
Q3 1 0.2607 0.4963 0.6610 11.00000 0.05 0.85
Q4 1 0.2776 0.4892 0.8369 11.00000 0.05 0.82
Q5 1 0.1155 0.4961 0.6855 11.00000 0.05 0.71
Q6 1 0.2292 0.6137 0.8925 11.00000 0.05 0.67
Q7 1 0.3280 0.5715 0.5600 11.00000 0.05 0.63
Q8 1 0.3371 0.4135 0.8199 11.00000 0.05 0.57
Q9 1 0.1740 0.5204 0.7787 11.00000 0.05 0.56
Q10 1 0.5465 0.5167 0.7725 11.00000 0.05 0.52
Q11 1 0.2195 0.3383 0.7114 11.00000 0.05 0.52
;
_shelx_res_checksum 46955
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.993
_oxdiff_exptl_absorpt_empirical_full_min 0.599
#######################################################################
#
# 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_s4602ma
_database_code_depnum_ccdc_archive 'CCDC 1812200'
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_audit_creation_date 2017-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number 2014/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C21 H39 In O6 S6'
_chemical_formula_sum 'C21 H39 In O6 S6'
_chemical_formula_weight 694.70
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 '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 12.5836(3)
_cell_length_b 22.3627(6)
_cell_length_c 22.8132(6)
_cell_angle_alpha 90
_cell_angle_beta 101.127(2)
_cell_angle_gamma 90
_cell_volume 6299.0(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 2861
_cell_measurement_temperature 180(2)
_cell_measurement_theta_max 71.62
_cell_measurement_theta_min 2.79
_shelx_estimated_absorpt_T_max 0.502
_shelx_estimated_absorpt_T_min 0.181
_exptl_absorpt_coefficient_mu 9.977
_exptl_absorpt_correction_T_max 0.502
_exptl_absorpt_correction_T_min 0.386692
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_absorpt_special_details ?
_exptl_crystal_colour white
_exptl_crystal_colour_primary white
_exptl_crystal_density_diffrn 1.465
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2864
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0932
_diffrn_reflns_av_unetI/netI 0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 41853
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 72.132
_diffrn_reflns_theta_min 2.793
_diffrn_ambient_temperature 180.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8323
_reflns_number_total 12232
_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 'Bruker SAINT'
_computing_data_collection 'Bruker APEX2'
_computing_data_reduction 'Bruker SAINT'
_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-97 (Sheldrick, 2008)'
_refine_diff_density_max 1.358
_refine_diff_density_min -1.006
_refine_diff_density_rms 0.104
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 636
_refine_ls_number_reflns 12232
_refine_ls_number_restraints 122
_refine_ls_R_factor_all 0.0902
_refine_ls_R_factor_gt 0.0553
_refine_ls_restrained_S_all 1.031
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+7.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1308
_refine_ls_wR_factor_ref 0.1509
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
O8-C28 \\sim O8-C28S
with sigma of 0.02
3. Rigid bond restraints
O8, C28, O8, C28S
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(C28S) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C28) = Uanis(C28S)
5. Rigid body (RIGU) restrains
C34, C32, C33, O10, C35, C31, C30, O9
with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
C28S, C28, O8, C25, C26, C27, C24, C23, O7
with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
Sof(C28S)=Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(1)
Sof(C28)=Sof(H28D)=Sof(H28E)=Sof(H28F)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B), C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B),
C17(H17A,H17B), C23(H23A,H23B), C24(H24A,H24B), C30(H30A,H30B), C31(H31A,H31B),
C37(H37A,H37B), C38(H38A,H38B)
7.b Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C20(H20A,H20B,
H20C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
C28S(H28A,H28B,H28C), C28(H28D,H28E,H28F), C33(H33A,H33B,H33C), C34(H34A,H34B,
H34C), C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
H42B,H42C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6693(5) 0.7267(3) 0.1801(3) 0.0438(14) Uani 1 1 d . . . . .
C2 C 0.7509(7) 0.7668(3) 0.1019(4) 0.0613(19) Uani 1 1 d . . . . .
H2A H 0.7928 0.8018 0.1201 0.074 Uiso 1 1 calc R . . . .
H2B H 0.6776 0.7804 0.0828 0.074 Uiso 1 1 calc R . . . .
C3 C 0.8064(7) 0.7383(3) 0.0564(3) 0.0588(18) Uani 1 1 d . . . . .
H3A H 0.7579 0.7074 0.0345 0.071 Uiso 1 1 calc R . . . .
H3B H 0.8727 0.7179 0.0774 0.071 Uiso 1 1 calc R . . . .
C4 C 0.8374(6) 0.7819(4) 0.0116(4) 0.0616(19) Uani 1 1 d . . . . .
C5 C 0.8828(9) 0.7460(5) -0.0357(4) 0.090(3) Uani 1 1 d . . . . .
H5A H 0.9063 0.7736 -0.0640 0.135 Uiso 1 1 calc GR . . . .
H5B H 0.8263 0.7196 -0.0572 0.135 Uiso 1 1 calc GR . . . .
H5C H 0.9446 0.7220 -0.0160 0.135 Uiso 1 1 calc GR . . . .
C6 C 0.7459(8) 0.8213(5) -0.0158(4) 0.087(3) Uani 1 1 d . . . . .
H6A H 0.7288 0.8489 0.0145 0.131 Uiso 1 1 calc GR . . . .
H6B H 0.6822 0.7968 -0.0315 0.131 Uiso 1 1 calc GR . . . .
H6C H 0.7665 0.8443 -0.0485 0.131 Uiso 1 1 calc GR . . . .
C7 C 0.9671(11) 0.8606(6) 0.0174(6) 0.145(6) Uani 1 1 d . . . . .
H7A H 1.0007 0.8423 -0.0135 0.217 Uiso 1 1 calc GR . . . .
H7B H 1.0224 0.8816 0.0462 0.217 Uiso 1 1 calc GR . . . .
H7C H 0.9114 0.8890 -0.0011 0.217 Uiso 1 1 calc GR . . . .
C8 C 0.4999(5) 0.8387(2) 0.3280(3) 0.0407(13) Uani 1 1 d . . . . .
C9 C 0.5811(7) 0.9081(3) 0.4013(3) 0.061(2) Uani 1 1 d . . . . .
H9A H 0.6474 0.9112 0.3842 0.074 Uiso 1 1 calc R . . . .
H9B H 0.5943 0.8786 0.4343 0.074 Uiso 1 1 calc R . . . .
C10 C 0.5541(7) 0.9679(3) 0.4245(3) 0.0609(19) Uani 1 1 d . . . . .
H10A H 0.5917 0.9712 0.4667 0.073 Uiso 1 1 calc R . . . .
H10B H 0.4753 0.9688 0.4241 0.073 Uiso 1 1 calc R . . . .
C11 C 0.5823(7) 1.0228(3) 0.3914(4) 0.062(2) Uani 1 1 d . . . . .
C12 C 0.5459(8) 1.0794(4) 0.4184(4) 0.082(3) Uani 1 1 d . . . . .
H12A H 0.5898 1.0854 0.4584 0.123 Uiso 1 1 calc GR . . . .
H12B H 0.4695 1.0756 0.4213 0.123 Uiso 1 1 calc GR . . . .
H12C H 0.5549 1.1136 0.3930 0.123 Uiso 1 1 calc GR . . . .
C13 C 0.5322(8) 1.0191(4) 0.3244(4) 0.078(3) Uani 1 1 d . . . . .
H13A H 0.5530 1.0545 0.3039 0.117 Uiso 1 1 calc GR . . . .
H13B H 0.4531 1.0174 0.3192 0.117 Uiso 1 1 calc GR . . . .
H13C H 0.5584 0.9831 0.3073 0.117 Uiso 1 1 calc GR . . . .
C14 C 0.7499(10) 1.0647(4) 0.3773(5) 0.100(4) Uani 1 1 d . . . . .
H14A H 0.7400 1.0603 0.3338 0.150 Uiso 1 1 calc GR . . . .
H14B H 0.8273 1.0631 0.3949 0.150 Uiso 1 1 calc GR . . . .
H14C H 0.7202 1.1033 0.3868 0.150 Uiso 1 1 calc GR . . . .
C15 C 0.3702(5) 0.6260(3) 0.2731(3) 0.0433(14) Uani 1 1 d . . . . .
C16 C 0.2974(6) 0.5520(3) 0.3309(3) 0.0539(17) Uani 1 1 d . . . . .
H16A H 0.2850 0.5817 0.3610 0.065 Uiso 1 1 calc R . . . .
H16B H 0.3664 0.5310 0.3462 0.065 Uiso 1 1 calc R . . . .
C17 C 0.2046(6) 0.5080(3) 0.3182(3) 0.0561(17) Uani 1 1 d . . . . .
H17A H 0.2238 0.4756 0.2925 0.067 Uiso 1 1 calc R . . . .
H17B H 0.1399 0.5287 0.2956 0.067 Uiso 1 1 calc R . . . .
C18 C 0.1762(7) 0.4805(3) 0.3737(3) 0.0537(17) Uani 1 1 d . . . . .
C19 C 0.2728(7) 0.4507(3) 0.4126(4) 0.072(2) Uani 1 1 d . . . . .
H19A H 0.3271 0.4811 0.4282 0.108 Uiso 1 1 calc GR . . . .
H19B H 0.3044 0.4216 0.3888 0.108 Uiso 1 1 calc GR . . . .
H19C H 0.2495 0.4303 0.4459 0.108 Uiso 1 1 calc GR . . . .
C20 C 0.0839(7) 0.4361(4) 0.3550(4) 0.072(2) Uani 1 1 d . . . . .
H20A H 0.0685 0.4157 0.3905 0.108 Uiso 1 1 calc GR . . . .
H20B H 0.1048 0.4065 0.3276 0.108 Uiso 1 1 calc GR . . . .
H20C H 0.0190 0.4575 0.3349 0.108 Uiso 1 1 calc GR . . . .
C21 C 0.1078(9) 0.5226(4) 0.4574(4) 0.088(3) Uani 1 1 d . . . . .
H21A H 0.0616 0.4870 0.4546 0.132 Uiso 1 1 calc GR . . . .
H21B H 0.0673 0.5575 0.4671 0.132 Uiso 1 1 calc GR . . . .
H21C H 0.1720 0.5167 0.4888 0.132 Uiso 1 1 calc GR . . . .
C22 C 0.8323(6) 0.6435(3) 0.4527(3) 0.0519(16) Uani 1 1 d . . . . .
C23 C 0.7504(8) 0.5696(4) 0.3837(5) 0.079(2) Uani 1 1 d . U . . .
H23A H 0.7199 0.6001 0.3536 0.095 Uiso 1 1 calc R . . . .
H23B H 0.6934 0.5576 0.4058 0.095 Uiso 1 1 calc R . . . .
C24 C 0.7893(10) 0.5159(4) 0.3535(5) 0.098(3) Uani 1 1 d . U . . .
H24A H 0.8421 0.5297 0.3294 0.118 Uiso 1 1 calc R . . . .
H24B H 0.8280 0.4888 0.3848 0.118 Uiso 1 1 calc R . . . .
C25 C 0.7032(11) 0.4813(4) 0.3142(6) 0.098(2) Uani 1 1 d . U . . .
C26 C 0.7534(11) 0.4317(5) 0.2823(6) 0.118(3) Uani 1 1 d . U . . .
H26A H 0.7644 0.3960 0.3078 0.177 Uiso 1 1 calc GR . . . .
H26B H 0.8232 0.4452 0.2742 0.177 Uiso 1 1 calc GR . . . .
H26C H 0.7047 0.4220 0.2446 0.177 Uiso 1 1 calc GR . . . .
C27 C 0.6319(11) 0.5199(4) 0.2700(5) 0.106(3) Uani 1 1 d . U . . .
H27A H 0.5910 0.4949 0.2381 0.159 Uiso 1 1 calc GR . . . .
H27B H 0.6763 0.5485 0.2528 0.159 Uiso 1 1 calc GR . . . .
H27C H 0.5813 0.5416 0.2899 0.159 Uiso 1 1 calc GR . . . .
C28S C 0.567(3) 0.4640(14) 0.3851(16) 0.137(4) Uani 0.334(15) 1 d D U P A 2
H28A H 0.5936 0.4504 0.4261 0.206 Uiso 0.334(15) 1 calc GR . P A 2
H28B H 0.5002 0.4422 0.3682 0.206 Uiso 0.334(15) 1 calc GR . P A 2
H28C H 0.5509 0.5069 0.3854 0.206 Uiso 0.334(15) 1 calc GR . P A 2
C28 C 0.5617(18) 0.4144(9) 0.3296(10) 0.137(4) Uani 0.666(15) 1 d D U P A 1
H28D H 0.4971 0.4364 0.3102 0.206 Uiso 0.666(15) 1 calc GR . P A 1
H28E H 0.5443 0.3902 0.3623 0.206 Uiso 0.666(15) 1 calc GR . P A 1
H28F H 0.5861 0.3882 0.3004 0.206 Uiso 0.666(15) 1 calc GR . P A 1
C29 C 0.6724(5) 0.7754(3) 0.5987(3) 0.0471(14) Uani 1 1 d . . . . .
C30 C 0.5976(7) 0.7586(4) 0.6858(4) 0.067(2) Uani 1 1 d . U . . .
H30A H 0.6712 0.7472 0.7068 0.080 Uiso 1 1 calc R . . . .
H30B H 0.5530 0.7220 0.6775 0.080 Uiso 1 1 calc R . . . .
C31 C 0.5464(7) 0.8025(4) 0.7229(4) 0.0723(19) Uani 1 1 d . U . . .
H31A H 0.5901 0.8396 0.7275 0.087 Uiso 1 1 calc R . . . .
H31B H 0.4733 0.8129 0.7004 0.087 Uiso 1 1 calc R . . . .
C32 C 0.5359(10) 0.7814(5) 0.7828(5) 0.090(2) Uani 1 1 d . U . . .
C33 C 0.4813(9) 0.8275(5) 0.8159(5) 0.103(3) Uani 1 1 d . U . . .
H33A H 0.4113 0.8387 0.7914 0.155 Uiso 1 1 calc GR . . . .
H33B H 0.5274 0.8630 0.8238 0.155 Uiso 1 1 calc GR . . . .
H33C H 0.4699 0.8105 0.8537 0.155 Uiso 1 1 calc GR . . . .
C34 C 0.6430(11) 0.7627(6) 0.8197(5) 0.118(3) Uani 1 1 d . U . . .
H34A H 0.6316 0.7460 0.8577 0.176 Uiso 1 1 calc GR . . . .
H34B H 0.6909 0.7976 0.8275 0.176 Uiso 1 1 calc GR . . . .
H34C H 0.6762 0.7324 0.7979 0.176 Uiso 1 1 calc GR . . . .
C35 C 0.4117(15) 0.7059(7) 0.7990(8) 0.166(7) Uani 1 1 d . U . . .
H35A H 0.4616 0.6856 0.8312 0.249 Uiso 1 1 calc GR . . . .
H35B H 0.3643 0.6762 0.7754 0.249 Uiso 1 1 calc GR . . . .
H35C H 0.3677 0.7347 0.8162 0.249 Uiso 1 1 calc GR . . . .
C36 C 0.9541(6) 0.8608(3) 0.4910(3) 0.0582(18) Uani 1 1 d . . . . .
C37 C 0.9793(8) 0.9440(4) 0.4274(4) 0.079(3) Uani 1 1 d . . . . .
H37A H 0.9705 0.9161 0.3931 0.095 Uiso 1 1 calc R . . . .
H37B H 0.9097 0.9651 0.4261 0.095 Uiso 1 1 calc R . . . .
C38 C 1.0654(9) 0.9879(4) 0.4231(5) 0.089(3) Uani 1 1 d . . . . .
H38A H 1.0938 1.0041 0.4635 0.107 Uiso 1 1 calc R . . . .
H38B H 1.0330 1.0215 0.3976 0.107 Uiso 1 1 calc R . . . .
C39 C 1.1606(9) 0.9629(5) 0.3976(5) 0.089(3) Uani 1 1 d . . . . .
C40 C 1.2379(11) 1.0156(6) 0.3914(6) 0.145(6) Uani 1 1 d . . . . .
H40A H 1.3091 0.9999 0.3879 0.218 Uiso 1 1 calc GR . . . .
H40B H 1.2453 1.0414 0.4266 0.218 Uiso 1 1 calc GR . . . .
H40C H 1.2080 1.0388 0.3555 0.218 Uiso 1 1 calc GR . . . .
C41 C 1.2145(10) 0.9110(6) 0.4343(6) 0.122(5) Uani 1 1 d . . . . .
H41A H 1.1677 0.8757 0.4269 0.183 Uiso 1 1 calc GR . . . .
H41B H 1.2266 0.9213 0.4768 0.183 Uiso 1 1 calc GR . . . .
H41C H 1.2841 0.9023 0.4228 0.183 Uiso 1 1 calc GR . . . .
C42 C 1.1829(12) 0.9219(8) 0.3092(7) 0.167(7) Uani 1 1 d . . . . .
H42A H 1.1760 0.9440 0.2715 0.251 Uiso 1 1 calc GR . . . .
H42B H 1.1685 0.8794 0.3006 0.251 Uiso 1 1 calc GR . . . .
H42C H 1.2564 0.9267 0.3324 0.251 Uiso 1 1 calc GR . . . .
In1 In 0.50961(4) 0.72787(2) 0.25857(2) 0.04029(12) Uani 1 1 d . . . . .
In2 In 0.82814(4) 0.75687(2) 0.51865(2) 0.04553(12) Uani 1 1 d . . . . .
O1 O 0.7439(4) 0.7225(2) 0.1469(2) 0.0531(11) Uani 1 1 d . . . . .
O2 O 0.9198(6) 0.8163(4) 0.0468(3) 0.099(2) Uani 1 1 d . . . . .
O3 O 0.4904(4) 0.88921(18) 0.3557(2) 0.0496(11) Uani 1 1 d . . . . .
O4 O 0.6972(5) 1.0195(2) 0.4001(3) 0.0789(18) Uani 1 1 d . . . . .
O5 O 0.3006(4) 0.5813(2) 0.2738(2) 0.0529(12) Uani 1 1 d . . . . .
O6 O 0.1398(5) 0.5321(2) 0.4025(3) 0.0681(15) Uani 1 1 d . . . . .
O7 O 0.8433(5) 0.5936(2) 0.4245(3) 0.0663(14) Uani 1 1 d . U . . .
O8 O 0.6420(9) 0.4538(4) 0.3518(5) 0.134(3) Uani 1 1 d D U . . .
O9 O 0.6021(4) 0.7902(2) 0.6311(2) 0.0573(12) Uani 1 1 d . U . . .
O10 O 0.4644(10) 0.7326(5) 0.7662(5) 0.144(3) Uani 1 1 d . U . . .
O11 O 1.0093(5) 0.9098(2) 0.4849(3) 0.0706(15) Uani 1 1 d . . . . .
O12 O 1.1101(7) 0.9435(4) 0.3410(4) 0.106(2) Uani 1 1 d . . . . .
S1 S 0.67485(15) 0.67332(7) 0.23318(8) 0.0492(4) Uani 1 1 d . . . . .
S2 S 0.57480(14) 0.78197(6) 0.17038(7) 0.0459(3) Uani 1 1 d . . . . .
S3 S 0.38961(13) 0.81752(7) 0.27594(7) 0.0477(4) Uani 1 1 d . . . . .
S4 S 0.61396(14) 0.79652(7) 0.34212(7) 0.0490(4) Uani 1 1 d . . . . .
S5 S 0.45934(14) 0.64856(7) 0.33411(6) 0.0455(4) Uani 1 1 d . . . . .
S6 S 0.36161(15) 0.65785(7) 0.20481(7) 0.0486(4) Uani 1 1 d . . . . .
S7 S 0.71454(14) 0.68205(7) 0.44195(8) 0.0526(4) Uani 1 1 d . . . . .
S8 S 0.94476(15) 0.66717(9) 0.50132(9) 0.0578(4) Uani 1 1 d . . . . .
S9 S 0.76182(14) 0.71855(7) 0.61406(7) 0.0461(3) Uani 1 1 d . . . . .
S10 S 0.66887(16) 0.82019(8) 0.53769(9) 0.0587(4) Uani 1 1 d . . . . .
S11 S 0.98362(16) 0.82917(9) 0.56065(8) 0.0582(4) Uani 1 1 d . . . . .
S12 S 0.85814(17) 0.83281(9) 0.43621(8) 0.0625(5) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.044(4) 0.043(3) 0.047(3) -0.002(3) 0.014(3) -0.008(3)
C2 0.055(4) 0.061(4) 0.077(5) 0.016(4) 0.034(4) 0.007(4)
C3 0.056(4) 0.064(4) 0.060(4) 0.005(3) 0.022(4) 0.006(4)
C4 0.046(4) 0.076(5) 0.065(4) 0.019(4) 0.018(4) 0.008(4)
C5 0.100(8) 0.114(8) 0.067(5) 0.021(5) 0.043(5) 0.037(6)
C6 0.076(6) 0.121(8) 0.072(6) 0.035(6) 0.032(5) 0.031(6)
C7 0.121(11) 0.204(16) 0.117(11) 0.009(10) 0.042(9) -0.080(11)
C8 0.040(3) 0.035(3) 0.045(3) 0.002(2) 0.002(3) 0.001(2)
C9 0.075(5) 0.045(3) 0.054(4) -0.003(3) -0.013(4) 0.001(3)
C10 0.073(5) 0.058(4) 0.049(4) -0.012(3) 0.006(4) -0.003(4)
C11 0.059(5) 0.043(3) 0.078(5) -0.003(3) -0.008(4) -0.005(3)
C12 0.092(7) 0.054(4) 0.098(7) -0.015(4) 0.015(6) 0.006(5)
C13 0.088(7) 0.068(5) 0.070(5) 0.013(4) -0.003(5) -0.007(5)
C14 0.113(9) 0.074(6) 0.125(9) 0.020(6) 0.055(8) 0.002(6)
C15 0.050(4) 0.043(3) 0.038(3) 0.001(2) 0.010(3) -0.010(3)
C16 0.065(5) 0.052(4) 0.046(4) 0.006(3) 0.015(3) -0.015(3)
C17 0.061(5) 0.049(4) 0.061(4) 0.006(3) 0.019(4) -0.010(3)
C18 0.069(5) 0.034(3) 0.063(4) 0.001(3) 0.026(4) -0.003(3)
C19 0.079(6) 0.057(4) 0.080(6) 0.026(4) 0.015(5) 0.003(4)
C20 0.072(6) 0.060(4) 0.088(6) 0.000(4) 0.026(5) -0.022(4)
C21 0.107(8) 0.083(6) 0.092(7) -0.006(5) 0.063(7) -0.005(6)
C22 0.052(4) 0.051(3) 0.053(4) 0.009(3) 0.012(3) 0.004(3)
C23 0.084(5) 0.057(4) 0.094(5) -0.014(4) 0.009(4) 0.010(3)
C24 0.121(5) 0.059(4) 0.118(5) -0.021(4) 0.031(4) 0.013(3)
C25 0.127(5) 0.050(3) 0.116(5) -0.015(3) 0.023(4) 0.007(3)
C26 0.134(7) 0.069(4) 0.151(7) -0.037(5) 0.023(6) 0.004(5)
C27 0.146(7) 0.075(5) 0.110(5) -0.006(4) 0.053(5) 0.031(5)
C28S 0.140(4) 0.133(5) 0.138(5) -0.002(3) 0.026(3) -0.010(3)
C28 0.140(4) 0.133(5) 0.138(5) -0.002(3) 0.026(3) -0.010(3)
C29 0.041(4) 0.047(3) 0.054(4) -0.002(3) 0.013(3) 0.001(3)
C30 0.070(5) 0.068(4) 0.069(3) 0.006(3) 0.028(3) 0.019(4)
C31 0.061(4) 0.087(4) 0.072(3) -0.007(3) 0.020(3) 0.022(4)
C32 0.099(5) 0.099(5) 0.080(4) 0.004(3) 0.041(3) 0.025(4)
C33 0.085(6) 0.136(6) 0.092(6) -0.027(5) 0.025(5) 0.022(5)
C34 0.115(5) 0.164(9) 0.084(5) 0.021(5) 0.047(4) 0.046(5)
C35 0.174(13) 0.166(11) 0.179(12) 0.015(9) 0.085(11) -0.020(10)
C36 0.055(4) 0.060(4) 0.061(4) 0.006(3) 0.013(4) -0.013(4)
C37 0.091(7) 0.073(5) 0.074(6) 0.027(4) 0.021(5) 0.002(5)
C38 0.107(8) 0.062(5) 0.100(7) 0.004(5) 0.024(6) -0.010(5)
C39 0.067(6) 0.108(8) 0.095(7) 0.026(6) 0.019(6) -0.010(6)
C40 0.114(11) 0.156(12) 0.147(13) 0.055(10) -0.022(9) -0.063(10)
C41 0.081(8) 0.149(11) 0.137(11) 0.063(9) 0.024(8) 0.016(8)
C42 0.137(13) 0.230(19) 0.165(15) -0.008(14) 0.103(13) 0.036(13)
In1 0.0431(2) 0.03700(19) 0.0419(2) -0.00207(16) 0.01103(17) -0.00652(17)
In2 0.0426(2) 0.0470(2) 0.0464(2) 0.00365(17) 0.00738(18) -0.00134(19)
O1 0.052(3) 0.056(3) 0.057(3) 0.008(2) 0.023(2) 0.007(2)
O2 0.094(5) 0.128(6) 0.084(4) 0.008(4) 0.042(4) -0.041(5)
O3 0.054(3) 0.038(2) 0.052(2) -0.0077(18) -0.004(2) 0.003(2)
O4 0.063(4) 0.050(3) 0.120(5) 0.006(3) 0.009(4) -0.001(3)
O5 0.063(3) 0.051(2) 0.045(2) 0.0055(19) 0.012(2) -0.022(2)
O6 0.087(4) 0.051(3) 0.076(4) -0.004(2) 0.039(3) -0.002(3)
O7 0.071(3) 0.051(3) 0.078(3) -0.006(2) 0.017(3) 0.012(2)
O8 0.147(5) 0.121(4) 0.133(5) -0.004(4) 0.026(4) -0.017(4)
O9 0.046(3) 0.062(3) 0.066(3) 0.004(2) 0.014(2) 0.017(2)
O10 0.172(7) 0.145(5) 0.135(6) -0.026(4) 0.080(5) -0.027(5)
O11 0.074(4) 0.072(3) 0.065(3) 0.009(3) 0.012(3) -0.026(3)
O12 0.096(6) 0.124(6) 0.097(5) 0.004(5) 0.022(5) 0.013(5)
S1 0.0525(10) 0.0450(8) 0.0523(8) 0.0087(7) 0.0154(7) 0.0054(7)
S2 0.0504(9) 0.0390(7) 0.0508(8) 0.0069(6) 0.0160(7) 0.0010(7)
S3 0.0388(8) 0.0480(8) 0.0533(8) -0.0081(7) 0.0012(7) -0.0002(7)
S4 0.0454(9) 0.0400(7) 0.0552(9) -0.0065(6) -0.0058(7) 0.0014(7)
S5 0.0520(9) 0.0494(8) 0.0344(7) 0.0015(6) 0.0067(7) -0.0110(7)
S6 0.0584(10) 0.0488(8) 0.0360(7) 0.0047(6) 0.0025(7) -0.0145(7)
S7 0.0472(9) 0.0478(8) 0.0582(9) -0.0029(7) -0.0012(7) 0.0027(7)
S8 0.0442(10) 0.0634(10) 0.0658(11) -0.0002(8) 0.0104(8) 0.0065(8)
S9 0.0488(9) 0.0416(7) 0.0489(8) 0.0040(6) 0.0120(7) 0.0054(7)
S10 0.0543(11) 0.0583(9) 0.0625(10) 0.0149(8) 0.0087(8) 0.0144(8)
S11 0.0556(11) 0.0711(11) 0.0443(8) 0.0068(8) 0.0004(8) -0.0155(9)
S12 0.0663(12) 0.0735(11) 0.0431(8) 0.0110(8) -0.0004(8) -0.0207(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.319(8) . ?
C1 S1 1.692(6) . ?
C1 S2 1.699(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.500(10) . ?
C2 O1 1.442(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(10) . ?
C4 C5 1.540(11) . ?
C4 C6 1.489(11) . ?
C4 O2 1.412(11) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 O2 1.392(12) . ?
C8 O3 1.311(7) . ?
C8 S3 1.711(6) . ?
C8 S4 1.695(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.501(9) . ?
C9 O3 1.452(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.518(10) . ?
C11 C12 1.517(11) . ?
C11 C13 1.539(11) . ?
C11 O4 1.423(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 O4 1.367(10) . ?
C15 O5 1.330(7) . ?
C15 S5 1.687(6) . ?
C15 S6 1.698(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.512(10) . ?
C16 O5 1.467(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.511(9) . ?
C18 C19 1.515(11) . ?
C18 C20 1.525(10) . ?
C18 O6 1.445(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 O6 1.404(9) . ?
C22 O7 1.308(8) . ?
C22 S7 1.692(7) . ?
C22 S8 1.705(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.512(11) . ?
C23 O7 1.450(11) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.484(15) . ?
C25 C26 1.528(13) . ?
C25 C27 1.490(15) . ?
C25 O8 1.402(14) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28S H28A 0.9800 . ?
C28S H28B 0.9800 . ?
C28S H28C 0.9800 . ?
C28S O8 1.35(2) . ?
C28 H28D 0.9800 . ?
C28 H28E 0.9800 . ?
C28 H28F 0.9800 . ?
C28 O8 1.363(19) . ?
C29 O9 1.301(8) . ?
C29 S9 1.690(7) . ?
C29 S10 1.707(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.519(10) . ?
C30 O9 1.444(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.476(12) . ?
C32 C33 1.517(12) . ?
C32 C34 1.504(16) . ?
C32 O10 1.420(14) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35 O10 1.245(14) . ?
C36 O11 1.318(8) . ?
C36 S11 1.714(8) . ?
C36 S12 1.682(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.478(12) . ?
C37 O11 1.505(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.533(14) . ?
C39 C40 1.552(14) . ?
C39 C41 1.512(14) . ?
C39 O12 1.393(13) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 O12 1.363(12) . ?
In1 S1 2.5714(17) . ?
In1 S2 2.6119(15) . ?
In1 S3 2.5860(16) . ?
In1 S4 2.5978(16) . ?
In1 S5 2.6336(15) . ?
In1 S6 2.5579(16) . ?
In2 S7 2.6342(17) . ?
In2 S8 2.5606(19) . ?
In2 S9 2.6211(16) . ?
In2 S10 2.5586(19) . ?
In2 S11 2.5762(19) . ?
In2 S12 2.6150(18) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 S1 115.2(5) . . ?
O1 C1 S2 122.3(5) . . ?
S1 C1 S2 122.5(4) . . ?
H2A C2 H2B 108.5 . . ?
C3 C2 H2A 110.2 . . ?
C3 C2 H2B 110.2 . . ?
O1 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
O1 C2 C3 107.6(6) . . ?
C2 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
C2 C3 C4 114.0(6) . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C3 C4 C5 108.4(7) . . ?
C6 C4 C3 112.7(7) . . ?
C6 C4 C5 112.0(8) . . ?
O2 C4 C3 102.9(7) . . ?
O2 C4 C5 110.6(7) . . ?
O2 C4 C6 109.8(8) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
O3 C8 S3 115.8(5) . . ?
O3 C8 S4 122.8(5) . . ?
S4 C8 S3 121.4(3) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
O3 C9 H9A 110.1 . . ?
O3 C9 H9B 110.1 . . ?
O3 C9 C10 108.2(6) . . ?
C9 C10 H10A 108.0 . . ?
C9 C10 H10B 108.0 . . ?
C9 C10 C11 117.0(7) . . ?
H10A C10 H10B 107.3 . . ?
C11 C10 H10A 108.0 . . ?
C11 C10 H10B 108.0 . . ?
C10 C11 C13 111.1(6) . . ?
C12 C11 C10 110.7(8) . . ?
C12 C11 C13 110.5(7) . . ?
O4 C11 C10 102.5(6) . . ?
O4 C11 C12 111.4(7) . . ?
O4 C11 C13 110.3(8) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
O5 C15 S5 123.4(5) . . ?
O5 C15 S6 113.5(5) . . ?
S5 C15 S6 123.1(4) . . ?
H16A C16 H16B 108.7 . . ?
C17 C16 H16A 110.6 . . ?
C17 C16 H16B 110.6 . . ?
O5 C16 H16A 110.6 . . ?
O5 C16 H16B 110.6 . . ?
O5 C16 C17 105.8(6) . . ?
C16 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C16 C17 C18 113.7(6) . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
C17 C18 C19 112.1(7) . . ?
C17 C18 C20 108.7(7) . . ?
C19 C18 C20 111.1(6) . . ?
O6 C18 C17 101.8(5) . . ?
O6 C18 C19 111.9(7) . . ?
O6 C18 C20 110.9(6) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
O7 C22 S7 122.4(6) . . ?
O7 C22 S8 115.6(6) . . ?
S7 C22 S8 122.0(4) . . ?
H23A C23 H23B 108.5 . . ?
C24 C23 H23A 110.3 . . ?
C24 C23 H23B 110.3 . . ?
O7 C23 H23A 110.3 . . ?
O7 C23 H23B 110.3 . . ?
O7 C23 C24 107.1(8) . . ?
C23 C24 H24A 108.5 . . ?
C23 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C25 C24 C23 115.3(10) . . ?
C25 C24 H24A 108.5 . . ?
C25 C24 H24B 108.5 . . ?
C24 C25 C26 110.3(10) . . ?
C24 C25 C27 112.4(9) . . ?
C27 C25 C26 110.5(10) . . ?
O8 C25 C24 106.3(11) . . ?
O8 C25 C26 107.4(9) . . ?
O8 C25 C27 109.7(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
H28A C28S H28B 109.5 . . ?
H28A C28S H28C 109.5 . . ?
H28B C28S H28C 109.5 . . ?
O8 C28S H28A 109.5 . . ?
O8 C28S H28B 109.5 . . ?
O8 C28S H28C 109.5 . . ?
H28D C28 H28E 109.5 . . ?
H28D C28 H28F 109.5 . . ?
H28E C28 H28F 109.5 . . ?
O8 C28 H28D 109.5 . . ?
O8 C28 H28E 109.5 . . ?
O8 C28 H28F 109.5 . . ?
O9 C29 S9 124.8(5) . . ?
O9 C29 S10 113.6(5) . . ?
S9 C29 S10 121.5(4) . . ?
H30A C30 H30B 108.9 . . ?
C31 C30 H30A 110.8 . . ?
C31 C30 H30B 110.8 . . ?
O9 C30 H30A 110.8 . . ?
O9 C30 H30B 110.8 . . ?
O9 C30 C31 104.8(6) . . ?
C30 C31 H31A 108.4 . . ?
C30 C31 H31B 108.4 . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 C30 115.7(8) . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
C31 C32 C33 112.0(9) . . ?
C31 C32 C34 112.1(9) . . ?
C34 C32 C33 110.7(10) . . ?
O10 C32 C31 99.4(9) . . ?
O10 C32 C33 109.3(9) . . ?
O10 C32 C34 112.9(10) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O10 C35 H35A 109.5 . . ?
O10 C35 H35B 109.5 . . ?
O10 C35 H35C 109.5 . . ?
O11 C36 S11 114.5(6) . . ?
O11 C36 S12 123.3(6) . . ?
S12 C36 S11 122.1(4) . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 H37A 109.8 . . ?
C38 C37 H37B 109.8 . . ?
C38 C37 O11 109.4(8) . . ?
O11 C37 H37A 109.8 . . ?
O11 C37 H37B 109.8 . . ?
C37 C38 H38A 108.6 . . ?
C37 C38 H38B 108.6 . . ?
C37 C38 C39 114.8(8) . . ?
H38A C38 H38B 107.5 . . ?
C39 C38 H38A 108.6 . . ?
C39 C38 H38B 108.6 . . ?
C38 C39 C40 107.9(10) . . ?
C41 C39 C38 111.7(9) . . ?
C41 C39 C40 114.3(10) . . ?
O12 C39 C38 102.4(9) . . ?
O12 C39 C40 109.4(9) . . ?
O12 C39 C41 110.4(11) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O12 C42 H42A 109.5 . . ?
O12 C42 H42B 109.5 . . ?
O12 C42 H42C 109.5 . . ?
S1 In1 S2 70.03(5) . . ?
S1 In1 S3 157.49(6) . . ?
S1 In1 S4 97.44(6) . . ?
S1 In1 S5 97.74(5) . . ?
S2 In1 S5 165.20(5) . . ?
S3 In1 S2 92.20(5) . . ?
S3 In1 S4 69.93(5) . . ?
S3 In1 S5 101.58(6) . . ?
S4 In1 S2 95.85(6) . . ?
S4 In1 S5 93.97(5) . . ?
S6 In1 S1 98.46(6) . . ?
S6 In1 S2 102.83(5) . . ?
S6 In1 S3 98.94(6) . . ?
S6 In1 S4 158.71(6) . . ?
S6 In1 S5 69.93(5) . . ?
S8 In2 S7 69.74(6) . . ?
S8 In2 S9 98.97(6) . . ?
S8 In2 S11 97.60(7) . . ?
S8 In2 S12 103.36(7) . . ?
S9 In2 S7 97.19(6) . . ?
S10 In2 S7 97.00(6) . . ?
S10 In2 S8 161.94(7) . . ?
S10 In2 S9 69.79(5) . . ?
S10 In2 S11 98.80(7) . . ?
S10 In2 S12 89.38(7) . . ?
S11 In2 S7 157.15(6) . . ?
S11 In2 S9 103.71(6) . . ?
S11 In2 S12 69.83(6) . . ?
S12 In2 S7 94.01(6) . . ?
S12 In2 S9 157.36(6) . . ?
C1 O1 C2 120.6(5) . . ?
C7 O2 C4 116.7(8) . . ?
C8 O3 C9 117.6(5) . . ?
C14 O4 C11 117.6(7) . . ?
C15 O5 C16 118.5(5) . . ?
C21 O6 C18 117.1(6) . . ?
C22 O7 C23 118.9(6) . . ?
C28S O8 C25 143.5(15) . . ?
C28 O8 C25 120.8(14) . . ?
C29 O9 C30 120.7(5) . . ?
C35 O10 C32 126.3(13) . . ?
C36 O11 C37 117.8(7) . . ?
C42 O12 C39 111.8(11) . . ?
C1 S1 In1 84.4(2) . . ?
C1 S2 In1 83.0(2) . . ?
C8 S3 In1 84.3(2) . . ?
C8 S4 In1 84.3(2) . . ?
C15 S5 In1 82.4(2) . . ?
C15 S6 In1 84.6(2) . . ?
C22 S7 In2 83.1(3) . . ?
C22 S8 In2 85.2(2) . . ?
C29 S9 In2 83.5(2) . . ?
C29 S10 In2 85.2(2) . . ?
C36 S11 In2 84.3(3) . . ?
C36 S12 In2 83.7(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5C S10 0.98 3.00 3.953(11) 163.6 4_675
C9 H9B S10 0.99 2.70 3.666(7) 164.7 .
C13 H13C O3 0.98 2.59 3.061(9) 109.4 .
C27 H27B S1 0.98 2.83 3.597(11) 136.2 .
C28 H28E O2 0.98 2.62 3.54(2) 157.0 2_645
C34 H34C S3 0.98 3.04 3.879(11) 144.6 4_676
C35 H35A S12 0.98 2.97 3.437(15) 110.6 4_576
C40 H40C S6 0.98 3.05 3.929(13) 150.5 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C3 C4 C5 -174.4(8) . . . . ?
C2 C3 C4 C6 -49.8(11) . . . . ?
C2 C3 C4 O2 68.4(9) . . . . ?
C3 C2 O1 C1 -156.4(6) . . . . ?
C3 C4 O2 C7 178.9(9) . . . . ?
C5 C4 O2 C7 63.3(12) . . . . ?
C6 C4 O2 C7 -60.9(11) . . . . ?
C9 C10 C11 C12 177.6(7) . . . . ?
C9 C10 C11 C13 54.4(10) . . . . ?
C9 C10 C11 O4 -63.4(9) . . . . ?
C10 C9 O3 C8 177.3(6) . . . . ?
C10 C11 O4 C14 -177.5(8) . . . . ?
C12 C11 O4 C14 -59.0(11) . . . . ?
C13 C11 O4 C14 64.1(10) . . . . ?
C16 C17 C18 C19 -55.5(8) . . . . ?
C16 C17 C18 C20 -178.6(7) . . . . ?
C16 C17 C18 O6 64.3(8) . . . . ?
C17 C16 O5 C15 174.7(6) . . . . ?
C17 C18 O6 C21 -179.1(8) . . . . ?
C19 C18 O6 C21 -59.2(10) . . . . ?
C20 C18 O6 C21 65.5(10) . . . . ?
C23 C24 C25 C26 175.2(10) . . . . ?
C23 C24 C25 C27 51.5(15) . . . . ?
C23 C24 C25 O8 -68.7(12) . . . . ?
C24 C23 O7 C22 174.6(7) . . . . ?
C24 C25 O8 C28S 75(4) . . . . ?
C24 C25 O8 C28 -174.2(14) . . . . ?
C26 C25 O8 C28S -167(4) . . . . ?
C26 C25 O8 C28 -56.2(18) . . . . ?
C27 C25 O8 C28S -47(4) . . . . ?
C27 C25 O8 C28 63.9(17) . . . . ?
C30 C31 C32 C33 -178.5(9) . . . . ?
C30 C31 C32 C34 56.4(14) . . . . ?
C30 C31 C32 O10 -63.1(11) . . . . ?
C31 C30 O9 C29 156.0(7) . . . . ?
C31 C32 O10 C35 -164.8(15) . . . . ?
C33 C32 O10 C35 -47(2) . . . . ?
C34 C32 O10 C35 76.3(18) . . . . ?
C37 C38 C39 C40 175.3(10) . . . . ?
C37 C38 C39 C41 -58.2(14) . . . . ?
C37 C38 C39 O12 60.0(11) . . . . ?
C38 C37 O11 C36 -166.3(7) . . . . ?
C38 C39 O12 C42 177.1(10) . . . . ?
C40 C39 O12 C42 62.8(14) . . . . ?
C41 C39 O12 C42 -63.8(13) . . . . ?
O1 C1 S1 In1 -179.8(5) . . . . ?
O1 C1 S2 In1 179.8(6) . . . . ?
O1 C2 C3 C4 -170.0(7) . . . . ?
O3 C8 S3 In1 178.1(5) . . . . ?
O3 C8 S4 In1 -178.1(5) . . . . ?
O3 C9 C10 C11 -87.6(9) . . . . ?
O5 C15 S5 In1 -178.5(6) . . . . ?
O5 C15 S6 In1 178.4(5) . . . . ?
O5 C16 C17 C18 -170.3(6) . . . . ?
O7 C22 S7 In2 -178.2(6) . . . . ?
O7 C22 S8 In2 178.1(5) . . . . ?
O7 C23 C24 C25 174.2(9) . . . . ?
O9 C29 S9 In2 -177.3(6) . . . . ?
O9 C29 S10 In2 177.4(5) . . . . ?
O9 C30 C31 C32 -178.0(9) . . . . ?
O11 C36 S11 In2 174.8(6) . . . . ?
O11 C36 S12 In2 -174.6(7) . . . . ?
O11 C37 C38 C39 84.9(11) . . . . ?
S1 C1 O1 C2 -177.3(6) . . . . ?
S1 C1 S2 In1 -0.4(4) . . . . ?
S2 C1 O1 C2 2.5(9) . . . . ?
S2 C1 S1 In1 0.4(4) . . . . ?
S3 C8 O3 C9 178.5(5) . . . . ?
S3 C8 S4 In1 1.6(4) . . . . ?
S4 C8 O3 C9 -1.8(8) . . . . ?
S4 C8 S3 In1 -1.7(4) . . . . ?
S5 C15 O5 C16 3.1(9) . . . . ?
S5 C15 S6 In1 -2.3(4) . . . . ?
S6 C15 O5 C16 -177.5(5) . . . . ?
S6 C15 S5 In1 2.2(4) . . . . ?
S7 C22 O7 C23 -1.8(10) . . . . ?
S7 C22 S8 In2 -1.9(4) . . . . ?
S8 C22 O7 C23 178.2(6) . . . . ?
S8 C22 S7 In2 1.8(4) . . . . ?
S9 C29 O9 C30 1.8(10) . . . . ?
S9 C29 S10 In2 -1.6(4) . . . . ?
S10 C29 O9 C30 -177.2(6) . . . . ?
S10 C29 S9 In2 1.6(4) . . . . ?
S11 C36 O11 C37 -173.3(6) . . . . ?
S11 C36 S12 In2 2.5(5) . . . . ?
S12 C36 O11 C37 4.0(11) . . . . ?
S12 C36 S11 In2 -2.6(5) . . . . ?
_shelx_res_file
;
TITL s4602ma in P2(1)/n
CELL 1.54178 12.5836 22.3627 22.8132 90 101.127 90
ZERR 8 0.0003 0.0006 0.0006 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H O S In
UNIT 168 312 48 48 8
EQIV $1 0.5+X,1.5-Y,-0.5+Z
EQIV $2 1.5-X,-0.5+Y,0.5-Z
EQIV $3 0.5+X,1.5-Y,0.5+Z
EQIV $4 -0.5+X,1.5-Y,0.5+Z
EQIV $5 1.5-X,0.5+Y,0.5-Z
SADI O8 C28 O8 C28S
DELU O8 C28 O8 C28S
RIGU 0.002 0.002 C34 C32 C33 O10 C35 C31 C30 O9
RIGU 0.002 0.002 C28S C28 O8 C25 C26 C27 C24 C23 O7
ISOR 0.002 0.004 C28 C28S
EADP C28 C28S
L.S. 64
PLAN 0
SIZE 0.08 0.16 0.26
TEMP -93
HTAB C40 S6_$5
HTAB C35 S12_$4
HTAB C34 S3_$3
HTAB C28 O2_$2
HTAB C27 S1
HTAB C13 O3
HTAB C9 S10
HTAB C5 S10_$1
BOND $H
CONF
HTAB
fmap 2
acta
bump
REM
REM
REM
WGHT 0.050400 7.277200
FVAR 0.05161 0.66647
C1 1 0.669301 0.726738 0.180128 11.00000 0.04361 0.04293 =
0.04719 -0.00206 0.01420 -0.00765
C2 1 0.750932 0.766803 0.101869 11.00000 0.05457 0.06122 =
0.07672 0.01576 0.03446 0.00688
AFIX 23
H2A 2 0.792845 0.801842 0.120075 11.00000 -1.20000
H2B 2 0.677563 0.780436 0.082755 11.00000 -1.20000
AFIX 0
C3 1 0.806430 0.738282 0.056378 11.00000 0.05639 0.06393 =
0.06042 0.00482 0.02184 0.00570
AFIX 23
H3A 2 0.757927 0.707445 0.034471 11.00000 -1.20000
H3B 2 0.872698 0.717860 0.077435 11.00000 -1.20000
AFIX 0
C4 1 0.837403 0.781853 0.011627 11.00000 0.04634 0.07620 =
0.06495 0.01906 0.01775 0.00794
C5 1 0.882759 0.745991 -0.035671 11.00000 0.09955 0.11379 =
0.06690 0.02062 0.04314 0.03698
AFIX 137
H5A 2 0.906325 0.773626 -0.063966 11.00000 -1.50000
H5B 2 0.826262 0.719566 -0.057157 11.00000 -1.50000
H5C 2 0.944558 0.721957 -0.015994 11.00000 -1.50000
AFIX 0
C6 1 0.745917 0.821340 -0.015799 11.00000 0.07562 0.12122 =
0.07199 0.03470 0.03169 0.03073
AFIX 137
H6A 2 0.728838 0.848884 0.014491 11.00000 -1.50000
H6B 2 0.682198 0.796833 -0.031467 11.00000 -1.50000
H6C 2 0.766522 0.844283 -0.048465 11.00000 -1.50000
AFIX 0
C7 1 0.967057 0.860588 0.017444 11.00000 0.12080 0.20402 =
0.11746 0.00902 0.04153 -0.08026
AFIX 137
H7A 2 1.000698 0.842266 -0.013490 11.00000 -1.50000
H7B 2 1.022372 0.881632 0.046213 11.00000 -1.50000
H7C 2 0.911366 0.889047 -0.001080 11.00000 -1.50000
AFIX 0
C8 1 0.499927 0.838688 0.328013 11.00000 0.04001 0.03468 =
0.04500 0.00190 0.00247 0.00141
C9 1 0.581101 0.908125 0.401309 11.00000 0.07490 0.04456 =
0.05434 -0.00268 -0.01321 0.00120
AFIX 23
H9A 2 0.647418 0.911184 0.384162 11.00000 -1.20000
H9B 2 0.594259 0.878599 0.434251 11.00000 -1.20000
AFIX 0
C10 1 0.554063 0.967938 0.424473 11.00000 0.07312 0.05839 =
0.04891 -0.01222 0.00613 -0.00276
AFIX 23
H10A 2 0.591707 0.971215 0.466662 11.00000 -1.20000
H10B 2 0.475286 0.968831 0.424124 11.00000 -1.20000
AFIX 0
C11 1 0.582288 1.022790 0.391378 11.00000 0.05857 0.04256 =
0.07778 -0.00339 -0.00806 -0.00483
C12 1 0.545910 1.079372 0.418419 11.00000 0.09173 0.05433 =
0.09825 -0.01469 0.01461 0.00575
AFIX 137
H12A 2 0.589793 1.085410 0.458392 11.00000 -1.50000
H12B 2 0.469491 1.075640 0.421299 11.00000 -1.50000
H12C 2 0.554940 1.113628 0.393038 11.00000 -1.50000
AFIX 0
C13 1 0.532154 1.019123 0.324377 11.00000 0.08823 0.06806 =
0.07033 0.01331 -0.00306 -0.00746
AFIX 137
H13A 2 0.553048 1.054518 0.303936 11.00000 -1.50000
H13B 2 0.453071 1.017443 0.319222 11.00000 -1.50000
H13C 2 0.558421 0.983074 0.307311 11.00000 -1.50000
AFIX 0
C14 1 0.749933 1.064733 0.377296 11.00000 0.11287 0.07411 =
0.12475 0.02008 0.05465 0.00220
AFIX 137
H14A 2 0.739998 1.060262 0.333845 11.00000 -1.50000
H14B 2 0.827340 1.063105 0.394897 11.00000 -1.50000
H14C 2 0.720245 1.103275 0.386777 11.00000 -1.50000
AFIX 0
C15 1 0.370168 0.626029 0.273141 11.00000 0.04966 0.04301 =
0.03791 0.00063 0.01047 -0.00951
C16 1 0.297396 0.552004 0.330921 11.00000 0.06452 0.05244 =
0.04646 0.00599 0.01487 -0.01530
AFIX 23
H16A 2 0.284960 0.581746 0.361029 11.00000 -1.20000
H16B 2 0.366438 0.530982 0.346158 11.00000 -1.20000
AFIX 0
C17 1 0.204565 0.507976 0.318153 11.00000 0.06106 0.04897 =
0.06138 0.00642 0.01938 -0.01012
AFIX 23
H17A 2 0.223752 0.475591 0.292490 11.00000 -1.20000
H17B 2 0.139898 0.528670 0.295560 11.00000 -1.20000
AFIX 0
C18 1 0.176162 0.480524 0.373687 11.00000 0.06880 0.03446 =
0.06314 0.00086 0.02616 -0.00263
C19 1 0.272813 0.450728 0.412609 11.00000 0.07891 0.05734 =
0.08044 0.02565 0.01463 0.00297
AFIX 137
H19A 2 0.327114 0.481068 0.428243 11.00000 -1.50000
H19B 2 0.304381 0.421582 0.388819 11.00000 -1.50000
H19C 2 0.249468 0.430258 0.445944 11.00000 -1.50000
AFIX 0
C20 1 0.083862 0.436095 0.354999 11.00000 0.07234 0.05976 =
0.08845 -0.00037 0.02596 -0.02212
AFIX 137
H20A 2 0.068454 0.415723 0.390466 11.00000 -1.50000
H20B 2 0.104828 0.406540 0.327612 11.00000 -1.50000
H20C 2 0.019006 0.457479 0.334911 11.00000 -1.50000
AFIX 0
C21 1 0.107771 0.522619 0.457394 11.00000 0.10698 0.08267 =
0.09171 -0.00585 0.06275 -0.00533
AFIX 137
H21A 2 0.061639 0.487024 0.454608 11.00000 -1.50000
H21B 2 0.067270 0.557477 0.467131 11.00000 -1.50000
H21C 2 0.172049 0.516733 0.488768 11.00000 -1.50000
AFIX 0
C22 1 0.832320 0.643455 0.452734 11.00000 0.05235 0.05120 =
0.05292 0.00926 0.01240 0.00391
C23 1 0.750388 0.569606 0.383719 11.00000 0.08417 0.05683 =
0.09390 -0.01420 0.00879 0.01011
AFIX 23
H23A 2 0.719902 0.600062 0.353647 11.00000 -1.20000
H23B 2 0.693437 0.557598 0.405844 11.00000 -1.20000
AFIX 0
C24 1 0.789302 0.515917 0.353523 11.00000 0.12135 0.05919 =
0.11796 -0.02139 0.03114 0.01301
AFIX 23
H24A 2 0.842146 0.529716 0.329445 11.00000 -1.20000
H24B 2 0.828044 0.488776 0.384771 11.00000 -1.20000
AFIX 0
C25 1 0.703232 0.481315 0.314151 11.00000 0.12733 0.05027 =
0.11627 -0.01521 0.02350 0.00686
C26 1 0.753362 0.431670 0.282323 11.00000 0.13362 0.06864 =
0.15075 -0.03733 0.02266 0.00415
AFIX 137
H26A 2 0.764359 0.396034 0.307775 11.00000 -1.50000
H26B 2 0.823191 0.445176 0.274207 11.00000 -1.50000
H26C 2 0.704691 0.421959 0.244571 11.00000 -1.50000
AFIX 0
C27 1 0.631853 0.519908 0.269955 11.00000 0.14558 0.07467 =
0.10954 -0.00563 0.05278 0.03098
AFIX 137
H27A 2 0.591034 0.494934 0.238079 11.00000 -1.50000
H27B 2 0.676264 0.548542 0.252779 11.00000 -1.50000
H27C 2 0.581299 0.541639 0.289930 11.00000 -1.50000
AFIX 0
PART 2
C28S 1 0.566562 0.464023 0.385135 -21.00000 0.14017 0.13339 =
0.13785 -0.00229 0.02557 -0.00958
AFIX 137
H28A 2 0.593639 0.450369 0.426115 -21.00000 -1.50000
H28B 2 0.500204 0.442182 0.368219 -21.00000 -1.50000
H28C 2 0.550907 0.506942 0.385363 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C28 1 0.561748 0.414358 0.329593 21.00000 0.14017 0.13339 =
0.13785 -0.00229 0.02557 -0.00958
AFIX 137
H28D 2 0.497135 0.436353 0.310162 21.00000 -1.50000
H28E 2 0.544314 0.390164 0.362289 21.00000 -1.50000
H28F 2 0.586114 0.388173 0.300366 21.00000 -1.50000
AFIX 0
PART 0
C29 1 0.672426 0.775435 0.598654 11.00000 0.04132 0.04749 =
0.05409 -0.00159 0.01292 0.00103
C30 1 0.597628 0.758577 0.685776 11.00000 0.07023 0.06787 =
0.06864 0.00643 0.02769 0.01930
AFIX 23
H30A 2 0.671202 0.747191 0.706762 11.00000 -1.20000
H30B 2 0.552977 0.721985 0.677469 11.00000 -1.20000
AFIX 0
C31 1 0.546382 0.802507 0.722859 11.00000 0.06092 0.08694 =
0.07183 -0.00721 0.02006 0.02233
AFIX 23
H31A 2 0.590114 0.839612 0.727526 11.00000 -1.20000
H31B 2 0.473346 0.812924 0.700374 11.00000 -1.20000
AFIX 0
C32 1 0.535894 0.781441 0.782802 11.00000 0.09932 0.09882 =
0.08046 0.00420 0.04149 0.02456
C33 1 0.481300 0.827473 0.815851 11.00000 0.08464 0.13600 =
0.09223 -0.02699 0.02457 0.02241
AFIX 137
H33A 2 0.411332 0.838677 0.791353 11.00000 -1.50000
H33B 2 0.527437 0.862996 0.823810 11.00000 -1.50000
H33C 2 0.469854 0.810492 0.853746 11.00000 -1.50000
AFIX 0
C34 1 0.642988 0.762728 0.819688 11.00000 0.11521 0.16448 =
0.08416 0.02148 0.04657 0.04572
AFIX 137
H34A 2 0.631621 0.745995 0.857701 11.00000 -1.50000
H34B 2 0.690883 0.797567 0.827451 11.00000 -1.50000
H34C 2 0.676248 0.732427 0.797948 11.00000 -1.50000
AFIX 0
C35 1 0.411697 0.705854 0.798980 11.00000 0.17408 0.16606 =
0.17899 0.01471 0.08538 -0.01993
AFIX 137
H35A 2 0.461627 0.685633 0.831168 11.00000 -1.50000
H35B 2 0.364277 0.676217 0.775421 11.00000 -1.50000
H35C 2 0.367693 0.734680 0.816199 11.00000 -1.50000
AFIX 0
C36 1 0.954076 0.860810 0.490968 11.00000 0.05488 0.05980 =
0.06067 0.00585 0.01288 -0.01341
C37 1 0.979322 0.944016 0.427359 11.00000 0.09135 0.07335 =
0.07366 0.02696 0.02065 0.00190
AFIX 23
H37A 2 0.970488 0.916065 0.393108 11.00000 -1.20000
H37B 2 0.909696 0.965058 0.426092 11.00000 -1.20000
AFIX 0
C38 1 1.065441 0.987857 0.423086 11.00000 0.10712 0.06211 =
0.10041 0.00379 0.02444 -0.01002
AFIX 23
H38A 2 1.093762 1.004072 0.463459 11.00000 -1.20000
H38B 2 1.032975 1.021525 0.397601 11.00000 -1.20000
AFIX 0
C39 1 1.160571 0.962907 0.397644 11.00000 0.06736 0.10761 =
0.09450 0.02615 0.01924 -0.00957
C40 1 1.237861 1.015617 0.391362 11.00000 0.11389 0.15563 =
0.14698 0.05452 -0.02184 -0.06270
AFIX 137
H40A 2 1.309082 0.999866 0.387938 11.00000 -1.50000
H40B 2 1.245287 1.041416 0.426643 11.00000 -1.50000
H40C 2 1.208007 1.038846 0.355537 11.00000 -1.50000
AFIX 0
C41 1 1.214482 0.911000 0.434262 11.00000 0.08080 0.14905 =
0.13735 0.06349 0.02408 0.01582
AFIX 137
H41A 2 1.167701 0.875681 0.426895 11.00000 -1.50000
H41B 2 1.226602 0.921331 0.476780 11.00000 -1.50000
H41C 2 1.284079 0.902348 0.422840 11.00000 -1.50000
AFIX 0
C42 1 1.182855 0.921900 0.309165 11.00000 0.13668 0.23045 =
0.16487 -0.00763 0.10337 0.03640
AFIX 137
H42A 2 1.175964 0.944006 0.271528 11.00000 -1.50000
H42B 2 1.168494 0.879398 0.300626 11.00000 -1.50000
H42C 2 1.256410 0.926738 0.332424 11.00000 -1.50000
AFIX 0
IN1 5 0.509609 0.727867 0.258571 11.00000 0.04314 0.03700 =
0.04187 -0.00207 0.01103 -0.00652
IN2 5 0.828137 0.756867 0.518646 11.00000 0.04263 0.04703 =
0.04644 0.00365 0.00738 -0.00134
O1 3 0.743921 0.722549 0.146916 11.00000 0.05203 0.05582 =
0.05655 0.00759 0.02311 0.00707
O2 3 0.919816 0.816311 0.046822 11.00000 0.09407 0.12788 =
0.08388 0.00776 0.04154 -0.04077
O3 3 0.490352 0.889205 0.355675 11.00000 0.05376 0.03792 =
0.05157 -0.00766 -0.00371 0.00321
O4 3 0.697226 1.019480 0.400130 11.00000 0.06336 0.04984 =
0.11998 0.00590 0.00905 -0.00070
O5 3 0.300639 0.581347 0.273760 11.00000 0.06294 0.05078 =
0.04530 0.00546 0.01160 -0.02202
O6 3 0.139795 0.532110 0.402490 11.00000 0.08657 0.05077 =
0.07623 -0.00379 0.03874 -0.00185
O7 3 0.843315 0.593602 0.424502 11.00000 0.07111 0.05136 =
0.07755 -0.00626 0.01694 0.01221
O8 3 0.641967 0.453835 0.351793 11.00000 0.14699 0.12123 =
0.13310 -0.00433 0.02627 -0.01657
O9 3 0.602101 0.790218 0.631114 11.00000 0.04622 0.06159 =
0.06558 0.00401 0.01436 0.01726
O10 3 0.464391 0.732565 0.766156 11.00000 0.17190 0.14479 =
0.13532 -0.02588 0.07958 -0.02654
O11 3 1.009276 0.909757 0.484943 11.00000 0.07418 0.07182 =
0.06544 0.00943 0.01234 -0.02561
O12 3 1.110096 0.943545 0.341045 11.00000 0.09643 0.12418 =
0.09738 0.00392 0.02181 0.01326
S1 4 0.674850 0.673315 0.233185 11.00000 0.05245 0.04499 =
0.05228 0.00873 0.01538 0.00537
S2 4 0.574796 0.781974 0.170375 11.00000 0.05035 0.03900 =
0.05081 0.00690 0.01602 0.00102
S3 4 0.389607 0.817519 0.275937 11.00000 0.03882 0.04803 =
0.05331 -0.00809 0.00123 -0.00018
S4 4 0.613964 0.796525 0.342119 11.00000 0.04540 0.04004 =
0.05524 -0.00648 -0.00582 0.00140
S5 4 0.459336 0.648560 0.334105 11.00000 0.05198 0.04936 =
0.03443 0.00152 0.00666 -0.01101
S6 4 0.361614 0.657846 0.204813 11.00000 0.05840 0.04876 =
0.03605 0.00471 0.00247 -0.01448
S7 4 0.714538 0.682053 0.441946 11.00000 0.04722 0.04776 =
0.05824 -0.00289 -0.00124 0.00269
S8 4 0.944759 0.667174 0.501322 11.00000 0.04421 0.06336 =
0.06580 -0.00023 0.01039 0.00646
S9 4 0.761822 0.718549 0.614063 11.00000 0.04878 0.04156 =
0.04889 0.00404 0.01202 0.00542
S10 4 0.668873 0.820191 0.537691 11.00000 0.05430 0.05833 =
0.06253 0.01488 0.00871 0.01436
S11 4 0.983621 0.829165 0.560651 11.00000 0.05556 0.07114 =
0.04432 0.00685 0.00036 -0.01548
S12 4 0.858145 0.832811 0.436205 11.00000 0.06634 0.07353 =
0.04315 0.01104 -0.00036 -0.02071
HKLF 4
REM s4602ma in P2(1)/n
REM R1 = 0.0553 for 8323 Fo > 4sig(Fo) and 0.0902 for all 12232 data
REM 636 parameters refined using 122 restraints
END
WGHT 0.0514 7.1109
REM Instructions for potential hydrogen bonds
HTAB C5 S10_$1
HTAB C9 S10
HTAB C27 S1
HTAB C28 O2_$2
HTAB C33 S1_$4
HTAB C35 S12_$4
REM Highest difference peak 1.358, deepest hole -1.006, 1-sigma level 0.104
Q1 1 0.5320 0.7145 0.8027 11.00000 0.05 1.36
Q2 1 0.5632 0.5143 0.2331 11.00000 0.05 1.06
Q3 1 0.6870 0.5295 0.2790 11.00000 0.05 0.80
Q4 1 0.5809 0.7269 0.2385 11.00000 0.05 0.67
Q5 1 0.6753 0.7856 0.8349 11.00000 0.05 0.66
Q6 1 0.9042 0.8017 0.4316 11.00000 0.05 0.66
Q7 1 0.4190 0.6940 0.7626 11.00000 0.05 0.65
Q8 1 1.2141 0.9814 0.4273 11.00000 0.05 0.60
Q9 1 0.8994 0.7482 0.4988 11.00000 0.05 0.59
Q10 1 0.5984 0.7318 0.8133 11.00000 0.05 0.58
Q11 1 0.4391 0.7317 0.2806 11.00000 0.05 0.58
Q12 1 0.7565 0.7532 0.5452 11.00000 0.05 0.55
Q13 1 0.7236 0.4207 0.3074 11.00000 0.05 0.55
Q14 1 1.0648 0.8743 0.4851 11.00000 0.05 0.55
Q15 1 0.4579 0.7956 0.2565 11.00000 0.05 0.47
Q16 1 1.0188 0.7978 0.5538 11.00000 0.05 0.46
Q17 1 0.6625 0.7969 0.5634 11.00000 0.05 0.45
Q18 1 0.4399 0.7446 0.7530 11.00000 0.05 0.44
Q19 1 0.8641 0.8130 0.5070 11.00000 0.05 0.44
Q20 1 1.0469 0.8995 0.4231 11.00000 0.05 0.43
;
_shelx_res_checksum 72936
_olex2_submission_special_instructions 'No special instructions were received'