# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_xcalibur
_database_code_depnum_ccdc_archive 'CCDC 1423795'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Sep 18 11:01:30 2013'
;
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H9 I N2 O'
_chemical_formula_weight         324.11

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_cell_setting           Monoclinic

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                   5.3119(3)
_cell_length_b                   14.3087(6)
_cell_length_c                   15.0594(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.017(5)
_cell_angle_gamma                90.00
_cell_volume                     1144.61(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    248.56(10)
_cell_measurement_reflns_used    2307
_cell_measurement_theta_min      1.9593
_cell_measurement_theta_max      28.2556
_cell_oxdiff_length_a            5.3133(3)
_cell_oxdiff_length_b            14.3226(18)
_cell_oxdiff_length_c            15.0409(19)
_cell_oxdiff_angle_alpha         90.032(10)
_cell_oxdiff_angle_beta          90.013(8)
_cell_oxdiff_angle_gamma         90.105(8)
_cell_oxdiff_volume              1144.6(2)
_cell_oxdiff_measurement_reflns_used 2301

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    2.777
_exptl_absorpt_correction_T_min  0.59038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      248.56(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8308
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         28.32
_diffrn_orient_matrix_UB_11      0.0177460000
_diffrn_orient_matrix_UB_12      0.0442205000
_diffrn_orient_matrix_UB_13      -0.0202929000
_diffrn_orient_matrix_UB_21      -0.1310284000
_diffrn_orient_matrix_UB_22      0.0027913000
_diffrn_orient_matrix_UB_23      -0.0086074000
_diffrn_orient_matrix_UB_31      -0.0183788000
_diffrn_orient_matrix_UB_32      0.0221285000
_diffrn_orient_matrix_UB_33      0.0416868000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   56.00   95.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
  2 omega  -54.00   63.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329    0.0000  -30.0000 117

#__ type_ start__ end____ width___ exp.time_
  3 omega   48.00  117.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000    0.0000 69

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00   92.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329 -178.0000   60.0000 57

#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00   29.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   19.0000 -120.0000 74

#__ type_ start__ end____ width___ exp.time_
  6 omega   73.00   99.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   19.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega   -2.00   80.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -99.0000   60.0000 82

;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             2604
_reflns_number_gt                2141
_reflns_threshold_expression     >2sigma(I)

_computing_structure_solution    'SHELXTL Bruker'
_computing_structure_refinement  'SHELXTL Bruker'
_computing_molecular_graphics    'SHELXTL Bruker'
_computing_publication_material  'SHELXTL Bruker'


_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)+(0.0256P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2604
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
I1 I 0.27949(17) 0.507141(16) 0.37051(2) 0.04383(11) Uani 1 1 d . . .
O1 O -0.1114(6) 0.0372(2) 0.3929(2) 0.0389(9) Uani 1 1 d . . .
N1 N 0.3012(16) 0.0098(2) 0.3795(3) 0.0336(11) Uani 1 1 d . . .
H20 H 0.4460 0.0366 0.3774 0.040 Uiso 1 1 calc R . .
C1 C 0.2269(9) 0.3611(3) 0.3770(3) 0.0307(11) Uani 1 1 d . . .
N2 N 0.3107(8) -0.2843(2) 0.3669(3) 0.0392(9) Uani 1 1 d . . .
C2 C 0.3999(11) 0.3023(3) 0.3361(3) 0.0365(13) Uani 1 1 d . . .
H2 H 0.5383 0.3274 0.3067 0.044 Uiso 1 1 calc R . .
C3 C 0.3662(9) 0.2062(3) 0.3391(3) 0.0302(12) Uani 1 1 d . . .
H3 H 0.4820 0.1666 0.3120 0.036 Uiso 1 1 calc R . .
C4 C 0.1575(9) 0.1694(3) 0.3830(3) 0.0260(11) Uani 1 1 d . . .
C5 C -0.0115(10) 0.2289(3) 0.4231(3) 0.0304(11) Uani 1 1 d . . .
H5 H -0.1515 0.2042 0.4518 0.036 Uiso 1 1 calc R . .
C6 C 0.0228(11) 0.3250(3) 0.4214(3) 0.0370(13) Uani 1 1 d . . .
H6 H -0.0905 0.3644 0.4500 0.044 Uiso 1 1 calc R . .
C7 C 0.1019(9) 0.0656(3) 0.3853(3) 0.0283(10) Uani 1 1 d . . .
C8 C 0.3009(9) -0.0899(2) 0.3765(3) 0.0262(9) Uani 1 1 d . . .
C9 C 0.1090(10) -0.1373(3) 0.3354(3) 0.0323(11) Uani 1 1 d . . .
H9 H -0.0262 -0.1058 0.3100 0.039 Uiso 1 1 calc R . .
C10 C 0.1246(10) -0.2352(3) 0.3332(3) 0.0389(13) Uani 1 1 d . . .
H10 H -0.0059 -0.2676 0.3059 0.047 Uiso 1 1 calc R . .
C11 C 0.4965(10) -0.2358(3) 0.4061(3) 0.0335(12) Uani 1 1 d . . .
H11 H 0.6299 -0.2687 0.4310 0.040 Uiso 1 1 calc R . .
C12 C 0.4996(10) -0.1394(3) 0.4112(3) 0.0324(11) Uani 1 1 d . . .
H12 H 0.6341 -0.1084 0.4376 0.039 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.110(4) . ?
O1 C7 1.209(5) . ?
N1 C7 1.330(8) . ?
N1 C8 1.427(4) . ?
N1 HN1 0.8600 . ?
C1 C6 1.376(6) . ?
C1 C2 1.390(6) . ?
N2 C10 1.315(6) . ?
N2 C11 1.343(6) . ?
C2 C3 1.388(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(6) . ?
C4 C7 1.514(5) . ?
C5 C6 1.386(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.372(6) . ?
C8 C12 1.373(6) . ?
C9 C10 1.404(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?

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
C7 N1 C8 127.0(6) . . ?
C7 N1 H20 116.5 . . ?
C8 N1 H20 116.5 . . ?
C6 C1 C2 120.6(4) . . ?
C6 C1 I1 119.9(3) . . ?
C2 C1 I1 119.5(3) . . ?
C10 N2 C11 116.5(4) . . ?
C3 C2 C1 120.0(5) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 C7 118.0(4) . . ?
C3 C4 C7 122.4(4) . . ?
C4 C5 C6 121.3(5) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 119.0(5) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
O1 C7 N1 123.4(4) . . ?
O1 C7 C4 121.0(4) . . ?
N1 C7 C4 115.6(4) . . ?
C9 C8 C12 119.2(4) . . ?
C9 C8 N1 120.6(5) . . ?
C12 C8 N1 120.1(5) . . ?
C8 C9 C10 117.4(5) . . ?
C8 C9 H9 121.3 . . ?
C10 C9 H9 121.3 . . ?
N2 C10 C9 124.6(5) . . ?
N2 C10 H10 117.7 . . ?
C9 C10 H10 117.7 . . ?
N2 C11 C12 123.3(5) . . ?
N2 C11 H11 118.3 . . ?
C12 C11 H11 118.3 . . ?
C8 C12 C11 118.9(5) . . ?
C8 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?

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
C6 C1 C2 C3 0.7(7) . . . . ?
I1 C1 C2 C3 -179.4(4) . . . . ?
C1 C2 C3 C4 0.3(7) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C2 C3 C4 C7 177.1(4) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C7 C4 C5 C6 -178.1(4) . . . . ?
C2 C1 C6 C5 -1.6(7) . . . . ?
I1 C1 C6 C5 178.5(4) . . . . ?
C4 C5 C6 C1 1.6(7) . . . . ?
C8 N1 C7 O1 3.5(8) . . . . ?
C8 N1 C7 C4 -177.3(4) . . . . ?
C5 C4 C7 O1 25.0(7) . . . . ?
C3 C4 C7 O1 -152.4(5) . . . . ?
C5 C4 C7 N1 -154.2(4) . . . . ?
C3 C4 C7 N1 28.4(7) . . . . ?
C7 N1 C8 C9 33.7(7) . . . . ?
C7 N1 C8 C12 -149.4(5) . . . . ?
C12 C8 C9 C10 1.5(7) . . . . ?
N1 C8 C9 C10 178.5(5) . . . . ?
C11 N2 C10 C9 0.1(8) . . . . ?
C8 C9 C10 N2 -0.6(8) . . . . ?
C10 N2 C11 C12 -0.6(8) . . . . ?
C9 C8 C12 C11 -2.0(7) . . . . ?
N1 C8 C12 C11 -178.9(4) . . . . ?
N2 C11 C12 C8 1.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.913
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.913
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.099
####################################################################### 
# 
# 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_xcalibur_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1423797'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jan 10 12:17:29 2012'
;
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H9 Hg I3 N2 O'
_chemical_formula_weight         778.50

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_cell_setting           monoclinic

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                   4.3030(12)
_cell_length_b                   14.824(5)
_cell_length_c                   25.840(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1648.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1302
_cell_measurement_theta_min      3.1471
_cell_measurement_theta_max      28.7650
_cell_oxdiff_length_a            4.3088(3)
_cell_oxdiff_length_b            14.8042(15)
_cell_oxdiff_length_c            25.843(3)
_cell_oxdiff_angle_alpha         89.980(9)
_cell_oxdiff_angle_beta          90.876(7)
_cell_oxdiff_angle_gamma         89.981(7)
_cell_oxdiff_volume              1648.3(3)
_cell_oxdiff_measurement_reflns_used 1302
_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    14.950
_exptl_absorpt_correction_T_min  0.67605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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 16.3990
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5264
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.00
_diffrn_orient_matrix_UB_11      -0.0171919000
_diffrn_orient_matrix_UB_12      -0.0418874000
_diffrn_orient_matrix_UB_13      0.0129753000
_diffrn_orient_matrix_UB_21      0.0086595000
_diffrn_orient_matrix_UB_22      0.0225715000
_diffrn_orient_matrix_UB_23      0.0241840000
_diffrn_orient_matrix_UB_31      -0.1635076000
_diffrn_orient_matrix_UB_32      0.0056160000
_diffrn_orient_matrix_UB_33      -0.0005058000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2740  -99.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega -100.00  -44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2740 -179.0000 -180.0000 56

#__ type_ start__ end____ width___ exp.time_
  3 omega  -46.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.7427  -19.0000  -60.0000 123

;
_reflns_number_total             2884
_reflns_number_gt                2172
_reflns_threshold_expression     >2sigma(I)


_computing_structure_solution    'SHELXTL Bruker'
_computing_structure_refinement  'SHELXTL Bruker'
_computing_molecular_graphics    'SHELXTL Bruker'
_computing_publication_material  'SHELXTL Bruker'

_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)+(0.0284P)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    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2884
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.004
_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
Hg1 Hg -0.58527(10) 1.19051(3) 0.248703(18) 0.04932(17) Uani 1 1 d . . .
O1 O -0.250(2) 0.9395(6) 0.0170(3) 0.064(2) Uani 1 1 d . . .
C1 C 0.239(2) 0.6546(7) -0.0408(4) 0.035(3) Uani 1 1 d . . .
I1 I 0.41625(16) 0.54864(5) -0.08564(3) 0.0473(2) Uani 1 1 d . . .
N1 N -0.214(2) 0.8627(6) 0.0928(4) 0.052(3) Uani 1 1 d . . .
H20 H -0.1615 0.8121 0.1066 0.062 Uiso 1 1 calc R . .
N2 N -0.5202(19) 1.0613(6) 0.1959(4) 0.045(2) Uani 1 1 d . . .
I2 I -0.99414(15) 1.28926(5) 0.19579(3) 0.0449(2) Uani 1 1 d . . .
C2 C 0.073(2) 0.6373(7) 0.0028(4) 0.040(3) Uani 1 1 d . . .
H2 H 0.0481 0.5779 0.0135 0.049 Uiso 1 1 calc R . .
I3 I -0.29941(17) 1.15891(6) 0.33775(3) 0.0551(3) Uani 1 1 d . . .
C3 C -0.058(2) 0.7054(7) 0.0314(4) 0.038(3) Uani 1 1 d . . .
H3 H -0.1668 0.6923 0.0616 0.046 Uiso 1 1 calc R . .
C4 C -0.026(2) 0.7928(7) 0.0150(4) 0.033(2) Uani 1 1 d . . .
C5 C 0.144(2) 0.8116(7) -0.0297(4) 0.042(3) Uani 1 1 d . . .
H5 H 0.1665 0.8708 -0.0410 0.050 Uiso 1 1 calc R . .
C6 C 0.277(2) 0.7430(9) -0.0568(4) 0.047(3) Uani 1 1 d . . .
H6 H 0.3934 0.7556 -0.0862 0.056 Uiso 1 1 calc R . .
C7 C -0.175(2) 0.8713(8) 0.0402(5) 0.045(3) Uani 1 1 d . . .
C8 C -0.331(2) 0.9285(8) 0.1257(4) 0.042(3) Uani 1 1 d . . .
C9 C -0.518(2) 1.0033(8) 0.1100(5) 0.044(3) Uani 1 1 d . . .
H9 H -0.5799 1.0095 0.0757 0.052 Uiso 1 1 calc R . .
C10 C -0.604(2) 1.0654(8) 0.1460(4) 0.046(3) Uani 1 1 d . . .
H10 H -0.7275 1.1134 0.1354 0.055 Uiso 1 1 calc R . .
C11 C -0.346(3) 0.9917(8) 0.2115(4) 0.048(3) Uani 1 1 d . . .
H11 H -0.2874 0.9884 0.2461 0.058 Uiso 1 1 calc R . .
C12 C -0.252(3) 0.9265(8) 0.1790(4) 0.047(3) Uani 1 1 d . . .
H12 H -0.1324 0.8791 0.1917 0.056 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 N2 2.369(9) . ?
Hg1 I3 2.6509(10) . ?
Hg1 I2 2.6661(10) . ?
Hg1 I2 3.2377(11) 1_655 ?
O1 C7 1.217(13) . ?
C1 C2 1.356(14) . ?
C1 C6 1.384(16) . ?
C1 I1 2.096(11) . ?
N1 C7 1.377(14) . ?
N1 C8 1.386(14) . ?
N2 C11 1.337(13) . ?
N2 C10 1.339(13) . ?
I2 Hg1 3.2377(11) 1_455 ?
C2 C3 1.373(14) . ?
C3 C4 1.371(14) . ?
C4 C5 1.397(15) . ?
C4 C7 1.479(15) . ?
C5 C6 1.359(15) . ?
C8 C12 1.419(14) . ?
C8 C9 1.430(15) . ?
C9 C10 1.359(15) . ?
C11 C12 1.343(15) . ?

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
N2 Hg1 I3 107.6(2) . . ?
N2 Hg1 I2 103.1(2) . . ?
I3 Hg1 I2 148.04(3) . . ?
N2 Hg1 I2 91.7(2) . 1_655 ?
I3 Hg1 I2 94.70(3) . 1_655 ?
I2 Hg1 I2 93.07(3) . 1_655 ?
C2 C1 C6 119.3(11) . . ?
C2 C1 I1 120.5(8) . . ?
C6 C1 I1 120.1(8) . . ?
C7 N1 C8 125.7(10) . . ?
C11 N2 C10 118.4(10) . . ?
C11 N2 Hg1 121.1(7) . . ?
C10 N2 Hg1 119.1(8) . . ?
Hg1 I2 Hg1 93.07(3) . 1_455 ?
C1 C2 C3 121.7(10) . . ?
C4 C3 C2 119.1(10) . . ?
C3 C4 C5 119.8(10) . . ?
C3 C4 C7 124.4(10) . . ?
C5 C4 C7 115.8(10) . . ?
C6 C5 C4 119.8(11) . . ?
C5 C6 C1 120.3(11) . . ?
O1 C7 N1 122.0(12) . . ?
O1 C7 C4 123.5(11) . . ?
N1 C7 C4 114.5(10) . . ?
N1 C8 C12 119.6(10) . . ?
N1 C8 C9 125.2(10) . . ?
C12 C8 C9 115.2(11) . . ?
C10 C9 C8 119.0(11) . . ?
N2 C10 C9 123.7(11) . . ?
N2 C11 C12 122.4(10) . . ?
C11 C12 C8 121.4(11) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.161
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.233
####################################################################### 
# 
# 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_d705a
_database_code_depnum_ccdc_archive 'CCDC 1423799'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 I2 N4 O6 Zn'
_chemical_formula_weight         955.81

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic'
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   14.2615(6)
_cell_length_b                   8.9996(3)
_cell_length_c                   29.6078(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3800.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9925
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.25

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1872
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4571
_exptl_absorpt_correction_T_max  0.6539
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'D8 VENTURE'
_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            40876
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3879
_reflns_number_gt                3390
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS)'
_computing_cell_refinement       'APEX2 v2013.6--2 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL--2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0317P)²+10.2353P] 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         3879
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Zn1 Zn 0.5000 0.06814(5) 0.2500 0.01888(12) Uani 1 2 d S . .
I1 I -0.122240(18) 0.77593(3) -0.004500(8) 0.04067(9) Uani 1 1 d . . .
O2 O 0.59154(14) -0.0305(2) 0.21022(7) 0.0257(5) Uani 1 1 d . . .
N2 N 0.40917(16) 0.2134(3) 0.21993(8) 0.0208(5) Uani 1 1 d . . .
C13 C 0.54674(19) -0.1204(3) 0.18493(9) 0.0203(6) Uani 1 1 d . . .
O3 O 0.45937(14) -0.1280(2) 0.18528(7) 0.0257(5) Uani 1 1 d . . .
N1 N 0.21262(18) 0.4594(3) 0.14619(8) 0.0214(5) Uani 1 1 d . . .
H1 H 0.159(2) 0.438(4) 0.1534(11) 0.019(8) Uiso 1 1 d . . .
C14 C 0.6024(2) -0.2186(3) 0.15411(10) 0.0231(6) Uani 1 1 d . . .
O1 O 0.30363(15) 0.6114(3) 0.10275(8) 0.0321(5) Uani 1 1 d . . .
C19 C 0.5557(2) -0.3151(4) 0.12503(11) 0.0290(7) Uani 1 1 d . . .
H19 H 0.488(2) -0.315(4) 0.1254(11) 0.026(9) Uiso 1 1 d . . .
C18 C 0.6061(3) -0.4066(4) 0.09634(13) 0.0381(8) Uani 1 1 d . . .
H18 H 0.575(3) -0.471(5) 0.0752(14) 0.049(12) Uiso 1 1 d . . .
C17 C 0.7034(3) -0.4021(5) 0.09660(14) 0.0463(10) Uani 1 1 d . . .
H17 H 0.739(3) -0.465(5) 0.0764(14) 0.058(13) Uiso 1 1 d . . .
C16 C 0.7497(3) -0.3071(5) 0.12549(15) 0.0484(10) Uani 1 1 d . . .
H16 H 0.815(3) -0.301(5) 0.1261(16) 0.071(15) Uiso 1 1 d . . .
C15 C 0.6995(2) -0.2145(4) 0.15419(12) 0.0352(8) Uani 1 1 d . . .
H15 H 0.730(2) -0.148(4) 0.1730(12) 0.034(10) Uiso 1 1 d . . .
C10 C 0.3163(2) 0.2071(3) 0.22865(10) 0.0218(6) Uani 1 1 d . . .
H10 H 0.300(2) 0.137(4) 0.2530(11) 0.031(9) Uiso 1 1 d . . .
C9 C 0.2512(2) 0.2905(3) 0.20572(9) 0.0215(6) Uani 1 1 d . . .
H9 H 0.188(2) 0.282(4) 0.2132(11) 0.025(9) Uiso 1 1 d . . .
C8 C 0.28092(19) 0.3861(3) 0.17130(9) 0.0202(6) Uani 1 1 d . . .
C12 C 0.3773(2) 0.3979(4) 0.16353(11) 0.0274(7) Uani 1 1 d . . .
H12 H 0.399(2) 0.459(4) 0.1432(12) 0.033(10) Uiso 1 1 d . . .
C11 C 0.4369(2) 0.3096(4) 0.18831(11) 0.0273(7) Uani 1 1 d . . .
H11 H 0.499(3) 0.312(4) 0.1834(13) 0.041(10) Uiso 1 1 d . . .
C7 C 0.2267(2) 0.5606(3) 0.11220(10) 0.0230(6) Uani 1 1 d . . .
C4 C 0.1405(2) 0.6068(3) 0.08680(9) 0.0231(6) Uani 1 1 d . . .
C5 C 0.0589(2) 0.5228(3) 0.08496(10) 0.0245(6) Uani 1 1 d . . .
H5 H 0.055(2) 0.433(4) 0.0995(11) 0.022(8) Uiso 1 1 d . . .
C6 C -0.0172(2) 0.5702(4) 0.05944(11) 0.0279(7) Uani 1 1 d . . .
H6 H -0.069(3) 0.515(4) 0.0589(11) 0.031(9) Uiso 1 1 d . . .
C1 C -0.0108(2) 0.7036(4) 0.03619(10) 0.0293(7) Uani 1 1 d . . .
C2 C 0.0698(3) 0.7881(4) 0.03750(11) 0.0317(7) Uani 1 1 d . . .
H2 H 0.074(3) 0.883(5) 0.0209(14) 0.052(12) Uiso 1 1 d . . .
C3 C 0.1457(2) 0.7396(4) 0.06278(11) 0.0291(7) Uani 1 1 d . . .
H3 H 0.200(2) 0.795(4) 0.0642(11) 0.026(9) Uiso 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
Zn1 O2 1.970(2) . ?
Zn1 O2 1.970(2) 3_655 ?
Zn1 N2 2.045(2) 3_655 ?
Zn1 N2 2.045(2) . ?
I1 C1 2.097(3) . ?
O2 C13 1.275(3) . ?
N2 C11 1.335(4) . ?
N2 C10 1.351(4) . ?
C13 O3 1.248(3) . ?
C13 C14 1.498(4) . ?
N1 C7 1.372(4) . ?
N1 C8 1.391(4) . ?
C14 C15 1.386(4) . ?
C14 C19 1.392(4) . ?
O1 C7 1.221(4) . ?
C19 C18 1.384(5) . ?
C18 C17 1.388(5) . ?
C17 C16 1.378(6) . ?
C16 C15 1.389(5) . ?
C10 C9 1.374(4) . ?
C9 C8 1.399(4) . ?
C8 C12 1.398(4) . ?
C12 C11 1.376(4) . ?
C7 C4 1.500(4) . ?
C4 C5 1.388(4) . ?
C4 C3 1.393(4) . ?
C5 C6 1.389(4) . ?
C6 C1 1.387(5) . ?
C1 C2 1.379(5) . ?
C2 C3 1.386(5) . ?

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 Zn1 O2 126.44(13) . 3_655 ?
O2 Zn1 N2 97.39(9) . 3_655 ?
O2 Zn1 N2 116.60(9) 3_655 3_655 ?
O2 Zn1 N2 116.60(9) . . ?
O2 Zn1 N2 97.39(9) 3_655 . ?
N2 Zn1 N2 100.49(14) 3_655 . ?
C13 O2 Zn1 107.77(17) . . ?
C11 N2 C10 116.9(3) . . ?
C11 N2 Zn1 122.1(2) . . ?
C10 N2 Zn1 120.7(2) . . ?
O3 C13 O2 122.0(3) . . ?
O3 C13 C14 120.1(3) . . ?
O2 C13 C14 117.8(2) . . ?
C7 N1 C8 127.1(3) . . ?
C15 C14 C19 119.7(3) . . ?
C15 C14 C13 120.9(3) . . ?
C19 C14 C13 119.4(3) . . ?
C18 C19 C14 120.2(3) . . ?
C19 C18 C17 119.8(3) . . ?
C16 C17 C18 120.1(4) . . ?
C17 C16 C15 120.3(4) . . ?
C14 C15 C16 119.9(3) . . ?
N2 C10 C9 123.1(3) . . ?
C10 C9 C8 119.4(3) . . ?
N1 C8 C12 124.4(3) . . ?
N1 C8 C9 117.9(2) . . ?
C12 C8 C9 117.7(3) . . ?
C11 C12 C8 118.5(3) . . ?
N2 C11 C12 124.4(3) . . ?
O1 C7 N1 123.3(3) . . ?
O1 C7 C4 121.2(3) . . ?
N1 C7 C4 115.5(3) . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 C7 123.8(3) . . ?
C3 C4 C7 116.8(3) . . ?
C4 C5 C6 120.6(3) . . ?
C1 C6 C5 119.0(3) . . ?
C2 C1 C6 121.2(3) . . ?
C2 C1 I1 118.5(2) . . ?
C6 C1 I1 120.3(3) . . ?
C1 C2 C3 119.5(3) . . ?
C2 C3 C4 120.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.089
####################################################################### 
# 
# 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_xcalibur_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1423796'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Jul 24 12:36:11 2013'
;
_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Ag I2 N5 O5'
_chemical_formula_weight         818.10

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_space_group_name_H-M   'P -1'
_symmetry_cell_setting           Triclinic

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

_cell_length_a                   9.3872(5)
_cell_length_b                   11.4744(4)
_cell_length_c                   13.2529(6)
_cell_angle_alpha                107.591(4)
_cell_angle_beta                 110.075(5)
_cell_angle_gamma                94.437(4)
_cell_volume                     1251.65(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    291.88(10)
_cell_measurement_reflns_used    5128
_cell_measurement_theta_min      1.8940
_cell_measurement_theta_max      28.0000
_cell_oxdiff_length_a            9.3872(5)
_cell_oxdiff_length_b            11.4744(4)
_cell_oxdiff_length_c            13.2529(6)
_cell_oxdiff_angle_alpha         107.591(4)
_cell_oxdiff_angle_beta          110.075(5)
_cell_oxdiff_angle_gamma         94.437(3)
_cell_oxdiff_volume              1251.65(9)
_cell_oxdiff_measurement_reflns_used 5128

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    3.318
_exptl_absorpt_correction_T_min  0.79551
_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      291.88(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8687
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         26.37
_diffrn_orient_matrix_UB_11      0.0550586000
_diffrn_orient_matrix_UB_12      -0.0016972000
_diffrn_orient_matrix_UB_13      -0.0257880000
_diffrn_orient_matrix_UB_21      -0.0609489000
_diffrn_orient_matrix_UB_22      -0.0209614000
_diffrn_orient_matrix_UB_23      -0.0550134000
_diffrn_orient_matrix_UB_31      -0.0013358000
_diffrn_orient_matrix_UB_32      0.0627890000
_diffrn_orient_matrix_UB_33      0.0034706000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    5.00   99.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767   57.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega   18.00   59.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -38.0000    0.0000 41

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00  105.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000   60.0000 70

#__ type_ start__ end____ width___ exp.time_
  4 omega  -52.00   56.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -38.0000  120.0000 108

#__ type_ start__ end____ width___ exp.time_
  5 omega   54.00   90.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767 -127.0000   27.0000 36

#__ type_ start__ end____ width___ exp.time_
  6 omega   11.00   96.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767   38.0000   60.0000 85

#__ type_ start__ end____ width___ exp.time_
  7 omega   73.00  106.00   1.0000    2.3500
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000 -120.0000 33

;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             5123
_reflns_number_gt                4616
_reflns_threshold_expression     >2sigma(I)


_computing_structure_solution    'SHELXTl Bruker-97'
_computing_structure_refinement  'SHELXTl Bruker-97'
_computing_molecular_graphics    'SHELXTl Bruker-97'
_computing_publication_material  'SHELXTl Bruker-97'

_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)+(0.0277P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5123
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0677
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.009
_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
Ag1 Ag 0.46638(3) 0.75628(2) 0.69941(2) 0.01700(8) Uani 1 1 d . . .
I1 I 1.45918(3) 1.81445(2) 0.97886(2) 0.02065(8) Uani 1 1 d . . .
O1 O 1.1314(3) 1.2643(2) 1.0205(2) 0.0208(6) Uani 1 1 d . . .
N1 N 0.6123(4) 0.9372(3) 0.7735(2) 0.0145(7) Uani 1 1 d . . .
C1 C 0.5759(5) 1.0245(3) 0.7244(3) 0.0154(8) Uani 1 1 d . . .
H1 H 0.4787 1.0094 0.6666 0.018 Uiso 1 1 calc R . .
I2 I -0.21188(3) -0.34609(2) 0.65938(2) 0.01577(7) Uani 1 1 d . . .
O2 O 0.3093(4) 0.1670(3) 0.7287(3) 0.0334(8) Uani 1 1 d . . .
C2 C 0.6771(4) 1.1345(3) 0.7567(3) 0.0134(8) Uani 1 1 d . . .
H2 H 0.6472 1.1926 0.7217 0.016 Uiso 1 1 calc R . .
N2 N 0.9261(4) 1.2683(3) 0.8663(2) 0.0157(7) Uani 1 1 d . . .
HN2 H 0.8944 1.3111 0.8227 0.019 Uiso 1 1 calc R . .
O3 O 0.4433(3) 0.7439(3) 0.4757(2) 0.0318(7) Uani 1 1 d . . .
N3 N 0.3343(4) 0.5737(2) 0.6522(2) 0.0149(7) Uani 1 1 d . . .
C3 C 0.8246(5) 1.1591(3) 0.8419(3) 0.0138(8) Uani 1 1 d . . .
N4 N 0.1000(4) 0.2388(3) 0.6397(2) 0.0130(6) Uani 1 1 d . . .
HN4 H 0.0005 0.2249 0.6098 0.016 Uiso 1 1 calc R . .
O4 O 0.2299(3) 0.7781(2) 0.4967(2) 0.0257(7) Uani 1 1 d . . .
C4 C 0.8600(5) 1.0708(3) 0.8961(3) 0.0163(8) Uani 1 1 d . . .
H4 H 0.9548 1.0848 0.9561 0.020 Uiso 1 1 calc R . .
O5 O 0.2240(4) 0.6495(3) 0.3351(2) 0.0313(8) Uani 1 1 d . . .
N5 N 0.3005(4) 0.7247(3) 0.4361(3) 0.0184(7) Uani 1 1 d . . .
C5 C 0.7515(5) 0.9633(3) 0.8584(3) 0.0168(8) Uani 1 1 d . . .
H5 H 0.7764 0.9052 0.8942 0.020 Uiso 1 1 calc R . .
C6 C 1.0723(4) 1.3159(3) 0.9527(3) 0.0156(8) Uani 1 1 d . . .
C7 C 1.1548(5) 1.4373(3) 0.9593(3) 0.0150(8) Uani 1 1 d . . .
C8 C 1.0893(5) 1.5054(3) 0.8902(3) 0.0174(8) Uani 1 1 d . . .
H8 H 0.9870 1.4777 0.8381 0.021 Uiso 1 1 calc R . .
C9 C 1.1760(5) 1.6142(3) 0.8988(3) 0.0196(9) Uani 1 1 d . . .
H9 H 1.1319 1.6589 0.8522 0.023 Uiso 1 1 calc R . .
C10 C 1.3270(5) 1.6558(3) 0.9761(3) 0.0149(8) Uani 1 1 d . . .
C11 C 1.3927(5) 1.5929(3) 1.0499(3) 0.0225(9) Uani 1 1 d . . .
H11 H 1.4933 1.6232 1.1046 0.027 Uiso 1 1 calc R . .
C12 C 1.3053(5) 1.4844(3) 1.0402(3) 0.0203(9) Uani 1 1 d . . .
H12 H 1.3484 1.4419 1.0891 0.024 Uiso 1 1 calc R . .
C13 C 0.4090(5) 0.4804(3) 0.6654(3) 0.0179(8) Uani 1 1 d . . .
H13 H 0.5140 0.4928 0.6789 0.021 Uiso 1 1 calc R . .
C14 C 0.3385(5) 0.3675(3) 0.6600(3) 0.0162(8) Uani 1 1 d . . .
H14 H 0.3949 0.3055 0.6688 0.019 Uiso 1 1 calc R . .
C15 C 0.1821(4) 0.3473(3) 0.6414(3) 0.0132(8) Uani 1 1 d . . .
C16 C 0.1024(5) 0.4414(3) 0.6223(3) 0.0151(8) Uani 1 1 d . . .
H16 H -0.0035 0.4303 0.6053 0.018 Uiso 1 1 calc R . .
C17 C 0.1826(5) 0.5507(3) 0.6289(3) 0.0152(8) Uani 1 1 d . . .
H17 H 0.1278 0.6125 0.6163 0.018 Uiso 1 1 calc R . .
C18 C 0.1689(5) 0.1528(3) 0.6832(3) 0.0173(8) Uani 1 1 d . . .
C19 C 0.0655(5) 0.0412(3) 0.6747(3) 0.0156(8) Uani 1 1 d . . .
C20 C 0.1406(5) -0.0287(3) 0.7399(3) 0.0214(9) Uani 1 1 d . . .
H20 H 0.2456 -0.0022 0.7858 0.026 Uiso 1 1 calc R . .
C21 C 0.0588(5) -0.1370(3) 0.7363(3) 0.0206(9) Uani 1 1 d . . .
H21 H 0.1085 -0.1824 0.7804 0.025 Uiso 1 1 calc R . .
C22 C -0.0973(5) -0.1771(3) 0.6664(3) 0.0144(8) Uani 1 1 d . . .
C23 C -0.1743(5) -0.1093(3) 0.6013(3) 0.0159(8) Uani 1 1 d . . .
H23 H -0.2792 -0.1363 0.5551 0.019 Uiso 1 1 calc R . .
C24 C -0.0904(5) 0.0001(3) 0.6067(3) 0.0151(8) Uani 1 1 d . . .
H24 H -0.1407 0.0462 0.5636 0.018 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.134(3) . ?
Ag1 N3 2.142(3) . ?
I1 C10 2.105(4) . ?
O1 C6 1.223(4) . ?
N1 C5 1.338(5) . ?
N1 C1 1.356(4) . ?
C1 C2 1.374(5) . ?
I2 C22 2.104(3) . ?
O2 C18 1.220(5) . ?
C2 C3 1.394(5) . ?
N2 C6 1.386(5) . ?
N2 C3 1.393(4) . ?
O3 N5 1.234(4) . ?
N3 C17 1.335(5) . ?
N3 C13 1.347(5) . ?
C3 C4 1.408(5) . ?
N4 C18 1.382(5) . ?
N4 C15 1.404(4) . ?
O4 N5 1.262(4) . ?
C4 C5 1.375(5) . ?
O5 N5 1.264(4) . ?
C6 C7 1.504(5) . ?
C7 C12 1.389(5) . ?
C7 C8 1.396(5) . ?
C8 C9 1.389(5) . ?
C9 C10 1.375(5) . ?
C10 C11 1.393(5) . ?
C11 C12 1.382(5) . ?
C13 C14 1.379(5) . ?
C14 C15 1.391(5) . ?
C15 C16 1.397(5) . ?
C16 C17 1.375(5) . ?
C18 C19 1.496(5) . ?
C19 C24 1.382(5) . ?
C19 C20 1.405(5) . ?
C20 C21 1.388(5) . ?
C21 C22 1.387(5) . ?
C22 C23 1.392(5) . ?
C23 C24 1.398(5) . ?

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
N1 Ag1 N3 170.85(10) . . ?
C5 N1 C1 117.2(3) . . ?
C5 N1 Ag1 121.9(2) . . ?
C1 N1 Ag1 120.2(2) . . ?
N1 C1 C2 122.5(3) . . ?
C1 C2 C3 120.1(3) . . ?
C6 N2 C3 127.5(3) . . ?
C17 N3 C13 116.4(3) . . ?
C17 N3 Ag1 123.4(2) . . ?
C13 N3 Ag1 119.2(3) . . ?
N2 C3 C2 117.8(3) . . ?
N2 C3 C4 124.9(3) . . ?
C2 C3 C4 117.3(3) . . ?
C18 N4 C15 124.1(3) . . ?
C5 C4 C3 118.6(3) . . ?
O3 N5 O4 120.3(3) . . ?
O3 N5 O5 120.1(4) . . ?
O4 N5 O5 119.6(4) . . ?
N1 C5 C4 124.1(3) . . ?
O1 C6 N2 123.0(3) . . ?
O1 C6 C7 121.4(3) . . ?
N2 C6 C7 115.6(3) . . ?
C12 C7 C8 118.4(3) . . ?
C12 C7 C6 117.5(3) . . ?
C8 C7 C6 124.2(3) . . ?
C9 C8 C7 120.3(4) . . ?
C10 C9 C8 120.0(3) . . ?
C9 C10 C11 120.7(3) . . ?
C9 C10 I1 118.9(3) . . ?
C11 C10 I1 120.4(3) . . ?
C12 C11 C10 118.6(4) . . ?
C11 C12 C7 121.8(3) . . ?
N3 C13 C14 123.7(4) . . ?
C13 C14 C15 119.2(3) . . ?
C14 C15 C16 117.4(3) . . ?
C14 C15 N4 124.3(3) . . ?
C16 C15 N4 118.3(3) . . ?
C17 C16 C15 119.1(4) . . ?
N3 C17 C16 124.2(3) . . ?
O2 C18 N4 121.8(3) . . ?
O2 C18 C19 120.3(3) . . ?
N4 C18 C19 117.9(3) . . ?
C24 C19 C20 119.0(3) . . ?
C24 C19 C18 126.3(3) . . ?
C20 C19 C18 114.7(3) . . ?
C21 C20 C19 120.4(4) . . ?
C22 C21 C20 119.6(3) . . ?
C21 C22 C23 121.1(3) . . ?
C21 C22 I2 117.6(3) . . ?
C23 C22 I2 121.3(3) . . ?
C22 C23 C24 118.6(4) . . ?
C19 C24 C23 121.4(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.134
####################################################################### 
# 
# 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_xcalibur_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1423798'
_audit_update_record             
;
2015-09-11 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Apr 22 14:04:04 2013'
;
_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Br2 I2 N4 O2 Zn'
_chemical_formula_weight         873.41

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
Zn Zn -1.5491 0.6778 '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'

_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_cell_setting           Monoclinic

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                   9.7184(2)
_cell_length_b                   27.7576(6)
_cell_length_c                   9.8707(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.040(2)
_cell_angle_gamma                90.00
_cell_volume                     2662.27(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    9757
_cell_measurement_theta_min      3.1450
_cell_measurement_theta_max      73.9270
_cell_oxdiff_length_a            9.7179(3)
_cell_oxdiff_length_b            27.7641(7)
_cell_oxdiff_length_c            9.8689(3)
_cell_oxdiff_angle_alpha         89.959(2)
_cell_oxdiff_angle_beta          91.051(2)
_cell_oxdiff_angle_gamma         89.978(2)
_cell_oxdiff_volume              2662.27(13)
_cell_oxdiff_measurement_reflns_used 9757

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_exptl_absorpt_coefficient_mu    23.252
_exptl_absorpt_correction_T_min  0.23460
_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.
;

_diffrn_ambient_temperature      100.00(10)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_detector_area_resol_mean 10.4023
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20071
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         74.29
_diffrn_orient_matrix_UB_11      0.1166419000
_diffrn_orient_matrix_UB_12      -0.0216438000
_diffrn_orient_matrix_UB_13      -0.0843269000
_diffrn_orient_matrix_UB_21      0.1065345000
_diffrn_orient_matrix_UB_22      0.0175424000
_diffrn_orient_matrix_UB_23      0.1064201000
_diffrn_orient_matrix_UB_31      -0.0135915000
_diffrn_orient_matrix_UB_32      -0.0479863000
_diffrn_orient_matrix_UB_33      0.0770703000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -39.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  125.0000   60.0000 35

#__ type_ start__ end____ width___ exp.time_
  2 omega   15.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
  3 omega   40.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000  -60.0000 67

#__ type_ start__ end____ width___ exp.time_
  4 omega -152.00 -126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -61.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   81.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   30.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
  6 omega  122.00  151.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   30.0000   30.0000 29

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000   90.0000 30

#__ type_ start__ end____ width___ exp.time_
  8 omega   39.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   41.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -30.0000 36

#__ type_ start__ end____ width___ exp.time_
 10 omega   43.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000  -30.0000 77

#__ type_ start__ end____ width___ exp.time_
 11 omega   30.00   58.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
 12 omega   36.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
 13 omega   84.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000  -60.0000 74

#__ type_ start__ end____ width___ exp.time_
 14 omega  120.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000 -180.0000 32

#__ type_ start__ end____ width___ exp.time_
 15 omega   33.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
 16 omega   45.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega  -90.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  125.0000  120.0000 80

#__ type_ start__ end____ width___ exp.time_
 18 omega -107.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  -40.0000   64.0000 58

#__ type_ start__ end____ width___ exp.time_
 19 omega   49.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
 20 omega  -49.00   -6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   30.0000  -60.0000 43

#__ type_ start__ end____ width___ exp.time_
 21 omega   93.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 22 omega   27.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -180.0000 81

#__ type_ start__ end____ width___ exp.time_
 23 omega   36.00   80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000 -150.0000 44

#__ type_ start__ end____ width___ exp.time_
 24 omega   97.00  147.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   77.0000 -120.0000 50

#__ type_ start__ end____ width___ exp.time_
 25 omega   37.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  150.0000 40

#__ type_ start__ end____ width___ exp.time_
 26 omega  119.00  157.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   40.0000 -141.0000 38

#__ type_ start__ end____ width___ exp.time_
 27 omega   49.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000   60.0000 42

#__ type_ start__ end____ width___ exp.time_
 28 omega   38.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000    0.0000 58

#__ type_ start__ end____ width___ exp.time_
 29 omega   94.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
 30 omega   44.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  120.0000 47

;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             5330
_reflns_number_gt                5079
_reflns_threshold_expression     >2sigma(I)


_computing_structure_solution    'SHELXTL Bruker'
_computing_structure_refinement  'SHELXTL Bruker'
_computing_molecular_graphics    'SHELXTL Bruker'
_computing_publication_material  'SHELXTL Bruker'

_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)+(0.0765P)²+11.2226P] 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         5330
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1287
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
I2 I -0.27495(4) 0.840073(16) 0.76534(5) 0.03462(14) Uani 1 1 d . . .
I1 I 0.61347(4) 0.388195(14) -0.43212(4) 0.02521(13) Uani 1 1 d . . .
Zn1 Zn 0.90661(8) 0.60505(3) 0.73128(7) 0.01636(17) Uani 1 1 d . . .
C22 C -0.0748(6) 0.8175(2) 0.7232(7) 0.0243(12) Uani 1 1 d . . .
C23 C -0.0335(7) 0.8117(2) 0.5898(6) 0.0251(12) Uani 1 1 d . . .
H23 H -0.0927 0.8193 0.5178 0.030 Uiso 1 1 calc R . .
O1 O 0.5569(5) 0.45643(16) 0.2546(4) 0.0246(9) Uani 1 1 d . . .
C21 C 0.0157(7) 0.8087(2) 0.8313(6) 0.0233(12) Uani 1 1 d . . .
H21 H -0.0109 0.8146 0.9198 0.028 Uiso 1 1 calc R . .
C24 C 0.0967(7) 0.7945(2) 0.5669(6) 0.0236(12) Uani 1 1 d . . .
H24 H 0.1252 0.7906 0.4782 0.028 Uiso 1 1 calc R . .
C20 C 0.1469(6) 0.7909(2) 0.8051(6) 0.0195(11) Uani 1 1 d . . .
H20 H 0.2079 0.7845 0.8765 0.023 Uiso 1 1 calc R . .
C19 C 0.1865(6) 0.7828(2) 0.6726(6) 0.0186(11) Uani 1 1 d . . .
C18 C 0.3226(6) 0.7606(2) 0.6395(5) 0.0174(10) Uani 1 1 d . . .
N3 N 0.7416(5) 0.65070(18) 0.7382(5) 0.0191(9) Uani 1 1 d . . .
N4 N 0.3860(5) 0.73641(17) 0.7429(5) 0.0190(9) Uani 1 1 d . . .
H4A H 0.3486 0.7386 0.8209 0.023 Uiso 1 1 calc R . .
O2 O 0.3680(5) 0.76226(17) 0.5252(4) 0.0253(9) Uani 1 1 d . . .
C15 C 0.5058(6) 0.7083(2) 0.7359(6) 0.0178(11) Uani 1 1 d . . .
C16 C 0.6086(7) 0.7154(2) 0.6401(7) 0.0254(12) Uani 1 1 d . . .
H16 H 0.5994 0.7389 0.5736 0.030 Uiso 1 1 calc R . .
C14 C 0.5236(7) 0.6716(2) 0.8302(7) 0.0273(13) Uani 1 1 d . . .
H14 H 0.4565 0.6658 0.8941 0.033 Uiso 1 1 calc R . .
C17 C 0.7232(7) 0.6865(2) 0.6470(6) 0.0247(12) Uani 1 1 d . . .
H17 H 0.7924 0.6919 0.5850 0.030 Uiso 1 1 calc R . .
Br2 Br 1.10996(6) 0.64983(2) 0.70664(6) 0.02350(16) Uani 1 1 d . . .
C13 C 0.6409(7) 0.6439(2) 0.8286(6) 0.0242(12) Uani 1 1 d . . .
H13 H 0.6511 0.6194 0.8924 0.029 Uiso 1 1 calc R . .
Br1 Br 0.87802(6) 0.55057(2) 0.91471(6) 0.02316(16) Uani 1 1 d . . .
N1 N 0.8682(5) 0.56605(16) 0.5595(5) 0.0175(9) Uani 1 1 d . . .
C1 C 0.9564(6) 0.5616(2) 0.4563(6) 0.0185(11) Uani 1 1 d . . .
H1 H 1.0400 0.5778 0.4619 0.022 Uiso 1 1 calc R . .
C5 C 0.7489(6) 0.5419(2) 0.5491(6) 0.0221(11) Uani 1 1 d . . .
H5 H 0.6872 0.5445 0.6197 0.027 Uiso 1 1 calc R . .
C2 C 0.9281(6) 0.5342(2) 0.3435(6) 0.0212(11) Uani 1 1 d . . .
H2 H 0.9917 0.5324 0.2745 0.025 Uiso 1 1 calc R . .
C4 C 0.7121(6) 0.5133(2) 0.4394(6) 0.0198(11) Uani 1 1 d . . .
H4 H 0.6283 0.4971 0.4370 0.024 Uiso 1 1 calc R . .
C3 C 0.8037(6) 0.5092(2) 0.3321(6) 0.0181(10) Uani 1 1 d . . .
N2 N 0.7756(5) 0.48285(17) 0.2157(5) 0.0195(9) Uani 1 1 d . . .
H2A H 0.8412 0.4809 0.1586 0.023 Uiso 1 1 calc R . .
C6 C 0.6551(6) 0.4593(2) 0.1800(6) 0.0200(11) Uani 1 1 d . . .
C7 C 0.6503(6) 0.4400(2) 0.0382(6) 0.0204(11) Uani 1 1 d . . .
C8 C 0.7644(6) 0.4212(2) -0.0261(6) 0.0198(11) Uani 1 1 d . . .
H8 H 0.8482 0.4190 0.0206 0.024 Uiso 1 1 calc R . .
C12 C 0.5248(6) 0.4430(2) -0.0322(6) 0.0200(11) Uani 1 1 d . . .
H12 H 0.4472 0.4542 0.0116 0.024 Uiso 1 1 calc R . .
C9 C 0.7544(6) 0.4056(2) -0.1593(6) 0.0201(11) Uani 1 1 d . . .
H9 H 0.8303 0.3924 -0.2017 0.024 Uiso 1 1 calc R . .
C11 C 0.5153(6) 0.4294(2) -0.1659(6) 0.0205(11) Uani 1 1 d . . .
H11 H 0.4327 0.4332 -0.2138 0.025 Uiso 1 1 calc R . .
C10 C 0.6284(7) 0.4101(2) -0.2291(6) 0.0209(11) 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
I2 C22 2.093(6) . ?
I1 C10 2.097(6) . ?
Zn1 N1 2.040(5) . ?
Zn1 N3 2.046(5) . ?
Zn1 Br2 2.3510(9) . ?
Zn1 Br1 2.3791(9) . ?
C22 C21 1.392(9) . ?
C22 C23 1.393(9) . ?
C23 C24 1.375(9) . ?
O1 C6 1.218(8) . ?
C21 C20 1.396(9) . ?
C24 C19 1.386(8) . ?
C20 C19 1.388(8) . ?
C19 C18 1.501(8) . ?
C18 O2 1.220(7) . ?
C18 N4 1.359(7) . ?
N3 C17 1.350(8) . ?
N3 C13 1.350(8) . ?
N4 C15 1.404(7) . ?
C15 C14 1.389(8) . ?
C15 C16 1.402(8) . ?
C16 C17 1.373(9) . ?
C14 C13 1.375(9) . ?
N1 C5 1.342(8) . ?
N1 C1 1.349(7) . ?
C1 C2 1.371(8) . ?
C5 C4 1.385(8) . ?
C2 C3 1.398(8) . ?
C4 C3 1.400(8) . ?
C3 N2 1.385(7) . ?
N2 C6 1.382(8) . ?
C6 C7 1.499(8) . ?
C7 C8 1.389(9) . ?
C7 C12 1.395(9) . ?
C8 C9 1.386(8) . ?
C12 C11 1.374(8) . ?
C9 C10 1.400(8) . ?
C11 C10 1.381(9) . ?

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
N1 Zn1 N3 103.0(2) . . ?
N1 Zn1 Br2 109.64(14) . . ?
N3 Zn1 Br2 109.68(15) . . ?
N1 Zn1 Br1 105.84(13) . . ?
N3 Zn1 Br1 105.42(14) . . ?
Br2 Zn1 Br1 121.65(4) . . ?
C21 C22 C23 121.1(6) . . ?
C21 C22 I2 118.4(5) . . ?
C23 C22 I2 120.5(5) . . ?
C24 C23 C22 118.5(6) . . ?
C22 C21 C20 119.1(5) . . ?
C23 C24 C19 121.8(6) . . ?
C19 C20 C21 120.1(5) . . ?
C24 C19 C20 119.3(6) . . ?
C24 C19 C18 118.6(5) . . ?
C20 C19 C18 122.1(5) . . ?
O2 C18 N4 123.2(5) . . ?
O2 C18 C19 121.3(5) . . ?
N4 C18 C19 115.4(5) . . ?
C17 N3 C13 117.1(5) . . ?
C17 N3 Zn1 121.9(4) . . ?
C13 N3 Zn1 120.9(4) . . ?
C18 N4 C15 127.0(5) . . ?
C14 C15 C16 118.2(5) . . ?
C14 C15 N4 117.9(5) . . ?
C16 C15 N4 123.9(5) . . ?
C17 C16 C15 118.2(5) . . ?
C13 C14 C15 119.8(6) . . ?
N3 C17 C16 124.1(5) . . ?
N3 C13 C14 122.6(5) . . ?
C5 N1 C1 117.1(5) . . ?
C5 N1 Zn1 118.3(4) . . ?
C1 N1 Zn1 124.5(4) . . ?
N1 C1 C2 122.9(5) . . ?
N1 C5 C4 123.9(5) . . ?
C1 C2 C3 120.1(6) . . ?
C5 C4 C3 118.6(5) . . ?
N2 C3 C2 119.1(5) . . ?
N2 C3 C4 123.5(5) . . ?
C2 C3 C4 117.4(5) . . ?
C6 N2 C3 128.0(5) . . ?
O1 C6 N2 123.1(5) . . ?
O1 C6 C7 122.0(5) . . ?
N2 C6 C7 114.8(5) . . ?
C8 C7 C12 119.5(5) . . ?
C8 C7 C6 123.3(5) . . ?
C12 C7 C6 117.1(5) . . ?
C9 C8 C7 120.5(5) . . ?
C11 C12 C7 120.3(6) . . ?
C8 C9 C10 119.0(5) . . ?
C12 C11 C10 120.0(6) . . ?
C11 C10 C9 120.6(5) . . ?
C11 C10 I1 120.2(4) . . ?
C9 C10 I1 119.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        74.29
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.895
_refine_diff_density_min         -2.123
_refine_diff_density_rms         0.211
