# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1(ZnCl3)2
_chemical_name_systematic        ?
_chemical_name_common            Zn
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H52 Cl6 N4 O8 Zn2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1204.46

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.5117(3)
_cell_length_b                   15.9674(5)
_cell_length_c                   20.4293(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.588(2)
_cell_angle_gamma                90
_cell_volume                     2752.23(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.3818
_cell_measurement_theta_max      24.6493
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       trapezoidal
_exptl_crystal_colour            'lustrous intense blue-green'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.170
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1308

_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.82

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            90784
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28

_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.
;

_reflns_number_total             8046
_reflns_number_gt                5921
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1617
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_number_reflns         8046
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.3993P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.061
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.3850(4) 0.3739(2) 1.01644(15) 0.0400(7) Uani d . 1 . .
H H1 0.4689 0.3861 1.0506 0.048 Uiso calc R 1 . .
C C2 0.3595(3) 0.42525(19) 0.96211(14) 0.0352(6) Uani d . 1 . .
H H2 0.4217 0.4743 0.9599 0.042 Uiso calc R 1 . .
C C3 0.2405(3) 0.40494(17) 0.90950(14) 0.0310(6) Uani d . 1 . .
C C4 0.1477(3) 0.33139(17) 0.91276(13) 0.0325(6) Uani d . 1 . .
C C5 0.1708(3) 0.28351(18) 0.97232(14) 0.0340(6) Uani d . 1 . .
C C6 0.2893(4) 0.3041(2) 1.02212(15) 0.0409(7) Uani d . 1 . .
H H6 0.3061 0.2705 1.0608 0.049 Uiso calc R 1 . .
C C7 0.0373(4) 0.30732(19) 0.85792(14) 0.0366(6) Uani d . 1 . .
H H7 -0.0229 0.2574 0.8593 0.044 Uiso calc R 1 . .
C C8 0.0186(4) 0.3575(2) 0.80247(14) 0.0375(6) Uani d . 1 . .
H H8 -0.0539 0.341 0.7653 0.045 Uiso calc R 1 . .
C C9 0.1034(4) 0.43196(19) 0.79947(14) 0.0363(6) Uani d . 1 . .
H H9 0.0865 0.4659 0.761 0.044 Uiso calc R 1 . .
C C10 0.2120(3) 0.45647(18) 0.85239(14) 0.0323(6) Uani d . 1 . .
C C11 0.7587(3) 0.42855(16) 0.88939(13) 0.0280(5) Uani d . 1 . .
H H11 0.7137 0.4373 0.8448 0.034 Uiso calc R 1 . .
C C12 0.8664(3) 0.48483(15) 0.91983(12) 0.0241(5) Uani d . 1 . .
H H12 0.8922 0.5336 0.8968 0.029 Uiso calc R 1 . .
C C13 0.9380(3) 0.47090(14) 0.98422(11) 0.0194(4) Uani d . 1 . .
C C14 0.8888(3) 0.40124(14) 1.01758(12) 0.0231(5) Uani d . 1 . .
H H14 0.9318 0.3914 1.0622 0.028 Uiso calc R 1 . .
C C15 0.7787(3) 0.34702(15) 0.98613(12) 0.0254(5) Uani d . 1 . .
H H15 0.7463 0.2997 1.0092 0.03 Uiso calc R 1 . .
C C23 0.2698(4) 0.5843(2) 0.80012(15) 0.0373(6) Uani d . 1 . .
H H23A 0.1552 0.5972 0.7916 0.045 Uiso calc R 1 . .
H H23B 0.3015 0.5583 0.7599 0.045 Uiso calc R 1 . .
C C24 0.3619(4) 0.6631(2) 0.81583(16) 0.0425(7) Uani d . 1 . .
H H24A 0.4741 0.6491 0.8311 0.051 Uiso calc R 1 . .
H H24B 0.3582 0.6978 0.7755 0.051 Uiso calc R 1 . .
C C25 0.3350(4) 0.7959(2) 0.86742(19) 0.0490(8) Uani d . 1 . .
H H25A 0.3595 0.8134 0.8234 0.059 Uiso calc R 1 . .
H H25B 0.4304 0.8058 0.8998 0.059 Uiso calc R 1 . .
C C26 0.2027(4) 0.8469(2) 0.88550(16) 0.0446(8) Uani d . 1 . .
H H26A 0.2189 0.9063 0.874 0.054 Uiso calc R 1 . .
H H26B 0.102 0.8278 0.8601 0.054 Uiso calc R 1 . .
C C27 0.0839(5) 0.1646(2) 1.02973(18) 0.0506(9) Uani d . 1 . .
H H27A 0.101 0.1959 1.0719 0.061 Uiso calc R 1 . .
H H27B 0.1773 0.1285 1.0269 0.061 Uiso calc R 1 . .
C C28 -0.0604(5) 0.1134(2) 1.02650(19) 0.0522(9) Uani d . 1 . .
H H28A -0.0888 0.0926 0.9808 0.063 Uiso calc R 1 . .
H H28B -0.039 0.0642 1.0558 0.063 Uiso calc R 1 . .
Cl Cl1 0.14610(8) 0.16512(4) 0.68249(3) 0.03174(16) Uani d . 1 . .
Cl Cl2 0.38701(9) -0.01242(4) 0.77079(3) 0.03638(17) Uani d . 1 . .
Cl Cl3 0.04779(11) 0.07443(5) 0.84572(4) 0.0470(2) Uani d . 1 . .
N N2 0.7159(2) 0.36022(12) 0.92272(10) 0.0234(4) Uani d . 1 . .
O O1 0.0624(3) 0.22200(13) 0.97488(10) 0.0407(5) Uani d . 1 . .
O O2 0.2999(2) 0.52718(13) 0.85475(10) 0.0361(5) Uani d . 1 . .
O O3 0.2975(3) 0.70918(13) 0.86607(11) 0.0430(5) Uani d . 1 . .
O O4 -0.1931(3) 0.15982(13) 1.04594(11) 0.0413(5) Uani d . 1 . .
Zn Zn1 0.23128(4) 0.100943(19) 0.778549(15) 0.03194(12) Uani d . 1 . .
N N1 0.3938(3) 0.18705(14) 0.82442(11) 0.0377(6) Uani d . 1 . .
C C16 0.3995(3) 0.26447(16) 0.80377(13) 0.0266(5) Uani d . 1 . .
H H16 0.3289 0.2808 0.766 0.032 Uiso calc R 1 . .
C C17 0.5035(3) 0.32391(16) 0.83438(13) 0.0271(5) Uani d . 1 . .
H H17 0.5034 0.3797 0.8181 0.033 Uiso calc R 1 . .
C C18 0.6060(3) 0.30020(16) 0.88843(13) 0.0290(5) Uani d . 1 . .
C C19 0.6082(7) 0.2191(2) 0.9086(2) 0.106(2) Uani d . 1 . .
H H19 0.6821 0.2003 0.9445 0.128 Uiso calc R 1 . .
C C20 0.4983(8) 0.1643(3) 0.8749(3) 0.118(3) Uani d . 1 . .
H H20 0.4986 0.1076 0.889 0.142 Uiso calc R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.374(4) ?
C1 C6 . 1.394(5) ?
C2 C3 . 1.414(4) ?
C3 C4 . 1.422(4) ?
C3 C10 . 1.422(4) ?
C4 C7 . 1.417(4) ?
C4 C5 . 1.428(4) ?
C5 O1 . 1.354(4) ?
C5 C6 . 1.374(4) ?
C7 C8 . 1.380(4) ?
C8 C9 . 1.396(5) ?
C9 C10 . 1.383(4) ?
C10 O2 . 1.352(4) ?
C11 N2 . 1.361(3) ?
C11 C12 . 1.373(3) ?
C12 C13 . 1.393(3) ?
C13 C14 . 1.397(3) ?
C13 C13 3_767 1.487(4) ?
C14 C15 . 1.372(3) ?
C15 N2 . 1.351(3) ?
C23 O2 . 1.438(3) ?
C23 C24 . 1.494(5) ?
C24 O3 . 1.430(4) ?
C25 O3 . 1.421(4) ?
C25 C26 . 1.476(5) ?
C26 O4 3_567 1.418(4) ?
C27 O1 . 1.440(4) ?
C27 C28 . 1.470(5) ?
C28 O4 . 1.449(4) ?
Cl1 Zn1 . 2.2475(7) ?
Cl2 Zn1 . 2.2615(8) ?
Cl3 Zn1 . 2.2512(9) ?
N2 C18 . 1.453(3) ?
O4 C26 3_567 1.418(4) ?
Zn1 N1 . 2.083(2) ?
N1 C16 . 1.309(3) ?
N1 C20 . 1.320(4) ?
C16 C17 . 1.389(3) ?
C17 C18 . 1.367(4) ?
C18 C19 . 1.359(4) ?
C19 C20 . 1.395(5) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 120.8(3) ?
C1 C2 C3 . . 119.9(3) ?
C2 C3 C4 . . 120.0(3) ?
C2 C3 C10 . . 121.2(3) ?
C4 C3 C10 . . 118.7(3) ?
C7 C4 C3 . . 120.1(3) ?
C7 C4 C5 . . 122.1(3) ?
C3 C4 C5 . . 117.8(3) ?
O1 C5 C6 . . 125.6(3) ?
O1 C5 C4 . . 113.8(3) ?
C6 C5 C4 . . 120.5(3) ?
C5 C6 C1 . . 120.6(3) ?
C8 C7 C4 . . 119.0(3) ?
C7 C8 C9 . . 121.8(3) ?
C10 C9 C8 . . 120.2(3) ?
O2 C10 C9 . . 125.0(3) ?
O2 C10 C3 . . 114.9(3) ?
C9 C10 C3 . . 120.1(3) ?
N2 C11 C12 . . 120.3(2) ?
C11 C12 C13 . . 120.4(2) ?
C12 C13 C14 . . 117.7(2) ?
C12 C13 C13 . 3_767 120.5(3) ?
C14 C13 C13 . 3_767 121.8(3) ?
C15 C14 C13 . . 120.3(2) ?
N2 C15 C14 . . 120.7(2) ?
O2 C23 C24 . . 109.4(3) ?
O3 C24 C23 . . 110.3(3) ?
O3 C25 C26 . . 111.5(3) ?
O4 C26 C25 3_567 . 110.5(3) ?
O1 C27 C28 . . 107.4(3) ?
O4 C28 C27 . . 112.3(3) ?
C15 N2 C11 . . 120.4(2) ?
C15 N2 C18 . . 120.5(2) ?
C11 N2 C18 . . 119.0(2) ?
C5 O1 C27 . . 118.3(3) ?
C10 O2 C23 . . 117.5(2) ?
C25 O3 C24 . . 114.2(2) ?
C26 O4 C28 3_567 . 112.4(3) ?
N1 Zn1 Cl1 . . 102.14(7) ?
N1 Zn1 Cl3 . . 108.83(8) ?
Cl1 Zn1 Cl3 . . 116.63(3) ?
N1 Zn1 Cl2 . . 101.50(8) ?
Cl1 Zn1 Cl2 . . 115.36(3) ?
Cl3 Zn1 Cl2 . . 110.64(3) ?
C16 N1 C20 . . 117.5(3) ?
C16 N1 Zn1 . . 121.93(19) ?
C20 N1 Zn1 . . 120.6(2) ?
N1 C16 C17 . . 123.3(2) ?
C18 C17 C16 . . 118.4(2) ?
C19 C18 C17 . . 119.4(3) ?
C19 C18 N2 . . 120.0(3) ?
C17 C18 N2 . . 120.5(2) ?
C18 C19 C20 . . 117.8(3) ?
N1 C20 C19 . . 123.5(3) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -3.5(4) ?
C1 C2 C3 C4 . . . . -0.2(4) ?
C1 C2 C3 C10 . . . . -179.5(3) ?
C2 C3 C4 C7 . . . . -174.9(3) ?
C10 C3 C4 C7 . . . . 4.5(4) ?
C2 C3 C4 C5 . . . . 4.7(4) ?
C10 C3 C4 C5 . . . . -175.9(2) ?
C7 C4 C5 O1 . . . . -9.6(4) ?
C3 C4 C5 O1 . . . . 170.8(2) ?
C7 C4 C5 C6 . . . . 173.8(3) ?
C3 C4 C5 C6 . . . . -5.8(4) ?
O1 C5 C6 C1 . . . . -173.8(3) ?
C4 C5 C6 C1 . . . . 2.4(4) ?
C2 C1 C6 C5 . . . . 2.4(5) ?
C3 C4 C7 C8 . . . . -1.8(4) ?
C5 C4 C7 C8 . . . . 178.6(3) ?
C4 C7 C8 C9 . . . . -1.1(4) ?
C7 C8 C9 C10 . . . . 1.3(5) ?
C8 C9 C10 O2 . . . . -179.8(3) ?
C8 C9 C10 C3 . . . . 1.5(4) ?
C2 C3 C10 O2 . . . . -3.8(4) ?
C4 C3 C10 O2 . . . . 176.9(2) ?
C2 C3 C10 C9 . . . . 175.0(3) ?
C4 C3 C10 C9 . . . . -4.4(4) ?
N2 C11 C12 C13 . . . . 2.7(4) ?
C11 C12 C13 C14 . . . . -4.1(4) ?
C11 C12 C13 C13 . . . 3_767 176.2(3) ?
C12 C13 C14 C15 . . . . 2.9(4) ?
C13 C13 C14 C15 3_767 . . . -177.5(3) ?
C13 C14 C15 N2 . . . . -0.2(4) ?
O2 C23 C24 O3 . . . . -70.2(3) ?
O3 C25 C26 O4 . . . 3_567 75.0(4) ?
O1 C27 C28 O4 . . . . -73.6(4) ?
C14 C15 N2 C11 . . . . -1.3(4) ?
C14 C15 N2 C18 . . . . 176.5(2) ?
C12 C11 N2 C15 . . . . 0.1(4) ?
C12 C11 N2 C18 . . . . -177.8(2) ?
C6 C5 O1 C27 . . . . -9.7(4) ?
C4 C5 O1 C27 . . . . 173.9(2) ?
C28 C27 O1 C5 . . . . 171.2(3) ?
C9 C10 O2 C23 . . . . 4.8(4) ?
C3 C10 O2 C23 . . . . -176.4(2) ?
C24 C23 O2 C10 . . . . 172.4(2) ?
C26 C25 O3 C24 . . . . 144.5(3) ?
C23 C24 O3 C25 . . . . -157.9(3) ?
C27 C28 O4 C26 . . . 3_567 -90.7(3) ?
Cl1 Zn1 N1 C16 . . . . 14.9(2) ?
Cl3 Zn1 N1 C16 . . . . -109.0(2) ?
Cl2 Zn1 N1 C16 . . . . 134.3(2) ?
Cl1 Zn1 N1 C20 . . . . -163.3(5) ?
Cl3 Zn1 N1 C20 . . . . 72.7(5) ?
Cl2 Zn1 N1 C20 . . . . -44.0(5) ?
C20 N1 C16 C17 . . . . -3.5(6) ?
Zn1 N1 C16 C17 . . . . 178.2(2) ?
N1 C16 C17 C18 . . . . 0.6(4) ?
C16 C17 C18 C19 . . . . 3.0(5) ?
C16 C17 C18 N2 . . . . -179.2(2) ?
C15 N2 C18 C19 . . . . -24.0(5) ?
C11 N2 C18 C19 . . . . 153.9(4) ?
C15 N2 C18 C17 . . . . 158.2(3) ?
C11 N2 C18 C17 . . . . -23.9(4) ?
C17 C18 C19 C20 . . . . -3.4(8) ?
N2 C18 C19 C20 . . . . 178.8(5) ?
C16 N1 C20 C19 . . . . 3.0(10) ?
Zn1 N1 C20 C19 . . . . -178.7(6) ?
C18 C19 C20 N1 . . . . 0.5(11) ?
_database_code_depnum_ccdc_archive 'CCDC 997295'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2(ZnCl3)2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H60 Cl6 N4 O10 Zn2'
_chemical_formula_weight         1292.52

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   17.5218(8)
_cell_length_b                   16.1106(7)
_cell_length_c                   20.7074(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.232(3)
_cell_angle_gamma                90.00
_cell_volume                     5752.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3240
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      19.99

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            82404
_diffrn_reflns_av_R_equivalents  0.1836
_diffrn_reflns_av_sigmaI/netI    0.2442
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         30.03
_reflns_number_total             16811
_reflns_number_gt                6195
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0568P)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         16811
_refine_ls_number_parameters     721
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2352
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1682
_refine_ls_wR_factor_gt          0.1210
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_restrained_S_all      0.938
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.10457(4) 0.37674(4) 0.27139(3) 0.02702(17) Uani 1 1 d . . .
Zn2 Zn 0.14475(4) 0.07760(4) 0.77708(3) 0.03134(18) Uani 1 1 d . . .
Cl1 Cl 0.18321(8) 0.48799(8) 0.27175(6) 0.0337(3) Uani 1 1 d . . .
Cl2 Cl 0.06146(8) 0.32233(8) 0.17138(6) 0.0328(3) Uani 1 1 d . . .
Cl3 Cl 0.01652(8) 0.39188(9) 0.33694(6) 0.0361(4) Uani 1 1 d . . .
Cl4 Cl 0.05604(8) 0.05452(10) 0.83925(6) 0.0453(4) Uani 1 1 d . . .
Cl5 Cl 0.09639(8) 0.14869(9) 0.68566(6) 0.0356(4) Uani 1 1 d . . .
Cl6 Cl 0.21561(8) -0.03685(9) 0.76647(6) 0.0372(4) Uani 1 1 d . . .
O1 O 0.8450(2) 1.0649(2) 0.65067(16) 0.0351(9) Uani 1 1 d . . .
O2 O 0.8143(2) 1.2307(2) 0.63714(18) 0.0416(10) Uani 1 1 d . . .
O3 O 0.8384(3) 1.3453(3) 0.5425(2) 0.0593(13) Uani 1 1 d . . .
O4A O 1.0101(7) 0.6148(7) 0.4814(5) 0.038(3) Uani 0.50 1 d P A 1
O4B O 1.0092(8) 0.6460(7) 0.4545(6) 0.048(3) Uani 0.50 1 d P A 2
O5 O 0.9152(2) 0.7573(2) 0.51601(17) 0.0359(10) Uani 1 1 d . . .
O6 O 0.8740(2) 0.5084(2) 0.14840(15) 0.0317(9) Uani 1 1 d . . .
O7 O 0.8365(2) 0.3285(2) 0.13491(16) 0.0345(9) Uani 1 1 d . . .
O8 O 0.8247(3) 0.1823(3) 0.05907(19) 0.0613(14) Uani 1 1 d . . .
C51 C 0.8446(4) 0.0424(4) 0.0235(2) 0.0411(16) Uani 1 1 d . . .
H51A H 0.8968 0.0434 0.0489 0.049 Uiso 1 1 calc R . .
H51B H 0.8250 -0.0139 0.0236 0.049 Uiso 1 1 calc R . .
C49 C 0.9805(3) 0.1162(4) -0.0324(3) 0.0406(15) Uani 1 1 d . . .
H49A H 0.9778 0.1259 0.0133 0.049 Uiso 1 1 calc R . .
H49B H 1.0316 0.0948 -0.0351 0.049 Uiso 1 1 calc R . .
N1 N 0.1825(2) 0.2893(3) 0.31627(19) 0.0242(10) Uani 1 1 d . . .
N2 N 0.3499(2) 0.1260(2) 0.41793(18) 0.0218(10) Uani 1 1 d . . .
N3 N 0.3704(2) 0.3468(2) 0.92761(18) 0.0211(9) Uani 1 1 d . . .
N4 N 0.2228(3) 0.1630(3) 0.82911(19) 0.0293(11) Uani 1 1 d . . .
C1 C 0.1882(3) 0.2114(3) 0.2954(2) 0.0255(12) Uani 1 1 d . . .
H1 H 0.1543 0.1945 0.2579 0.031 Uiso 1 1 calc R . .
C2 C 0.2418(3) 0.1546(3) 0.3265(2) 0.0207(11) Uani 1 1 d . . .
H2 H 0.2443 0.1009 0.3105 0.025 Uiso 1 1 calc R . .
C3 C 0.2919(3) 0.1813(3) 0.3827(2) 0.0207(11) Uani 1 1 d . . .
C4 C 0.2867(3) 0.2611(3) 0.4047(2) 0.0307(13) Uani 1 1 d . . .
H4 H 0.3198 0.2797 0.4420 0.037 Uiso 1 1 calc R . .
C5 C 0.2318(3) 0.3131(3) 0.3705(2) 0.0293(13) Uani 1 1 d . . .
H5 H 0.2286 0.3671 0.3855 0.035 Uiso 1 1 calc R . .
C6 C 0.3787(3) 0.0636(3) 0.3860(2) 0.0229(12) Uani 1 1 d . . .
H6 H 0.3592 0.0549 0.3417 0.028 Uiso 1 1 calc R . .
C7 C 0.4359(3) 0.0130(3) 0.4175(2) 0.0224(12) Uani 1 1 d . . .
H7 H 0.4537 -0.0308 0.3950 0.027 Uiso 1 1 calc R . .
C8 C 0.4677(3) 0.0263(3) 0.4829(2) 0.0194(11) Uani 1 1 d . . .
C9 C 0.4351(3) 0.0889(3) 0.5155(2) 0.0233(12) Uani 1 1 d . . .
H9 H 0.4531 0.0979 0.5599 0.028 Uiso 1 1 calc R . .
C10 C 0.3769(3) 0.1374(3) 0.4828(2) 0.0241(12) Uani 1 1 d . . .
H10 H 0.3554 0.1787 0.5054 0.029 Uiso 1 1 calc R . .
C11 C 0.4106(3) 0.3340(3) 0.9896(2) 0.0247(12) Uani 1 1 d . . .
H11 H 0.4043 0.2851 1.0121 0.030 Uiso 1 1 calc R . .
C12 C 0.4601(3) 0.3945(3) 1.0180(2) 0.0253(12) Uani 1 1 d . . .
H12 H 0.4868 0.3865 1.0605 0.030 Uiso 1 1 calc R . .
C13 C 0.4722(3) 0.4677(3) 0.9855(2) 0.0206(11) Uani 1 1 d . . .
C14 C 0.4274(3) 0.4784(3) 0.9231(2) 0.0236(12) Uani 1 1 d . . .
H14 H 0.4311 0.5276 0.9003 0.028 Uiso 1 1 calc R . .
C15 C 0.3784(3) 0.4171(3) 0.8952(2) 0.0257(12) Uani 1 1 d . . .
H15 H 0.3502 0.4245 0.8531 0.031 Uiso 1 1 calc R . .
C16 C 0.2917(3) 0.1424(3) 0.8639(2) 0.0328(14) Uani 1 1 d . . .
H16 H 0.3064 0.0869 0.8655 0.039 Uiso 1 1 calc R . .
C17 C 0.3429(3) 0.2006(3) 0.8983(2) 0.0312(13) Uani 1 1 d . . .
H17 H 0.3905 0.1846 0.9226 0.037 Uiso 1 1 calc R . .
C18 C 0.3199(3) 0.2826(3) 0.8947(2) 0.0257(12) Uani 1 1 d . . .
C19 C 0.2491(3) 0.3042(3) 0.8590(2) 0.0257(12) Uani 1 1 d . . .
H19 H 0.2328 0.3592 0.8567 0.031 Uiso 1 1 calc R . .
C20 C 0.2026(3) 0.2427(4) 0.8265(2) 0.0313(14) Uani 1 1 d . . .
H20 H 0.1551 0.2576 0.8017 0.038 Uiso 1 1 calc R . .
C21 C 0.8852(3) 0.9932(3) 0.6476(3) 0.0315(13) Uani 1 1 d . . .
C22 C 0.9434(3) 0.9643(4) 0.6959(2) 0.0320(14) Uani 1 1 d . . .
H22 H 0.9598 0.9955 0.7336 0.038 Uiso 1 1 calc R . .
C23 C 0.9775(3) 0.8875(3) 0.6876(3) 0.0321(13) Uani 1 1 d . . .
H23 H 1.0159 0.8675 0.7208 0.039 Uiso 1 1 calc R . .
C24 C 0.9562(3) 0.8406(4) 0.6318(3) 0.0330(14) Uani 1 1 d . . .
H24 H 0.9790 0.7893 0.6277 0.040 Uiso 1 1 calc R . .
C25 C 0.8981(3) 0.8721(3) 0.5802(2) 0.0277(13) Uani 1 1 d . . .
C26 C 0.8616(3) 0.9491(3) 0.5877(2) 0.0272(13) Uani 1 1 d . . .
C27 C 0.8023(3) 0.9796(3) 0.5381(2) 0.0287(13) Uani 1 1 d . . .
H27 H 0.7776 1.0296 0.5435 0.034 Uiso 1 1 calc R . .
C28 C 0.7819(3) 0.9342(4) 0.4823(3) 0.0328(14) Uani 1 1 d . . .
H28 H 0.7423 0.9535 0.4499 0.039 Uiso 1 1 calc R . .
C29 C 0.8184(3) 0.8599(4) 0.4720(2) 0.0345(14) Uani 1 1 d . . .
H29 H 0.8045 0.8317 0.4325 0.041 Uiso 1 1 calc R . .
C30 C 0.8754(3) 0.8277(3) 0.5203(2) 0.0281(13) Uani 1 1 d . . .
C31 C 0.8915(3) 0.7072(4) 0.4578(3) 0.0474(17) Uani 1 1 d . A .
H31A H 0.9075 0.7331 0.4201 0.057 Uiso 1 1 calc R . .
H31B H 0.8356 0.7007 0.4488 0.057 Uiso 1 1 calc R . .
C32 C 0.9302(4) 0.6248(4) 0.4715(4) 0.058(2) Uani 1 1 d . . .
H32A H 0.9132 0.6028 0.5102 0.070 Uiso 1 1 calc R A 1
H32B H 0.9087 0.5887 0.4354 0.070 Uiso 1 1 calc R A 1
C33A C 1.0285(8) 0.6031(10) 0.4167(5) 0.037(3) Uani 0.50 1 d P . 1
H33A H 1.0143 0.6520 0.3900 0.044 Uiso 0.50 1 calc PR . 1
H33B H 1.0003 0.5559 0.3953 0.044 Uiso 0.50 1 calc PR . 1
C33B C 1.0547(8) 0.5706(7) 0.4577(8) 0.043(3) Uani 0.50 1 d P . 2
H33C H 1.0733 0.5550 0.5030 0.052 Uiso 0.50 1 calc PR . 2
H33D H 1.0236 0.5254 0.4360 0.052 Uiso 0.50 1 calc PR . 2
C34 C 0.8815(3) 1.4126(4) 0.5747(3) 0.0434(16) Uani 1 1 d . . .
H34A H 0.8674 1.4206 0.6175 0.052 Uiso 1 1 calc R . .
H34B H 0.8684 1.4629 0.5494 0.052 Uiso 1 1 calc R . .
C35 C 0.7649(4) 1.3342(4) 0.5601(3) 0.0523(18) Uani 1 1 d . . .
H35A H 0.7352 1.2958 0.5294 0.063 Uiso 1 1 calc R . .
H35B H 0.7377 1.3870 0.5557 0.063 Uiso 1 1 calc R . .
C36 C 0.7670(3) 1.3022(4) 0.6284(3) 0.0409(15) Uani 1 1 d . . .
H36A H 0.7878 1.3443 0.6601 0.049 Uiso 1 1 calc R . .
H36B H 0.7150 1.2885 0.6349 0.049 Uiso 1 1 calc R . .
C37 C 0.8104(3) 1.1890(4) 0.6966(3) 0.0393(15) Uani 1 1 d . . .
H37A H 0.7583 1.1679 0.6955 0.047 Uiso 1 1 calc R . .
H37B H 0.8221 1.2275 0.7331 0.047 Uiso 1 1 calc R . .
C38 C 0.8673(3) 1.1186(4) 0.7060(3) 0.0406(15) Uani 1 1 d . . .
H38A H 0.9197 1.1390 0.7074 0.049 Uiso 1 1 calc R . .
H38B H 0.8651 1.0893 0.7465 0.049 Uiso 1 1 calc R . .
C39 C 0.9247(3) 0.5729(3) 0.1603(2) 0.0299(13) Uani 1 1 d . . .
C40 C 0.9737(3) 0.5865(3) 0.2188(2) 0.0329(14) Uani 1 1 d . . .
H40 H 0.9746 0.5498 0.2535 0.039 Uiso 1 1 calc R . .
C41 C 1.0230(3) 0.6567(4) 0.2258(3) 0.0360(14) Uani 1 1 d . . .
H41 H 1.0550 0.6667 0.2659 0.043 Uiso 1 1 calc R . .
C42 C 1.0243(3) 0.7103(3) 0.1746(2) 0.0341(14) Uani 1 1 d . . .
H42 H 1.0575 0.7558 0.1799 0.041 Uiso 1 1 calc R . .
C43 C 0.9753(3) 0.6962(3) 0.1139(2) 0.0294(13) Uani 1 1 d . . .
C44 C 0.9230(3) 0.6283(4) 0.1063(2) 0.0321(14) Uani 1 1 d . . .
C45 C 0.8726(3) 0.6177(4) 0.0453(2) 0.0333(14) Uani 1 1 d . . .
H45 H 0.8376 0.5737 0.0398 0.040 Uiso 1 1 calc R . .
C46 C 0.8747(3) 0.6707(4) -0.0051(2) 0.0358(15) Uani 1 1 d . . .
H46 H 0.8405 0.6627 -0.0444 0.043 Uiso 1 1 calc R . .
C47 C 0.9268(3) 0.7372(4) 0.0004(3) 0.0380(15) Uani 1 1 d . . .
H47 H 0.9274 0.7730 -0.0348 0.046 Uiso 1 1 calc R . .
C48 C 1.0227(3) 0.2514(4) -0.0588(3) 0.0355(14) Uani 1 1 d . . .
O10 O 0.9660(2) 0.1920(2) -0.06945(18) 0.0430(10) Uani 1 1 d . . .
C50 C 0.9178(4) 0.0544(4) -0.0626(3) 0.0454(17) Uani 1 1 d . . .
H50A H 0.9101 0.0586 -0.1100 0.054 Uiso 1 1 calc R . .
H50B H 0.9354 -0.0015 -0.0506 0.054 Uiso 1 1 calc R . .
O9 O 0.8456(2) 0.0684(2) -0.04163(17) 0.0398(10) Uani 1 1 d . . .
C52 C 0.7937(3) 0.0998(4) 0.0532(3) 0.0475(17) Uani 1 1 d . . .
H52A H 0.7425 0.1008 0.0261 0.057 Uiso 1 1 calc R . .
H52B H 0.7884 0.0795 0.0963 0.057 Uiso 1 1 calc R . .
C53 C 0.8855(4) 0.1958(4) 0.1146(3) 0.0492(18) Uani 1 1 d . . .
H53A H 0.9296 0.2215 0.1001 0.059 Uiso 1 1 calc R . .
H53B H 0.9023 0.1429 0.1346 0.059 Uiso 1 1 calc R . .
C54 C 0.8583(4) 0.2494(4) 0.1632(3) 0.0438(16) Uani 1 1 d . . .
H54A H 0.8141 0.2238 0.1778 0.053 Uiso 1 1 calc R . .
H54B H 0.8992 0.2562 0.2011 0.053 Uiso 1 1 calc R . .
C55 C 0.8151(3) 0.3857(4) 0.1811(3) 0.0384(15) Uani 1 1 d . . .
H55A H 0.8055 0.3553 0.2193 0.046 Uiso 1 1 calc R . .
H55B H 0.7671 0.4129 0.1616 0.046 Uiso 1 1 calc R . .
C56 C 0.8750(3) 0.4496(3) 0.2023(2) 0.0332(14) Uani 1 1 d . . .
H56A H 0.8641 0.4783 0.2409 0.040 Uiso 1 1 calc R . .
H56B H 0.9257 0.4239 0.2133 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.065(4) . ?
Zn1 Cl3 2.2421(15) . ?
Zn1 Cl2 2.2521(14) . ?
Zn1 Cl1 2.2598(15) . ?
Zn2 N4 2.098(4) . ?
Zn2 Cl4 2.2187(16) . ?
Zn2 Cl5 2.2458(15) . ?
Zn2 Cl6 2.2553(16) . ?
O1 C21 1.361(6) . ?
O1 C38 1.433(6) . ?
O2 C36 1.411(6) . ?
O2 C37 1.415(6) . ?
O3 C35 1.410(7) . ?
O3 C34 1.417(6) . ?
O4A C32 1.389(14) . ?
O4A C33A 1.444(16) . ?
O4B C33B 1.448(18) . ?
O4B C32 1.527(15) . ?
O5 C30 1.343(6) . ?
O5 C31 1.449(6) . ?
O6 C39 1.361(6) . ?
O6 C56 1.462(6) . ?
O7 C55 1.426(6) . ?
O7 C54 1.426(6) . ?
O8 C52 1.433(7) . ?
O8 C53 1.438(6) . ?
C51 O9 1.416(6) . ?
C51 C52 1.492(7) . ?
C49 O10 1.440(6) . ?
C49 C50 1.532(8) . ?
N1 C1 1.336(6) . ?
N1 C5 1.345(6) . ?
N2 C6 1.349(6) . ?
N2 C10 1.355(5) . ?
N2 C3 1.447(6) . ?
N3 C15 1.338(6) . ?
N3 C11 1.366(6) . ?
N3 C18 1.449(6) . ?
N4 C20 1.330(6) . ?
N4 C16 1.333(6) . ?
C1 C2 1.386(6) . ?
C2 C3 1.396(6) . ?
C3 C4 1.373(7) . ?
C4 C5 1.373(7) . ?
C6 C7 1.366(6) . ?
C7 C8 1.386(6) . ?
C8 C9 1.392(6) . ?
C8 C8 1.486(9) 3_656 ?
C9 C10 1.364(6) . ?
C11 C12 1.367(7) . ?
C12 C13 1.392(6) . ?
C13 C14 1.398(6) . ?
C13 C13 1.479(9) 3_667 ?
C14 C15 1.367(6) . ?
C16 C17 1.402(7) . ?
C17 C18 1.379(7) . ?
C18 C19 1.372(7) . ?
C19 C20 1.380(7) . ?
C21 C22 1.376(7) . ?
C21 C26 1.426(7) . ?
C22 C23 1.398(7) . ?
C23 C24 1.375(7) . ?
C24 C25 1.431(7) . ?
C25 C26 1.416(7) . ?
C25 C30 1.426(7) . ?
C26 C27 1.413(7) . ?
C27 C28 1.360(7) . ?
C28 C29 1.392(7) . ?
C29 C30 1.381(7) . ?
C31 C32 1.494(8) . ?
C33A C34 1.575(15) 3_776 ?
C33B C34 1.428(15) 3_776 ?
C34 C33B 1.428(15) 3_776 ?
C34 C33A 1.575(15) 3_776 ?
C35 C36 1.500(7) . ?
C37 C38 1.501(7) . ?
C39 C40 1.371(7) . ?
C39 C44 1.427(7) . ?
C40 C41 1.414(7) . ?
C41 C42 1.371(7) . ?
C42 C43 1.409(7) . ?
C43 C44 1.417(7) . ?
C43 C48 1.425(7) 3_765 ?
C44 C45 1.418(6) . ?
C45 C46 1.354(7) . ?
C46 C47 1.399(7) . ?
C47 C48 1.378(7) 3_765 ?
C48 O10 1.369(6) . ?
C48 C47 1.378(7) 3_765 ?
C48 C43 1.425(7) 3_765 ?
C50 O9 1.426(6) . ?
C53 C54 1.470(7) . ?
C55 C56 1.481(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 Cl3 105.85(11) . . ?
N1 Zn1 Cl2 103.61(12) . . ?
Cl3 Zn1 Cl2 116.39(6) . . ?
N1 Zn1 Cl1 100.69(12) . . ?
Cl3 Zn1 Cl1 113.36(6) . . ?
Cl2 Zn1 Cl1 114.61(5) . . ?
N4 Zn2 Cl4 105.79(12) . . ?
N4 Zn2 Cl5 102.26(13) . . ?
Cl4 Zn2 Cl5 112.10(6) . . ?
N4 Zn2 Cl6 105.43(13) . . ?
Cl4 Zn2 Cl6 111.97(6) . . ?
Cl5 Zn2 Cl6 117.82(6) . . ?
C21 O1 C38 118.7(4) . . ?
C36 O2 C37 112.4(4) . . ?
C35 O3 C34 114.3(5) . . ?
C32 O4A C33A 105.3(10) . . ?
C33B O4B C32 108.5(10) . . ?
C30 O5 C31 116.8(4) . . ?
C39 O6 C56 115.9(4) . . ?
C55 O7 C54 112.6(4) . . ?
C52 O8 C53 115.0(5) . . ?
O9 C51 C52 108.6(5) . . ?
O10 C49 C50 106.8(4) . . ?
C1 N1 C5 117.7(4) . . ?
C1 N1 Zn1 125.1(3) . . ?
C5 N1 Zn1 117.2(3) . . ?
C6 N2 C10 119.5(4) . . ?
C6 N2 C3 120.1(4) . . ?
C10 N2 C3 120.4(4) . . ?
C15 N3 C11 121.1(4) . . ?
C15 N3 C18 118.6(4) . . ?
C11 N3 C18 120.2(4) . . ?
C20 N4 C16 118.1(5) . . ?
C20 N4 Zn2 117.9(4) . . ?
C16 N4 Zn2 124.0(4) . . ?
N1 C1 C2 123.5(4) . . ?
C1 C2 C3 117.3(5) . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 N2 119.4(4) . . ?
C2 C3 N2 120.8(4) . . ?
C3 C4 C5 118.8(5) . . ?
N1 C5 C4 123.0(5) . . ?
N2 C6 C7 121.1(4) . . ?
C6 C7 C8 120.6(5) . . ?
C7 C8 C9 117.1(4) . . ?
C7 C8 C8 121.1(5) . 3_656 ?
C9 C8 C8 121.8(5) . 3_656 ?
C10 C9 C8 120.7(4) . . ?
N2 C10 C9 120.8(5) . . ?
N3 C11 C12 118.5(5) . . ?
C11 C12 C13 122.4(4) . . ?
C12 C13 C14 116.3(4) . . ?
C12 C13 C13 123.0(5) . 3_667 ?
C14 C13 C13 120.7(5) . 3_667 ?
C15 C14 C13 120.5(5) . . ?
N3 C15 C14 121.0(4) . . ?
N4 C16 C17 123.0(5) . . ?
C18 C17 C16 117.3(5) . . ?
C19 C18 C17 120.0(5) . . ?
C19 C18 N3 119.3(5) . . ?
C17 C18 N3 120.7(5) . . ?
C18 C19 C20 118.7(5) . . ?
N4 C20 C19 122.9(5) . . ?
O1 C21 C22 125.1(5) . . ?
O1 C21 C26 113.0(5) . . ?
C22 C21 C26 121.8(5) . . ?
C21 C22 C23 119.2(5) . . ?
C24 C23 C22 122.1(5) . . ?
C23 C24 C25 118.9(5) . . ?
C26 C25 C30 118.1(5) . . ?
C26 C25 C24 120.3(5) . . ?
C30 C25 C24 121.6(5) . . ?
C27 C26 C25 120.9(5) . . ?
C27 C26 C21 121.4(5) . . ?
C25 C26 C21 117.6(5) . . ?
C28 C27 C26 118.5(5) . . ?
C27 C28 C29 122.3(5) . . ?
C30 C29 C28 120.2(5) . . ?
O5 C30 C29 125.8(5) . . ?
O5 C30 C25 114.4(5) . . ?
C29 C30 C25 119.8(5) . . ?
O5 C31 C32 106.5(5) . . ?
O4A C32 C31 122.9(7) . . ?
O4A C32 O4B 29.2(4) . . ?
C31 C32 O4B 99.0(7) . . ?
O4A C33A C34 107.4(10) . 3_776 ?
C34 C33B O4B 106.8(11) 3_776 . ?
O3 C34 C33B 108.7(7) . 3_776 ?
O3 C34 C33A 111.7(7) . 3_776 ?
C33B C34 C33A 39.9(6) 3_776 3_776 ?
O3 C35 C36 114.6(5) . . ?
O2 C36 C35 108.5(5) . . ?
O2 C37 C38 109.7(5) . . ?
O1 C38 C37 105.8(4) . . ?
O6 C39 C40 124.6(5) . . ?
O6 C39 C44 114.4(5) . . ?
C40 C39 C44 121.0(5) . . ?
C39 C40 C41 119.6(5) . . ?
C42 C41 C40 121.2(5) . . ?
C41 C42 C43 119.8(5) . . ?
C42 C43 C44 120.2(5) . . ?
C42 C43 C48 121.4(5) . 3_765 ?
C44 C43 C48 118.4(5) . 3_765 ?
C43 C44 C45 118.7(5) . . ?
C43 C44 C39 118.2(5) . . ?
C45 C44 C39 123.1(5) . . ?
C46 C45 C44 120.8(6) . . ?
C45 C46 C47 121.9(5) . . ?
C48 C47 C46 118.7(5) 3_765 . ?
O10 C48 C47 124.7(5) . 3_765 ?
O10 C48 C43 113.9(5) . 3_765 ?
C47 C48 C43 121.4(6) 3_765 3_765 ?
C48 O10 C49 116.9(4) . . ?
O9 C50 C49 112.6(5) . . ?
C51 O9 C50 113.9(4) . . ?
O8 C52 C51 111.4(5) . . ?
O8 C53 C54 110.6(5) . . ?
O7 C54 C53 109.8(5) . . ?
O7 C55 C56 113.1(4) . . ?
O6 C56 C55 108.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 997296'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1(ZnBr3)2+CH3OH

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H56 Br6 N4 O9 Zn2'
_chemical_formula_weight         1503.22

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   8.49590(10)
_cell_length_b                   16.3216(2)
_cell_length_c                   20.7112(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9030(10)
_cell_angle_gamma                90.00
_cell_volume                     2844.68(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4919
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      21.22

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_absorpt_coefficient_mu    5.114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6361
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40093
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_sigmaI/netI    0.2016
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         30.03
_reflns_number_total             8294
_reflns_number_gt                3319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0740P)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         8294
_refine_ls_number_parameters     340
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2136
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.1776
_refine_ls_wR_factor_gt          0.1362
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.33995(9) 0.33518(4) 0.31752(4) 0.0359(2) Uani 1 1 d . . .
Br2 Br 1.08846(10) 0.52019(5) 0.22374(4) 0.0429(2) Uani 1 1 d . . .
Br3 Br 1.45152(11) 0.42734(5) 0.15029(4) 0.0531(3) Uani 1 1 d . . .
Zn1 Zn 1.25061(10) 0.40185(5) 0.21701(4) 0.0345(3) Uani 1 1 d . . .
O1 O 0.2045(6) -0.0255(3) 0.1433(3) 0.0459(14) Uani 1 1 d . . .
O2 O 0.2106(7) -0.2032(3) 0.1331(3) 0.0512(15) Uani 1 1 d . . .
O3 O 0.6807(7) 0.3328(3) -0.0488(3) 0.0526(16) Uani 1 1 d . . .
O4 O 0.4291(7) 0.2754(3) 0.0244(2) 0.0511(16) Uani 1 1 d . . .
O5 O 1.0000 0.5000 0.0000 0.279(16) Uani 1 2 d SD . .
N1 N 1.0910(8) 0.3159(4) 0.1721(3) 0.0375(16) Uani 1 1 d . . .
N2 N 0.7775(6) 0.1404(3) 0.0755(3) 0.0240(13) Uani 1 1 d . . .
C1 C 1.0957(8) 0.2390(4) 0.1893(3) 0.0303(17) Uani 1 1 d . . .
H1 H 1.1713 0.2233 0.2239 0.036 Uiso 1 1 calc R . .
C2 C 0.9948(8) 0.1791(4) 0.1592(3) 0.0322(18) Uani 1 1 d . . .
H2 H 1.0034 0.1249 0.1733 0.039 Uiso 1 1 calc R . .
C3 C 0.8848(9) 0.2011(4) 0.1094(3) 0.0290(17) Uani 1 1 d . . .
C4 C 0.8662(14) 0.2828(5) 0.0918(4) 0.094(4) Uani 1 1 d . . .
H4 H 0.7854 0.3001 0.0599 0.112 Uiso 1 1 calc R . .
C5 C 0.9772(15) 0.3386(6) 0.1252(5) 0.108(5) Uani 1 1 d . . .
H5 H 0.9697 0.3936 0.1136 0.130 Uiso 1 1 calc R . .
C6 C 0.7386(8) 0.0738(4) 0.1085(3) 0.0289(17) Uani 1 1 d . . .
H6 H 0.7835 0.0663 0.1516 0.035 Uiso 1 1 calc R . .
C7 C 0.6348(8) 0.0179(4) 0.0793(3) 0.0262(16) Uani 1 1 d . . .
H7 H 0.6125 -0.0288 0.1022 0.031 Uiso 1 1 calc R . .
C8 C 0.5600(7) 0.0293(4) 0.0151(3) 0.0210(15) Uani 1 1 d . . .
C9 C 0.6070(8) 0.0985(4) -0.0177(3) 0.0268(16) Uani 1 1 d . . .
H9 H 0.5639 0.1074 -0.0609 0.032 Uiso 1 1 calc R . .
C10 C 0.7149(8) 0.1529(4) 0.0127(3) 0.0280(17) Uani 1 1 d . . .
H10 H 0.7451 0.1983 -0.0098 0.034 Uiso 1 1 calc R . .
C11 C 0.2901(9) 0.0452(5) 0.1454(4) 0.039(2) Uani 1 1 d . . .
C12 C 0.3985(9) 0.0701(5) 0.1986(4) 0.042(2) Uani 1 1 d . . .
H12 H 0.4166 0.0381 0.2360 0.051 Uiso 1 1 calc R . .
C13 C 0.4807(10) 0.1454(5) 0.1944(4) 0.044(2) Uani 1 1 d . . .
H13 H 0.5500 0.1631 0.2304 0.053 Uiso 1 1 calc R . .
C14 C 0.4614(10) 0.1925(5) 0.1396(4) 0.046(2) Uani 1 1 d . . .
H14 H 0.5215 0.2398 0.1371 0.056 Uiso 1 1 calc R . .
C15 C 0.3479(9) 0.1682(5) 0.0861(4) 0.040(2) Uani 1 1 d . . .
C16 C 0.2585(10) 0.0947(5) 0.0899(4) 0.043(2) Uani 1 1 d . . .
C17 C 0.1408(9) 0.0734(5) 0.0369(4) 0.043(2) Uani 1 1 d . . .
H17 H 0.0835 0.0250 0.0382 0.051 Uiso 1 1 calc R . .
C18 C 0.1125(11) 0.1230(6) -0.0146(4) 0.055(2) Uani 1 1 d . . .
H18 H 0.0286 0.1109 -0.0469 0.066 Uiso 1 1 calc R . .
C19 C 0.2057(11) 0.1931(6) -0.0217(4) 0.056(3) Uani 1 1 d . . .
H19 H 0.1869 0.2245 -0.0594 0.067 Uiso 1 1 calc R . .
C20 C 0.3235(11) 0.2147(5) 0.0270(4) 0.048(2) Uani 1 1 d . . .
C21 C 0.4067(12) 0.3303(6) -0.0308(5) 0.066(3) Uani 1 1 d . . .
H21A H 0.3891 0.2990 -0.0710 0.079 Uiso 1 1 calc R . .
H21B H 0.3143 0.3646 -0.0286 0.079 Uiso 1 1 calc R . .
C22 C 0.5464(13) 0.3808(6) -0.0301(4) 0.069(3) Uani 1 1 d . . .
H22A H 0.5758 0.4032 0.0133 0.083 Uiso 1 1 calc R . .
H22B H 0.5230 0.4261 -0.0601 0.083 Uiso 1 1 calc R . .
C23 C 0.6922(11) 0.3386(5) -0.1153(4) 0.056(2) Uani 1 1 d . . .
H23A H 0.7090 0.3954 -0.1265 0.067 Uiso 1 1 calc R . .
H23B H 0.5935 0.3204 -0.1404 0.067 Uiso 1 1 calc R . .
C24 C 0.1766(11) -0.2888(5) 0.1322(5) 0.064(3) Uani 1 1 d . . .
H24A H 0.0829 -0.2991 0.1009 0.077 Uiso 1 1 calc R . .
H24B H 0.1528 -0.3052 0.1749 0.077 Uiso 1 1 calc R . .
C25 C 0.1478(10) -0.1570(5) 0.1832(4) 0.052(2) Uani 1 1 d . . .
H25A H 0.1540 -0.1896 0.2226 0.062 Uiso 1 1 calc R . .
H25B H 0.0369 -0.1442 0.1691 0.062 Uiso 1 1 calc R . .
C26 C 0.2381(9) -0.0802(5) 0.1971(4) 0.042(2) Uani 1 1 d . . .
H26A H 0.2089 -0.0549 0.2361 0.050 Uiso 1 1 calc R . .
H26B H 0.3510 -0.0921 0.2046 0.050 Uiso 1 1 calc R . .
C27 C 0.925(6) 0.5750(19) -0.002(2) 0.37(5) Uani 0.50 1 d PD . .


_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
Br1 Zn1 2.3790(11) . ?
Br2 Zn1 2.3876(12) . ?
Br3 Zn1 2.3758(12) . ?
Zn1 N1 2.081(6) . ?
O1 C11 1.362(9) . ?
O1 C26 1.426(8) . ?
O2 C24 1.425(9) . ?
O2 C25 1.444(9) . ?
O3 C23 1.398(9) . ?
O3 C22 1.479(10) . ?
O4 C20 1.343(9) . ?
O4 C21 1.445(9) . ?
O5 C27 1.38(2) . ?
O5 C27 1.38(2) 3_765 ?
N1 C1 1.303(8) . ?
N1 C5 1.325(10) . ?
N2 C6 1.349(8) . ?
N2 C10 1.351(8) . ?
N2 C3 1.459(8) . ?
C1 C2 1.390(9) . ?
C2 C3 1.343(9) . ?
C3 C4 1.385(10) . ?
C4 C5 1.420(11) . ?
C6 C7 1.352(8) . ?
C7 C8 1.405(8) . ?
C8 C9 1.404(8) . ?
C8 C8 1.474(12) 3_655 ?
C9 C10 1.366(8) . ?
C11 C12 1.396(11) . ?
C11 C16 1.400(10) . ?
C12 C13 1.422(11) . ?
C13 C14 1.363(10) . ?
C14 C15 1.422(10) . ?
C15 C16 1.428(11) . ?
C15 C20 1.431(11) . ?
C16 C17 1.422(10) . ?
C17 C18 1.334(11) . ?
C18 C19 1.410(12) . ?
C19 C20 1.366(11) . ?
C21 C22 1.443(12) . ?
C23 C24 1.461(11) 3_655 ?
C24 C23 1.461(11) 3_655 ?
C25 C26 1.476(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 Br3 109.52(17) . . ?
N1 Zn1 Br1 101.12(17) . . ?
Br3 Zn1 Br1 114.88(5) . . ?
N1 Zn1 Br2 103.06(19) . . ?
Br3 Zn1 Br2 111.02(4) . . ?
Br1 Zn1 Br2 115.86(4) . . ?
C11 O1 C26 117.2(6) . . ?
C24 O2 C25 115.3(6) . . ?
C23 O3 C22 112.6(6) . . ?
C20 O4 C21 118.2(7) . . ?
C27 O5 C27 179.999(6) . 3_765 ?
C1 N1 C5 117.5(6) . . ?
C1 N1 Zn1 122.2(5) . . ?
C5 N1 Zn1 120.2(5) . . ?
C6 N2 C10 121.1(5) . . ?
C6 N2 C3 118.9(5) . . ?
C10 N2 C3 119.9(5) . . ?
N1 C1 C2 124.1(7) . . ?
C3 C2 C1 118.5(7) . . ?
C2 C3 C4 120.2(7) . . ?
C2 C3 N2 120.7(6) . . ?
C4 C3 N2 119.1(6) . . ?
C3 C4 C5 116.4(8) . . ?
N1 C5 C4 123.0(8) . . ?
N2 C6 C7 120.5(6) . . ?
C6 C7 C8 121.0(6) . . ?
C9 C8 C7 116.3(6) . . ?
C9 C8 C8 122.8(7) . 3_655 ?
C7 C8 C8 120.9(7) . 3_655 ?
C10 C9 C8 121.1(6) . . ?
N2 C10 C9 119.8(6) . . ?
O1 C11 C12 124.3(7) . . ?
O1 C11 C16 115.0(7) . . ?
C12 C11 C16 120.7(8) . . ?
C11 C12 C13 118.7(7) . . ?
C14 C13 C12 122.3(8) . . ?
C13 C14 C15 118.9(8) . . ?
C14 C15 C16 120.0(7) . . ?
C14 C15 C20 121.4(8) . . ?
C16 C15 C20 118.6(8) . . ?
C11 C16 C17 121.9(8) . . ?
C11 C16 C15 119.2(8) . . ?
C17 C16 C15 119.0(7) . . ?
C18 C17 C16 119.9(9) . . ?
C17 C18 C19 122.3(9) . . ?
C20 C19 C18 119.8(8) . . ?
O4 C20 C19 126.0(9) . . ?
O4 C20 C15 114.0(8) . . ?
C19 C20 C15 120.0(9) . . ?
C22 C21 O4 109.0(8) . . ?
C21 C22 O3 111.0(8) . . ?
O3 C23 C24 110.9(7) . 3_655 ?
O2 C24 C23 112.9(7) . 3_655 ?
O2 C25 C26 110.5(6) . . ?
O1 C26 C25 109.6(6) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.153
_database_code_depnum_ccdc_archive 'CCDC 997297'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2(ZnBr3)2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H60 Br6 N4 O10 Zn2'
_chemical_formula_weight         1559.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   17.5924(2)
_cell_length_b                   16.3095(2)
_cell_length_c                   21.2570(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.7990(10)
_cell_angle_gamma                90.00
_cell_volume                     5991.11(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9831
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3096
_exptl_absorpt_coefficient_mu    4.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3234
_exptl_absorpt_correction_T_max  0.6421
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            162070
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         30.03
_reflns_number_total             17520
_reflns_number_gt                11007
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+9.5795P] 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         17520
_refine_ls_number_parameters     722
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.48564(2) 0.10439(3) 0.66173(2) 0.03128(10) Uani 1 1 d . . .
Br2 Br 0.43460(2) 0.18133(3) 0.829558(19) 0.02921(10) Uani 1 1 d . . .
Br3 Br 0.30652(3) 0.00782(3) 0.72525(2) 0.03096(10) Uani 1 1 d . . .
Br4 Br 0.10003(3) 0.84408(3) 0.18298(2) 0.03274(11) Uani 1 1 d . . .
Br5 Br 0.22322(3) 1.04128(3) 0.26816(2) 0.03258(10) Uani 1 1 d . . .
Br6 Br 0.05647(3) 0.93766(4) 0.34087(2) 0.04476(13) Uani 1 1 d . . .
Zn1 Zn 0.39055(3) 0.12364(3) 0.72616(2) 0.02250(10) Uani 1 1 d . . .
Zn2 Zn 0.15103(3) 0.91941(3) 0.27773(2) 0.02774(11) Uani 1 1 d . . .
O1 O 0.08691(16) 0.75864(18) 0.98060(13) 0.0309(7) Uani 1 1 d . . .
O3 O 0.15396(17) 1.06473(19) 0.85046(15) 0.0372(7) Uani 1 1 d . . .
O4 O 0.18288(19) 1.2282(2) 0.86649(16) 0.0431(8) Uani 1 1 d . . .
O5 O 0.1566(2) 1.3395(2) 0.96010(19) 0.0662(12) Uani 1 1 d . . .
O6 O 0.37501(17) 1.00741(18) 0.14350(13) 0.0314(7) Uani 1 1 d . . .
O7 O 0.33649(18) 0.82881(18) 0.13149(13) 0.0333(7) Uani 1 1 d . . .
O8 O 0.3199(2) 0.6810(2) 0.05882(16) 0.0535(10) Uani 1 1 d . . .
O9 O 0.3496(2) 0.5735(2) -0.03942(15) 0.0426(8) Uani 1 1 d . . .
O10 O 0.53147(19) 1.3049(2) 0.06565(16) 0.0425(8) Uani 1 1 d . . .
N1 N 0.31410(18) 0.2114(2) 0.67983(14) 0.0211(7) Uani 1 1 d . . .
N2 N 0.15011(17) 0.37440(18) 0.57993(14) 0.0179(6) Uani 1 1 d . . .
N3 N 0.37210(18) 0.65257(19) 0.42891(15) 0.0209(7) Uani 1 1 d . . .
N4 N 0.22853(19) 0.8343(2) 0.32960(16) 0.0278(8) Uani 1 1 d . . .
C1 C 0.3098(2) 0.2886(2) 0.70016(18) 0.0213(8) Uani 1 1 d . . .
H1 H 0.3437 0.3051 0.7369 0.026 Uiso 1 1 calc R . .
C2 C 0.2575(2) 0.3445(2) 0.66904(17) 0.0210(8) Uani 1 1 d . . .
H2 H 0.2555 0.3976 0.6845 0.025 Uiso 1 1 calc R . .
C3 C 0.2078(2) 0.3192(2) 0.61392(17) 0.0195(8) Uani 1 1 d . . .
C4 C 0.2121(2) 0.2399(2) 0.59222(19) 0.0287(9) Uani 1 1 d . . .
H4 H 0.1793 0.2218 0.5554 0.034 Uiso 1 1 calc R . .
C5 C 0.2663(2) 0.1883(3) 0.6265(2) 0.0298(9) Uani 1 1 d . . .
H5 H 0.2697 0.1349 0.6119 0.036 Uiso 1 1 calc R . .
C6 C 0.1218(2) 0.4361(2) 0.61175(17) 0.0202(8) Uani 1 1 d . . .
H6 H 0.1416 0.4442 0.6550 0.024 Uiso 1 1 calc R . .
C7 C 0.0647(2) 0.4862(2) 0.58092(17) 0.0208(8) Uani 1 1 d . . .
H7 H 0.0472 0.5292 0.6031 0.025 Uiso 1 1 calc R . .
C8 C 0.0324(2) 0.4739(2) 0.51665(17) 0.0176(7) Uani 1 1 d . . .
C9 C 0.0641(2) 0.4116(2) 0.48439(18) 0.0212(8) Uani 1 1 d . . .
H9 H 0.0452 0.4026 0.4411 0.025 Uiso 1 1 calc R . .
C10 C 0.1225(2) 0.3639(2) 0.51647(17) 0.0212(8) Uani 1 1 d . . .
H10 H 0.1439 0.3235 0.4943 0.025 Uiso 1 1 calc R . .
C11 C 0.3791(2) 0.5824(2) 0.39718(18) 0.0226(8) Uani 1 1 d . . .
H11 H 0.3506 0.5753 0.3561 0.027 Uiso 1 1 calc R . .
C12 C 0.4276(2) 0.5216(2) 0.42472(17) 0.0218(8) Uani 1 1 d . . .
H12 H 0.4307 0.4727 0.4027 0.026 Uiso 1 1 calc R . .
C13 C 0.4726(2) 0.5322(2) 0.48553(17) 0.0179(7) Uani 1 1 d . . .
C14 C 0.4627(2) 0.6051(2) 0.51756(18) 0.0217(8) Uani 1 1 d . . .
H14 H 0.4901 0.6135 0.5589 0.026 Uiso 1 1 calc R . .
C15 C 0.4127(2) 0.6648(2) 0.48862(18) 0.0228(8) Uani 1 1 d . . .
H15 H 0.4069 0.7133 0.5102 0.027 Uiso 1 1 calc R . .
C16 C 0.2047(2) 0.7570(3) 0.3300(2) 0.0311(10) Uani 1 1 d . . .
H16 H 0.1556 0.7438 0.3075 0.037 Uiso 1 1 calc R . .
C17 C 0.2497(2) 0.6952(3) 0.36265(19) 0.0282(9) Uani 1 1 d . . .
H17 H 0.2320 0.6414 0.3620 0.034 Uiso 1 1 calc R . .
C18 C 0.3220(2) 0.7169(2) 0.39625(18) 0.0231(8) Uani 1 1 d . . .
C19 C 0.3484(2) 0.7963(2) 0.39729(19) 0.0267(9) Uani 1 1 d . . .
H19 H 0.3969 0.8111 0.4199 0.032 Uiso 1 1 calc R . .
C20 C 0.2983(3) 0.8535(3) 0.3627(2) 0.0312(10) Uani 1 1 d . . .
H20 H 0.3145 0.9078 0.3627 0.037 Uiso 1 1 calc R . .
C21 C 0.1256(2) 0.8303(3) 0.97711(19) 0.0273(9) Uani 1 1 d . . .
C22 C 0.1821(2) 0.8602(3) 1.0240(2) 0.0285(9) Uani 1 1 d . . .
H22 H 0.1973 0.8309 1.0618 0.034 Uiso 1 1 calc R . .
C23 C 0.2172(2) 0.9354(3) 1.0153(2) 0.0307(10) Uani 1 1 d . . .
H23 H 0.2557 0.9554 1.0478 0.037 Uiso 1 1 calc R . .
C24 C 0.1965(2) 0.9800(3) 0.9604(2) 0.0288(9) Uani 1 1 d . . .
H24 H 0.2209 1.0295 0.9554 0.035 Uiso 1 1 calc R . .
C25 C 0.1375(2) 0.9499(3) 0.91135(19) 0.0261(9) Uani 1 1 d . . .
C26 C 0.1015(2) 0.8737(3) 0.91859(18) 0.0249(9) Uani 1 1 d . . .
C27 C 0.0436(2) 0.8431(3) 0.86831(19) 0.0283(9) Uani 1 1 d . . .
H27 H 0.0209 0.7924 0.8722 0.034 Uiso 1 1 calc R . .
C28 C 0.0216(2) 0.8893(3) 0.8139(2) 0.0327(10) Uani 1 1 d . . .
H28 H -0.0170 0.8697 0.7814 0.039 Uiso 1 1 calc R . .
C29 C 0.0560(2) 0.9651(3) 0.8061(2) 0.0331(10) Uani 1 1 d . . .
H29 H 0.0397 0.9957 0.7691 0.040 Uiso 1 1 calc R . .
C30 C 0.1141(2) 0.9945(3) 0.8534(2) 0.0304(9) Uani 1 1 d . . .
C31 C 0.1310(3) 1.1192(3) 0.7972(2) 0.0384(11) Uani 1 1 d . . .
H31A H 0.0786 1.1384 0.7959 0.046 Uiso 1 1 calc R . .
H31B H 0.1332 1.0914 0.7573 0.046 Uiso 1 1 calc R . .
C32 C 0.1864(3) 1.1890(3) 0.8073(2) 0.0386(11) Uani 1 1 d . . .
H32A H 0.2385 1.1692 0.8077 0.046 Uiso 1 1 calc R . .
H32B H 0.1735 1.2280 0.7724 0.046 Uiso 1 1 calc R . .
C33 C 0.2287(3) 1.2995(3) 0.8768(2) 0.0423(12) Uani 1 1 d . . .
H33A H 0.2070 1.3419 0.8467 0.051 Uiso 1 1 calc R . .
H33B H 0.2808 1.2877 0.8704 0.051 Uiso 1 1 calc R . .
C34 C 0.2306(3) 1.3282(4) 0.9441(3) 0.0557(15) Uani 1 1 d . . .
H34A H 0.2591 1.2885 0.9733 0.067 Uiso 1 1 calc R . .
H34B H 0.2585 1.3797 0.9503 0.067 Uiso 1 1 calc R . .
C35 C 0.1137(3) 1.4057(3) 0.9286(3) 0.0471(13) Uani 1 1 d . . .
H35A H 0.0921 1.3909 0.8847 0.056 Uiso 1 1 calc R . .
H35B H 0.1469 1.4531 0.9282 0.056 Uiso 1 1 calc R . .
C38 C 0.1121(3) 0.7093(3) 1.0369(2) 0.0385(11) Uani 1 1 d . A .
H38A H 0.0983 0.7356 1.0741 0.046 Uiso 1 1 calc R . .
H38B H 0.1678 0.7024 1.0444 0.046 Uiso 1 1 calc R . .
C39 C 0.4254(2) 1.0715(3) 0.1551(2) 0.0299(9) Uani 1 1 d . . .
C40 C 0.4756(2) 1.0850(3) 0.2122(2) 0.0334(10) Uani 1 1 d . . .
H40 H 0.4773 1.0486 0.2461 0.040 Uiso 1 1 calc R . .
C41 C 0.5246(3) 1.1545(3) 0.2191(2) 0.0349(10) Uani 1 1 d . . .
H41 H 0.5573 1.1641 0.2582 0.042 Uiso 1 1 calc R . .
C42 C 0.5248(2) 1.2082(3) 0.1691(2) 0.0342(10) Uani 1 1 d . . .
H42 H 0.5577 1.2534 0.1743 0.041 Uiso 1 1 calc R . .
C43 C 0.4746(2) 1.1942(3) 0.1098(2) 0.0301(10) Uani 1 1 d . . .
C44 C 0.4233(2) 1.1266(3) 0.10230(19) 0.0300(9) Uani 1 1 d . . .
C45 C 0.3712(3) 1.1148(3) 0.0433(2) 0.0320(10) Uani 1 1 d . . .
H45 H 0.3369 1.0708 0.0383 0.038 Uiso 1 1 calc R . .
C46 C 0.3718(3) 1.1685(3) -0.0059(2) 0.0373(11) Uani 1 1 d . . .
H46 H 0.3368 1.1611 -0.0441 0.045 Uiso 1 1 calc R . .
C47 C 0.4239(3) 1.2346(3) -0.0005(2) 0.0397(12) Uani 1 1 d . . .
H47 H 0.4237 1.2699 -0.0349 0.048 Uiso 1 1 calc R . .
C48 C 0.4753(3) 1.2466(3) 0.0564(2) 0.0347(10) Uani 1 1 d . . .
C49 C 0.5172(3) 1.3788(3) 0.0290(2) 0.0475(13) Uani 1 1 d . . .
H49A H 0.4660 1.3997 0.0306 0.057 Uiso 1 1 calc R . .
H49B H 0.5204 1.3684 -0.0154 0.057 Uiso 1 1 calc R . .
C50 C 0.4208(3) 0.5593(3) -0.0586(2) 0.0453(13) Uani 1 1 d . . .
H50A H 0.4135 0.5626 -0.1049 0.054 Uiso 1 1 calc R . .
H50B H 0.4385 0.5043 -0.0459 0.054 Uiso 1 1 calc R . .
C51 C 0.3473(3) 0.5456(3) 0.0231(2) 0.0428(12) Uani 1 1 d . . .
H51A H 0.3985 0.5486 0.0495 0.051 Uiso 1 1 calc R . .
H51B H 0.3303 0.4889 0.0217 0.051 Uiso 1 1 calc R . .
C52 C 0.2926(3) 0.5980(3) 0.0507(2) 0.0449(12) Uani 1 1 d . . .
H52A H 0.2424 0.5972 0.0226 0.054 Uiso 1 1 calc R . .
H52B H 0.2865 0.5759 0.0918 0.054 Uiso 1 1 calc R . .
C53 C 0.3806(3) 0.6948(3) 0.1128(2) 0.0442(12) Uani 1 1 d . . .
H53A H 0.4248 0.7188 0.0984 0.053 Uiso 1 1 calc R . .
H53B H 0.3967 0.6429 0.1332 0.053 Uiso 1 1 calc R . .
C54 C 0.3544(3) 0.7507(3) 0.1600(2) 0.0381(11) Uani 1 1 d . . .
H54A H 0.3090 0.7280 0.1734 0.046 Uiso 1 1 calc R . .
H54B H 0.3949 0.7562 0.1976 0.046 Uiso 1 1 calc R . .
C55 C 0.3163(3) 0.8873(3) 0.1761(2) 0.0341(10) Uani 1 1 d . . .
H55A H 0.3072 0.8586 0.2140 0.041 Uiso 1 1 calc R . .
H55B H 0.2687 0.9146 0.1569 0.041 Uiso 1 1 calc R . .
C56 C 0.3778(2) 0.9496(3) 0.19515(19) 0.0309(10) Uani 1 1 d . . .
H56A H 0.3698 0.9778 0.2336 0.037 Uiso 1 1 calc R . .
H56B H 0.4281 0.9232 0.2042 0.037 Uiso 1 1 calc R . .
O2B O -0.0031(6) 0.6188(6) 1.0187(5) 0.032(2) Uani 0.476(13) 1 d P A 2
O2A O -0.0090(5) 0.6484(5) 1.0381(5) 0.035(2) Uani 0.524(13) 1 d P A 1
C36B C -0.0220(6) 0.6115(7) 1.0809(6) 0.041(4) Uani 0.476(13) 1 d P . 2
H36A H -0.0089 0.6616 1.1050 0.050 Uiso 0.476(13) 1 calc PR A 2
H36B H 0.0067 0.5666 1.1042 0.050 Uiso 0.476(13) 1 calc PR A 2
C36A C -0.0527(6) 0.5757(6) 1.0372(6) 0.041(3) Uani 0.524(13) 1 d P . 1
H36C H -0.0207 0.5315 1.0580 0.050 Uiso 0.524(13) 1 calc PR A 1
H36D H -0.0740 0.5596 0.9936 0.050 Uiso 0.524(13) 1 calc PR A 1
C37 C 0.0729(3) 0.6281(3) 1.0255(3) 0.0465(13) Uani 1 1 d . . .
H37A H 0.0983 0.5870 1.0551 0.056 Uiso 1 1 calc R A 1
H37B H 0.0711 0.6095 0.9819 0.056 Uiso 1 1 calc R A 1


_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
Br1 Zn1 2.3731(6) . ?
Br2 Zn1 2.3829(6) . ?
Br3 Zn1 2.3966(6) . ?
Br4 Zn2 2.3862(7) . ?
Br5 Zn2 2.3878(7) . ?
Br6 Zn2 2.3439(7) . ?
Zn1 N1 2.081(3) . ?
Zn2 N4 2.106(3) . ?
O1 C21 1.362(5) . ?
O1 C38 1.441(5) . ?
O3 C30 1.351(5) . ?
O3 C31 1.435(5) . ?
O4 C33 1.409(6) . ?
O4 C32 1.424(6) . ?
O5 C35 1.413(6) . ?
O5 C34 1.418(6) . ?
O6 C39 1.362(5) . ?
O6 C56 1.441(5) . ?
O7 C54 1.420(5) . ?
O7 C55 1.435(5) . ?
O8 C53 1.431(5) . ?
O8 C52 1.436(6) . ?
O9 C50 1.407(6) . ?
O9 C51 1.412(5) . ?
O10 C48 1.359(6) . ?
O10 C49 1.431(6) . ?
N1 C5 1.334(5) . ?
N1 C1 1.338(5) . ?
N2 C6 1.357(5) . ?
N2 C10 1.356(5) . ?
N2 C3 1.444(5) . ?
N3 C11 1.345(5) . ?
N3 C15 1.349(5) . ?
N3 C18 1.459(5) . ?
N4 C16 1.330(5) . ?
N4 C20 1.333(5) . ?
C1 C2 1.374(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.373(6) . ?
C6 C7 1.364(5) . ?
C7 C8 1.392(5) . ?
C8 C9 1.399(5) . ?
C8 C8 1.491(7) 3_566 ?
C9 C10 1.366(5) . ?
C11 C12 1.368(5) . ?
C12 C13 1.394(5) . ?
C13 C14 1.398(5) . ?
C13 C13 1.479(7) 3_666 ?
C14 C15 1.376(5) . ?
C16 C17 1.385(6) . ?
C17 C18 1.383(6) . ?
C18 C19 1.375(6) . ?
C19 C20 1.394(6) . ?
C21 C22 1.359(6) . ?
C21 C26 1.425(6) . ?
C22 C23 1.401(6) . ?
C23 C24 1.365(6) . ?
C24 C25 1.415(6) . ?
C25 C26 1.417(6) . ?
C25 C30 1.422(6) . ?
C26 C27 1.421(6) . ?
C27 C28 1.374(6) . ?
C28 C29 1.400(6) . ?
C29 C30 1.377(6) . ?
C31 C32 1.489(7) . ?
C33 C34 1.500(7) . ?
C35 C36A 1.435(11) 3_577 ?
C35 C36B 1.612(12) 3_577 ?
C38 C37 1.491(7) . ?
C39 C40 1.379(6) . ?
C39 C44 1.434(6) . ?
C40 C41 1.415(6) . ?
C41 C42 1.378(6) . ?
C42 C43 1.417(6) . ?
C43 C44 1.414(6) . ?
C43 C48 1.422(6) . ?
C44 C45 1.421(6) . ?
C45 C46 1.367(6) . ?
C46 C47 1.405(7) . ?
C47 C48 1.382(6) . ?
C49 C50 1.533(7) 3_675 ?
C50 C49 1.533(7) 3_675 ?
C51 C52 1.487(7) . ?
C53 C54 1.492(6) . ?
C55 C56 1.484(6) . ?
O2B C37 1.327(11) . ?
O2B C36B 1.428(15) . ?
O2A C36A 1.411(14) . ?
O2A C37 1.549(10) . ?
C36B C35 1.612(12) 3_577 ?
C36A C35 1.435(10) 3_577 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 Br1 106.31(8) . . ?
N1 Zn1 Br2 103.57(9) . . ?
Br1 Zn1 Br2 116.24(2) . . ?
N1 Zn1 Br3 101.26(9) . . ?
Br1 Zn1 Br3 113.05(2) . . ?
Br2 Zn1 Br3 114.34(2) . . ?
N4 Zn2 Br6 104.07(9) . . ?
N4 Zn2 Br4 101.94(10) . . ?
Br6 Zn2 Br4 110.71(3) . . ?
N4 Zn2 Br5 106.89(10) . . ?
Br6 Zn2 Br5 112.88(3) . . ?
Br4 Zn2 Br5 118.60(2) . . ?
C21 O1 C38 116.5(3) . . ?
C30 O3 C31 119.3(3) . . ?
C33 O4 C32 112.9(3) . . ?
C35 O5 C34 114.7(4) . . ?
C39 O6 C56 115.8(3) . . ?
C54 O7 C55 112.1(3) . . ?
C53 O8 C52 115.3(4) . . ?
C50 O9 C51 113.8(4) . . ?
C48 O10 C49 117.5(4) . . ?
C5 N1 C1 118.4(3) . . ?
C5 N1 Zn1 117.2(3) . . ?
C1 N1 Zn1 124.4(3) . . ?
C6 N2 C10 119.5(3) . . ?
C6 N2 C3 120.1(3) . . ?
C10 N2 C3 120.4(3) . . ?
C11 N3 C15 121.0(3) . . ?
C11 N3 C18 118.4(3) . . ?
C15 N3 C18 120.5(3) . . ?
C16 N4 C20 118.7(4) . . ?
C16 N4 Zn2 117.0(3) . . ?
C20 N4 Zn2 124.3(3) . . ?
N1 C1 C2 122.8(4) . . ?
C1 C2 C3 118.0(4) . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 N2 119.7(3) . . ?
C2 C3 N2 120.7(3) . . ?
C5 C4 C3 118.3(4) . . ?
N1 C5 C4 122.8(4) . . ?
N2 C6 C7 120.7(3) . . ?
C6 C7 C8 120.9(3) . . ?
C7 C8 C9 117.3(3) . . ?
C7 C8 C8 121.3(4) . 3_566 ?
C9 C8 C8 121.4(4) . 3_566 ?
C10 C9 C8 120.0(3) . . ?
N2 C10 C9 121.4(3) . . ?
N3 C11 C12 120.7(3) . . ?
C11 C12 C13 120.4(4) . . ?
C12 C13 C14 117.2(3) . . ?
C12 C13 C13 120.6(4) . 3_666 ?
C14 C13 C13 122.2(4) . 3_666 ?
C15 C14 C13 120.7(3) . . ?
N3 C15 C14 119.8(4) . . ?
N4 C16 C17 122.8(4) . . ?
C16 C17 C18 117.2(4) . . ?
C19 C18 C17 121.6(4) . . ?
C19 C18 N3 119.8(4) . . ?
C17 C18 N3 118.5(4) . . ?
C18 C19 C20 116.4(4) . . ?
N4 C20 C19 123.3(4) . . ?
O1 C21 C22 124.9(4) . . ?
O1 C21 C26 113.8(4) . . ?
C22 C21 C26 121.3(4) . . ?
C21 C22 C23 119.9(4) . . ?
C24 C23 C22 121.6(4) . . ?
C23 C24 C25 119.2(4) . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 C30 121.0(4) . . ?
C26 C25 C30 118.6(4) . . ?
C25 C26 C27 119.9(4) . . ?
C25 C26 C21 117.7(4) . . ?
C27 C26 C21 122.4(4) . . ?
C28 C27 C26 119.3(4) . . ?
C27 C28 C29 121.6(4) . . ?
C30 C29 C28 119.9(4) . . ?
O3 C30 C29 125.5(4) . . ?
O3 C30 C25 113.9(4) . . ?
C29 C30 C25 120.6(4) . . ?
O3 C31 C32 106.3(4) . . ?
O4 C32 C31 109.5(4) . . ?
O4 C33 C34 108.4(4) . . ?
O5 C34 C33 114.4(5) . . ?
O5 C35 C36A 107.8(5) . 3_577 ?
O5 C35 C36B 111.1(5) . 3_577 ?
C36A C35 C36B 43.6(5) 3_577 3_577 ?
O1 C38 C37 107.4(4) . . ?
O6 C39 C40 124.8(4) . . ?
O6 C39 C44 114.8(4) . . ?
C40 C39 C44 120.4(4) . . ?
C39 C40 C41 119.8(4) . . ?
C42 C41 C40 121.3(4) . . ?
C41 C42 C43 119.5(4) . . ?
C44 C43 C42 120.3(4) . . ?
C44 C43 C48 118.6(4) . . ?
C42 C43 C48 121.0(4) . . ?
C43 C44 C45 119.9(4) . . ?
C43 C44 C39 118.6(4) . . ?
C45 C44 C39 121.5(4) . . ?
C46 C45 C44 119.5(4) . . ?
C45 C46 C47 121.8(4) . . ?
C48 C47 C46 119.4(4) . . ?
O10 C48 C47 124.4(4) . . ?
O10 C48 C43 114.8(4) . . ?
C47 C48 C43 120.7(5) . . ?
O10 C49 C50 107.1(4) . 3_675 ?
O9 C50 C49 112.1(4) . 3_675 ?
O9 C51 C52 108.7(4) . . ?
O8 C52 C51 111.3(4) . . ?
O8 C53 C54 110.9(4) . . ?
O7 C54 C53 109.4(4) . . ?
O7 C55 C56 112.2(4) . . ?
O6 C56 C55 108.7(3) . . ?
C37 O2B C36B 108.2(9) . . ?
C36A O2A C37 110.0(7) . . ?
O2B C36B C35 107.4(9) . 3_577 ?
O2A C36A C35 105.9(9) . 3_577 ?
O2B C37 C38 123.1(6) . . ?
O2B C37 O2A 24.8(4) . . ?
C38 C37 O2A 101.5(5) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.123
_database_code_depnum_ccdc_archive 'CCDC 997298'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2[CdBr4]+0.5CHCl3+1.5CH3OH+0.5H2O

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H67.50 Br4 Cd Cl1.50 N4 O12'
_chemical_formula_weight         1497.87

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'
Cd Cd -0.8075 1.2024 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1323(2)
_cell_length_b                   20.1613(3)
_cell_length_c                   28.3599(5)
_cell_angle_alpha                91.8350(10)
_cell_angle_beta                 100.9020(10)
_cell_angle_gamma                92.9550(10)
_cell_volume                     6236.29(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9164
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      22.63

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_F_000             3012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.076
_exptl_absorpt_coefficient_mu    3.039
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            174034
_diffrn_reflns_av_unetI/netI     0.2103
_diffrn_reflns_av_R_equivalents  0.1536
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.012
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             37707
_reflns_number_gt                15215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1064P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         37707
_refine_ls_number_parameters     1452
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.2281
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.2483
_refine_ls_wR_factor_gt          0.1918
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.017
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.22815(5) 0.72598(3) 0.09752(2) 0.02526(15) Uani 1 1 d . . . . .
Cd2 Cd 0.18494(5) 0.75575(3) 0.57630(2) 0.02933(16) Uani 1 1 d . . . . .
Br1 Br 0.15627(8) 0.72957(4) 0.17916(3) 0.0337(2) Uani 1 1 d . . . . .
Br2 Br 0.20758(7) 0.59898(4) 0.07311(3) 0.02616(19) Uani 1 1 d . . . . .
Br3 Br 0.10024(9) 0.80165(4) 0.03919(3) 0.0397(2) Uani 1 1 d . . . . .
Br4 Br 0.45700(8) 0.76943(4) 0.10820(3) 0.0390(2) Uani 1 1 d . . . . .
Br5 Br 0.09189(9) 0.77333(4) 0.65276(3) 0.0427(3) Uani 1 1 d . . . . .
Br6 Br 0.18494(8) 0.62731(4) 0.56525(3) 0.0364(2) Uani 1 1 d . . . . .
Br7 Br 0.04854(9) 0.81102(5) 0.50616(4) 0.0499(3) Uani 1 1 d . . . . .
Br8 Br 0.40795(8) 0.80548(5) 0.59526(3) 0.0421(2) Uani 1 1 d . . . . .
Cl1 Cl 0.8070(4) 0.9146(2) -0.00645(15) 0.1089(13) Uani 1 1 d . . . . .
Cl2 Cl 0.8538(3) 0.96617(15) 0.09322(13) 0.0846(10) Uani 1 1 d . . . . .
Cl3 Cl 0.7246(3) 0.83940(15) 0.06745(13) 0.0776(9) Uani 1 1 d . . . . .
O1 O 0.1383(5) 0.9134(3) 0.2958(2) 0.0303(13) Uani 1 1 d . . . . .
O2 O 0.1824(5) 0.8235(3) 0.3741(2) 0.0331(14) Uani 1 1 d . . . . .
O3 O 0.4284(5) 0.8461(3) 0.42480(19) 0.0363(14) Uani 1 1 d . . . . .
O4 O 0.6203(5) 0.7605(3) 0.4154(2) 0.0383(15) Uani 1 1 d . . . . .
O5 O 0.7478(5) 0.8251(2) 0.34583(19) 0.0256(12) Uani 1 1 d . . . . .
O6 O 0.8889(5) 1.0385(3) 0.22236(19) 0.0291(13) Uani 1 1 d . . . . .
O7 O 0.8349(5) 1.1211(3) 0.1433(2) 0.0293(13) Uani 1 1 d . . . . .
O8 O 0.6361(5) 1.1728(3) 0.0822(2) 0.0320(13) Uani 1 1 d . . . . .
O9 O 0.4111(5) 1.1898(3) 0.1154(2) 0.0346(14) Uani 1 1 d . . . . .
O10 O 0.2794(5) 1.1349(3) 0.1789(2) 0.0335(14) Uani 1 1 d . . . . .
O11 O 0.6379(5) 0.6563(3) 0.6804(2) 0.0429(16) Uani 1 1 d . . . . .
O12 O 0.5681(6) 0.5738(4) 0.6004(2) 0.061(2) Uani 1 1 d . . . . .
O13 O 0.5762(6) 0.4375(5) 0.5697(4) 0.103(4) Uani 1 1 d . . . . .
O14 O 0.7782(6) 0.3680(3) 0.5789(2) 0.0445(16) Uani 1 1 d . . . . .
O15 O 1.0126(6) 0.3720(3) 0.6430(2) 0.0427(16) Uani 1 1 d . . . . .
O16 O 1.4153(5) 0.4269(3) 0.8121(2) 0.0415(16) Uani 1 1 d . . . . .
O17 O 1.4111(5) 0.4898(3) 0.9012(2) 0.0381(15) Uani 1 1 d . . . . .
O18 O 1.3936(5) 0.6257(3) 0.91338(19) 0.0301(13) Uani 1 1 d . . . . .
O19 O 1.1625(5) 0.6309(2) 0.94017(19) 0.0285(13) Uani 1 1 d . . . . .
O20 O 0.9512(5) 0.6253(3) 0.8716(2) 0.0406(16) Uani 1 1 d . . . . .
O21 O 0.4666(8) 0.9370(4) 0.1125(3) 0.070(2) Uani 1 1 d . . . . .
H21 H 0.5377 0.9511 0.1141 0.105 Uiso 1 1 calc R U . . .
O22 O 0.5952(13) 0.0096(8) 0.4067(4) 0.147(5) Uani 1 1 d D . . . .
H22 H 0.6540 0.0207 0.4281 0.221 Uiso 1 1 calc R U . . .
O23 O 0.7803(17) 0.0100(10) 0.4760(4) 0.278(11) Uani 1 1 d . . . . .
O24A O 0.218(3) 0.1273(16) 0.4299(10) 0.171(11) Uiso 0.5 1 d D . P A 1
C114 C 0.195(4) 0.1899(17) 0.4099(14) 0.151(14) Uiso 0.5 1 d D . P A 1
O24B O 0.170(2) 0.0704(18) 0.4358(12) 0.221(15) Uiso 0.5 1 d D . P B 2
C914 C 0.2933(18) 0.0443(10) 0.4383(7) 0.049(5) Uiso 0.5 1 d D . P B 2
N1 N 0.3290(6) 0.6141(3) 0.2864(2) 0.0273(15) Uani 1 1 d . . . . .
N2 N 0.4283(5) 0.8166(3) 0.2746(2) 0.0200(14) Uani 1 1 d . . . . .
N3 N 0.6104(5) 1.1467(3) 0.2424(2) 0.0241(15) Uani 1 1 d . . . . .
N4 N 0.6926(6) 1.3502(3) 0.2237(3) 0.0359(18) Uani 1 1 d . . . . .
N5 N 0.1953(7) 0.3915(4) 0.5194(3) 0.0409(19) Uani 1 1 d . . . . .
N6 N 0.1032(6) 0.4338(3) 0.3737(2) 0.0235(14) Uani 1 1 d . . . . .
N7 N -0.0743(5) 0.5390(3) 0.1386(2) 0.0218(14) Uani 1 1 d . . . . .
N8 N -0.2067(6) 0.6245(3) 0.0062(2) 0.0307(16) Uani 1 1 d . . . . .
C1 C 0.2935(7) 0.6618(4) 0.3142(3) 0.0296(19) Uani 1 1 d . . . . .
H1 H 0.2441 0.6489 0.3358 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3258(6) 0.7284(4) 0.3129(3) 0.0228(17) Uani 1 1 d . . . . .
H2 H 0.3008 0.7600 0.3330 0.027 Uiso 1 1 calc R U . . .
C3 C 0.3974(6) 0.7459(4) 0.2799(3) 0.0209(16) Uani 1 1 d . . . . .
C4 C 0.4379(7) 0.6985(4) 0.2523(3) 0.0265(18) Uani 1 1 d . . . . .
H4 H 0.4887 0.7102 0.2310 0.032 Uiso 1 1 calc R U . . .
C5 C 0.4022(7) 0.6329(4) 0.2566(3) 0.0251(18) Uani 1 1 d . . . . .
H5 H 0.4304 0.6006 0.2380 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4572(7) 0.8589(4) 0.3128(3) 0.0244(17) Uani 1 1 d . . . . .
H6 H 0.4541 0.8439 0.3433 0.029 Uiso 1 1 calc R U . . .
C7 C 0.4909(6) 0.9235(4) 0.3075(3) 0.0241(17) Uani 1 1 d . . . . .
H7 H 0.5106 0.9526 0.3343 0.029 Uiso 1 1 calc R U . . .
C8 C 0.4962(7) 0.9462(3) 0.2622(3) 0.0218(17) Uani 1 1 d . . . . .
C9 C 0.4601(6) 0.9032(4) 0.2232(3) 0.0233(17) Uani 1 1 d . . . . .
H9 H 0.4589 0.9177 0.1923 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4253(7) 0.8380(4) 0.2301(3) 0.0234(17) Uani 1 1 d . . . . .
H10 H 0.3996 0.8087 0.2037 0.028 Uiso 1 1 calc R U . . .
C11 C 0.6236(7) 1.1233(4) 0.2871(3) 0.0292(19) Uani 1 1 d . . . . .
H11 H 0.6576 1.1511 0.3136 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5871(7) 1.0589(4) 0.2935(3) 0.0272(18) Uani 1 1 d . . . . .
H12 H 0.5954 1.0438 0.3245 0.033 Uiso 1 1 calc R U . . .
C13 C 0.5384(7) 1.0160(3) 0.2553(3) 0.0231(17) Uani 1 1 d . . . . .
C14 C 0.5307(7) 1.0402(4) 0.2088(3) 0.0247(18) Uani 1 1 d . . . . .
H14 H 0.5022 1.0121 0.1819 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5656(7) 1.1051(4) 0.2035(3) 0.0278(18) Uani 1 1 d . . . . .
H15 H 0.5585 1.1212 0.1728 0.033 Uiso 1 1 calc R U . . .
C16 C 0.6493(8) 1.3297(4) 0.2625(3) 0.038(2) Uani 1 1 d . . . . .
H16 H 0.6384 1.3615 0.2855 0.045 Uiso 1 1 calc R U . . .
C17 C 0.6203(7) 1.2638(4) 0.2696(3) 0.032(2) Uani 1 1 d . . . . .
H17 H 0.5888 1.2515 0.2964 0.039 Uiso 1 1 calc R U . . .
C18 C 0.6392(7) 1.2165(4) 0.2358(3) 0.0259(18) Uani 1 1 d . . . . .
C19 C 0.6842(7) 1.2352(4) 0.1959(3) 0.0270(18) Uani 1 1 d . . . . .
H19 H 0.6981 1.2040 0.1729 0.032 Uiso 1 1 calc R U . . .
C20 C 0.7081(7) 1.3039(4) 0.1915(3) 0.032(2) Uani 1 1 d . . . . .
H20 H 0.7365 1.3176 0.1644 0.038 Uiso 1 1 calc R U . . .
C21 C 0.1578(6) 0.9397(4) 0.2539(3) 0.0226(17) Uani 1 1 d . . . . .
C22 C 0.1338(7) 0.9069(4) 0.2096(3) 0.0254(18) Uani 1 1 d . . . . .
H22A H 0.1015 0.8631 0.2064 0.031 Uiso 1 1 calc R U . . .
C23 C 0.1583(7) 0.9396(4) 0.1691(3) 0.0294(19) Uani 1 1 d . . . . .
H23 H 0.1434 0.9167 0.1394 0.035 Uiso 1 1 calc R U . . .
C24 C 0.2031(7) 1.0036(4) 0.1724(3) 0.031(2) Uani 1 1 d . . . . .
H24 H 0.2181 1.0245 0.1452 0.038 Uiso 1 1 calc R U . . .
C25 C 0.2268(6) 1.0379(4) 0.2172(3) 0.0246(18) Uani 1 1 d . . . . .
C26 C 0.2082(7) 1.0071(4) 0.2594(3) 0.0256(18) Uani 1 1 d . . . . .
C27 C 0.2366(7) 1.0424(4) 0.3045(3) 0.0304(19) Uani 1 1 d . . . . .
H27 H 0.2243 1.0216 0.3322 0.036 Uiso 1 1 calc R U . . .
C28 C 0.2817(7) 1.1061(4) 0.3073(3) 0.033(2) Uani 1 1 d . . . . .
H28 H 0.3027 1.1284 0.3372 0.040 Uiso 1 1 calc R U . . .
C29 C 0.2974(6) 1.1393(4) 0.2658(3) 0.0279(19) Uani 1 1 d . . . . .
H29 H 0.3270 1.1836 0.2687 0.034 Uiso 1 1 calc R U . . .
C30 C 0.2702(7) 1.1079(4) 0.2217(3) 0.032(2) Uani 1 1 d . . . . .
C31 C 0.3076(8) 1.2043(4) 0.1806(4) 0.045(3) Uani 1 1 d . . . . .
H31A H 0.3849 1.2154 0.2023 0.054 Uiso 1 1 calc R U . . .
H31B H 0.2441 1.2279 0.1920 0.054 Uiso 1 1 calc R U . . .
C32 C 0.3159(8) 1.2237(4) 0.1309(4) 0.044(3) Uani 1 1 d . . . . .
H32A H 0.2386 1.2122 0.1092 0.053 Uiso 1 1 calc R U . . .
H32B H 0.3328 1.2713 0.1305 0.053 Uiso 1 1 calc R U . . .
C33 C 0.4363(8) 1.2153(4) 0.0723(3) 0.039(2) Uani 1 1 d . . . . .
H33A H 0.4770 1.2592 0.0785 0.047 Uiso 1 1 calc R U . . .
H33B H 0.3605 1.2187 0.0494 0.047 Uiso 1 1 calc R U . . .
C34 C 0.5178(8) 1.1688(4) 0.0520(3) 0.040(2) Uani 1 1 d . . . . .
H34A H 0.4825 1.1236 0.0503 0.048 Uiso 1 1 calc R U . . .
H34B H 0.5246 1.1811 0.0198 0.048 Uiso 1 1 calc R U . . .
C35 C 0.7185(8) 1.1307(4) 0.0649(3) 0.038(2) Uani 1 1 d . . . . .
H35A H 0.7241 1.1412 0.0322 0.046 Uiso 1 1 calc R U . . .
H35B H 0.6889 1.0846 0.0649 0.046 Uiso 1 1 calc R U . . .
C36 C 0.8436(8) 1.1413(4) 0.0972(3) 0.038(2) Uani 1 1 d . . . . .
H36A H 0.9024 1.1155 0.0845 0.045 Uiso 1 1 calc R U . . .
H36B H 0.8712 1.1878 0.0986 0.045 Uiso 1 1 calc R U . . .
C37 C 0.9534(7) 1.1206(4) 0.1740(3) 0.033(2) Uani 1 1 d . . . . .
H37A H 0.9967 1.1637 0.1743 0.040 Uiso 1 1 calc R U . . .
H37B H 1.0012 1.0875 0.1618 0.040 Uiso 1 1 calc R U . . .
C38 C 0.9391(7) 1.1053(4) 0.2232(3) 0.0293(19) Uani 1 1 d . . . . .
H38A H 1.0180 1.1100 0.2448 0.035 Uiso 1 1 calc R U . . .
H38B H 0.8849 1.1357 0.2344 0.035 Uiso 1 1 calc R U . . .
C39 C 0.8714(7) 1.0150(4) 0.2653(3) 0.0300(19) Uani 1 1 d . . . . .
C40 C 0.9015(8) 1.0490(4) 0.3088(3) 0.033(2) Uani 1 1 d . . . . .
H40 H 0.9367 1.0921 0.3105 0.040 Uiso 1 1 calc R U . . .
C41 C 0.8801(8) 1.0201(4) 0.3508(3) 0.034(2) Uani 1 1 d . . . . .
H41 H 0.8984 1.0444 0.3799 0.041 Uiso 1 1 calc R U . . .
C42 C 0.8321(8) 0.9558(4) 0.3491(3) 0.032(2) Uani 1 1 d . . . . .
H42 H 0.8184 0.9369 0.3773 0.039 Uiso 1 1 calc R U . . .
C43 C 0.8033(7) 0.9180(4) 0.3055(3) 0.0234(17) Uani 1 1 d . . . . .
C44 C 0.8210(7) 0.9468(4) 0.2624(3) 0.0264(18) Uani 1 1 d . . . . .
C45 C 0.7901(7) 0.9106(4) 0.2186(3) 0.0292(19) Uani 1 1 d . . . . .
H45 H 0.8012 0.9306 0.1905 0.035 Uiso 1 1 calc R U . . .
C46 C 0.7438(7) 0.8462(4) 0.2163(3) 0.033(2) Uani 1 1 d . . . . .
H46 H 0.7212 0.8228 0.1868 0.040 Uiso 1 1 calc R U . . .
C47 C 0.7307(7) 0.8153(4) 0.2599(3) 0.0282(19) Uani 1 1 d . . . . .
H47 H 0.7025 0.7710 0.2589 0.034 Uiso 1 1 calc R U . . .
C48 C 0.7587(7) 0.8498(4) 0.3026(3) 0.0251(18) Uani 1 1 d . . . . .
C49 C 0.7256(7) 0.7545(4) 0.3477(3) 0.0267(18) Uani 1 1 d . . . . .
H49A H 0.7901 0.7316 0.3364 0.032 Uiso 1 1 calc R U . . .
H49B H 0.6481 0.7405 0.3271 0.032 Uiso 1 1 calc R U . . .
C50 C 0.7227(8) 0.7378(4) 0.3983(3) 0.034(2) Uani 1 1 d . . . . .
H50A H 0.7229 0.6899 0.4007 0.041 Uiso 1 1 calc R U . . .
H50B H 0.7967 0.7570 0.4189 0.041 Uiso 1 1 calc R U . . .
C51 C 0.6377(8) 0.8219(5) 0.4398(3) 0.043(2) Uani 1 1 d . . . . .
H51A H 0.6510 0.8562 0.4178 0.051 Uiso 1 1 calc R U . . .
H51B H 0.7099 0.8223 0.4650 0.051 Uiso 1 1 calc R U . . .
C52 C 0.5275(8) 0.8363(5) 0.4613(3) 0.039(2) Uani 1 1 d . . . . .
H52A H 0.5077 0.7994 0.4801 0.046 Uiso 1 1 calc R U . . .
H52B H 0.5456 0.8758 0.4825 0.046 Uiso 1 1 calc R U . . .
C53 C 0.3224(7) 0.8626(4) 0.4437(3) 0.035(2) Uani 1 1 d . . . . .
H53A H 0.3432 0.9001 0.4666 0.042 Uiso 1 1 calc R U . . .
H53B H 0.2948 0.8252 0.4603 0.042 Uiso 1 1 calc R U . . .
C54 C 0.2245(8) 0.8792(4) 0.4045(3) 0.040(2) Uani 1 1 d . . . . .
H54A H 0.1571 0.8959 0.4178 0.048 Uiso 1 1 calc R U . . .
H54B H 0.2547 0.9140 0.3862 0.048 Uiso 1 1 calc R U . . .
C55 C 0.1997(8) 0.4534(4) 0.5049(3) 0.038(2) Uani 1 1 d . . . . .
H55 H 0.2228 0.4876 0.5281 0.045 Uiso 1 1 calc R U . . .
C56 C 0.1724(7) 0.4698(4) 0.4578(3) 0.033(2) Uani 1 1 d . . . . .
H56 H 0.1783 0.5138 0.4492 0.039 Uiso 1 1 calc R U . . .
C57 C 0.1360(7) 0.4195(4) 0.4237(3) 0.0283(19) Uani 1 1 d . . . . .
C58 C 0.1285(8) 0.3541(4) 0.4376(3) 0.035(2) Uani 1 1 d . . . . .
H58 H 0.1016 0.3192 0.4152 0.042 Uiso 1 1 calc R U . . .
C59 C 0.1620(8) 0.3432(4) 0.4853(3) 0.039(2) Uani 1 1 d . . . . .
H59 H 0.1618 0.2995 0.4947 0.047 Uiso 1 1 calc R U . . .
C60 C 0.1766(7) 0.4786(4) 0.3552(3) 0.0249(18) Uani 1 1 d . . . . .
H60 H 0.2487 0.4968 0.3743 0.030 Uiso 1 1 calc R U . . .
C61 C 0.1441(7) 0.4965(4) 0.3089(3) 0.0245(18) Uani 1 1 d . . . . .
H61 H 0.1935 0.5280 0.2971 0.029 Uiso 1 1 calc R U . . .
C62 C 0.0387(6) 0.4688(3) 0.2786(3) 0.0203(16) Uani 1 1 d . . . . .
C63 C -0.0320(7) 0.4212(4) 0.2976(3) 0.0251(18) Uani 1 1 d . . . . .
H63 H -0.1018 0.4007 0.2783 0.030 Uiso 1 1 calc R U . . .
C64 C 0.0013(7) 0.4044(4) 0.3451(3) 0.0266(18) Uani 1 1 d . . . . .
H64 H -0.0465 0.3727 0.3576 0.032 Uiso 1 1 calc R U . . .
C65 C 0.0350(7) 0.5614(4) 0.1658(3) 0.0282(19) Uani 1 1 d . . . . .
H65 H 0.0848 0.5923 0.1537 0.034 Uiso 1 1 calc R U . . .
C66 C 0.0717(7) 0.5394(4) 0.2103(3) 0.0245(18) Uani 1 1 d . . . . .
H66 H 0.1457 0.5561 0.2288 0.029 Uiso 1 1 calc R U . . .
C67 C -0.0003(6) 0.4916(3) 0.2290(3) 0.0203(16) Uani 1 1 d . . . . .
C68 C -0.1113(7) 0.4678(4) 0.1986(3) 0.0260(18) Uani 1 1 d . . . . .
H68 H -0.1617 0.4358 0.2094 0.031 Uiso 1 1 calc R U . . .
C69 C -0.1448(7) 0.4908(4) 0.1544(3) 0.0248(18) Uani 1 1 d . . . . .
H69 H -0.2167 0.4737 0.1346 0.030 Uiso 1 1 calc R U . . .
C70 C -0.1530(7) 0.6616(4) 0.0453(3) 0.031(2) Uani 1 1 d . . . . .
H70 H -0.1464 0.7074 0.0427 0.037 Uiso 1 1 calc R U . . .
C71 C -0.1073(7) 0.6365(4) 0.0891(3) 0.0258(18) Uani 1 1 d . . . . .
H71 H -0.0721 0.6643 0.1154 0.031 Uiso 1 1 calc R U . . .
C72 C -0.1156(6) 0.5681(4) 0.0926(3) 0.0233(17) Uani 1 1 d . . . . .
C73 C -0.1679(7) 0.5283(4) 0.0534(3) 0.0292(19) Uani 1 1 d . . . . .
H73 H -0.1748 0.4824 0.0554 0.035 Uiso 1 1 calc R U . . .
C74 C -0.2096(7) 0.5576(4) 0.0113(3) 0.034(2) Uani 1 1 d . . . . .
H74 H -0.2422 0.5303 -0.0155 0.041 Uiso 1 1 calc R U . . .
C75 C 0.7415(8) 0.6686(4) 0.7138(3) 0.0309(19) Uani 1 1 d . . . . .
C76 C 0.8388(8) 0.7110(4) 0.7103(3) 0.038(2) Uani 1 1 d . . . . .
H76 H 0.8368 0.7343 0.6824 0.045 Uiso 1 1 calc R U . . .
C77 C 0.9410(8) 0.7206(4) 0.7473(3) 0.032(2) Uani 1 1 d . . . . .
H77 H 1.0068 0.7489 0.7434 0.038 Uiso 1 1 calc R U . . .
C78 C 0.9447(7) 0.6889(4) 0.7887(3) 0.0301(19) Uani 1 1 d . . . . .
H78 H 1.0118 0.6966 0.8137 0.036 Uiso 1 1 calc R U . . .
C79 C 0.8467(7) 0.6438(4) 0.7943(3) 0.0257(18) Uani 1 1 d . . . . .
C80 C 0.7431(8) 0.6329(4) 0.7567(3) 0.031(2) Uani 1 1 d . . . . .
C81 C 0.6467(8) 0.5869(4) 0.7629(3) 0.033(2) Uani 1 1 d . . . . .
H81 H 0.5788 0.5787 0.7384 0.040 Uiso 1 1 calc R U . . .
C82 C 0.6540(8) 0.5546(4) 0.8053(3) 0.033(2) Uani 1 1 d . . . . .
H82 H 0.5907 0.5243 0.8088 0.039 Uiso 1 1 calc R U . . .
C83 C 0.7542(8) 0.5661(4) 0.8433(3) 0.031(2) Uani 1 1 d . . . . .
H83 H 0.7573 0.5437 0.8716 0.038 Uiso 1 1 calc R U . . .
C84 C 0.8487(7) 0.6112(4) 0.8382(3) 0.0298(19) Uani 1 1 d . . . . .
C85 C 0.9487(7) 0.6132(4) 0.9212(3) 0.0299(19) Uani 1 1 d . . . . .
H85A H 0.9572 0.5664 0.9272 0.036 Uiso 1 1 calc R U . . .
H85B H 0.8719 0.6260 0.9291 0.036 Uiso 1 1 calc R U . . .
C86 C 1.0537(7) 0.6542(4) 0.9506(3) 0.035(2) Uani 1 1 d . . . . .
H86A H 1.0475 0.7006 0.9430 0.042 Uiso 1 1 calc R U . . .
H86B H 1.0526 0.6504 0.9845 0.042 Uiso 1 1 calc R U . . .
C87 C 1.2682(7) 0.6739(4) 0.9617(3) 0.0289(19) Uani 1 1 d . . . . .
H87A H 1.2622 0.6872 0.9943 0.035 Uiso 1 1 calc R U . . .
H87B H 1.2710 0.7137 0.9435 0.035 Uiso 1 1 calc R U . . .
C88 C 1.3822(7) 0.6375(4) 0.9620(3) 0.0294(19) Uani 1 1 d . . . . .
H88A H 1.4530 0.6640 0.9793 0.035 Uiso 1 1 calc R U . . .
H88B H 1.3767 0.5957 0.9777 0.035 Uiso 1 1 calc R U . . .
C89 C 1.5052(7) 0.5971(4) 0.9087(3) 0.036(2) Uani 1 1 d . . . . .
H89A H 1.5730 0.6245 0.9273 0.043 Uiso 1 1 calc R U . . .
H89B H 1.5134 0.5978 0.8752 0.043 Uiso 1 1 calc R U . . .
C90 C 1.5149(7) 0.5278(4) 0.9246(3) 0.0270(18) Uani 1 1 d . . . . .
H90A H 1.5880 0.5096 0.9168 0.032 Uiso 1 1 calc R U . . .
H90B H 1.5204 0.5271 0.9591 0.032 Uiso 1 1 calc R U . . .
C91 C 1.4304(8) 0.4209(4) 0.8986(3) 0.039(2) Uani 1 1 d . . . . .
H91A H 1.3533 0.3959 0.8981 0.047 Uiso 1 1 calc R U . . .
H91B H 1.4871 0.4097 0.9272 0.047 Uiso 1 1 calc R U . . .
C92 C 1.4795(8) 0.4005(4) 0.8559(3) 0.040(2) Uani 1 1 d . . . . .
H92A H 1.5654 0.4154 0.8607 0.048 Uiso 1 1 calc R U . . .
H92B H 1.4743 0.3523 0.8525 0.048 Uiso 1 1 calc R U . . .
C93 C 1.3103(8) 0.3949(4) 0.7896(3) 0.032(2) Uani 1 1 d . . . . .
C94 C 1.2472(7) 0.3438(4) 0.8079(3) 0.032(2) Uani 1 1 d . . . . .
H94 H 1.2775 0.3276 0.8379 0.039 Uiso 1 1 calc R U . . .
C95 C 1.1354(8) 0.3168(4) 0.7798(3) 0.034(2) Uani 1 1 d . . . . .
H95 H 1.0918 0.2837 0.7928 0.041 Uiso 1 1 calc R U . . .
C96 C 1.0889(8) 0.3360(4) 0.7358(3) 0.032(2) Uani 1 1 d . . . . .
H96 H 1.0155 0.3162 0.7188 0.038 Uiso 1 1 calc R U . . .
C97 C 1.1535(8) 0.3878(4) 0.7149(3) 0.0303(19) Uani 1 1 d . . . . .
C98 C 1.2611(7) 0.4192(4) 0.7422(3) 0.033(2) Uani 1 1 d . . . . .
C99 C 1.3238(8) 0.4710(4) 0.7224(3) 0.037(2) Uani 1 1 d . . . . .
H99 H 1.3931 0.4929 0.7409 0.044 Uiso 1 1 calc R U . . .
C100 C 1.2838(9) 0.4890(4) 0.6763(3) 0.045(2) Uani 1 1 d . . . . .
H100 H 1.3256 0.5230 0.6635 0.054 Uiso 1 1 calc R U . . .
C101 C 1.1782(9) 0.4554(5) 0.6483(3) 0.044(2) Uani 1 1 d . . . . .
H101 H 1.1515 0.4666 0.6166 0.053 Uiso 1 1 calc R U . . .
C102 C 1.1160(8) 0.4070(4) 0.6674(4) 0.038(2) Uani 1 1 d . . . . .
C103 C 0.9934(8) 0.3739(5) 0.5912(3) 0.051(3) Uani 1 1 d . . . . .
H10A H 1.0622 0.3557 0.5798 0.061 Uiso 1 1 calc R U . . .
H10B H 0.9873 0.4195 0.5815 0.061 Uiso 1 1 calc R U . . .
C104 C 0.8777(9) 0.3339(5) 0.5699(3) 0.046(2) Uani 1 1 d . . . . .
H10C H 0.8722 0.3270 0.5355 0.055 Uiso 1 1 calc R U . . .
H10D H 0.8774 0.2907 0.5841 0.055 Uiso 1 1 calc R U . . .
C105 C 0.6625(9) 0.3386(4) 0.5538(3) 0.045(3) Uani 1 1 d . . . . .
H10E H 0.6541 0.2925 0.5621 0.055 Uiso 1 1 calc R U . . .
H10F H 0.6591 0.3397 0.5194 0.055 Uiso 1 1 calc R U . . .
C106 C 0.5629(10) 0.3744(6) 0.5666(5) 0.076(4) Uani 1 1 d . . . . .
H10G H 0.4895 0.3621 0.5429 0.091 Uiso 1 1 calc R U . . .
H10H H 0.5488 0.3592 0.5973 0.091 Uiso 1 1 calc R U . . .
C107 C 0.4791(11) 0.4623(8) 0.5915(6) 0.123(7) Uani 1 1 d . . . . .
H10I H 0.5001 0.4619 0.6262 0.147 Uiso 1 1 calc R U . . .
H10J H 0.4028 0.4361 0.5805 0.147 Uiso 1 1 calc R U . . .
C108 C 0.4695(11) 0.5318(7) 0.5749(6) 0.099(5) Uani 1 1 d . . . . .
H10K H 0.4704 0.5320 0.5408 0.119 Uiso 1 1 calc R U . . .
H10L H 0.3925 0.5485 0.5799 0.119 Uiso 1 1 calc R U . . .
C109 C 0.5428(9) 0.6405(6) 0.6004(4) 0.061(3) Uani 1 1 d . . . . .
H10M H 0.4650 0.6459 0.6103 0.073 Uiso 1 1 calc R U . . .
H10N H 0.5368 0.6566 0.5682 0.073 Uiso 1 1 calc R U . . .
C110 C 0.6417(9) 0.6796(5) 0.6339(3) 0.053(3) Uani 1 1 d . . . . .
H11A H 0.7208 0.6727 0.6255 0.063 Uiso 1 1 calc R U . . .
H11B H 0.6277 0.7267 0.6328 0.063 Uiso 1 1 calc R U . . .
C111 C 0.8383(12) 0.8928(5) 0.0548(4) 0.072(4) Uani 1 1 d . . . . .
H111 H 0.9158 0.8706 0.0608 0.086 Uiso 1 1 calc R U . . .
C112 C 0.3948(15) 0.9627(6) 0.0748(5) 0.118(7) Uani 1 1 d . . . . .
H11C H 0.3683 1.0047 0.0845 0.178 Uiso 1 1 calc R U . . .
H11D H 0.3246 0.9328 0.0634 0.178 Uiso 1 1 calc R U . . .
H11E H 0.4403 0.9690 0.0495 0.178 Uiso 1 1 calc R U . . .
C113 C 0.4994(13) 0.0264(7) 0.4190(6) 0.103(6) Uani 1 1 d D . . . .
H11F H 0.5129 0.0322 0.4534 0.155 Uiso 1 1 calc R U . . .
H11G H 0.4353 -0.0075 0.4085 0.155 Uiso 1 1 calc R U . . .
H11H H 0.4760 0.0675 0.4047 0.155 Uiso 1 1 calc R U . . .
C118 C 0.0826(7) 0.8472(4) 0.2931(3) 0.0303(19) Uani 1 1 d . . . . .
H11I H 0.1338 0.8162 0.2806 0.036 Uiso 1 1 calc R U . . .
H11J H 0.0032 0.8451 0.2718 0.036 Uiso 1 1 calc R U . . .
C119 C 0.0680(7) 0.8291(4) 0.3420(3) 0.0283(19) Uani 1 1 d . . . . .
H11K H 0.0226 0.8626 0.3551 0.034 Uiso 1 1 calc R U . . .
H11L H 0.0204 0.7871 0.3399 0.034 Uiso 1 1 calc R U . . .


_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
Cd1 Br3 2.5664(11) . ?
Cd1 Br1 2.5887(10) . ?
Cd1 Br4 2.6097(10) . ?
Cd1 Br2 2.6180(9) . ?
Cd2 Br8 2.5810(10) . ?
Cd2 Br7 2.5842(12) . ?
Cd2 Br5 2.5960(10) . ?
Cd2 Br6 2.5984(10) . ?
Cl1 C111 1.779(11) . ?
Cl2 C111 1.792(12) . ?
Cl3 C111 1.717(12) . ?
O1 C21 1.367(9) . ?
O1 C118 1.437(8) . ?
O2 C54 1.399(9) . ?
O2 C119 1.430(9) . ?
O3 C52 1.391(10) . ?
O3 C53 1.434(9) . ?
O4 C51 1.385(10) . ?
O4 C50 1.411(9) . ?
O5 C48 1.361(9) . ?
O5 C49 1.436(8) . ?
O6 C39 1.364(9) . ?
O6 C38 1.429(8) . ?
O7 C36 1.399(9) . ?
O7 C37 1.437(9) . ?
O8 C35 1.423(10) . ?
O8 C34 1.426(10) . ?
O9 C33 1.413(10) . ?
O9 C32 1.419(10) . ?
O10 C30 1.366(10) . ?
O10 C31 1.417(9) . ?
O11 C75 1.353(10) . ?
O11 C110 1.422(10) . ?
O12 C109 1.390(12) . ?
O12 C108 1.417(13) . ?
O13 C106 1.271(13) . ?
O13 C107 1.447(14) . ?
O14 C104 1.393(10) . ?
O14 C105 1.437(10) . ?
O15 C102 1.373(10) . ?
O15 C103 1.445(10) . ?
O16 C93 1.343(10) . ?
O16 C92 1.443(11) . ?
O17 C90 1.395(9) . ?
O17 C91 1.420(10) . ?
O18 C88 1.423(9) . ?
O18 C89 1.423(9) . ?
O19 C86 1.401(9) . ?
O19 C87 1.448(9) . ?
O20 C84 1.350(9) . ?
O20 C85 1.438(9) . ?
O21 C112 1.344(13) . ?
O22 C113 1.243(12) . ?
O24A C114 1.416(19) . ?
O24B C914 1.482(18) . ?
N1 C5 1.331(9) . ?
N1 C1 1.346(9) . ?
N2 C6 1.335(9) . ?
N2 C10 1.341(9) . ?
N2 C3 1.468(9) . ?
N3 C11 1.350(9) . ?
N3 C15 1.362(9) . ?
N3 C18 1.454(9) . ?
N4 C20 1.325(10) . ?
N4 C16 1.350(10) . ?
N5 C55 1.328(10) . ?
N5 C59 1.337(11) . ?
N6 C64 1.359(9) . ?
N6 C60 1.369(9) . ?
N6 C57 1.438(10) . ?
N7 C69 1.357(8) . ?
N7 C65 1.359(9) . ?
N7 C72 1.453(10) . ?
N8 C70 1.342(10) . ?
N8 C74 1.359(10) . ?
C1 C2 1.377(10) . ?
C2 C3 1.380(10) . ?
C3 C4 1.364(10) . ?
C4 C5 1.375(10) . ?
C6 C7 1.358(10) . ?
C7 C8 1.387(10) . ?
C8 C9 1.368(10) . ?
C8 C13 1.492(9) . ?
C9 C10 1.382(10) . ?
C11 C12 1.368(10) . ?
C12 C13 1.372(10) . ?
C13 C14 1.409(10) . ?
C14 C15 1.368(10) . ?
C16 C17 1.382(10) . ?
C17 C18 1.382(10) . ?
C18 C19 1.377(10) . ?
C19 C20 1.412(10) . ?
C21 C22 1.374(10) . ?
C21 C26 1.436(10) . ?
C22 C23 1.406(10) . ?
C23 C24 1.353(10) . ?
C24 C25 1.401(11) . ?
C25 C26 1.410(10) . ?
C25 C30 1.462(10) . ?
C26 C27 1.416(11) . ?
C27 C28 1.349(10) . ?
C28 C29 1.407(11) . ?
C29 C30 1.358(11) . ?
C31 C32 1.493(12) . ?
C33 C34 1.510(12) . ?
C35 C36 1.515(11) . ?
C37 C38 1.476(11) . ?
C39 C40 1.367(11) . ?
C39 C44 1.453(10) . ?
C40 C41 1.398(11) . ?
C41 C42 1.372(10) . ?
C42 C43 1.407(10) . ?
C43 C44 1.413(10) . ?
C43 C48 1.430(10) . ?
C44 C45 1.397(11) . ?
C45 C46 1.367(10) . ?
C46 C47 1.432(11) . ?
C47 C48 1.353(10) . ?
C49 C50 1.492(11) . ?
C51 C52 1.507(11) . ?
C53 C54 1.462(12) . ?
C55 C56 1.366(11) . ?
C56 C57 1.371(11) . ?
C57 C58 1.390(11) . ?
C58 C59 1.362(12) . ?
C60 C61 1.359(10) . ?
C61 C62 1.396(10) . ?
C62 C63 1.395(9) . ?
C62 C67 1.487(10) . ?
C63 C64 1.387(10) . ?
C65 C66 1.345(10) . ?
C66 C67 1.402(9) . ?
C67 C68 1.417(10) . ?
C68 C69 1.342(10) . ?
C70 C71 1.372(11) . ?
C71 C72 1.385(10) . ?
C72 C73 1.366(10) . ?
C73 C74 1.361(11) . ?
C75 C76 1.365(11) . ?
C75 C80 1.433(11) . ?
C76 C77 1.395(12) . ?
C77 C78 1.350(11) . ?
C78 C79 1.420(10) . ?
C79 C80 1.418(11) . ?
C79 C84 1.422(11) . ?
C80 C81 1.421(10) . ?
C81 C82 1.377(11) . ?
C82 C83 1.400(11) . ?
C83 C84 1.387(10) . ?
C85 C86 1.495(11) . ?
C87 C88 1.496(11) . ?
C89 C90 1.486(11) . ?
C91 C92 1.475(12) . ?
C93 C94 1.387(10) . ?
C93 C98 1.462(12) . ?
C94 C95 1.416(11) . ?
C95 C96 1.334(12) . ?
C96 C97 1.444(11) . ?
C97 C102 1.404(12) . ?
C97 C98 1.405(11) . ?
C98 C99 1.415(11) . ?
C99 C100 1.364(12) . ?
C100 C101 1.416(13) . ?
C101 C102 1.354(12) . ?
C103 C104 1.498(13) . ?
C105 C106 1.448(14) . ?
C107 C108 1.49(2) . ?
C109 C110 1.485(13) . ?
C118 C119 1.481(10) . ?

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
Br3 Cd1 Br1 109.78(4) . . ?
Br3 Cd1 Br4 107.53(3) . . ?
Br1 Cd1 Br4 110.65(3) . . ?
Br3 Cd1 Br2 116.18(3) . . ?
Br1 Cd1 Br2 102.99(3) . . ?
Br4 Cd1 Br2 109.66(3) . . ?
Br8 Cd2 Br7 113.44(4) . . ?
Br8 Cd2 Br5 107.64(4) . . ?
Br7 Cd2 Br5 108.06(4) . . ?
Br8 Cd2 Br6 109.44(4) . . ?
Br7 Cd2 Br6 113.79(4) . . ?
Br5 Cd2 Br6 103.84(3) . . ?
C21 O1 C118 117.5(6) . . ?
C54 O2 C119 115.6(6) . . ?
C52 O3 C53 111.5(6) . . ?
C51 O4 C50 115.8(6) . . ?
C48 O5 C49 117.5(6) . . ?
C39 O6 C38 116.5(6) . . ?
C36 O7 C37 111.7(6) . . ?
C35 O8 C34 112.4(6) . . ?
C33 O9 C32 110.8(6) . . ?
C30 O10 C31 115.8(7) . . ?
C75 O11 C110 115.6(7) . . ?
C109 O12 C108 113.1(9) . . ?
C106 O13 C107 108.2(11) . . ?
C104 O14 C105 113.0(7) . . ?
C102 O15 C103 115.4(7) . . ?
C93 O16 C92 118.3(7) . . ?
C90 O17 C91 112.9(6) . . ?
C88 O18 C89 113.3(6) . . ?
C86 O19 C87 111.8(6) . . ?
C84 O20 C85 119.1(6) . . ?
C5 N1 C1 117.4(6) . . ?
C6 N2 C10 120.6(6) . . ?
C6 N2 C3 121.2(6) . . ?
C10 N2 C3 118.2(6) . . ?
C11 N3 C15 119.8(6) . . ?
C11 N3 C18 120.2(6) . . ?
C15 N3 C18 119.9(7) . . ?
C20 N4 C16 117.3(7) . . ?
C55 N5 C59 116.9(8) . . ?
C64 N6 C60 120.1(7) . . ?
C64 N6 C57 121.4(6) . . ?
C60 N6 C57 118.5(6) . . ?
C69 N7 C65 120.6(7) . . ?
C69 N7 C72 120.4(6) . . ?
C65 N7 C72 118.9(6) . . ?
C70 N8 C74 115.6(7) . . ?
N1 C1 C2 124.1(7) . . ?
C1 C2 C3 116.4(7) . . ?
C4 C3 C2 120.8(7) . . ?
C4 C3 N2 120.3(6) . . ?
C2 C3 N2 118.9(7) . . ?
C3 C4 C5 118.7(7) . . ?
N1 C5 C4 122.5(7) . . ?
N2 C6 C7 120.5(7) . . ?
C6 C7 C8 120.2(7) . . ?
C9 C8 C7 118.5(7) . . ?
C9 C8 C13 119.8(7) . . ?
C7 C8 C13 121.6(7) . . ?
C8 C9 C10 119.3(7) . . ?
N2 C10 C9 120.6(7) . . ?
N3 C11 C12 120.2(7) . . ?
C11 C12 C13 121.7(8) . . ?
C12 C13 C14 117.4(7) . . ?
C12 C13 C8 121.9(7) . . ?
C14 C13 C8 120.7(7) . . ?
C15 C14 C13 119.5(7) . . ?
N3 C15 C14 121.2(7) . . ?
N4 C16 C17 123.2(8) . . ?
C16 C17 C18 118.2(8) . . ?
C19 C18 C17 120.5(7) . . ?
C19 C18 N3 120.0(7) . . ?
C17 C18 N3 119.5(7) . . ?
C18 C19 C20 116.8(7) . . ?
N4 C20 C19 124.0(8) . . ?
O1 C21 C22 125.3(7) . . ?
O1 C21 C26 113.9(7) . . ?
C22 C21 C26 120.8(7) . . ?
C21 C22 C23 119.8(7) . . ?
C24 C23 C22 121.5(8) . . ?
C23 C24 C25 119.3(8) . . ?
C24 C25 C26 121.9(7) . . ?
C24 C25 C30 120.8(7) . . ?
C26 C25 C30 117.4(7) . . ?
C25 C26 C27 120.7(7) . . ?
C25 C26 C21 116.6(7) . . ?
C27 C26 C21 122.7(7) . . ?
C28 C27 C26 119.9(8) . . ?
C27 C28 C29 121.2(8) . . ?
C30 C29 C28 121.1(8) . . ?
C29 C30 O10 126.7(7) . . ?
C29 C30 C25 119.6(8) . . ?
O10 C30 C25 113.7(7) . . ?
O10 C31 C32 107.6(8) . . ?
O9 C32 C31 109.1(7) . . ?
O9 C33 C34 108.6(7) . . ?
O8 C34 C33 109.3(7) . . ?
O8 C35 C36 108.8(7) . . ?
O7 C36 C35 108.8(7) . . ?
O7 C37 C38 109.8(6) . . ?
O6 C38 C37 108.2(7) . . ?
C40 C39 O6 125.7(7) . . ?
C40 C39 C44 120.1(8) . . ?
O6 C39 C44 114.1(7) . . ?
C39 C40 C41 121.0(7) . . ?
C42 C41 C40 120.1(8) . . ?
C41 C42 C43 121.0(8) . . ?
C42 C43 C44 119.8(7) . . ?
C42 C43 C48 122.7(7) . . ?
C44 C43 C48 117.4(7) . . ?
C45 C44 C43 120.7(7) . . ?
C45 C44 C39 121.5(7) . . ?
C43 C44 C39 117.8(7) . . ?
C46 C45 C44 121.1(8) . . ?
C45 C46 C47 118.9(8) . . ?
C48 C47 C46 120.9(7) . . ?
C47 C48 O5 125.1(7) . . ?
C47 C48 C43 121.0(7) . . ?
O5 C48 C43 113.9(7) . . ?
O5 C49 C50 108.8(6) . . ?
O4 C50 C49 114.0(7) . . ?
O4 C51 C52 110.4(7) . . ?
O3 C52 C51 109.5(7) . . ?
O3 C53 C54 109.8(7) . . ?
O2 C54 C53 110.9(7) . . ?
N5 C55 C56 123.9(8) . . ?
C55 C56 C57 118.0(8) . . ?
C56 C57 C58 119.8(8) . . ?
C56 C57 N6 120.5(7) . . ?
C58 C57 N6 119.7(7) . . ?
C59 C58 C57 117.3(8) . . ?
N5 C59 C58 124.1(8) . . ?
C61 C60 N6 120.0(7) . . ?
C60 C61 C62 121.8(7) . . ?
C63 C62 C61 117.2(7) . . ?
C63 C62 C67 121.3(7) . . ?
C61 C62 C67 121.5(6) . . ?
C64 C63 C62 120.3(7) . . ?
N6 C64 C63 120.5(7) . . ?
C66 C65 N7 120.6(7) . . ?
C65 C66 C67 120.8(7) . . ?
C66 C67 C68 116.6(7) . . ?
C66 C67 C62 120.7(7) . . ?
C68 C67 C62 122.7(6) . . ?
C69 C68 C67 120.9(7) . . ?
C68 C69 N7 120.3(7) . . ?
N8 C70 C71 124.4(8) . . ?
C70 C71 C72 117.5(7) . . ?
C73 C72 C71 120.1(8) . . ?
C73 C72 N7 120.0(7) . . ?
C71 C72 N7 119.8(7) . . ?
C74 C73 C72 118.3(8) . . ?
N8 C74 C73 124.1(8) . . ?
O11 C75 C76 126.8(8) . . ?
O11 C75 C80 113.7(7) . . ?
C76 C75 C80 119.5(8) . . ?
C75 C76 C77 122.1(8) . . ?
C78 C77 C76 120.1(8) . . ?
C77 C78 C79 120.3(8) . . ?
C78 C79 C80 120.0(7) . . ?
C78 C79 C84 120.7(7) . . ?
C80 C79 C84 119.2(7) . . ?
C81 C80 C79 119.1(8) . . ?
C81 C80 C75 123.0(8) . . ?
C79 C80 C75 117.9(7) . . ?
C82 C81 C80 119.9(8) . . ?
C81 C82 C83 121.8(7) . . ?
C84 C83 C82 119.3(8) . . ?
O20 C84 C83 124.8(8) . . ?
O20 C84 C79 114.4(7) . . ?
C83 C84 C79 120.7(8) . . ?
O20 C85 C86 106.8(6) . . ?
O19 C86 C85 108.1(7) . . ?
O19 C87 C88 109.3(6) . . ?
O18 C88 C87 107.6(6) . . ?
O18 C89 C90 114.3(6) . . ?
O17 C90 C89 108.5(7) . . ?
O17 C91 C92 113.2(7) . . ?
O16 C92 C91 113.1(7) . . ?
O16 C93 C94 125.8(8) . . ?
O16 C93 C98 114.4(7) . . ?
C94 C93 C98 119.7(8) . . ?
C93 C94 C95 118.4(9) . . ?
C96 C95 C94 123.9(8) . . ?
C95 C96 C97 119.5(8) . . ?
C102 C97 C98 118.0(8) . . ?
C102 C97 C96 122.8(8) . . ?
C98 C97 C96 119.1(8) . . ?
C97 C98 C99 119.6(8) . . ?
C97 C98 C93 119.1(7) . . ?
C99 C98 C93 121.1(8) . . ?
C100 C99 C98 120.8(9) . . ?
C99 C100 C101 119.3(8) . . ?
C102 C101 C100 120.1(9) . . ?
C101 C102 O15 124.2(9) . . ?
C101 C102 C97 122.0(9) . . ?
O15 C102 C97 113.8(8) . . ?
O15 C103 C104 109.0(8) . . ?
O14 C104 C103 108.8(8) . . ?
O14 C105 C106 110.2(8) . . ?
O13 C106 C105 117.3(10) . . ?
O13 C107 C108 103.5(14) . . ?
O12 C108 C107 110.6(11) . . ?
O12 C109 C110 109.7(8) . . ?
O11 C110 C109 105.9(9) . . ?
Cl3 C111 Cl1 111.2(7) . . ?
Cl3 C111 Cl2 109.8(7) . . ?
Cl1 C111 Cl2 109.9(6) . . ?
O1 C118 C119 108.5(6) . . ?
O2 C119 C118 113.1(6) . . ?

_refine_diff_density_max         2.811
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.178
_database_code_depnum_ccdc_archive 'CCDC 997299'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3[CdBr4]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H56 Br4 Cd N4 O10'
_chemical_formula_weight         1281.01

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

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

_cell_length_a                   18.9050(2)
_cell_length_b                   17.30640(10)
_cell_length_c                   31.5699(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10328.96(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.77

_exptl_crystal_description       fragment
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5120
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6631
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            171593
_diffrn_reflns_av_R_equivalents  0.1033
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.29
_diffrn_reflns_theta_max         30.54
_reflns_number_total             15776
_reflns_number_gt                9854
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0292P)²+9.8326P] 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         15776
_refine_ls_number_parameters     631
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.002
_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
Cd1 Cd 0.436465(12) 0.666656(12) 0.631070(7) 0.02092(6) Uani 1 1 d . . .
Br1 Br 0.349196(19) 0.700792(18) 0.692474(11) 0.02819(8) Uani 1 1 d . . .
Br2 Br 0.37123(2) 0.608054(18) 0.565771(11) 0.02931(9) Uani 1 1 d . . .
Br3 Br 0.512555(18) 0.564129(19) 0.668687(11) 0.02915(8) Uani 1 1 d . . .
Br4 Br 0.496038(19) 0.786142(19) 0.598348(11) 0.02997(8) Uani 1 1 d . . .
O1 O 0.04914(12) 0.80318(13) 0.66045(7) 0.0272(5) Uani 1 1 d . . .
O2 O 0.07258(12) 0.79369(13) 0.74774(7) 0.0298(5) Uani 1 1 d . . .
O3 O 0.18910(12) 0.76649(13) 0.80450(7) 0.0295(6) Uani 1 1 d . . .
O4 O 0.31264(12) 0.84119(13) 0.83144(7) 0.0279(5) Uani 1 1 d . . .
O5 O 0.35531(12) 0.94948(14) 0.76663(7) 0.0301(6) Uani 1 1 d . . .
O6 O 0.38517(12) 1.05365(14) 0.60191(8) 0.0354(6) Uani 1 1 d . . .
O7 O 0.3785(2) 1.0755(3) 0.51612(14) 0.0217(10) Uani 0.50 1 d PD A 1
C43 C 0.3864(4) 1.1089(4) 0.4751(2) 0.0257(15) Uani 0.50 1 d PD A 1
H43A H 0.4069 1.0716 0.4557 0.031 Uiso 0.50 1 calc PR A 1
H43B H 0.4174 1.1535 0.4765 0.031 Uiso 0.50 1 calc PR A 1
C44 C 0.3138(6) 1.1329(5) 0.4599(4) 0.037(3) Uani 0.50 1 d PD A 1
H44A H 0.2917 1.1679 0.4799 0.044 Uiso 0.50 1 calc PR A 1
H44B H 0.3168 1.1584 0.4325 0.044 Uiso 0.50 1 calc PR A 1
O107 O 0.4066(3) 1.0258(4) 0.50469(16) 0.0438(15) Uani 0.50 1 d PD A 2
C143 C 0.4069(4) 1.0566(6) 0.4628(3) 0.046(2) Uani 0.50 1 d PD A 2
H14A H 0.4058 1.0145 0.4426 0.055 Uiso 0.50 1 calc PR A 2
H14B H 0.4505 1.0852 0.4584 0.055 Uiso 0.50 1 calc PR A 2
C144 C 0.3441(6) 1.1098(5) 0.4550(3) 0.044(3) Uani 0.50 1 d PD A 2
H14C H 0.3436 1.1504 0.4762 0.053 Uiso 0.50 1 calc PR A 2
H14D H 0.3489 1.1339 0.4274 0.053 Uiso 0.50 1 calc PR A 2
O8 O 0.27609(14) 1.06580(14) 0.45680(8) 0.0406(7) Uani 1 1 d D . .
O9 O 0.17694(16) 0.9640(2) 0.42980(10) 0.0652(9) Uani 1 1 d . A .
O10 O 0.13822(17) 0.8580(2) 0.49631(9) 0.0631(10) Uani 1 1 d . . .
N1 N 0.09818(16) 1.02351(17) 0.85075(9) 0.0324(7) Uani 1 1 d . . .
N2 N 0.16905(13) 0.95068(14) 0.73011(8) 0.0174(5) Uani 1 1 d . . .
N3 N 0.31083(13) 0.85668(14) 0.53153(8) 0.0179(5) Uani 1 1 d . . .
N4 N 0.40113(17) 0.79465(16) 0.41379(9) 0.0321(7) Uani 1 1 d . . .
C1 C 0.1592(2) 0.9855(2) 0.84570(11) 0.0355(9) Uani 1 1 d . . .
H1 H 0.1862 0.9755 0.8697 0.043 Uiso 1 1 calc R . .
C2 C 0.18502(19) 0.96023(19) 0.80712(10) 0.0286(8) Uani 1 1 d . . .
H2 H 0.2280 0.9342 0.8051 0.034 Uiso 1 1 calc R . .
C3 C 0.14447(16) 0.97508(17) 0.77161(10) 0.0205(7) Uani 1 1 d . . .
C4 C 0.08139(17) 1.01387(18) 0.77551(11) 0.0249(7) Uani 1 1 d . . .
H4 H 0.0533 1.0243 0.7520 0.030 Uiso 1 1 calc R . .
C5 C 0.06124(19) 1.03671(19) 0.81559(11) 0.0295(8) Uani 1 1 d . . .
H5 H 0.0187 1.0633 0.8182 0.035 Uiso 1 1 calc R . .
C6 C 0.20523(16) 0.88425(17) 0.72534(10) 0.0203(7) Uani 1 1 d . . .
H6 H 0.2118 0.8517 0.7484 0.024 Uiso 1 1 calc R . .
C7 C 0.23224(17) 0.86448(17) 0.68674(10) 0.0213(7) Uani 1 1 d . . .
H7 H 0.2583 0.8192 0.6839 0.026 Uiso 1 1 calc R . .
C8 C 0.22107(16) 0.91164(16) 0.65133(10) 0.0177(6) Uani 1 1 d . . .
C9 C 0.18111(17) 0.97822(17) 0.65727(10) 0.0216(7) Uani 1 1 d . . .
H9 H 0.1712 1.0101 0.6343 0.026 Uiso 1 1 calc R . .
C10 C 0.15632(17) 0.99722(18) 0.69651(10) 0.0227(7) Uani 1 1 d . . .
H10 H 0.1305 1.0425 0.7002 0.027 Uiso 1 1 calc R . .
C11 C 0.30764(17) 0.80276(17) 0.56251(10) 0.0221(7) Uani 1 1 d . . .
H11 H 0.3253 0.7535 0.5574 0.027 Uiso 1 1 calc R . .
C12 C 0.27913(16) 0.81934(17) 0.60103(10) 0.0209(7) Uani 1 1 d . . .
H12 H 0.2776 0.7814 0.6219 0.025 Uiso 1 1 calc R . .
C13 C 0.25218(16) 0.89277(16) 0.60946(9) 0.0173(6) Uani 1 1 d . . .
C14 C 0.25515(17) 0.94679(17) 0.57680(10) 0.0210(7) Uani 1 1 d . . .
H14 H 0.2371 0.9961 0.5812 0.025 Uiso 1 1 calc R . .
C15 C 0.28422(17) 0.92844(17) 0.53849(10) 0.0218(7) Uani 1 1 d . . .
H15 H 0.2858 0.9653 0.5171 0.026 Uiso 1 1 calc R . .
C16 C 0.42595(18) 0.7677(2) 0.45049(11) 0.0303(8) Uani 1 1 d . . .
H16 H 0.4639 0.7336 0.4495 0.036 Uiso 1 1 calc R . .
C17 C 0.39924(17) 0.78684(19) 0.48989(10) 0.0252(7) Uani 1 1 d . . .
H17 H 0.4187 0.7667 0.5146 0.030 Uiso 1 1 calc R . .
C18 C 0.34279(17) 0.83673(17) 0.49109(10) 0.0213(7) Uani 1 1 d . . .
C19 C 0.31421(19) 0.86596(19) 0.45458(10) 0.0281(8) Uani 1 1 d . . .
H19 H 0.2756 0.8992 0.4550 0.034 Uiso 1 1 calc R . .
C20 C 0.3463(2) 0.8429(2) 0.41663(11) 0.0346(9) Uani 1 1 d . . .
H20 H 0.3281 0.8628 0.3915 0.042 Uiso 1 1 calc R . .
C21 C 0.07033(18) 0.81241(19) 0.61958(11) 0.0265(7) Uani 1 1 d . . .
C22 C 0.0548(2) 0.8833(2) 0.60127(11) 0.0326(8) Uani 1 1 d . . .
H22 H 0.0302 0.9204 0.6166 0.039 Uiso 1 1 calc R . .
C23 C 0.0760(2) 0.8989(2) 0.56019(12) 0.0440(11) Uani 1 1 d . . .
H23 H 0.0662 0.9467 0.5482 0.053 Uiso 1 1 calc R . .
C24 C 0.1116(2) 0.8435(3) 0.53700(12) 0.0452(11) Uani 1 1 d . . .
C25 C 0.1261(2) 0.7740(3) 0.55469(13) 0.0448(11) Uani 1 1 d . . .
H25 H 0.1498 0.7368 0.5389 0.054 Uiso 1 1 calc R . .
C26 C 0.10620(18) 0.7573(2) 0.59613(12) 0.0349(9) Uani 1 1 d . . .
H26 H 0.1169 0.7095 0.6080 0.042 Uiso 1 1 calc R . .
C27 C 0.0676(2) 0.73238(19) 0.68058(12) 0.0341(9) Uani 1 1 d . . .
H27A H 0.1186 0.7264 0.6808 0.041 Uiso 1 1 calc R . .
H27B H 0.0475 0.6893 0.6651 0.041 Uiso 1 1 calc R . .
C28 C 0.0402(2) 0.7328(2) 0.72461(12) 0.0355(9) Uani 1 1 d . . .
H28A H -0.0106 0.7399 0.7243 0.043 Uiso 1 1 calc R . .
H28B H 0.0505 0.6837 0.7381 0.043 Uiso 1 1 calc R . .
C29 C 0.06589(19) 0.7844(2) 0.79244(11) 0.0334(8) Uani 1 1 d . . .
H29A H 0.0195 0.7633 0.7987 0.040 Uiso 1 1 calc R . .
H29B H 0.0691 0.8348 0.8058 0.040 Uiso 1 1 calc R . .
C30 C 0.12126(18) 0.7325(2) 0.81102(12) 0.0334(9) Uani 1 1 d . . .
H30A H 0.1128 0.7257 0.8411 0.040 Uiso 1 1 calc R . .
H30B H 0.1194 0.6822 0.7975 0.040 Uiso 1 1 calc R . .
C31 C 0.24209(18) 0.7281(2) 0.82814(11) 0.0301(8) Uani 1 1 d . . .
H31A H 0.2423 0.6735 0.8212 0.036 Uiso 1 1 calc R . .
H31B H 0.2326 0.7335 0.8582 0.036 Uiso 1 1 calc R . .
C32 C 0.31238(17) 0.76303(19) 0.81771(11) 0.0279(8) Uani 1 1 d . . .
H32A H 0.3498 0.7346 0.8318 0.033 Uiso 1 1 calc R . .
H32B H 0.3206 0.7606 0.7874 0.033 Uiso 1 1 calc R . .
C33 C 0.38056(19) 0.8765(2) 0.82849(11) 0.0333(8) Uani 1 1 d . . .
H33A H 0.4154 0.8431 0.8417 0.040 Uiso 1 1 calc R . .
H33B H 0.3800 0.9249 0.8440 0.040 Uiso 1 1 calc R . .
C34 C 0.40212(18) 0.8920(2) 0.78349(11) 0.0316(8) Uani 1 1 d . . .
H34A H 0.4506 0.9103 0.7825 0.038 Uiso 1 1 calc R . .
H34B H 0.3989 0.8449 0.7669 0.038 Uiso 1 1 calc R . .
C35 C 0.36586(17) 0.97125(19) 0.72515(11) 0.0260(7) Uani 1 1 d . . .
C36 C 0.33156(18) 1.03778(19) 0.71215(12) 0.0282(8) Uani 1 1 d . . .
H36 H 0.3042 1.0655 0.7313 0.034 Uiso 1 1 calc R . .
C37 C 0.33764(18) 1.06316(19) 0.67099(12) 0.0302(8) Uani 1 1 d . . .
H37 H 0.3136 1.1074 0.6624 0.036 Uiso 1 1 calc R . .
C38 C 0.37947(17) 1.02308(19) 0.64204(11) 0.0271(8) Uani 1 1 d . . .
C39 C 0.41240(17) 0.95572(19) 0.65478(11) 0.0261(7) Uani 1 1 d . . .
H39 H 0.4390 0.9274 0.6355 0.031 Uiso 1 1 calc R . .
C40 C 0.40589(17) 0.93004(19) 0.69642(11) 0.0261(7) Uani 1 1 d . . .
H40 H 0.4286 0.8850 0.7049 0.031 Uiso 1 1 calc R . .
C41 C 0.4423(2) 1.0256(2) 0.57661(11) 0.0336(8) Uani 1 1 d . A .
H41A H 0.4348 0.9716 0.5699 0.040 Uiso 1 1 calc R . .
H41B H 0.4864 1.0302 0.5921 0.040 Uiso 1 1 calc R . .
C42 C 0.4462(2) 1.0722(2) 0.53650(11) 0.0369(9) Uani 1 1 d D . .
H42A H 0.4620 1.1242 0.5430 0.044 Uiso 1 1 calc R A 1
H42B H 0.4804 1.0490 0.5175 0.044 Uiso 1 1 calc R A 1
C45 C 0.2107(3) 1.0919(3) 0.43955(14) 0.0620(15) Uani 1 1 d . A .
H45A H 0.2158 1.1011 0.4094 0.074 Uiso 1 1 calc R . .
H45B H 0.1967 1.1400 0.4530 0.074 Uiso 1 1 calc R . .
C46 C 0.1561(3) 1.0317(4) 0.44712(16) 0.080(2) Uani 1 1 d . . .
H46A H 0.1489 1.0252 0.4773 0.096 Uiso 1 1 calc R A .
H46B H 0.1115 1.0478 0.4346 0.096 Uiso 1 1 calc R . .
C47 C 0.1243(3) 0.9026(4) 0.42639(16) 0.102(3) Uani 1 1 d . . .
H47A H 0.1474 0.8563 0.4160 0.123 Uiso 1 1 calc R A .
H47B H 0.0892 0.9179 0.4056 0.123 Uiso 1 1 calc R . .
C48 C 0.0871(3) 0.8835(5) 0.46721(15) 0.107(3) Uani 1 1 d . A .
H48A H 0.0631 0.9289 0.4781 0.128 Uiso 1 1 calc R . .
H48B H 0.0522 0.8434 0.4625 0.128 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 Br4 2.5713(4) . ?
Cd1 Br3 2.5745(4) . ?
Cd1 Br2 2.6075(4) . ?
Cd1 Br1 2.6132(4) . ?
O1 C21 1.360(4) . ?
O1 C27 1.424(4) . ?
O2 C28 1.421(4) . ?
O2 C29 1.426(4) . ?
O3 C31 1.414(4) . ?
O3 C30 1.426(4) . ?
O4 C32 1.420(4) . ?
O4 C33 1.425(4) . ?
O5 C35 1.377(4) . ?
O5 C34 1.434(4) . ?
O6 C38 1.377(4) . ?
O6 C41 1.428(4) . ?
O7 C43 1.425(7) . ?
O7 C42 1.433(5) . ?
C43 C44 1.514(11) . ?
C44 O8 1.366(10) . ?
O107 C143 1.425(8) . ?
O107 C42 1.488(6) . ?
C143 C144 1.524(12) . ?
C144 O8 1.496(10) . ?
O8 C45 1.424(5) . ?
O9 C46 1.353(7) . ?
O9 C47 1.459(6) . ?
O10 C48 1.404(6) . ?
O10 C24 1.403(5) . ?
N1 C5 1.331(4) . ?
N1 C1 1.338(4) . ?
N2 C6 1.346(4) . ?
N2 C10 1.354(4) . ?
N2 C3 1.453(4) . ?
N3 C11 1.353(4) . ?
N3 C15 1.358(4) . ?
N3 C18 1.454(4) . ?
N4 C20 1.334(5) . ?
N4 C16 1.334(4) . ?
C1 C2 1.383(5) . ?
C2 C3 1.382(4) . ?
C3 C4 1.374(4) . ?
C4 C5 1.379(4) . ?
C6 C7 1.365(4) . ?
C7 C8 1.400(4) . ?
C8 C9 1.391(4) . ?
C8 C13 1.483(4) . ?
C9 C10 1.365(4) . ?
C11 C12 1.361(4) . ?
C12 C13 1.395(4) . ?
C13 C14 1.393(4) . ?
C14 C15 1.366(4) . ?
C16 C17 1.383(4) . ?
C17 C18 1.373(4) . ?
C18 C19 1.370(4) . ?
C19 C20 1.401(5) . ?
C21 C26 1.385(5) . ?
C21 C22 1.387(5) . ?
C22 C23 1.384(5) . ?
C23 C24 1.381(6) . ?
C24 C25 1.354(6) . ?
C25 C26 1.392(5) . ?
C27 C28 1.483(5) . ?
C29 C30 1.499(5) . ?
C31 C32 1.496(5) . ?
C33 C34 1.502(5) . ?
C35 C40 1.380(5) . ?
C35 C36 1.384(5) . ?
C36 C37 1.376(5) . ?
C37 C38 1.394(5) . ?
C38 C39 1.382(5) . ?
C39 C40 1.393(4) . ?
C41 C42 1.503(5) . ?
C45 C46 1.487(7) . ?
C47 C48 1.505(7) . ?

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
Br4 Cd1 Br3 119.661(14) . . ?
Br4 Cd1 Br2 101.674(13) . . ?
Br3 Cd1 Br2 111.154(13) . . ?
Br4 Cd1 Br1 113.125(13) . . ?
Br3 Cd1 Br1 99.577(13) . . ?
Br2 Cd1 Br1 112.075(14) . . ?
C21 O1 C27 116.9(3) . . ?
C28 O2 C29 112.8(3) . . ?
C31 O3 C30 111.6(2) . . ?
C32 O4 C33 113.1(3) . . ?
C35 O5 C34 117.0(3) . . ?
C38 O6 C41 116.3(3) . . ?
C43 O7 C42 109.3(5) . . ?
O7 C43 C44 107.8(7) . . ?
O8 C44 C43 105.2(6) . . ?
C143 O107 C42 114.9(5) . . ?
O107 C143 C144 112.0(8) . . ?
O8 C144 C143 110.8(6) . . ?
C44 O8 C45 102.1(5) . . ?
C44 O8 C144 28.5(4) . . ?
C45 O8 C144 124.7(5) . . ?
C46 O9 C47 117.5(5) . . ?
C48 O10 C24 114.1(4) . . ?
C5 N1 C1 115.9(3) . . ?
C6 N2 C10 120.7(3) . . ?
C6 N2 C3 120.8(2) . . ?
C10 N2 C3 118.5(2) . . ?
C11 N3 C15 119.8(3) . . ?
C11 N3 C18 119.3(2) . . ?
C15 N3 C18 120.9(3) . . ?
C20 N4 C16 115.7(3) . . ?
N1 C1 C2 124.4(3) . . ?
C1 C2 C3 117.4(3) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 N2 120.0(3) . . ?
C2 C3 N2 120.0(3) . . ?
C3 C4 C5 117.5(3) . . ?
N1 C5 C4 124.8(3) . . ?
N2 C6 C7 120.3(3) . . ?
C6 C7 C8 120.7(3) . . ?
C9 C8 C7 117.2(3) . . ?
C9 C8 C13 121.2(3) . . ?
C7 C8 C13 121.6(3) . . ?
C10 C9 C8 120.6(3) . . ?
N2 C10 C9 120.5(3) . . ?
N3 C11 C12 121.2(3) . . ?
C11 C12 C13 120.5(3) . . ?
C14 C13 C12 117.1(3) . . ?
C14 C13 C8 121.9(3) . . ?
C12 C13 C8 121.0(3) . . ?
C15 C14 C13 121.0(3) . . ?
N3 C15 C14 120.3(3) . . ?
N4 C16 C17 124.7(3) . . ?
C18 C17 C16 117.3(3) . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 N3 119.2(3) . . ?
C17 C18 N3 119.8(3) . . ?
C18 C19 C20 116.3(3) . . ?
N4 C20 C19 124.9(3) . . ?
O1 C21 C26 124.8(3) . . ?
O1 C21 C22 115.9(3) . . ?
C26 C21 C22 119.3(3) . . ?
C23 C22 C21 120.1(4) . . ?
C24 C23 C22 120.2(4) . . ?
C25 C24 C23 119.8(4) . . ?
C25 C24 O10 117.7(4) . . ?
C23 C24 O10 122.4(4) . . ?
C24 C25 C26 121.2(4) . . ?
C21 C26 C25 119.4(4) . . ?
O1 C27 C28 109.2(3) . . ?
O2 C28 C27 109.6(3) . . ?
O2 C29 C30 113.1(3) . . ?
O3 C30 C29 108.9(3) . . ?
O3 C31 C32 108.9(3) . . ?
O4 C32 C31 108.7(3) . . ?
O4 C33 C34 112.5(3) . . ?
O5 C34 C33 107.9(3) . . ?
O5 C35 C40 124.3(3) . . ?
O5 C35 C36 116.2(3) . . ?
C40 C35 C36 119.5(3) . . ?
C37 C36 C35 120.4(3) . . ?
C36 C37 C38 120.5(3) . . ?
O6 C38 C39 123.8(3) . . ?
O6 C38 C37 117.2(3) . . ?
C39 C38 C37 119.0(3) . . ?
C38 C39 C40 120.3(3) . . ?
C35 C40 C39 120.3(3) . . ?
O6 C41 C42 109.1(3) . . ?
O7 C42 O107 43.0(3) . . ?
O7 C42 C41 110.8(3) . . ?
O107 C42 C41 104.7(3) . . ?
O8 C45 C46 108.6(3) . . ?
O9 C46 C45 109.9(4) . . ?
O9 C47 C48 114.6(4) . . ?
O10 C48 C47 107.9(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.54
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.123
_database_code_depnum_ccdc_archive 'CCDC 997300'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2(CdI3)2+2CH3OH

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H68 Cd2 I6 N4 O12'
_chemical_formula_weight         1999.36

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'
Cd Cd -0.8075 1.2024 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3078(4)
_cell_length_b                   11.4735(4)
_cell_length_c                   15.1493(5)
_cell_angle_alpha                69.170(2)
_cell_angle_beta                 77.757(2)
_cell_angle_gamma                72.357(2)
_cell_volume                     1738.56(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9901
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      22.34

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_F_000             954
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.331
_shelx_estimated_absorpt_T_min   0.435
_shelx_estimated_absorpt_T_max   0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5616
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54912
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.448
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6440
_reflns_number_gt                4441
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0466P)²+1.4017P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6440
_refine_ls_number_parameters     368
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.82880(4) 0.54272(4) 0.36526(3) 0.05150(14) Uani 1 1 d . . . . .
I1 I 0.68112(4) 0.77937(4) 0.36657(3) 0.07261(15) Uani 1 1 d . . . . .
I2 I 1.08075(4) 0.47326(4) 0.35470(3) 0.07227(15) Uani 1 1 d . . . . .
I3 I 0.75077(4) 0.46254(4) 0.23841(3) 0.07535(16) Uani 1 1 d . . . . .
O1 O 0.9570(4) 0.0117(3) 0.8341(3) 0.0654(11) Uani 1 1 d . . . . .
O2 O 0.9977(4) -0.0262(4) 0.6500(3) 0.0597(10) Uani 1 1 d . . . . .
O3 O 0.7617(4) -0.0442(4) 0.6285(3) 0.0645(11) Uani 1 1 d . . . . .
O4 O 0.5724(4) -0.1760(5) 0.7087(3) 0.0810(13) Uani 1 1 d . . . . .
O5 O 0.6128(4) 0.2057(4) 1.1367(3) 0.0768(12) Uani 1 1 d . . . . .
N1 N 0.7546(4) 0.4129(4) 0.5134(3) 0.0459(10) Uani 1 1 d . . . . .
N2 N 0.6110(4) 0.1872(4) 0.7764(3) 0.0401(9) Uani 1 1 d . . . . .
C1 C 0.8226(5) 0.3012(5) 0.5606(3) 0.0480(13) Uani 1 1 d . . . . .
H1 H 0.9037 0.2728 0.5342 0.058 Uiso 1 1 calc R U . . .
C2 C 0.7802(5) 0.2235(5) 0.6473(3) 0.0468(13) Uani 1 1 d . . . . .
H2 H 0.8314 0.1454 0.6788 0.056 Uiso 1 1 calc R U . . .
C3 C 0.6607(5) 0.2651(4) 0.6854(3) 0.0413(12) Uani 1 1 d . . . . .
C4 C 0.5877(5) 0.3828(5) 0.6386(3) 0.0555(15) Uani 1 1 d . . . . .
H4 H 0.5066 0.4139 0.6638 0.067 Uiso 1 1 calc R U . . .
C5 C 0.6400(5) 0.4520(5) 0.5533(4) 0.0568(15) Uani 1 1 d . . . . .
H5 H 0.5917 0.5318 0.5213 0.068 Uiso 1 1 calc R U . . .
C6 C 0.6438(5) 0.0579(5) 0.7996(4) 0.0524(14) Uani 1 1 d . . . . .
H6 H 0.6962 0.0187 0.7564 0.063 Uiso 1 1 calc R U . . .
C7 C 0.6005(5) -0.0161(5) 0.8860(3) 0.0512(14) Uani 1 1 d . . . . .
H7 H 0.6236 -0.1053 0.9008 0.061 Uiso 1 1 calc R U . . .
C8 C 0.5225(4) 0.0396(5) 0.9524(3) 0.0413(12) Uani 1 1 d . . . . .
C9 C 0.4885(5) 0.1741(4) 0.9243(3) 0.0460(13) Uani 1 1 d . . . . .
H9 H 0.4344 0.2161 0.9653 0.055 Uiso 1 1 calc R U . . .
C10 C 0.5333(5) 0.2432(5) 0.8386(3) 0.0484(13) Uani 1 1 d . . . . .
H10 H 0.5100 0.3326 0.8218 0.058 Uiso 1 1 calc R U . . .
C11 C 0.6790(6) 0.2218(6) 1.0480(4) 0.0614(15) Uani 1 1 d . . . . .
C12 C 0.6792(6) 0.3404(6) 0.9805(4) 0.0685(17) Uani 1 1 d . . . . .
H12 H 0.6302 0.4159 0.9922 0.082 Uiso 1 1 calc R U . . .
C13 C 0.7553(6) 0.3441(6) 0.8936(4) 0.0704(17) Uani 1 1 d . . . . .
H13 H 0.7581 0.4237 0.8487 0.084 Uiso 1 1 calc R U . . .
C14 C 0.8249(5) 0.2359(5) 0.8728(4) 0.0571(14) Uani 1 1 d . . . . .
H14 H 0.8734 0.2421 0.8142 0.068 Uiso 1 1 calc R U . . .
C15 C 0.8234(5) 0.1142(5) 0.9402(4) 0.0514(13) Uani 1 1 d . . . . .
C16 C 0.7494(5) 0.1064(5) 1.0299(4) 0.0534(14) Uani 1 1 d . . . . .
C17 C 0.7501(6) -0.0151(6) 1.0989(4) 0.0640(16) Uani 1 1 d . . . . .
H17 H 0.7018 -0.0204 1.1574 0.077 Uiso 1 1 calc R U . . .
C18 C 0.8193(7) -0.1214(6) 1.0804(5) 0.0770(19) Uani 1 1 d . . . . .
H18 H 0.8197 -0.2005 1.1270 0.092 Uiso 1 1 calc R U . . .
C19 C 0.8923(6) -0.1184(5) 0.9925(5) 0.0697(17) Uani 1 1 d . . . . .
H19 H 0.9399 -0.1948 0.9815 0.084 Uiso 1 1 calc R U . . .
C20 C 0.8934(5) -0.0037(5) 0.9232(4) 0.0558(14) Uani 1 1 d . . . . .
C21 C 1.0406(6) -0.1000(6) 0.8137(5) 0.0720(18) Uani 1 1 d . . . . .
H21A H 0.9966 -0.1660 0.8267 0.086 Uiso 1 1 calc R U . . .
H21B H 1.1085 -0.1346 0.8529 0.086 Uiso 1 1 calc R U . . .
C22 C 1.0902(6) -0.0583(7) 0.7104(5) 0.0736(18) Uani 1 1 d . . . . .
H22A H 1.1231 0.0159 0.6970 0.088 Uiso 1 1 calc R U . . .
H22B H 1.1584 -0.1272 0.6969 0.088 Uiso 1 1 calc R U . . .
C23 C 0.9771(6) -0.1343(6) 0.6380(5) 0.0760(19) Uani 1 1 d . . . . .
H23A H 0.9563 -0.1934 0.6996 0.091 Uiso 1 1 calc R U . . .
H23B H 1.0528 -0.1786 0.6074 0.091 Uiso 1 1 calc R U . . .
C24 C 0.8746(5) -0.0942(6) 0.5795(4) 0.0681(17) Uani 1 1 d . . . . .
H24A H 0.8920 -0.0292 0.5201 0.082 Uiso 1 1 calc R U . . .
H24B H 0.8679 -0.1675 0.5648 0.082 Uiso 1 1 calc R U . . .
C25 C 0.6561(6) -0.0202(7) 0.5836(5) 0.0786(19) Uani 1 1 d . . . . .
H25A H 0.6779 0.0093 0.5153 0.094 Uiso 1 1 calc R U . . .
H25B H 0.5912 0.0483 0.6010 0.094 Uiso 1 1 calc R U . . .
C26 C 0.6070(6) -0.1339(7) 0.6091(4) 0.0774(19) Uani 1 1 d . . . . .
H26A H 0.5349 -0.1127 0.5761 0.093 Uiso 1 1 calc R U . . .
H26B H 0.6703 -0.2021 0.5901 0.093 Uiso 1 1 calc R U . . .
C27 C 0.5098(7) -0.2747(8) 0.7370(5) 0.093(2) Uani 1 1 d . . . . .
H27A H 0.5644 -0.3486 0.7196 0.112 Uiso 1 1 calc R U . . .
H27B H 0.4365 -0.2451 0.7037 0.112 Uiso 1 1 calc R U . . .
C28 C 0.5287(6) 0.3140(7) 1.1595(5) 0.0784(19) Uani 1 1 d . . . . .
H28A H 0.4562 0.3435 1.1254 0.094 Uiso 1 1 calc R U . . .
H28B H 0.5692 0.3839 1.1413 0.094 Uiso 1 1 calc R U . . .
O6A O 0.7416(14) 0.6584(13) 0.9464(10) 0.135(4) Uiso 0.5 1 d D . P A 1
C29A C 0.877(3) 0.564(6) 0.962(5) 0.42(4) Uiso 0.5 1 d D . P A 1
O6B O 0.7802(15) 0.6999(15) 0.8471(12) 0.172(6) Uiso 0.5 1 d D . P B 2
C29B C 0.837(2) 0.5990(19) 0.9352(13) 0.106(6) Uiso 0.5 1 d D . P B 2


_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
Cd1 N1 2.354(4) . ?
Cd1 I2 2.7016(6) . ?
Cd1 I1 2.7271(5) . ?
Cd1 I3 2.7903(6) . ?
O1 C20 1.367(6) . ?
O1 C21 1.433(7) . ?
O2 C23 1.407(7) . ?
O2 C22 1.414(7) . ?
O3 C24 1.402(6) . ?
O3 C25 1.405(7) . ?
O4 C27 1.407(8) . ?
O4 C26 1.417(7) . ?
O5 C11 1.371(6) . ?
O5 C28 1.421(7) . ?
N1 C1 1.315(6) . ?
N1 C5 1.325(6) . ?
N2 C10 1.346(6) . ?
N2 C6 1.346(6) . ?
N2 C3 1.454(6) . ?
C1 C2 1.381(6) . ?
C2 C3 1.364(7) . ?
C3 C4 1.378(7) . ?
C4 C5 1.371(7) . ?
C6 C7 1.366(7) . ?
C7 C8 1.391(6) . ?
C8 C9 1.398(6) . ?
C8 C8 1.484(9) 2_657 ?
C9 C10 1.343(6) . ?
C11 C12 1.382(8) . ?
C11 C16 1.410(8) . ?
C12 C13 1.406(8) . ?
C13 C14 1.356(8) . ?
C14 C15 1.409(7) . ?
C15 C16 1.425(7) . ?
C15 C20 1.426(8) . ?
C16 C17 1.413(8) . ?
C17 C18 1.323(9) . ?
C18 C19 1.406(9) . ?
C19 C20 1.362(8) . ?
C21 C22 1.501(9) . ?
C23 C24 1.471(8) . ?
C25 C26 1.465(9) . ?
C27 C28 1.476(9) 2_657 ?
C28 C27 1.476(9) 2_657 ?
O6A C29A 1.59(2) . ?
O6B C29B 1.535(16) . ?

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 Cd1 I2 106.55(10) . . ?
N1 Cd1 I1 100.58(10) . . ?
I2 Cd1 I1 125.40(2) . . ?
N1 Cd1 I3 101.98(10) . . ?
I2 Cd1 I3 110.086(18) . . ?
I1 Cd1 I3 109.247(19) . . ?
C20 O1 C21 118.0(5) . . ?
C23 O2 C22 113.3(5) . . ?
C24 O3 C25 113.8(4) . . ?
C27 O4 C26 112.6(5) . . ?
C11 O5 C28 119.7(5) . . ?
C1 N1 C5 117.0(4) . . ?
C1 N1 Cd1 123.0(3) . . ?
C5 N1 Cd1 120.0(3) . . ?
C10 N2 C6 119.4(4) . . ?
C10 N2 C3 120.5(4) . . ?
C6 N2 C3 120.1(4) . . ?
N1 C1 C2 123.7(5) . . ?
C3 C2 C1 117.9(5) . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 N2 120.3(4) . . ?
C4 C3 N2 119.8(4) . . ?
C5 C4 C3 117.1(5) . . ?
N1 C5 C4 124.4(5) . . ?
N2 C6 C7 120.5(4) . . ?
C6 C7 C8 121.1(5) . . ?
C7 C8 C9 116.4(4) . . ?
C7 C8 C8 121.8(5) . 2_657 ?
C9 C8 C8 121.8(5) . 2_657 ?
C10 C9 C8 120.5(4) . . ?
C9 C10 N2 122.1(5) . . ?
O5 C11 C12 123.8(6) . . ?
O5 C11 C16 114.7(5) . . ?
C12 C11 C16 121.4(5) . . ?
C11 C12 C13 118.3(6) . . ?
C14 C13 C12 122.5(6) . . ?
C13 C14 C15 119.8(5) . . ?
C14 C15 C16 119.4(5) . . ?
C14 C15 C20 123.0(5) . . ?
C16 C15 C20 117.5(5) . . ?
C11 C16 C17 121.6(5) . . ?
C11 C16 C15 118.5(5) . . ?
C17 C16 C15 119.9(5) . . ?
C18 C17 C16 120.1(6) . . ?
C17 C18 C19 122.0(6) . . ?
C20 C19 C18 120.0(6) . . ?
C19 C20 O1 125.6(6) . . ?
C19 C20 C15 120.4(6) . . ?
O1 C20 C15 114.0(5) . . ?
O1 C21 C22 107.0(5) . . ?
O2 C22 C21 112.5(5) . . ?
O2 C23 C24 110.2(5) . . ?
O3 C24 C23 110.0(5) . . ?
O3 C25 C26 112.9(5) . . ?
O4 C26 C25 109.4(6) . . ?
O4 C27 C28 111.5(6) . 2_657 ?
O5 C28 C27 108.1(6) . 2_657 ?

_refine_diff_density_max         1.187
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 997301'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3[CdI4]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H56 Cd I4 N4 O10'
_chemical_formula_weight         1468.97

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

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

_cell_length_a                   18.7667(2)
_cell_length_b                   18.3528(2)
_cell_length_c                   31.9417(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11001.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5489
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      22.29

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5696
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5520
_exptl_absorpt_correction_T_max  0.8337
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            104749
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_sigmaI/netI    0.1305
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         30.57
_reflns_number_total             16836
_reflns_number_gt                8139
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0145P)²+189.5742P] 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       0.000151(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         16836
_refine_ls_number_parameters     595
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1779
_refine_ls_R_factor_gt           0.0820
_refine_ls_wR_factor_ref         0.1701
_refine_ls_wR_factor_gt          0.1412
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I -0.01490(4) 0.04074(4) 0.34668(2) 0.04271(19) Uani 1 1 d . . .
I2 I 0.15861(3) 0.18881(3) 0.31005(2) 0.03186(16) Uani 1 1 d . . .
I3 I -0.00738(4) 0.28244(4) 0.39660(2) 0.0471(2) Uani 1 1 d . . .
I4 I 0.13907(7) 0.11434(4) 0.44734(3) 0.0780(4) Uani 1 1 d . . .
Cd1 Cd 0.06529(4) 0.15592(4) 0.37635(2) 0.03273(18) Uani 1 1 d . . .
O1 O 0.1534(3) 0.4271(3) 0.23495(18) 0.0307(15) Uani 1 1 d . . .
O2 O 0.1972(3) 0.3199(4) 0.17359(18) 0.0328(15) Uani 1 1 d . . .
O3 O 0.3202(4) 0.2467(4) 0.2058(2) 0.0389(17) Uani 1 1 d . . .
O4 O 0.4391(4) 0.2730(4) 0.2613(2) 0.0432(18) Uani 1 1 d . . .
O5 O 0.4561(5) 0.2812(6) 0.3477(3) 0.013(2) Uiso 0.50 1 d PD A 1
O6 O 0.3438(9) 0.3328(9) 0.5009(5) 0.048(5) Uiso 0.50 1 d PD A 1
C35 C 0.4280(8) 0.2885(7) 0.3860(4) 0.015(3) Uiso 0.50 1 d PD A 1
C36 C 0.3813(9) 0.2396(10) 0.4059(5) 0.024(4) Uiso 0.50 1 d PD A 1
H36 H 0.3672 0.1972 0.3923 0.029 Uiso 0.50 1 calc PR A 1
C37 C 0.3569(8) 0.2543(8) 0.4450(4) 0.014(3) Uiso 0.50 1 d PD A 1
H37 H 0.3272 0.2212 0.4585 0.017 Uiso 0.50 1 calc PR A 1
C38 C 0.3757(9) 0.3178(8) 0.4646(5) 0.022(4) Uiso 0.50 1 d PD A 1
C39 C 0.4183(9) 0.3691(10) 0.4445(5) 0.030(4) Uiso 0.50 1 d PD A 1
H39 H 0.4279 0.4135 0.4573 0.036 Uiso 0.50 1 calc PR A 1
C40 C 0.4458(8) 0.3539(8) 0.4059(4) 0.020(3) Uiso 0.50 1 d PD A 1
H40 H 0.4761 0.3869 0.3929 0.024 Uiso 0.50 1 calc PR A 1
C41 C 0.3692(12) 0.3437(14) 0.5423(6) 0.047(6) Uiso 0.50 1 d PD A 1
H41A H 0.4114 0.3740 0.5402 0.056 Uiso 0.50 1 calc PR A 1
H41B H 0.3846 0.2966 0.5526 0.056 Uiso 0.50 1 calc PR A 1
C42 C 0.3222(11) 0.3770(8) 0.5757(6) 0.027(4) Uiso 0.50 1 d PD A 1
H42A H 0.2786 0.3492 0.5792 0.032 Uiso 0.50 1 calc PR A 1
H42B H 0.3469 0.3793 0.6024 0.032 Uiso 0.50 1 calc PR A 1
O105 O 0.3918(12) 0.2325(16) 0.3493(6) 0.159(12) Uiso 0.50 1 d PD A 2
O106 O 0.3262(8) 0.3185(9) 0.5107(5) 0.047(5) Uiso 0.50 1 d PD A 2
C135 C 0.3838(13) 0.2469(15) 0.3928(6) 0.059(8) Uiso 0.50 1 d PD A 2
C136 C 0.3208(15) 0.2176(18) 0.4107(7) 0.107(12) Uiso 0.50 1 d PD A 2
H136 H 0.2890 0.1861 0.3976 0.129 Uiso 0.50 1 calc PR A 2
C137 C 0.3153(17) 0.2430(15) 0.4495(7) 0.084(9) Uiso 0.50 1 d PD A 2
H137 H 0.2792 0.2212 0.4650 0.100 Uiso 0.50 1 calc PR A 2
C138 C 0.3531(13) 0.2962(14) 0.4716(7) 0.070(9) Uiso 0.50 1 d PD A 2
C139 C 0.4128(18) 0.326(2) 0.4516(9) 0.132(16) Uiso 0.50 1 d PD A 2
H139 H 0.4392 0.3634 0.4636 0.159 Uiso 0.50 1 calc PR A 2
C140 C 0.4310(15) 0.2965(15) 0.4122(8) 0.080(9) Uiso 0.50 1 d PD A 2
H140 H 0.4735 0.3095 0.3992 0.096 Uiso 0.50 1 calc PR A 2
C141 C 0.3873(10) 0.3565(12) 0.5302(6) 0.035(5) Uiso 0.50 1 d PD A 2
H14A H 0.4050 0.3961 0.5129 0.042 Uiso 0.50 1 calc PR A 2
H14B H 0.4259 0.3235 0.5371 0.042 Uiso 0.50 1 calc PR A 2
C142 C 0.3481(10) 0.3842(9) 0.5695(5) 0.024(4) Uiso 0.50 1 d PD A 2
H14C H 0.3164 0.3465 0.5798 0.029 Uiso 0.50 1 calc PR A 2
H14D H 0.3824 0.3951 0.5913 0.029 Uiso 0.50 1 calc PR A 2
O7 O 0.3075(4) 0.4486(3) 0.56003(19) 0.0385(17) Uani 1 1 d D . .
O8 O 0.2016(3) 0.5611(3) 0.55799(18) 0.0296(15) Uani 1 1 d . A .
O9 O 0.1186(3) 0.5685(3) 0.48237(19) 0.0311(15) Uani 1 1 d . . .
O10 O 0.1130(3) 0.5497(3) 0.39170(19) 0.0326(15) Uani 1 1 d . . .
N1 N 0.6001(5) 0.3170(5) -0.0967(2) 0.045(2) Uani 1 1 d . . .
N2 N 0.6833(4) 0.3654(4) 0.0226(2) 0.0279(17) Uani 1 1 d . . .
N3 N 0.8360(4) 0.4331(4) 0.2196(2) 0.0249(16) Uani 1 1 d . . .
N4 N 0.9185(4) 0.4877(4) 0.3385(2) 0.0339(19) Uani 1 1 d . . .
C1 C 0.6104(5) 0.3848(6) -0.0846(3) 0.034(2) Uani 1 1 d . . .
H1 H 0.5995 0.4219 -0.1034 0.041 Uiso 1 1 calc R . .
C2 C 0.6368(5) 0.4047(5) -0.0452(3) 0.030(2) Uani 1 1 d . . .
H2 H 0.6419 0.4533 -0.0376 0.035 Uiso 1 1 calc R . .
C3 C 0.6547(6) 0.3490(5) -0.0181(3) 0.032(2) Uani 1 1 d . . .
C4 C 0.6441(8) 0.2785(6) -0.0298(3) 0.061(4) Uani 1 1 d . . .
H4 H 0.6548 0.2405 -0.0116 0.073 Uiso 1 1 calc R . .
C5 C 0.6169(8) 0.2644(6) -0.0694(3) 0.068(4) Uani 1 1 d . . .
H5 H 0.6100 0.2162 -0.0774 0.082 Uiso 1 1 calc R . .
C6 C 0.7284(5) 0.4218(5) 0.0274(3) 0.030(2) Uani 1 1 d . . .
H6 H 0.7399 0.4511 0.0047 0.037 Uiso 1 1 calc R . .
C7 C 0.7576(5) 0.4361(5) 0.0662(3) 0.032(2) Uani 1 1 d . . .
H7 H 0.7878 0.4759 0.0695 0.039 Uiso 1 1 calc R . .
C8 C 0.7426(5) 0.3918(5) 0.1005(3) 0.0251(19) Uani 1 1 d . . .
C9 C 0.6950(6) 0.3354(5) 0.0941(3) 0.039(3) Uani 1 1 d . . .
H9 H 0.6820 0.3055 0.1163 0.047 Uiso 1 1 calc R . .
C10 C 0.6672(6) 0.3233(5) 0.0560(3) 0.041(3) Uani 1 1 d . . .
H10 H 0.6359 0.2845 0.0525 0.049 Uiso 1 1 calc R . .
C11 C 0.8096(5) 0.3668(5) 0.2108(3) 0.028(2) Uani 1 1 d . . .
H11 H 0.8114 0.3304 0.2309 0.034 Uiso 1 1 calc R . .
C12 C 0.7801(5) 0.3522(5) 0.1725(3) 0.029(2) Uani 1 1 d . . .
H12 H 0.7619 0.3060 0.1671 0.035 Uiso 1 1 calc R . .
C13 C 0.7769(5) 0.4058(5) 0.1416(3) 0.026(2) Uani 1 1 d . . .
C14 C 0.8059(5) 0.4740(5) 0.1512(3) 0.0260(19) Uani 1 1 d . . .
H14 H 0.8053 0.5114 0.1316 0.031 Uiso 1 1 calc R . .
C15 C 0.8351(5) 0.4851(5) 0.1902(3) 0.029(2) Uani 1 1 d . . .
H15 H 0.8548 0.5303 0.1964 0.035 Uiso 1 1 calc R . .
C16 C 0.8622(6) 0.4447(5) 0.3343(3) 0.035(2) Uani 1 1 d . . .
H16 H 0.8411 0.4269 0.3586 0.042 Uiso 1 1 calc R . .
C17 C 0.8323(5) 0.4239(5) 0.2958(3) 0.033(2) Uani 1 1 d . . .
H17 H 0.7926 0.3937 0.2944 0.039 Uiso 1 1 calc R . .
C18 C 0.8649(5) 0.4508(5) 0.2604(3) 0.026(2) Uani 1 1 d . . .
C19 C 0.9241(5) 0.4954(5) 0.2632(3) 0.033(2) Uani 1 1 d . . .
H19 H 0.9470 0.5133 0.2395 0.040 Uiso 1 1 calc R . .
C20 C 0.9473(6) 0.5118(5) 0.3031(3) 0.037(2) Uani 1 1 d . . .
H20 H 0.9866 0.5424 0.3054 0.045 Uiso 1 1 calc R . .
C21 C 0.1400(5) 0.4539(5) 0.2744(3) 0.028(2) Uani 1 1 d . . .
C22 C 0.1040(5) 0.4152(5) 0.3055(3) 0.030(2) Uani 1 1 d . . .
H22 H 0.0869 0.3685 0.3000 0.036 Uiso 1 1 calc R . .
C23 C 0.0936(5) 0.4465(5) 0.3448(3) 0.029(2) Uani 1 1 d . . .
H23 H 0.0685 0.4209 0.3652 0.035 Uiso 1 1 calc R . .
C24 C 0.1200(5) 0.5147(5) 0.3539(3) 0.028(2) Uani 1 1 d . . .
C25 C 0.1583(5) 0.5519(5) 0.3232(3) 0.033(2) Uani 1 1 d . . .
H25 H 0.1783 0.5969 0.3295 0.039 Uiso 1 1 calc R . .
C26 C 0.1671(5) 0.5226(5) 0.2833(3) 0.030(2) Uani 1 1 d . . .
H26 H 0.1910 0.5489 0.2627 0.036 Uiso 1 1 calc R . .
C27 C 0.1066(5) 0.3716(5) 0.2201(3) 0.032(2) Uani 1 1 d . . .
H27A H 0.0578 0.3889 0.2203 0.039 Uiso 1 1 calc R . .
H27B H 0.1096 0.3289 0.2379 0.039 Uiso 1 1 calc R . .
C28 C 0.1290(5) 0.3524(6) 0.1759(3) 0.033(2) Uani 1 1 d . . .
H28A H 0.0942 0.3192 0.1640 0.040 Uiso 1 1 calc R . .
H28B H 0.1289 0.3964 0.1590 0.040 Uiso 1 1 calc R . .
C29 C 0.1969(5) 0.2465(5) 0.1881(3) 0.036(2) Uani 1 1 d . . .
H29A H 0.1602 0.2190 0.1736 0.043 Uiso 1 1 calc R . .
H29B H 0.1867 0.2453 0.2178 0.043 Uiso 1 1 calc R . .
C30 C 0.2687(6) 0.2136(6) 0.1797(3) 0.041(3) Uani 1 1 d . . .
H30A H 0.2672 0.1616 0.1852 0.049 Uiso 1 1 calc R . .
H30B H 0.2815 0.2207 0.1506 0.049 Uiso 1 1 calc R . .
C31 C 0.3876(6) 0.2133(6) 0.2009(4) 0.052(3) Uani 1 1 d . . .
H31A H 0.3961 0.2032 0.1715 0.063 Uiso 1 1 calc R . .
H31B H 0.3884 0.1674 0.2159 0.063 Uiso 1 1 calc R . .
C32 C 0.4452(6) 0.2621(7) 0.2173(3) 0.049(3) Uani 1 1 d . . .
H32A H 0.4912 0.2407 0.2111 0.059 Uiso 1 1 calc R . .
H32B H 0.4425 0.3088 0.2032 0.059 Uiso 1 1 calc R . .
C33 C 0.4710(6) 0.2159(6) 0.2844(3) 0.048(3) Uani 1 1 d D A .
H33A H 0.4577 0.1692 0.2724 0.057 Uiso 1 1 calc R . .
H33B H 0.5225 0.2202 0.2831 0.057 Uiso 1 1 calc R . .
C34 C 0.4476(8) 0.2198(8) 0.3271(4) 0.103(7) Uani 1 1 d D . .
H34A H 0.3973 0.2079 0.3276 0.124 Uiso 1 1 calc R A 1
H34B H 0.4722 0.1818 0.3425 0.124 Uiso 1 1 calc R A 1
C43 C 0.2906(6) 0.4948(5) 0.5941(3) 0.038(3) Uani 1 1 d . A .
H43A H 0.3315 0.4997 0.6125 0.046 Uiso 1 1 calc R . .
H43B H 0.2516 0.4743 0.6102 0.046 Uiso 1 1 calc R . .
C44 C 0.2698(5) 0.5679(5) 0.5771(3) 0.034(2) Uani 1 1 d . . .
H44A H 0.2679 0.6034 0.5996 0.041 Uiso 1 1 calc R A .
H44B H 0.3046 0.5841 0.5567 0.041 Uiso 1 1 calc R . .
C45 C 0.1795(5) 0.6272(5) 0.5390(3) 0.033(2) Uani 1 1 d . . .
H45A H 0.2146 0.6428 0.5186 0.040 Uiso 1 1 calc R A .
H45B H 0.1749 0.6649 0.5601 0.040 Uiso 1 1 calc R . .
C46 C 0.1083(5) 0.6150(5) 0.5177(3) 0.029(2) Uani 1 1 d . A .
H46A H 0.0751 0.5926 0.5371 0.035 Uiso 1 1 calc R . .
H46B H 0.0886 0.6612 0.5087 0.035 Uiso 1 1 calc R . .
C47 C 0.0559(5) 0.5661(5) 0.4576(3) 0.033(2) Uani 1 1 d . . .
H47A H 0.0447 0.6146 0.4475 0.039 Uiso 1 1 calc R . .
H47B H 0.0163 0.5492 0.4745 0.039 Uiso 1 1 calc R . .
C48 C 0.0664(5) 0.5158(5) 0.4211(3) 0.031(2) Uani 1 1 d . . .
H48A H 0.0869 0.4701 0.4306 0.037 Uiso 1 1 calc R . .
H48B H 0.0209 0.5054 0.4079 0.037 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cd1 2.7623(10) . ?
I2 Cd1 2.8134(9) . ?
I3 Cd1 2.7696(10) . ?
I4 Cd1 2.7643(11) . ?
O1 C21 1.375(10) . ?
O1 C27 1.426(10) . ?
O2 C28 1.413(11) . ?
O2 C29 1.424(11) . ?
O3 C31 1.415(11) . ?
O3 C30 1.413(11) . ?
O4 C32 1.423(12) . ?
O4 C33 1.414(12) . ?
O5 C34 1.315(14) . ?
O5 C35 1.339(13) . ?
O6 C38 1.332(15) . ?
O6 C41 1.419(16) . ?
C35 C40 1.398(15) . ?
C35 C36 1.406(15) . ?
C36 C37 1.358(16) . ?
C37 C38 1.369(15) . ?
C38 C39 1.393(16) . ?
C39 C40 1.365(15) . ?
C41 C42 1.514(17) . ?
C42 O7 1.433(14) . ?
O105 C34 1.285(16) . ?
O105 C135 1.424(15) . ?
O106 C138 1.408(16) . ?
O106 C141 1.479(16) . ?
C135 C140 1.413(17) . ?
C135 C136 1.419(18) . ?
C136 C137 1.329(18) . ?
C137 C138 1.398(17) . ?
C138 C139 1.402(18) . ?
C139 C140 1.411(18) . ?
C141 C142 1.541(17) . ?
C142 O7 1.437(14) . ?
O7 C43 1.417(11) . ?
O8 C45 1.417(11) . ?
O8 C44 1.423(11) . ?
O9 C47 1.418(10) . ?
O9 C46 1.428(10) . ?
O10 C24 1.373(11) . ?
O10 C48 1.425(10) . ?
N1 C1 1.318(12) . ?
N1 C5 1.336(13) . ?
N2 C6 1.346(11) . ?
N2 C10 1.353(11) . ?
N2 C3 1.437(11) . ?
N3 C15 1.339(10) . ?
N3 C11 1.343(11) . ?
N3 C18 1.448(11) . ?
N4 C20 1.329(12) . ?
N4 C16 1.326(12) . ?
C1 C2 1.401(12) . ?
C2 C3 1.380(13) . ?
C3 C4 1.363(14) . ?
C4 C5 1.388(14) . ?
C6 C7 1.380(13) . ?
C7 C8 1.393(12) . ?
C8 C9 1.384(13) . ?
C8 C13 1.484(12) . ?
C9 C10 1.340(13) . ?
C11 C12 1.368(12) . ?
C12 C13 1.395(12) . ?
C13 C14 1.399(12) . ?
C14 C15 1.375(12) . ?
C16 C17 1.404(13) . ?
C17 C18 1.380(12) . ?
C18 C19 1.382(13) . ?
C19 C20 1.382(13) . ?
C21 C26 1.388(13) . ?
C21 C22 1.397(12) . ?
C22 C23 1.395(12) . ?
C23 C24 1.378(12) . ?
C24 C25 1.394(13) . ?
C25 C26 1.394(12) . ?
C27 C28 1.514(13) . ?
C29 C30 1.502(14) . ?
C31 C32 1.498(15) . ?
C33 C34 1.436(13) . ?
C43 C44 1.499(13) . ?
C45 C46 1.515(13) . ?
C47 C48 1.502(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
I1 Cd1 I4 110.06(3) . . ?
I1 Cd1 I3 116.96(4) . . ?
I4 Cd1 I3 106.64(3) . . ?
I1 Cd1 I2 104.19(3) . . ?
I4 Cd1 I2 111.40(4) . . ?
I3 Cd1 I2 107.61(3) . . ?
C21 O1 C27 116.7(7) . . ?
C28 O2 C29 112.2(7) . . ?
C31 O3 C30 111.1(7) . . ?
C32 O4 C33 112.1(8) . . ?
C34 O5 C35 119.7(11) . . ?
C38 O6 C41 133.6(18) . . ?
O5 C35 C40 114.0(12) . . ?
O5 C35 C36 126.4(13) . . ?
C40 C35 C36 119.5(13) . . ?
C37 C36 C35 119.9(15) . . ?
C36 C37 C38 120.3(15) . . ?
O6 C38 C37 117.3(14) . . ?
O6 C38 C39 121.3(15) . . ?
C37 C38 C39 120.7(14) . . ?
C40 C39 C38 119.8(16) . . ?
C39 C40 C35 119.6(14) . . ?
O6 C41 C42 121.3(18) . . ?
O7 C42 C41 103.6(15) . . ?
C34 O105 C135 131(2) . . ?
C138 O106 C141 103.5(14) . . ?
C140 C135 C136 126(2) . . ?
C140 C135 O105 118.8(16) . . ?
C136 C135 O105 114.3(16) . . ?
C137 C136 C135 108(3) . . ?
C136 C137 C138 133(3) . . ?
C137 C138 C139 117(2) . . ?
C137 C138 O106 118.0(17) . . ?
C139 C138 O106 125.3(18) . . ?
C138 C139 C140 117(3) . . ?
C135 C140 C139 119(3) . . ?
O106 C141 C142 97.3(14) . . ?
O7 C142 C141 110.7(14) . . ?
C43 O7 C142 116.7(9) . . ?
C43 O7 C42 108.8(9) . . ?
C142 O7 C42 21.7(10) . . ?
C45 O8 C44 111.9(7) . . ?
C47 O9 C46 110.3(7) . . ?
C24 O10 C48 115.6(7) . . ?
C1 N1 C5 117.2(9) . . ?
C6 N2 C10 119.2(8) . . ?
C6 N2 C3 120.0(7) . . ?
C10 N2 C3 120.7(8) . . ?
C15 N3 C11 119.6(8) . . ?
C15 N3 C18 118.3(7) . . ?
C11 N3 C18 122.1(7) . . ?
C20 N4 C16 115.8(8) . . ?
N1 C1 C2 124.1(9) . . ?
C3 C2 C1 117.2(9) . . ?
C4 C3 C2 119.7(9) . . ?
C4 C3 N2 120.2(8) . . ?
C2 C3 N2 120.1(8) . . ?
C3 C4 C5 118.8(10) . . ?
N1 C5 C4 123.1(10) . . ?
N2 C6 C7 119.9(8) . . ?
C6 C7 C8 121.0(9) . . ?
C7 C8 C9 116.7(8) . . ?
C7 C8 C13 120.5(8) . . ?
C9 C8 C13 122.8(8) . . ?
C10 C9 C8 120.7(9) . . ?
C9 C10 N2 122.3(9) . . ?
N3 C11 C12 121.0(8) . . ?
C11 C12 C13 120.7(8) . . ?
C12 C13 C14 117.4(8) . . ?
C12 C13 C8 121.5(8) . . ?
C14 C13 C8 121.1(8) . . ?
C15 C14 C13 119.0(8) . . ?
N3 C15 C14 122.3(8) . . ?
N4 C16 C17 124.8(9) . . ?
C18 C17 C16 116.4(9) . . ?
C19 C18 C17 121.0(9) . . ?
C19 C18 N3 119.5(8) . . ?
C17 C18 N3 119.5(8) . . ?
C18 C19 C20 116.3(9) . . ?
N4 C20 C19 125.8(10) . . ?
O1 C21 C26 116.5(8) . . ?
O1 C21 C22 123.8(8) . . ?
C26 C21 C22 119.6(8) . . ?
C23 C22 C21 119.9(9) . . ?
C24 C23 C22 121.0(9) . . ?
O10 C24 C23 125.2(8) . . ?
O10 C24 C25 116.0(8) . . ?
C23 C24 C25 118.8(9) . . ?
C24 C25 C26 121.0(9) . . ?
C21 C26 C25 119.6(9) . . ?
O1 C27 C28 107.8(7) . . ?
O2 C28 C27 113.5(8) . . ?
O2 C29 C30 108.7(8) . . ?
O3 C30 C29 109.6(8) . . ?
O3 C31 C32 110.3(8) . . ?
O4 C32 C31 111.9(9) . . ?
C34 C33 O4 109.2(9) . . ?
O105 C34 O5 70.6(14) . . ?
O105 C34 C33 141.5(16) . . ?
O5 C34 C33 118.8(13) . . ?
O7 C43 C44 108.4(7) . . ?
O8 C44 C43 108.2(8) . . ?
O8 C45 C46 108.9(7) . . ?
O9 C46 C45 108.9(7) . . ?
O9 C47 C48 110.1(8) . . ?
O10 C48 C47 108.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.623
_refine_diff_density_min         -3.833
_refine_diff_density_rms         0.208
_database_code_depnum_ccdc_archive 'CCDC 997302'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1[Hg2Br6]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H52 Br6 Hg2 N4 O8'
_chemical_formula_weight         1741.62

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                   9.82030(10)
_cell_length_b                   11.5983(2)
_cell_length_c                   12.8782(2)
_cell_angle_alpha                94.8350(10)
_cell_angle_beta                 106.3330(10)
_cell_angle_gamma                103.1390(10)
_cell_volume                     1353.42(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9871
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      30.28

_exptl_crystal_description       block
_exptl_crystal_colour            blue/red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             826
_exptl_absorpt_coefficient_mu    10.150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58173
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         30.03
_reflns_number_total             7890
_reflns_number_gt                7162
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0128P)²+3.9827P] 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         7890
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0495
_refine_ls_wR_factor_gt          0.0479
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.572492(12) 0.164369(9) 0.076055(9) 0.02087(3) Uani 1 1 d . . .
Br3 Br 0.42563(4) -0.03880(3) 0.11952(2) 0.02826(7) Uani 1 1 d . . .
Br2 Br 0.43058(4) 0.31595(3) 0.02847(3) 0.03251(7) Uani 1 1 d . . .
Br1 Br 0.83670(4) 0.20790(3) 0.19453(3) 0.03400(7) Uani 1 1 d . . .
O1 O 0.1143(2) 0.04336(17) 0.27924(15) 0.0202(4) Uani 1 1 d . . .
O3 O 0.1512(2) -0.40329(18) 0.14869(16) 0.0222(4) Uani 1 1 d . . .
O4 O 0.5481(2) 0.35393(18) 0.68247(17) 0.0235(4) Uani 1 1 d . . .
O2 O 0.0573(2) -0.18452(18) 0.13122(16) 0.0260(4) Uani 1 1 d . . .
N2 N 0.1804(3) 0.7649(2) 0.45098(18) 0.0173(4) Uani 1 1 d . . .
N1 N -0.2215(3) 0.5014(2) 0.3901(2) 0.0290(6) Uani 1 1 d . . .
C15 C 0.3841(3) 0.2545(2) 0.5116(2) 0.0197(5) Uani 1 1 d . . .
C26 C 0.0702(3) 0.0231(2) 0.1616(2) 0.0219(5) Uani 1 1 d . . .
H26A H 0.1559 0.0303 0.1368 0.026 Uiso 1 1 calc R . .
H26B H 0.0203 0.0823 0.1330 0.026 Uiso 1 1 calc R . .
C7 C 0.3427(3) 0.8999(2) 0.3838(2) 0.0194(5) Uani 1 1 d . . .
H7 H 0.3674 0.9282 0.3242 0.023 Uiso 1 1 calc R . .
C16 C 0.2612(3) 0.1603(2) 0.4487(2) 0.0179(5) Uani 1 1 d . . .
C8 C 0.4343(3) 0.9492(2) 0.4898(2) 0.0166(5) Uani 1 1 d . . .
C20 C 0.4207(3) 0.2687(2) 0.6283(2) 0.0202(5) Uani 1 1 d . . .
C11 C 0.2271(3) 0.1426(2) 0.3322(2) 0.0197(5) Uani 1 1 d . . .
C18 C 0.2101(3) 0.1074(3) 0.6138(2) 0.0225(5) Uani 1 1 d . . .
H18 H 0.1515 0.0600 0.6479 0.027 Uiso 1 1 calc R . .
C25 C -0.0317(3) -0.1013(3) 0.1210(2) 0.0243(6) Uani 1 1 d . . .
H25A H -0.0982 -0.1181 0.1644 0.029 Uiso 1 1 calc R . .
H25B H -0.0897 -0.1079 0.0451 0.029 Uiso 1 1 calc R . .
C5 C -0.1606(3) 0.5783(3) 0.4837(3) 0.0261(6) Uani 1 1 d . . .
H5 H -0.2087 0.5719 0.5365 0.031 Uiso 1 1 calc R . .
C4 C -0.0303(3) 0.6672(3) 0.5077(2) 0.0223(5) Uani 1 1 d . . .
H4 H 0.0063 0.7203 0.5733 0.027 Uiso 1 1 calc R . .
C9 C 0.3948(3) 0.8992(2) 0.5757(2) 0.0191(5) Uani 1 1 d . . .
H9 H 0.4535 0.9288 0.6476 0.023 Uiso 1 1 calc R . .
C23 C 0.1173(3) -0.3503(2) 0.0520(2) 0.0236(6) Uani 1 1 d . . .
H23A H 0.0856 -0.4116 -0.0122 0.028 Uiso 1 1 calc R . .
H23B H 0.2042 -0.2921 0.0497 0.028 Uiso 1 1 calc R . .
C17 C 0.1746(3) 0.0867(2) 0.5021(2) 0.0204(5) Uani 1 1 d . . .
H17 H 0.0940 0.0246 0.4611 0.024 Uiso 1 1 calc R . .
C12 C 0.3070(3) 0.2199(3) 0.2819(2) 0.0225(5) Uani 1 1 d . . .
H12 H 0.2820 0.2095 0.2059 0.027 Uiso 1 1 calc R . .
C6 C 0.2169(3) 0.8104(2) 0.3662(2) 0.0206(5) Uani 1 1 d . . .
H6 H 0.1557 0.7805 0.2949 0.025 Uiso 1 1 calc R . .
C1 C -0.1492(4) 0.5119(3) 0.3164(3) 0.0292(6) Uani 1 1 d . . .
H1 H -0.1909 0.4602 0.2499 0.035 Uiso 1 1 calc R . .
C3 C 0.0430(3) 0.6740(2) 0.4304(2) 0.0191(5) Uani 1 1 d . . .
C19 C 0.3336(3) 0.1990(3) 0.6784(2) 0.0225(5) Uani 1 1 d . . .
H19 H 0.3559 0.2121 0.7542 0.027 Uiso 1 1 calc R . .
C22 C 0.2650(3) -0.4635(3) 0.1558(3) 0.0268(6) Uani 1 1 d . . .
H22A H 0.2526 -0.5038 0.0833 0.032 Uiso 1 1 calc R . .
H22B H 0.2544 -0.5244 0.2023 0.032 Uiso 1 1 calc R . .
C14 C 0.4674(3) 0.3318(2) 0.4583(2) 0.0220(5) Uani 1 1 d . . .
H14 H 0.5487 0.3933 0.4993 0.026 Uiso 1 1 calc R . .
C10 C 0.2704(3) 0.8072(2) 0.5550(2) 0.0189(5) Uani 1 1 d . . .
H10 H 0.2474 0.7734 0.6129 0.023 Uiso 1 1 calc R . .
C24 C -0.0023(3) -0.2898(3) 0.0513(2) 0.0240(6) Uani 1 1 d . . .
H24A H -0.0410 -0.2691 -0.0206 0.029 Uiso 1 1 calc R . .
H24B H -0.0820 -0.3434 0.0680 0.029 Uiso 1 1 calc R . .
C21 C 0.5832(3) 0.3816(3) 0.7996(2) 0.0267(6) Uani 1 1 d . . .
H21A H 0.5785 0.3086 0.8316 0.032 Uiso 1 1 calc R . .
H21B H 0.5131 0.4203 0.8177 0.032 Uiso 1 1 calc R . .
C13 C 0.4268(3) 0.3148(2) 0.3464(3) 0.0235(6) Uani 1 1 d . . .
H13 H 0.4795 0.3671 0.3119 0.028 Uiso 1 1 calc R . .
C2 C -0.0156(3) 0.5951(3) 0.3322(2) 0.0241(6) Uani 1 1 d . . .
H2 H 0.0323 0.5977 0.2793 0.029 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 Br2 2.4948(3) . ?
Hg1 Br1 2.5225(3) . ?
Hg1 Br3 2.6604(3) . ?
Hg1 Br3 2.8081(3) 2_655 ?
Br3 Hg1 2.8081(3) 2_655 ?
O1 C11 1.371(3) . ?
O1 C26 1.437(3) . ?
O3 C23 1.424(3) . ?
O3 C22 1.433(4) . ?
O4 C20 1.363(3) . ?
O4 C21 1.440(4) . ?
O2 C24 1.421(3) . ?
O2 C25 1.432(4) . ?
N2 C6 1.353(3) . ?
N2 C10 1.358(3) . ?
N2 C3 1.452(4) . ?
N1 C1 1.334(4) . ?
N1 C5 1.334(4) . ?
C15 C16 1.417(4) . ?
C15 C20 1.429(4) . ?
C15 C14 1.426(4) . ?
C26 C25 1.510(4) . ?
C7 C6 1.369(4) . ?
C7 C8 1.395(4) . ?
C16 C17 1.422(4) . ?
C16 C11 1.428(4) . ?
C8 C9 1.398(4) . ?
C8 C8 1.480(5) 2_676 ?
C20 C19 1.373(4) . ?
C11 C12 1.379(4) . ?
C18 C17 1.368(4) . ?
C18 C19 1.411(4) . ?
C5 C4 1.385(4) . ?
C4 C3 1.381(4) . ?
C9 C10 1.370(4) . ?
C23 C24 1.496(4) . ?
C12 C13 1.412(4) . ?
C1 C2 1.390(4) . ?
C3 C2 1.387(4) . ?
C22 C21 1.495(4) 2_656 ?
C14 C13 1.366(4) . ?
C21 C22 1.495(4) 2_656 ?

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
Br2 Hg1 Br1 125.957(13) . . ?
Br2 Hg1 Br3 115.718(12) . . ?
Br1 Hg1 Br3 107.633(12) . . ?
Br2 Hg1 Br3 108.278(11) . 2_655 ?
Br1 Hg1 Br3 102.632(11) . 2_655 ?
Br3 Hg1 Br3 89.451(9) . 2_655 ?
Hg1 Br3 Hg1 90.548(9) . 2_655 ?
C11 O1 C26 117.0(2) . . ?
C23 O3 C22 113.2(2) . . ?
C20 O4 C21 116.9(2) . . ?
C24 O2 C25 114.7(2) . . ?
C6 N2 C10 119.7(2) . . ?
C6 N2 C3 119.8(2) . . ?
C10 N2 C3 120.5(2) . . ?
C1 N1 C5 116.5(3) . . ?
C16 C15 C20 118.2(3) . . ?
C16 C15 C14 120.0(3) . . ?
C20 C15 C14 121.8(3) . . ?
O1 C26 C25 108.3(2) . . ?
C6 C7 C8 120.8(2) . . ?
C15 C16 C17 119.8(2) . . ?
C15 C16 C11 118.6(3) . . ?
C17 C16 C11 121.7(2) . . ?
C7 C8 C9 116.9(2) . . ?
C7 C8 C8 121.3(3) . 2_676 ?
C9 C8 C8 121.8(3) . 2_676 ?
O4 C20 C19 124.6(3) . . ?
O4 C20 C15 114.2(2) . . ?
C19 C20 C15 121.2(3) . . ?
C12 C11 O1 125.2(3) . . ?
C12 C11 C16 120.6(3) . . ?
O1 C11 C16 114.2(2) . . ?
C17 C18 C19 121.4(3) . . ?
O2 C25 C26 107.6(2) . . ?
N1 C5 C4 124.4(3) . . ?
C3 C4 C5 117.5(3) . . ?
C10 C9 C8 120.8(2) . . ?
O3 C23 C24 109.6(2) . . ?
C18 C17 C16 119.8(3) . . ?
C11 C12 C13 119.7(3) . . ?
N2 C6 C7 120.9(2) . . ?
N1 C1 C2 124.4(3) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 N2 120.1(2) . . ?
C2 C3 N2 119.9(3) . . ?
C20 C19 C18 119.4(3) . . ?
O3 C22 C21 113.6(2) . 2_656 ?
C13 C14 C15 119.4(3) . . ?
N2 C10 C9 120.7(2) . . ?
O2 C24 C23 108.5(2) . . ?
O4 C21 C22 108.4(3) . 2_656 ?
C14 C13 C12 121.7(3) . . ?
C3 C2 C1 117.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.112
_database_code_depnum_ccdc_archive 'CCDC 997303'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2(Hg2Br6)2+PyBP+CH3OH

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77 H80 Br12 Hg4 N8 O11'
_chemical_formula_weight         3054.77

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                   10.9943(2)
_cell_length_b                   15.1689(2)
_cell_length_c                   15.5408(3)
_cell_angle_alpha                111.5800(10)
_cell_angle_beta                 101.9510(10)
_cell_angle_gamma                104.7280(10)
_cell_volume                     2196.86(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3928
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      22.61

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow/purple
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1426
_exptl_absorpt_coefficient_mu    12.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5264
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61152
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_sigmaI/netI    0.1120
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.50
_diffrn_reflns_theta_max         30.03
_reflns_number_total             12778
_reflns_number_gt                7328
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)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         12778
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.18643(3) 0.25951(2) 0.269957(18) 0.02640(8) Uani 1 1 d . . .
Hg2 Hg 0.55276(3) 0.21314(2) 0.397926(19) 0.02912(8) Uani 1 1 d . . .
Br1 Br 0.02540(8) 0.07844(6) 0.20069(5) 0.0380(2) Uani 1 1 d . . .
Br2 Br 0.13936(7) 0.38332(6) 0.20856(5) 0.03108(18) Uani 1 1 d . . .
Br3 Br 0.42642(7) 0.26446(6) 0.25425(5) 0.02993(18) Uani 1 1 d . . .
Br4 Br 0.36367(7) 0.05505(6) 0.36719(5) 0.03269(18) Uani 1 1 d . . .
Br5 Br 0.62088(6) 0.36310(6) 0.56407(5) 0.02456(16) Uani 1 1 d . . .
Br6 Br 0.74906(7) 0.19996(7) 0.33409(5) 0.0419(2) Uani 1 1 d . . .
O1 O 0.8646(4) 0.4783(3) 0.1676(3) 0.0199(10) Uani 1 1 d . . .
O2 O 0.9937(4) 0.6745(4) 0.3216(3) 0.0296(12) Uani 1 1 d . . .
O3 O 0.9508(4) 0.8534(3) 0.3580(3) 0.0196(10) Uani 1 1 d . . .
O4 O 0.2447(4) 0.0660(4) -0.4002(3) 0.0228(11) Uani 1 1 d . . .
O5 O 0.4948(4) 0.1935(4) -0.2383(3) 0.0246(11) Uani 1 1 d . . .
O6 O 0.0913(13) 0.5424(14) 0.5401(12) 0.085(5) Uani 0.50 1 d P . .
N1 N 0.2486(5) 0.3179(5) 0.4400(4) 0.0213(13) Uani 1 1 d . . .
N2 N 0.3894(5) 0.4138(4) 0.7437(3) 0.0154(12) Uani 1 1 d . . .
N3 N 1.1484(5) 0.2552(4) 0.9305(4) 0.0229(13) Uani 1 1 d . . .
N4 N 0.7950(5) 0.1079(4) 0.9646(4) 0.0165(12) Uani 1 1 d . . .
C1 C 0.2262(5) 0.2504(5) 0.4769(4) 0.0160(14) Uani 1 1 d . . .
H1 H 0.1793 0.1820 0.4339 0.019 Uiso 1 1 calc R . .
C2 C 0.2703(5) 0.2791(5) 0.5768(4) 0.0174(15) Uani 1 1 d . . .
H2 H 0.2537 0.2313 0.6011 0.021 Uiso 1 1 calc R . .
C3 C 0.3394(5) 0.3803(5) 0.6384(4) 0.0132(14) Uani 1 1 d . . .
C4 C 0.3618(6) 0.4519(5) 0.6022(4) 0.0181(14) Uani 1 1 d . . .
H4 H 0.4073 0.5209 0.6437 0.022 Uiso 1 1 calc R . .
C5 C 0.3136(6) 0.4158(5) 0.5021(5) 0.0240(16) Uani 1 1 d . . .
H5 H 0.3272 0.4625 0.4762 0.029 Uiso 1 1 calc R . .
C6 C 0.3132(6) 0.3702(5) 0.7863(4) 0.0188(15) Uani 1 1 d . . .
H6 H 0.2308 0.3184 0.7478 0.023 Uiso 1 1 calc R . .
C7 C 0.3569(6) 0.4021(5) 0.8851(4) 0.0189(15) Uani 1 1 d . . .
H7 H 0.3043 0.3704 0.9127 0.023 Uiso 1 1 calc R . .
C8 C 0.4776(5) 0.4805(5) 0.9455(4) 0.0144(14) Uani 1 1 d . . .
C9 C 0.5544(6) 0.5223(5) 0.8990(4) 0.0159(14) Uani 1 1 d . . .
H9 H 0.6368 0.5746 0.9365 0.019 Uiso 1 1 calc R . .
C10 C 0.5103(6) 0.4875(5) 0.7996(4) 0.0175(14) Uani 1 1 d . . .
H10 H 0.5642 0.5149 0.7699 0.021 Uiso 1 1 calc R . .
C11 C 1.0325(6) 0.2601(5) 0.8906(5) 0.0257(17) Uani 1 1 d . . .
H11 H 1.0322 0.2981 0.8553 0.031 Uiso 1 1 calc R . .
C12 C 0.9127(6) 0.2125(5) 0.8979(4) 0.0202(15) Uani 1 1 d . . .
H12 H 0.8336 0.2177 0.8688 0.024 Uiso 1 1 calc R . .
C13 C 0.9171(6) 0.1568(5) 0.9507(4) 0.0195(15) Uani 1 1 d . . .
C14 C 1.0335(6) 0.1495(5) 0.9931(4) 0.0196(15) Uani 1 1 d . . .
H14 H 1.0368 0.1119 1.0287 0.024 Uiso 1 1 calc R . .
C15 C 1.1472(6) 0.2013(6) 0.9802(5) 0.0286(18) Uani 1 1 d . . .
H15 H 1.2277 0.1975 1.0087 0.034 Uiso 1 1 calc R . .
C16 C 0.6895(7) 0.0375(6) 0.8881(5) 0.043(2) Uani 1 1 d . . .
H16 H 0.6953 0.0166 0.8253 0.052 Uiso 1 1 calc R . .
C17 C 0.5720(7) -0.0048(6) 0.9004(5) 0.041(2) Uani 1 1 d . . .
H17 H 0.4977 -0.0515 0.8458 0.049 Uiso 1 1 calc R . .
C18 C 0.5638(6) 0.0217(5) 0.9928(5) 0.0201(15) Uani 1 1 d . . .
C19 C 0.6747(6) 0.0918(6) 1.0710(5) 0.035(2) Uani 1 1 d . . .
H19 H 0.6729 0.1097 1.1346 0.042 Uiso 1 1 calc R . .
C20 C 0.7898(6) 0.1363(6) 1.0559(5) 0.0304(19) Uani 1 1 d . . .
H20 H 0.8636 0.1861 1.1092 0.037 Uiso 1 1 calc R . .
C21 C 0.7509(6) 0.3993(5) 0.1027(4) 0.0179(14) Uani 1 1 d . . .
C22 C 0.6594(6) 0.3403(5) 0.1246(4) 0.0221(16) Uani 1 1 d . . .
H22 H 0.6730 0.3518 0.1894 0.027 Uiso 1 1 calc R . .
C23 C 0.5435(6) 0.2616(5) 0.0495(5) 0.0215(16) Uani 1 1 d . . .
H23 H 0.4792 0.2245 0.0661 0.026 Uiso 1 1 calc R . .
C24 C 0.5243(6) 0.2391(5) -0.0469(5) 0.0234(16) Uani 1 1 d . . .
H24 H 0.4491 0.1853 -0.0955 0.028 Uiso 1 1 calc R . .
C25 C 0.6182(6) 0.2973(5) -0.0724(4) 0.0164(14) Uani 1 1 d . . .
C26 C 0.7329(6) 0.3802(5) 0.0018(4) 0.0169(14) Uani 1 1 d . . .
C27 C 0.8246(6) 0.4402(5) -0.0240(4) 0.0195(15) Uani 1 1 d . . .
H27 H 0.8979 0.4958 0.0247 0.023 Uiso 1 1 calc R . .
C28 C 0.8061(6) 0.4169(5) -0.1210(5) 0.0220(15) Uani 1 1 d . . .
H28 H 0.8670 0.4574 -0.1372 0.026 Uiso 1 1 calc R . .
C29 C 0.6972(6) 0.3332(5) -0.1962(5) 0.0232(16) Uani 1 1 d . . .
H29 H 0.6879 0.3174 -0.2616 0.028 Uiso 1 1 calc R . .
C30 C 0.6052(6) 0.2753(5) -0.1732(4) 0.0188(15) Uani 1 1 d . . .
C31 C 0.4871(6) 0.1505(5) -0.3398(4) 0.0218(15) Uani 1 1 d . . .
H31A H 0.5685 0.1387 -0.3453 0.026 Uiso 1 1 calc R . .
H31B H 0.4750 0.1964 -0.3679 0.026 Uiso 1 1 calc R . .
C32 C 0.3701(6) 0.0519(5) -0.3925(5) 0.0252(16) Uani 1 1 d . . .
H32A H 0.3717 0.0150 -0.4579 0.030 Uiso 1 1 calc R . .
H32B H 0.3779 0.0109 -0.3578 0.030 Uiso 1 1 calc R . .
C33 C 0.1948(6) 0.0626(6) -0.3226(4) 0.0268(17) Uani 1 1 d . . .
H33A H 0.2478 0.1233 -0.2617 0.032 Uiso 1 1 calc R . .
H33B H 0.1992 0.0037 -0.3129 0.032 Uiso 1 1 calc R . .
C34 C 0.9468(6) 0.9439(6) 0.3519(5) 0.0302(18) Uani 1 1 d . . .
H34A H 0.9863 0.9526 0.3039 0.036 Uiso 1 1 calc R . .
H34B H 0.9978 1.0022 0.4150 0.036 Uiso 1 1 calc R . .
C35 C 1.0820(6) 0.8538(6) 0.3784(5) 0.0314(19) Uani 1 1 d . . .
H35A H 1.1420 0.9173 0.4343 0.038 Uiso 1 1 calc R . .
H35B H 1.1109 0.8484 0.3223 0.038 Uiso 1 1 calc R . .
C36 C 1.0867(6) 0.7662(6) 0.4003(5) 0.0283(18) Uani 1 1 d . . .
H36A H 1.1757 0.7639 0.4104 0.034 Uiso 1 1 calc R . .
H36B H 1.0660 0.7750 0.4600 0.034 Uiso 1 1 calc R . .
C37 C 1.0179(6) 0.5892(6) 0.3287(5) 0.0279(17) Uani 1 1 d . . .
H37A H 1.0425 0.6008 0.3967 0.033 Uiso 1 1 calc R . .
H37B H 1.0910 0.5796 0.3052 0.033 Uiso 1 1 calc R . .
C38 C 0.8940(6) 0.4962(6) 0.2681(4) 0.0260(17) Uani 1 1 d . . .
H38A H 0.9076 0.4380 0.2748 0.031 Uiso 1 1 calc R . .
H38B H 0.8202 0.5063 0.2902 0.031 Uiso 1 1 calc R . .
C39 C 0.040(3) 0.441(2) 0.4632(19) 0.104(9) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 N1 2.336(5) . ?
Hg1 Br2 2.5125(7) . ?
Hg1 Br1 2.5300(8) . ?
Hg1 Br3 2.6845(7) . ?
Hg2 Br5 2.5327(8) . ?
Hg2 Br4 2.5519(8) . ?
Hg2 Br6 2.5772(8) . ?
Hg2 Br3 2.8399(7) . ?
O1 C21 1.357(7) . ?
O1 C38 1.432(6) . ?
O2 C36 1.408(8) . ?
O2 C37 1.423(8) . ?
O3 C35 1.410(6) . ?
O3 C34 1.421(7) . ?
O4 C32 1.435(7) . ?
O4 C33 1.437(6) . ?
O5 C30 1.356(7) . ?
O5 C31 1.443(7) . ?
O6 C39 1.43(3) . ?
O6 C39 1.52(2) 2_566 ?
N1 C5 1.329(8) . ?
N1 C1 1.341(7) . ?
N2 C6 1.359(6) . ?
N2 C10 1.350(7) . ?
N2 C3 1.454(7) . ?
N3 C15 1.315(7) . ?
N3 C11 1.330(7) . ?
N4 C16 1.328(8) . ?
N4 C20 1.341(7) . ?
N4 C13 1.459(7) . ?
C1 C2 1.385(7) . ?
C2 C3 1.370(9) . ?
C3 C4 1.389(8) . ?
C4 C5 1.373(8) . ?
C6 C7 1.360(7) . ?
C7 C8 1.385(8) . ?
C8 C9 1.398(7) . ?
C8 C8 1.493(11) 2_667 ?
C9 C10 1.364(7) . ?
C11 C12 1.381(8) . ?
C12 C13 1.381(8) . ?
C13 C14 1.365(8) . ?
C14 C15 1.393(8) . ?
C16 C17 1.374(8) . ?
C17 C18 1.371(8) . ?
C18 C19 1.368(9) . ?
C18 C18 1.489(11) 2_657 ?
C19 C20 1.385(8) . ?
C21 C22 1.354(8) . ?
C21 C26 1.446(7) . ?
C22 C23 1.413(8) . ?
C23 C24 1.364(8) . ?
C24 C25 1.403(8) . ?
C25 C26 1.423(8) . ?
C25 C30 1.443(8) . ?
C26 C27 1.406(8) . ?
C27 C28 1.372(8) . ?
C28 C29 1.402(9) . ?
C29 C30 1.360(8) . ?
C31 C32 1.499(8) . ?
C33 C34 1.495(8) 2_665 ?
C34 C33 1.495(8) 2_665 ?
C35 C36 1.499(9) . ?
C37 C38 1.499(9) . ?
C39 O6 1.52(2) 2_566 ?

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 Hg1 Br2 115.40(14) . . ?
N1 Hg1 Br1 104.41(14) . . ?
Br2 Hg1 Br1 122.51(3) . . ?
N1 Hg1 Br3 97.18(12) . . ?
Br2 Hg1 Br3 103.30(2) . . ?
Br1 Hg1 Br3 111.20(3) . . ?
Br5 Hg2 Br4 114.92(2) . . ?
Br5 Hg2 Br6 113.38(3) . . ?
Br4 Hg2 Br6 121.61(3) . . ?
Br5 Hg2 Br3 107.49(2) . . ?
Br4 Hg2 Br3 100.17(2) . . ?
Br6 Hg2 Br3 94.73(2) . . ?
Hg1 Br3 Hg2 107.37(2) . . ?
C21 O1 C38 116.2(5) . . ?
C36 O2 C37 110.9(5) . . ?
C35 O3 C34 110.9(5) . . ?
C32 O4 C33 114.2(4) . . ?
C30 O5 C31 117.5(4) . . ?
C39 O6 C39 98.6(18) . 2_566 ?
C5 N1 C1 118.5(5) . . ?
C5 N1 Hg1 122.1(4) . . ?
C1 N1 Hg1 119.3(4) . . ?
C6 N2 C10 119.7(5) . . ?
C6 N2 C3 119.4(5) . . ?
C10 N2 C3 120.9(5) . . ?
C15 N3 C11 117.0(5) . . ?
C16 N4 C20 120.2(5) . . ?
C16 N4 C13 120.8(5) . . ?
C20 N4 C13 119.0(5) . . ?
N1 C1 C2 122.3(6) . . ?
C3 C2 C1 117.6(6) . . ?
C2 C3 C4 121.2(5) . . ?
C2 C3 N2 119.6(5) . . ?
C4 C3 N2 119.3(6) . . ?
C5 C4 C3 116.7(6) . . ?
N1 C5 C4 123.7(6) . . ?
N2 C6 C7 120.3(6) . . ?
C6 C7 C8 121.8(5) . . ?
C7 C8 C9 116.3(5) . . ?
C7 C8 C8 121.9(6) . 2_667 ?
C9 C8 C8 121.8(7) . 2_667 ?
C10 C9 C8 121.0(6) . . ?
N2 C10 C9 120.8(5) . . ?
N3 C11 C12 124.4(6) . . ?
C13 C12 C11 116.2(5) . . ?
C14 C13 C12 121.6(5) . . ?
C14 C13 N4 119.4(5) . . ?
C12 C13 N4 119.0(5) . . ?
C13 C14 C15 116.4(6) . . ?
N3 C15 C14 124.4(6) . . ?
N4 C16 C17 121.0(6) . . ?
C18 C17 C16 120.2(7) . . ?
C17 C18 C19 118.0(6) . . ?
C17 C18 C18 120.8(8) . 2_657 ?
C19 C18 C18 121.1(7) . 2_657 ?
C18 C19 C20 120.3(6) . . ?
N4 C20 C19 120.2(6) . . ?
C22 C21 O1 126.4(5) . . ?
C22 C21 C26 120.2(6) . . ?
O1 C21 C26 113.3(5) . . ?
C21 C22 C23 120.5(6) . . ?
C24 C23 C22 121.2(6) . . ?
C23 C24 C25 119.8(6) . . ?
C24 C25 C26 120.2(5) . . ?
C24 C25 C30 122.3(6) . . ?
C26 C25 C30 117.4(5) . . ?
C27 C26 C25 120.0(5) . . ?
C27 C26 C21 122.1(6) . . ?
C25 C26 C21 117.9(5) . . ?
C28 C27 C26 120.1(6) . . ?
C27 C28 C29 121.4(6) . . ?
C30 C29 C28 119.8(6) . . ?
O5 C30 C29 125.8(5) . . ?
O5 C30 C25 112.9(5) . . ?
C29 C30 C25 121.3(6) . . ?
O5 C31 C32 107.0(5) . . ?
O4 C32 C31 112.7(6) . . ?
O4 C33 C34 107.6(5) . 2_665 ?
O3 C34 C33 109.6(5) . 2_665 ?
O3 C35 C36 109.6(5) . . ?
O2 C36 C35 109.7(5) . . ?
O2 C37 C38 109.1(5) . . ?
O1 C38 C37 108.4(5) . . ?
O6 C39 O6 81.4(18) . 2_566 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.507
_refine_diff_density_min         -2.132
_refine_diff_density_rms         0.253
_database_code_depnum_ccdc_archive 'CCDC 997304'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1[Hg2I6]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H52 Hg2 I6 N4 O8'
_chemical_formula_weight         2023.56

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'
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'
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'

_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                   10.0390(10)
_cell_length_b                   11.7664(12)
_cell_length_c                   13.0968(13)
_cell_angle_alpha                93.757(6)
_cell_angle_beta                 106.866(6)
_cell_angle_gamma                105.202(7)
_cell_volume                     1411.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5310
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      22.62

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             934
_exptl_absorpt_coefficient_mu    8.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39316
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         30.60
_reflns_number_total             8564
_reflns_number_gt                5312
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1784P)²+4.6687P] 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       0.0057(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8564
_refine_ls_number_parameters     326
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2910
_refine_ls_wR_factor_gt          0.2520
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.41536(6) 0.83702(4) 0.42577(4) 0.0467(2) Uani 1 1 d . . .
I1 I 0.5741(4) 1.03615(16) 0.37827(17) 0.1613(12) Uani 1 1 d . . .
I2 I 0.55262(12) 0.67390(10) 0.47127(8) 0.0613(3) Uani 1 1 d . . .
I3 I 0.13842(19) 0.7954(3) 0.30912(12) 0.1348(9) Uani 1 1 d . . .
O1 O 0.8805(11) 0.9659(8) 1.2217(7) 0.051(2) Uani 1 1 d . . .
O2 O 0.0598(14) 0.8048(9) 0.6362(9) 0.072(3) Uani 1 1 d . . .
O3 O 0.1542(11) 0.5926(9) 0.6598(8) 0.055(2) Uani 1 1 d . . .
O4 O 0.4479(9) 0.6483(8) 0.8279(7) 0.047(2) Uani 1 1 d . . .
N1 N 1.2255(12) 0.4978(11) 0.1075(11) 0.060(3) Uani 1 1 d D . .
N2 N 0.8205(11) 0.2357(8) 0.0464(8) 0.040(2) Uani 1 1 d . . .
C1 C 1.1439(17) 0.4928(13) 0.1780(13) 0.071(5) Uani 1 1 d D . .
H1 H 1.1810 0.5485 0.2405 0.085 Uiso 1 1 calc R . .
C2 C 1.0142(16) 0.4111(13) 0.1598(13) 0.057(4) Uani 1 1 d . . .
H2 H 0.9626 0.4120 0.2083 0.069 Uiso 1 1 calc R . .
C3 C 0.9572(14) 0.3242(11) 0.0668(11) 0.045(3) Uani 1 1 d . . .
C4 C 1.0366(15) 0.3278(12) -0.0043(13) 0.051(3) Uani 1 1 d . . .
H4 H 1.0012 0.2708 -0.0660 0.061 Uiso 1 1 calc R . .
C5 C 1.1642(14) 0.4125(13) 0.0145(13) 0.063(4) Uani 1 1 d D . .
H5 H 1.2132 0.4144 -0.0360 0.076 Uiso 1 1 calc R . .
C6 C 0.7807(15) 0.1912(12) 0.1300(11) 0.051(3) Uani 1 1 d . . .
H6 H 0.8404 0.2229 0.2004 0.061 Uiso 1 1 calc R . .
C7 C 0.6579(15) 0.1031(11) 0.1135(10) 0.045(3) Uani 1 1 d . . .
H7 H 0.6340 0.0768 0.1731 0.054 Uiso 1 1 calc R . .
C8 C 0.5649(14) 0.0495(10) 0.0115(10) 0.040(2) Uani 1 1 d . . .
C9 C 0.6084(13) 0.0972(11) -0.0772(10) 0.040(2) Uani 1 1 d . . .
H9 H 0.5535 0.0638 -0.1482 0.048 Uiso 1 1 calc R . .
C10 C 0.7297(12) 0.1910(10) -0.0555(9) 0.038(2) Uani 1 1 d . . .
H10 H 0.7515 0.2260 -0.1126 0.045 Uiso 1 1 calc R . .
C11 C 0.7686(14) 0.8658(10) 1.1702(10) 0.043(3) Uani 1 1 d . . .
C12 C 0.6881(16) 0.7873(11) 1.2190(11) 0.048(3) Uani 1 1 d . . .
H12 H 0.7125 0.7980 1.2939 0.057 Uiso 1 1 calc R . .
C13 C 0.5715(15) 0.6930(11) 1.1575(10) 0.044(3) Uani 1 1 d . . .
H13 H 0.5204 0.6404 1.1926 0.053 Uiso 1 1 calc R . .
C14 C 0.5286(15) 0.6738(11) 1.0486(12) 0.046(3) Uani 1 1 d . . .
H14 H 0.4465 0.6118 1.0095 0.056 Uiso 1 1 calc R . .
C15 C 0.6112(14) 0.7499(11) 0.9951(10) 0.042(3) Uani 1 1 d . . .
C16 C 0.7368(13) 0.8448(10) 1.0584(10) 0.040(2) Uani 1 1 d . . .
C17 C 0.8232(14) 0.9195(11) 1.0052(10) 0.042(2) Uani 1 1 d . . .
H17 H 0.9034 0.9827 1.0451 0.050 Uiso 1 1 calc R . .
C18 C 0.7863(13) 0.8967(11) 0.8919(9) 0.043(3) Uani 1 1 d . . .
H18 H 0.8443 0.9435 0.8573 0.052 Uiso 1 1 calc R . .
C19 C 0.6617(13) 0.8034(12) 0.8304(10) 0.044(3) Uani 1 1 d . . .
H19 H 0.6384 0.7896 0.7557 0.053 Uiso 1 1 calc R . .
C20 C 0.5752(14) 0.7332(11) 0.8792(10) 0.043(3) Uani 1 1 d . . .
C21 C 0.4137(15) 0.6183(13) 0.7115(10) 0.050(3) Uani 1 1 d . . .
H21A H 0.4818 0.5802 0.6958 0.060 Uiso 1 1 calc R . .
H21B H 0.4192 0.6895 0.6777 0.060 Uiso 1 1 calc R . .
C22 C 0.2645(16) 0.5362(13) 0.6712(12) 0.056(3) Uani 1 1 d . . .
H22A H 0.2505 0.4925 0.6017 0.067 Uiso 1 1 calc R . .
H22B H 0.2541 0.4788 0.7205 0.067 Uiso 1 1 calc R . .
C23 C 0.1207(18) 0.6449(14) 0.5616(12) 0.058(4) Uani 1 1 d . . .
H23A H 0.2067 0.7049 0.5597 0.070 Uiso 1 1 calc R . .
H23B H 0.0897 0.5838 0.4991 0.070 Uiso 1 1 calc R . .
C24 C 0.0059(15) 0.6983(13) 0.5592(11) 0.055(3) Uani 1 1 d . . .
H24A H -0.0331 0.7167 0.4875 0.066 Uiso 1 1 calc R . .
H24B H -0.0723 0.6422 0.5755 0.066 Uiso 1 1 calc R . .
C25 C 1.029(2) 1.1164(16) 1.3748(12) 0.073(5) Uani 1 1 d . . .
H25A H 1.0890 1.1253 1.4494 0.088 Uiso 1 1 calc R . .
H25B H 1.0924 1.1341 1.3307 0.088 Uiso 1 1 calc R . .
C26 C 0.924(2) 0.9869(14) 1.3368(11) 0.075(5) Uani 1 1 d . . .
H26A H 0.9730 0.9300 1.3667 0.090 Uiso 1 1 calc R . .
H26B H 0.8394 0.9786 1.3606 0.090 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 I2 2.6454(10) . ?
Hg1 I3 2.6508(17) . ?
Hg1 I1 2.6880(19) . ?
Hg1 I1 2.8431(17) 2_676 ?
I1 Hg1 2.8430(17) 2_676 ?
O1 C11 1.367(15) . ?
O1 C26 1.426(15) . ?
O2 C24 1.429(16) . ?
O2 C25 1.43(2) 2_677 ?
O3 C22 1.411(19) . ?
O3 C23 1.451(18) . ?
O4 C20 1.351(14) . ?
O4 C21 1.459(15) . ?
N1 C1 1.395(16) . ?
N1 C5 1.397(15) . ?
N2 C10 1.356(15) . ?
N2 C6 1.361(17) . ?
N2 C3 1.429(16) . ?
C1 C2 1.345(19) . ?
C2 C3 1.41(2) . ?
C3 C4 1.386(19) . ?
C4 C5 1.345(19) . ?
C6 C7 1.336(19) . ?
C7 C8 1.383(18) . ?
C8 C8 1.44(2) 2_655 ?
C8 C9 1.451(16) . ?
C9 C10 1.354(16) . ?
C11 C12 1.380(18) . ?
C11 C16 1.395(17) . ?
C12 C13 1.380(19) . ?
C13 C14 1.350(19) . ?
C14 C15 1.419(18) . ?
C15 C16 1.435(17) . ?
C15 C20 1.441(17) . ?
C16 C17 1.428(17) . ?
C17 C18 1.411(17) . ?
C18 C19 1.413(17) . ?
C19 C20 1.364(18) . ?
C21 C22 1.473(19) . ?
C23 C24 1.44(2) . ?
C25 O2 1.43(2) 2_677 ?
C25 C26 1.56(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
I2 Hg1 I3 125.83(7) . . ?
I2 Hg1 I1 114.18(8) . . ?
I3 Hg1 I1 108.80(9) . . ?
I2 Hg1 I1 109.06(7) . 2_676 ?
I3 Hg1 I1 101.44(8) . 2_676 ?
I1 Hg1 I1 90.91(5) . 2_676 ?
Hg1 I1 Hg1 89.09(5) . 2_676 ?
C11 O1 C26 117.1(12) . . ?
C24 O2 C25 117.1(12) . 2_677 ?
C22 O3 C23 114.3(12) . . ?
C20 O4 C21 115.9(10) . . ?
C1 N1 C5 116.0(12) . . ?
C10 N2 C6 118.3(10) . . ?
C10 N2 C3 121.6(10) . . ?
C6 N2 C3 120.1(11) . . ?
C2 C1 N1 123.2(14) . . ?
C1 C2 C3 119.4(15) . . ?
C4 C3 C2 118.2(13) . . ?
C4 C3 N2 121.3(12) . . ?
C2 C3 N2 120.5(12) . . ?
C5 C4 C3 121.0(15) . . ?
C4 C5 N1 122.1(14) . . ?
C7 C6 N2 121.6(12) . . ?
C6 C7 C8 122.8(12) . . ?
C7 C8 C8 125.3(13) . 2_655 ?
C7 C8 C9 115.2(11) . . ?
C8 C8 C9 119.5(14) 2_655 . ?
C10 C9 C8 119.4(11) . . ?
C9 C10 N2 122.4(10) . . ?
O1 C11 C12 125.7(12) . . ?
O1 C11 C16 114.9(11) . . ?
C12 C11 C16 119.3(11) . . ?
C11 C12 C13 120.4(12) . . ?
C14 C13 C12 122.8(12) . . ?
C13 C14 C15 118.7(13) . . ?
C14 C15 C16 118.9(12) . . ?
C14 C15 C20 122.1(12) . . ?
C16 C15 C20 118.9(12) . . ?
C11 C16 C17 121.2(11) . . ?
C11 C16 C15 119.5(11) . . ?
C17 C16 C15 119.3(11) . . ?
C18 C17 C16 119.6(12) . . ?
C17 C18 C19 120.5(12) . . ?
C20 C19 C18 120.9(12) . . ?
O4 C20 C19 125.7(11) . . ?
O4 C20 C15 113.5(11) . . ?
C19 C20 C15 120.8(12) . . ?
O4 C21 C22 106.5(11) . . ?
O3 C22 C21 114.3(12) . . ?
C24 C23 O3 108.8(14) . . ?
O2 C24 C23 110.6(12) . . ?
O2 C25 C26 107.1(15) 2_677 . ?
O1 C26 C25 107.3(13) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        30.60
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         3.308
_refine_diff_density_min         -5.544
_refine_diff_density_rms         0.359
_database_code_depnum_ccdc_archive 'CCDC 997305'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2[Hg2I6]+3CH3OH

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C59 H72 Hg2 I6 N4 O13'
_chemical_formula_weight         2207.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_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                   11.3555(2)
_cell_length_b                   12.1082(2)
_cell_length_c                   14.2423(3)
_cell_angle_alpha                103.3720(10)
_cell_angle_beta                 97.0080(10)
_cell_angle_gamma                115.6650(10)
_cell_volume                     1661.16(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9974
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      30.49

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    7.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1542
_exptl_absorpt_correction_T_max  0.2569
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            94488
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         30.57
_reflns_number_total             10141
_reflns_number_gt                9381
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.5000P] 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         10141
_refine_ls_number_parameters     453
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.1197
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.689033(15) 0.521927(13) 0.494112(11) 0.02693(6) Uani 1 1 d . . .
I1 I 0.75071(3) 0.33541(3) 0.41487(2) 0.03731(9) Uani 1 1 d . . .
I2 I 0.54096(2) 0.50244(2) 0.645480(16) 0.02137(7) Uani 1 1 d . . .
I3 I 0.89671(2) 0.76544(2) 0.55429(2) 0.02786(7) Uani 1 1 d . . .
O1 O 0.6386(3) 0.1359(3) 0.8644(2) 0.0235(5) Uani 1 1 d . . .
O2 O 0.7198(6) 0.3417(6) 0.7839(5) 0.0310(12) Uani 0.50 1 d PD A 1
O3 O 0.9839(9) 0.3688(8) 0.7799(7) 0.0366(17) Uani 0.50 1 d PD A 1
C23 C 0.7979(8) -0.3917(7) 1.2530(6) 0.0259(15) Uani 0.50 1 d PD . 1
H23A H 0.7031 -0.4529 1.2405 0.031 Uiso 0.50 1 calc PR . 1
H23B H 0.8402 -0.3607 1.3238 0.031 Uiso 0.50 1 calc PR . 1
C24 C 1.1290(10) 0.4504(10) 0.8091(8) 0.038(2) Uani 0.50 1 d PD . 1
H24A H 1.1624 0.4640 0.8791 0.045 Uiso 0.50 1 calc PR . 1
H24B H 1.1500 0.5340 0.8014 0.045 Uiso 0.50 1 calc PR . 1
C25 C 0.9146(12) 0.4055(11) 0.7119(10) 0.034(3) Uani 0.50 1 d PD A 1
H25A H 0.9396 0.3932 0.6490 0.041 Uiso 0.50 1 calc PR A 1
H25B H 0.9392 0.4959 0.7396 0.041 Uiso 0.50 1 calc PR A 1
C26 C 0.7643(10) 0.3219(14) 0.6953(7) 0.034(2) Uani 0.50 1 d PD A 1
H26A H 0.7163 0.3405 0.6453 0.041 Uiso 0.50 1 calc PR A 1
H26B H 0.7419 0.2318 0.6697 0.041 Uiso 0.50 1 calc PR A 1
C27 C 0.5843(10) 0.2515(8) 0.7709(8) 0.0254(18) Uani 0.50 1 d PD A 1
H27A H 0.5322 0.2431 0.7079 0.030 Uiso 0.50 1 calc PR A 1
H27B H 0.5508 0.2858 0.8234 0.030 Uiso 0.50 1 calc PR A 1
O102 O 0.7474(5) 0.2720(5) 0.7351(4) 0.0169(9) Uani 0.50 1 d PD A 2
O103 O 1.0251(8) 0.4125(9) 0.7651(7) 0.0363(18) Uani 0.50 1 d PD A 2
C123 C 0.7626(10) -0.4292(8) 1.1819(9) 0.038(2) Uani 0.50 1 d PD . 2
H12A H 0.7737 -0.4605 1.1162 0.046 Uiso 0.50 1 calc PR . 2
H12B H 0.6678 -0.4738 1.1811 0.046 Uiso 0.50 1 calc PR . 2
C124 C 1.1518(9) 0.4471(10) 0.7393(7) 0.0365(19) Uani 0.50 1 d PD . 2
H12C H 1.1940 0.5362 0.7397 0.044 Uiso 0.50 1 calc PR . 2
H12D H 1.1392 0.3916 0.6736 0.044 Uiso 0.50 1 calc PR . 2
C125 C 0.9367(12) 0.4034(13) 0.6819(8) 0.030(3) Uani 0.50 1 d PD A 2
H12E H 0.9167 0.3289 0.6263 0.036 Uiso 0.50 1 calc PR A 2
H12F H 0.9781 0.4802 0.6621 0.036 Uiso 0.50 1 calc PR A 2
C126 C 0.8094(8) 0.3900(8) 0.7103(6) 0.0195(14) Uani 0.50 1 d PD A 2
H12G H 0.8300 0.4634 0.7671 0.023 Uiso 0.50 1 calc PR A 2
H12H H 0.7480 0.3874 0.6551 0.023 Uiso 0.50 1 calc PR A 2
C127 C 0.6195(9) 0.2433(8) 0.7495(7) 0.0190(16) Uani 0.50 1 d PD A 2
H12I H 0.5622 0.2373 0.6901 0.023 Uiso 0.50 1 calc PR A 2
H12J H 0.6263 0.3119 0.8047 0.023 Uiso 0.50 1 calc PR A 2
O4 O 0.8163(4) -0.2854(4) 1.2139(5) 0.0652(16) Uani 1 1 d D . .
O5 O 0.7221(3) -0.1226(3) 1.1563(2) 0.0260(5) Uani 1 1 d . . .
O6 O 0.7793(4) 0.5987(4) 0.9247(4) 0.0482(9) Uani 1 1 d . . .
H6 H 0.8005 0.5412 0.9194 0.072 Uiso 1 1 calc R . .
O7 O 0.8712(9) 0.4326(9) 0.9458(6) 0.0479(18) Uani 0.50 1 d P . .
N1 N 0.6543(4) 0.9567(4) 0.4802(3) 0.0303(7) Uani 1 1 d . . .
N2 N 0.8332(3) 0.9850(3) 0.7687(2) 0.0193(5) Uani 1 1 d . . .
C1 C 0.5874(4) 0.8752(4) 0.5269(3) 0.0286(8) Uani 1 1 d . . .
H1 H 0.4999 0.8104 0.4937 0.034 Uiso 1 1 calc R . .
C2 C 0.6407(4) 0.8813(4) 0.6227(3) 0.0229(7) Uani 1 1 d . . .
H2 H 0.5903 0.8228 0.6530 0.027 Uiso 1 1 calc R . .
C3 C 0.7710(4) 0.9773(3) 0.6709(3) 0.0210(6) Uani 1 1 d . . .
C4 C 0.8444(4) 1.0640(4) 0.6246(3) 0.0244(7) Uani 1 1 d . . .
H4 H 0.9324 1.1291 0.6559 0.029 Uiso 1 1 calc R . .
C5 C 0.7803(5) 1.0492(4) 0.5292(3) 0.0296(8) Uani 1 1 d . . .
H5 H 0.8279 1.1071 0.4976 0.036 Uiso 1 1 calc R . .
C6 C 0.8067(4) 0.8749(3) 0.7903(3) 0.0218(6) Uani 1 1 d . . .
H6A H 0.7452 0.7956 0.7433 0.026 Uiso 1 1 calc R . .
C7 C 0.8692(4) 0.8784(3) 0.8807(3) 0.0205(6) Uani 1 1 d . . .
H7 H 0.8487 0.8017 0.8946 0.025 Uiso 1 1 calc R . .
C8 C 0.9637(3) 0.9965(3) 0.9520(3) 0.0182(6) Uani 1 1 d . . .
C9 C 0.9870(4) 1.1086(3) 0.9279(3) 0.0212(6) Uani 1 1 d . . .
H9 H 1.0481 1.1891 0.9736 0.025 Uiso 1 1 calc R . .
C10 C 0.9197(4) 1.1009(3) 0.8366(3) 0.0225(7) Uani 1 1 d . . .
H10 H 0.9343 1.1762 0.8221 0.027 Uiso 1 1 calc R . .
C11 C 0.6099(4) 0.0304(4) 0.8949(3) 0.0195(6) Uani 1 1 d . . .
C12 C 0.5152(4) -0.0937(4) 0.8391(3) 0.0219(6) Uani 1 1 d . . .
H12 H 0.4640 -0.1104 0.7764 0.026 Uiso 1 1 calc R . .
C13 C 0.4964(4) -0.1956(4) 0.8780(3) 0.0249(7) Uani 1 1 d . . .
H13 H 0.4330 -0.2798 0.8397 0.030 Uiso 1 1 calc R . .
C14 C 0.5694(4) -0.1735(4) 0.9708(3) 0.0237(7) Uani 1 1 d . . .
H14 H 0.5548 -0.2420 0.9953 0.028 Uiso 1 1 calc R . .
C15 C 0.6674(3) -0.0456(3) 1.0291(3) 0.0184(6) Uani 1 1 d . . .
C16 C 0.6877(4) 0.0583(3) 0.9921(3) 0.0189(6) Uani 1 1 d . . .
C17 C 0.7829(4) 0.1869(4) 1.0505(3) 0.0229(7) Uani 1 1 d . . .
H17 H 0.7969 0.2551 1.0257 0.027 Uiso 1 1 calc R . .
C18 C 0.8542(4) 0.2094(4) 1.1438(3) 0.0268(7) Uani 1 1 d . . .
H18 H 0.9164 0.2939 1.1821 0.032 Uiso 1 1 calc R . .
C19 C 0.8362(4) 0.1088(4) 1.1834(3) 0.0253(7) Uani 1 1 d . . .
H19 H 0.8852 0.1264 1.2472 0.030 Uiso 1 1 calc R . .
C20 C 0.7447(4) -0.0164(4) 1.1262(3) 0.0208(6) Uani 1 1 d . . .
C21 C 0.7902(4) -0.0984(5) 1.2560(3) 0.0290(8) Uani 1 1 d . . .
H21A H 0.7624 -0.0489 1.3033 0.035 Uiso 1 1 calc R . .
H21B H 0.8871 -0.0493 1.2658 0.035 Uiso 1 1 calc R . .
C22 C 0.7540(5) -0.2261(5) 1.2714(4) 0.0396(11) Uani 1 1 d . . .
H22A H 0.7849 -0.2138 1.3415 0.048 Uiso 1 1 calc R . .
H22B H 0.6567 -0.2806 1.2509 0.048 Uiso 1 1 calc R . .
C28 C 0.5582(4) 0.1178(4) 0.7713(3) 0.0216(6) Uani 1 1 d D . .
H28A H 0.4633 0.0632 0.7654 0.026 Uiso 1 1 calc R A 1
H28B H 0.5841 0.0777 0.7163 0.026 Uiso 1 1 calc R A 1
C29 C 0.6552(7) 0.5597(6) 0.9515(5) 0.0498(13) Uani 1 1 d . . .
H29A H 0.6644 0.6254 1.0091 0.075 Uiso 1 1 calc R . .
H29B H 0.6299 0.4804 0.9664 0.075 Uiso 1 1 calc R . .
H29C H 0.5867 0.5469 0.8971 0.075 Uiso 1 1 calc R . .
C30 C 0.9851(19) 0.5226(19) 1.0019(18) 0.074(6) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 I1 2.6923(3) . ?
Hg1 I3 2.7027(3) . ?
Hg1 I2 2.8821(3) . ?
Hg1 I2 2.9419(3) 2_666 ?
I2 Hg1 2.9419(3) 2_666 ?
O1 C11 1.362(4) . ?
O1 C28 1.427(4) . ?
O2 C27 1.405(11) . ?
O2 C26 1.423(10) . ?
O3 C25 1.439(12) . ?
O3 C24 1.448(12) . ?
C23 O4 1.461(7) . ?
C23 C24 1.542(11) 2_757 ?
C24 C23 1.542(11) 2_757 ?
C25 C26 1.513(13) . ?
C27 C28 1.516(9) . ?
O102 C127 1.393(9) . ?
O102 C126 1.444(8) . ?
O103 C125 1.405(13) . ?
O103 C124 1.435(11) . ?
C123 O4 1.502(9) . ?
C123 C124 1.509(12) 2_757 ?
C124 C123 1.509(12) 2_757 ?
C125 C126 1.499(12) . ?
C127 C28 1.498(9) . ?
O4 C22 1.413(7) . ?
O5 C20 1.377(4) . ?
O5 C21 1.429(5) . ?
O6 C29 1.412(8) . ?
O7 C30 1.27(2) . ?
O7 C30 1.503(19) 2_767 ?
N1 C1 1.331(6) . ?
N1 C5 1.340(6) . ?
N2 C10 1.348(5) . ?
N2 C6 1.352(5) . ?
N2 C3 1.446(5) . ?
C1 C2 1.396(6) . ?
C2 C3 1.381(5) . ?
C3 C4 1.388(5) . ?
C4 C5 1.393(6) . ?
C6 C7 1.374(5) . ?
C7 C8 1.400(5) . ?
C8 C9 1.398(5) . ?
C8 C8 1.473(7) 2_777 ?
C9 C10 1.388(5) . ?
C11 C12 1.373(5) . ?
C11 C16 1.428(5) . ?
C12 C13 1.411(5) . ?
C13 C14 1.372(6) . ?
C14 C15 1.419(5) . ?
C15 C16 1.414(5) . ?
C15 C20 1.420(5) . ?
C16 C17 1.417(5) . ?
C17 C18 1.369(5) . ?
C18 C19 1.405(6) . ?
C19 C20 1.379(6) . ?
C21 C22 1.497(6) . ?
C30 C30 0.75(4) 2_767 ?
C30 O7 1.503(19) 2_767 ?

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
I1 Hg1 I3 115.158(10) . . ?
I1 Hg1 I2 121.049(11) . . ?
I3 Hg1 I2 107.118(9) . . ?
I1 Hg1 I2 109.849(9) . 2_666 ?
I3 Hg1 I2 110.907(9) . 2_666 ?
I2 Hg1 I2 89.925(7) . 2_666 ?
Hg1 I2 Hg1 90.075(8) . 2_666 ?
C11 O1 C28 117.8(3) . . ?
C27 O2 C26 112.2(8) . . ?
C25 O3 C24 113.4(9) . . ?
O4 C23 C24 100.1(7) . 2_757 ?
O3 C24 C23 112.5(8) . 2_757 ?
O3 C25 C26 108.2(10) . . ?
O2 C26 C25 112.8(9) . . ?
O2 C27 C28 115.9(7) . . ?
C127 O102 C126 112.3(6) . . ?
C125 O103 C124 105.4(9) . . ?
O4 C123 C124 103.1(8) . 2_757 ?
O103 C124 C123 105.4(8) . 2_757 ?
O103 C125 C126 108.1(8) . . ?
O102 C126 C125 108.7(8) . . ?
O102 C127 C28 109.9(6) . . ?
C22 O4 C23 102.0(5) . . ?
C22 O4 C123 121.5(5) . . ?
C23 O4 C123 37.8(5) . . ?
C20 O5 C21 117.0(3) . . ?
C30 O7 C30 30.1(17) . 2_767 ?
C1 N1 C5 117.1(4) . . ?
C10 N2 C6 120.5(3) . . ?
C10 N2 C3 120.1(3) . . ?
C6 N2 C3 119.4(3) . . ?
N1 C1 C2 123.9(4) . . ?
C3 C2 C1 117.5(4) . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 N2 119.8(3) . . ?
C4 C3 N2 119.8(3) . . ?
C3 C4 C5 117.0(4) . . ?
N1 C5 C4 124.1(4) . . ?
N2 C6 C7 120.9(3) . . ?
C6 C7 C8 120.6(3) . . ?
C9 C8 C7 117.0(3) . . ?
C9 C8 C8 121.1(4) . 2_777 ?
C7 C8 C8 121.9(4) . 2_777 ?
C10 C9 C8 120.6(3) . . ?
N2 C10 C9 120.3(3) . . ?
O1 C11 C12 124.5(3) . . ?
O1 C11 C16 114.3(3) . . ?
C12 C11 C16 121.2(3) . . ?
C11 C12 C13 119.3(4) . . ?
C14 C13 C12 121.5(4) . . ?
C13 C14 C15 119.6(3) . . ?
C16 C15 C14 120.0(3) . . ?
C16 C15 C20 117.8(3) . . ?
C14 C15 C20 122.2(3) . . ?
C15 C16 C17 120.6(3) . . ?
C15 C16 C11 118.4(3) . . ?
C17 C16 C11 121.0(3) . . ?
C18 C17 C16 119.0(4) . . ?
C17 C18 C19 122.0(4) . . ?
C20 C19 C18 118.9(3) . . ?
O5 C20 C19 123.8(3) . . ?
O5 C20 C15 114.6(3) . . ?
C19 C20 C15 121.6(3) . . ?
O5 C21 C22 107.8(4) . . ?
O4 C22 C21 108.4(4) . . ?
O1 C28 C127 107.4(4) . . ?
O1 C28 C27 106.0(4) . . ?
C127 C28 C27 21.3(3) . . ?
C30 C30 O7 92(4) 2_767 . ?
C30 C30 O7 58(3) 2_767 2_767 ?
O7 C30 O7 149.9(17) . 2_767 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.878
_refine_diff_density_min         -3.494
_refine_diff_density_rms         0.270
_database_code_depnum_ccdc_archive 'CCDC 997306'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_PyBP[CdI4]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H16 Cd I4 N4'
_chemical_formula_weight         932.37

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'
Cd Cd -0.8075 1.2024 '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   'P2(1)/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                   10.2446(9)
_cell_length_b                   16.4684(14)
_cell_length_c                   14.9546(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2523.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3343
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.24

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    5.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4402
_exptl_absorpt_correction_T_max  0.8458
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 The A- and B-level alerts in the CheckCIF appear due to the
following reason. When the unit cell of the
crystal was measured, all three angles were very close to 90 degrees, therefore the data was collected with orthorhombic settings. However, it was impossible to solve the structure in an orthorhombic space group. Upon considering a lower symmetry setting (monoclinic), a solution was immediately found in the space group P21/n. Unfortunately, since the data set was collected considering an orthorhombic cell, there is not enough data for an ideal refinement in the lower symmetry monoclinic cell,
leading to the CheckCIF alerts. Despite this shortcoming, the
final refinement values are as good as or even better than some
of the ones for the other structures reported herein. Indeed,
the data converged to a final R value of 4.2% (Rw  = 8.9%), residual max/min electron density less than 1e/A3, error on bond lengths: 0.001 angstrom, good thermal ellipsoids.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16113
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_sigmaI/netI    0.2151
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         30.69
_reflns_number_total             5724
_reflns_number_gt                2527
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.8151P] 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         5724
_refine_ls_number_parameters     262
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1345
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   0.555
_refine_ls_restrained_S_all      0.554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.81620(8) 0.20967(4) 0.80355(4) 0.02842(19) Uani 1 1 d . . .
I2 I 1.08886(8) 0.28649(4) 0.58324(4) 0.02727(19) Uani 1 1 d . . .
I3 I 0.76002(8) 0.45568(4) 0.65900(4) 0.02797(19) Uani 1 1 d . . .
I4 I 1.08969(8) 0.41785(4) 0.85517(4) 0.02905(19) Uani 1 1 d . . .
Cd1 Cd 0.93599(8) 0.34052(4) 0.72366(5) 0.02406(19) Uani 1 1 d . . .
N1 N 0.4911(10) 0.4110(5) 0.8968(6) 0.028(2) Uani 1 1 d . . .
N2 N 0.7626(9) 0.6019(4) 0.9111(5) 0.023(2) Uani 1 1 d . . .
N3 N 1.1559(9) 0.9448(5) 0.8781(5) 0.0206(19) Uani 1 1 d U . .
N4 N 1.3508(11) 1.1660(5) 0.8332(6) 0.034(2) Uani 1 1 d . . .
C1 C 0.4534(12) 0.4893(5) 0.8880(6) 0.028(3) Uani 1 1 d . . .
H1 H 0.3653 0.5006 0.8798 0.034 Uiso 1 1 calc R . .
C2 C 0.5399(11) 0.5523(6) 0.8908(7) 0.026(2) Uani 1 1 d . . .
H2 H 0.5117 0.6052 0.8812 0.031 Uiso 1 1 calc R . .
C3 C 0.6685(11) 0.5366(5) 0.9078(6) 0.022(2) Uani 1 1 d . . .
C4 C 0.7122(12) 0.4569(5) 0.9160(6) 0.025(2) Uani 1 1 d . . .
H4 H 0.8001 0.4450 0.9246 0.030 Uiso 1 1 calc R . .
C5 C 0.6192(13) 0.3963(6) 0.9109(7) 0.034(3) Uani 1 1 d . . .
H5 H 0.6461 0.3427 0.9174 0.041 Uiso 1 1 calc R . .
C6 C 0.7352(10) 0.6700(6) 0.9596(6) 0.021(2) Uani 1 1 d . . .
H6 H 0.6605 0.6714 0.9949 0.025 Uiso 1 1 calc R . .
C7 C 0.8144(10) 0.7354(6) 0.9573(6) 0.022(2) Uani 1 1 d . . .
H7 H 0.7934 0.7819 0.9897 0.026 Uiso 1 1 calc R . .
C8 C 0.9291(11) 0.7328(6) 0.9056(7) 0.027(2) Uani 1 1 d . . .
C9 C 0.9582(11) 0.6618(5) 0.8593(7) 0.026(2) Uani 1 1 d . . .
H9 H 1.0345 0.6576 0.8259 0.031 Uiso 1 1 calc R . .
C10 C 0.8723(11) 0.5980(6) 0.8639(6) 0.026(2) Uani 1 1 d . . .
H10 H 0.8914 0.5505 0.8329 0.031 Uiso 1 1 calc R . .
C11 C 1.1169(11) 0.9230(5) 0.9604(6) 0.024(2) Uani 1 1 d . . .
H11 H 1.1396 0.9544 1.0098 0.029 Uiso 1 1 calc R . .
C12 C 1.0421(11) 0.8529(5) 0.9713(6) 0.025(3) Uani 1 1 d . . .
H12 H 1.0102 0.8391 1.0275 0.030 Uiso 1 1 calc R . .
C13 C 1.0155(11) 0.8038(5) 0.8982(6) 0.022(2) Uani 1 1 d . . .
C14 C 1.0613(11) 0.8255(5) 0.8141(6) 0.025(3) Uani 1 1 d . . .
H14 H 1.0460 0.7929 0.7645 0.030 Uiso 1 1 calc R . .
C15 C 1.1301(11) 0.8971(6) 0.8067(6) 0.028(3) Uani 1 1 d . . .
H15 H 1.1599 0.9132 0.7507 0.034 Uiso 1 1 calc R . .
C16 C 1.2254(13) 1.1547(6) 0.8067(8) 0.035(3) Uani 1 1 d . . .
H16 H 1.1831 1.1967 0.7769 0.042 Uiso 1 1 calc R . .
C17 C 1.1578(12) 1.0835(6) 0.8222(7) 0.033(3) Uani 1 1 d . . .
H17 H 1.0708 1.0779 0.8054 0.040 Uiso 1 1 calc R . .
C18 C 1.2243(10) 1.0206(6) 0.8637(6) 0.020(2) Uani 1 1 d . . .
C19 C 1.3498(11) 1.0302(5) 0.8912(6) 0.023(2) Uani 1 1 d . . .
H19 H 1.3940 0.9882 0.9198 0.028 Uiso 1 1 calc R . .
C20 C 1.4107(12) 1.1046(6) 0.8753(7) 0.032(3) Uani 1 1 d . . .
H20 H 1.4961 1.1118 0.8947 0.039 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cd1 2.7527(9) . ?
I2 Cd1 2.7665(9) . ?
I3 Cd1 2.7895(11) . ?
I4 Cd1 2.8231(11) . ?
N1 C1 1.352(12) . ?
N1 C5 1.351(17) . ?
N2 C10 1.329(12) . ?
N2 C6 1.364(11) . ?
N2 C3 1.446(13) . ?
N3 C15 1.350(12) . ?
N3 C11 1.344(11) . ?
N3 C18 1.448(12) . ?
N4 C16 1.357(17) . ?
N4 C20 1.340(14) . ?
C1 C2 1.365(14) . ?
C2 C3 1.366(16) . ?
C3 C4 1.391(12) . ?
C4 C5 1.383(16) . ?
C6 C7 1.349(14) . ?
C7 C8 1.407(13) . ?
C8 C9 1.392(13) . ?
C8 C13 1.471(14) . ?
C9 C10 1.372(14) . ?
C11 C12 1.396(13) . ?
C12 C13 1.387(13) . ?
C13 C14 1.389(12) . ?
C14 C15 1.378(13) . ?
C16 C17 1.383(14) . ?
C17 C18 1.386(15) . ?
C18 C19 1.359(15) . ?
C19 C20 1.396(13) . ?

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
I1 Cd1 I2 109.27(3) . . ?
I1 Cd1 I3 113.24(4) . . ?
I2 Cd1 I3 108.75(3) . . ?
I1 Cd1 I4 107.42(3) . . ?
I2 Cd1 I4 110.99(4) . . ?
I3 Cd1 I4 107.17(3) . . ?
C1 N1 C5 117.6(9) . . ?
C10 N2 C6 119.8(8) . . ?
C10 N2 C3 120.6(7) . . ?
C6 N2 C3 119.6(8) . . ?
C15 N3 C11 120.8(8) . . ?
C15 N3 C18 118.6(7) . . ?
C11 N3 C18 120.6(8) . . ?
C16 N4 C20 117.8(9) . . ?
N1 C1 C2 122.4(11) . . ?
C3 C2 C1 119.2(10) . . ?
C2 C3 C4 120.4(10) . . ?
C2 C3 N2 120.5(8) . . ?
C4 C3 N2 119.0(10) . . ?
C5 C4 C3 117.0(11) . . ?
N1 C5 C4 123.3(9) . . ?
C7 C6 N2 121.3(8) . . ?
C6 C7 C8 119.4(9) . . ?
C9 C8 C7 118.6(9) . . ?
C9 C8 C13 120.1(9) . . ?
C7 C8 C13 121.3(8) . . ?
C10 C9 C8 118.8(9) . . ?
N2 C10 C9 122.1(9) . . ?
N3 C11 C12 119.4(9) . . ?
C11 C12 C13 119.9(8) . . ?
C12 C13 C14 119.8(9) . . ?
C12 C13 C8 121.5(8) . . ?
C14 C13 C8 118.4(9) . . ?
C15 C14 C13 117.7(9) . . ?
N3 C15 C14 122.3(8) . . ?
N4 C16 C17 122.8(11) . . ?
C18 C17 C16 117.5(12) . . ?
C19 C18 C17 120.9(9) . . ?
C19 C18 N3 120.9(9) . . ?
C17 C18 N3 118.2(10) . . ?
C18 C19 C20 118.2(10) . . ?
N4 C20 C19 122.6(11) . . ?

_diffrn_measured_fraction_theta_max 0.731
_diffrn_reflns_theta_full        30.69
_diffrn_measured_fraction_theta_full 0.731
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.181
_database_code_depnum_ccdc_archive 'CCDC 997307'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_PyBP(ZnI3)2+3CH3OH

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H28 I6 N4 O3 Zn2'
_chemical_formula_weight         1300.63

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   28.1847(3)
_cell_length_b                   9.04820(10)
_cell_length_c                   14.2578(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.6990(10)
_cell_angle_gamma                90
_cell_volume                     3594.21(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9861
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.14

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_F_000             2384
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.517
_shelx_estimated_absorpt_T_min   0.263
_shelx_estimated_absorpt_T_max   0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55141
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.462
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4463
_reflns_number_gt                3565
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0140P)²+240.9497P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4463
_refine_ls_number_parameters     228
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1411
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.60156(5) 0.78342(12) 0.11684(9) 0.0338(3) Uani 1 1 d . . . . .
I1 I 0.62659(4) 1.04280(7) 0.17902(5) 0.0497(2) Uani 1 1 d . . . . .
I2 I 0.61909(4) 0.73466(8) -0.05284(5) 0.0529(3) Uani 1 1 d . . . . .
I3 I 0.62740(4) 0.56433(8) 0.22793(5) 0.0532(3) Uani 1 1 d . . . . .
O1 O 0.7436(5) 0.3208(18) 0.5901(15) 0.147(8) Uani 1 1 d . . . . .
C12 C 0.4858(19) 0.714(5) 0.816(3) 0.26(8) Uani 0.5 1 d D . P A -1
H12A H 0.5073 0.7236 0.8743 0.393 Uiso 0.5 1 calc R U P A -1
H12B H 0.4728 0.6155 0.8108 0.393 Uiso 0.5 1 calc R U P A -1
H12C H 0.4601 0.7839 0.8142 0.393 Uiso 0.5 1 calc R U P A -1
O2 O 0.5118(16) 0.742(8) 0.736(3) 0.22(3) Uani 0.5 1 d D . P A -1
N1A N 0.5287(11) 0.781(3) 0.1167(13) 0.020(4) Uani 0.5 1 d . . P B 1
C1A C 0.5043(10) 0.904(2) 0.1034(16) 0.024(5) Uani 0.5 1 d . . P B 1
H1A H 0.5207 0.9930 0.1068 0.029 Uiso 0.5 1 calc R U P B 1
C2A C 0.4547(7) 0.9047(19) 0.0842(13) 0.020(4) Uani 0.5 1 d . . P B 1
H2A H 0.4386 0.9947 0.0828 0.024 Uiso 0.5 1 calc R U P B 1
C4A C 0.4558(6) 0.6399(19) 0.0848(14) 0.025(4) Uani 0.5 1 d . . P B 1
H4A H 0.4411 0.5478 0.0838 0.030 Uiso 0.5 1 calc R U P B 1
C5A C 0.5062(7) 0.6495(18) 0.1045(14) 0.028(4) Uani 0.5 1 d . . P B 1
H5A H 0.5243 0.5632 0.1092 0.033 Uiso 0.5 1 calc R U P B 1
N1B N 0.5228(12) 0.781(4) 0.0815(17) 0.035(6) Uani 0.5 1 d . . P B 2
C1B C 0.4965(11) 0.860(4) 0.134(2) 0.051(8) Uani 0.5 1 d . . P B 2
H1B H 0.5127 0.9220 0.1794 0.061 Uiso 0.5 1 calc R U P B 2
C2B C 0.4462(9) 0.856(4) 0.1255(19) 0.053(7) Uani 0.5 1 d . . P B 2
H2B H 0.4291 0.9145 0.1623 0.063 Uiso 0.5 1 calc R U P B 2
C4B C 0.4478(9) 0.705(3) -0.009(2) 0.059(8) Uani 0.5 1 d . . P B 2
H4B H 0.4301 0.6621 -0.0630 0.070 Uiso 0.5 1 calc R U P B 2
C5B C 0.4982(11) 0.712(3) 0.006(2) 0.068(9) Uani 0.5 1 d . . P B 2
H5B H 0.5151 0.6676 -0.0372 0.081 Uiso 0.5 1 calc R U P B 2
N2 N 0.3752(3) 0.7632(8) 0.0472(5) 0.0286(17) Uani 1 1 d . . . . .
C3 C 0.4268(4) 0.7699(11) 0.0663(8) 0.033(2) Uani 1 1 d . . . . .
C6 C 0.3491(5) 0.8692(13) 0.0807(10) 0.052(4) Uani 1 1 d . . . . .
H6 H 0.3646 0.9460 0.1163 0.063 Uiso 1 1 calc R U . . .
C7 C 0.3005(4) 0.8661(13) 0.0634(9) 0.045(3) Uani 1 1 d . . . . .
H7 H 0.2830 0.9405 0.0873 0.055 Uiso 1 1 calc R U . . .
C8 C 0.2768(4) 0.7529(10) 0.0103(6) 0.0274(19) Uani 1 1 d . . . . .
C9 C 0.3049(4) 0.6485(13) -0.0252(9) 0.049(3) Uani 1 1 d . . . . .
H9 H 0.2903 0.5720 -0.0625 0.059 Uiso 1 1 calc R U . . .
C10 C 0.3535(5) 0.6554(13) -0.0066(9) 0.051(3) Uani 1 1 d . . . . .
H10 H 0.3718 0.5841 -0.0316 0.061 Uiso 1 1 calc R U . . .
C11 C 0.7548(6) 0.231(2) 0.6738(18) 0.124(10) Uani 1 1 d . . . . .
H11A H 0.7869 0.1938 0.6777 0.186 Uiso 1 1 calc R U . . .
H11B H 0.7327 0.1500 0.6706 0.186 Uiso 1 1 calc R U . . .
H11C H 0.7523 0.2899 0.7289 0.186 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1A 2.05(3) . ?
Zn1 N1B 2.20(3) . ?
Zn1 I1 2.5696(13) . ?
Zn1 I3 2.5730(14) . ?
Zn1 I2 2.5793(14) . ?
O1 C11 1.44(2) . ?
C12 O2 1.46(2) . ?
N1A C1A 1.31(4) . ?
N1A C5A 1.35(3) . ?
C1A C2A 1.38(3) . ?
C2A C3 1.45(2) . ?
C4A C5A 1.41(2) . ?
C4A C3 1.43(2) . ?
N1B C1B 1.33(4) . ?
N1B C5B 1.34(3) . ?
C1B C2B 1.40(4) . ?
C2B C3 1.22(2) . ?
C4B C5B 1.40(4) . ?
C4B C3 1.43(3) . ?
N2 C10 1.331(13) . ?
N2 C6 1.340(13) . ?
N2 C3 1.439(13) . ?
C6 C7 1.354(17) . ?
C7 C8 1.384(13) . ?
C8 C9 1.377(14) . ?
C8 C8 1.49(2) 7_565 ?
C9 C10 1.358(17) . ?

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
N1A Zn1 I1 103.5(8) . . ?
N1B Zn1 I1 107.6(9) . . ?
N1A Zn1 I3 100.4(7) . . ?
N1B Zn1 I3 108.4(9) . . ?
I1 Zn1 I3 117.00(6) . . ?
N1A Zn1 I2 109.3(5) . . ?
N1B Zn1 I2 96.5(6) . . ?
I1 Zn1 I2 113.47(5) . . ?
I3 Zn1 I2 111.65(5) . . ?
C1A N1A C5A 120(3) . . ?
C1A N1A Zn1 120(2) . . ?
C5A N1A Zn1 118(2) . . ?
N1A C1A C2A 122(2) . . ?
C1A C2A C3 122.1(16) . . ?
C5A C4A C3 121.0(14) . . ?
N1A C5A C4A 121.6(19) . . ?
C1B N1B C5B 115(3) . . ?
C1B N1B Zn1 120(2) . . ?
C5B N1B Zn1 125(2) . . ?
N1B C1B C2B 126(3) . . ?
C3 C2B C1B 114(2) . . ?
C5B C4B C3 112(2) . . ?
N1B C5B C4B 123(3) . . ?
C10 N2 C6 120.0(10) . . ?
C10 N2 C3 120.2(9) . . ?
C6 N2 C3 119.8(9) . . ?
C2B C3 C4B 126.4(19) . . ?
C2B C3 N2 119.5(15) . . ?
C4A C3 N2 122.1(10) . . ?
C4B C3 N2 111.1(13) . . ?
C4A C3 C2A 112.2(12) . . ?
N2 C3 C2A 124.9(11) . . ?
N2 C6 C7 121.0(10) . . ?
C6 C7 C8 120.4(10) . . ?
C9 C8 C7 116.8(10) . . ?
C9 C8 C8 121.6(10) . 7_565 ?
C7 C8 C8 121.6(11) . 7_565 ?
C10 C9 C8 121.1(10) . . ?
N2 C10 C9 120.6(10) . . ?

_refine_diff_density_max         5.381
_refine_diff_density_min         -4.475
_refine_diff_density_rms         0.248

#===END
_database_code_depnum_ccdc_archive 'CCDC 997308'
