# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1030651'
_audit_update_record             
;
2014-10-23 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H18 Cu2 N10 O6 S2'
_chemical_formula_sum            'C24 H18 Cu2 N10 O6 S2'
_chemical_formula_weight         733.68

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3215(10)
_cell_length_b                   12.3215(9)
_cell_length_c                   16.7717(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2752.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      26.33

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON  100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32709
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         25.34
_reflns_number_total             2518
_reflns_number_gt                2083
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_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 > 2sigma(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)+(0.0578P)²+1.5300P] 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         2518
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1297(2) 0.2830(2) 0.58619(17) 0.0333(6) Uani 1 1 d . . .
C2 C 0.1490(2) 0.3247(3) 0.51155(17) 0.0358(7) Uani 1 1 d . . .
C3 C 0.1427(3) 0.4362(3) 0.4989(2) 0.0426(8) Uani 1 1 d . . .
H3 H 0.1583 0.4643 0.4489 0.051 Uiso 1 1 calc R . .
C4 C 0.1138(3) 0.5053(3) 0.5589(2) 0.0522(9) Uani 1 1 d . . .
H4 H 0.1097 0.5796 0.5498 0.063 Uiso 1 1 calc R . .
C5 C 0.0910(3) 0.4628(3) 0.6331(2) 0.0520(9) Uani 1 1 d . . .
H5 H 0.0700 0.5090 0.6738 0.062 Uiso 1 1 calc R . .
C6 C 0.0989(2) 0.3535(3) 0.6476(2) 0.0464(8) Uani 1 1 d . . .
H6 H 0.0838 0.3260 0.6978 0.056 Uiso 1 1 calc R . .
C11 C 0.1530(2) 0.1295(3) 0.67054(17) 0.0379(7) Uani 1 1 d . . .
H11 H 0.1664 0.1751 0.7134 0.045 Uiso 1 1 calc R . .
C12 C 0.1491(2) 0.0117(3) 0.68078(16) 0.0325(6) Uani 1 1 d . . .
C13 C 0.1601(2) -0.0392(3) 0.75376(18) 0.0426(8) Uani 1 1 d . . .
H13 H 0.1754 0.0005 0.7994 0.051 Uiso 1 1 calc R . .
C14 C 0.1480(2) -0.1506(3) 0.75721(18) 0.0470(8) Uani 1 1 d . . .
H14 H 0.1537 -0.1869 0.8056 0.056 Uiso 1 1 calc R . .
C15 C 0.1274(2) -0.2068(3) 0.68869(19) 0.0442(8) Uani 1 1 d . . .
H15 H 0.1191 -0.2817 0.6903 0.053 Uiso 1 1 calc R . .
C16 C 0.1192(2) -0.1516(3) 0.61692(18) 0.0380(7) Uani 1 1 d . . .
H16 H 0.1063 -0.1904 0.5705 0.046 Uiso 1 1 calc R . .
N1 N 0.13749(18) 0.1681(2) 0.60034(13) 0.0321(5) Uani 1 1 d . . .
N3 N 0.12928(17) -0.04400(19) 0.61310(14) 0.0306(5) Uani 1 1 d . . .
N11 N 0.0703(2) -0.0718(2) 0.45105(14) 0.0345(6) Uani 1 1 d . . .
N12 N 0.08632(19) -0.0749(2) 0.38044(15) 0.0373(6) Uani 1 1 d . . .
N13 N 0.0974(3) -0.0827(3) 0.31305(17) 0.0665(10) Uani 1 1 d . . .
O11 O 0.10871(17) 0.15223(19) 0.42968(12) 0.0462(6) Uani 1 1 d . . .
O12 O 0.28419(18) 0.1981(2) 0.44922(15) 0.0541(6) Uani 1 1 d . . .
O13 O 0.1775(2) 0.30382(19) 0.35918(12) 0.0563(7) Uani 1 1 d . . .
S1 S 0.18528(6) 0.23982(6) 0.43052(4) 0.0377(2) Uani 1 1 d . . .
Cu1 Cu 0.10543(3) 0.05147(3) 0.519197(19) 0.03124(15) Uani 1 1 d . . .


_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 C2 1.377(4) . ?
C1 C6 1.408(4) . ?
C1 N1 1.439(4) . ?
C2 C3 1.393(4) . ?
C2 S1 1.781(3) . ?
C3 C4 1.374(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C11 N1 1.287(4) . ?
C11 C12 1.463(4) . ?
C11 H11 0.9300 . ?
C12 N3 1.352(4) . ?
C12 C13 1.383(4) . ?
C13 C14 1.383(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.369(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(4) . ?
C15 H15 0.9300 . ?
C16 N3 1.334(4) . ?
C16 H16 0.9300 . ?
N1 Cu1 2.024(2) . ?
N3 Cu1 1.991(2) . ?
N11 N12 1.204(3) . ?
N11 Cu1 1.957(2) . ?
N11 Cu1 2.406(3) 5_556 ?
N12 N13 1.144(4) . ?
O11 S1 1.485(2) . ?
O11 Cu1 1.949(2) . ?
O12 S1 1.449(3) . ?
O13 S1 1.437(2) . ?
Cu1 N11 2.406(3) 5_556 ?

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 C6 119.3(3) . . ?
C2 C1 N1 120.2(3) . . ?
C6 C1 N1 120.5(3) . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 S1 121.7(2) . . ?
C3 C2 S1 118.6(2) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.1(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 119.9(3) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
N1 C11 C12 117.9(3) . . ?
N1 C11 H11 121.0 . . ?
C12 C11 H11 121.0 . . ?
N3 C12 C13 122.3(3) . . ?
N3 C12 C11 114.3(2) . . ?
C13 C12 C11 123.3(3) . . ?
C12 C13 C14 118.3(3) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 119.7(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
N3 C16 C15 121.4(3) . . ?
N3 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C11 N1 C1 121.7(2) . . ?
C11 N1 Cu1 112.8(2) . . ?
C1 N1 Cu1 124.89(18) . . ?
C16 N3 C12 118.9(2) . . ?
C16 N3 Cu1 127.5(2) . . ?
C12 N3 Cu1 113.30(19) . . ?
N12 N11 Cu1 123.8(2) . . ?
N12 N11 Cu1 112.3(2) . 5_556 ?
Cu1 N11 Cu1 91.78(9) . 5_556 ?
N13 N12 N11 175.9(4) . . ?
S1 O11 Cu1 118.11(12) . . ?
O13 S1 O12 116.15(15) . . ?
O13 S1 O11 109.97(14) . . ?
O12 S1 O11 111.64(15) . . ?
O13 S1 C2 107.07(14) . . ?
O12 S1 C2 106.86(14) . . ?
O11 S1 C2 104.32(13) . . ?
O11 Cu1 N11 92.85(9) . . ?
O11 Cu1 N3 169.16(9) . . ?
N11 Cu1 N3 92.39(10) . . ?
O11 Cu1 N1 93.50(10) . . ?
N11 Cu1 N1 173.47(10) . . ?
N3 Cu1 N1 81.60(10) . . ?
O11 Cu1 N11 96.62(9) . 5_556 ?
N11 Cu1 N11 88.22(10) . 5_556 ?
N3 Cu1 N11 93.02(9) . 5_556 ?
N1 Cu1 N11 89.55(9) . 5_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1030652'
_audit_update_record             
;
2014-10-23 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H18 Cu2 N6 O6 S4'
_chemical_formula_sum            'C26 H18 Cu2 N6 O6 S4'
_chemical_formula_weight         765.78

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'
Cu Cu 0.3201 1.2651 '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   '
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   7.2488(4)
_cell_length_b                   8.5638(4)
_cell_length_c                   13.1244(7)
_cell_angle_alpha                83.205(2)
_cell_angle_beta                 89.661(3)
_cell_angle_gamma                70.551(2)
_cell_volume                     762.35(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3082
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      25.68

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             386
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_T_max  0.8891
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5933
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         25.35
_reflns_number_total             2719
_reflns_number_gt                2319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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 > 2sigma(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)+(0.0706P)²+0.9171P] 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         2719
_refine_ls_number_parameters     199
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1283
_refine_ls_wR_factor_gt          0.1219
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.216
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 1.000 57 18 ' '
_platon_squeeze_details          ?



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 0.3089(6) 0.4929(6) 0.1281(3) 0.0393(10) Uani 1 1 d . . .
C2 C 0.2383(7) 0.6671(6) 0.1158(3) 0.0468(11) Uani 1 1 d . . .
C3 C 0.1623(8) 0.7522(8) 0.0211(4) 0.0658(17) Uani 1 1 d . . .
H3 H 0.1149 0.8683 0.0127 0.079 Uiso 1 1 calc R . .
C4 C 0.1556(8) 0.6686(10) -0.0606(4) 0.0736(19) Uani 1 1 d . . .
H4 H 0.1056 0.7278 -0.1241 0.088 Uiso 1 1 calc R . .
C5 C 0.2216(9) 0.4999(10) -0.0492(4) 0.0704(18) Uani 1 1 d . . .
H5 H 0.2163 0.4435 -0.1049 0.085 Uiso 1 1 calc R . .
C6 C 0.2974(7) 0.4099(7) 0.0455(4) 0.0515(12) Uani 1 1 d . . .
H6 H 0.3404 0.2939 0.0531 0.062 Uiso 1 1 calc R . .
C10 C -0.1383(6) 0.4397(5) 0.4259(3) 0.0341(9) Uani 1 1 d . . .
C11 C 0.5207(6) 0.2602(5) 0.2312(3) 0.0397(10) Uani 1 1 d . . .
H11 H 0.5694 0.2132 0.1721 0.048 Uiso 1 1 calc R . .
C12 C 0.5932(6) 0.1727(5) 0.3328(4) 0.0397(10) Uani 1 1 d . . .
C13 C 0.7434(7) 0.0213(6) 0.3478(5) 0.0539(13) Uani 1 1 d . . .
H13 H 0.8002 -0.0331 0.2924 0.065 Uiso 1 1 calc R . .
C14 C 0.8068(8) -0.0470(7) 0.4472(5) 0.0614(15) Uani 1 1 d . . .
H14 H 0.9073 -0.1490 0.4599 0.074 Uiso 1 1 calc R . .
C15 C 0.7204(8) 0.0368(7) 0.5273(4) 0.0589(15) Uani 1 1 d . . .
H15 H 0.7627 -0.0077 0.5946 0.071 Uiso 1 1 calc R . .
C16 C 0.5695(7) 0.1887(6) 0.5073(4) 0.0480(12) Uani 1 1 d . . .
H16 H 0.5120 0.2457 0.5617 0.058 Uiso 1 1 calc R . .
N1 N 0.3876(5) 0.4039(4) 0.2261(3) 0.0336(7) Uani 1 1 d . . .
N3 N 0.5055(5) 0.2544(4) 0.4113(3) 0.0367(8) Uani 1 1 d . . .
N10 N 0.2216(6) 0.5213(5) 0.5015(3) 0.0458(9) Uani 1 1 d . . .
O11 O 0.1694(7) 0.7056(4) 0.3070(3) 0.0700(12) Uani 1 1 d . . .
O12 O 0.1325(9) 0.9502(6) 0.1880(4) 0.1024(16) Uani 1 1 d U . .
O13 O 0.4592(9) 0.7511(6) 0.2372(3) 0.0883(15) Uani 1 1 d . . .
S1 S 0.2532(3) 0.78013(15) 0.21840(11) 0.0721(5) Uani 1 1 d . . .
S2 S -0.02008(18) 0.38028(18) 0.32367(9) 0.0504(3) Uani 1 1 d . . .
Cu1 Cu 0.29307(8) 0.47004(6) 0.36383(4) 0.0391(2) Uani 1 1 d . . .


_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 C6 1.382(7) . ?
C1 C2 1.396(7) . ?
C1 N1 1.431(5) . ?
C2 C3 1.381(7) . ?
C2 S1 1.773(5) . ?
C3 C4 1.367(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.352(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C10 N10 1.147(6) 2_566 ?
C10 S2 1.629(4) . ?
C11 N1 1.281(5) . ?
C11 C12 1.457(6) . ?
C11 H11 0.9300 . ?
C12 N3 1.350(6) . ?
C12 C13 1.381(6) . ?
C13 C14 1.380(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.390(7) . ?
C15 H15 0.9300 . ?
C16 N3 1.337(6) . ?
C16 H16 0.9300 . ?
N1 Cu1 2.007(3) . ?
N3 Cu1 2.003(3) . ?
N10 C10 1.147(6) 2_566 ?
N10 Cu1 1.937(4) . ?
O11 S1 1.484(4) . ?
O11 Cu1 1.969(3) . ?
O12 S1 1.437(5) . ?
O13 S1 1.447(6) . ?
S2 Cu1 2.7006(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 119.0(4) . . ?
C6 C1 N1 121.3(4) . . ?
C2 C1 N1 119.6(4) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 S1 119.7(4) . . ?
C1 C2 S1 121.0(3) . . ?
C4 C3 C2 121.0(6) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 120.1(6) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
N10 C10 S2 178.8(4) 2_566 . ?
N1 C11 C12 117.8(4) . . ?
N1 C11 H11 121.1 . . ?
C12 C11 H11 121.1 . . ?
N3 C12 C13 122.6(4) . . ?
N3 C12 C11 114.4(4) . . ?
C13 C12 C11 123.0(5) . . ?
C14 C13 C12 118.2(5) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C15 C14 C13 119.5(5) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 119.6(5) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N3 C16 C15 121.2(5) . . ?
N3 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C11 N1 C1 119.8(4) . . ?
C11 N1 Cu1 113.4(3) . . ?
C1 N1 Cu1 126.5(3) . . ?
C16 N3 C12 118.9(4) . . ?
C16 N3 Cu1 128.3(4) . . ?
C12 N3 Cu1 112.8(3) . . ?
C10 N10 Cu1 164.9(4) 2_566 . ?
S1 O11 Cu1 120.8(2) . . ?
O12 S1 O13 116.3(3) . . ?
O12 S1 O11 110.4(3) . . ?
O13 S1 O11 111.1(3) . . ?
O12 S1 C2 106.6(3) . . ?
O13 S1 C2 106.4(2) . . ?
O11 S1 C2 105.2(2) . . ?
C10 S2 Cu1 96.69(15) . . ?
N10 Cu1 O11 91.37(16) . . ?
N10 Cu1 N3 94.26(16) . . ?
O11 Cu1 N3 158.99(17) . . ?
N10 Cu1 N1 175.40(16) . . ?
O11 Cu1 N1 92.23(13) . . ?
N3 Cu1 N1 81.37(14) . . ?
N10 Cu1 S2 95.79(12) . . ?
O11 Cu1 S2 95.00(15) . . ?
N3 Cu1 S2 104.52(10) . . ?
N1 Cu1 S2 86.75(10) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1030653'
_audit_update_record             
;
2014-10-23 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H9 Cu N5 O3 S, H2 O'
_chemical_formula_sum            'C14 H11 Cu N5 O4 S'
_chemical_formula_weight         408.88

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.5179(6)
_cell_length_b                   15.1779(7)
_cell_length_c                   12.2602(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.219(3)
_cell_angle_gamma                90.00
_cell_volume                     1583.86(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6684
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      25.17

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6720
_exptl_absorpt_correction_T_max  0.8865
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18641
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         25.36
_reflns_number_total             2905
_reflns_number_gt                2344
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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 > 2sigma(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)+(0.0653P)²+0.7170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2905
_refine_ls_number_parameters     232
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.1066
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6032(4) 0.4836(2) 0.8013(3) 0.0340(7) Uani 1 1 d . . .
C2 C 0.4995(4) 0.5549(2) 0.7988(3) 0.0353(7) Uani 1 1 d . . .
C3 C 0.3585(4) 0.5493(3) 0.8499(3) 0.0467(9) Uani 1 1 d . . .
H3 H 0.2902 0.5971 0.8489 0.056 Uiso 1 1 calc R . .
C4 C 0.3193(5) 0.4721(3) 0.9027(4) 0.0565(11) Uani 1 1 d . . .
H4 H 0.2232 0.4677 0.9359 0.068 Uiso 1 1 calc R . .
C5 C 0.4211(5) 0.4026(3) 0.9063(4) 0.0586(11) Uani 1 1 d . . .
H5 H 0.3942 0.3512 0.9424 0.070 Uiso 1 1 calc R . .
C6 C 0.5640(5) 0.4080(2) 0.8567(3) 0.0465(9) Uani 1 1 d . . .
H6 H 0.6335 0.3607 0.8606 0.056 Uiso 1 1 calc R . .
C10 C 1.0022(4) 0.7683(2) 0.6163(3) 0.0356(8) Uani 1 1 d . . .
C11 C 0.8190(4) 0.4220(2) 0.7149(2) 0.0345(7) Uani 1 1 d . . .
H11 H 0.7731 0.3668 0.7214 0.041 Uiso 1 1 calc R . .
C12 C 0.9721(4) 0.4319(2) 0.6666(2) 0.0344(7) Uani 1 1 d . . .
C13 C 1.0600(5) 0.3617(3) 0.6320(3) 0.0458(9) Uani 1 1 d . . .
H13 H 1.0235 0.3043 0.6389 0.055 Uiso 1 1 calc R . .
C14 C 1.2034(5) 0.3782(3) 0.5870(3) 0.0547(11) Uani 1 1 d . . .
H14 H 1.2658 0.3319 0.5641 0.066 Uiso 1 1 calc R . .
C15 C 1.2522(5) 0.4640(3) 0.5767(3) 0.0533(10) Uani 1 1 d . . .
H15 H 1.3474 0.4767 0.5455 0.064 Uiso 1 1 calc R . .
C16 C 1.1585(4) 0.5310(3) 0.6130(3) 0.0450(9) Uani 1 1 d . . .
H16 H 1.1921 0.5889 0.6057 0.054 Uiso 1 1 calc R . .
C20 C 1.0075(4) 0.6349(2) 0.9769(3) 0.0349(8) Uani 1 1 d . . .
N1 N 0.7497(3) 0.49107(16) 0.7481(2) 0.0302(6) Uani 1 1 d . . .
N3 N 1.0215(3) 0.51563(18) 0.6583(2) 0.0334(6) Uani 1 1 d . . .
N10 N 0.9786(4) 0.7033(2) 0.6602(2) 0.0495(8) Uani 1 1 d . . .
N11 N 1.0353(4) 0.8451(2) 0.5790(2) 0.0526(9) Uani 1 1 d . . .
N20 N 0.9856(4) 0.6097(2) 0.8902(2) 0.0451(8) Uani 1 1 d . . .
O11 O 0.7027(3) 0.67793(16) 0.7730(2) 0.0519(7) Uani 1 1 d . . .
O12 O 0.5415(4) 0.6342(2) 0.6167(2) 0.0625(8) Uani 1 1 d . . .
O13 O 0.4296(4) 0.71795(19) 0.7629(3) 0.0622(8) Uani 1 1 d . . .
O20 O 0.3134(5) 0.7092(3) 0.4623(3) 0.1039(15) Uani 1 1 d D . .
S1 S 0.54349(11) 0.65445(6) 0.73138(7) 0.0414(2) Uani 1 1 d . . .
Cu1 Cu 0.87830(5) 0.60209(2) 0.72753(3) 0.03302(16) Uani 1 1 d . . .
H20A H 0.371(4) 0.737(2) 0.413(2) 0.050 Uiso 1 1 d D . .
H20B H 0.383(4) 0.691(2) 0.516(2) 0.050 Uiso 1 1 d D . .


_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 C6 1.382(5) . ?
C1 C2 1.396(5) . ?
C1 N1 1.434(4) . ?
C2 C3 1.378(5) . ?
C2 S1 1.770(3) . ?
C3 C4 1.386(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.366(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C10 N10 1.145(4) . ?
C10 N11 1.288(4) . ?
C11 N1 1.277(4) . ?
C11 C12 1.461(5) . ?
C11 H11 0.9300 . ?
C12 N3 1.344(4) . ?
C12 C13 1.378(5) . ?
C13 C14 1.382(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.377(5) . ?
C15 H15 0.9300 . ?
C16 N3 1.333(4) . ?
C16 H16 0.9300 . ?
C20 N20 1.138(4) . ?
C20 N11 1.301(4) 4_576 ?
N1 Cu1 2.031(3) . ?
N3 Cu1 2.002(3) . ?
N10 Cu1 1.956(3) . ?
N11 C20 1.301(4) 4_575 ?
N20 Cu1 2.164(3) . ?
O11 S1 1.474(3) . ?
O11 Cu1 1.984(3) . ?
O12 S1 1.439(3) . ?
O13 S1 1.431(3) . ?
O20 H20A 0.897(18) . ?
O20 H20B 0.913(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 119.3(3) . . ?
C6 C1 N1 121.3(3) . . ?
C2 C1 N1 119.3(3) . . ?
C3 C2 C1 120.3(3) . . ?
C3 C2 S1 117.9(3) . . ?
C1 C2 S1 121.8(3) . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.5(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 119.9(4) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
N10 C10 N11 172.6(4) . . ?
N1 C11 C12 118.5(3) . . ?
N1 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
N3 C12 C13 122.2(3) . . ?
N3 C12 C11 114.5(3) . . ?
C13 C12 C11 123.4(3) . . ?
C12 C13 C14 118.8(4) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C15 C14 C13 118.9(4) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 119.3(4) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
N3 C16 C15 122.3(4) . . ?
N3 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
N20 C20 N11 173.7(4) . 4_576 ?
C11 N1 C1 120.1(3) . . ?
C11 N1 Cu1 112.5(2) . . ?
C1 N1 Cu1 127.2(2) . . ?
C16 N3 C12 118.6(3) . . ?
C16 N3 Cu1 128.3(2) . . ?
C12 N3 Cu1 113.0(2) . . ?
C10 N10 Cu1 164.2(3) . . ?
C10 N11 C20 121.2(3) . 4_575 ?
C20 N20 Cu1 157.9(3) . . ?
S1 O11 Cu1 117.12(15) . . ?
H20A O20 H20B 106(3) . . ?
O13 S1 O12 115.19(18) . . ?
O13 S1 O11 111.56(18) . . ?
O12 S1 O11 111.47(18) . . ?
O13 S1 C2 106.91(17) . . ?
O12 S1 C2 106.21(17) . . ?
O11 S1 C2 104.69(16) . . ?
N10 Cu1 O11 90.52(13) . . ?
N10 Cu1 N3 93.03(13) . . ?
O11 Cu1 N3 167.76(11) . . ?
N10 Cu1 N1 161.93(12) . . ?
O11 Cu1 N1 91.73(11) . . ?
N3 Cu1 N1 81.33(11) . . ?
N10 Cu1 N20 99.85(13) . . ?
O11 Cu1 N20 90.35(12) . . ?
N3 Cu1 N20 100.56(11) . . ?
N1 Cu1 N20 98.06(11) . . ?

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
O20 H20A O13 0.897(18) 2.04(2) 2.892(5) 158(3) 4_575
O20 H20B O12 0.913(18) 1.99(2) 2.893(5) 170(4) .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.125
