# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_2013ncs0255_twin
_database_code_depnum_ccdc_archive 'CCDC 1051494'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;
_audit_creation_date             13-04-05
_audit_creation_method           
;
Rigaku CrystalClear-SM Expert 3.1 b25
;
_shelxl_version_number           2012-9
_chemical_name_common            ?
_chemical_name_systematic        
;
(exo-methylene- BEDT-TTF)perchlorate.
;
_chemical_formula_moiety         'Cl O4, C11 H8 S8'
_chemical_formula_sum            'C11 H8 Cl O4 S8'
_chemical_formula_weight         496.10
_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'
Cl Cl 0.1484 0.1585 '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                   6.401(2)
_cell_length_b                   16.234(5)
_cell_length_c                   16.417(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.579(9)
_cell_angle_gamma                90
_cell_volume                     1697.9(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8160
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   None
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       column
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1358
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12665
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.493
_diffrn_reflns_transf_matrix_11  0.151958
_diffrn_reflns_transf_matrix_12  0.011981
_diffrn_reflns_transf_matrix_13  -0.037480
_diffrn_reflns_transf_matrix_21  0.014161
_diffrn_reflns_transf_matrix_22  0.006743
_diffrn_reflns_transf_matrix_23  0.059569
_diffrn_reflns_transf_matrix_31  0.005939
_diffrn_reflns_transf_matrix_32  -0.029953
_diffrn_reflns_transf_matrix_33  0.001979
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 172
	           Slice: -99.0000 - 73.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 14.0000
	             Phi: 77.0000
	             XTD: 44.9219
	          2theta: -17.0750
scan:
	Number of images: 129
	           Slice: -56.0000 - 73.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: 25.0000
	             XTD: 44.9219
	          2theta: -17.0750
scan:
	Number of images: 15
	           Slice: -29.0000 - -14.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 43.0000
	             Phi: -26.0000
	             XTD: 44.9219
	          2theta: -17.0750
scan:
	Number of images: 10
	           Slice: -11.0000 - -1.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: 25.0000
	             XTD: 44.9219
	          2theta: -17.0750
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.151958
_diffrn_orient_matrix_UB_12      0.011981
_diffrn_orient_matrix_UB_13      -0.037480
_diffrn_orient_matrix_UB_21      0.014161
_diffrn_orient_matrix_UB_22      0.006743
_diffrn_orient_matrix_UB_23      0.059569
_diffrn_orient_matrix_UB_31      0.005939
_diffrn_orient_matrix_UB_32      -0.029953
_diffrn_orient_matrix_UB_33      0.001979
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8291
_reflns_number_total             12665
_reflns_special_details          
;
 _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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
;
_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.230
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         12665
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.1115
_refine_ls_restrained_S_all      1.067
_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/[σ²(Fo²)+(0.0161P)²+17.8637P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.2219
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 Cl1-O2 \\sim Cl1-O4 \\sim Cl1-O3 \\sim Cl1-O1 \\sim Cl1-O4A \\sim Cl1-O3A
 with sigma of 0.02
 O1-O2 \\sim O1-O3 \\sim O1-O4 \\sim O1-O3A \\sim O1-O4A \\sim O3A-O4A \\sim
O2-O3 \\sim O2-O4 \\sim O3-O4
 with sigma of 0.02
3. Others
 Sof(O3A)=Sof(O4A)=1-FVAR(1)
 Sof(O3)=Sof(O4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B)
4.b X=CH2 refined with riding coordinates:
 C11(H11A,H11B)
;
_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
Cl1 Cl 0.4686(7) 0.1716(2) 0.5070(2) 0.0538(10) Uani 1 1 d D . . . .
O1 O 0.4284(15) 0.2390(5) 0.4519(6) 0.066(3) Uani 1 1 d D . . . .
S1 S 0.7808(6) 0.5167(2) 0.1848(2) 0.0433(9) Uani 1 1 d . . . . .
S2 S 1.2968(5) 0.4380(2) 0.2221(2) 0.0404(8) Uani 1 1 d . . . . .
S3 S 0.7489(5) 0.46764(19) 0.35729(19) 0.0347(8) Uani 1 1 d . . . . .
S4 S 1.1758(5) 0.40649(18) 0.38577(19) 0.0338(7) Uani 1 1 d . . . . .
S5 S 0.6634(5) 0.40740(18) 0.54100(18) 0.0328(7) Uani 1 1 d . . . . .
S6 S 1.0859(5) 0.34060(19) 0.56231(19) 0.0363(8) Uani 1 1 d . . . . .
S7 S 0.5422(5) 0.35301(19) 0.70151(19) 0.0356(8) Uani 1 1 d . . . . .
S8 S 1.0503(5) 0.2701(2) 0.7254(2) 0.0460(9) Uani 1 1 d . . . . .
C1 C 0.959(2) 0.4829(9) 0.1122(8) 0.055(4) Uani 1 1 d . . . . .
H1A H 0.9400 0.4230 0.1034 0.066 Uiso 1 1 calc R U . . .
H1B H 0.9193 0.5106 0.0592 0.066 Uiso 1 1 calc R U . . .
C2 C 1.191(2) 0.4999(8) 0.1380(8) 0.050(4) Uani 1 1 d . . . . .
H2A H 1.2077 0.5588 0.1531 0.060 Uiso 1 1 calc R U . . .
H2B H 1.2720 0.4898 0.0907 0.060 Uiso 1 1 calc R U . . .
C3 C 0.906(2) 0.4738(7) 0.2750(7) 0.033(3) Uani 1 1 d . . . . .
C4 C 1.1014(18) 0.4447(7) 0.2886(7) 0.031(3) Uani 1 1 d . . . . .
C5 C 0.9373(18) 0.4218(7) 0.4248(7) 0.032(3) Uani 1 1 d . . . . .
C6 C 0.8993(18) 0.3942(7) 0.5015(7) 0.030(3) Uani 1 1 d . . . . .
C7 C 0.7326(18) 0.3582(6) 0.6334(7) 0.029(3) Uani 1 1 d . . . . .
C8 C 0.932(2) 0.3261(7) 0.6427(7) 0.034(3) Uani 1 1 d . . . . .
C9 C 0.636(2) 0.2617(8) 0.7581(8) 0.046(4) Uani 1 1 d . . . . .
H9A H 0.5460 0.2513 0.8027 0.056 Uiso 1 1 calc R U . . .
H9B H 0.6251 0.2135 0.7210 0.056 Uiso 1 1 calc R U . . .
C10 C 0.853(2) 0.2709(8) 0.7928(8) 0.046(4) Uani 1 1 d . . . . .
C11 C 0.910(3) 0.2758(8) 0.8718(10) 0.069(5) Uani 1 1 d . . . . .
H11A H 0.8070 0.2734 0.9096 0.083 Uiso 1 1 calc R U . . .
H11B H 1.0541 0.2817 0.8910 0.083 Uiso 1 1 calc R U . . .
O2 O 0.455(2) 0.0964(5) 0.4690(7) 0.099(5) Uani 1 1 d D . . . .
O3 O 0.357(3) 0.1840(10) 0.5772(10) 0.068(7) Uiso 0.59(3) 1 d D . P A 1
O4 O 0.696(3) 0.1793(10) 0.5390(11) 0.070(7) Uiso 0.59(3) 1 d D . P A 1
O3A O 0.247(3) 0.1518(18) 0.5296(19) 0.093(13) Uiso 0.41(3) 1 d D . P A 2
O4A O 0.591(5) 0.1854(17) 0.5789(14) 0.094(13) Uiso 0.41(3) 1 d D . P A 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
Cl1 O1 1.428(8) . ?
Cl1 O2 1.370(8) . ?
Cl1 O3 1.428(13) . ?
Cl1 O4 1.502(15) . ?
Cl1 O3A 1.534(19) . ?
Cl1 O4A 1.369(18) . ?
S1 C1 1.811(13) . ?
S1 C3 1.758(12) . ?
S2 C2 1.789(13) . ?
S2 C4 1.742(12) . ?
S3 C3 1.764(12) . ?
S3 C5 1.725(12) . ?
S4 C4 1.734(12) . ?
S4 C5 1.730(12) . ?
S5 C6 1.714(12) . ?
S5 C7 1.733(11) . ?
S6 C6 1.718(11) . ?
S6 C8 1.739(12) . ?
S7 C7 1.735(12) . ?
S7 C9 1.820(13) . ?
S8 C8 1.744(12) . ?
S8 C10 1.757(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.529(18) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.334(16) . ?
C5 C6 1.380(14) . ?
C7 C8 1.372(16) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.459(17) . ?
C10 C11 1.314(17) . ?
C11 H11A 0.9500 . ?
C11 H11B 0.9500 . ?

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 Cl1 O4 105.4(8) . . ?
O1 Cl1 O3A 101.5(10) . . ?
O2 Cl1 O1 113.2(6) . . ?
O2 Cl1 O3 118.6(9) . . ?
O2 Cl1 O4 104.6(8) . . ?
O2 Cl1 O3A 84.5(14) . . ?
O3 Cl1 O1 109.2(7) . . ?
O3 Cl1 O4 104.5(9) . . ?
O4A Cl1 O1 118.2(12) . . ?
O4A Cl1 O2 123.0(14) . . ?
O4A Cl1 O3A 106.8(14) . . ?
C3 S1 C1 99.8(6) . . ?
C4 S2 C2 101.9(6) . . ?
C5 S3 C3 95.8(6) . . ?
C5 S4 C4 96.7(6) . . ?
C6 S5 C7 96.6(6) . . ?
C6 S6 C8 95.5(6) . . ?
C7 S7 C9 98.6(6) . . ?
C8 S8 C10 101.7(6) . . ?
S1 C1 H1A 108.6 . . ?
S1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.5 . . ?
C2 C1 S1 114.8(10) . . ?
C2 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
S2 C2 H2A 108.9 . . ?
S2 C2 H2B 108.9 . . ?
C1 C2 S2 113.4(10) . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
S1 C3 S3 114.8(7) . . ?
C4 C3 S1 128.6(10) . . ?
C4 C3 S3 116.6(9) . . ?
S4 C4 S2 113.8(7) . . ?
C3 C4 S2 129.5(10) . . ?
C3 C4 S4 116.7(9) . . ?
S3 C5 S4 114.3(7) . . ?
C6 C5 S3 123.5(9) . . ?
C6 C5 S4 122.1(9) . . ?
S5 C6 S6 115.6(7) . . ?
C5 C6 S5 123.0(9) . . ?
C5 C6 S6 121.4(9) . . ?
S5 C7 S7 116.8(7) . . ?
C8 C7 S5 115.4(9) . . ?
C8 C7 S7 127.8(9) . . ?
S6 C8 S8 115.2(7) . . ?
C7 C8 S6 116.9(9) . . ?
C7 C8 S8 127.9(9) . . ?
S7 C9 H9A 109.3 . . ?
S7 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 S7 111.8(10) . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
C9 C10 S8 117.9(10) . . ?
C11 C10 S8 118.4(13) . . ?
C11 C10 C9 123.6(14) . . ?
C10 C11 H11A 120.0 . . ?
C10 C11 H11B 120.0 . . ?
H11A C11 H11B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S2 69.7(13) . . . . ?
S1 C3 C4 S2 -0.9(18) . . . . ?
S1 C3 C4 S4 179.9(7) . . . . ?
S3 C3 C4 S2 178.1(7) . . . . ?
S3 C3 C4 S4 -1.1(13) . . . . ?
S3 C5 C6 S5 -3.7(15) . . . . ?
S3 C5 C6 S6 173.9(6) . . . . ?
S4 C5 C6 S5 -179.1(6) . . . . ?
S4 C5 C6 S6 -1.5(14) . . . . ?
S5 C7 C8 S6 0.9(13) . . . . ?
S5 C7 C8 S8 -177.7(7) . . . . ?
S7 C7 C8 S6 179.3(6) . . . . ?
S7 C7 C8 S8 0.6(17) . . . . ?
S7 C9 C10 S8 -70.9(12) . . . . ?
S7 C9 C10 C11 112.4(14) . . . . ?
C1 S1 C3 S3 -163.4(7) . . . . ?
C1 S1 C3 C4 15.6(13) . . . . ?
C2 S2 C4 S4 -168.7(7) . . . . ?
C2 S2 C4 C3 12.0(13) . . . . ?
C3 S1 C1 C2 -49.2(12) . . . . ?
C3 S3 C5 S4 1.5(7) . . . . ?
C3 S3 C5 C6 -174.2(10) . . . . ?
C4 S2 C2 C1 -44.9(11) . . . . ?
C4 S4 C5 S3 -1.9(7) . . . . ?
C4 S4 C5 C6 173.8(10) . . . . ?
C5 S3 C3 S1 178.9(7) . . . . ?
C5 S3 C3 C4 -0.2(10) . . . . ?
C5 S4 C4 S2 -177.5(6) . . . . ?
C5 S4 C4 C3 1.9(10) . . . . ?
C6 S5 C7 S7 180.0(7) . . . . ?
C6 S5 C7 C8 -1.5(10) . . . . ?
C6 S6 C8 S8 178.9(7) . . . . ?
C6 S6 C8 C7 0.1(10) . . . . ?
C7 S5 C6 S6 1.6(7) . . . . ?
C7 S5 C6 C5 179.3(10) . . . . ?
C7 S7 C9 C10 56.1(11) . . . . ?
C8 S6 C6 S5 -1.2(7) . . . . ?
C8 S6 C6 C5 -178.9(10) . . . . ?
C8 S8 C10 C9 39.1(12) . . . . ?
C8 S8 C10 C11 -144.0(11) . . . . ?
C9 S7 C7 S5 154.7(7) . . . . ?
C9 S7 C7 C8 -23.6(12) . . . . ?
C10 S8 C8 S6 178.7(7) . . . . ?
C10 S8 C8 C7 -2.7(13) . . . . ?
_vrf_PLAT021_2013ncs0255_twin    
;
PROBLEM: Ratio Unique/Expected Reflections too High 3.233          

RESPONSE: refined in SHELXL with HLKF5
;
_vrf_PLAT340_2013ncs0255_twin    
;
PROBLEM: 
Low Bond Precision on  C-C Bonds 0.0177 Ang        

RESPONSE: refinement of a twinned structure, 
with disordered perchlorate
;
_vrf_PLAT202_2013ncs0255_twin    
;
PROBLEM: two isotropic atoms
        

RESPONSE: These were part of the model for disordered ClO4
;
####################################################################### 
# 
# 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_V130218b
_database_code_depnum_ccdc_archive 'CCDC 1051495'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C11 H8 I4 S8'
_chemical_formula_moiety         'C11 H8 S8, I3, 0.5(I2) '
_chemical_formula_weight         904.28
_chemical_melting_point          ?
_chemical_name_systematic        
;
(exo-methylene-BEDT-TTF)triiodide.0.5iodine.
;

#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.2014(15)
_cell_length_b                   9.1986(16)
_cell_length_c                   15.637(3)
_cell_angle_alpha                86.967(10)
_cell_angle_beta                 86.049(10)
_cell_angle_gamma                72.972(7)
_cell_volume                     1124.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3348
_cell_measurement_theta_min      1.31
_cell_measurement_theta_max      30.17
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    2.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828.00
_exptl_absorpt_coefficient_mu    6.281
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_T_max  0.882

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            8677
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 0.951
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_reflns_number_total             4911
_reflns_number_gt                3208
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1517
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4901
_refine_ls_number_parameters     208
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0701P)²+0.0392P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.470
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
I I -0.4742 1.8119
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.05004(8) 0.13696(7) 0.43369(4) 0.0583(2) Uani 1.0 2 d . . .
I2 I 0.08844(7) 0.29165(6) 0.27245(3) 0.04820(18) Uani 1.0 2 d . . .
I3 I 0.12472(9) 0.43481(7) 0.10141(4) 0.0606(3) Uani 1.0 2 d . . .
I4 I 0.03894(12) 0.12873(9) 0.02650(5) 0.0911(3) Uani 1.0 2 d . . .
S1 S 0.6385(4) 0.4767(4) 0.16681(18) 0.0743(8) Uani 1.0 2 d . . .
S2 S 0.2663(4) 0.7746(4) 0.21355(18) 0.0694(8) Uani 1.0 2 d . . .
S3 S 0.5747(3) 0.3673(3) 0.34194(15) 0.0507(6) Uani 1.0 2 d . . .
S4 S 0.2626(3) 0.6078(3) 0.37966(15) 0.0478(5) Uani 1.0 2 d . . .
S5 S 0.5241(3) 0.1922(3) 0.51899(14) 0.0476(5) Uani 1.0 2 d . . .
S6 S 0.2090(3) 0.4292(3) 0.56167(14) 0.0465(5) Uani 1.0 2 d . . .
S7 S 0.5106(3) -0.0002(3) 0.67355(16) 0.0570(6) Uani 1.0 2 d . . .
S8 S 0.1278(3) 0.2749(3) 0.72409(15) 0.0560(6) Uani 1.0 2 d . . .
C1 C 0.561(3) 0.651(2) 0.1145(11) 0.186(12) Uani 1.0 2 d . . .
C2 C 0.3980(17) 0.742(2) 0.1179(10) 0.123(6) Uani 1.0 2 d . . .
C3 C 0.5085(13) 0.5028(11) 0.2587(6) 0.054(3) Uani 1.0 2 d . . .
C4 C 0.3600(11) 0.6164(11) 0.2793(6) 0.051(3) Uani 1.0 2 d . . .
C5 C 0.4044(10) 0.4389(10) 0.4127(6) 0.0421(19) Uani 1.0 2 d . . .
C6 C 0.3817(10) 0.3630(9) 0.4890(6) 0.0434(19) Uani 1.0 2 d . . .
C7 C 0.4125(10) 0.1645(10) 0.6136(5) 0.043(2) Uani 1.0 2 d . . .
C8 C 0.2660(10) 0.2735(10) 0.6341(6) 0.0437(19) Uani 1.0 2 d . . .
C9 C 0.3592(14) -0.0065(11) 0.7560(7) 0.066(3) Uani 1.0 2 d . . .
C10 C 0.1798(14) 0.0672(13) 0.7400(7) 0.074(3) Uani 1.0 2 d . . .
C11 C 0.4104(18) -0.0827(16) 0.8257(9) 0.105(5) Uani 1.0 2 d . . .
H1A H 0.6291 0.7136 0.1319 0.2234 Uiso 1.0 2 calc R . .
H1B H 0.5912 0.6334 0.0541 0.2234 Uiso 1.0 2 calc R . .
H2A H 0.3377 0.7030 0.0777 0.1475 Uiso 1.0 2 calc R . .
H2B H 0.4018 0.8414 0.0950 0.1475 Uiso 1.0 2 calc R . .
H10A H 0.1093 0.0441 0.7881 0.0891 Uiso 1.0 2 calc R . .
H10B H 0.1515 0.0249 0.6894 0.0891 Uiso 1.0 2 calc R . .
H11A H 0.3312 -0.0930 0.8694 0.1256 Uiso 1.0 2 calc R . .
H11B H 0.5264 -0.1271 0.8324 0.1256 Uiso 1.0 2 calc R . .



#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_molecular_graphics    'CrystalStructure 4.0'

#==============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
I1 I2 2.8730(10) yes . .
I2 I3 2.9534(10) yes . .
I4 I4 2.8054(14) yes . 2_555
S1 C1 1.730(17) yes . .
S1 C3 1.713(10) yes . .
S2 C2 1.768(15) yes . .
S2 C4 1.750(9) yes . .
S3 C3 1.753(9) yes . .
S3 C5 1.713(8) yes . .
S4 C4 1.720(9) yes . .
S4 C5 1.724(8) yes . .
S5 C6 1.725(8) yes . .
S5 C7 1.733(9) yes . .
S6 C6 1.736(8) yes . .
S6 C8 1.750(9) yes . .
S7 C7 1.749(8) yes . .
S7 C9 1.739(11) yes . .
S8 C8 1.743(9) yes . .
S8 C10 1.839(12) yes . .
C1 C2 1.35(3) yes . .
C3 C4 1.384(12) yes . .
C5 C6 1.380(12) yes . .
C7 C8 1.352(10) yes . .
C9 C10 1.462(15) yes . .
C9 C11 1.290(17) yes . .
C1 H1A 0.970 no . .
C1 H1B 0.970 no . .
C2 H2A 0.970 no . .
C2 H2B 0.970 no . .
C10 H10A 0.970 no . .
C10 H10B 0.970 no . .
C11 H11A 0.930 no . .
C11 H11B 0.930 no . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
I1 I2 I3 176.50(3) yes . . .
C1 S1 C3 100.7(7) yes . . .
C2 S2 C4 103.2(6) yes . . .
C3 S3 C5 96.9(4) yes . . .
C4 S4 C5 95.9(4) yes . . .
C6 S5 C7 96.1(4) yes . . .
C6 S6 C8 95.8(4) yes . . .
C7 S7 C9 103.7(4) yes . . .
C8 S8 C10 96.4(5) yes . . .
S1 C1 C2 127.0(17) yes . . .
S2 C2 C1 123.5(12) yes . . .
S1 C3 S3 115.6(5) yes . . .
S1 C3 C4 130.5(8) yes . . .
S3 C3 C4 113.8(7) yes . . .
S2 C4 S4 116.4(5) yes . . .
S2 C4 C3 125.6(7) yes . . .
S4 C4 C3 118.0(7) yes . . .
S3 C5 S4 115.1(5) yes . . .
S3 C5 C6 121.7(6) yes . . .
S4 C5 C6 123.2(6) yes . . .
S5 C6 S6 114.7(5) yes . . .
S5 C6 C5 121.9(6) yes . . .
S6 C6 C5 123.3(6) yes . . .
S5 C7 S7 114.9(4) yes . . .
S5 C7 C8 117.2(7) yes . . .
S7 C7 C8 127.9(7) yes . . .
S6 C8 S8 116.8(4) yes . . .
S6 C8 C7 116.1(7) yes . . .
S8 C8 C7 127.1(7) yes . . .
S7 C9 C10 117.7(8) yes . . .
S7 C9 C11 118.4(10) yes . . .
C10 C9 C11 123.8(12) yes . . .
S8 C10 C9 113.6(9) yes . . .
S1 C1 H1A 105.566 no . . .
S1 C1 H1B 105.569 no . . .
C2 C1 H1A 105.561 no . . .
C2 C1 H1B 105.566 no . . .
H1A C1 H1B 106.091 no . . .
S2 C2 H2A 106.468 no . . .
S2 C2 H2B 106.471 no . . .
C1 C2 H2A 106.463 no . . .
C1 C2 H2B 106.467 no . . .
H2A C2 H2B 106.488 no . . .
S8 C10 H10A 108.848 no . . .
S8 C10 H10B 108.853 no . . .
C9 C10 H10A 108.848 no . . .
C9 C10 H10B 108.852 no . . .
H10A C10 H10B 107.706 no . . .
C9 C11 H11A 120.001 no . . .
C9 C11 H11B 120.001 no . . .
H11A C11 H11B 119.998 no . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 S1 C3 S3 -166.0(10) no . . . .
C1 S1 C3 C4 12.2(13) no . . . .
C3 S1 C1 C2 -32.4(18) no . . . .
C2 S2 C4 S4 -179.3(8) no . . . .
C2 S2 C4 C3 3.7(11) no . . . .
C4 S2 C2 C1 -22.3(16) no . . . .
C3 S3 C5 S4 -5.2(7) no . . . .
C3 S3 C5 C6 172.9(8) no . . . .
C5 S3 C3 S1 -177.8(7) no . . . .
C5 S3 C3 C4 3.6(8) no . . . .
C4 S4 C5 S3 4.8(7) no . . . .
C4 S4 C5 C6 -173.3(8) no . . . .
C5 S4 C4 S2 -179.5(7) no . . . .
C5 S4 C4 C3 -2.3(9) no . . . .
C6 S5 C7 S7 -178.5(6) no . . . .
C6 S5 C7 C8 -1.0(8) no . . . .
C7 S5 C6 S6 1.9(7) no . . . .
C7 S5 C6 C5 -177.6(7) no . . . .
C6 S6 C8 S8 -178.3(6) no . . . .
C6 S6 C8 C7 1.3(8) no . . . .
C8 S6 C6 S5 -1.9(7) no . . . .
C8 S6 C6 C5 177.5(8) no . . . .
C7 S7 C9 C10 26.4(9) no . . . .
C7 S7 C9 C11 -157.3(8) no . . . .
C9 S7 C7 S5 -173.5(6) no . . . .
C9 S7 C7 C8 9.4(10) no . . . .
C8 S8 C10 C9 60.8(7) no . . . .
C10 S8 C8 S6 152.1(6) no . . . .
C10 S8 C8 C7 -27.5(9) no . . . .
S1 C1 C2 S2 42(3) no . . . .
S1 C3 C4 S2 -2.3(17) no . . . .
S1 C3 C4 S4 -179.2(7) no . . . .
S3 C3 C4 S2 176.0(7) no . . . .
S3 C3 C4 S4 -0.9(12) no . . . .
S3 C5 C6 S5 0.7(13) no . . . .
S3 C5 C6 S6 -178.7(6) no . . . .
S4 C5 C6 S5 178.7(6) no . . . .
S4 C5 C6 S6 -0.7(13) no . . . .
S5 C7 C8 S6 -0.2(11) no . . . .
S5 C7 C8 S8 179.4(6) no . . . .
S7 C7 C8 S6 176.9(6) no . . . .
S7 C7 C8 S8 -3.6(15) no . . . .
S7 C9 C10 S8 -65.7(11) no . . . .
C11 C9 C10 S8 118.3(13) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
S1 S2 3.517(4) no . .
S3 S5 3.192(4) no . .
S4 S6 3.279(4) no . .
S7 S8 3.479(3) no . .
C1 C4 3.02(2) no . .
C2 C3 3.018(18) no . .
C7 C10 2.940(15) no . .
C8 C9 3.063(13) no . .
I1 I1 3.4273(11) no . 2_556
I3 I4 3.3789(13) no . .
I4 I3 3.3789(13) no . .
S2 S8 3.462(4) no . 2_566
S2 C10 3.558(11) no . 2_566
S3 S6 3.397(4) no . 2_666
S3 S7 3.666(4) no . 2_656
S3 C9 3.608(11) no . 2_656
S4 S5 3.396(4) no . 2_666
S4 S8 3.544(4) no . 2_566
S5 S4 3.396(4) no . 2_666
S5 S7 3.639(4) no . 2_656
S6 S3 3.397(4) no . 2_666
S7 S3 3.666(4) no . 2_656
S7 S5 3.639(4) no . 2_656
S8 S2 3.462(4) no . 2_566
S8 S4 3.544(4) no . 2_566
C3 C8 3.673(15) no . 2_666
C4 C7 3.651(15) no . 2_666
C5 C5 3.623(13) no . 2_666
C5 C6 3.362(14) no . 2_666
C6 C5 3.362(14) no . 2_666
C6 C6 3.645(14) no . 2_666
C7 C4 3.651(15) no . 2_666
C8 C3 3.673(15) no . 2_666
C9 S3 3.608(11) no . 2_656
C10 S2 3.558(11) no . 2_566
S1 H2A 3.0853 no . .
S1 H2B 3.5170 no . .
S2 H1A 3.0613 no . .
S2 H1B 3.5223 no . .
S7 H10A 3.5622 no . .
S7 H10B 2.8800 no . .
S7 H11A 3.4801 no . .
S7 H11B 2.6825 no . .
C3 H1A 3.0188 no . .
C3 H1B 3.4515 no . .
C3 H2A 3.4419 no . .
C4 H1A 3.3490 no . .
C4 H2A 3.2148 no . .
C4 H2B 3.5139 no . .
C7 H10B 2.9552 no . .
C8 H10A 3.5391 no . .
C8 H10B 2.7913 no . .
C10 H11A 2.6014 no . .
C10 H11B 3.2680 no . .
C11 H10A 2.4988 no . .
C11 H10B 3.0333 no . .
H1A H2A 2.6195 no . .
H1A H2B 1.9957 no . .
H1B H2A 2.0019 no . .
H1B H2B 2.1759 no . .
H10A H11A 2.3070 no . .
H10A H11B 3.4231 no . .
H10B H11A 3.2528 no . .
I1 H10B 3.2923 no . 2_556
I2 H11B 3.4210 no . 2_656
I3 H1B 3.2027 no . 2_665
I3 H2A 3.4081 no . .
I3 H11B 3.5531 no . 2_656
I4 H2A 3.4958 no . 2_565
I4 H2B 3.5389 no . 1_545
I4 H10A 3.5450 no . 2_556
I4 H11A 3.5772 no . 1_554
I4 H11A 3.4378 no . 2_556
S1 H11A 3.5373 no . 2_656
S2 H10A 3.0442 no . 2_566
S2 H10B 3.6504 no . 2_566
S3 H10B 3.6859 no . 2_656
S8 H1A 3.1339 no . 2_666
C9 H1A 3.3187 no . 2_666
C10 H1A 3.6396 no . 2_666
C11 H1A 3.4106 no . 2_666
C11 H2B 3.3751 no . 2_666
H1A S8 3.1339 no . 2_666
H1A C9 3.3187 no . 2_666
H1A C10 3.6396 no . 2_666
H1A C11 3.4106 no . 2_666
H1A H11A 3.5981 no . 2_666
H1B I3 3.2027 no . 2_665
H1B H2A 3.6903 no . 2_665
H2A I3 3.4081 no . .
H2A I4 3.4958 no . 2_565
H2A H1B 3.6903 no . 2_665
H2A H11A 3.6675 no . 1_564
H2B I4 3.5389 no . 1_565
H2B C11 3.3751 no . 2_666
H2B H11A 3.6058 no . 1_564
H2B H11B 3.1402 no . 2_666
H10A I4 3.5450 no . 2_556
H10A S2 3.0442 no . 2_566
H10B I1 3.2923 no . 2_556
H10B S2 3.6504 no . 2_566
H10B S3 3.6859 no . 2_656
H11A I4 3.5772 no . 1_556
H11A I4 3.4378 no . 2_556
H11A S1 3.5373 no . 2_656
H11A H1A 3.5981 no . 2_666
H11A H2A 3.6675 no . 1_546
H11A H2B 3.6058 no . 1_546
H11B I2 3.4210 no . 2_656
H11B I3 3.5531 no . 2_656
H11B H2B 3.1402 no . 2_666

#==============================================================================

_vrf_PLAT241_V130218b            
; 
PROBLEM: Large Hirshfeld Difference C1     --  C2      ..       0.30 Ang
           High  Ueq as Compared to Neighbors for .....         C1 Check 

RESPONSE: there is some conformational disorder in the ethylene bridge,
          leading to these artefacts.  
;

_vrf_PLAT360_V130218b            
; 
PROBLEM: Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        4.5 Ratio 
         Low       Ueq as Compared to Neighbors for .....         S1 Check 
         Low       Ueq as Compared to Neighbors for .....         S2 Check 
         Low Bond Precision on  C-C Bonds ...............     0.0173 Ang
         Short  C(sp3)-C(sp3) Bond  C1     -   C2     ...       1.35 Ang.  


RESPONSE: there is some conformational disorder in the ethylene bridge,
          leading to these artefacts.  
;
####################################################################### 
# 
# 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_2013ncs0478_twin
_database_code_depnum_ccdc_archive 'CCDC 1051496'
_audit_update_record             
;
2015-02-27 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;
_audit_creation_date             2014-02-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4779)
;
_shelxl_version_number           2012-9
_chemical_name_common            ?
_chemical_name_systematic        
;
(Allyloxymethyl_BEDT-TTF) diperchlorate
;
_chemical_formula_moiety         '2(Cl O4), C14 H14 O S8'
_chemical_formula_sum            'C14 H14 Cl2 O9 S8'
_chemical_formula_weight         653.63
_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 0.0030 0.0010 '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'
Cl Cl 0.1420 0.1510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1180 0.1170 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   5.9156(4)
_cell_length_b                   9.5177(7)
_cell_length_c                   21.3112(16)
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 97.871(4)
_cell_angle_gamma                90.000(3)
_cell_volume                     1188.58(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11257
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_av_unetI/netI     0.031
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11232
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.203
_diffrn_reflns_theta_min         2.275
_diffrn_reflns_transf_matrix_11  -0.139118
_diffrn_reflns_transf_matrix_12  -0.043472
_diffrn_reflns_transf_matrix_13  -0.088763
_diffrn_reflns_transf_matrix_21  0.060506
_diffrn_reflns_transf_matrix_22  -0.027418
_diffrn_reflns_transf_matrix_23  -0.081403
_diffrn_reflns_transf_matrix_31  -0.002397
_diffrn_reflns_transf_matrix_32  -0.045345
_diffrn_reflns_transf_matrix_33  0.013492
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
scan:
	Number of images: 175
	           Slice: -60.0000 - 115.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 59.6396
	          2theta: 30.1352
scan:
	Number of images: 120
	           Slice: -60.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -50.0000
	             Phi: 0.0000
	             XTD: 59.6396
	          2theta: 30.1352
scan:
	Number of images: 120
	           Slice: -60.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -50.0000
	             Phi: 120.0000
	             XTD: 59.6396
	          2theta: 30.1352
scan:
	Number of images: 120
	           Slice: -60.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -50.0000
	             Phi: 240.0000
	             XTD: 59.6396
	          2theta: 30.1352
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.139118
_diffrn_orient_matrix_UB_12      -0.043472
_diffrn_orient_matrix_UB_13      -0.088763
_diffrn_orient_matrix_UB_21      0.060506
_diffrn_orient_matrix_UB_22      -0.027418
_diffrn_orient_matrix_UB_23      -0.081403
_diffrn_orient_matrix_UB_31      -0.002397
_diffrn_orient_matrix_UB_32      -0.045345
_diffrn_orient_matrix_UB_33      0.013492
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.875
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                8296
_reflns_number_total             9058
_reflns_special_details          
;
 _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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 
;
 Flack x determined using 1551 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.14(15)
_chemical_absolute_configuration ad
# the material is racemic 
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0792
_refine_ls_restrained_S_all      1.031
_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/[σ²(Fo²)+(0.1586P)²+3.0982P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2091
_refine_ls_wR_factor_ref         0.2176
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C13-C14
 1.5 with sigma of 0.02
 C14-C15
 1.316 with sigma of 0.02
 C11-O12 = C11A-O12
 1.4 with sigma of 0.02
 O12-C13 = C11-O12 = C11A-O12
 1.416 with sigma of 0.02
 C9A-C10A \\sim C9-C10
 with sigma of 0.02
 C11-C10 \\sim C11A-C9A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Uiso(C11A)=Uiso(C11)=FVAR(1)
 Fixed Sof: C9(0.5) H9A(0.5) H9B(0.5) C9A(0.5) H9AA(0.5) C10(0.5) H10(0.5)
 C10A(0.5) H10A(0.5) H10B(0.5) C11A(0.5) H11A(0.5) H11B(0.5) C11(0.5) H11C(0.5)
 H11D(0.5)
5.a Ternary CH refined with riding coordinates:
 C9A(H9AA), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10A(H10A,H10B), C11A(H11A,H11B),
 C11(H11C,H11D), C13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14)
5.d X=CH2 refined with riding coordinates:
 C15(H15A,H15B)
;
_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
Cl1 Cl 0.3895(8) 0.5927(4) 0.4204(2) 0.0354(10) Uani 1 1 d . . . . .
Cl2 Cl 0.8457(11) 0.2401(5) 0.1703(2) 0.0460(13) Uani 1 1 d . . . . .
S1 S 0.6626(10) -0.0553(4) 0.3846(2) 0.0414(13) Uani 1 1 d . . . . .
S2 S 1.1568(9) 0.1476(4) 0.4373(2) 0.0389(12) Uani 1 1 d . . . . .
S3 S 0.5153(9) 0.2028(5) 0.3142(2) 0.0395(12) Uani 1 1 d . . . . .
S4 S 0.9153(9) 0.3660(4) 0.3582(2) 0.0350(11) Uani 1 1 d . . . . .
S5 S 0.3089(10) 0.4656(4) 0.2283(2) 0.0419(13) Uani 1 1 d . . . . .
S6 S 0.6984(9) 0.6326(4) 0.2763(2) 0.0386(12) Uani 1 1 d . . . . .
S7 S 0.0610(10) 0.6903(5) 0.1511(3) 0.0505(15) Uani 1 1 d . . . . .
S8 S 0.5482(11) 0.8931(5) 0.2087(3) 0.0529(16) Uani 1 1 d . . . . .
O1 O 0.620(2) 0.6202(14) 0.4182(6) 0.040(3) Uani 1 1 d . . . . .
O2 O 0.361(3) 0.4412(13) 0.4285(7) 0.045(3) Uani 1 1 d . . . . .
O3 O 0.319(3) 0.6648(15) 0.4732(6) 0.045(3) Uani 1 1 d . . . . .
O4 O 0.250(3) 0.6381(15) 0.3626(7) 0.047(3) Uani 1 1 d . . . . .
O5 O 0.614(3) 0.1983(18) 0.1706(8) 0.065(4) Uani 1 1 d . . . . .
O6 O 0.923(5) 0.185(2) 0.1147(8) 0.085(6) Uani 1 1 d . . . . .
O7 O 0.983(3) 0.1902(16) 0.2273(7) 0.053(4) Uani 1 1 d . . . . .
O8 O 0.851(3) 0.3932(14) 0.1699(8) 0.052(4) Uani 1 1 d . . . . .
C1 C 0.950(4) -0.1157(19) 0.4135(11) 0.045(5) Uani 1 1 d . . . . .
H1A H 0.9399 -0.2108 0.4318 0.054 Uiso 1 1 calc R . . . .
H1B H 1.0365 -0.1238 0.3771 0.054 Uiso 1 1 calc R . . . .
C2 C 1.079(4) -0.023(2) 0.4621(11) 0.051(6) Uani 1 1 d . . . . .
H2A H 1.2206 -0.0730 0.4796 0.061 Uiso 1 1 calc R . . . .
H2B H 0.9866 -0.0113 0.4970 0.061 Uiso 1 1 calc R . . . .
C3 C 0.723(3) 0.1196(17) 0.3656(9) 0.037(4) Uani 1 1 d . . . . .
C4 C 0.917(4) 0.1962(18) 0.3858(8) 0.035(4) Uani 1 1 d . . . . .
C5 C 0.652(3) 0.3568(18) 0.3131(8) 0.034(4) Uani 1 1 d . . . . .
C6 C 0.563(4) 0.4752(17) 0.2754(8) 0.034(4) Uani 1 1 d . . . . .
C7 C 0.305(4) 0.640(2) 0.2028(9) 0.039(4) Uani 1 1 d . . . . .
C8 C 0.494(4) 0.7181(19) 0.2247(8) 0.038(4) Uani 1 1 d . . . . .
C9 C 0.094(8) 0.883(4) 0.152(2) 0.046(10) Uani 0.5 1 d . . P A 1
H9A H -0.0204 0.9261 0.1198 0.056 Uiso 0.5 1 calc R . P A 1
H9B H 0.0716 0.9203 0.1943 0.056 Uiso 0.5 1 calc R . P A 1
C9A C 0.144(8) 0.865(4) 0.120(2) 0.043(11) Uani 0.5 1 d . . P A 2
H9AA H 0.0021 0.9196 0.1065 0.051 Uiso 0.5 1 calc R . P A 2
C10 C 0.333(8) 0.915(5) 0.139(2) 0.051(10) Uani 0.5 1 d . . P A 1
H10 H 0.3258 1.0194 0.1353 0.061 Uiso 0.5 1 calc R . P A 1
C10A C 0.293(12) 0.949(5) 0.170(3) 0.072(16) Uani 0.5 1 d . . P A 2
H10A H 0.1967 0.9710 0.2038 0.087 Uiso 0.5 1 calc R . P A 2
H10B H 0.3228 1.0401 0.1504 0.087 Uiso 0.5 1 calc R . P A 2
C11A C 0.267(13) 0.845(5) 0.065(3) 0.089(13) Uiso 0.5 1 d D . P A 2
H11A H 0.4168 0.7992 0.0781 0.106 Uiso 0.5 1 calc R . P A 2
H11B H 0.1768 0.7856 0.0327 0.106 Uiso 0.5 1 calc R . P A 2
C11 C 0.433(12) 0.880(7) 0.081(2) 0.089(13) Uiso 0.5 1 d D . P A 1
H11C H 0.5984 0.9006 0.0855 0.106 Uiso 0.5 1 calc R . P A 1
H11D H 0.4034 0.7817 0.0673 0.106 Uiso 0.5 1 calc R . P A 1
C13 C 0.390(7) 0.991(5) -0.0159(17) 0.105(12) Uiso 1 1 d D . . . .
H13A H 0.3246 1.0754 -0.0388 0.126 Uiso 1 1 calc R . . . .
H13B H 0.3390 0.9083 -0.0423 0.126 Uiso 1 1 calc R . . . .
O12 O 0.297(7) 0.981(4) 0.0413(16) 0.153(12) Uiso 1 1 d D . . . .
C14 C 0.634(10) 1.000(10) -0.011(4) 0.22(3) Uiso 1 1 d D . . . .
H14 H 0.7139 1.0713 0.0143 0.270 Uiso 1 1 calc R . . . .
C15 C 0.743(13) 0.910(7) -0.039(3) 0.16(2) Uiso 1 1 d D . . . .
H15A H 0.6634 0.8385 -0.0643 0.193 Uiso 1 1 calc R . . . .
H15B H 0.9051 0.9155 -0.0360 0.193 Uiso 1 1 calc R . . . .


_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
Cl1 O1 1.398(16) . ?
Cl1 O2 1.465(13) . ?
Cl1 O3 1.429(16) . ?
Cl1 O4 1.450(14) . ?
Cl2 O5 1.43(2) . ?
Cl2 O6 1.43(2) . ?
Cl2 O7 1.448(15) . ?
Cl2 O8 1.457(14) . ?
S1 C1 1.82(2) . ?
S1 C3 1.761(18) . ?
S2 C2 1.79(2) . ?
S2 C4 1.733(19) . ?
S3 C3 1.724(17) . ?
S3 C5 1.676(18) . ?
S4 C4 1.719(17) . ?
S4 C5 1.714(19) . ?
S5 C6 1.69(2) . ?
S5 C7 1.744(19) . ?
S6 C6 1.699(18) . ?
S6 C8 1.721(18) . ?
S7 C7 1.76(2) . ?
S7 C9 1.84(4) . ?
S7 C9A 1.88(4) . ?
S8 C8 1.739(18) . ?
S8 C10 1.84(4) . ?
S8 C10A 1.70(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.49(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.38(3) . ?
C5 C6 1.444(19) . ?
C7 C8 1.37(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.51(5) . ?
C9A H9AA 1.0000 . ?
C9A C10A 1.52(5) . ?
C9A C11A 1.48(6) . ?
C10 H10 1.0000 . ?
C10 C11 1.47(6) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A O12 1.41(3) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C11 O12 1.45(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 O12 1.41(3) . ?
C13 C14 1.44(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.28(4) . ?
C15 H15A 0.9500 . ?
C15 H15B 0.9500 . ?

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 Cl1 O2 108.6(9) . . ?
O1 Cl1 O3 109.2(9) . . ?
O1 Cl1 O4 111.1(9) . . ?
O3 Cl1 O2 109.1(9) . . ?
O3 Cl1 O4 109.4(9) . . ?
O4 Cl1 O2 109.4(8) . . ?
O5 Cl2 O7 109.5(11) . . ?
O5 Cl2 O8 107.4(11) . . ?
O6 Cl2 O5 108.7(14) . . ?
O6 Cl2 O7 111.7(12) . . ?
O6 Cl2 O8 110.6(12) . . ?
O7 Cl2 O8 108.8(9) . . ?
C3 S1 C1 99.6(9) . . ?
C4 S2 C2 102.0(10) . . ?
C5 S3 C3 96.1(9) . . ?
C5 S4 C4 96.1(9) . . ?
C6 S5 C7 96.1(9) . . ?
C6 S6 C8 96.9(9) . . ?
C7 S7 C9 100.8(15) . . ?
C7 S7 C9A 103.2(15) . . ?
C8 S8 C10 98.1(16) . . ?
C10A S8 C8 103(2) . . ?
S1 C1 H1A 108.6 . . ?
S1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 S1 114.6(17) . . ?
C2 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
S2 C2 H2A 107.9 . . ?
S2 C2 H2B 107.9 . . ?
C1 C2 S2 117.5(15) . . ?
C1 C2 H2A 107.9 . . ?
C1 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
S3 C3 S1 115.5(11) . . ?
C4 C3 S1 128.0(13) . . ?
C4 C3 S3 116.5(12) . . ?
S4 C4 S2 115.7(11) . . ?
C3 C4 S2 129.1(13) . . ?
C3 C4 S4 115.2(13) . . ?
S3 C5 S4 116.2(10) . . ?
C6 C5 S3 123.2(12) . . ?
C6 C5 S4 120.6(12) . . ?
S5 C6 S6 115.8(10) . . ?
C5 C6 S5 121.2(12) . . ?
C5 C6 S6 123.0(13) . . ?
S5 C7 S7 115.5(11) . . ?
C8 C7 S5 115.8(14) . . ?
C8 C7 S7 128.8(14) . . ?
S6 C8 S8 116.5(12) . . ?
C7 C8 S6 115.4(13) . . ?
C7 C8 S8 128.1(14) . . ?
S7 C9 H9A 110.3 . . ?
S7 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
C10 C9 S7 107(3) . . ?
C10 C9 H9A 110.3 . . ?
C10 C9 H9B 110.3 . . ?
S7 C9A H9AA 108.4 . . ?
C10A C9A S7 112(3) . . ?
C10A C9A H9AA 108.4 . . ?
C11A C9A S7 110(3) . . ?
C11A C9A H9AA 108.4 . . ?
C11A C9A C10A 109(5) . . ?
S8 C10 H10 100.6 . . ?
C9 C10 S8 112(3) . . ?
C9 C10 H10 100.6 . . ?
C11 C10 S8 110(3) . . ?
C11 C10 C9 128(5) . . ?
C11 C10 H10 100.6 . . ?
S8 C10A H10A 106.3 . . ?
S8 C10A H10B 106.3 . . ?
C9A C10A S8 124(4) . . ?
C9A C10A H10A 106.3 . . ?
C9A C10A H10B 106.3 . . ?
H10A C10A H10B 106.4 . . ?
C9A C11A H11A 110.6 . . ?
C9A C11A H11B 110.6 . . ?
H11A C11A H11B 108.8 . . ?
O12 C11A C9A 105(4) . . ?
O12 C11A H11A 110.6 . . ?
O12 C11A H11B 110.6 . . ?
C10 C11 H11C 112.8 . . ?
C10 C11 H11D 112.8 . . ?
H11C C11 H11D 110.2 . . ?
O12 C11 C10 95(4) . . ?
O12 C11 H11C 112.8 . . ?
O12 C11 H11D 112.8 . . ?
H13A C13 H13B 107.4 . . ?
O12 C13 H13A 108.2 . . ?
O12 C13 H13B 108.2 . . ?
O12 C13 C14 116(5) . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
C13 O12 C11A 117(4) . . ?
C13 O12 C11 108(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 120(8) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15A 120.0 . . ?
C14 C15 H15B 120.0 . . ?
H15A C15 H15B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S2 -67(2) . . . . ?
S1 C3 C4 S2 -2(3) . . . . ?
S1 C3 C4 S4 -179.2(13) . . . . ?
S3 C3 C4 S2 179.4(12) . . . . ?
S3 C3 C4 S4 2(2) . . . . ?
S3 C5 C6 S5 -1(2) . . . . ?
S3 C5 C6 S6 178.0(13) . . . . ?
S4 C5 C6 S5 177.4(13) . . . . ?
S4 C5 C6 S6 -4(2) . . . . ?
S5 C7 C8 S6 -2(2) . . . . ?
S5 C7 C8 S8 179.6(13) . . . . ?
S7 C7 C8 S6 178.9(13) . . . . ?
S7 C7 C8 S8 1(3) . . . . ?
S7 C9 C10 S8 -80(4) . . . . ?
S7 C9 C10 C11 61(5) . . . . ?
S7 C9A C10A S8 59(7) . . . . ?
S7 C9A C11A O12 173(4) . . . . ?
S8 C10 C11 O12 -147(4) . . . . ?
C1 S1 C3 S3 160.8(13) . . . . ?
C1 S1 C3 C4 -18(2) . . . . ?
C2 S2 C4 S4 173.2(13) . . . . ?
C2 S2 C4 C3 -4(2) . . . . ?
C3 S1 C1 C2 50.5(19) . . . . ?
C3 S3 C5 S4 0.5(14) . . . . ?
C3 S3 C5 C6 178.5(15) . . . . ?
C4 S2 C2 C1 39(2) . . . . ?
C4 S4 C5 S3 0.5(14) . . . . ?
C4 S4 C5 C6 -177.6(15) . . . . ?
C5 S3 C3 S1 179.6(13) . . . . ?
C5 S3 C3 C4 -1.7(19) . . . . ?
C5 S4 C4 S2 -179.2(12) . . . . ?
C5 S4 C4 C3 -1.7(17) . . . . ?
C6 S5 C7 S7 -178.6(13) . . . . ?
C6 S5 C7 C8 2.5(18) . . . . ?
C6 S6 C8 S8 179.2(13) . . . . ?
C6 S6 C8 C7 1.1(18) . . . . ?
C7 S5 C6 S6 -1.8(14) . . . . ?
C7 S5 C6 C5 176.9(15) . . . . ?
C7 S7 C9 C10 51(3) . . . . ?
C7 S7 C9A C10A -36(5) . . . . ?
C7 S7 C9A C11A 86(4) . . . . ?
C8 S6 C6 S5 0.7(14) . . . . ?
C8 S6 C6 C5 -177.9(16) . . . . ?
C8 S8 C10 C9 58(4) . . . . ?
C8 S8 C10 C11 -90(4) . . . . ?
C8 S8 C10A C9A -42(6) . . . . ?
C9 S7 C7 S5 166.9(19) . . . . ?
C9 S7 C7 C8 -14(3) . . . . ?
C9 S7 C9A C10A 51(5) . . . . ?
C9 S7 C9A C11A 173(7) . . . . ?
C9 C10 C11 O12 70(6) . . . . ?
C9A S7 C7 S5 -167.9(18) . . . . ?
C9A S7 C7 C8 11(3) . . . . ?
C9A S7 C9 C10 -47(4) . . . . ?
C9A C11A O12 C11 99(6) . . . . ?
C9A C11A O12 C13 -174(4) . . . . ?
C10 S8 C8 S6 165.2(19) . . . . ?
C10 S8 C8 C7 -17(3) . . . . ?
C10 S8 C10A C9A 40(4) . . . . ?
C10 C11 O12 C11A -80(5) . . . . ?
C10 C11 O12 C13 168(4) . . . . ?
C10A S8 C8 S6 -168(3) . . . . ?
C10A S8 C8 C7 9(3) . . . . ?
C10A S8 C10 C9 -45(5) . . . . ?
C10A S8 C10 C11 167(8) . . . . ?
C10A C9A C11A O12 -63(6) . . . . ?
C11A C9A C10A S8 -64(7) . . . . ?
O12 C13 C14 C15 124(7) . . . . ?
C14 C13 O12 C11A -89(8) . . . . ?
C14 C13 O12 C11 -44(8) . . . . ?
_vrf_PLAT019_2013ncs0478_twin    
;
PROBLEM: diffrn_measured_fraction_theta_full/_max < 1.0 0.976 Report          

RESPONSE: 0.991 fraction measured at theta_max.
;
_vrf_PLAT021_2013ncs0478_twin    
;
PROBLEM: Ratio Unique/Expected Reflections too High 4.060          

RESPONSE: due to twinning and use of HLKF5 in SHELXL
;
_vrf_PLAT201_2013ncs0478_twin    
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 4 Report          

RESPONSE: disordered model with two points of attachment of sidechain.
	   side chain atoms refined isotropically.
;
_vrf_PLAT220_2013ncs0478_twin    
;
PROBLEM:Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        6.5 Ratio 
          

RESPONSE:  disordered model and a twinned crystal.
;
