# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2003

data_global
_journal_coden_Cambridge         0440
#===============================================================================
_audit_creation_date             3-06-02

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Mir Wais Hosseini'

_publ_contact_author_email       lccs@scrx.u-strasbg.fr
_publ_contact_letter             
;
?
;

_publ_requested_category         FM
#===============================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_coden_ASTM              ?
_journal_name_full               'New J.Chem.(Nouv.J.Chim.)'
_journal_year                    ?
_journal_volume                  ?

_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?

#===============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
Gradual increase in the dimensionality of cobalt and mercury coordination
networks based on conformation of tetradentate tectons
;

# The loop structure below should contain the names  and addresses of all
# authors, in the required order  of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address
'Philippe Grohans'
;Laboratoire de Chimie de Coordination Organique
Institut Le Bel
Universite Louis Pasteur
4, rue Blaise Pascal
67000 Strasbourg
FRANCE
;
'Mir Wais Hosseini'
;Laboratoire de Chimie de Coordination Organique
Institut Le Bel
Universite Louis Pasteur
4, rue Blaise Pascal
67000 Strasbourg
FRANCE
;
'Abdelaziz Jouaiti'
;Laboratoire de Chimie de Coordination Organique
Institut Le Bel
Universite Louis Pasteur
4, rue Blaise Pascal
67000 Strasbourg
FRANCE
;
'Nathalie Kyritsakas'
;Service commun de rayons X
Institut Le Bel
Universite Louis Pasteur
4, rue Blaise Pascal
67000 Strasbourg
FRANCE
;

# 4. TEXT

_publ_section_abstract           
; ?
;

_publ_section_comment            
; ?
;

_publ_section_exptl_prep         
; ?
;

_publ_section_exptl_refinement   
; ?
;

_publ_section_references         
;

Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G.,
Spagna, R. &Viterbo, D. (1989).  SIR.  J. Appl. Cryst. 22, 389-393.

OpenMoleN, Interactive Intelligent Structure  solution (1997)
Nonius B.V., Delft, The Netherlands.

KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands.

Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326.

Walker, N. & Stuart, D. (1983). Acta Cryst.,  A39, 158-166.

;

_publ_section_figure_captions    
; ?
;

_publ_section_acknowledgements   
; ?
;

#===============================================================================
# If more than one structure is reported, sections 5-10 should be filled in
# per structure. For each data set, replace the ? in the data_? line below
# by a unique identifier.

data_st1168
_database_code_CSD               202740

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C32 H27 Cl11 Co N4 O8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C32 H27 Cl11 Co N4 O8'
_chemical_formula_weight         1044.51
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,+z
-x,1/2+y,1/2-z
1/2+x,-y,1/2-z
-x,-y,-z
1/2+x,1/2+y,-z
+x,1/2-y,1/2+z
1/2-x,+y,1/2+z
_cell_length_a                   12.2414(2)
_cell_length_b                   13.1257(2)
_cell_length_c                   27.1081(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4355.6(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_special_details            
;
Cell parameters refined using Scalepack part of DENZO
Z. Otwinowski, W. Minor, 1997
;

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.59
_exptl_crystal_density_method    none

_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_T_max  0.935

#===============================================================================

# 7. EXPERIMENTAL DATA

_diffrn_special_details          
; ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a

_diffrn_source                   xray_tube

_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'

_diffrn_measurement_details      
;
7020 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  1.2 deg 1 scans of   80 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    8.80 Omega =    0.00 Kappa =    0.00  183 frames
Set 2 Theta =   -8.50 Kappa = -173.00 Phi   =    0.00   38 frames
Friedel pairs were averaged. Internal R = 0.04
;

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0

_diffrn_reflns_number            7020
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.5
_diffrn_reflns_theta_max         30.04

_reflns_number_total             7020
_reflns_number_gt                4594
_reflns_threshold_expression     >3.0\s(I)

_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_molecular_graphics    ?
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)

#===============================================================================

# 8. REFINEMENT DATA

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_expression ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         4594
_refine_ls_number_parameters     240
_refine_ls_number_restraints     11
_refine_ls_number_constraints    9
_refine_ls_R_factor_all          0.109
_refine_ls_R_factor_gt           0.080
_refine_ls_wR_factor_all         0.199
_refine_ls_wR_factor_ref         0.093
_refine_ls_goodness_of_fit_all   1.453
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_shift/su_max          0.016
_refine_ls_shift/esd_mean        0.004
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.400

#===============================================================================

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
CO 0.7500 0.2500 0.16539(3) 0.0130(3) 0.500 Uani ? ? Co
CL1 0.84522(9) 0.08789(8) 0.16174(4) 0.0211(4) 1.000 Uani ? ? Cl
N1 0.8673(3) 0.3076(3) 0.1086(1) 0.019(2) 1.000 Uani ? ? N
C1 0.9005(4) 0.4049(4) 0.1094(2) 0.030(2) 1.000 Uani ? ? C
C2 0.9823(5) 0.4434(4) 0.0798(2) 0.035(3) 1.000 Uani ? ? C
C3 1.0335(4) 0.3785(4) 0.0467(2) 0.031(2) 1.000 Uani ? ? C
C4 1.0003(4) 0.2778(3) 0.0449(2) 0.021(2) 1.000 Uani ? ? C
C5 0.9175(4) 0.2451(4) 0.0766(1) 0.020(2) 1.000 Uani ? ? C
C6 1.0529(4) 0.2023(3) 0.0120(2) 0.022(2) 1.000 Uani ? ? C
O1 1.0380(3) 0.1118(3) 0.0137(1) 0.039(2) 1.000 Uani ? ? O
O2 1.1206(3) 0.2475(3) -0.0200(1) 0.023(1) 1.000 Uani ? ? O
C7 1.1783(4) 0.1808(3) -0.0537(2) 0.018(2) 1.000 Uani ? ? C
C8 1.2500 0.2500 -0.0856(2) 0.015(2) 0.500 Uani ? ? C
C9 1.1792(3) 0.3203(3) -0.1175(2) 0.018(2) 1.000 Uani ? ? C
O3 1.1178(3) 0.2551(3) -0.1498(1) 0.025(1) 1.000 Uani ? ? O
C10 1.0427(4) 0.3000(4) -0.1785(2) 0.023(2) 1.000 Uani ? ? C
O4 1.0258(3) 0.3902(3) -0.1785(1) 0.038(2) 1.000 Uani ? ? O
C11 0.9833(4) 0.2235(3) -0.2088(2) 0.023(2) 1.000 Uani ? ? C
C12 0.9965(5) 0.1195(4) -0.2008(2) 0.034(2) 1.000 Uani ? ? C
C13 0.9133(4) 0.2568(4) -0.2458(2) 0.020(2) 1.000 Uani ? ? C
N2 0.8563(3) 0.1924(3) -0.2743(1) 0.021(2) 1.000 Uani ? ? N
C14 0.8675(5) 0.0922(4) -0.2654(2) 0.032(2) 1.000 Uani ? ? C
C15 0.9369(6) 0.0527(4) -0.2299(2) 0.040(3) 1.000 Uani ? ? C
C16 1.1640(7) -0.0699(6) 0.0589(3) 0.062(4) 1.000 Uani ? ? C
CL2 1.2224(3) -0.0017(3) 0.1054(1) 0.178(2) 1.000 Uani ? ? Cl
CL3 1.1185(2) -0.1909(2) 0.08173(8) 0.063(1) 1.000 Uani ? ? Cl
CL4 1.2571(2) -0.0886(2) 0.01075(8) 0.064(1) 1.000 Uani ? ? Cl
C17 0.2500 0.2500 0.1914(2) 0.0823 0.500 Uiso ? ? C
CL5 0.1332(3) 0.2354(3) 0.1640(1) 0.099(2) 0.500 Uiso ? ? Cl
CL6 0.2492(3) 0.3345(3) 0.2341(1) 0.119(2) 0.500 Uiso ? ? Cl
CL7 0.1539(3) 0.3533(3) 0.1878(1) 0.270(7) 0.500 Uiso ? ? Cl
H1 0.8654 0.4502 0.1316 0.0402 1.000 Uiso calc C1 H
H2 1.0033 0.5129 0.0821 0.0503 1.000 Uiso calc C2 H
H3 1.0899 0.4027 0.0257 0.0407 1.000 Uiso calc C3 H
H4 0.8957 0.1757 0.0754 0.0257 1.000 Uiso calc C5 H
H5 1.1279 0.1445 -0.0737 0.0229 1.000 Uiso calc C7 H
H6 1.2222 0.1339 -0.0359 0.0229 1.000 Uiso calc C7 H
H7 1.2241 0.3651 -0.1362 0.0239 1.000 Uiso calc C9 H
H8 1.1313 0.3590 -0.0973 0.0239 1.000 Uiso calc C9 H
H9 1.0450 0.0950 -0.1761 0.0461 1.000 Uiso calc C12 H
H10 0.9054 0.3280 -0.2511 0.0259 1.000 Uiso calc C13 H
H11 0.8255 0.0459 -0.2846 0.0436 1.000 Uiso calc C14 H
H12 0.9436 -0.0188 -0.2255 0.0585 1.000 Uiso calc C15 H

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
CO 0.0134(3) 0.0145(3) 0.0114(3) 0.0015(3) 0.0000 0.0000 Co
CL1 0.0214(4) 0.0188(4) 0.0235(4) 0.0064(4) 0.0004(4) 0.0022(4) Cl
N1 0.022(2) 0.018(2) 0.018(2) -0.000(1) 0.006(1) -0.001(1) N
C1 0.035(2) 0.019(2) 0.038(2) -0.002(2) 0.017(2) -0.005(2) C
C2 0.045(3) 0.019(2) 0.052(3) -0.009(2) 0.027(2) -0.007(2) C
C3 0.033(2) 0.024(2) 0.037(2) -0.005(2) 0.019(2) -0.003(2) C
C4 0.022(2) 0.021(2) 0.020(2) -0.001(2) 0.007(2) -0.001(2) C
C5 0.022(2) 0.018(2) 0.019(2) -0.000(2) 0.006(2) -0.002(2) C
C6 0.022(2) 0.022(2) 0.023(2) -0.004(2) 0.011(2) -0.002(2) C
O1 0.056(2) 0.021(2) 0.049(2) -0.007(2) 0.033(2) -0.006(2) O
O2 0.025(1) 0.023(1) 0.021(1) -0.003(1) 0.012(1) -0.004(1) O
C7 0.018(2) 0.019(2) 0.016(2) 0.000(2) 0.004(1) -0.003(2) C
C8 0.012(2) 0.021(2) 0.012(2) 0.004(3) 0.0000 0.0000 C
C9 0.015(2) 0.023(2) 0.017(2) 0.002(2) -0.004(1) -0.001(2) C
O3 0.027(1) 0.024(1) 0.024(1) 0.005(1) -0.015(1) -0.005(1) O
C10 0.025(2) 0.026(2) 0.019(2) 0.001(2) -0.009(2) -0.002(2) C
O4 0.052(2) 0.021(2) 0.049(2) 0.003(2) -0.031(2) -0.002(2) O
C11 0.025(2) 0.022(2) 0.022(2) 0.004(2) -0.012(2) -0.006(2) C
C12 0.048(3) 0.024(2) 0.034(2) 0.013(2) -0.026(2) -0.002(2) C
C13 0.023(2) 0.018(2) 0.019(2) 0.004(2) -0.006(2) -0.002(2) C
N2 0.023(2) 0.022(2) 0.019(2) 0.005(2) -0.009(1) -0.000(1) N
C14 0.045(3) 0.023(2) 0.033(2) 0.004(2) -0.021(2) -0.007(2) C
C15 0.070(4) 0.020(2) 0.044(3) 0.011(3) -0.033(3) -0.005(2) C
C16 0.057(4) 0.056(4) 0.076(5) -0.013(4) 0.016(4) -0.018(4) C
CL2 0.164(2) 0.252(3) 0.136(2) -0.130(2) 0.053(2) -0.123(2) Cl
CL3 0.0439(8) 0.079(1) 0.071(1) 0.0027(9) 0.0086(8) 0.017(1) Cl
CL4 0.062(1) 0.058(1) 0.072(1) -0.005(1) 0.0204(9) 0.0015(9) Cl

# 10. MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
CO CL1 2.428(1) . . ?
CO CL1 2.428(1) . 2_655 ?
CO N1 2.237(4) . . ?
CO N1 2.237(4) . 2_655 ?
CO N2 2.221(4) . 7_555 ?
CO N2 2.221(4) . 8_655 ?
N1 C1 1.340(6) . . ?
N1 C5 1.344(5) . . ?
C1 C2 1.379(7) . . ?
C2 C3 1.387(7) . . ?
C3 C4 1.383(7) . . ?
C4 C5 1.396(6) . . ?
C4 C6 1.481(6) . . ?
C6 O1 1.202(6) . . ?
C6 O2 1.339(5) . . ?
O2 C7 1.448(5) . . ?
C7 C8 1.531(5) . . ?
C7 C8 1.531(5) . 2_755 ?
C8 C9 1.533(5) . . ?
C8 C9 1.533(5) . 2_755 ?
C9 O3 1.437(5) . . ?
O3 C10 1.340(5) . . ?
C10 O4 1.201(6) . . ?
C10 C11 1.488(6) . . ?
C11 C12 1.391(7) . . ?
C11 C13 1.391(6) . . ?
C12 C15 1.387(8) . . ?
C13 N2 1.342(6) . . ?
N2 C14 1.345(6) . . ?
C14 C15 1.385(7) . . ?
C16 CL2 1.705(9) . . ?
C16 CL3 1.794(8) . . ?
C16 CL4 1.750(8) . . ?
C17 CL5 1.622(2) . . ?
C17 CL5 1.622(2) . 2_555 ?
C17 CL6 1.604(3) . . ?
C17 CL6 1.604(3) . 2_555 ?
C17 CL7 1.7979(2) . . ?
C17 CL7 1.7979(2) . 2_555 ?
CL5 CL7 1.6968 . . ?
CL6 CL7 1.7308 . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL1 CO CL1 175.33(6) . . 2_655 ?
CL1 CO N1 87.7(1) . . . ?
CL1 CO N1 89.1(1) . . 2_655 ?
CL1 CO N2 92.7(1) . . 7_555 ?
CL1 CO N2 90.7(1) . . 8_655 ?
CL1 CO N1 89.1(1) 2_655 . . ?
CL1 CO N1 87.7(1) 2_655 . 2_655 ?
CL1 CO N2 90.7(1) 2_655 . 7_555 ?
CL1 CO N2 92.7(1) 2_655 . 8_655 ?
N1 CO N1 93.1(2) . . 2_655 ?
N1 CO N2 90.8(1) . . 7_555 ?
N1 CO N2 175.8(1) . . 8_655 ?
N1 CO N2 175.8(1) 2_655 . 7_555 ?
N1 CO N2 90.8(1) 2_655 . 8_655 ?
N2 CO N2 85.3(2) 7_555 . 8_655 ?
C1 N1 C5 117.0(4) . . . ?
N1 C1 C2 124.1(5) . . . ?
C1 C2 C3 118.7(5) . . . ?
C2 C3 C4 118.4(5) . . . ?
C3 C4 C5 119.1(4) . . . ?
C3 C4 C6 122.2(4) . . . ?
C5 C4 C6 118.7(4) . . . ?
N1 C5 C4 122.8(4) . . . ?
C4 C6 O1 125.0(4) . . . ?
C4 C6 O2 111.3(4) . . . ?
O1 C6 O2 123.8(4) . . . ?
C6 O2 C7 116.3(4) . . . ?
O2 C7 C8 106.1(3) . . . ?
C7 C8 C7 111.2(5) . . 2_755 ?
C7 C8 C9 110.6(2) . . . ?
C7 C8 C9 106.6(2) . . 2_755 ?
C7 C8 C9 106.6(2) 2_755 . . ?
C7 C8 C9 110.6(2) 2_755 . 2_755 ?
C9 C8 C9 111.4(5) . . 2_755 ?
C8 C9 O3 106.3(3) . . . ?
C9 O3 C10 116.7(4) . . . ?
O3 C10 O4 123.5(4) . . . ?
O3 C10 C11 111.0(4) . . . ?
O4 C10 C11 125.5(4) . . . ?
C10 C11 C12 121.3(4) . . . ?
C10 C11 C13 119.2(4) . . . ?
C12 C11 C13 119.5(4) . . . ?
C11 C12 C15 118.1(4) . . . ?
C11 C13 N2 122.6(4) . . . ?
C13 N2 C14 117.4(4) . . . ?
N2 C14 C15 123.6(5) . . . ?
C12 C15 C14 118.8(5) . . . ?
CL2 C16 CL3 109.8(5) . . . ?
CL2 C16 CL4 110.6(5) . . . ?
CL3 C16 CL4 109.6(4) . . . ?
CL5 C17 CL5 125.6(3) . . 2_555 ?
CL5 C17 CL6 114.02(6) . . . ?
CL5 C17 CL6 104.68(5) . . 2_555 ?
CL5 C17 CL7 59.23(4) . . . ?
CL5 C17 CL7 117.6(1) . . 2_555 ?
CL5 C17 CL6 104.68(5) 2_555 . . ?
CL5 C17 CL6 114.02(6) 2_555 . 2_555 ?
CL5 C17 CL7 117.6(1) 2_555 . . ?
CL5 C17 CL7 59.23(4) 2_555 . 2_555 ?
CL6 C17 CL6 87.5(2) . . 2_555 ?
CL6 C17 CL7 60.85(5) . . . ?
CL6 C17 CL7 124.3(2) . . 2_555 ?
CL6 C17 CL7 124.3(2) 2_555 . . ?
CL6 C17 CL7 60.85(5) 2_555 . 2_555 ?
CL7 C17 CL7 173.9(3) . . 2_555 ?
C17 CL5 CL7 65.57(3) . . . ?
C17 CL6 CL7 65.13(7) . . . ?
C17 CL7 CL5 55.20(7) . . . ?
C17 CL7 CL6 54.0(1) . . . ?
CL5 CL7 CL6 104.23 . . . ?

data_st1190
_database_code_CSD               202741

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C33 H28 Cl12 Hg2 N4 O8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C33 H28 Cl12 Hg2 N4 O8'
_chemical_formula_weight         1435.23
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Hg ? -3.084 9.223 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,+y,1/2-z
-x,-y,-z
+x,-y,1/2+z
1/2+x,1/2+y,+z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a                   24.2740(6)
_cell_length_b                   10.8173(3)
_cell_length_c                   20.6707(6)
_cell_angle_alpha                90
_cell_angle_beta                 123.094(5)
_cell_angle_gamma                90
_cell_volume                     4547.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    9574
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      29.1
_cell_special_details            
;
Cell parameters refined using Scalepack part of DENZO
Z. Otwinowski, W. Minor, 1997
;

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.10
_exptl_crystal_density_method    none

_exptl_crystal_F_000             2728
_exptl_absorpt_coefficient_mu    7.501
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_T_max  0.741

#===============================================================================

# 7. EXPERIMENTAL DATA

_diffrn_special_details          
; ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a

_diffrn_source                   xray_tube

_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'

_diffrn_measurement_details      
;
9574 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  2.0 deg 1 scans of   60 sec per frame.
Data collection was divided into  1 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    7.80 Omega =    0.00 Kappa =    0.00   90 frames
Friedel pairs were averaged. Internal R = 0.04
;

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0

_diffrn_reflns_number            9574
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.5
_diffrn_reflns_theta_max         29.15

_reflns_number_total             6213
_reflns_number_gt                3397
_reflns_threshold_expression     >3.0\s(I)

_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_molecular_graphics    ?
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)

#===============================================================================

# 8. REFINEMENT DATA

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_expression ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         3397
_refine_ls_number_parameters     267
_refine_ls_number_restraints     4
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.080
_refine_ls_R_factor_gt           0.038
_refine_ls_wR_factor_all         0.195
_refine_ls_wR_factor_ref         0.053
_refine_ls_goodness_of_fit_all   1.961
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_shift/su_max          0.005
_refine_ls_shift/esd_mean        0.000
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.189

#===============================================================================

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
HG 1.44685(1) 0.60036(2) 0.64409(1) 0.0371 1.000 Uani ? ? Hg
CL1 1.52027(8) 0.4427(2) 0.6630(1) 0.0558(9) 1.000 Uani ? ? Cl
CL2 1.39583(9) 0.7364(2) 0.6834(1) 0.0512(9) 1.000 Uani ? ? Cl
N1 1.3479(2) 0.5159(5) 0.5285(3) 0.036(3) 1.000 Uani ? ? N
C1 1.3496(3) 0.3980(7) 0.5112(5) 0.045(4) 1.000 Uani ? ? C
C2 1.2932(3) 0.3347(6) 0.4568(5) 0.042(4) 1.000 Uani ? ? C
C3 1.2342(3) 0.3952(6) 0.4182(4) 0.033(3) 1.000 Uani ? ? C
C4 1.2322(3) 0.5181(6) 0.4347(4) 0.035(3) 1.000 Uani ? ? C
C5 1.2885(3) 0.5730(6) 0.4903(4) 0.042(3) 1.000 Uani ? ? C
C6 1.1740(3) 0.3241(6) 0.3608(4) 0.039(3) 1.000 Uani ? ? C
O1 1.1758(2) 0.2155(5) 0.3466(4) 0.059(3) 1.000 Uani ? ? O
O2 1.1187(2) 0.3893(4) 0.3305(2) 0.031(2) 1.000 Uani ? ? O
C7 1.0594(3) 0.3185(5) 0.2876(4) 0.030(3) 1.000 Uani ? ? C
C8 1.0000 0.4047(7) 0.2500 0.023(4) 0.500 Uani ? ? C
C9 0.9987(3) 0.4910(6) 0.3078(4) 0.035(3) 1.000 Uani ? ? C
O3 0.9837(2) 0.4269(4) 0.3580(2) 0.036(2) 1.000 Uani ? ? O
C10 1.0322(3) 0.3976(6) 0.4284(4) 0.041(3) 1.000 Uani ? ? C
O4 1.0901(2) 0.4161(6) 0.4533(3) 0.054(3) 1.000 Uani ? ? O
C11 1.0102(3) 0.3405(6) 0.4755(3) 0.038(3) 1.000 Uani ? ? C
C12 1.0555(3) 0.3118(8) 0.5512(4) 0.047(4) 1.000 Uani ? ? C
C13 1.0352(3) 0.2576(9) 0.5944(4) 0.051(4) 1.000 Uani ? ? C
N2 0.9729(3) 0.2298(5) 0.5675(3) 0.046(3) 1.000 Uani ? ? N
C14 0.9291(3) 0.2602(7) 0.4940(5) 0.057(4) 1.000 Uani ? ? C
C15 0.9452(3) 0.3144(8) 0.4460(4) 0.053(4) 1.000 Uani ? ? C
C16 1.2852(5) 0.455(1) 0.2105(9) 0.291(8) 1.000 Uani ? ? C
CL3 1.2805(2) 0.3023(4) 0.2286(3) 0.309(3) 1.000 Uani ? ? Cl
CL4 1.2184(1) 0.4712(3) 0.0993(2) 0.094(1) 1.000 Uani ? ? Cl
C17 1.2618(4) 0.538(2) 0.2299(7) 0.128(8) 1.000 Uani ? ? C
CL5 1.3320(1) 0.5315(7) 0.3387(2) 0.134(3) 1.000 Uani ? ? Cl
CL6 1.1874(1) 0.5092(3) 0.2258(1) 0.077(1) 1.000 Uani ? ? Cl
H1 1.3906 0.3559 0.5369 0.0682 1.000 Uiso calc C1 H
H2 1.2956 0.2500 0.4464 0.0733 1.000 Uiso calc C2 H
H3 1.1921 0.5631 0.4075 0.0499 1.000 Uiso calc C4 H
H4 1.2863 0.6563 0.5034 0.0592 1.000 Uiso calc C5 H
H5 1.0566 0.2634 0.3215 0.0440 1.000 Uiso calc C7 H
H6 1.0598 0.2726 0.2487 0.0440 1.000 Uiso calc C7 H
H7 0.9662 0.5526 0.2799 0.0443 1.000 Uiso calc C9 H
H8 1.0406 0.5290 0.3387 0.0443 1.000 Uiso calc C9 H
H9 1.1007 0.3294 0.5735 0.0678 1.000 Uiso calc C12 H
H10 1.0675 0.2387 0.6468 0.0737 1.000 Uiso calc C13 H
H11 0.8840 0.2437 0.4735 0.0800 1.000 Uiso calc C14 H
H12 0.9123 0.3330 0.3938 0.0746 1.000 Uiso calc C15 H
H13 1.3312 0.4675 0.2355 0.3509 1.000 Uiso calc C16 H
H14 1.2506 0.6088 0.1982 0.1823 1.000 Uiso calc C17 H

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
HG 0.0360 0.0339(1) 0.0418(1) -0.0023(1) 0.01709(8) 0.0029(1) Hg
CL1 0.0444(8) 0.0438(8) 0.090(1) 0.0134(8) 0.0323(7) 0.026(1) Cl
CL2 0.0593(9) 0.0439(9) 0.0516(9) -0.0045(8) 0.0288(6) -0.0103(8) Cl
N1 0.031(2) 0.037(3) 0.042(3) 0.002(2) 0.015(2) -0.002(3) N
C1 0.041(4) 0.049(4) 0.044(4) 0.012(3) 0.008(3) -0.001(4) C
C2 0.035(3) 0.037(4) 0.059(5) 0.014(3) 0.001(3) -0.010(4) C
C3 0.030(3) 0.040(3) 0.031(3) 0.003(3) 0.010(2) -0.004(3) C
C4 0.030(3) 0.035(3) 0.043(3) 0.003(3) 0.015(2) -0.006(3) C
C5 0.040(3) 0.037(3) 0.051(4) -0.001(3) 0.019(3) -0.003(3) C
C6 0.035(3) 0.039(4) 0.043(4) -0.002(3) 0.010(3) -0.012(3) C
O1 0.046(3) 0.043(3) 0.106(4) 0.008(2) -0.001(3) -0.036(3) O
O2 0.023(2) 0.034(2) 0.038(2) 0.005(2) 0.011(1) -0.004(2) O
C7 0.031(3) 0.022(3) 0.039(3) -0.003(2) 0.013(2) -0.006(3) C
C8 0.022(3) 0.023(4) 0.025(4) 0.0000 0.006(3) 0.0000 C
C9 0.037(3) 0.029(3) 0.039(3) 0.007(3) 0.022(2) 0.004(3) C
O3 0.034(2) 0.036(2) 0.039(2) 0.003(2) 0.020(1) 0.007(2) O
C10 0.046(3) 0.040(4) 0.038(3) -0.001(3) 0.024(2) -0.005(3) C
O4 0.035(2) 0.108(4) 0.041(2) -0.010(3) 0.017(2) 0.012(3) O
C11 0.042(3) 0.035(3) 0.038(3) 0.002(3) 0.025(2) 0.005(3) C
C12 0.036(3) 0.081(5) 0.035(3) -0.024(3) 0.017(2) -0.005(4) C
C13 0.046(3) 0.089(6) 0.032(3) -0.009(4) 0.020(2) -0.002(4) C
N2 0.048(3) 0.039(3) 0.052(3) 0.000(2) 0.029(2) 0.011(3) N
C14 0.041(3) 0.054(4) 0.082(4) -0.002(3) 0.029(3) 0.032(4) C
C15 0.041(3) 0.078(5) 0.047(3) 0.013(4) 0.020(2) 0.038(4) C
C16 0.287(6) 0.145(7) 0.60(1) 0.170(5) 0.381(5) 0.243(7) C
CL3 0.297(2) 0.164(3) 0.607(3) 0.124(2) 0.371(2) 0.225(2) Cl
CL4 0.096(1) 0.091(2) 0.095(1) -0.021(1) 0.058(1) -0.013(1) Cl
C17 0.061(4) 0.21(1) 0.167(8) 0.015(7) 0.070(4) 0.069(9) C
CL5 0.064(1) 0.539(9) 0.069(2) -0.032(3) 0.036(1) 0.007(4) Cl
CL6 0.0463(9) 0.135(2) 0.072(1) -0.009(1) 0.0322(7) 0.008(2) Cl

# 10. MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
HG CL1 2.340(2) . . ?
HG CL2 2.336(2) . . ?
HG N1 2.459(5) . . ?
HG N2 2.441(6) . 5_555 ?
N1 C1 1.330(9) . . ?
N1 C5 1.358(9) . . ?
C1 C2 1.39(1) . . ?
C2 C3 1.37(1) . . ?
C3 C4 1.38(1) . . ?
C3 C6 1.50(1) . . ?
C4 C5 1.35(1) . . ?
C6 O1 1.218(9) . . ?
C6 O2 1.332(8) . . ?
O2 C7 1.432(8) . . ?
C7 C8 1.525(8) . . ?
C7 C8 1.525(8) . 2_755 ?
C8 C9 1.530(9) . . ?
C8 C9 1.530(9) . 2_755 ?
C9 O3 1.450(9) . . ?
O3 C10 1.317(9) . . ?
C10 O4 1.220(9) . . ?
C10 C11 1.48(1) . . ?
C11 C12 1.37(1) . . ?
C11 C15 1.37(1) . . ?
C12 C13 1.36(1) . . ?
C13 N2 1.33(1) . . ?
N2 C14 1.33(1) . . ?
C14 C15 1.38(1) . . ?
C16 CL3 1.71(2) . . ?
C16 CL4 1.97(3) . . ?
C16 C17 1.23(3) . . ?
C17 CL5 1.94(2) . . ?
C17 CL6 1.79(1) . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL1 HG CL2 154.27(6) . . . ?
CL1 HG N1 98.18(14) . . . ?
CL1 HG N2 94.78 . . 5_555 ?
CL2 HG N1 98.62(14) . . . ?
CL2 HG N2 103.80(14) . . 5_555 ?
N1 HG N2 92.52 . . 5_555 ?
C1 N1 C5 117.3(6) . . . ?
N1 C1 C2 122.0(7) . . . ?
C1 C2 C3 119.4(7) . . . ?
C2 C3 C4 119.0(7) . . . ?
C2 C3 C6 118.4(7) . . . ?
C4 C3 C6 122.6(7) . . . ?
C3 C4 C5 118.5(7) . . . ?
N1 C5 C4 123.7(7) . . . ?
C3 C6 O1 122.6(7) . . . ?
C3 C6 O2 113.4(6) . . . ?
O1 C6 O2 123.9(7) . . . ?
C6 O2 C7 115.0(5) . . . ?
O2 C7 C8 109.9(5) . . . ?
C7 C8 C7 104.7(7) . . 2_755 ?
C7 C8 C9 113.0(4) . . . ?
C7 C8 C9 110.8(4) . . 2_755 ?
C7 C8 C9 110.8(4) 2_755 . . ?
C7 C8 C9 113.0(4) 2_755 . 2_755 ?
C9 C8 C9 104.8(7) . . 2_755 ?
C8 C9 O3 112.8(5) . . . ?
C9 O3 C10 118.9(6) . . . ?
O3 C10 O4 123.8(8) . . . ?
O3 C10 C11 113.7(7) . . . ?
O4 C10 C11 122.5(8) . . . ?
C10 C11 C12 119.6(7) . . . ?
C10 C11 C15 122.2(7) . . . ?
C12 C11 C15 118.2(7) . . . ?
C11 C12 C13 119.5(7) . . . ?
C12 C13 N2 123.9(8) . . . ?
C13 N2 C14 115.9(7) . . . ?
N2 C14 C15 124.1(7) . . . ?
C11 C15 C14 118.3(7) . . . ?
CL3 C16 CL4 103(1) . . . ?
CL3 C16 C17 121(1) . . . ?
CL4 C16 C17 94(1) . . . ?
C16 C17 CL5 94(1) . . . ?
C16 C17 CL6 119(1) . . . ?
CL5 C17 CL6 105.9(8) . . . ?

data_st1219
_database_code_CSD               202742

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H27 Cl6 Hg2 N4 O9'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C30 H27 Cl6 Hg2 N4 O9'
_chemical_formula_weight         1201.47
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Hg ? -3.084 9.223 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a                   14.7630(3)
_cell_length_b                   13.2294(3)
_cell_length_c                   20.6902(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.285(5)
_cell_angle_gamma                90
_cell_volume                     4039.9(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    19235
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      29.1
_cell_special_details            
;
Cell parameters refined using Scalepack part of DENZO
Z. Otwinowski, W. Minor, 1997
;

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.98
_exptl_crystal_density_method    none

_exptl_crystal_F_000             2276
_exptl_absorpt_coefficient_mu    8.040
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_T_max  0.526

#===============================================================================

# 7. EXPERIMENTAL DATA

_diffrn_special_details          
; ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a

_diffrn_source                   xray_tube

_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'

_diffrn_measurement_details      
;
19235 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  0.9 deg 1 scans of   90 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    7.80 Omega =    0.00 Kappa =    0.00  202 frames
Set 2 Theta =   -7.50 Kappa =  -73.00 Phi   =    0.00   83 frames
Friedel pairs were averaged. Internal R = 0.06
;

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0

_diffrn_reflns_number            19235
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.5
_diffrn_reflns_theta_max         29.11

_reflns_number_total             11285
_reflns_number_gt                6214
_reflns_threshold_expression     >3.0\s(I)

_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_molecular_graphics    ?
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)

#===============================================================================

# 8. REFINEMENT DATA

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_expression ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         6214
_refine_ls_number_parameters     441
_refine_ls_number_restraints     0
_refine_ls_number_constraints    15
_refine_ls_R_factor_all          0.126
_refine_ls_R_factor_gt           0.060
_refine_ls_wR_factor_all         0.351
_refine_ls_wR_factor_ref         0.074
_refine_ls_goodness_of_fit_all   1.518
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/esd_mean        0.000
_refine_diff_density_max         1.826
_refine_diff_density_min         -0.381

#===============================================================================

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
HG1 1.06455(3) 0.32421(4) 0.87019(3) 0.0416 1.000 Uani ? ? Hg
HG2 2.04554(3) 0.26584(4) 0.32414(3) 0.0444 1.000 Uani ? ? Hg
CL1 1.1245(2) 0.1590(3) 0.8873(2) 0.051(2) 1.000 Uani ? ? Cl
CL2 1.0142(3) 0.4797(3) 0.9089(2) 0.063(2) 1.000 Uani ? ? Cl
CL3 1.9893(3) 0.1005(3) 0.3092(2) 0.058(2) 1.000 Uani ? ? Cl
CL4 2.0917(3) 0.4254(3) 0.2883(2) 0.072(2) 1.000 Uani ? ? Cl
C1 1.5520(7) 0.3015(9) 0.5959(5) 0.031(5) 1.000 Uani ? ? C
C2 1.4857(8) 0.2394(9) 0.6358(6) 0.038(6) 1.000 Uani ? ? C
O1 1.4139(5) 0.3073(6) 0.6548(4) 0.038(4) 1.000 Uani ? ? O
C3 1.3624(8) 0.2742(9) 0.7037(6) 0.037(6) 1.000 Uani ? ? C
O2 1.3748(6) 0.1965(7) 0.7317(5) 0.049(5) 1.000 Uani ? ? O
C4 1.2897(8) 0.3470(9) 0.7184(6) 0.038(6) 1.000 Uani ? ? C
C5 1.2777(8) 0.440(1) 0.6886(6) 0.040(6) 1.000 Uani ? ? C
C6 1.2064(9) 0.501(1) 0.7074(7) 0.043(7) 1.000 Uani ? ? C
C7 1.1510(8) 0.4663(9) 0.7553(6) 0.038(6) 1.000 Uani ? ? C
N1 1.1628(6) 0.3773(8) 0.7862(5) 0.036(5) 1.000 Uani ? ? N
C8 1.2310(8) 0.320(1) 0.7679(6) 0.040(6) 1.000 Uani ? ? C
C9 1.6171(8) 0.2248(9) 0.5647(6) 0.033(6) 1.000 Uani ? ? C
O3 1.6911(5) 0.2845(6) 0.5400(4) 0.038(4) 1.000 Uani ? ? O
C10 1.7466(8) 0.236(1) 0.5016(7) 0.041(6) 1.000 Uani ? ? C
O4 1.7419(7) 0.1486(7) 0.4878(6) 0.061(6) 1.000 Uani ? ? O
C11 1.8163(7) 0.3071(9) 0.4751(6) 0.031(6) 1.000 Uani ? ? C
C12 1.820(1) 0.409(1) 0.4921(7) 0.050(7) 1.000 Uani ? ? C
C13 1.886(1) 0.467(1) 0.4659(8) 0.061(8) 1.000 Uani ? ? C
C14 1.946(1) 0.425(1) 0.4237(7) 0.052(8) 1.000 Uani ? ? C
N2 1.9451(7) 0.3273(8) 0.4088(5) 0.040(5) 1.000 Uani ? ? N
C15 1.8799(8) 0.2684(9) 0.4339(6) 0.035(6) 1.000 Uani ? ? C
C16 1.5036(8) 0.3665(9) 0.5451(6) 0.036(6) 1.000 Uani ? ? C
O5 1.4450(6) 0.2982(6) 0.5096(4) 0.039(4) 1.000 Uani ? ? O
C17 1.3757(9) 0.338(1) 0.4744(6) 0.041(6) 1.000 Uani ? ? C
O6 1.3631(7) 0.4260(7) 0.4671(5) 0.052(6) 1.000 Uani ? ? O
C18 1.3169(9) 0.2576(9) 0.4482(6) 0.041(6) 1.000 Uani ? ? C
C19 1.3313(9) 0.1557(9) 0.4626(6) 0.037(6) 1.000 Uani ? ? C
C20 1.268(1) 0.086(1) 0.4374(8) 0.048(8) 1.000 Uani ? ? C
C21 1.197(1) 0.119(1) 0.3995(8) 0.051(8) 1.000 Uani ? ? C
N3 1.1841(7) 0.2163(9) 0.3852(6) 0.044(6) 1.000 Uani ? ? N
C22 1.2432(8) 0.284(1) 0.4079(6) 0.040(6) 1.000 Uani ? ? C
C23 1.6061(9) 0.371(1) 0.6414(6) 0.040(6) 1.000 Uani ? ? C
O7 1.6694(6) 0.3089(7) 0.6784(4) 0.043(5) 1.000 Uani ? ? O
C24 1.731(1) 0.350(1) 0.716(1) 0.053(9) 1.000 Uani ? ? C
O8 1.7236(9) 0.436(1) 0.7351(9) 0.103(9) 1.000 Uani ? ? O
C25 1.8023(8) 0.283(1) 0.7406(8) 0.041(7) 1.000 Uani ? ? C
C26 1.802(1) 0.180(1) 0.7275(8) 0.051(8) 1.000 Uani ? ? C
C27 1.873(1) 0.121(1) 0.7488(9) 0.07(1) 1.000 Uani ? ? C
C28 1.938(1) 0.166(1) 0.7871(9) 0.061(9) 1.000 Uani ? ? C
N4 1.9390(8) 0.2619(9) 0.8031(6) 0.049(6) 1.000 Uani ? ? N
C29 1.8711(9) 0.321(1) 0.7781(8) 0.047(7) 1.000 Uani ? ? C
C30 0.0762(5) 0.1265(5) 0.6198(3) 0.09(1) 0.500 Uiso ? ? C
CL5 0.1892(5) 0.0832(5) 0.6245(3) 0.157(6) 0.500 Uiso ? ? Cl
CL6 0.0227(5) 0.0947(5) 0.5401(3) 0.180(8) 0.500 Uiso ? ? Cl
C31 0.0845(5) 0.2332(5) 0.6199(3) 0.13(2) 0.500 Uiso ? ? C
CL7 0.0121(5) 0.2913(5) 0.6426(3) 0.075(2) 0.500 Uiso ? ? Cl
CL8 0.1680(5) 0.2678(5) 0.5657(3) 0.102(3) 0.500 Uiso ? ? Cl
O10 -0.085(1) 0.137(1) 0.5867(7) 0.030(3) 0.500 Uiso ? ? O
O11 0.098(1) 0.218(1) 0.5199(9) 0.048(5) 0.500 Uiso ? ? O
H1 1.5159 0.2127 0.6731 0.0504 1.000 Uiso calc C2 H
H2 1.4613 0.1856 0.6105 0.0504 1.000 Uiso calc C2 H
H3 1.3174 0.4613 0.6558 0.0517 1.000 Uiso calc C5 H
H4 1.1961 0.5645 0.6877 0.0572 1.000 Uiso calc C6 H
H5 1.1015 0.5076 0.7672 0.0491 1.000 Uiso calc C7 H
H6 1.2405 0.2567 0.7892 0.0526 1.000 Uiso calc C8 H
H7 1.5870 0.1894 0.5305 0.0433 1.000 Uiso calc C9 H
H8 1.6390 0.1778 0.5960 0.0433 1.000 Uiso calc C9 H
H9 1.7775 0.4367 0.5209 0.0659 1.000 Uiso calc C12 H
H10 1.8908 0.5368 0.4769 0.0796 1.000 Uiso calc C13 H
H11 1.9902 0.4674 0.4044 0.0679 1.000 Uiso calc C14 H
H12 1.8778 0.1987 0.4229 0.0467 1.000 Uiso calc C15 H
H13 1.5462 0.3965 0.5172 0.0471 1.000 Uiso calc C16 H
H14 1.4692 0.4179 0.5652 0.0471 1.000 Uiso calc C16 H
H15 1.3818 0.1345 0.4884 0.0480 1.000 Uiso calc C19 H
H16 1.2741 0.0155 0.4468 0.0685 1.000 Uiso calc C20 H
H17 1.1551 0.0703 0.3825 0.0685 1.000 Uiso calc C21 H
H18 1.2351 0.3525 0.3962 0.0520 1.000 Uiso calc C22 H
H19 1.5663 0.4049 0.6697 0.0519 1.000 Uiso calc C23 H
H20 1.6382 0.4197 0.6170 0.0519 1.000 Uiso calc C23 H
H21 1.7524 0.1499 0.7042 0.0716 1.000 Uiso calc C26 H
H22 1.8774 0.0516 0.7373 0.0923 1.000 Uiso calc C27 H
H23 1.9867 0.1249 0.8031 0.0807 1.000 Uiso calc C28 H
H24 1.8720 0.3918 0.7870 0.0657 1.000 Uiso calc C29 H

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
HG1 0.0384 0.0404(2) 0.0463(2) 0.0025(2) 0.0153(2) -0.0009(2) Hg
HG2 0.0328 0.0483(3) 0.0554(3) 0.0033(2) 0.0107(2) 0.0053(3) Hg
CL1 0.055(2) 0.047(2) 0.052(2) 0.015(2) 0.007(2) 0.004(2) Cl
CL2 0.075(2) 0.039(2) 0.085(2) 0.003(2) 0.040(2) -0.005(2) Cl
CL3 0.049(2) 0.050(2) 0.081(3) 0.007(2) -0.006(2) -0.002(2) Cl
CL4 0.057(2) 0.065(2) 0.100(3) 0.005(2) 0.033(2) 0.031(2) Cl
C1 0.029(5) 0.031(5) 0.034(5) -0.002(5) 0.012(4) -0.001(5) C
C2 0.039(6) 0.027(5) 0.051(7) -0.004(5) 0.019(5) -0.005(5) C
O1 0.035(4) 0.031(4) 0.050(5) 0.007(4) 0.019(3) 0.004(4) O
C3 0.030(5) 0.033(6) 0.049(7) 0.001(5) 0.012(5) -0.001(6) C
O2 0.048(5) 0.034(4) 0.071(6) 0.001(4) 0.029(4) 0.016(4) O
C4 0.035(6) 0.033(6) 0.047(6) -0.000(5) 0.020(5) 0.002(5) C
C5 0.037(6) 0.037(6) 0.046(7) 0.000(6) 0.012(5) 0.006(6) C
C6 0.044(7) 0.033(6) 0.056(8) 0.008(6) 0.010(6) 0.003(6) C
C7 0.042(6) 0.033(6) 0.038(6) 0.011(5) 0.010(5) -0.004(5) C
N1 0.026(4) 0.036(5) 0.049(6) 0.000(4) 0.013(4) 0.003(5) N
C8 0.035(6) 0.040(6) 0.047(6) -0.000(6) 0.015(5) 0.002(6) C
C9 0.031(5) 0.035(6) 0.034(6) 0.001(5) 0.007(5) 0.005(5) C
O3 0.038(4) 0.037(4) 0.041(4) -0.002(4) 0.016(3) -0.001(4) O
C10 0.033(6) 0.037(6) 0.055(7) 0.003(5) 0.015(5) -0.001(6) C
O4 0.060(5) 0.037(5) 0.103(7) 0.001(5) 0.043(5) -0.009(5) O
C11 0.019(5) 0.038(6) 0.041(6) -0.001(5) -0.006(5) 0.001(5) C
C12 0.056(8) 0.042(7) 0.054(8) 0.001(7) 0.012(7) -0.013(6) C
C13 0.069(9) 0.046(7) 0.070(9) -0.022(7) 0.026(7) -0.008(7) C
C14 0.050(8) 0.055(8) 0.053(8) -0.011(7) 0.010(6) 0.002(7) C
N2 0.035(5) 0.042(5) 0.041(5) -0.004(5) 0.010(4) -0.002(5) N
C15 0.029(5) 0.032(5) 0.047(7) 0.005(5) 0.010(5) -0.002(5) C
C16 0.044(6) 0.026(5) 0.040(6) -0.002(5) 0.018(5) 0.003(5) C
O5 0.036(4) 0.031(4) 0.051(5) -0.002(4) 0.003(4) -0.001(4) O
C17 0.043(6) 0.037(6) 0.044(7) 0.001(6) 0.011(5) 0.007(6) C
O6 0.051(6) 0.035(5) 0.081(7) 0.001(5) -0.011(5) 0.009(5) O
C18 0.043(6) 0.032(6) 0.049(7) 0.004(5) 0.020(5) 0.000(5) C
C19 0.039(6) 0.037(6) 0.035(6) 0.000(6) -0.004(5) -0.004(5) C
C20 0.047(8) 0.029(6) 0.08(1) 0.002(6) -0.004(8) 0.008(7) C
C21 0.047(8) 0.039(7) 0.071(9) -0.008(7) -0.004(7) 0.002(7) C
N3 0.031(5) 0.045(6) 0.060(7) 0.002(5) -0.000(5) 0.005(6) N
C22 0.036(6) 0.036(6) 0.048(7) -0.002(5) 0.012(5) 0.006(6) C
C23 0.044(6) 0.037(6) 0.039(6) -0.007(6) 0.012(5) -0.008(5) C
O7 0.049(5) 0.039(5) 0.041(5) -0.006(4) -0.011(4) 0.002(4) O
C24 0.032(7) 0.038(7) 0.12(1) 0.002(6) -0.002(8) -0.017(8) C
O8 0.067(7) 0.072(7) 0.23(2) 0.021(7) -0.059(9) -0.059(9) O
C25 0.028(6) 0.032(6) 0.077(9) -0.000(5) 0.006(6) 0.002(7) C
C26 0.037(7) 0.040(7) 0.09(1) -0.005(6) -0.010(7) -0.002(8) C
C27 0.08(1) 0.043(8) 0.09(1) -0.005(9) -0.01(1) 0.008(9) C
C28 0.064(9) 0.046(8) 0.08(1) 0.002(8) -0.004(9) 0.007(8) C
N4 0.042(6) 0.050(6) 0.056(7) 0.001(5) 0.009(5) -0.004(6) N
C29 0.030(6) 0.044(7) 0.077(9) -0.000(6) 0.012(6) -0.000(7) C

# 10. MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
HG1 CL1 2.382(4) . . ?
HG1 CL2 2.335(4) . . ?
HG1 N1 2.394(10) . . ?
HG2 CL3 2.358(4) . . ?
HG2 CL4 2.344(4) . . ?
HG2 N2 2.459(10) . . ?
C1 C2 1.53(2) . . ?
C1 C9 1.55(2) . . ?
C1 C16 1.52(2) . . ?
C1 C23 1.53(2) . . ?
C2 O1 1.45(1) . . ?
O1 C3 1.35(1) . . ?
C3 O2 1.19(2) . . ?
C3 C4 1.48(2) . . ?
C4 C5 1.38(2) . . ?
C4 C8 1.40(2) . . ?
C5 C6 1.39(2) . . ?
C6 C7 1.37(2) . . ?
C7 N1 1.35(2) . . ?
N1 C8 1.33(2) . . ?
C9 O3 1.45(1) . . ?
O3 C10 1.32(1) . . ?
C10 O4 1.19(2) . . ?
C10 C11 1.51(2) . . ?
C11 C12 1.39(2) . . ?
C11 C15 1.38(2) . . ?
C12 C13 1.37(2) . . ?
C13 C14 1.38(2) . . ?
C14 N2 1.33(2) . . ?
N2 C15 1.35(2) . . ?
C16 O5 1.44(2) . . ?
O5 C17 1.35(2) . . ?
C17 O6 1.19(2) . . ?
C17 C18 1.47(2) . . ?
C18 C19 1.40(2) . . ?
C18 C22 1.40(2) . . ?
C19 C20 1.41(2) . . ?
C20 C21 1.36(2) . . ?
C21 N3 1.34(2) . . ?
N3 C22 1.32(2) . . ?
C23 O7 1.45(2) . . ?
O7 C24 1.30(2) . . ?
C24 O8 1.21(2) . . ?
C24 C25 1.46(2) . . ?
C25 C26 1.39(2) . . ?
C25 C29 1.36(2) . . ?
C26 C27 1.37(2) . . ?
C27 C28 1.37(2) . . ?
C28 N4 1.31(2) . . ?
N4 C29 1.37(2) . . ?
C30 CL5 1.764(7) . . ?
C30 CL6 1.861(7) . . ?
C30 C31 1.416(7) . . ?
CL6 O10 1.95(2) . . ?
C31 CL7 1.4056 . . ?
C31 CL8 1.7462 . . ?
CL8 O11 1.53(2) . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL1 HG1 CL2 151.36(15) . . . ?
CL1 HG1 N1 98.5(3) . . . ?
CL2 HG1 N1 101.1(3) . . . ?
CL3 HG2 CL4 153.93(15) . . . ?
CL3 HG2 N2 100.6(3) . . . ?
CL4 HG2 N2 96.4(3) . . . ?
C2 C1 C9 106.5(9) . . . ?
C2 C1 C16 112(1) . . . ?
C2 C1 C23 108(1) . . . ?
C9 C1 C16 111.6(9) . . . ?
C9 C1 C23 109(1) . . . ?
C16 C1 C23 108(1) . . . ?
C1 C2 O1 107.1(9) . . . ?
C2 O1 C3 115.4(9) . . . ?
O1 C3 O2 124(1) . . . ?
O1 C3 C4 111(1) . . . ?
O2 C3 C4 124(1) . . . ?
C3 C4 C5 124(1) . . . ?
C3 C4 C8 116(1) . . . ?
C5 C4 C8 118(1) . . . ?
C4 C5 C6 118(1) . . . ?
C5 C6 C7 118(1) . . . ?
C6 C7 N1 123(1) . . . ?
C7 N1 C8 117(1) . . . ?
C4 C8 N1 123(1) . . . ?
C1 C9 O3 105.6(9) . . . ?
C9 O3 C10 115(1) . . . ?
O3 C10 O4 125(1) . . . ?
O3 C10 C11 110(1) . . . ?
O4 C10 C11 123(1) . . . ?
C10 C11 C12 122(1) . . . ?
C10 C11 C15 118(1) . . . ?
C12 C11 C15 119(1) . . . ?
C11 C12 C13 118(1) . . . ?
C12 C13 C14 119(1) . . . ?
C13 C14 N2 122(1) . . . ?
C14 N2 C15 118(1) . . . ?
C11 C15 N2 121(1) . . . ?
C1 C16 O5 105.4(9) . . . ?
C16 O5 C17 118(1) . . . ?
O5 C17 O6 124(1) . . . ?
O5 C17 C18 110(1) . . . ?
O6 C17 C18 124(1) . . . ?
C17 C18 C19 122(1) . . . ?
C17 C18 C22 119(1) . . . ?
C19 C18 C22 118(1) . . . ?
C18 C19 C20 117(1) . . . ?
C19 C20 C21 119(1) . . . ?
C20 C21 N3 122(1) . . . ?
C21 N3 C22 118(1) . . . ?
C18 C22 N3 122(1) . . . ?
C1 C23 O7 107(1) . . . ?
C23 O7 C24 120(1) . . . ?
O7 C24 O8 121(1) . . . ?
O7 C24 C25 116(1) . . . ?
O8 C24 C25 121(1) . . . ?
C24 C25 C26 121(1) . . . ?
C24 C25 C29 119(1) . . . ?
C26 C25 C29 118(1) . . . ?
C25 C26 C27 119(1) . . . ?
C26 C27 C28 117(1) . . . ?
C27 C28 N4 124(1) . . . ?
C28 N4 C29 117(1) . . . ?
C25 C29 N4 122(1) . . . ?
CL5 C30 CL6 111.0(4) . . . ?
CL5 C30 C31 104.0(4) . . . ?
CL6 C30 C31 105.1(4) . . . ?
C30 CL6 O10 80.3(5) . . . ?
C30 C31 CL7 118.6(3) . . . ?
C30 C31 CL8 108.8(3) . . . ?
CL7 C31 CL8 128.63 . . . ?
C31 CL8 O11 79.1(7) . . . ?

data_st1231
_database_code_CSD               202743

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C60 H64 Cl10 Co2 N8 O23'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C60 H64 Cl10 Co2 N8 O23'
_chemical_formula_weight         1737.61
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,+z
-y,1/2+x,1/2+z
1/2+y,-x,1/2+z
-x,-y,-z
1/2+x,1/2+y,-z
+y,1/2-x,1/2-z
1/2-y,+x,1/2-z
_cell_length_a                   13.0678(9)
_cell_length_b                   13.0678(9)
_cell_length_c                   25.914(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4425.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173
_cell_measurement_reflns_used    9331
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      27.5
_cell_special_details            
;
Cell parameters refined using Scalepack part of DENZO
Z. Otwinowski, W. Minor, 1997
;

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.30
_exptl_crystal_density_method    none

_exptl_crystal_F_000             1776
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_T_max  0.862

#===============================================================================

# 7. EXPERIMENTAL DATA

_diffrn_special_details          
; ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a

_diffrn_source                   xray_tube

_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'

_diffrn_measurement_details      
;
9331 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  0.3 deg 1 scans of   90 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  327 frames
Set 2 Theta =   -6.00 Kappa = -174.00 Phi   =    0.00  141 frames
Friedel pairs were averaged. Internal R = 0.08
;

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0

_diffrn_reflns_number            9331
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.5
_diffrn_reflns_theta_max         27.45

_reflns_number_total             5179
_reflns_number_gt                2101
_reflns_threshold_expression     >3.0\s(I)

_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_molecular_graphics    ?
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)

#===============================================================================

# 8. REFINEMENT DATA

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_expression ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         2101
_refine_ls_number_parameters     222
_refine_ls_number_restraints     10
_refine_ls_number_constraints    9
_refine_ls_R_factor_all          0.186
_refine_ls_R_factor_gt           0.143
_refine_ls_wR_factor_all         0.323
_refine_ls_wR_factor_ref         0.173
_refine_ls_goodness_of_fit_all   1.726
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_shift/su_max          0.007
_refine_ls_shift/esd_mean        0.001
_refine_diff_density_max         1.907
_refine_diff_density_min         -0.610

#===============================================================================

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
CO 0.2500 0.2500 0.6187(1) 0.027(1) 0.500 Uani ? ? Co
CL 0.3278(3) 0.0824(3) 0.6190(2) 0.040(2) 1.000 Uani ? ? Cl
N1 0.143(1) 0.200(1) 0.5590(4) 0.030(7) 1.000 Uani ? ? N
C1 0.171(1) 0.141(2) 0.5198(6) 0.04(1) 1.000 Uani ? ? C
C2 0.107(1) 0.115(1) 0.4779(6) 0.037(9) 1.000 Uani ? ? C
C3 0.006(1) 0.153(1) 0.4801(5) 0.028(8) 1.000 Uani ? ? C
C4 -0.025(1) 0.210(1) 0.5211(6) 0.040(9) 1.000 Uani ? ? C
C5 0.048(1) 0.232(1) 0.5595(6) 0.042(9) 1.000 Uani ? ? C
C6 -0.063(1) 0.131(1) 0.4349(5) 0.027(8) 1.000 Uani ? ? C
O1 -0.037(1) 0.080(1) 0.3989(5) 0.056(8) 1.000 Uani ? ? O
O2 -0.1541(8) 0.1745(8) 0.4421(4) 0.030(5) 1.000 Uani ? ? O
C7 -0.232(1) 0.154(1) 0.4028(6) 0.028(8) 1.000 Uani ? ? C
C8 -0.2500 0.2500 0.3694(8) 0.03(1) 0.500 Uani ? ? C
C9 -0.344(1) 0.232(1) 0.3362(5) 0.032(8) 1.000 Uani ? ? C
O3 -0.3171(9) 0.1491(9) 0.3023(4) 0.037(6) 1.000 Uani ? ? O
C10 -0.390(1) 0.115(2) 0.2691(7) 0.05(1) 1.000 Uani ? ? C
C11 -0.359(1) 0.031(1) 0.2365(5) 0.026(8) 1.000 Uani ? ? C
C12 0.490(1) 0.262(1) 0.7405(5) 0.027(8) 1.000 Uani ? ? C
C13 0.409(1) 0.235(1) 0.7090(5) 0.032(8) 1.000 Uani ? ? C
N2 0.367(1) 0.298(1) 0.6744(4) 0.029(7) 1.000 Uani ? ? N
C14 0.409(1) 0.392(1) 0.6704(5) 0.028(8) 1.000 Uani ? ? C
C15 0.490(1) 0.424(1) 0.7000(6) 0.035(9) 1.000 Uani ? ? C
O4 -0.474(1) 0.155(1) 0.2677(6) 0.11(1) 1.000 Uani ? ? O
O5 0.176(2) 0.173(2) 0.323(1) 0.13(2) 1.000 Uani ? ? O
C18 0.011(1) 0.074(1) 0.0769(6) 0.21(4) 0.500 Uiso ? ? C
CL1 -0.0880(1) 0.1827(1) 0.0948(6) 0.23(1) 0.500 Uiso ? ? Cl
CL2 -0.0031(1) 0.0662(1) 0.0032(6) 0.28(2) 0.500 Uiso ? ? Cl
CL3 0.1306(1) 0.1006(1) 0.0935(6) 0.121(6) 0.500 Uiso ? ? Cl
O6 -0.2500 0.2500 0.165(2) 0.06(1) 0.250 Uiso ? ? O
O7 -0.055(3) 0.115(3) 0.156(2) 0.12(1) 0.500 Uiso ? ? O
H1 0.2389 0.1147 0.5200 0.0588 1.000 Uiso calc C1 H
H2 0.1303 0.0750 0.4499 0.0510 1.000 Uiso calc C2 H
H3 -0.0935 0.2343 0.5238 0.0528 1.000 Uiso calc C4 H
H4 0.0272 0.2735 0.5878 0.0579 1.000 Uiso calc C5 H
H5 -0.2944 0.1358 0.4193 0.0394 1.000 Uiso calc C7 H
H6 -0.2100 0.0996 0.3814 0.0394 1.000 Uiso calc C7 H
H7 -0.3593 0.2919 0.3168 0.0453 1.000 Uiso calc C9 H
H8 -0.4007 0.2142 0.3570 0.0453 1.000 Uiso calc C9 H
H9 0.5180 0.2140 0.7644 0.0402 1.000 Uiso calc C12 H
H10 0.3808 0.1677 0.7122 0.0435 1.000 Uiso calc C13 H
H11 0.3819 0.4389 0.6459 0.0384 1.000 Uiso calc C14 H
H12 0.5171 0.4905 0.6956 0.0460 1.000 Uiso calc C15 H

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
CO 0.032(1) 0.032(1) 0.020(1) -0.000(2) 0.0000 0.0000 Co
CL 0.045(2) 0.033(2) 0.042(2) -0.002(2) 0.003(2) -0.001(2) Cl
N1 0.027(7) 0.046(8) 0.022(6) 0.009(6) -0.005(6) 0.001(6) N
C1 0.04(1) 0.07(1) 0.031(7) -0.001(9) -0.008(8) -0.025(8) C
C2 0.05(1) 0.05(1) 0.022(7) -0.000(9) 0.002(8) -0.014(7) C
C3 0.037(9) 0.033(9) 0.018(6) -0.007(7) 0.000(7) 0.005(7) C
C4 0.05(1) 0.04(1) 0.032(8) 0.004(9) -0.000(8) -0.010(8) C
C5 0.05(1) 0.06(1) 0.026(7) 0.006(9) -0.007(8) -0.022(8) C
C6 0.023(8) 0.047(9) 0.018(6) -0.022(7) 0.005(6) -0.009(7) C
O1 0.057(8) 0.070(9) 0.044(6) 0.010(7) -0.007(6) -0.029(6) O
O2 0.039(6) 0.040(6) 0.018(4) -0.002(5) -0.004(5) -0.005(5) O
C7 0.032(9) 0.016(7) 0.043(8) -0.008(7) 0.004(7) -0.015(6) C
C8 0.04(1) 0.03(1) 0.023(9) -0.02(1) 0.0000 0.0000 C
C9 0.042(9) 0.05(1) 0.017(6) -0.002(8) -0.013(7) -0.017(7) C
O3 0.051(7) 0.039(6) 0.025(5) 0.007(6) -0.002(5) -0.009(5) O
C10 0.04(1) 0.08(1) 0.046(9) 0.00(1) -0.023(8) -0.029(9) C
C11 0.025(8) 0.028(8) 0.026(7) 0.008(6) -0.006(6) -0.003(6) C
C12 0.05(1) 0.019(7) 0.020(7) 0.001(7) -0.011(7) 0.012(6) C
C13 0.05(1) 0.031(9) 0.022(6) -0.002(8) -0.004(7) 0.010(7) C
N2 0.040(8) 0.027(7) 0.024(6) 0.016(6) -0.005(6) -0.008(6) N
C14 0.042(9) 0.025(8) 0.021(7) -0.006(7) -0.004(7) 0.005(7) C
C15 0.04(1) 0.027(8) 0.036(8) -0.015(7) -0.010(8) -0.003(7) C
O4 0.060(9) 0.16(1) 0.13(1) 0.051(9) -0.055(8) -0.111(8) O
O5 0.09(1) 0.09(1) 0.29(3) -0.04(1) -0.00(2) -0.05(2) O

# 10. MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
CO CL 2.415(4) . . ?
CO N1 2.19(1) . . ?
CO N2 2.19(1) . . ?
N1 C1 1.33(2) . . ?
N1 C5 1.30(2) . . ?
C1 C2 1.41(2) . . ?
C2 C3 1.41(2) . . ?
C3 C4 1.36(2) . . ?
C3 C6 1.50(2) . . ?
C4 C5 1.41(2) . . ?
C6 O1 1.20(2) . . ?
C6 O2 1.33(2) . . ?
O2 C7 1.47(2) . . ?
C7 C8 1.54(2) . . ?
C7 C8 1.54(2) . 2_455 ?
C8 C9 1.51(2) . . ?
C8 C9 1.51(2) . 2_455 ?
C9 O3 1.44(2) . . ?
O3 C10 1.36(2) . . ?
C10 C11 1.44(2) . . ?
C10 O4 1.21(2) . . ?
C11 C12 1.38(2) . 3_544 ?
C11 C15 1.38(2) . 3_544 ?
C12 C13 1.39(2) . . ?
C13 N2 1.34(2) . . ?
N2 C14 1.36(2) . . ?
C14 C15 1.36(2) . . ?
C18 CL1 1.98(2) . . ?
C18 CL2 1.92(1) . . ?
C18 CL3 1.66(2) . . ?
CL1 O7 1.86(4) . . ?
CL2 CL2 1.7409 . 5_555 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL CO N1 90.3(4) . . . ?
CL CO N2 87.9(4) . . . ?
N1 CO N2 175.7(5) . . . ?
C1 N1 C5 117(1) . . . ?
N1 C1 C2 123(1) . . . ?
C1 C2 C3 116(1) . . . ?
C2 C3 C4 119(1) . . . ?
C2 C3 C6 117(1) . . . ?
C4 C3 C6 122(1) . . . ?
C3 C4 C5 117(1) . . . ?
N1 C5 C4 124(1) . . . ?
C3 C6 O1 122(1) . . . ?
C3 C6 O2 109(1) . . . ?
O1 C6 O2 127(1) . . . ?
C6 O2 C7 116(1) . . . ?
O2 C7 C8 110(1) . . . ?
C7 C8 C7 111(1) . . 2_455 ?
C7 C8 C9 108.5(9) . . . ?
C7 C8 C9 108.8(9) . . 2_455 ?
C7 C8 C9 108.8(9) 2_455 . . ?
C7 C8 C9 108.5(9) 2_455 . 2_455 ?
C9 C8 C9 110(1) . . 2_455 ?
C8 C9 O3 105(1) . . . ?
C9 O3 C10 117(1) . . . ?
O3 C10 C11 114(1) . . . ?
O3 C10 O4 120(1) . . . ?
C11 C10 O4 124(1) . . . ?
C10 C11 C12 120(1) . . 3_544 ?
C10 C11 C15 121(1) . . 3_544 ?
C12 C11 C15 117(1) 3_544 . 3_544 ?
C11 C12 C13 119(1) 4_555 . . ?
C12 C13 N2 123(1) . . . ?
C13 N2 C14 116(1) . . . ?
N2 C14 C15 123(1) . . . ?
C11 C15 C14 120(1) 4_555 . . ?
CL1 C18 CL2 102.1(7) . . . ?
CL1 C18 CL3 114.0(8) . . . ?
CL2 C18 CL3 111.2(8) . . . ?
C18 CL1 O7 72(1) . . . ?
C18 CL2 CL2 98.3(4) . . 5_555 ?