# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1030582'
_audit_update_record             
;
2015-04-28 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_date             2015-04-21T12:48:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C16 H10 N4 O4, 2(C2 H6 O S)'
_chemical_formula_sum            'C20 H22 N4 O6 S2'
_chemical_formula_weight         478.56
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.315(4)
_cell_length_b                   7.088(4)
_cell_length_c                   20.776(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.069(18)
_cell_angle_gamma                90
_cell_volume                     1077.3(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    344
_cell_measurement_theta_min      4
_cell_measurement_theta_max      17.95
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             500

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER TWINABS'
_exptl_absorpt_correction_T_min  0.7641
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.907
_shelx_estimated_absorpt_T_max   0.994

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_number            4536
_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       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         0.98
_diffrn_reflns_theta_max         19.774
_diffrn_reflns_theta_full        19.774
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_number_total             974
_reflns_number_gt                752
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0932P)²+0.1030P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         974
_refine_ls_number_parameters     151
_refine_ls_number_restraints     18
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1379
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.01
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.082

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.2685(9) 0.6583(9) 0.8827(3) 0.0260(18) Uani 1 d . .
H1O H 1.316(12) 0.771(12) 0.869(4) 0.031 Uiso 1 d . .
O2 O 1.0362(9) 0.8400(9) 0.8494(3) 0.0283(18) Uani 1 d . .
C1 C 1.0909(14) 0.6950(16) 0.8761(5) 0.022(3) Uani 1 d . .
C2 C 0.9732(14) 0.5523(12) 0.9043(4) 0.018(2) Uani 1 d . .
C3 C 1.0368(14) 0.3804(13) 0.9266(4) 0.027(3) Uani 1 d . .
H3 H 1.1646 0.3564 0.9255 0.033 Uiso 1 calc . .
C4 C 0.9211(13) 0.2408(14) 0.9506(4) 0.025(3) Uani 1 d . .
H4 H 0.9697 0.1238 0.965 0.03 Uiso 1 calc . .
C5 C 0.7303(13) 0.2750(13) 0.9534(4) 0.024(3) Uani 1 d . .
C6 C 0.6645(13) 0.4507(13) 0.9327(4) 0.022(3) Uani 1 d . .
H6 H 0.5378 0.4784 0.9361 0.026 Uiso 1 calc . .
C7 C 0.7819(14) 0.5833(13) 0.9076(4) 0.024(3) Uani 1 d . .
H7 H 0.7335 0.699 0.8921 0.029 Uiso 1 calc . .
C8 C 0.6081(15) 0.1315(14) 0.9778(4) 0.018(3) Uani 1 d . .
N1 N 0.4274(12) 0.1574(11) 0.9735(4) 0.025(2) Uani 1 d . .
N2 N 0.3158(10) 0.0252(12) 0.9953(4) 0.0230(19) Uani 1 d . .
S1 S 0.4979(5) 0.0231(3) 0.78513(12) 0.0366(9) Uani 1 d . .
O3 O 0.5023(12) -0.0898(8) 0.8464(3) 0.0459(18) Uani 1 d . .
C9 C 0.7118(13) 0.1416(12) 0.7802(5) 0.038(3) Uani 1 d . .
H9A H 0.7205 0.2352 0.8148 0.057 Uiso 1 calc . .
H9B H 0.7217 0.2051 0.7384 0.057 Uiso 1 calc . .
H9C H 0.8112 0.0497 0.7846 0.057 Uiso 1 calc . .
C10 C 0.3553(14) 0.2171(12) 0.8013(5) 0.032(3) Uani 1 d . .
H10A H 0.2295 0.1731 0.8074 0.048 Uiso 1 calc . .
H10B H 0.3594 0.3053 0.765 0.048 Uiso 1 calc . .
H10C H 0.3974 0.281 0.8404 0.048 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
O1 C1 1.332(12) . ?
O1 H1O 0.92(9) . ?
O2 C1 1.235(11) . ?
C1 C2 1.452(13) . ?
C2 C3 1.384(12) . ?
C2 C7 1.418(13) . ?
C3 C4 1.395(12) . ?
C3 H3 0.95 . ?
C4 C5 1.418(12) . ?
C4 H4 0.95 . ?
C5 C6 1.402(12) . ?
C5 C8 1.446(12) . ?
C6 C7 1.376(12) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 N1 1.337(11) . ?
C8 N2 1.363(11) 3_657 ?
N1 N2 1.323(9) . ?
N2 C8 1.363(11) 3_657 ?
S1 O3 1.504(6) . ?
S1 C10 1.759(9) . ?
S1 C9 1.779(10) . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?

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 O1 H1O 100(5) . . ?
O2 C1 O1 121.6(9) . . ?
O2 C1 C2 124.7(10) . . ?
O1 C1 C2 113.7(10) . . ?
C3 C2 C7 116.8(9) . . ?
C3 C2 C1 123.3(9) . . ?
C7 C2 C1 119.8(9) . . ?
C2 C3 C4 122.7(9) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 119.4(9) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 118.5(9) . . ?
C6 C5 C8 121.3(9) . . ?
C4 C5 C8 120.2(9) . . ?
C7 C6 C5 120.5(9) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 121.9(9) . . ?
C6 C7 H7 119 . . ?
C2 C7 H7 119 . . ?
N1 C8 N2 122.8(9) . 3_657 ?
N1 C8 C5 119.4(10) . . ?
N2 C8 C5 117.7(10) 3_657 . ?
N2 N1 C8 119.4(8) . . ?
N1 N2 C8 117.8(7) . 3_657 ?
O3 S1 C10 105.5(4) . . ?
O3 S1 C9 106.4(5) . . ?
C10 S1 C9 99.4(5) . . ?
S1 C9 H9A 109.5 . . ?
S1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
S1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
S1 C10 H10A 109.5 . . ?
S1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 171.5(9) . . . . ?
O1 C1 C2 C3 -9.8(13) . . . . ?
O2 C1 C2 C7 -6.0(14) . . . . ?
O1 C1 C2 C7 172.6(8) . . . . ?
C7 C2 C3 C4 0.9(13) . . . . ?
C1 C2 C3 C4 -176.7(9) . . . . ?
C2 C3 C4 C5 -0.8(14) . . . . ?
C3 C4 C5 C6 -1.1(13) . . . . ?
C3 C4 C5 C8 179.6(8) . . . . ?
C4 C5 C6 C7 2.9(13) . . . . ?
C8 C5 C6 C7 -177.8(8) . . . . ?
C5 C6 C7 C2 -2.9(13) . . . . ?
C3 C2 C7 C6 1.0(13) . . . . ?
C1 C2 C7 C6 178.7(8) . . . . ?
C6 C5 C8 N1 8.1(13) . . . . ?
C4 C5 C8 N1 -172.6(9) . . . . ?
C6 C5 C8 N2 -171.5(8) . . . 3_657 ?
C4 C5 C8 N2 7.8(12) . . . 3_657 ?
N2 C8 N1 N2 -1.1(16) 3_657 . . . ?
C5 C8 N1 N2 179.4(7) . . . . ?
C8 N1 N2 C8 1.1(15) . . . 3_657 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.92(9) 1.75(9) 2.586(10) 151(8) 1_665


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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1030583'
_audit_update_record             
;
2015-04-28 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;

_audit_creation_date             2015-04-21T13:24:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C16  H9  N4  O4  K1'
_chemical_formula_sum            'C16 H9 K N4 O4'
_chemical_formula_weight         360.37

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/a'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   5.9700(10)
_cell_length_b                   6.7380(12)
_cell_length_c                   34.500(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.680(5)
_cell_angle_gamma                90
_cell_volume                     1383.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1788
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      55.29
_cell_measurement_wavelength     1.54178

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_T_max  0.751
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.897

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_number            2558
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         55.293
_diffrn_reflns_theta_full        55.293
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_reflns_number_total             854
_reflns_number_gt                765
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0339P)²+3.7908P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         854
_refine_ls_number_parameters     117
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.09

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2727(5) 0.2323(5) 0.55635(9) 0.0203(8) Uani 1 d . .
C2 C 0.3735(5) 0.2418(4) 0.59728(9) 0.0182(8) Uani 1 d . .
C3 C 0.5882(5) 0.3209(4) 0.60630(9) 0.0189(8) Uani 1 d . .
H3 H 0.6713 0.3716 0.5862 0.023 Uiso 1 calc . .
C4 C 0.6794(5) 0.3254(4) 0.64424(9) 0.0201(8) Uani 1 d . .
H4 H 0.8266 0.3768 0.65 0.024 Uiso 1 calc . .
C5 C 0.5586(5) 0.2556(4) 0.67444(9) 0.0187(8) Uani 1 d . .
C6 C 0.3420(5) 0.1816(5) 0.66536(9) 0.0199(8) Uani 1 d . .
H6 H 0.2556 0.137 0.6856 0.024 Uiso 1 calc . .
C7 C 0.2526(5) 0.1726(5) 0.62728(9) 0.0202(8) Uani 1 d . .
H7 H 0.1067 0.1186 0.6215 0.024 Uiso 1 calc . .
C8 C 0.6595(5) 0.2544(4) 0.71478(9) 0.0189(8) Uani 1 d . .
N1 N 0.8543(4) 0.3533(4) 0.72267(7) 0.0236(7) Uani 1 d . .
N2 N 0.5536(4) 0.1506(4) 0.74121(8) 0.0242(7) Uani 1 d . .
K1 K 0.75 0.21232(15) 0.5 0.0253(4) Uani 1 d . .
O2 O 0.1175(4) 0.1160(3) 0.54668(6) 0.0246(6) Uani 1 d . .
O1 O 0.3570(4) 0.3553(3) 0.53208(6) 0.0242(6) Uani 1 d . .
H1O H 0.284(14) 0.347(8) 0.5096(19) 0.029 Uiso 0.5 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.238(4) . ?
C1 O1 1.308(4) . ?
C1 C2 1.490(4) . ?
C2 C7 1.390(4) . ?
C2 C3 1.400(4) . ?
C3 C4 1.377(4) . ?
C3 H3 0.95 . ?
C4 C5 1.396(4) . ?
C4 H4 0.95 . ?
C5 C6 1.398(4) . ?
C5 C8 1.471(4) . ?
C6 C7 1.378(4) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 N2 1.347(4) . ?
C8 N1 1.349(4) . ?
N1 N2 1.320(4) 7_656 ?
N2 N1 1.320(4) 7_656 ?
K1 O2 2.693(2) 2_556 ?
K1 O2 2.693(2) 1_655 ?
K1 O1 2.842(2) . ?
K1 O1 2.843(2) 2_656 ?
K1 O2 2.885(2) 5_656 ?
K1 O2 2.885(2) 6_655 ?
K1 O1 3.163(2) 6_665 ?
K1 O1 3.163(2) 5_666 ?
K1 H1O 2.97(8) . ?
O2 K1 2.693(2) 1_455 ?
O2 K1 2.885(2) 5_656 ?
O1 K1 3.163(2) 5_666 ?
O1 H1O 0.86(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
O2 C1 O1 123.2(3) . . ?
O2 C1 C2 121.2(3) . . ?
O1 C1 C2 115.6(3) . . ?
C7 C2 C3 118.9(3) . . ?
C7 C2 C1 119.8(3) . . ?
C3 C2 C1 121.2(3) . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.9(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 118.5(3) . . ?
C4 C5 C8 120.8(3) . . ?
C6 C5 C8 120.7(3) . . ?
C7 C6 C5 120.6(3) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 120.7(3) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
N2 C8 N1 124.4(3) . . ?
N2 C8 C5 117.7(3) . . ?
N1 C8 C5 117.9(3) . . ?
N2 N1 C8 117.8(2) 7_656 . ?
N1 N2 C8 117.8(3) 7_656 . ?
O2 K1 O2 152.12(10) 2_556 1_655 ?
O2 K1 O1 69.91(6) 2_556 . ?
O2 K1 O1 120.45(6) 1_655 . ?
O2 K1 O1 120.45(6) 2_556 2_656 ?
O2 K1 O1 69.91(6) 1_655 2_656 ?
O1 K1 O1 140.38(10) . 2_656 ?
O2 K1 O2 74.24(5) 2_556 5_656 ?
O2 K1 O2 84.38(7) 1_655 5_656 ?
O1 K1 O2 138.58(7) . 5_656 ?
O1 K1 O2 76.70(6) 2_656 5_656 ?
O2 K1 O2 84.38(7) 2_556 6_655 ?
O2 K1 O2 74.24(5) 1_655 6_655 ?
O1 K1 O2 76.70(6) . 6_655 ?
O1 K1 O2 138.58(7) 2_656 6_655 ?
O2 K1 O2 79.84(9) 5_656 6_655 ?
O2 K1 O1 124.23(7) 2_556 6_665 ?
O2 K1 O1 83.17(6) 1_655 6_665 ?
O1 K1 O1 72.62(5) . 6_665 ?
O1 K1 O1 71.01(7) 2_656 6_665 ?
O2 K1 O1 147.67(6) 5_656 6_665 ?
O2 K1 O1 124.60(6) 6_655 6_665 ?
O2 K1 O1 83.17(6) 2_556 5_666 ?
O2 K1 O1 124.23(7) 1_655 5_666 ?
O1 K1 O1 71.00(7) . 5_666 ?
O1 K1 O1 72.62(5) 2_656 5_666 ?
O2 K1 O1 124.60(6) 5_656 5_666 ?
O2 K1 O1 147.67(6) 6_655 5_666 ?
O1 K1 O1 45.84(8) 6_665 5_666 ?
O2 K1 K1 43.98(5) 2_556 5_656 ?
O2 K1 K1 112.72(6) 1_655 5_656 ?
O1 K1 K1 67.40(5) . 5_656 ?
O1 K1 K1 148.56(5) 2_656 5_656 ?
O2 K1 K1 72.55(5) 5_656 5_656 ?
O2 K1 K1 40.40(4) 6_655 5_656 ?
O1 K1 K1 139.69(4) 6_665 5_656 ?
O1 K1 K1 120.80(4) 5_666 5_656 ?
O2 K1 K1 112.72(6) 2_556 5_756 ?
O2 K1 K1 43.98(5) 1_655 5_756 ?
O1 K1 K1 148.57(5) . 5_756 ?
O1 K1 K1 67.40(4) 2_656 5_756 ?
O2 K1 K1 40.40(4) 5_656 5_756 ?
O2 K1 K1 72.55(5) 6_655 5_756 ?
O1 K1 K1 120.80(4) 6_665 5_756 ?
O1 K1 K1 139.69(4) 5_666 5_756 ?
K1 K1 K1 92.43(4) 5_656 5_756 ?
O2 K1 K1 131.16(5) 2_556 5_766 ?
O2 K1 K1 73.95(5) 1_655 5_766 ?
O1 K1 K1 104.74(6) . 5_766 ?
O1 K1 K1 37.69(4) 2_656 5_766 ?
O2 K1 K1 114.37(4) 5_656 5_766 ?
O2 K1 K1 143.39(4) 6_655 5_766 ?
O1 K1 K1 33.32(4) 6_665 5_766 ?
O1 K1 K1 51.40(4) 5_666 5_766 ?
K1 K1 K1 171.38(3) 5_656 5_766 ?
K1 K1 K1 96.192(14) 5_756 5_766 ?
O2 K1 K1 73.95(5) 2_556 5_666 ?
O2 K1 K1 131.16(5) 1_655 5_666 ?
O1 K1 K1 37.68(4) . 5_666 ?
O1 K1 K1 104.74(6) 2_656 5_666 ?
O2 K1 K1 143.39(4) 5_656 5_666 ?
O2 K1 K1 114.37(4) 6_655 5_666 ?
O1 K1 K1 51.40(4) 6_665 5_666 ?
O1 K1 K1 33.32(4) 5_666 5_666 ?
K1 K1 K1 96.192(15) 5_656 5_666 ?
K1 K1 K1 171.38(4) 5_756 5_666 ?
K1 K1 K1 75.19(3) 5_766 5_666 ?
O2 K1 H1O 54.3(11) 2_556 . ?
O2 K1 H1O 137.0(12) 1_655 . ?
O1 K1 H1O 16.8(12) . . ?
O1 K1 H1O 138.5(12) 2_656 . ?
O2 K1 H1O 126.8(11) 5_656 . ?
O2 K1 H1O 82.6(13) 6_655 . ?
O1 K1 H1O 81.0(11) 6_665 . ?
O1 K1 H1O 66.0(12) 5_666 . ?
K1 K1 H1O 61.9(12) 5_656 . ?
K1 K1 H1O 153.5(12) 5_756 . ?
K1 K1 H1O 109.5(12) 5_766 . ?
K1 K1 H1O 35.0(12) 5_666 . ?
C1 O2 K1 124.31(19) . 1_455 ?
C1 O2 K1 113.75(19) . 5_656 ?
K1 O2 K1 95.62(7) 1_455 5_656 ?
C1 O1 K1 114.08(18) . . ?
C1 O1 K1 136.89(18) . 5_666 ?
K1 O1 K1 109.00(7) . 5_666 ?
C1 O1 H1O 110(5) . . ?
K1 O1 H1O 90(6) . . ?
K1 O1 H1O 71(4) 5_666 . ?

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
O2 C1 C2 C7 -21.3(4) . . . . ?
O1 C1 C2 C7 157.9(3) . . . . ?
O2 C1 C2 C3 159.2(3) . . . . ?
O1 C1 C2 C3 -21.5(4) . . . . ?
C7 C2 C3 C4 1.5(4) . . . . ?
C1 C2 C3 C4 -179.0(3) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C3 C4 C5 C8 177.9(3) . . . . ?
C4 C5 C6 C7 1.8(4) . . . . ?
C8 C5 C6 C7 -176.4(3) . . . . ?
C5 C6 C7 C2 -1.7(5) . . . . ?
C3 C2 C7 C6 0.0(4) . . . . ?
C1 C2 C7 C6 -179.4(3) . . . . ?
C4 C5 C8 N2 -167.2(3) . . . . ?
C6 C5 C8 N2 11.0(4) . . . . ?
C4 C5 C8 N1 11.3(4) . . . . ?
C6 C5 C8 N1 -170.5(3) . . . . ?
N2 C8 N1 N2 -0.6(5) . . . 7_656 ?
C5 C8 N1 N2 -179.0(2) . . . 7_656 ?
N1 C8 N2 N1 0.6(5) . . . 7_656 ?
C5 C8 N2 N1 179.0(2) . . . 7_656 ?
O1 C1 O2 K1 -42.9(4) . . . 1_455 ?
C2 C1 O2 K1 136.3(2) . . . 1_455 ?
O1 C1 O2 K1 72.6(3) . . . 5_656 ?
C2 C1 O2 K1 -108.3(3) . . . 5_656 ?
O2 C1 O1 K1 -96.0(3) . . . . ?
C2 C1 O1 K1 84.7(3) . . . . ?
O2 C1 O1 K1 86.4(4) . . . 5_666 ?
C2 C1 O1 K1 -92.9(3) . . . 5_666 ?


# END of CIF
