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

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

data_f:\solution\619-r-sol\kh619-r-abs1
_database_code_depnum_ccdc_archive 'CCDC 1015768'
_audit_update_record             
;
2014-07-23 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 Cl4 Hg2 N8 O2'
_chemical_formula_weight         1043.50

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'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   14.5287(5)
_cell_length_b                   14.0469(3)
_cell_length_c                   15.7245(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.798(3)
_cell_angle_gamma                90.00
_cell_volume                     2979.65(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    36823
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.18

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    10.692
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0221
_exptl_absorpt_correction_T_max  0.0421
_exptl_absorpt_process_details   'shape of crystal determined optically'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36823
_diffrn_reflns_av_R_equivalents  0.1113
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         29.18
_reflns_number_total             8021
_reflns_number_gt                6548
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (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)+(0.0368P)²+9.3675P] 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         8021
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1225
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.231
_refine_ls_shift/su_max          0.014
_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 0.3829(6) 1.4860(6) 0.5343(5) 0.0375(16) Uani 1 1 d . . .
H1 H 0.3990 1.5189 0.4904 0.045 Uiso 1 1 calc R . .
C2 C 0.3641(6) 1.5370(6) 0.6019(5) 0.0354(15) Uani 1 1 d . . .
H2 H 0.3707 1.6029 0.6038 0.042 Uiso 1 1 calc R . .
C3 C 0.3339(6) 1.3989(5) 0.6619(5) 0.0322(15) Uani 1 1 d . . .
H3 H 0.3167 1.3662 0.7052 0.039 Uiso 1 1 calc R . .
C4 C 0.3561(5) 1.3482(5) 0.5961(5) 0.0294(14) Uani 1 1 d . . .
C5 C 0.3586(5) 1.2406(5) 0.6005(4) 0.0266(13) Uani 1 1 d . . .
C6 C 0.3564(5) 1.1000(5) 0.5068(5) 0.0263(13) Uani 1 1 d . . .
C7 C 0.3154(5) 1.0661(5) 0.4157(5) 0.0286(13) Uani 1 1 d . . .
H7 H 0.2809 1.1089 0.3697 0.034 Uiso 1 1 calc R . .
C8 C 0.3742(5) 0.9130(5) 0.4596(4) 0.0250(12) Uani 1 1 d . . .
C9 C 0.3867(5) 0.8187(5) 0.4358(5) 0.0315(14) Uani 1 1 d . . .
H9 H 0.3600 0.7995 0.3749 0.038 Uiso 1 1 calc R . .
C10 C 0.4377(6) 0.7556(5) 0.5020(5) 0.0363(15) Uani 1 1 d . . .
H10 H 0.4469 0.6938 0.4854 0.044 Uiso 1 1 calc R . .
C11 C 0.4770(6) 0.7814(5) 0.5948(5) 0.0380(16) Uani 1 1 d . . .
H11 H 0.5107 0.7368 0.6393 0.046 Uiso 1 1 calc R . .
C12 C 0.4653(6) 0.8727(6) 0.6194(5) 0.0369(15) Uani 1 1 d . . .
H12 H 0.4913 0.8900 0.6809 0.044 Uiso 1 1 calc R . .
C13 C 0.4140(5) 0.9416(5) 0.5525(4) 0.0274(13) Uani 1 1 d . . .
C14 C 0.4057(5) 1.0376(5) 0.5751(4) 0.0300(14) Uani 1 1 d . . .
H14 H 0.4333 1.0581 0.6356 0.036 Uiso 1 1 calc R . .
C15 C 0.1259(6) 0.5463(6) 0.4685(5) 0.0382(16) Uani 1 1 d . . .
H15 H 0.1124 0.5126 0.5135 0.046 Uiso 1 1 calc R . .
C16 C 0.1449(6) 0.4971(5) 0.4011(5) 0.0343(15) Uani 1 1 d . . .
H16 H 0.1405 0.4311 0.4001 0.041 Uiso 1 1 calc R . .
C17 C 0.1676(6) 0.6355(6) 0.3382(5) 0.0358(16) Uani 1 1 d . . .
H17 H 0.1823 0.6687 0.2936 0.043 Uiso 1 1 calc R . .
C18 C 0.1446(5) 0.6856(5) 0.4036(5) 0.0298(14) Uani 1 1 d . . .
C19 C 0.1375(5) 0.7922(5) 0.3994(5) 0.0312(14) Uani 1 1 d . . .
C20 C 0.1365(5) 0.9314(5) 0.4929(5) 0.0304(14) Uani 1 1 d . . .
C21 C 0.1771(5) 0.9649(5) 0.5838(4) 0.0285(13) Uani 1 1 d . . .
H21 H 0.2098 0.9214 0.6297 0.034 Uiso 1 1 calc R . .
C22 C 0.1225(5) 1.1190(5) 0.5413(4) 0.0255(12) Uani 1 1 d . . .
C23 C 0.1156(6) 1.2151(5) 0.5654(5) 0.0354(15) Uani 1 1 d . . .
H23 H 0.1443 1.2343 0.6262 0.043 Uiso 1 1 calc R . .
C24 C 0.0668(6) 1.2794(6) 0.4991(6) 0.0394(17) Uani 1 1 d . . .
H24 H 0.0596 1.3417 0.5154 0.047 Uiso 1 1 calc R . .
C25 C 0.0271(6) 1.2526(6) 0.4060(6) 0.0432(18) Uani 1 1 d . . .
H25 H -0.0036 1.2980 0.3614 0.052 Uiso 1 1 calc R . .
C26 C 0.0335(6) 1.1612(6) 0.3810(5) 0.0394(16) Uani 1 1 d . . .
H26 H 0.0060 1.1441 0.3195 0.047 Uiso 1 1 calc R . .
C27 C 0.0820(5) 1.0912(5) 0.4483(5) 0.0299(14) Uani 1 1 d . . .
C28 C 0.0886(5) 0.9949(5) 0.4252(5) 0.0308(14) Uani 1 1 d . . .
H28 H 0.0608 0.9751 0.3645 0.037 Uiso 1 1 calc R . .
N1 N 0.3786(5) 1.3909(4) 0.5307(4) 0.0317(12) Uani 1 1 d . . .
N2 N 0.3368(5) 1.4935(5) 0.6637(5) 0.0376(14) Uani 1 1 d . . .
N3 N 0.3478(5) 1.1975(4) 0.5203(4) 0.0303(12) Uani 1 1 d . . .
H3B H 0.3343 1.2336 0.4731 0.036 Uiso 1 1 calc R . .
N4 N 0.3233(4) 0.9781(4) 0.3925(4) 0.0286(11) Uani 1 1 d . . .
N5 N 0.1264(5) 0.6407(4) 0.4708(4) 0.0333(13) Uani 1 1 d . . .
N6 N 0.1691(5) 0.5402(4) 0.3381(4) 0.0351(13) Uani 1 1 d . . .
N7 N 0.1456(5) 0.8341(4) 0.4794(4) 0.0319(12) Uani 1 1 d . . .
H7B H 0.1574 0.7975 0.5262 0.038 Uiso 1 1 calc R . .
N8 N 0.1719(4) 1.0539(4) 0.6082(4) 0.0303(12) Uani 1 1 d . . .
O1 O 0.3708(5) 1.1997(4) 0.6723(4) 0.0417(13) Uani 1 1 d . . .
O2 O 0.1248(5) 0.8343(4) 0.3278(4) 0.0464(14) Uani 1 1 d . . .
Hg1 Hg 0.26644(2) 1.09545(2) 0.762861(19) 0.03514(9) Uani 1 1 d . . .
Hg2 Hg 0.22715(2) 0.93850(2) 0.236580(19) 0.03623(9) Uani 1 1 d . . .
Cl1 Cl 0.39039(16) 0.97647(17) 0.80400(14) 0.0483(5) Uani 1 1 d . . .
Cl2 Cl 0.22029(19) 1.23951(14) 0.81161(14) 0.0475(5) Uani 1 1 d . . .
Cl3 Cl 0.10987(16) 1.06257(17) 0.20006(15) 0.0476(5) Uani 1 1 d . . .
Cl4 Cl 0.27307(19) 0.79412(14) 0.18824(13) 0.0488(5) 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 N1 1.338(10) . ?
C1 C2 1.390(10) . ?
C1 H1 0.9300 . ?
C2 N2 1.327(10) . ?
C2 H2 0.9300 . ?
C3 N2 1.329(10) . ?
C3 C4 1.388(9) . ?
C3 H3 0.9300 . ?
C4 N1 1.332(9) . ?
C4 C5 1.512(10) . ?
C5 O1 1.219(8) . ?
C5 N3 1.355(8) . ?
C6 C14 1.365(9) . ?
C6 N3 1.399(9) . ?
C6 C7 1.414(9) . ?
C7 N4 1.306(9) . ?
C7 H7 0.9300 . ?
C8 N4 1.385(8) . ?
C8 C9 1.407(9) . ?
C8 C13 1.414(9) . ?
C9 C10 1.358(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.403(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.369(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.420(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.412(10) . ?
C14 H14 0.9300 . ?
C15 N5 1.327(10) . ?
C15 C16 1.376(10) . ?
C15 H15 0.9300 . ?
C16 N6 1.315(9) . ?
C16 H16 0.9300 . ?
C17 N6 1.340(10) . ?
C17 C18 1.385(9) . ?
C17 H17 0.9300 . ?
C18 N5 1.339(9) . ?
C18 C19 1.500(10) . ?
C19 O2 1.224(9) . ?
C19 N7 1.354(9) . ?
C20 C28 1.365(10) . ?
C20 N7 1.397(9) . ?
C20 C21 1.411(9) . ?
C21 N8 1.317(9) . ?
C21 H21 0.9300 . ?
C22 N8 1.378(8) . ?
C22 C27 1.414(9) . ?
C22 C23 1.415(10) . ?
C23 C24 1.362(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.411(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.356(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.425(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.413(10) . ?
C28 H28 0.9300 . ?
N2 Hg1 2.631(6) 2_556 ?
N3 H3B 0.8600 . ?
N4 Hg2 2.393(5) . ?
N6 Hg2 2.647(6) 2_545 ?
N7 H7B 0.8600 . ?
N8 Hg1 2.380(6) . ?
Hg1 Cl2 2.348(2) . ?
Hg1 Cl1 2.364(2) . ?
Hg1 N2 2.631(6) 2_546 ?
Hg2 Cl4 2.348(2) . ?
Hg2 Cl3 2.354(2) . ?
Hg2 N6 2.647(6) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 121.8(7) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
N2 C2 C1 121.3(7) . . ?
N2 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
N2 C3 C4 120.9(7) . . ?
N2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
N1 C4 C3 122.4(6) . . ?
N1 C4 C5 118.5(6) . . ?
C3 C4 C5 119.1(6) . . ?
O1 C5 N3 125.2(6) . . ?
O1 C5 C4 120.5(6) . . ?
N3 C5 C4 114.3(6) . . ?
C14 C6 N3 124.0(6) . . ?
C14 C6 C7 118.8(6) . . ?
N3 C6 C7 117.1(6) . . ?
N4 C7 C6 123.6(6) . . ?
N4 C7 H7 118.2 . . ?
C6 C7 H7 118.2 . . ?
N4 C8 C9 120.3(6) . . ?
N4 C8 C13 119.8(6) . . ?
C9 C8 C13 119.9(6) . . ?
C10 C9 C8 119.9(7) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.6(7) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C12 C11 C10 119.4(7) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 121.0(7) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C8 119.4(6) . . ?
C14 C13 C12 122.3(6) . . ?
C8 C13 C12 118.2(6) . . ?
C6 C14 C13 118.9(6) . . ?
C6 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N5 C15 C16 121.5(7) . . ?
N5 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
N6 C16 C15 122.4(7) . . ?
N6 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
N6 C17 C18 121.2(7) . . ?
N6 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
N5 C18 C17 121.3(7) . . ?
N5 C18 C19 118.3(6) . . ?
C17 C18 C19 120.4(6) . . ?
O2 C19 N7 125.2(7) . . ?
O2 C19 C18 120.5(6) . . ?
N7 C19 C18 114.3(6) . . ?
C28 C20 N7 124.9(6) . . ?
C28 C20 C21 118.2(6) . . ?
N7 C20 C21 116.9(6) . . ?
N8 C21 C20 124.3(6) . . ?
N8 C21 H21 117.8 . . ?
C20 C21 H21 117.8 . . ?
N8 C22 C27 120.3(6) . . ?
N8 C22 C23 119.9(6) . . ?
C27 C22 C23 119.8(6) . . ?
C24 C23 C22 119.7(7) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.9(7) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 120.5(7) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 120.4(7) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C22 119.3(6) . . ?
C28 C27 C26 122.1(7) . . ?
C22 C27 C26 118.6(7) . . ?
C20 C28 C27 119.3(6) . . ?
C20 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C4 N1 C1 116.0(6) . . ?
C2 N2 C3 117.4(6) . . ?
C2 N2 Hg1 116.4(5) . 2_556 ?
C3 N2 Hg1 122.3(5) . 2_556 ?
C5 N3 C6 126.4(6) . . ?
C5 N3 H3B 116.8 . . ?
C6 N3 H3B 116.8 . . ?
C7 N4 C8 119.4(6) . . ?
C7 N4 Hg2 115.3(4) . . ?
C8 N4 Hg2 124.8(4) . . ?
C15 N5 C18 116.7(6) . . ?
C16 N6 C17 116.7(6) . . ?
C16 N6 Hg2 116.2(5) . 2_545 ?
C17 N6 Hg2 123.5(5) . 2_545 ?
C19 N7 C20 125.8(6) . . ?
C19 N7 H7B 117.1 . . ?
C20 N7 H7B 117.1 . . ?
C21 N8 C22 118.6(6) . . ?
C21 N8 Hg1 117.1(5) . . ?
C22 N8 Hg1 123.8(4) . . ?
Cl2 Hg1 Cl1 143.20(8) . . ?
Cl2 Hg1 N8 114.76(15) . . ?
Cl1 Hg1 N8 101.42(15) . . ?
Cl2 Hg1 N2 92.71(16) . 2_546 ?
Cl1 Hg1 N2 89.74(16) . 2_546 ?
N8 Hg1 N2 96.2(2) . 2_546 ?
Cl4 Hg2 Cl3 145.82(8) . . ?
Cl4 Hg2 N4 113.86(15) . . ?
Cl3 Hg2 N4 99.90(15) . . ?
Cl4 Hg2 N6 92.60(15) . 2 ?
Cl3 Hg2 N6 88.42(15) . 2 ?
N4 Hg2 N6 96.7(2) . 2 ?

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
N1 C1 C2 N2 -2.9(12) . . . . ?
N2 C3 C4 N1 -1.8(11) . . . . ?
N2 C3 C4 C5 175.9(7) . . . . ?
N1 C4 C5 O1 156.0(7) . . . . ?
C3 C4 C5 O1 -21.9(10) . . . . ?
N1 C4 C5 N3 -23.1(9) . . . . ?
C3 C4 C5 N3 159.1(6) . . . . ?
C14 C6 C7 N4 -1.2(11) . . . . ?
N3 C6 C7 N4 175.7(7) . . . . ?
N4 C8 C9 C10 179.2(7) . . . . ?
C13 C8 C9 C10 -0.6(10) . . . . ?
C8 C9 C10 C11 1.5(12) . . . . ?
C9 C10 C11 C12 -1.2(12) . . . . ?
C10 C11 C12 C13 0.0(12) . . . . ?
N4 C8 C13 C14 -3.2(10) . . . . ?
C9 C8 C13 C14 176.6(6) . . . . ?
N4 C8 C13 C12 179.7(6) . . . . ?
C9 C8 C13 C12 -0.5(10) . . . . ?
C11 C12 C13 C14 -176.2(7) . . . . ?
C11 C12 C13 C8 0.8(11) . . . . ?
N3 C6 C14 C13 -176.7(6) . . . . ?
C7 C6 C14 C13 0.0(10) . . . . ?
C8 C13 C14 C6 2.1(10) . . . . ?
C12 C13 C14 C6 179.1(7) . . . . ?
N5 C15 C16 N6 3.3(13) . . . . ?
N6 C17 C18 N5 2.3(11) . . . . ?
N6 C17 C18 C19 -176.4(7) . . . . ?
N5 C18 C19 O2 -158.7(7) . . . . ?
C17 C18 C19 O2 20.0(11) . . . . ?
N5 C18 C19 N7 20.9(10) . . . . ?
C17 C18 C19 N7 -160.4(7) . . . . ?
C28 C20 C21 N8 0.2(11) . . . . ?
N7 C20 C21 N8 -177.8(7) . . . . ?
N8 C22 C23 C24 179.9(7) . . . . ?
C27 C22 C23 C24 2.4(11) . . . . ?
C22 C23 C24 C25 -3.2(12) . . . . ?
C23 C24 C25 C26 2.6(13) . . . . ?
C24 C25 C26 C27 -1.1(13) . . . . ?
N8 C22 C27 C28 2.9(10) . . . . ?
C23 C22 C27 C28 -179.5(7) . . . . ?
N8 C22 C27 C26 -178.5(6) . . . . ?
C23 C22 C27 C26 -1.0(10) . . . . ?
C25 C26 C27 C28 178.9(8) . . . . ?
C25 C26 C27 C22 0.4(12) . . . . ?
N7 C20 C28 C27 178.0(7) . . . . ?
C21 C20 C28 C27 0.2(10) . . . . ?
C22 C27 C28 C20 -1.8(10) . . . . ?
C26 C27 C28 C20 179.7(7) . . . . ?
C3 C4 N1 C1 2.9(10) . . . . ?
C5 C4 N1 C1 -174.9(7) . . . . ?
C2 C1 N1 C4 -0.6(11) . . . . ?
C1 C2 N2 C3 3.9(11) . . . . ?
C1 C2 N2 Hg1 -154.6(6) . . . 2_556 ?
C4 C3 N2 C2 -1.6(11) . . . . ?
C4 C3 N2 Hg1 155.5(5) . . . 2_556 ?
O1 C5 N3 C6 -5.4(12) . . . . ?
C4 C5 N3 C6 173.6(6) . . . . ?
C14 C6 N3 C5 -20.9(11) . . . . ?
C7 C6 N3 C5 162.3(7) . . . . ?
C6 C7 N4 C8 0.1(10) . . . . ?
C6 C7 N4 Hg2 172.0(5) . . . . ?
C9 C8 N4 C7 -177.7(6) . . . . ?
C13 C8 N4 C7 2.1(9) . . . . ?
C9 C8 N4 Hg2 11.3(8) . . . . ?
C13 C8 N4 Hg2 -168.9(5) . . . . ?
C16 C15 N5 C18 1.1(12) . . . . ?
C17 C18 N5 C15 -3.7(11) . . . . ?
C19 C18 N5 C15 175.0(7) . . . . ?
C15 C16 N6 C17 -4.6(12) . . . . ?
C15 C16 N6 Hg2 154.9(6) . . . 2_545 ?
C18 C17 N6 C16 1.9(11) . . . . ?
C18 C17 N6 Hg2 -156.0(5) . . . 2_545 ?
O2 C19 N7 C20 3.1(12) . . . . ?
C18 C19 N7 C20 -176.5(6) . . . . ?
C28 C20 N7 C19 21.7(12) . . . . ?
C21 C20 N7 C19 -160.6(7) . . . . ?
C20 C21 N8 C22 1.0(10) . . . . ?
C20 C21 N8 Hg1 -171.5(5) . . . . ?
C27 C22 N8 C21 -2.5(10) . . . . ?
C23 C22 N8 C21 180.0(7) . . . . ?
C27 C22 N8 Hg1 169.4(5) . . . . ?
C23 C22 N8 Hg1 -8.1(9) . . . . ?
C21 N8 Hg1 Cl2 -163.7(5) . . . . ?
C22 N8 Hg1 Cl2 24.3(6) . . . . ?
C21 N8 Hg1 Cl1 23.2(5) . . . . ?
C22 N8 Hg1 Cl1 -148.8(5) . . . . ?
C21 N8 Hg1 N2 -67.8(5) . . . 2_546 ?
C22 N8 Hg1 N2 120.2(5) . . . 2_546 ?
C7 N4 Hg2 Cl4 165.4(4) . . . . ?
C8 N4 Hg2 Cl4 -23.2(5) . . . . ?
C7 N4 Hg2 Cl3 -20.0(5) . . . . ?
C8 N4 Hg2 Cl3 151.3(5) . . . . ?
C7 N4 Hg2 N6 69.6(5) . . . 2 ?
C8 N4 Hg2 N6 -119.1(5) . . . 2 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.18
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.015
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.237
####################################################################### 
# 
# 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_d:\determination\solution\670\kh670
_database_code_depnum_ccdc_archive 'CCDC 1015771'
_audit_update_record             
;
2014-07-23 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 Hg3 I6 N8 O2'
_chemical_formula_weight         1863.69

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'
Hg Hg -2.3894 9.2266 '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           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   8.1811(4)
_cell_length_b                   7.7210(3)
_cell_length_c                   29.8371(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.637(4)
_cell_angle_gamma                90.00
_cell_volume                     1880.90(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    14543
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      29.20

_exptl_crystal_description       Prim
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1636
_exptl_absorpt_coefficient_mu    17.176
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.1313
_exptl_absorpt_correction_T_max  0.2112
_exptl_absorpt_process_details   'shape of crystal determined optically'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14543
_diffrn_reflns_av_R_equivalents  0.1162
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         29.20
_reflns_number_total             5057
_reflns_number_gt                4200
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (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)+(0.0939P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00176(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5057
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.005
_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
C1 C -0.1097(14) 0.4662(15) 0.1379(4) 0.042(2) Uani 1 1 d . . .
H1 H -0.1263 0.4209 0.1662 0.051 Uiso 1 1 calc R . .
C2 C -0.2322(13) 0.4521(14) 0.1046(4) 0.040(2) Uani 1 1 d . . .
H2 H -0.3300 0.3991 0.1112 0.048 Uiso 1 1 calc R . .
C3 C -0.0747(11) 0.5899(13) 0.0563(3) 0.0357(19) Uani 1 1 d . . .
H3 H -0.0581 0.6358 0.0281 0.043 Uiso 1 1 calc R . .
C4 C 0.0486(12) 0.6050(12) 0.0898(3) 0.0343(19) Uani 1 1 d . . .
C5 C 0.2088(11) 0.6949(12) 0.0812(3) 0.0333(18) Uani 1 1 d . . .
C6 C 0.4704(11) 0.7820(11) 0.1217(3) 0.0298(17) Uani 1 1 d . . .
C7 C 0.5554(11) 0.7769(13) 0.1632(4) 0.0344(19) Uani 1 1 d . . .
H7 H 0.5050 0.7264 0.1871 0.041 Uiso 1 1 calc R . .
C8 C 0.7798(11) 0.9188(11) 0.1363(3) 0.0308(17) Uani 1 1 d . . .
C9 C 0.9423(11) 0.9846(12) 0.1440(3) 0.0325(18) Uani 1 1 d . . .
H9 H 0.9983 0.9770 0.1720 0.039 Uiso 1 1 calc R . .
C10 C 1.0129(12) 1.0605(14) 0.1076(3) 0.038(2) Uani 1 1 d . . .
H10 H 1.1180 1.1061 0.1120 0.045 Uiso 1 1 calc R . .
C11 C 0.9342(14) 1.0714(14) 0.0654(3) 0.043(2) Uani 1 1 d . . .
H11 H 0.9879 1.1213 0.0420 0.051 Uiso 1 1 calc R . .
C12 C 0.7773(15) 1.0093(13) 0.0574(4) 0.042(2) Uani 1 1 d . . .
H12 H 0.7237 1.0185 0.0291 0.051 Uiso 1 1 calc R . .
C13 C 0.6984(11) 0.9301(11) 0.0938(3) 0.0326(18) Uani 1 1 d . . .
C14 C 0.5408(11) 0.8620(11) 0.0863(3) 0.0309(17) Uani 1 1 d . . .
H14 H 0.4848 0.8704 0.0583 0.037 Uiso 1 1 calc R . .
N1 N 0.0325(10) 0.5429(12) 0.1311(3) 0.0363(17) Uani 1 1 d . . .
N2 N -0.2165(11) 0.5120(11) 0.0627(3) 0.0397(19) Uani 1 1 d . . .
N3 N 0.3120(9) 0.7073(12) 0.1182(3) 0.0346(17) Uani 1 1 d . . .
H3B H 0.2774 0.6649 0.1425 0.041 Uiso 1 1 calc R . .
N4 N 0.7041(9) 0.8402(10) 0.1707(3) 0.0305(15) Uani 1 1 d . . .
O1 O 0.2345(10) 0.7486(11) 0.0442(3) 0.0469(18) Uani 1 1 d . . .
Hg1 Hg -0.5000 0.5000 0.0000 0.0498(2) Uani 1 2 d S . .
Hg2 Hg 0.82849(5) 0.81437(7) 0.245092(15) 0.04646(17) Uani 1 1 d . . .
I1 I -0.63567(8) 0.27443(9) 0.04947(3) 0.04134(19) Uani 1 1 d . . .
I2 I 0.60209(11) 0.73909(15) 0.30134(3) 0.0656(3) Uani 1 1 d . . .
I3 I 1.14492(8) 0.71534(9) 0.24429(2) 0.03897(18) 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 N1 1.333(13) . ?
C1 C2 1.370(16) . ?
C1 H1 0.9300 . ?
C2 N2 1.346(14) . ?
C2 H2 0.9300 . ?
C3 N2 1.331(12) . ?
C3 C4 1.381(14) . ?
C3 H3 0.9300 . ?
C4 N1 1.335(13) . ?
C4 C5 1.520(13) . ?
C5 O1 1.209(13) . ?
C5 N3 1.351(13) . ?
C6 C14 1.379(13) . ?
C6 C7 1.383(14) . ?
C6 N3 1.417(12) . ?
C7 N4 1.317(12) . ?
C7 H7 0.9300 . ?
C8 N4 1.373(11) . ?
C8 C13 1.396(14) . ?
C8 C9 1.428(13) . ?
C9 C10 1.390(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.382(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.376(16) . ?
C11 H11 0.9300 . ?
C12 C13 1.435(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.397(13) . ?
C14 H14 0.9300 . ?
N3 H3B 0.8600 . ?
N4 Hg2 2.391(8) . ?
Hg1 I1 2.5792(6) . ?
Hg1 I1 2.5793(6) 3_465 ?
Hg2 I2 2.6419(9) . ?
Hg2 I3 2.7009(8) . ?
Hg2 I3 3.1183(9) 2_755 ?
I3 Hg2 3.1182(9) 2_745 ?

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 C1 C2 122.0(10) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
N2 C2 C1 122.5(10) . . ?
N2 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
N2 C3 C4 122.4(9) . . ?
N2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
N1 C4 C3 121.9(9) . . ?
N1 C4 C5 117.2(9) . . ?
C3 C4 C5 120.9(9) . . ?
O1 C5 N3 125.9(9) . . ?
O1 C5 C4 120.9(9) . . ?
N3 C5 C4 113.2(8) . . ?
C14 C6 C7 119.2(9) . . ?
C14 C6 N3 123.4(9) . . ?
C7 C6 N3 117.3(8) . . ?
N4 C7 C6 123.1(9) . . ?
N4 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
N4 C8 C13 119.6(8) . . ?
N4 C8 C9 119.8(9) . . ?
C13 C8 C9 120.6(8) . . ?
C10 C9 C8 117.0(9) . . ?
C10 C9 H9 121.5 . . ?
C8 C9 H9 121.5 . . ?
C11 C10 C9 123.0(9) . . ?
C11 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
C12 C11 C10 120.8(9) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 118.5(10) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C8 C13 C14 120.2(8) . . ?
C8 C13 C12 120.1(9) . . ?
C14 C13 C12 119.6(10) . . ?
C6 C14 C13 118.1(9) . . ?
C6 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C1 N1 C4 116.0(9) . . ?
C3 N2 C2 115.2(9) . . ?
C5 N3 C6 127.6(8) . . ?
C5 N3 H3B 116.2 . . ?
C6 N3 H3B 116.2 . . ?
C7 N4 C8 119.6(9) . . ?
C7 N4 Hg2 117.4(6) . . ?
C8 N4 Hg2 123.1(6) . . ?
I1 Hg1 I1 180.0 . 3_465 ?
N4 Hg2 I2 109.52(17) . . ?
N4 Hg2 I3 111.53(18) . . ?
I2 Hg2 I3 130.87(3) . . ?
N4 Hg2 I3 91.97(19) . 2_755 ?
I2 Hg2 I3 101.60(3) . 2_755 ?
I3 Hg2 I3 102.78(2) . 2_755 ?
Hg2 I3 Hg2 109.93(3) . 2_745 ?

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
N1 C1 C2 N2 1.0(18) . . . . ?
N2 C3 C4 N1 -0.4(16) . . . . ?
N2 C3 C4 C5 -180.0(9) . . . . ?
N1 C4 C5 O1 177.2(10) . . . . ?
C3 C4 C5 O1 -3.2(15) . . . . ?
N1 C4 C5 N3 -3.3(13) . . . . ?
C3 C4 C5 N3 176.3(9) . . . . ?
C14 C6 C7 N4 -2.3(14) . . . . ?
N3 C6 C7 N4 179.3(8) . . . . ?
N4 C8 C9 C10 179.1(9) . . . . ?
C13 C8 C9 C10 0.6(13) . . . . ?
C8 C9 C10 C11 -1.1(15) . . . . ?
C9 C10 C11 C12 1.4(17) . . . . ?
C10 C11 C12 C13 -1.1(16) . . . . ?
N4 C8 C13 C14 0.1(13) . . . . ?
C9 C8 C13 C14 178.6(8) . . . . ?
N4 C8 C13 C12 -178.9(8) . . . . ?
C9 C8 C13 C12 -0.4(13) . . . . ?
C11 C12 C13 C8 0.7(15) . . . . ?
C11 C12 C13 C14 -178.3(9) . . . . ?
C7 C6 C14 C13 2.0(13) . . . . ?
N3 C6 C14 C13 -179.7(8) . . . . ?
C8 C13 C14 C6 -1.0(13) . . . . ?
C12 C13 C14 C6 178.0(9) . . . . ?
C2 C1 N1 C4 -0.1(16) . . . . ?
C3 C4 N1 C1 -0.2(15) . . . . ?
C5 C4 N1 C1 179.4(9) . . . . ?
C4 C3 N2 C2 1.3(15) . . . . ?
C1 C2 N2 C3 -1.6(16) . . . . ?
O1 C5 N3 C6 -1.0(17) . . . . ?
C4 C5 N3 C6 179.5(9) . . . . ?
C14 C6 N3 C5 2.9(15) . . . . ?
C7 C6 N3 C5 -178.8(9) . . . . ?
C6 C7 N4 C8 1.4(14) . . . . ?
C6 C7 N4 Hg2 -179.4(7) . . . . ?
C13 C8 N4 C7 -0.3(13) . . . . ?
C9 C8 N4 C7 -178.8(8) . . . . ?
C13 C8 N4 Hg2 -179.4(6) . . . . ?
C9 C8 N4 Hg2 2.1(11) . . . . ?
C7 N4 Hg2 I2 -15.7(7) . . . . ?
C8 N4 Hg2 I2 163.4(6) . . . . ?
C7 N4 Hg2 I3 136.7(6) . . . . ?
C8 N4 Hg2 I3 -44.2(7) . . . . ?
C7 N4 Hg2 I3 -118.8(7) . . . 2_755 ?
C8 N4 Hg2 I3 60.4(7) . . . 2_755 ?
N4 Hg2 I3 Hg2 -94.9(2) . . . 2_745 ?
I2 Hg2 I3 Hg2 49.81(5) . . . 2_745 ?
I3 Hg2 I3 Hg2 167.78(3) 2_755 . . 2_745 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        29.20
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.400
####################################################################### 
# 
# 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_d:\determination\solution\672\kh672
_database_code_depnum_ccdc_archive 'CCDC 1015772'
_audit_update_record             
;
2014-07-23 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 Br6 Hg3 N8 O2'
_chemical_formula_weight         1581.69

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'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Moniclinic
_symmetry_space_group_name_H-M   P21/c

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                   7.8761(4)
_cell_length_b                   7.5061(4)
_cell_length_c                   29.2866(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.498(4)
_cell_angle_gamma                90.00
_cell_volume                     1730.80(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    17823
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      29.20

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420
_exptl_absorpt_coefficient_mu    20.240
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3712
_exptl_absorpt_correction_T_max  0.4646
_exptl_absorpt_process_details   'shape of crystal determined optically'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17823
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         29.20
_reflns_number_total             4654
_reflns_number_gt                3513
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (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)+(0.0411P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4654
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1121
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.007
_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
C1 C 1.6451(12) 1.5439(12) -0.1414(3) 0.0324(19) Uani 1 1 d . . .
H1 H 1.6694 1.5890 -0.1700 0.039 Uiso 1 1 calc R . .
C2 C 1.7652(12) 1.5571(13) -0.1064(3) 0.034(2) Uani 1 1 d . . .
H2 H 1.8687 1.6108 -0.1123 0.041 Uiso 1 1 calc R . .
C3 C 1.5884(11) 1.4219(13) -0.0573(3) 0.0327(19) Uani 1 1 d . . .
H3 H 1.5645 1.3777 -0.0286 0.039 Uiso 1 1 calc R . .
C4 C 1.4660(10) 1.4099(11) -0.0926(3) 0.0279(17) Uani 1 1 d . . .
C5 C 1.2993(11) 1.3207(12) -0.0840(3) 0.0313(18) Uani 1 1 d . . .
C6 C 1.0440(10) 1.2117(11) -0.1251(3) 0.0288(18) Uani 1 1 d . . .
C7 C 0.9577(11) 1.2136(12) -0.1676(3) 0.0324(19) Uani 1 1 d . . .
H7 H 1.0117 1.2644 -0.1923 0.039 Uiso 1 1 calc R . .
C8 C 0.7208(10) 1.0715(11) -0.1395(3) 0.0264(16) Uani 1 1 d . . .
C9 C 0.5527(11) 1.0035(12) -0.1454(3) 0.0334(18) Uani 1 1 d . . .
H9 H 0.4976 1.0094 -0.1738 0.040 Uiso 1 1 calc R . .
C10 C 0.4725(12) 0.9294(13) -0.1090(3) 0.036(2) Uani 1 1 d . . .
H10 H 0.3624 0.8864 -0.1131 0.044 Uiso 1 1 calc R . .
C11 C 0.5521(12) 0.9168(12) -0.0659(3) 0.0343(19) Uani 1 1 d . . .
H11 H 0.4942 0.8677 -0.0416 0.041 Uiso 1 1 calc R . .
C12 C 0.7158(12) 0.9770(11) -0.0592(3) 0.0322(19) Uani 1 1 d . . .
H12 H 0.7701 0.9641 -0.0308 0.039 Uiso 1 1 calc R . .
C13 C 0.8020(11) 1.0588(11) -0.0957(3) 0.0285(17) Uani 1 1 d . . .
C14 C 0.9645(10) 1.1297(11) -0.0895(3) 0.0291(17) Uani 1 1 d . . .
H14 H 1.0197 1.1214 -0.0611 0.035 Uiso 1 1 calc R . .
N1 N 1.4944(9) 1.4678(10) -0.1348(3) 0.0327(16) Uani 1 1 d . . .
N2 N 1.7389(9) 1.4959(10) -0.0645(3) 0.0329(16) Uani 1 1 d . . .
N3 N 1.2034(9) 1.2952(9) -0.1223(2) 0.0295(15) Uani 1 1 d . . .
H3B H 1.2439 1.3340 -0.1474 0.035 Uiso 1 1 calc R . .
N4 N 0.8029(9) 1.1466(10) -0.1746(2) 0.0297(15) Uani 1 1 d . . .
O1 O 1.2627(8) 1.2718(9) -0.0456(2) 0.0408(15) Uani 1 1 d . . .
Hg1 Hg 2.0000 1.5000 0.0000 0.03557(14) Uani 1 2 d S . .
Hg2 Hg 0.67691(5) 1.18337(6) -0.248197(14) 0.04707(13) Uani 1 1 d . . .
Br1 Br 1.86327(12) 1.26658(14) 0.04291(4) 0.0424(2) Uani 1 1 d . . .
Br2 Br 0.90976(18) 1.2256(2) -0.30149(5) 0.0747(4) Uani 1 1 d . . .
Br3 Br 0.37155(13) 1.27921(14) -0.24323(3) 0.0426(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 N1 1.335(12) . ?
C1 C2 1.380(13) . ?
C1 H1 0.9300 . ?
C2 N2 1.331(12) . ?
C2 H2 0.9300 . ?
C3 N2 1.330(11) . ?
C3 C4 1.397(12) . ?
C3 H3 0.9300 . ?
C4 N1 1.336(11) . ?
C4 C5 1.500(12) . ?
C5 O1 1.224(11) . ?
C5 N3 1.349(11) . ?
C6 C14 1.376(12) . ?
C6 C7 1.401(12) . ?
C6 N3 1.404(10) . ?
C7 N4 1.329(11) . ?
C7 H7 0.9300 . ?
C8 N4 1.352(11) . ?
C8 C13 1.421(12) . ?
C8 C9 1.425(12) . ?
C9 C10 1.371(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.398(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.375(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.420(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(12) . ?
C14 H14 0.9300 . ?
N3 H3B 0.8600 . ?
N4 Hg2 2.366(7) . ?
Hg1 Br1 2.4247(9) 3_985 ?
Hg1 Br1 2.4247(9) . ?
Hg2 Br2 2.4597(13) . ?
Hg2 Br3 2.5181(11) . ?
Hg2 Br3 3.0670(12) 2_644 ?
Br3 Hg2 3.0670(12) 2_654 ?

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 C1 C2 121.2(8) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
N2 C2 C1 122.6(8) . . ?
N2 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
N2 C3 C4 120.8(8) . . ?
N2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
N1 C4 C3 122.3(8) . . ?
N1 C4 C5 118.0(7) . . ?
C3 C4 C5 119.7(8) . . ?
O1 C5 N3 125.5(8) . . ?
O1 C5 C4 121.1(8) . . ?
N3 C5 C4 113.4(8) . . ?
C14 C6 C7 117.2(7) . . ?
C14 C6 N3 125.3(8) . . ?
C7 C6 N3 117.5(8) . . ?
N4 C7 C6 123.7(8) . . ?
N4 C7 H7 118.2 . . ?
C6 C7 H7 118.2 . . ?
N4 C8 C13 120.1(8) . . ?
N4 C8 C9 121.3(8) . . ?
C13 C8 C9 118.7(8) . . ?
C10 C9 C8 119.8(8) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.7(9) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C12 C11 C10 120.1(8) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.0(9) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 121.5(8) . . ?
C14 C13 C8 118.8(8) . . ?
C12 C13 C8 119.7(8) . . ?
C6 C14 C13 120.5(8) . . ?
C6 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C1 N1 C4 116.3(7) . . ?
C3 N2 C2 116.8(8) . . ?
C5 N3 C6 126.4(7) . . ?
C5 N3 H3B 116.8 . . ?
C6 N3 H3B 116.8 . . ?
C7 N4 C8 119.7(7) . . ?
C7 N4 Hg2 117.2(6) . . ?
C8 N4 Hg2 122.9(6) . . ?
Br1 Hg1 Br1 180.00(3) 3_985 . ?
N4 Hg2 Br2 106.93(17) . . ?
N4 Hg2 Br3 111.05(17) . . ?
Br2 Hg2 Br3 136.80(5) . . ?
N4 Hg2 Br3 90.44(18) . 2_644 ?
Br2 Hg2 Br3 99.72(5) . 2_644 ?
Br3 Hg2 Br3 99.81(3) . 2_644 ?
Hg2 Br3 Hg2 113.26(4) . 2_654 ?

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
N1 C1 C2 N2 -0.1(15) . . . . ?
N2 C3 C4 N1 1.4(14) . . . . ?
N2 C3 C4 C5 178.1(8) . . . . ?
N1 C4 C5 O1 -176.8(8) . . . . ?
C3 C4 C5 O1 6.4(13) . . . . ?
N1 C4 C5 N3 6.0(11) . . . . ?
C3 C4 C5 N3 -170.9(8) . . . . ?
C14 C6 C7 N4 2.5(14) . . . . ?
N3 C6 C7 N4 -176.9(8) . . . . ?
N4 C8 C9 C10 -179.5(8) . . . . ?
C13 C8 C9 C10 0.6(13) . . . . ?
C8 C9 C10 C11 -0.6(14) . . . . ?
C9 C10 C11 C12 -1.0(14) . . . . ?
C10 C11 C12 C13 2.6(14) . . . . ?
C11 C12 C13 C14 176.6(8) . . . . ?
C11 C12 C13 C8 -2.6(13) . . . . ?
N4 C8 C13 C14 1.8(12) . . . . ?
C9 C8 C13 C14 -178.2(8) . . . . ?
N4 C8 C13 C12 -179.0(7) . . . . ?
C9 C8 C13 C12 1.0(12) . . . . ?
C7 C6 C14 C13 -2.6(13) . . . . ?
N3 C6 C14 C13 176.7(8) . . . . ?
C12 C13 C14 C6 -178.6(8) . . . . ?
C8 C13 C14 C6 0.6(13) . . . . ?
C2 C1 N1 C4 1.6(13) . . . . ?
C3 C4 N1 C1 -2.2(13) . . . . ?
C5 C4 N1 C1 -179.0(8) . . . . ?
C4 C3 N2 C2 0.2(13) . . . . ?
C1 C2 N2 C3 -0.8(14) . . . . ?
O1 C5 N3 C6 1.2(15) . . . . ?
C4 C5 N3 C6 178.3(8) . . . . ?
C14 C6 N3 C5 -5.2(14) . . . . ?
C7 C6 N3 C5 174.1(8) . . . . ?
C6 C7 N4 C8 -0.1(13) . . . . ?
C6 C7 N4 Hg2 176.0(7) . . . . ?
C13 C8 N4 C7 -2.1(12) . . . . ?
C9 C8 N4 C7 178.0(8) . . . . ?
C13 C8 N4 Hg2 -177.9(6) . . . . ?
C9 C8 N4 Hg2 2.2(11) . . . . ?
C7 N4 Hg2 Br2 23.5(7) . . . . ?
C8 N4 Hg2 Br2 -160.6(6) . . . . ?
C7 N4 Hg2 Br3 -135.5(6) . . . . ?
C8 N4 Hg2 Br3 40.4(7) . . . . ?
C7 N4 Hg2 Br3 123.8(6) . . . 2_644 ?
C8 N4 Hg2 Br3 -60.3(6) . . . 2_644 ?
N4 Hg2 Br3 Hg2 96.46(19) . . . 2_654 ?
Br2 Hg2 Br3 Hg2 -53.51(8) . . . 2_654 ?
Br3 Hg2 Br3 Hg2 -169.25(5) 2_644 . . 2_654 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.20
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.736
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.217
####################################################################### 
# 
# 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_d:\determination\solution\c308\khc308-abs
_database_code_depnum_ccdc_archive 'CCDC 1015774'
_audit_update_record             
;
2014-07-23 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 Br2 Hg1 N8 O2'
_chemical_formula_weight         860.91

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'
Br Br -0.2901 2.4595 '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_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   3.9332(9)
_cell_length_b                   12.278(3)
_cell_length_c                   14.441(3)
_cell_angle_alpha                99.278(19)
_cell_angle_beta                 91.024(18)
_cell_angle_gamma                92.56(2)
_cell_volume                     687.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7446
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      29.16

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             410
_exptl_absorpt_coefficient_mu    8.548
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0967
_exptl_absorpt_correction_T_max  0.5409
_exptl_absorpt_process_details   'shape of crystal determined optically'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7446
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         29.16
_reflns_number_total             3690
_reflns_number_gt                2377
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (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)+(0.0847P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3690
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1754
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.006
_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 0.777(3) 0.5604(9) 0.1806(8) 0.047(2) Uani 1 1 d . . .
H1 H 0.8989 0.6180 0.1597 0.057 Uiso 1 1 calc R . .
C2 C 0.699(3) 0.5688(9) 0.2736(8) 0.047(2) Uani 1 1 d . . .
H2 H 0.7697 0.6336 0.3131 0.056 Uiso 1 1 calc R . .
C3 C 0.432(2) 0.4008(10) 0.2507(8) 0.045(2) Uani 1 1 d . . .
H3 H 0.3134 0.3434 0.2728 0.054 Uiso 1 1 calc R . .
C4 C 0.502(2) 0.3907(9) 0.1560(8) 0.043(2) Uani 1 1 d . . .
C5 C 0.378(2) 0.2874(10) 0.0909(8) 0.043(2) Uani 1 1 d . . .
C6 C 0.455(2) 0.1944(9) -0.0738(7) 0.040(2) Uani 1 1 d . . .
C7 C 0.302(3) 0.0924(9) -0.0634(8) 0.045(2) Uani 1 1 d . . .
H7 H 0.2016 0.0816 -0.0075 0.053 Uiso 1 1 calc R . .
C8 C 0.305(2) 0.0080(9) -0.1393(8) 0.044(2) Uani 1 1 d . . .
H8 H 0.2053 -0.0611 -0.1350 0.052 Uiso 1 1 calc R . .
C9 C 0.458(2) 0.0265(9) -0.2230(7) 0.042(2) Uani 1 1 d . . .
C10 C 0.475(3) -0.0591(10) -0.3024(8) 0.051(3) Uani 1 1 d . . .
H10 H 0.3845 -0.1299 -0.3004 0.061 Uiso 1 1 calc R . .
C11 C 0.630(3) -0.0344(11) -0.3825(8) 0.055(3) Uani 1 1 d . . .
H11 H 0.6499 -0.0890 -0.4346 0.066 Uiso 1 1 calc R . .
C12 C 0.756(3) 0.0732(11) -0.3841(8) 0.051(3) Uani 1 1 d . . .
H12 H 0.8564 0.0889 -0.4387 0.061 Uiso 1 1 calc R . .
C13 C 0.740(2) 0.1575(10) -0.3090(8) 0.046(2) Uani 1 1 d . . .
H13 H 0.8238 0.2285 -0.3133 0.055 Uiso 1 1 calc R . .
C14 C 0.594(2) 0.1342(9) -0.2254(7) 0.037(2) Uani 1 1 d . . .
N1 N 0.678(2) 0.4693(8) 0.1193(6) 0.0423(19) Uani 1 1 d . . .
N2 N 0.532(2) 0.4924(8) 0.3111(6) 0.049(2) Uani 1 1 d . . .
N3 N 0.486(2) 0.2832(8) 0.0007(6) 0.047(2) Uani 1 1 d . . .
H3B H 0.5856 0.3427 -0.0119 0.056 Uiso 1 1 calc R . .
N4 N 0.598(2) 0.2181(8) -0.1501(6) 0.0417(19) Uani 1 1 d . . .
O1 O 0.202(2) 0.2191(8) 0.1200(6) 0.063(2) Uani 1 1 d . . .
Br1 Br 0.9106(2) 0.66266(9) 0.52425(8) 0.0492(3) Uani 1 1 d . . .
Hg1 Hg 0.5000 0.5000 0.5000 0.0439(2) Uani 1 2 d S . .


_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 N1 1.349(15) . ?
C1 C2 1.371(16) . ?
C1 H1 0.9300 . ?
C2 N2 1.314(14) . ?
C2 H2 0.9300 . ?
C3 N2 1.346(15) . ?
C3 C4 1.386(15) . ?
C3 H3 0.9300 . ?
C4 N1 1.345(13) . ?
C4 C5 1.507(16) . ?
C5 O1 1.197(12) . ?
C5 N3 1.371(14) . ?
C6 N4 1.314(12) . ?
C6 C7 1.397(14) . ?
C6 N3 1.402(14) . ?
C7 C8 1.382(16) . ?
C7 H7 0.9300 . ?
C8 C9 1.407(14) . ?
C8 H8 0.9300 . ?
C9 C14 1.410(15) . ?
C9 C10 1.430(16) . ?
C10 C11 1.387(17) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(18) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(17) . ?
C12 H12 0.9300 . ?
C13 C14 1.410(13) . ?
C13 H13 0.9300 . ?
C14 N4 1.372(14) . ?
N3 H3B 0.8600 . ?
Br1 Hg1 2.4870(12) . ?
Br1 Hg1 3.1150(13) 1_655 ?
Hg1 Br1 2.4870(12) 2_666 ?
Hg1 Br1 3.1150(13) 1_455 ?
Hg1 Br1 3.1150(13) 2_766 ?

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 C1 C2 120.4(10) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
N2 C2 C1 125.1(10) . . ?
N2 C2 H2 117.4 . . ?
C1 C2 H2 117.4 . . ?
N2 C3 C4 121.2(10) . . ?
N2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
N1 C4 C3 122.7(10) . . ?
N1 C4 C5 118.1(9) . . ?
C3 C4 C5 119.2(9) . . ?
O1 C5 N3 126.5(11) . . ?
O1 C5 C4 119.8(10) . . ?
N3 C5 C4 113.7(9) . . ?
N4 C6 C7 125.8(10) . . ?
N4 C6 N3 112.1(9) . . ?
C7 C6 N3 122.1(9) . . ?
C8 C7 C6 117.5(9) . . ?
C8 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C7 C8 C9 120.1(10) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C14 116.8(10) . . ?
C8 C9 C10 122.0(10) . . ?
C14 C9 C10 121.2(9) . . ?
C11 C10 C9 118.6(11) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 119.3(11) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C13 C12 C11 123.3(10) . . ?
C13 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C12 C13 C14 118.9(11) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
N4 C14 C9 123.6(9) . . ?
N4 C14 C13 117.6(9) . . ?
C9 C14 C13 118.7(10) . . ?
C4 N1 C1 115.5(9) . . ?
C2 N2 C3 115.1(9) . . ?
C5 N3 C6 128.4(9) . . ?
C5 N3 H3B 115.8 . . ?
C6 N3 H3B 115.8 . . ?
C6 N4 C14 116.1(9) . . ?
Hg1 Br1 Hg1 88.45(4) . 1_655 ?
Br1 Hg1 Br1 180.0 . 2_666 ?
Br1 Hg1 Br1 88.45(4) . 1_455 ?
Br1 Hg1 Br1 91.55(4) 2_666 1_455 ?
Br1 Hg1 Br1 91.55(4) . 2_766 ?
Br1 Hg1 Br1 88.45(4) 2_666 2_766 ?
Br1 Hg1 Br1 180.0 1_455 2_766 ?

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
N1 C1 C2 N2 0.9(18) . . . . ?
N2 C3 C4 N1 1.4(17) . . . . ?
N2 C3 C4 C5 -178.9(9) . . . . ?
N1 C4 C5 O1 -175.0(10) . . . . ?
C3 C4 C5 O1 5.3(16) . . . . ?
N1 C4 C5 N3 4.6(14) . . . . ?
C3 C4 C5 N3 -175.1(9) . . . . ?
N4 C6 C7 C8 1.1(16) . . . . ?
N3 C6 C7 C8 -175.7(10) . . . . ?
C6 C7 C8 C9 0.0(15) . . . . ?
C7 C8 C9 C14 -1.9(14) . . . . ?
C7 C8 C9 C10 178.3(10) . . . . ?
C8 C9 C10 C11 179.9(10) . . . . ?
C14 C9 C10 C11 0.1(15) . . . . ?
C9 C10 C11 C12 -1.6(16) . . . . ?
C10 C11 C12 C13 1.0(18) . . . . ?
C11 C12 C13 C14 1.1(17) . . . . ?
C8 C9 C14 N4 3.1(14) . . . . ?
C10 C9 C14 N4 -177.1(9) . . . . ?
C8 C9 C14 C13 -177.9(9) . . . . ?
C10 C9 C14 C13 1.9(15) . . . . ?
C12 C13 C14 N4 176.6(10) . . . . ?
C12 C13 C14 C9 -2.5(14) . . . . ?
C3 C4 N1 C1 -1.3(15) . . . . ?
C5 C4 N1 C1 179.1(8) . . . . ?
C2 C1 N1 C4 0.2(16) . . . . ?
C1 C2 N2 C3 -0.7(17) . . . . ?
C4 C3 N2 C2 -0.4(16) . . . . ?
O1 C5 N3 C6 -9.2(18) . . . . ?
C4 C5 N3 C6 171.2(9) . . . . ?
N4 C6 N3 C5 -177.8(9) . . . . ?
C7 C6 N3 C5 -0.6(16) . . . . ?
C7 C6 N4 C14 -0.1(14) . . . . ?
N3 C6 N4 C14 177.0(9) . . . . ?
C9 C14 N4 C6 -2.1(13) . . . . ?
C13 C14 N4 C6 178.8(9) . . . . ?
Hg1 Br1 Hg1 Br1 57(12) 1_655 . . 2_666 ?
Hg1 Br1 Hg1 Br1 180.0 1_655 . . 1_455 ?
Hg1 Br1 Hg1 Br1 0.0 1_655 . . 2_766 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        29.16
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.249
####################################################################### 
# 
# 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_d:\determination\solution\879\kh879
_database_code_depnum_ccdc_archive 'CCDC 1015778'
_audit_update_record             
;
2014-07-23 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H10 Hg1 I2 N4 O1'
_chemical_formula_weight         704.65

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'
Hg Hg -2.3894 9.2266 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.7642(5)
_cell_length_b                   7.7232(7)
_cell_length_c                   17.7949(15)
_cell_angle_alpha                91.562(7)
_cell_angle_beta                 93.790(6)
_cell_angle_gamma                113.327(6)
_cell_volume                     850.32(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7617
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.00

_exptl_crystal_description       Plate
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_absorpt_coefficient_mu    12.687
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2351
_exptl_absorpt_correction_T_max  0.2910
_exptl_absorpt_process_details   'shape of crystal determined optically'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7617
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3690
_reflns_number_gt                2794
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (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)+(0.2000P)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         3690
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0901
_refine_ls_wR_factor_ref         0.1918
_refine_ls_wR_factor_gt          0.1815
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
C1 C 0.874(2) 1.029(2) 0.2811(9) 0.057(3) Uani 1 1 d . . .
H1 H 1.0228 1.0642 0.2820 0.068 Uiso 1 1 calc R . .
C2 C 0.762(2) 0.9319(19) 0.3409(8) 0.051(3) Uani 1 1 d . . .
H2 H 0.8409 0.9110 0.3819 0.061 Uiso 1 1 calc R . .
C3 C 0.448(2) 0.9096(19) 0.2816(7) 0.048(3) Uani 1 1 d . . .
H3 H 0.2987 0.8683 0.2797 0.058 Uiso 1 1 calc R . .
C4 C 0.5526(19) 1.0081(16) 0.2228(9) 0.046(3) Uani 1 1 d . . .
C5 C 0.429(2) 1.0503(15) 0.1577(8) 0.043(3) Uani 1 1 d . . .
C6 C 0.496(2) 1.2033(15) 0.0344(7) 0.043(3) Uani 1 1 d . . .
C7 C 0.278(2) 1.1699(19) 0.0116(9) 0.052(3) Uani 1 1 d . . .
H7 H 0.1663 1.1061 0.0413 0.062 Uiso 1 1 calc R . .
C8 C 0.241(2) 1.2344(19) -0.0543(9) 0.055(3) Uani 1 1 d . . .
H8 H 0.0998 1.2131 -0.0714 0.065 Uiso 1 1 calc R . .
C9 C 0.412(2) 1.3344(16) -0.0990(8) 0.046(3) Uani 1 1 d . . .
C10 C 0.383(3) 1.4112(19) -0.1696(11) 0.065(4) Uani 1 1 d . . .
H10 H 0.2453 1.3935 -0.1891 0.078 Uiso 1 1 calc R . .
C11 C 0.555(3) 1.509(2) -0.2079(8) 0.065(4) Uani 1 1 d . . .
H11 H 0.5370 1.5577 -0.2537 0.078 Uiso 1 1 calc R . .
C12 C 0.768(3) 1.535(2) -0.1757(9) 0.066(4) Uani 1 1 d . . .
H12 H 0.8866 1.6035 -0.2015 0.079 Uiso 1 1 calc R . .
C13 C 0.801(3) 1.463(2) -0.1097(10) 0.060(4) Uani 1 1 d . . .
H13 H 0.9401 1.4819 -0.0912 0.072 Uiso 1 1 calc R . .
C14 C 0.625(2) 1.3608(15) -0.0694(8) 0.046(3) Uani 1 1 d . . .
N1 N 0.7685(18) 1.0697(16) 0.2228(7) 0.052(3) Uani 1 1 d . . .
N2 N 0.5516(19) 0.8697(16) 0.3419(7) 0.051(3) Uani 1 1 d . . .
N3 N 0.5532(18) 1.1386(14) 0.1020(7) 0.046(2) Uani 1 1 d . . .
H3A H 0.6874 1.1577 0.1092 0.055 Uiso 1 1 calc R . .
N4 N 0.6596(17) 1.2927(13) -0.0029(7) 0.045(2) Uani 1 1 d . . .
O1 O 0.2332(16) 1.0059(16) 0.1598(7) 0.060(3) Uani 1 1 d . . .
Hg1 Hg 0.34030(10) 0.69803(10) 0.44800(4) 0.0663(3) Uani 1 1 d . . .
I1 I -0.03852(17) 0.53043(15) 0.37536(7) 0.0644(4) Uani 1 1 d . . .
I2 I 0.66395(18) 0.80714(17) 0.55075(6) 0.0717(4) 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 N1 1.338(19) . ?
C1 C2 1.40(2) . ?
C1 H1 0.9300 . ?
C2 N2 1.312(19) . ?
C2 H2 0.9300 . ?
C3 N2 1.352(17) . ?
C3 C4 1.374(19) . ?
C3 H3 0.9300 . ?
C4 N1 1.345(16) . ?
C4 C5 1.50(2) . ?
C5 O1 1.235(16) . ?
C5 N3 1.358(17) . ?
C6 N4 1.289(17) . ?
C6 N3 1.404(17) . ?
C6 C7 1.420(18) . ?
C7 C8 1.33(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.42(2) . ?
C8 H8 0.9300 . ?
C9 C14 1.434(19) . ?
C9 C10 1.44(2) . ?
C10 C11 1.35(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.45(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.36(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.40(2) . ?
C13 H13 0.9300 . ?
C14 N4 1.352(19) . ?
N2 Hg1 2.521(11) . ?
N3 H3A 0.8600 . ?
Hg1 I1 2.5993(12) . ?
Hg1 I2 2.6023(12) . ?

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 C1 C2 120.4(13) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
N2 C2 C1 123.2(13) . . ?
N2 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
N2 C3 C4 123.4(13) . . ?
N2 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
N1 C4 C3 120.4(14) . . ?
N1 C4 C5 118.7(13) . . ?
C3 C4 C5 120.9(12) . . ?
O1 C5 N3 127.0(13) . . ?
O1 C5 C4 119.0(12) . . ?
N3 C5 C4 114.0(11) . . ?
N4 C6 N3 112.8(11) . . ?
N4 C6 C7 125.3(12) . . ?
N3 C6 C7 121.8(12) . . ?
C8 C7 C6 116.9(14) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
C7 C8 C9 121.5(13) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C14 116.2(12) . . ?
C8 C9 C10 124.3(13) . . ?
C14 C9 C10 119.5(13) . . ?
C11 C10 C9 120.7(16) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 118.2(15) . . ?
C10 C11 H11 120.9 . . ?
C12 C11 H11 120.9 . . ?
C13 C12 C11 122.9(16) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C12 C13 C14 119.7(16) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
N4 C14 C13 119.2(14) . . ?
N4 C14 C9 121.7(12) . . ?
C13 C14 C9 119.0(14) . . ?
C1 N1 C4 117.4(13) . . ?
C2 N2 C3 115.2(12) . . ?
C2 N2 Hg1 124.9(9) . . ?
C3 N2 Hg1 119.9(9) . . ?
C5 N3 C6 129.9(11) . . ?
C5 N3 H3A 115.0 . . ?
C6 N3 H3A 115.0 . . ?
C6 N4 C14 118.3(11) . . ?
N2 Hg1 I1 99.5(3) . . ?
N2 Hg1 I2 96.6(3) . . ?
I1 Hg1 I2 163.81(6) . . ?

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
N1 C1 C2 N2 3(2) . . . . ?
N2 C3 C4 N1 0(2) . . . . ?
N2 C3 C4 C5 -179.2(12) . . . . ?
N1 C4 C5 O1 -175.0(12) . . . . ?
C3 C4 C5 O1 4.6(18) . . . . ?
N1 C4 C5 N3 4.2(15) . . . . ?
C3 C4 C5 N3 -176.2(11) . . . . ?
N4 C6 C7 C8 1(2) . . . . ?
N3 C6 C7 C8 -178.7(13) . . . . ?
C6 C7 C8 C9 -1(2) . . . . ?
C7 C8 C9 C14 0(2) . . . . ?
C7 C8 C9 C10 -178.5(13) . . . . ?
C8 C9 C10 C11 178.4(14) . . . . ?
C14 C9 C10 C11 0(2) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
C10 C11 C12 C13 1(2) . . . . ?
C11 C12 C13 C14 -1(2) . . . . ?
C12 C13 C14 N4 -178.9(13) . . . . ?
C12 C13 C14 C9 0(2) . . . . ?
C8 C9 C14 N4 0.4(17) . . . . ?
C10 C9 C14 N4 179.4(12) . . . . ?
C8 C9 C14 C13 -178.2(12) . . . . ?
C10 C9 C14 C13 0.8(18) . . . . ?
C2 C1 N1 C4 -3(2) . . . . ?
C3 C4 N1 C1 1.0(18) . . . . ?
C5 C4 N1 C1 -179.4(12) . . . . ?
C1 C2 N2 C3 -2(2) . . . . ?
C1 C2 N2 Hg1 -179.4(11) . . . . ?
C4 C3 N2 C2 0.0(19) . . . . ?
C4 C3 N2 Hg1 177.7(10) . . . . ?
O1 C5 N3 C6 1(2) . . . . ?
C4 C5 N3 C6 -178.2(11) . . . . ?
N4 C6 N3 C5 175.5(11) . . . . ?
C7 C6 N3 C5 -4.7(19) . . . . ?
N3 C6 N4 C14 179.5(10) . . . . ?
C7 C6 N4 C14 -0.3(18) . . . . ?
C13 C14 N4 C6 178.1(12) . . . . ?
C9 C14 N4 C6 -0.5(17) . . . . ?
C2 N2 Hg1 I1 -159.0(10) . . . . ?
C3 N2 Hg1 I1 23.6(10) . . . . ?
C2 N2 Hg1 I2 19.0(11) . . . . ?
C3 N2 Hg1 I2 -158.4(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.511
