# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_ncb05_recupero
_database_code_depnum_ccdc_archive 'CCDC 1033185'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'C6_Nt$n_Form A'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H32 N2 O4 S4'
_chemical_formula_weight         636.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.6152(7)
_cell_length_b                   11.558(1)
_cell_length_c                   14.422(2)
_cell_angle_alpha                80.38(1)
_cell_angle_beta                 88.11(1)
_cell_angle_gamma                86.45(1)
_cell_volume                     756.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    874
_cell_measurement_theta_min      2.8540
_cell_measurement_theta_max      21.2290

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             334
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_min  0.77584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5206
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.1449
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         28.12
_reflns_number_total             3000
_reflns_number_gt                1627
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0605P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3000
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.0890
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.1610
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C16 C -0.8234(15) 1.5386(5) -0.2158(4) 0.069(2) Uani 1 1 d . . .
H16A H -0.9578 1.5864 -0.2574 0.104 Uiso 1 1 calc R . .
H16B H -0.6935 1.4937 -0.2513 0.104 Uiso 1 1 calc R . .
H16C H -0.7138 1.5881 -0.1846 0.104 Uiso 1 1 calc R . .
S2 S 0.1948(3) 0.59708(11) 0.39872(10) 0.0403(4) Uani 1 1 d . . .
S1 S -0.2364(3) 0.93998(12) 0.42014(10) 0.0509(5) Uani 1 1 d . . .
C8 C -0.1180(11) 0.8108(4) 0.3786(4) 0.0358(13) Uani 1 1 d . . .
C6 C -0.4460(11) 0.9802(4) 0.3239(3) 0.0366(13) Uani 1 1 d . . .
C5 C -0.4317(11) 0.8999(4) 0.2658(4) 0.0370(13) Uani 1 1 d . . .
C7 C -0.2419(11) 0.7982(4) 0.2930(4) 0.0365(13) Uani 1 1 d . . .
H7 H -0.2068 0.7356 0.2604 0.044 Uiso 1 1 calc R . .
O1 O -0.7113(9) 1.1699(3) 0.3181(3) 0.0650(13) Uani 1 1 d . . .
C4 C 0.0869(12) 0.7294(4) 0.4348(4) 0.0364(13) Uani 1 1 d . . .
C1 C 0.4188(11) 0.5568(4) 0.4941(3) 0.0331(12) Uani 1 1 d . . .
C3 C 0.2188(12) 0.7383(4) 0.5158(4) 0.0420(14) Uani 1 1 d . . .
H3 H 0.1860 0.8025 0.5467 0.050 Uiso 1 1 calc R . .
C2 C 0.4090(12) 0.6419(4) 0.5486(4) 0.0408(14) Uani 1 1 d . . .
H2 H 0.5177 0.6369 0.6024 0.049 Uiso 1 1 calc R . .
C9 C -0.6231(13) 0.9446(5) 0.1847(4) 0.0462(15) Uani 1 1 d . . .
N1 N -0.7450(10) 1.0528(4) 0.2039(3) 0.0433(12) Uani 1 1 d . . .
C13 C -0.9610(12) 1.2921(4) -0.0024(4) 0.0438(14) Uani 1 1 d . . .
H13A H -1.0682 1.2425 -0.0354 0.053 Uiso 1 1 calc R . .
H13B H -1.1008 1.3372 0.0309 0.053 Uiso 1 1 calc R . .
C15 C -0.9883(14) 1.4563(5) -0.1434(4) 0.0532(17) Uani 1 1 d . . .
H15A H -1.1026 1.4083 -0.1758 0.064 Uiso 1 1 calc R . .
H15B H -1.1221 1.5025 -0.1090 0.064 Uiso 1 1 calc R . .
C11 C -0.9350(12) 1.1317(5) 0.1394(4) 0.0451(15) Uani 1 1 d . . .
H11A H -1.0660 1.1771 0.1754 0.054 Uiso 1 1 calc R . .
H11B H -1.0516 1.0852 0.1065 0.054 Uiso 1 1 calc R . .
C10 C -0.6432(12) 1.0818(5) 0.2871(4) 0.0422(14) Uani 1 1 d . . .
C14 C -0.7961(12) 1.3757(5) -0.0736(4) 0.0449(15) Uani 1 1 d . . .
H14A H -0.6600 1.3304 -0.1080 0.054 Uiso 1 1 calc R . .
H14B H -0.6844 1.4236 -0.0404 0.054 Uiso 1 1 calc R . .
C12 C -0.7688(12) 1.2149(5) 0.0681(4) 0.0455(15) Uani 1 1 d . . .
H12A H -0.6295 1.1696 0.0348 0.055 Uiso 1 1 calc R . .
H12B H -0.6610 1.2645 0.1010 0.055 Uiso 1 1 calc R . .
O2 O -0.6730(10) 0.9022(4) 0.1174(3) 0.0709(14) 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
C16 0.085(5) 0.066(4) 0.049(4) 0.010(3) 0.005(4) 0.004(4)
S2 0.0442(10) 0.0347(8) 0.0410(9) -0.0058(6) -0.0094(7) 0.0100(6)
S1 0.0573(12) 0.0423(9) 0.0516(10) -0.0066(8) -0.0118(8) 0.0129(8)
C8 0.035(3) 0.025(3) 0.047(3) -0.006(2) 0.003(3) 0.001(2)
C6 0.038(3) 0.035(3) 0.034(3) 0.001(3) -0.008(3) 0.004(2)
C5 0.038(3) 0.033(3) 0.040(3) -0.007(3) 0.002(3) 0.002(2)
C7 0.034(3) 0.027(3) 0.045(3) 0.004(2) -0.013(3) 0.002(2)
O1 0.078(3) 0.042(2) 0.075(3) -0.017(2) -0.014(3) 0.025(2)
C4 0.037(3) 0.031(3) 0.040(3) -0.003(2) 0.000(3) 0.003(2)
C1 0.034(3) 0.031(3) 0.032(3) 0.001(2) -0.001(2) 0.000(2)
C3 0.053(4) 0.030(3) 0.044(4) -0.012(3) -0.009(3) 0.009(3)
C2 0.045(4) 0.040(3) 0.035(3) 0.001(3) -0.010(3) 0.006(3)
C9 0.044(4) 0.040(3) 0.053(4) -0.003(3) -0.008(3) 0.000(3)
N1 0.049(3) 0.037(3) 0.041(3) 0.002(2) -0.008(2) 0.005(2)
C13 0.042(4) 0.048(3) 0.041(3) -0.005(3) -0.008(3) -0.002(3)
C15 0.066(5) 0.052(4) 0.039(4) -0.002(3) -0.004(3) 0.003(3)
C11 0.039(4) 0.051(3) 0.041(3) 0.003(3) -0.004(3) 0.004(3)
C10 0.043(4) 0.037(3) 0.044(4) -0.001(3) 0.000(3) 0.003(3)
C14 0.043(4) 0.050(3) 0.041(3) -0.005(3) -0.005(3) -0.003(3)
C12 0.041(4) 0.048(3) 0.043(3) 0.004(3) -0.010(3) 0.005(3)
O2 0.086(4) 0.069(3) 0.063(3) -0.028(3) -0.036(3) 0.014(3)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C16 C15 1.510(7) . ?
S2 C1 1.731(5) . ?
S2 C4 1.735(5) . ?
S1 C6 1.702(5) . ?
S1 C8 1.750(5) . ?
C8 C7 1.411(7) . ?
C8 C4 1.457(7) . ?
C6 C5 1.347(6) . ?
C6 C10 1.476(7) . ?
C5 C7 1.429(6) . ?
C5 C9 1.491(7) . ?
O1 C10 1.200(6) . ?
C4 C3 1.356(7) . ?
C1 C2 1.357(6) . ?
C1 C1 1.457(9) 2_666 ?
C3 C2 1.402(6) . ?
C9 O2 1.194(6) . ?
C9 N1 1.405(6) . ?
N1 C10 1.401(6) . ?
N1 C11 1.462(6) . ?
C13 C14 1.508(7) . ?
C13 C12 1.509(6) . ?
C15 C14 1.521(7) . ?
C11 C12 1.509(7) . ?

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
C1 S2 C4 91.8(2) . . ?
C6 S1 C8 89.8(3) . . ?
C7 C8 C4 127.7(4) . . ?
C7 C8 S1 114.0(4) . . ?
C4 C8 S1 118.2(4) . . ?
C5 C6 C10 110.8(5) . . ?
C5 C6 S1 113.1(4) . . ?
C10 C6 S1 136.1(4) . . ?
C6 C5 C7 116.1(5) . . ?
C6 C5 C9 108.1(5) . . ?
C7 C5 C9 135.8(5) . . ?
C8 C7 C5 107.0(5) . . ?
C3 C4 C8 130.3(5) . . ?
C3 C4 S2 110.3(4) . . ?
C8 C4 S2 119.4(4) . . ?
C2 C1 C1 129.8(6) . 2_666 ?
C2 C1 S2 110.7(4) . . ?
C1 C1 S2 119.5(5) 2_666 . ?
C4 C3 C2 113.9(5) . . ?
C1 C2 C3 113.3(5) . . ?
O2 C9 N1 125.0(5) . . ?
O2 C9 C5 130.4(5) . . ?
N1 C9 C5 104.6(5) . . ?
C10 N1 C9 112.7(4) . . ?
C10 N1 C11 123.6(4) . . ?
C9 N1 C11 123.5(4) . . ?
C14 C13 C12 113.5(4) . . ?
C16 C15 C14 114.1(5) . . ?
N1 C11 C12 112.7(4) . . ?
O1 C10 N1 125.5(5) . . ?
O1 C10 C6 130.7(5) . . ?
N1 C10 C6 103.8(4) . . ?
C13 C14 C15 114.0(5) . . ?
C11 C12 C13 113.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.813
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.074
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_5296
_database_code_depnum_ccdc_archive 'CCDC 1033186'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'C3-NT4N form B high temperature'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H10 N O2 S2'
_chemical_formula_weight         276.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.265(1)
_cell_length_b                   5.473(5)
_cell_length_c                   22.49(3)
_cell_angle_alpha                87.9(1)
_cell_angle_beta                 87.40(6)
_cell_angle_gamma                87.05(6)
_cell_volume                     646.1(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1401
_cell_measurement_theta_min      3.7220
_cell_measurement_theta_max      22.2950

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             286
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_min  0.90284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5814
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         27.86
_reflns_number_total             2522
_reflns_number_gt                1594
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2522
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.1322
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0530(6) -0.0318(6) 0.02824(14) 0.0431(9) Uani 1 1 d . . .
C2 C 0.0029(7) -0.2226(6) 0.06755(17) 0.0529(10) Uani 1 1 d . . .
H2 H -0.1143 -0.3385 0.0606 0.063 Uiso 1 1 calc R . .
C3 C 0.1437(7) -0.2282(6) 0.11933(17) 0.0524(10) Uani 1 1 d . . .
H3 H 0.1277 -0.3469 0.1497 0.063 Uiso 1 1 calc R . .
C4 C 0.3056(7) -0.0429(6) 0.12053(16) 0.0458(9) Uani 1 1 d . . .
C5 C 0.4781(6) 0.0063(6) 0.16741(16) 0.0429(9) Uani 1 1 d . . .
C6 C 0.5136(7) -0.1248(6) 0.22076(16) 0.0455(9) Uani 1 1 d . . .
H6 H 0.4264 -0.2626 0.2330 0.055 Uiso 1 1 calc R . .
C7 C 0.6988(7) -0.0209(6) 0.25358(16) 0.0451(9) Uani 1 1 d . . .
C8 C 0.7991(6) 0.1821(6) 0.22703(15) 0.0437(9) Uani 1 1 d . . .
C9 C 0.9976(7) 0.2723(7) 0.26371(17) 0.0485(10) Uani 1 1 d . . .
C10 C 0.8242(7) -0.0701(7) 0.31174(17) 0.0515(10) Uani 1 1 d . . .
C11 C 1.1809(8) 0.1288(7) 0.36177(17) 0.0643(12) Uani 1 1 d . . .
H11A H 1.3255 0.2186 0.3466 0.077 Uiso 1 1 calc R . .
H11B H 1.2434 -0.0356 0.3729 0.077 Uiso 1 1 calc R . .
C12 C 1.0699(9) 0.2493(8) 0.41624(19) 0.0813(14) Uani 1 1 d . . .
H12A H 0.9346 0.1525 0.4337 0.098 Uiso 1 1 calc R . .
H12B H 0.9961 0.4095 0.4051 0.098 Uiso 1 1 calc R . .
C13 C 1.2692(10) 0.2773(10) 0.4624(2) 0.131(2) Uani 1 1 d . . .
H13A H 1.1900 0.3515 0.4970 0.196 Uiso 1 1 calc R . .
H13B H 1.3997 0.3790 0.4458 0.196 Uiso 1 1 calc R . .
H13C H 1.3434 0.1191 0.4734 0.196 Uiso 1 1 calc R . .
N1 N 1.0023(6) 0.1139(5) 0.31389(13) 0.0514(8) Uani 1 1 d . . .
O1 O 0.7898(5) -0.2283(5) 0.34956(12) 0.0727(9) Uani 1 1 d . . .
O2 O 1.1334(5) 0.4437(4) 0.25468(12) 0.0660(8) Uani 1 1 d . . .
S1 S 0.67196(18) 0.25677(16) 0.15985(4) 0.0498(3) Uani 1 1 d . . .
S2 S 0.28114(18) 0.14383(16) 0.05705(4) 0.0505(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.045(2) 0.033(2) 0.052(3) -0.0045(19) -0.0007(19) -0.0036(16)
C2 0.057(3) 0.040(2) 0.063(3) -0.003(2) -0.010(2) -0.0152(18)
C3 0.061(3) 0.041(2) 0.056(3) 0.0087(18) -0.012(2) -0.0134(19)
C4 0.043(2) 0.040(2) 0.055(3) -0.0037(18) 0.0004(19) -0.0052(17)
C5 0.038(2) 0.038(2) 0.053(3) -0.0051(18) 0.0034(19) -0.0072(16)
C6 0.051(2) 0.032(2) 0.055(3) -0.0038(18) -0.001(2) -0.0110(17)
C7 0.044(2) 0.040(2) 0.052(3) 0.0030(18) 0.0010(19) -0.0079(17)
C8 0.046(2) 0.041(2) 0.045(2) -0.0018(18) -0.0008(19) -0.0108(17)
C9 0.050(2) 0.049(2) 0.046(3) 0.0006(19) 0.0030(19) -0.0066(19)
C10 0.050(3) 0.050(3) 0.054(3) 0.005(2) 0.000(2) -0.0043(19)
C11 0.055(3) 0.077(3) 0.060(3) 0.008(2) -0.004(2) -0.007(2)
C12 0.079(3) 0.104(4) 0.060(3) -0.007(3) -0.014(3) 0.010(3)
C13 0.124(5) 0.183(6) 0.088(4) -0.039(4) -0.049(4) 0.021(4)
N1 0.050(2) 0.061(2) 0.045(2) 0.0035(16) -0.0076(16) -0.0119(16)
O1 0.086(2) 0.0636(19) 0.069(2) 0.0263(16) -0.0095(17) -0.0151(15)
O2 0.0636(18) 0.0676(19) 0.070(2) 0.0041(15) -0.0052(15) -0.0372(15)
S1 0.0533(6) 0.0466(6) 0.0507(7) 0.0047(5) -0.0032(5) -0.0173(4)
S2 0.0538(6) 0.0490(6) 0.0501(7) 0.0014(5) -0.0033(5) -0.0177(5)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.371(5) . ?
C1 C1 1.435(7) 2 ?
C1 S2 1.738(4) . ?
C2 C3 1.407(5) . ?
C3 C4 1.359(5) . ?
C4 C5 1.463(5) . ?
C4 S2 1.731(4) . ?
C5 C6 1.390(5) . ?
C5 S1 1.750(4) . ?
C6 C7 1.404(5) . ?
C7 C8 1.361(4) . ?
C7 C10 1.501(5) . ?
C8 C9 1.476(5) . ?
C8 S1 1.708(4) . ?
C9 O2 1.214(4) . ?
C9 N1 1.398(5) . ?
C10 O1 1.206(4) . ?
C10 N1 1.414(4) . ?
C11 N1 1.468(4) . ?
C11 C12 1.494(5) . ?
C12 C13 1.526(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
C2 C1 C1 129.9(4) . 2 ?
C2 C1 S2 109.1(3) . . ?
C1 C1 S2 121.1(3) 2 . ?
C1 C2 C3 114.4(3) . . ?
C4 C3 C2 113.4(3) . . ?
C3 C4 C5 127.7(3) . . ?
C3 C4 S2 110.4(3) . . ?
C5 C4 S2 121.9(3) . . ?
C6 C5 C4 128.0(3) . . ?
C6 C5 S1 111.8(3) . . ?
C4 C5 S1 120.2(3) . . ?
C5 C6 C7 110.9(3) . . ?
C8 C7 C6 114.3(3) . . ?
C8 C7 C10 107.9(3) . . ?
C6 C7 C10 137.8(3) . . ?
C7 C8 C9 110.2(3) . . ?
C7 C8 S1 112.4(3) . . ?
C9 C8 S1 137.3(3) . . ?
O2 C9 N1 125.0(4) . . ?
O2 C9 C8 130.1(4) . . ?
N1 C9 C8 104.9(3) . . ?
O1 C10 N1 125.3(4) . . ?
O1 C10 C7 130.0(4) . . ?
N1 C10 C7 104.7(3) . . ?
N1 C11 C12 114.4(3) . . ?
C11 C12 C13 112.0(4) . . ?
C9 N1 C10 112.2(3) . . ?
C9 N1 C11 123.9(3) . . ?
C10 N1 C11 123.8(3) . . ?
C8 S1 C5 90.68(19) . . ?
C4 S2 C1 92.82(18) . . ?

_diffrn_measured_fraction_theta_max 0.824
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.057
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_C4_NT4N_from_powder
_database_code_depnum_ccdc_archive 'CCDC 1033187'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;
_chemical_formula_sum            'C28 H24 N2 O4 S4'
_chemical_formula_weight         580.76
_chemical_formula_moiety         'C28 H24 N2 O4 S4 '
_chemical_name_mineral           'C4-NT4N form B'
_cell_length_a                   5.127(3)
_cell_length_b                   5.526(2)
_cell_length_c                   25.038(2)
_cell_angle_alpha                84.04(3)
_cell_angle_beta                 89.75(4)
_cell_angle_gamma                86.19(7)
_cell_volume                     704.0696
_exptl_crystal_density_diffrn    1.370
_cell_measurement_temperature    293
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_cell_formula_units_Z            1
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'x, y, z'
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      293
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_monochromator  none
_diffrn_measurement_device_type  
;
 Panalytical X'pert in Debye-Scherrer geometry
;

_pd_proc_2theta_range_min        2
_pd_proc_2theta_range_max        60

_pd_proc_info_excluded_regions   no
_pd_proc_ls_background_function  Chebyschev
_pd_proc_ls_pref_orient_corr     
;
Spherical Harmonics
;


_pd_proc_ls_prof_R_factor        0.08033
_pd_proc_ls_prof_wR_factor       0.10699
_pd_proc_ls_prof_wR_expected     0.03737
_refine_ls_R_I_factor            0.01613

_refine_ls_goodness_of_fit_all   2.863


_pd_spec_mount_mode              transmission
_pd_spec_mounting                
;
0.5 mm borosilicate glass capillary
;
_pd_spec_shape                   cylinder
_refine_ls_hydrogen_treatment    constr


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
S1 S 1 0.1872957 -0.1095802 -0.05460952 1 9.38639
C2 C 1 0.1903895 0.07891968 -0.1166177 1 4.05112
C3 C 1 0.4508849 0.03931466 -0.02842674 1 4.05112
C4 C 1 0.3845012 0.2427386 -0.1155407 1 4.05112
C5 C 1 0.01252193 0.04929827 -0.1594706 1 4.05112
C6 C 1 0.528827 0.22151 -0.06639763 1 4.05112
C9 C 1 -0.02338284 0.1877452 -0.20892 1 4.05112
S10 S 1 -0.1896129 -0.2037684 -0.1528284 1 9.38639
C15 C 1 -0.2142259 0.09133569 -0.2403713 1 4.05112
C16 C 1 -0.3163902 -0.1154344 -0.2160906 1 4.05112
C20 C 1 -0.3634461 0.1616899 -0.2916508 1 4.05112
O24 O 1 -0.3426216 0.3401714 -0.3243608 1 4.05112
N25 N 1 -0.5466992 -0.01688183 -0.2947803 1 4.05112
C21 C 1 -0.5323168 -0.1886148 -0.2486314 1 4.05112
O26 O 1 -0.6805067 -0.352373 -0.2383547 1 4.05112
C29 C 1 -0.6999146 -0.05252146 -0.3432813 1 4.05112
C35 C 1 -0.7357493 -0.3195675 -0.3524385 1 4.05112
C40 C 1 -0.8547242 -0.3265047 -0.4091094 1 4.05112
C46 C 1 -0.6934525 -0.1881524 -0.4533793 1 4.05112
H6 H 1 0.6629397 0.3208056 -0.0603797 1 4.861344
H4 H 1 0.4175393 0.3565361 -0.1443954 1 4.861344
H9 H 1 0.06576514 0.3253319 -0.2199583 1 4.861344
H29A H 1 -0.6115646 0.02296081 -0.3744021 1 4.861344
H29B H 1 -0.8720041 0.02885617 -0.3401632 1 4.861344
H35A H 1 -0.5676387 -0.4115424 -0.3500028 1 4.861344
H35B H 1 -0.8372219 -0.3954224 -0.3232987 1 4.861344
H40A H 1 -0.8588558 -0.4950958 -0.4164818 1 4.861344
H40B H 1 -1.031421 -0.2517516 -0.4096598 1 4.861344
H46A H 1 -0.5165879 -0.2623301 -0.4532937 1 4.861344
H46B H 1 -0.7735781 -0.1964858 -0.4881069 1 4.861344
H46C H 1 -0.6891566 -0.01896523 -0.446472 1 4.861344
# start Validation Reply Form
_vrf_GEOM001_C4_NT4N_from_powder 
;
PROBLEM: _geom_bond_atom_site_label_1 is missing
RESPONSE:geometry details are not insert in CIF by TOPAS
;
_vrf_GEOM003_C4_NT4N_from_powder 
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: geometry details are not insert in CIF by TOPAS
;
_vrf_GEOM006_C4_NT4N_from_powder 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: geometry details are not insert in CIF by TOPAS
;
_vrf_GEOM007_C4_NT4N_from_powder 
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: geometry details are not insert in CIF by TOPAS
;

_chemical_name_common            'C4_NT4N form B'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ncb13_chcl3_vd_f_lu
_database_code_depnum_ccdc_archive 'CCDC 1033188'
_audit_update_record             
;
2014-11-07 deposited with the CCDC.
2014-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            C5-NT4N
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 N2 O4 S4'
_chemical_formula_weight         608.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.289(2)
_cell_length_b                   5.474(2)
_cell_length_c                   25.81(2)
_cell_angle_alpha                85.15(5)
_cell_angle_beta                 84.36(4)
_cell_angle_gamma                87.27(3)
_cell_volume                     740.1(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    166
_cell_measurement_theta_min      3.1775
_cell_measurement_theta_max      26.5837

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             318
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1671
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.3812
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.1775
_diffrn_reflns_theta_max         26.5837
_reflns_number_total             1406
_reflns_number_gt                385
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1608P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1406
_refine_ls_number_parameters     91
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.3652
_refine_ls_R_factor_gt           0.1390
_refine_ls_wR_factor_ref         0.4279
_refine_ls_wR_factor_gt          0.2936
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.3110(12) 0.1699(13) 0.9494(3) 0.069(3) Uani 1 1 d . . .
S2 S 0.7664(14) 0.3231(14) 0.8615(3) 0.087(4) Uani 1 1 d . . .
C1 C 0.064(4) -0.025(4) 0.9740(8) 0.054(6) Uiso 1 1 d . . .
O2 O 1.273(3) 0.553(3) 0.7787(7) 0.088(6) Uiso 1 1 d . . .
O1 O 0.996(3) -0.068(4) 0.6963(7) 0.101(6) Uiso 1 1 d . . .
C2 C 0.051(5) -0.191(5) 0.9407(10) 0.077(7) Uiso 1 1 d . . .
H2 H -0.0653 -0.3146 0.9468 0.092 Uiso 1 1 calc R . .
C11 C 1.394(5) 0.290(5) 0.6863(10) 0.084(8) Uiso 1 1 d . . .
H11A H 1.5306 0.3725 0.6994 0.101 Uiso 1 1 calc R . .
H11B H 1.4612 0.1312 0.6760 0.101 Uiso 1 1 calc R . .
C3 C 0.210(4) -0.174(5) 0.8983(10) 0.078(8) Uiso 1 1 d . . .
H3 H 0.2078 -0.2784 0.8717 0.094 Uiso 1 1 calc R . .
C4 C 0.377(4) 0.007(5) 0.8963(9) 0.060(6) Uiso 1 1 d . . .
C10 C 0.923(4) 0.275(4) 0.8032(9) 0.055(6) Uiso 1 1 d . . .
C5 C 0.576(4) 0.073(5) 0.8542(9) 0.060(6) Uiso 1 1 d . . .
C6 C 0.634(3) -0.029(4) 0.8076(8) 0.043(6) Uiso 1 1 d . . .
H6 H 0.5471 -0.1566 0.7967 0.052 Uiso 1 1 calc R . .
N1 N 1.185(3) 0.256(4) 0.7275(7) 0.064(5) Uiso 1 1 d . . .
C9 C 1.141(5) 0.391(6) 0.7689(11) 0.088(9) Uiso 1 1 d . . .
C7 C 0.847(4) 0.088(4) 0.7776(9) 0.065(7) Uiso 1 1 d . . .
C8 C 1.004(5) 0.070(6) 0.7291(12) 0.091(9) Uiso 1 1 d . . .
C12 C 1.303(5) 0.437(6) 0.6407(12) 0.116(10) Uiso 1 1 d . . .
H12A H 1.2188 0.5900 0.6506 0.139 Uiso 1 1 calc R . .
H12B H 1.1872 0.3469 0.6233 0.139 Uiso 1 1 calc R . .
C15 C 1.773(9) 0.818(9) 0.5395(18) 0.24(2) Uiso 1 1 d . . .
H15A H 1.8310 0.9742 0.5465 0.366 Uiso 1 1 calc R . .
H15B H 1.7157 0.8290 0.5051 0.366 Uiso 1 1 calc R . .
H15C H 1.9105 0.6967 0.5415 0.366 Uiso 1 1 calc R . .
C13 C 1.549(9) 0.483(9) 0.6062(18) 0.23(2) Uiso 1 1 d D . .
H13A H 1.5691 0.3671 0.5795 0.271 Uiso 1 1 calc R . .
H13B H 1.6919 0.4556 0.6273 0.271 Uiso 1 1 calc R . .
C14 C 1.555(11) 0.743(9) 0.580(2) 0.28(3) Uiso 1 1 d D . .
H14A H 1.5486 0.8547 0.6072 0.339 Uiso 1 1 calc R . .
H14B H 1.3985 0.7735 0.5629 0.339 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.079(4) 0.038(5) 0.091(5) 0.006(5) -0.007(4) -0.023(4)
S2 0.091(5) 0.066(7) 0.106(6) -0.008(6) -0.005(5) -0.027(5)

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C4 1.695(19) . ?
S1 C1 1.76(2) . ?
S2 C10 1.68(2) . ?
S2 C5 1.77(2) . ?
C1 C2 1.31(2) . ?
C1 C1 1.49(4) 2_557 ?
O2 C9 1.22(2) . ?
O1 C8 1.19(2) . ?
C2 C3 1.31(3) . ?
C11 C12 1.47(4) . ?
C11 N1 1.47(3) . ?
C3 C4 1.36(3) . ?
C4 C5 1.47(3) . ?
C10 C7 1.36(2) . ?
C10 C9 1.51(3) . ?
C5 C6 1.37(2) . ?
C6 C7 1.45(3) . ?
N1 C9 1.34(2) . ?
N1 C8 1.42(3) . ?
C7 C8 1.44(3) . ?
C12 C13 1.52(5) . ?
C15 C14 1.52(6) . ?
C13 C14 1.52(2) . ?

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
C4 S1 C1 91.2(10) . . ?
C10 S2 C5 88.5(10) . . ?
C2 C1 C1 136(3) . 2_557 ?
C2 C1 S1 108.0(15) . . ?
C1 C1 S1 116.1(19) 2_557 . ?
C3 C2 C1 117(2) . . ?
C12 C11 N1 110(2) . . ?
C2 C3 C4 115(2) . . ?
C3 C4 C5 127.6(19) . . ?
C3 C4 S1 109.3(16) . . ?
C5 C4 S1 123.0(16) . . ?
C7 C10 C9 106.9(17) . . ?
C7 C10 S2 117.1(15) . . ?
C9 C10 S2 136.0(16) . . ?
C6 C5 C4 128.7(18) . . ?
C6 C5 S2 113.1(16) . . ?
C4 C5 S2 118.1(14) . . ?
C5 C6 C7 111.0(17) . . ?
C9 N1 C8 111(2) . . ?
C9 N1 C11 125(2) . . ?
C8 N1 C11 123.7(19) . . ?
O2 C9 N1 125(2) . . ?
O2 C9 C10 128(2) . . ?
N1 C9 C10 106(2) . . ?
C10 C7 C8 109.5(19) . . ?
C10 C7 C6 110.1(16) . . ?
C8 C7 C6 140(2) . . ?
O1 C8 N1 125(3) . . ?
O1 C8 C7 130(3) . . ?
N1 C8 C7 106(2) . . ?
C11 C12 C13 102(3) . . ?
C12 C13 C14 112(4) . . ?
C13 C14 C15 120(5) . . ?

_diffrn_measured_fraction_theta_max 0.452
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.524
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.076

# start Validation Reply Form
_vrf_RFACG01_ncb13_chcl3_vd_f_lu 
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: Not enough data to converge a better R value
;
_vrf_PLAT026_ncb13_chcl3_vd_f_lu 
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         27 %     
RESPONSE:  small crystal hardly diffracts above 2teta>30 deg 
;
_vrf_PLAT029_ncb13_chcl3_vd_f_lu 
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.524 Note  
RESPONSE: small crystal hardly diffracts above 2teta>30 deg
;
_vrf_PLAT201_ncb13_chcl3_vd_f_lu 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         18 Report
RESPONSE: Not enought reflections to describe C, N, O anisotropically
;
_exptl_crystal_preparation       Luminescent
