 
 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
 'C20 H20 N12 O2 Zn, F6 Si, H2O'
_chemical_formula_sum 
 'C20 H22 F6 N12 O3 Si Zn' 
_chemical_formula_weight          685.96 
 
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' 
 'F'  'F'   0.0171   0.0103 
 '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' 
 'Si'  'Si'   0.0817   0.0704 
 '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            Triclinic
_symmetry_space_group_name_H-M    'P -1'
_symmetry_space_group_name_Hall    '-P 1'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    7.003(3) 
_cell_length_b                    9.800(4) 
_cell_length_c                    10.744(4) 
_cell_angle_alpha                 63.290(4) 
_cell_angle_beta                  87.998(5) 
_cell_angle_gamma                 70.983(4) 
_cell_volume                      617.3(4) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     642
_cell_measurement_theta_min        2.41
_cell_measurement_theta_max       21.67
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.845 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              348 
_exptl_absorpt_coefficient_mu     1.143 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7631 
_exptl_absorpt_correction_T_max   0.8750 
_exptl_absorpt_process_details    'SADABS (Bruker, 2000)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             4415 
_diffrn_reflns_av_R_equivalents   0.0524 
_diffrn_reflns_av_sigmaI/netI     0.0914 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.14 
_diffrn_reflns_theta_max          25.25 
_reflns_number_total              2191 
_reflns_number_gt                 1550 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0688P)²+0.2339P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2191 
_refine_ls_number_parameters      208 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0848 
_refine_ls_R_factor_gt            0.0553 
_refine_ls_wR_factor_ref          0.1496 
_refine_ls_wR_factor_gt           0.1223 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.052 
_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 
C1 C 0.2903(8) 0.3965(6) 1.0267(5) 0.0191(12) Uani 1 1 d . . . 
C2 C 0.3698(8) 0.2274(6) 1.0913(5) 0.0193(12) Uani 1 1 d . . . 
H2 H 0.3552 0.1691 1.0438 0.023 Uiso 1 1 calc R . . 
C3 C 0.4715(8) 0.1456(7) 1.2276(6) 0.0222(12) Uani 1 1 d . . . 
C4 C 0.4935(8) 0.2306(6) 1.2973(5) 0.0210(12) Uani 1 1 d . . . 
H4 H 0.5626 0.1736 1.3905 0.025 Uiso 1 1 calc R . . 
C5 C 0.4143(8) 0.3983(7) 1.2300(6) 0.0230(13) Uani 1 1 d . . . 
H5 H 0.4309 0.4576 1.2760 0.028 Uiso 1 1 calc R . . 
C6 C 0.3121(8) 0.4793(7) 1.0972(6) 0.0246(13) Uani 1 1 d . . . 
H6 H 0.2549 0.5948 1.0526 0.030 Uiso 1 1 calc R . . 
C7 C 0.1033(8) 0.6456(7) 0.8024(6) 0.0257(13) Uani 1 1 d . . . 
H7 H 0.0971 0.7242 0.8326 0.031 Uiso 1 1 calc R . . 
C8 C 0.1583(8) 0.4174(6) 0.8032(5) 0.0209(12) Uani 1 1 d U . . 
H8 H 0.1972 0.3042 0.8316 0.025 Uiso 1 1 calc R . . 
C9 C 0.4334(9) -0.1233(7) 1.3138(6) 0.0285(14) Uani 1 1 d . . . 
H9 H 0.2932 -0.0833 1.2788 0.034 Uiso 1 1 calc R . . 
C10 C 0.7341(8) -0.1291(7) 1.3586(5) 0.0240(13) Uani 1 1 d . . . 
H10 H 0.8464 -0.0961 1.3621 0.029 Uiso 1 1 calc R . . 
F1 F 1.0042(5) 0.9384(4) -0.1244(3) 0.0291(8) Uani 1 1 d . . . 
F2 F 0.7909(5) 0.9524(4) 0.0509(3) 0.0312(8) Uani 1 1 d . . . 
F3 F 1.1486(5) 0.8067(4) 0.1167(3) 0.0324(8) Uani 1 1 d . . . 
N1 N 0.0680(7) 0.5340(5) 0.6768(4) 0.0223(11) Uani 1 1 d . . . 
N2 N 0.0331(7) 0.6820(6) 0.6770(5) 0.0270(11) Uani 1 1 d . . . 
N3 N 0.1880(6) 0.4800(5) 0.8868(4) 0.0207(10) Uani 1 1 d . . . 
N4 N 0.7396(6) -0.2808(5) 1.4140(4) 0.0208(10) Uani 1 1 d . . . 
N5 N 0.5444(7) -0.2778(5) 1.3853(5) 0.0279(11) Uani 1 1 d . . . 
N6 N 0.5452(7) -0.0292(5) 1.2968(4) 0.0214(10) Uani 1 1 d . . . 
O1 O 0.1775(6) 0.6418(5) 0.3905(4) 0.0290(10) Uani 1 1 d D . . 
H1A H 0.306(6) 0.599(7) 0.427(6) 0.035 Uiso 1 1 d D . . 
H1B H 0.158(9) 0.706(6) 0.299(4) 0.035 Uiso 1 1 d D . . 
O2 O 0.9168(18) 0.0247(14) 0.5393(11) 0.078(4) Uani 0.50 1 d P . . 
H2A H 0.9802 -0.0741 0.5587 0.094 Uiso 0.50 1 d PR . . 
H2B H 0.9631 0.0856 0.4703 0.094 Uiso 0.50 1 d PR . . 
Si1 Si 1.0000 1.0000 0.0000 0.0201(5) Uani 1 2 d S . . 
Zn1 Zn 0.0000 0.5000 0.5000 0.0213(3) Uani 1 2 d S . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
C1 C6 1.377(7) . ? 
C1 C2 1.389(7) . ? 
C1 N3 1.425(6) . ? 
C2 C3 1.392(7) . ? 
C2 H2 0.9500 . ? 
C3 C4 1.390(7) . ? 
C3 N6 1.435(7) . ? 
C4 C5 1.378(7) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.364(7) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C7 N2 1.298(7) . ? 
C7 N3 1.377(7) . ? 
C7 H7 0.9500 . ? 
C8 N1 1.321(6) . ? 
C8 N3 1.348(6) . ? 
C8 H8 0.9500 . ? 
C9 N5 1.310(7) . ? 
C9 N6 1.344(7) . ? 
C9 H9 0.9500 . ? 
C10 N4 1.317(7) . ? 
C10 N6 1.335(7) . ? 
C10 H10 0.9500 . ? 
F1 Si1 1.692(3) . ? 
F2 Si1 1.679(3) . ? 
F3 Si1 1.708(3) . ? 
N1 N2 1.392(6) . ? 
N1 Zn1 2.164(4) . ? 
N4 N5 1.400(6) . ? 
N4 Zn1 2.139(4) 1_646 ? 
O1 Zn1 2.101(4) . ? 
O1 H1A 0.88(4) . ? 
O1 H1B 0.88(4) . ? 
O2 O2 1.50(2) 2_756 ? 
O2 H2A 0.8500 . ? 
O2 H2B 0.8501 . ? 
Si1 F2 1.679(3) 2_775 ? 
Si1 F1 1.692(3) 2_775 ? 
Si1 F3 1.708(3) 2_775 ? 
Zn1 O1 2.101(4) 2_566 ? 
Zn1 N4 2.139(4) 2_657 ? 
Zn1 N4 2.139(4) 1_464 ? 
Zn1 N1 2.164(4) 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 
C6 C1 C2 120.1(5) . . ? 
C6 C1 N3 121.7(5) . . ? 
C2 C1 N3 118.2(5) . . ? 
C1 C2 C3 118.3(5) . . ? 
C1 C2 H2 120.8 . . ? 
C3 C2 H2 120.8 . . ? 
C4 C3 C2 121.0(5) . . ? 
C4 C3 N6 120.6(5) . . ? 
C2 C3 N6 118.3(5) . . ? 
C5 C4 C3 119.3(5) . . ? 
C5 C4 H4 120.3 . . ? 
C3 C4 H4 120.3 . . ? 
C6 C5 C4 120.0(5) . . ? 
C6 C5 H5 120.0 . . ? 
C4 C5 H5 120.0 . . ? 
C5 C6 C1 121.2(5) . . ? 
C5 C6 H6 119.4 . . ? 
C1 C6 H6 119.4 . . ? 
N2 C7 N3 112.3(5) . . ? 
N2 C7 H7 123.8 . . ? 
N3 C7 H7 123.8 . . ? 
N1 C8 N3 111.2(4) . . ? 
N1 C8 H8 124.4 . . ? 
N3 C8 H8 124.4 . . ? 
N5 C9 N6 110.7(5) . . ? 
N5 C9 H9 124.7 . . ? 
N6 C9 H9 124.7 . . ? 
N4 C10 N6 108.9(5) . . ? 
N4 C10 H10 125.5 . . ? 
N6 C10 H10 125.5 . . ? 
C8 N1 N2 107.3(4) . . ? 
C8 N1 Zn1 126.1(4) . . ? 
N2 N1 Zn1 126.6(3) . . ? 
C7 N2 N1 105.8(4) . . ? 
C8 N3 C7 103.4(4) . . ? 
C8 N3 C1 128.8(4) . . ? 
C7 N3 C1 127.8(4) . . ? 
C10 N4 N5 108.0(4) . . ? 
C10 N4 Zn1 128.4(4) . 1_646 ? 
N5 N4 Zn1 122.7(3) . 1_646 ? 
C9 N5 N4 105.4(4) . . ? 
C10 N6 C9 107.0(5) . . ? 
C10 N6 C3 127.2(5) . . ? 
C9 N6 C3 125.8(5) . . ? 
Zn1 O1 H1A 114(4) . . ? 
Zn1 O1 H1B 125(4) . . ? 
H1A O1 H1B 113(5) . . ? 
O2 O2 H2A 57.1 2_756 . ? 
O2 O2 H2B 51.8 2_756 . ? 
H2A O2 H2B 109.0 . . ? 
F2 Si1 F2 179.999(1) . 2_775 ? 
F2 Si1 F1 89.85(15) . 2_775 ? 
F2 Si1 F1 90.15(15) 2_775 2_775 ? 
F2 Si1 F1 90.15(15) . . ? 
F2 Si1 F1 89.86(15) 2_775 . ? 
F1 Si1 F1 179.999(1) 2_775 . ? 
F2 Si1 F3 89.64(16) . . ? 
F2 Si1 F3 90.36(16) 2_775 . ? 
F1 Si1 F3 90.55(14) 2_775 . ? 
F1 Si1 F3 89.45(14) . . ? 
F2 Si1 F3 90.36(16) . 2_775 ? 
F2 Si1 F3 89.64(16) 2_775 2_775 ? 
F1 Si1 F3 89.45(14) 2_775 2_775 ? 
F1 Si1 F3 90.55(14) . 2_775 ? 
F3 Si1 F3 179.999(2) . 2_775 ? 
O1 Zn1 O1 179.999(1) . 2_566 ? 
O1 Zn1 N4 92.20(17) . 2_657 ? 
O1 Zn1 N4 87.80(16) 2_566 2_657 ? 
O1 Zn1 N4 87.80(17) . 1_464 ? 
O1 Zn1 N4 92.20(17) 2_566 1_464 ? 
N4 Zn1 N4 180.000(1) 2_657 1_464 ? 
O1 Zn1 N1 86.91(16) . . ? 
O1 Zn1 N1 93.09(16) 2_566 . ? 
N4 Zn1 N1 87.35(16) 2_657 . ? 
N4 Zn1 N1 92.65(16) 1_464 . ? 
O1 Zn1 N1 93.09(16) . 2_566 ? 
O1 Zn1 N1 86.91(16) 2_566 2_566 ? 
N4 Zn1 N1 92.65(16) 2_657 2_566 ? 
N4 Zn1 N1 87.35(16) 1_464 2_566 ? 
N1 Zn1 N1 180.0(2) . 2_566 ? 
 
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              25.25 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    0.451 
_refine_diff_density_min   -0.613 
_refine_diff_density_rms    0.113 


# END

  
data_2 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C20 H24 Cd F6 N12 O4 Si' 
_chemical_formula_weight          751.00 
  
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' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Si'  'Si'   0.0817   0.0704 
 '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            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    7.5550(5) 
_cell_length_b                    9.5468(6) 
_cell_length_c                    10.3006(6) 
_cell_angle_alpha                 113.6790(10) 
_cell_angle_beta                  91.9870(10) 
_cell_angle_gamma                 104.3270(10) 
_cell_volume                      651.67(7) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     2295 
_cell_measurement_theta_min       2.18 
_cell_measurement_theta_max       28.30 
  
_exptl_crystal_description        BLOCK 
_exptl_crystal_colour             PALE-YELLOW 
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.13 
_exptl_crystal_density_meas       NONE 
_exptl_crystal_density_diffrn     1.914 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              376 
_exptl_absorpt_coefficient_mu     0.984 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.8665 
_exptl_absorpt_correction_T_max   0.8828 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3342 
_diffrn_reflns_av_R_equivalents   0.0132 
_diffrn_reflns_av_sigmaI/netI     0.0257 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        7 
_diffrn_reflns_theta_min          2.18 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              2268 
_reflns_number_gt                 2112 
_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, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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)+(0.0169P)²+2.1104P] 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          2268 
_refine_ls_number_parameters      202 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0398 
_refine_ls_R_factor_gt            0.0365 
_refine_ls_wR_factor_ref          0.0815 
_refine_ls_wR_factor_gt           0.0788 
_refine_ls_goodness_of_fit_ref    1.080 
_refine_ls_restrained_S_all       1.080 
_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 
Cd1 Cd 0.0000 -0.5000 0.0000 0.03655(16) Uani 1 2 d S . . 
Si1 Si 0.0000 0.0000 0.5000 0.0148(3) Uani 1 2 d S . . 
F1 F 0.1913(3) -0.0430(2) 0.4393(2) 0.0310(5) Uani 1 1 d . . . 
F2 F 0.1296(3) 0.1876(2) 0.6096(2) 0.0344(5) Uani 1 1 d . . . 
F3 F 0.0334(3) -0.0608(3) 0.6275(3) 0.0468(7) Uani 1 1 d . . . 
O1 O 0.1830(4) -0.6672(3) -0.1021(3) 0.0363(7) Uani 1 1 d . . . 
H1A H 0.1692 -0.7088 -0.1921 0.054 Uiso 1 1 d R . . 
H1B H 0.1696 -0.7418 -0.0763 0.054 Uiso 1 1 d R . . 
O2 O 0.1262(4) 1.0333(3) 0.9139(3) 0.0411(7) Uani 1 1 d . . . 
H2A H 0.1040 0.9842 0.8240 0.062 Uiso 1 1 d R . . 
N1 N 0.4392(4) -0.0342(3) 0.2071(3) 0.0211(6) Uani 1 1 d . . . 
N2 N 0.2598(4) -0.2779(4) 0.0971(3) 0.0308(7) Uani 1 1 d . . . 
N3 N 0.4143(4) -0.2821(3) 0.1715(3) 0.0279(7) Uani 1 1 d . . . 
N4 N 0.8007(4) 0.4721(3) 0.5799(3) 0.0271(7) Uani 1 1 d . . . 
N5 N 0.9474(4) 0.5292(4) 0.7896(4) 0.0368(8) Uani 1 1 d . . . 
N6 N 0.9498(5) 0.6716(4) 0.7825(5) 0.0580(13) Uani 1 1 d . . . 
C1 C 0.2788(6) -0.1312(4) 0.1205(4) 0.0333(9) Uani 1 1 d . . . 
H1 H 0.1917 -0.0960 0.0819 0.040 Uiso 1 1 calc R . . 
C2 C 0.5174(5) -0.1344(4) 0.2362(4) 0.0237(7) Uani 1 1 d . . . 
H2 H 0.6322 -0.1012 0.2960 0.028 Uiso 1 1 calc R . . 
C3 C 0.5107(5) 0.1351(4) 0.2587(4) 0.0228(7) Uani 1 1 d . . . 
C4 C 0.6155(5) 0.2204(4) 0.3930(4) 0.0203(7) Uani 1 1 d . . . 
H4 H 0.6364 0.1680 0.4509 0.024 Uiso 1 1 calc R . . 
C5 C 0.6897(5) 0.3839(4) 0.4419(4) 0.0244(8) Uani 1 1 d . . . 
C6 C 0.6547(7) 0.4619(4) 0.3597(4) 0.0394(11) Uani 1 1 d . . . 
H6 H 0.7037 0.5743 0.3945 0.047 Uiso 1 1 calc R . . 
C7 C 0.5478(8) 0.3738(5) 0.2270(5) 0.0531(14) Uani 1 1 d . . . 
H7 H 0.5229 0.4266 0.1705 0.064 Uiso 1 1 calc R . . 
C8 C 0.4758(7) 0.2101(5) 0.1739(4) 0.0416(11) Uani 1 1 d . . . 
H8 H 0.4039 0.1502 0.0814 0.050 Uiso 1 1 calc R . . 
C9 C 0.8593(5) 0.4135(4) 0.6677(4) 0.0263(8) Uani 1 1 d . . . 
H9 H 0.8392 0.3033 0.6439 0.032 Uiso 1 1 calc R . . 
C10 C 0.8625(6) 0.6341(5) 0.6579(6) 0.0506(13) Uani 1 1 d . . . 
H10 H 0.8435 0.7094 0.6245 0.061 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 O1 2.326(2) . ? 
Cd1 O1 2.326(2) 2_545 ? 
Cd1 N5 2.327(4) 1_444 ? 
Cd1 N5 2.327(4) 2_656 ? 
Cd1 N2 2.334(3) . ? 
Cd1 N2 2.334(3) 2_545 ? 
Si1 F3 1.670(2) 2_556 ? 
Si1 F3 1.670(2) . ? 
Si1 F1 1.673(2) . ? 
Si1 F1 1.673(2) 2_556 ? 
Si1 F2 1.6948(19) . ? 
Si1 F2 1.6948(19) 2_556 ? 
O1 H1A 0.8400 . ? 
O1 H1B 0.8401 . ? 
O2 H2A 0.8401 . ? 
O2 H2B 0.8453 . ? 
N1 C1 1.352(5) . ? 
N1 C2 1.361(4) . ? 
N1 C3 1.430(4) . ? 
N2 C1 1.292(5) . ? 
N2 N3 1.392(4) . ? 
N3 C2 1.305(4) . ? 
N4 C9 1.351(5) . ? 
N4 C10 1.369(5) . ? 
N4 C5 1.429(5) . ? 
N5 C9 1.305(5) . ? 
N5 N6 1.387(5) . ? 
N5 Cd1 2.327(4) 1_666 ? 
N6 C10 1.290(7) . ? 
C1 H1 0.9500 . ? 
C2 H2 0.9500 . ? 
C3 C4 1.380(5) . ? 
C3 C8 1.387(5) . ? 
C4 C5 1.386(5) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.389(5) . ? 
C6 C7 1.375(7) . ? 
C6 H6 0.9500 . ? 
C7 C8 1.382(6) . ? 
C7 H7 0.9500 . ? 
C8 H8 0.9500 . ? 
C9 H9 0.9500 . ? 
C10 H10 0.9500 . ? 
  
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 
O1 Cd1 O1 180.0 . 2_545 ? 
O1 Cd1 N5 91.58(11) . 1_444 ? 
O1 Cd1 N5 88.42(11) 2_545 1_444 ? 
O1 Cd1 N5 88.42(11) . 2_656 ? 
O1 Cd1 N5 91.58(11) 2_545 2_656 ? 
N5 Cd1 N5 180.000(1) 1_444 2_656 ? 
O1 Cd1 N2 91.19(10) . . ? 
O1 Cd1 N2 88.81(10) 2_545 . ? 
N5 Cd1 N2 94.10(11) 1_444 . ? 
N5 Cd1 N2 85.90(11) 2_656 . ? 
O1 Cd1 N2 88.81(10) . 2_545 ? 
O1 Cd1 N2 91.19(10) 2_545 2_545 ? 
N5 Cd1 N2 85.90(11) 1_444 2_545 ? 
N5 Cd1 N2 94.10(11) 2_656 2_545 ? 
N2 Cd1 N2 180.0 . 2_545 ? 
F3 Si1 F3 180.000(1) 2_556 . ? 
F3 Si1 F1 90.54(12) 2_556 . ? 
F3 Si1 F1 89.46(12) . . ? 
F3 Si1 F1 89.46(12) 2_556 2_556 ? 
F3 Si1 F1 90.54(12) . 2_556 ? 
F1 Si1 F1 179.999(1) . 2_556 ? 
F3 Si1 F2 89.66(12) 2_556 . ? 
F3 Si1 F2 90.34(12) . . ? 
F1 Si1 F2 89.33(10) . . ? 
F1 Si1 F2 90.67(10) 2_556 . ? 
F3 Si1 F2 90.34(12) 2_556 2_556 ? 
F3 Si1 F2 89.66(12) . 2_556 ? 
F1 Si1 F2 90.67(10) . 2_556 ? 
F1 Si1 F2 89.33(10) 2_556 2_556 ? 
F2 Si1 F2 180.0 . 2_556 ? 
Cd1 O1 H1A 115.4 . . ? 
Cd1 O1 H1B 113.4 . . ? 
H1A O1 H1B 106.9 . . ? 
H2A O2 H2B 106.8 . . ? 
C1 N1 C2 104.1(3) . . ? 
C1 N1 C3 128.4(3) . . ? 
C2 N1 C3 127.4(3) . . ? 
C1 N2 N3 107.7(3) . . ? 
C1 N2 Cd1 130.3(2) . . ? 
N3 N2 Cd1 120.5(2) . . ? 
C2 N3 N2 105.8(3) . . ? 
C9 N4 C10 103.9(3) . . ? 
C9 N4 C5 127.5(3) . . ? 
C10 N4 C5 128.5(4) . . ? 
C9 N5 N6 107.4(4) . . ? 
C9 N5 Cd1 124.7(3) . 1_666 ? 
N6 N5 Cd1 125.1(3) . 1_666 ? 
C10 N6 N5 106.5(3) . . ? 
N2 C1 N1 111.0(3) . . ? 
N2 C1 H1 124.5 . . ? 
N1 C1 H1 124.5 . . ? 
N3 C2 N1 111.3(3) . . ? 
N3 C2 H2 124.3 . . ? 
N1 C2 H2 124.3 . . ? 
C4 C3 C8 121.4(3) . . ? 
C4 C3 N1 118.5(3) . . ? 
C8 C3 N1 120.1(3) . . ? 
C3 C4 C5 118.8(3) . . ? 
C3 C4 H4 120.6 . . ? 
C5 C4 H4 120.6 . . ? 
C4 C5 C6 120.9(4) . . ? 
C4 C5 N4 118.9(3) . . ? 
C6 C5 N4 120.3(3) . . ? 
C7 C6 C5 118.9(3) . . ? 
C7 C6 H6 120.5 . . ? 
C5 C6 H6 120.5 . . ? 
C6 C7 C8 121.5(4) . . ? 
C6 C7 H7 119.3 . . ? 
C8 C7 H7 119.3 . . ? 
C7 C8 C3 118.6(4) . . ? 
C7 C8 H8 120.7 . . ? 
C3 C8 H8 120.7 . . ? 
N5 C9 N4 110.7(3) . . ? 
N5 C9 H9 124.6 . . ? 
N4 C9 H9 124.6 . . ? 
N6 C10 N4 111.5(4) . . ? 
N6 C10 H10 124.2 . . ? 
N4 C10 H10 124.2 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O1 Cd1 N2 C1 147.5(4) . . . . ? 
O1 Cd1 N2 C1 -32.5(4) 2_545 . . . ? 
N5 Cd1 N2 C1 55.8(4) 1_444 . . . ? 
N5 Cd1 N2 C1 -124.2(4) 2_656 . . . ? 
N2 Cd1 N2 C1 44(13) 2_545 . . . ? 
O1 Cd1 N2 N3 -48.1(3) . . . . ? 
O1 Cd1 N2 N3 131.9(3) 2_545 . . . ? 
N5 Cd1 N2 N3 -139.8(3) 1_444 . . . ? 
N5 Cd1 N2 N3 40.2(3) 2_656 . . . ? 
N2 Cd1 N2 N3 -151(13) 2_545 . . . ? 
C1 N2 N3 C2 0.3(4) . . . . ? 
Cd1 N2 N3 C2 -167.3(2) . . . . ? 
C9 N5 N6 C10 0.4(5) . . . . ? 
Cd1 N5 N6 C10 -161.1(3) 1_666 . . . ? 
N3 N2 C1 N1 0.1(5) . . . . ? 
Cd1 N2 C1 N1 166.0(3) . . . . ? 
C2 N1 C1 N2 -0.4(4) . . . . ? 
C3 N1 C1 N2 -179.7(3) . . . . ? 
N2 N3 C2 N1 -0.5(4) . . . . ? 
C1 N1 C2 N3 0.6(4) . . . . ? 
C3 N1 C2 N3 179.9(3) . . . . ? 
C1 N1 C3 C4 147.3(4) . . . . ? 
C2 N1 C3 C4 -31.9(5) . . . . ? 
C1 N1 C3 C8 -33.3(6) . . . . ? 
C2 N1 C3 C8 147.6(4) . . . . ? 
C8 C3 C4 C5 -1.3(5) . . . . ? 
N1 C3 C4 C5 178.2(3) . . . . ? 
C3 C4 C5 C6 2.1(5) . . . . ? 
C3 C4 C5 N4 -179.0(3) . . . . ? 
C9 N4 C5 C4 6.7(5) . . . . ? 
C10 N4 C5 C4 -168.7(4) . . . . ? 
C9 N4 C5 C6 -174.4(4) . . . . ? 
C10 N4 C5 C6 10.2(6) . . . . ? 
C4 C5 C6 C7 -1.3(6) . . . . ? 
N4 C5 C6 C7 179.8(4) . . . . ? 
C5 C6 C7 C8 -0.3(7) . . . . ? 
C6 C7 C8 C3 1.1(7) . . . . ? 
C4 C3 C8 C7 -0.3(6) . . . . ? 
N1 C3 C8 C7 -179.7(4) . . . . ? 
N6 N5 C9 N4 -0.7(4) . . . . ? 
Cd1 N5 C9 N4 160.9(2) 1_666 . . . ? 
C10 N4 C9 N5 0.7(4) . . . . ? 
C5 N4 C9 N5 -175.6(3) . . . . ? 
N5 N6 C10 N4 0.0(6) . . . . ? 
C9 N4 C10 N6 -0.4(5) . . . . ? 
C5 N4 C10 N6 175.8(4) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              25.01 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.524 
_refine_diff_density_min   -2.073 
_refine_diff_density_rms    0.084 
  
#END

 
data_3 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
 'C10 H8 Br2 N6 Zn, H2 O'
_chemical_formula_sum 
 'C10 H10 Br2 N6 O Zn' 
_chemical_formula_weight          455.43 
 
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' 
 'Zn'  'Zn'   0.2839   1.4301 
 '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 '
_symmetry_space_group_name_Hall   '-P 2ac 2ab'
 
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                    10.135(3) 
_cell_length_b                    13.562(4) 
_cell_length_c                    20.655(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2839.2(15) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     950
_cell_measurement_theta_min        2.70
_cell_measurement_theta_max       21.05
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.16 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.131 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1760 
_exptl_absorpt_coefficient_mu     7.363 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.3854 
_exptl_absorpt_correction_T_max   0.6267 
_exptl_absorpt_process_details    'SADABS (Bruker, 2000)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             11548 
_diffrn_reflns_av_R_equivalents   0.1004 
_diffrn_reflns_av_sigmaI/netI     0.0833 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          1.97 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              2442 
_reflns_number_gt                 1546 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1058P)²+1.8722P] 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          2442 
_refine_ls_number_parameters      181 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1206 
_refine_ls_R_factor_gt            0.0717 
_refine_ls_wR_factor_ref          0.1937 
_refine_ls_wR_factor_gt           0.1684 
_refine_ls_goodness_of_fit_ref    1.067 
_refine_ls_restrained_S_all       1.067 
_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 
Br1 Br 0.47826(11) 0.61643(9) 0.42900(6) 0.0333(4) Uani 1 1 d . . . 
Br2 Br 0.32846(13) 0.37679(10) 0.34678(6) 0.0419(4) Uani 1 1 d . . . 
C1 C 0.9423(11) 0.3720(8) 0.4937(5) 0.025(3) Uani 1 1 d . . . 
C2 C 0.8970(11) 0.3861(9) 0.5569(5) 0.029(3) Uani 1 1 d . . . 
H2 H 0.8064 0.3986 0.5651 0.035 Uiso 1 1 calc R . . 
C3 C 0.9865(11) 0.3817(8) 0.6068(5) 0.026(3) Uani 1 1 d . . . 
C4 C 1.1193(10) 0.3614(7) 0.5955(5) 0.020(2) Uani 1 1 d . . . 
H4 H 1.1794 0.3554 0.6306 0.025 Uiso 1 1 calc R . . 
C5 C 1.1619(12) 0.3500(9) 0.5328(6) 0.032(3) Uani 1 1 d . . . 
H5 H 1.2531 0.3394 0.5247 0.038 Uiso 1 1 calc R . . 
C6 C 1.0752(11) 0.3539(8) 0.4815(6) 0.025(3) Uani 1 1 d . . . 
H6 H 1.1056 0.3444 0.4384 0.031 Uiso 1 1 calc R . . 
C7 C 0.8643(13) 0.3416(10) 0.3793(6) 0.041(3) Uani 1 1 d . . . 
H7 H 0.9402 0.3085 0.3633 0.049 Uiso 1 1 calc R . . 
C8 C 0.7342(11) 0.4237(9) 0.4423(5) 0.028(3) Uani 1 1 d . . . 
H8 H 0.6988 0.4580 0.4785 0.034 Uiso 1 1 calc R . . 
C9 C 0.8249(12) 0.3801(9) 0.6995(6) 0.038(3) Uani 1 1 d . . . 
H9 H 0.7554 0.3447 0.6792 0.045 Uiso 1 1 calc R . . 
C10 C 1.0119(12) 0.4559(9) 0.7166(5) 0.032(3) Uani 1 1 d . . . 
H10 H 1.0977 0.4826 0.7109 0.039 Uiso 1 1 calc R . . 
N1 N 0.6766(9) 0.4153(7) 0.3854(4) 0.027(2) Uani 1 1 d . . . 
N2 N 0.7552(11) 0.3611(8) 0.3446(4) 0.038(3) Uani 1 1 d . . . 
N3 N 0.8502(9) 0.3766(7) 0.4413(4) 0.025(2) Uani 1 1 d . . . 
N4 N 0.9414(9) 0.4613(7) 0.7700(5) 0.028(2) Uani 1 1 d . . . 
N5 N 0.8239(10) 0.4124(8) 0.7598(5) 0.037(3) Uani 1 1 d . . . 
N6 N 0.9421(9) 0.4057(7) 0.6707(5) 0.030(2) Uani 1 1 d . . . 
O1 O 0.0641(9) 0.2734(8) 0.2600(5) 0.061(3) Uani 1 1 d . . . 
H1A H 0.0992 0.2899 0.2243 0.074 Uiso 1 1 d R . . 
H1B H 0.1151 0.2921 0.2903 0.074 Uiso 1 1 d R . . 
Zn1 Zn 0.50903(12) 0.48354(10) 0.35666(6) 0.0261(4) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Br1 Zn1 2.3618(19) . ? 
Br2 Zn1 2.3424(19) . ? 
C1 C6 1.392(16) . ? 
C1 C2 1.395(16) . ? 
C1 N3 1.432(13) . ? 
C2 C3 1.375(15) . ? 
C2 H2 0.9500 . ? 
C3 C4 1.394(15) . ? 
C3 N6 1.431(14) . ? 
C4 C5 1.373(16) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.379(16) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C7 N2 1.344(15) . ? 
C7 N3 1.372(15) . ? 
C7 H7 0.9500 . ? 
C8 N1 1.317(14) . ? 
C8 N3 1.338(14) . ? 
C8 H8 0.9500 . ? 
C9 N5 1.321(15) . ? 
C9 N6 1.373(15) . ? 
C9 H9 0.9500 . ? 
C10 N4 1.317(14) . ? 
C10 N6 1.364(14) . ? 
C10 H10 0.9500 . ? 
N1 N2 1.373(13) . ? 
N1 Zn1 2.024(9) . ? 
N4 N5 1.380(13) . ? 
N4 Zn1 2.004(10) 2_665 ? 
O1 H1A 0.8501 . ? 
O1 H1B 0.8499 . ? 
Zn1 N4 2.004(10) 2_664 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C6 C1 C2 120.8(10) . . ? 
C6 C1 N3 120.0(10) . . ? 
C2 C1 N3 119.2(10) . . ? 
C3 C2 C1 118.6(11) . . ? 
C3 C2 H2 120.7 . . ? 
C1 C2 H2 120.7 . . ? 
C2 C3 C4 121.2(10) . . ? 
C2 C3 N6 118.4(10) . . ? 
C4 C3 N6 120.2(9) . . ? 
C5 C4 C3 119.0(10) . . ? 
C5 C4 H4 120.5 . . ? 
C3 C4 H4 120.5 . . ? 
C4 C5 C6 121.3(11) . . ? 
C4 C5 H5 119.3 . . ? 
C6 C5 H5 119.3 . . ? 
C5 C6 C1 118.9(10) . . ? 
C5 C6 H6 120.6 . . ? 
C1 C6 H6 120.6 . . ? 
N2 C7 N3 110.1(11) . . ? 
N2 C7 H7 125.0 . . ? 
N3 C7 H7 125.0 . . ? 
N1 C8 N3 109.5(10) . . ? 
N1 C8 H8 125.3 . . ? 
N3 C8 H8 125.3 . . ? 
N5 C9 N6 109.4(11) . . ? 
N5 C9 H9 125.3 . . ? 
N6 C9 H9 125.3 . . ? 
N4 C10 N6 109.2(10) . . ? 
N4 C10 H10 125.4 . . ? 
N6 C10 H10 125.4 . . ? 
C8 N1 N2 109.7(9) . . ? 
C8 N1 Zn1 126.4(8) . . ? 
N2 N1 Zn1 123.5(7) . . ? 
C7 N2 N1 104.8(9) . . ? 
C8 N3 C7 105.8(9) . . ? 
C8 N3 C1 125.5(9) . . ? 
C7 N3 C1 128.5(10) . . ? 
C10 N4 N5 108.3(9) . . ? 
C10 N4 Zn1 129.3(8) . 2_665 ? 
N5 N4 Zn1 122.1(7) . 2_665 ? 
C9 N5 N4 107.2(10) . . ? 
C10 N6 C9 105.9(10) . . ? 
C10 N6 C3 126.2(9) . . ? 
C9 N6 C3 127.8(10) . . ? 
H1A O1 H1B 107.8 . . ? 
N4 Zn1 N1 102.8(4) 2_664 . ? 
N4 Zn1 Br2 110.4(3) 2_664 . ? 
N1 Zn1 Br2 113.5(3) . . ? 
N4 Zn1 Br1 108.3(3) 2_664 . ? 
N1 Zn1 Br1 105.9(3) . . ? 
Br2 Zn1 Br1 115.06(7) . . ? 
 
_diffrn_measured_fraction_theta_max    0.980 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.980 
_refine_diff_density_max    2.418 
_refine_diff_density_min   -0.934 
_refine_diff_density_rms    0.220 

#END

 
data_4
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
 'C22 H16 Cd N14 S2, 2(H2 O)'
_chemical_formula_sum 
 'C22 H20 Cd N14 O2 S2' 
_chemical_formula_weight          689.04 
 
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' 
 'Cd'  'Cd'  -0.8075   1.2024 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'P 21/c'
_symmetry_space_group_name_Hall    '-P 2ybc'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    8.905(3) 
_cell_length_b                    11.572(4) 
_cell_length_c                    14.981(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  120.870(14) 
_cell_angle_gamma                 90.00 
_cell_volume                      1325.1(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     838
_cell_measurement_theta_min        2.37
_cell_measurement_theta_max       19.55
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.22 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.727 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              692 
_exptl_absorpt_coefficient_mu     1.034 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7821 
_exptl_absorpt_correction_T_max   0.8199 
_exptl_absorpt_process_details    'SADABS (Bruker, 2000)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             8503 
_diffrn_reflns_av_R_equivalents   0.0835 
_diffrn_reflns_av_sigmaI/netI     0.0889 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.37 
_diffrn_reflns_theta_max          25.99 
_reflns_number_total              2555 
_reflns_number_gt                 1814 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0409P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2555 
_refine_ls_number_parameters      193 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0747 
_refine_ls_R_factor_gt            0.0493 
_refine_ls_wR_factor_ref          0.1212 
_refine_ls_wR_factor_gt           0.1081 
_refine_ls_goodness_of_fit_ref    1.063 
_refine_ls_restrained_S_all       1.068 
_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 
C1 C 0.2560(7) 0.5365(4) -0.2575(4) 0.0257(12) Uani 1 1 d . . . 
C2 C 0.5288(6) 0.9766(4) 0.1383(4) 0.0219(11) Uani 1 1 d . . . 
C3 C 0.6944(6) 0.9759(4) 0.2273(4) 0.0228(12) Uani 1 1 d . . . 
H3 H 0.7641 0.9079 0.2483 0.027 Uiso 1 1 calc R . . 
C4 C 0.7552(6) 1.0774(4) 0.2849(4) 0.0233(11) Uani 1 1 d . . . 
C5 C 0.6536(6) 1.1753(4) 0.2579(4) 0.0259(12) Uani 1 1 d . . . 
H5 H 0.6962 1.2430 0.2995 0.031 Uiso 1 1 calc R . . 
C6 C 0.4887(7) 1.1741(4) 0.1697(4) 0.0264(12) Uani 1 1 d . . . 
H6 H 0.4183 1.2417 0.1507 0.032 Uiso 1 1 calc R . . 
C7 C 0.4247(6) 1.0766(4) 0.1088(4) 0.0244(12) Uani 1 1 d . . . 
H7 H 0.3119 1.0769 0.0478 0.029 Uiso 1 1 calc R . . 
C8 C 0.3004(6) 0.8556(4) -0.0074(4) 0.0265(12) Uani 1 1 d . . . 
H8 H 0.2109 0.9126 -0.0364 0.032 Uiso 1 1 calc R . . 
C9 C 0.5457(6) 0.7701(4) 0.0914(4) 0.0264(12) Uani 1 1 d . . . 
H9 H 0.6623 0.7539 0.1450 0.032 Uiso 1 1 calc R . . 
C10 C 1.0009(7) 1.1398(4) 0.4616(4) 0.0276(12) Uani 1 1 d . . . 
H10 H 0.9354 1.1857 0.4822 0.033 Uiso 1 1 calc R . . 
C11 C 1.0712(7) 1.0289(4) 0.3739(4) 0.0273(12) Uani 1 1 d . . . 
H11 H 1.0644 0.9815 0.3202 0.033 Uiso 1 1 calc R . . 
Cd1 Cd 0.5000 0.5000 0.0000 0.02101(19) Uani 1 2 d S . . 
N1 N 0.3765(6) 0.5252(4) -0.1750(4) 0.0318(11) Uani 1 1 d . . . 
N2 N 0.4411(5) 0.6965(3) 0.0199(3) 0.0258(10) Uani 1 1 d . . . 
N3 N 0.2833(5) 0.7517(4) -0.0438(3) 0.0262(10) Uani 1 1 d . . . 
N4 N 0.4625(5) 0.8730(3) 0.0775(3) 0.0230(9) Uani 1 1 d . . . 
N5 N 1.2170(5) 1.0540(4) 0.4605(3) 0.0259(10) Uani 1 1 d . . . 
N6 N 1.1720(6) 1.1260(4) 0.5169(3) 0.0307(11) Uani 1 1 d . . . 
N7 N 0.9311(5) 1.0796(3) 0.3712(3) 0.0231(9) Uani 1 1 d . . . 
O1 O 0.9612(6) 0.7379(5) 0.7515(4) 0.0746(17) Uani 1 1 d D . . 
H1A H 0.914(8) 0.771(7) 0.785(5) 0.089 Uiso 1 1 d D . . 
H1B H 1.069(3) 0.725(6) 0.793(4) 0.089 Uiso 1 1 d D . . 
S1 S 0.08462(19) 0.55252(13) -0.37544(11) 0.0349(4) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
C1 N1 1.156(7) . ? 
C1 S1 1.649(6) . ? 
C2 C3 1.391(7) . ? 
C2 C7 1.404(7) . ? 
C2 N4 1.437(6) . ? 
C3 C4 1.391(7) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.375(6) . ? 
C4 N7 1.431(6) . ? 
C5 C6 1.383(7) . ? 
C5 H5 0.9500 . ? 
C6 C7 1.377(7) . ? 
C6 H6 0.9500 . ? 
C7 H7 0.9500 . ? 
C8 N3 1.296(6) . ? 
C8 N4 1.363(6) . ? 
C8 H8 0.9500 . ? 
C9 N2 1.310(6) . ? 
C9 N4 1.361(6) . ? 
C9 H9 0.9500 . ? 
C10 N6 1.318(6) . ? 
C10 N7 1.357(6) . ? 
C10 H10 0.9500 . ? 
C11 N5 1.313(6) . ? 
C11 N7 1.360(6) . ? 
C11 H11 0.9500 . ? 
Cd1 N1 2.282(5) 3_665 ? 
Cd1 N1 2.282(5) . ? 
Cd1 N5 2.358(4) 4_475 ? 
Cd1 N5 2.358(4) 2_745 ? 
Cd1 N2 2.387(4) . ? 
Cd1 N2 2.387(4) 3_665 ? 
N2 N3 1.384(5) . ? 
N5 N6 1.384(6) . ? 
N5 Cd1 2.358(4) 2_755 ? 
O1 H1A 0.89(2) . ? 
O1 H1B 0.85(2) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 C1 S1 179.8(5) . . ? 
C3 C2 C7 120.7(4) . . ? 
C3 C2 N4 119.4(4) . . ? 
C7 C2 N4 119.9(4) . . ? 
C2 C3 C4 118.2(4) . . ? 
C2 C3 H3 120.9 . . ? 
C4 C3 H3 120.9 . . ? 
C5 C4 C3 121.7(5) . . ? 
C5 C4 N7 120.0(4) . . ? 
C3 C4 N7 118.2(4) . . ? 
C4 C5 C6 119.2(5) . . ? 
C4 C5 H5 120.4 . . ? 
C6 C5 H5 120.4 . . ? 
C7 C6 C5 121.1(5) . . ? 
C7 C6 H6 119.4 . . ? 
C5 C6 H6 119.4 . . ? 
C6 C7 C2 119.0(5) . . ? 
C6 C7 H7 120.5 . . ? 
C2 C7 H7 120.5 . . ? 
N3 C8 N4 111.6(4) . . ? 
N3 C8 H8 124.2 . . ? 
N4 C8 H8 124.2 . . ? 
N2 C9 N4 109.9(4) . . ? 
N2 C9 H9 125.0 . . ? 
N4 C9 H9 125.0 . . ? 
N6 C10 N7 110.8(5) . . ? 
N6 C10 H10 124.6 . . ? 
N7 C10 H10 124.6 . . ? 
N5 C11 N7 111.2(5) . . ? 
N5 C11 H11 124.4 . . ? 
N7 C11 H11 124.4 . . ? 
N1 Cd1 N1 180.0 3_665 . ? 
N1 Cd1 N5 94.45(15) 3_665 4_475 ? 
N1 Cd1 N5 85.55(15) . 4_475 ? 
N1 Cd1 N5 85.55(15) 3_665 2_745 ? 
N1 Cd1 N5 94.45(15) . 2_745 ? 
N5 Cd1 N5 180.00(19) 4_475 2_745 ? 
N1 Cd1 N2 89.19(15) 3_665 . ? 
N1 Cd1 N2 90.81(15) . . ? 
N5 Cd1 N2 90.51(14) 4_475 . ? 
N5 Cd1 N2 89.49(14) 2_745 . ? 
N1 Cd1 N2 90.81(15) 3_665 3_665 ? 
N1 Cd1 N2 89.19(15) . 3_665 ? 
N5 Cd1 N2 89.49(14) 4_475 3_665 ? 
N5 Cd1 N2 90.51(14) 2_745 3_665 ? 
N2 Cd1 N2 180.0 . 3_665 ? 
C1 N1 Cd1 151.5(4) . . ? 
C9 N2 N3 107.9(4) . . ? 
C9 N2 Cd1 127.7(3) . . ? 
N3 N2 Cd1 124.3(3) . . ? 
C8 N3 N2 106.3(4) . . ? 
C9 N4 C8 104.2(4) . . ? 
C9 N4 C2 128.3(4) . . ? 
C8 N4 C2 127.5(4) . . ? 
C11 N5 N6 106.6(4) . . ? 
C11 N5 Cd1 125.3(3) . 2_755 ? 
N6 N5 Cd1 127.8(3) . 2_755 ? 
C10 N6 N5 107.0(4) . . ? 
C10 N7 C11 104.3(4) . . ? 
C10 N7 C4 129.8(4) . . ? 
C11 N7 C4 125.5(4) . . ? 
H1A O1 H1B 111(5) . . ? 
 
_diffrn_measured_fraction_theta_max    0.983 
_diffrn_reflns_theta_full              25.99 
_diffrn_measured_fraction_theta_full   0.983 
_refine_diff_density_max    1.068 
_refine_diff_density_min   -0.929 
_refine_diff_density_rms    0.132 

# END

 
data_5 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety           
 'C20 H16 Cd N12, 2(B F4)'
_chemical_formula_sum 
 'C20 H16 B2 Cd F8 N12' 
_chemical_formula_weight          710.47 
 
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' 
 'F'  'F'   0.0171   0.0103 
 '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' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'P 21/c'
_symmetry_space_group_name_Hall    '-P 2ybc'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    14.287(11) 
_cell_length_b                    22.046(16) 
_cell_length_c                    8.268(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.563(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2575(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used    1139
_cell_measurement_theta_min        2.35
_cell_measurement_theta_max       20.53
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.833 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1400 
_exptl_absorpt_coefficient_mu     0.944 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8336 
_exptl_absorpt_correction_T_max   0.9283 
_exptl_absorpt_process_details    'SADABS (Bruker, 2000)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             11671 
_diffrn_reflns_av_R_equivalents   0.1077 
_diffrn_reflns_av_sigmaI/netI     0.1618 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          1.44 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              4504 
_reflns_number_gt                 2288 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1363P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0057(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          4504 
_refine_ls_number_parameters      369 
_refine_ls_number_restraints      381 
_refine_ls_R_factor_all           0.1698 
_refine_ls_R_factor_gt            0.0910 
_refine_ls_wR_factor_ref          0.2697 
_refine_ls_wR_factor_gt           0.2301 
_refine_ls_goodness_of_fit_ref    1.061 
_refine_ls_restrained_S_all       1.135 
_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 
B1 B 0.8658(9) 0.4845(6) 0.7016(15) 0.054(6) Uiso 1 1 d D . . 
F4 F 0.9071(8) 0.4288(4) 0.7169(13) 0.083(4) Uiso 1 1 d D A . 
F1 F 0.9216(16) 0.5228(8) 0.806(3) 0.096(11) Uiso 0.46(3) 1 d PD A 1 
F2 F 0.8513(18) 0.5058(9) 0.5492(18) 0.081(10) Uiso 0.46(3) 1 d PD A 1 
F3 F 0.7800(12) 0.4807(9) 0.759(3) 0.093(11) Uiso 0.46(3) 1 d PD A 1 
F1' F 0.7770(12) 0.4775(9) 0.614(3) 0.125(12) Uiso 0.54(3) 1 d PD A 2 
F2' F 0.9160(16) 0.5193(8) 0.605(3) 0.111(11) Uiso 0.54(3) 1 d PD A 2 
F3' F 0.8652(17) 0.5113(8) 0.8448(18) 0.096(9) Uiso 0.54(3) 1 d PD A 2 
B2 B 0.5413(9) 0.3392(6) 0.1293(15) 0.050(5) Uiso 1 1 d D . . 
F5 F 0.6399(9) 0.3420(9) 0.145(2) 0.070(8) Uiso 0.52(2) 1 d PD B 3 
F6 F 0.5060(13) 0.3224(9) -0.0258(17) 0.080(8) Uiso 0.52(2) 1 d PD B 3 
F7 F 0.5253(16) 0.2910(8) 0.229(2) 0.102(10) Uiso 0.52(2) 1 d PD B 3 
F8 F 0.5096(16) 0.3907(7) 0.179(3) 0.098(9) Uiso 0.52(2) 1 d PD B 3 
F5' F 0.4541(12) 0.3179(10) 0.145(3) 0.093(10) Uiso 0.48(2) 1 d PD B 4 
F6' F 0.6079(13) 0.2979(9) 0.151(2) 0.074(8) Uiso 0.48(2) 1 d PD B 4 
F7' F 0.5355(18) 0.3673(12) -0.022(2) 0.134(13) Uiso 0.48(2) 1 d PD B 4 
F8' F 0.5608(17) 0.3866(8) 0.241(3) 0.095(10) Uiso 0.48(2) 1 d PD B 4 
C1 C -0.1727(11) 0.9080(6) -0.326(2) 0.043(4) Uani 1 1 d . . . 
C2 C -0.1399(10) 0.9666(6) -0.2938(18) 0.033(4) Uani 1 1 d . . . 
H2 H -0.0767 0.9748 -0.2449 0.039 Uiso 1 1 calc R . . 
C3 C -0.2050(12) 1.0121(6) -0.337(2) 0.045(4) Uani 1 1 d . . . 
C4 C -0.2934(12) 1.0030(7) -0.413(2) 0.047(4) Uani 1 1 d . . . 
H4 H -0.3332 1.0369 -0.4442 0.056 Uiso 1 1 calc R . . 
C5 C -0.3276(13) 0.9442(8) -0.447(2) 0.054(5) Uani 1 1 d . . . 
H5 H -0.3909 0.9377 -0.4979 0.065 Uiso 1 1 calc R . . 
C6 C -0.2667(11) 0.8951(8) -0.404(2) 0.050(5) Uani 1 1 d . . . 
H6 H -0.2872 0.8545 -0.4264 0.060 Uiso 1 1 calc R . . 
C7 C -0.0634(10) 0.8376(7) -0.1457(18) 0.033(4) Uani 1 1 d . . . 
H7 H -0.0792 0.8500 -0.0431 0.040 Uiso 1 1 calc R . . 
C8 C -0.0651(10) 0.8290(7) -0.4035(18) 0.032(4) Uani 1 1 d . . . 
H8 H -0.0822 0.8334 -0.5184 0.038 Uiso 1 1 calc R . . 
C9 C -0.1526(12) 1.1083(6) -0.176(2) 0.043(4) Uani 1 1 d . . . 
H9 H -0.1632 1.0945 -0.0709 0.052 Uiso 1 1 calc R . . 
C10 C -0.1435(11) 1.1103(6) -0.430(2) 0.041(4) Uani 1 1 d . . . 
H10 H -0.1463 1.0987 -0.5417 0.049 Uiso 1 1 calc R . . 
C11 C 0.4449(10) 0.6309(7) 0.3684(18) 0.035(4) Uani 1 1 d . . . 
C12 C 0.5237(13) 0.6588(9) 0.446(2) 0.055(5) Uani 1 1 d . . . 
H12 H 0.5205 0.7001 0.4781 0.065 Uiso 1 1 calc R . . 
C13 C 0.6088(12) 0.6278(8) 0.479(2) 0.052(5) Uani 1 1 d . . . 
C14 C 0.6158(12) 0.5691(7) 0.432(2) 0.049(5) Uani 1 1 d . . . 
H14 H 0.6746 0.5482 0.4506 0.058 Uiso 1 1 calc R . . 
C15 C 0.5326(11) 0.5402(7) 0.356(2) 0.056(5) Uani 1 1 d . . . 
H15 H 0.5357 0.4989 0.3247 0.067 Uiso 1 1 calc R . . 
C16 C 0.4481(12) 0.5697(7) 0.326(2) 0.051(5) Uani 1 1 d . . . 
H16 H 0.3925 0.5490 0.2776 0.061 Uiso 1 1 calc R . . 
C17 C 0.3070(10) 0.6804(7) 0.4595(19) 0.037(4) Uani 1 1 d . . . 
H17 H 0.3256 0.6736 0.5732 0.044 Uiso 1 1 calc R . . 
C18 C 0.3095(11) 0.6798(6) 0.2012(18) 0.034(4) Uani 1 1 d . . . 
H18 H 0.3286 0.6731 0.0974 0.041 Uiso 1 1 calc R . . 
C19 C 0.7082(16) 0.7193(10) 0.561(3) 0.096(9) Uani 1 1 d . . . 
H19 H 0.6686 0.7482 0.4989 0.116 Uiso 1 1 calc R . . 
C20 C 0.7619(13) 0.6365(8) 0.667(2) 0.055(5) Uani 1 1 d . . . 
H20 H 0.7679 0.5953 0.7013 0.067 Uiso 1 1 calc R . . 
Cd1 Cd 0.11109(6) 0.75295(4) 0.03095(11) 0.0200(4) Uani 1 1 d . . . 
N1 N 0.0000(9) 0.7924(5) -0.3336(15) 0.034(3) Uani 1 1 d . . . 
N2 N -0.0006(9) 0.7980(5) -0.1665(15) 0.035(3) Uani 1 1 d . . . 
N3 N -0.1038(9) 0.8590(5) -0.2942(16) 0.038(3) Uani 1 1 d . . . 
N4 N -0.1178(9) 1.1636(5) -0.3704(16) 0.036(3) Uani 1 1 d . . . 
N5 N -0.1237(9) 1.1630(5) -0.2043(14) 0.033(3) Uani 1 1 d . . . 
N6 N -0.1653(9) 1.0744(5) -0.3096(16) 0.037(3) Uani 1 1 d . . . 
N7 N 0.2303(9) 0.7084(5) 0.2272(15) 0.035(3) Uani 1 1 d . . . 
N8 N 0.2310(9) 0.7080(5) 0.3977(15) 0.037(3) Uani 1 1 d . . . 
N9 N 0.3564(8) 0.6625(6) 0.3432(13) 0.030(3) Uani 1 1 d . . . 
N10 N 0.8227(11) 0.6787(7) 0.716(2) 0.068(5) Uani 1 1 d . . . 
N11 N 0.7877(12) 0.7319(7) 0.655(3) 0.090(7) Uani 1 1 d . . . 
N12 N 0.6904(10) 0.6585(7) 0.5648(19) 0.057(4) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
B1 F3' 1.324(13) . ? 
B1 F2 1.332(13) . ? 
B1 F4 1.360(12) . ? 
B1 F1' 1.372(13) . ? 
B1 F1 1.373(13) . ? 
B1 F3 1.382(13) . ? 
B1 F2' 1.384(13) . ? 
B2 F6' 1.310(13) . ? 
B2 F8 1.311(13) . ? 
B2 F5' 1.355(13) . ? 
B2 F6 1.358(13) . ? 
B2 F7 1.387(13) . ? 
B2 F7' 1.388(13) . ? 
B2 F8' 1.393(13) . ? 
B2 F5 1.397(13) . ? 
C1 C2 1.386(19) . ? 
C1 C6 1.43(2) . ? 
C1 N3 1.458(19) . ? 
C2 C3 1.38(2) . ? 
C2 H2 0.9500 . ? 
C3 C4 1.34(2) . ? 
C3 N6 1.490(18) . ? 
C4 C5 1.40(2) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.40(2) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C7 N2 1.280(17) . ? 
C7 N3 1.362(17) . ? 
C7 H7 0.9500 . ? 
C8 N1 1.300(17) . ? 
C8 N3 1.307(18) . ? 
C8 H8 0.9500 . ? 
C9 N5 1.308(18) . ? 
C9 N6 1.327(18) . ? 
C9 H9 0.9500 . ? 
C10 N4 1.308(17) . ? 
C10 N6 1.347(19) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.36(2) . ? 
C11 C16 1.40(2) . ? 
C11 N9 1.432(17) . ? 
C12 C13 1.39(2) . ? 
C12 H12 0.9500 . ? 
C13 C14 1.36(2) . ? 
C13 N12 1.44(2) . ? 
C14 C15 1.41(2) . ? 
C14 H14 0.9500 . ? 
C15 C16 1.36(2) . ? 
C15 H15 0.9500 . ? 
C16 H16 0.9500 . ? 
C17 N8 1.282(17) . ? 
C17 N9 1.335(18) . ? 
C17 H17 0.9500 . ? 
C18 N9 1.319(17) . ? 
C18 N7 1.341(18) . ? 
C18 H18 0.9500 . ? 
C19 N11 1.31(2) . ? 
C19 N12 1.36(2) . ? 
C19 H19 0.9500 . ? 
C20 N10 1.29(2) . ? 
C20 N12 1.32(2) . ? 
C20 H20 0.9500 . ? 
Cd1 N1 2.302(13) 4_576 ? 
Cd1 N2 2.329(11) . ? 
Cd1 N5 2.333(11) 3_575 ? 
Cd1 N8 2.335(13) 4_575 ? 
Cd1 N7 2.382(12) . ? 
Cd1 N4 2.385(11) 2_544 ? 
N1 N2 1.389(16) . ? 
N1 Cd1 2.302(13) 4_575 ? 
N4 N5 1.389(16) . ? 
N4 Cd1 2.385(11) 2_554 ? 
N5 Cd1 2.333(11) 3_575 ? 
N7 N8 1.408(17) . ? 
N8 Cd1 2.335(13) 4_576 ? 
N10 N11 1.34(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 
F3' B1 F2 131.9(15) . . ? 
F3' B1 F4 112.3(11) . . ? 
F2 B1 F4 114.2(11) . . ? 
F3' B1 F1' 113.2(12) . . ? 
F2 B1 F1' 62.6(12) . . ? 
F4 B1 F1' 107.5(11) . . ? 
F3' B1 F1 41.0(11) . . ? 
F2 B1 F1 111.7(12) . . ? 
F4 B1 F1 107.1(11) . . ? 
F1' B1 F1 143.6(14) . . ? 
F3' B1 F3 66.1(12) . . ? 
F2 B1 F3 109.1(11) . . ? 
F4 B1 F3 107.9(11) . . ? 
F1' B1 F3 51.5(12) . . ? 
F1 B1 F3 106.4(11) . . ? 
F3' B1 F2' 110.1(11) . . ? 
F2 B1 F2' 43.8(11) . . ? 
F4 B1 F2' 107.4(11) . . ? 
F1' B1 F2' 106.0(11) . . ? 
F1 B1 F2' 73.7(12) . . ? 
F3 B1 F2' 142.8(14) . . ? 
F6' B2 F8 146.8(14) . . ? 
F6' B2 F5' 113.9(11) . . ? 
F8 B2 F5' 84.6(13) . . ? 
F6' B2 F6 95.7(13) . . ? 
F8 B2 F6 115.9(12) . . ? 
F5' B2 F6 77.2(13) . . ? 
F6' B2 F7 64.3(11) . . ? 
F8 B2 F7 112.5(12) . . ? 
F5' B2 F7 56.1(11) . . ? 
F6 B2 F7 106.5(11) . . ? 
F6' B2 F7' 112.2(12) . . ? 
F8 B2 F7' 85.4(14) . . ? 
F5' B2 F7' 108.0(11) . . ? 
F6 B2 F7' 46.1(12) . . ? 
F7 B2 F7' 152.5(14) . . ? 
F6' B2 F8' 111.1(11) . . ? 
F8 B2 F8' 35.7(11) . . ? 
F5' B2 F8' 107.1(11) . . ? 
F6 B2 F8' 147.0(13) . . ? 
F7 B2 F8' 102.4(14) . . ? 
F7' B2 F8' 103.9(11) . . ? 
F6' B2 F5 46.8(10) . . ? 
F8 B2 F5 108.8(11) . . ? 
F5' B2 F5 159.1(13) . . ? 
F6 B2 F5 109.2(11) . . ? 
F7 B2 F5 103.3(10) . . ? 
F7' B2 F5 89.4(13) . . ? 
F8' B2 F5 78.7(12) . . ? 
C2 C1 C6 122.7(15) . . ? 
C2 C1 N3 117.1(13) . . ? 
C6 C1 N3 119.8(13) . . ? 
C3 C2 C1 115.6(14) . . ? 
C3 C2 H2 122.2 . . ? 
C1 C2 H2 122.2 . . ? 
C4 C3 C2 124.5(15) . . ? 
C4 C3 N6 121.3(14) . . ? 
C2 C3 N6 113.9(14) . . ? 
C3 C4 C5 120.6(16) . . ? 
C3 C4 H4 119.7 . . ? 
C5 C4 H4 119.7 . . ? 
C6 C5 C4 118.7(16) . . ? 
C6 C5 H5 120.7 . . ? 
C4 C5 H5 120.7 . . ? 
C5 C6 C1 117.8(15) . . ? 
C5 C6 H6 121.1 . . ? 
C1 C6 H6 121.1 . . ? 
N2 C7 N3 109.1(13) . . ? 
N2 C7 H7 125.5 . . ? 
N3 C7 H7 125.5 . . ? 
N1 C8 N3 110.8(13) . . ? 
N1 C8 H8 124.6 . . ? 
N3 C8 H8 124.6 . . ? 
N5 C9 N6 112.0(14) . . ? 
N5 C9 H9 124.0 . . ? 
N6 C9 H9 124.0 . . ? 
N4 C10 N6 109.2(15) . . ? 
N4 C10 H10 125.4 . . ? 
N6 C10 H10 125.4 . . ? 
C12 C11 C16 120.1(15) . . ? 
C12 C11 N9 120.0(14) . . ? 
C16 C11 N9 119.7(14) . . ? 
C11 C12 C13 120.6(17) . . ? 
C11 C12 H12 119.7 . . ? 
C13 C12 H12 119.7 . . ? 
C14 C13 C12 121.0(17) . . ? 
C14 C13 N12 119.9(15) . . ? 
C12 C13 N12 119.1(16) . . ? 
C13 C14 C15 117.5(15) . . ? 
C13 C14 H14 121.2 . . ? 
C15 C14 H14 121.2 . . ? 
C16 C15 C14 122.2(15) . . ? 
C16 C15 H15 118.9 . . ? 
C14 C15 H15 118.9 . . ? 
C15 C16 C11 118.4(15) . . ? 
C15 C16 H16 120.8 . . ? 
C11 C16 H16 120.8 . . ? 
N8 C17 N9 111.1(14) . . ? 
N8 C17 H17 124.4 . . ? 
N9 C17 H17 124.4 . . ? 
N9 C18 N7 108.8(13) . . ? 
N9 C18 H18 125.6 . . ? 
N7 C18 H18 125.6 . . ? 
N11 C19 N12 110.0(19) . . ? 
N11 C19 H19 125.0 . . ? 
N12 C19 H19 125.0 . . ? 
N10 C20 N12 110.7(16) . . ? 
N10 C20 H20 124.7 . . ? 
N12 C20 H20 124.7 . . ? 
N1 Cd1 N2 94.4(4) 4_576 . ? 
N1 Cd1 N5 92.4(4) 4_576 3_575 ? 
N2 Cd1 N5 94.2(4) . 3_575 ? 
N1 Cd1 N8 175.4(4) 4_576 4_575 ? 
N2 Cd1 N8 89.2(4) . 4_575 ? 
N5 Cd1 N8 90.1(4) 3_575 4_575 ? 
N1 Cd1 N7 88.0(4) 4_576 . ? 
N2 Cd1 N7 177.7(5) . . ? 
N5 Cd1 N7 85.8(4) 3_575 . ? 
N8 Cd1 N7 88.5(4) 4_575 . ? 
N1 Cd1 N4 90.0(4) 4_576 2_544 ? 
N2 Cd1 N4 92.4(4) . 2_544 ? 
N5 Cd1 N4 172.7(4) 3_575 2_544 ? 
N8 Cd1 N4 87.0(4) 4_575 2_544 ? 
N7 Cd1 N4 87.4(4) . 2_544 ? 
C8 N1 N2 106.0(12) . . ? 
C8 N1 Cd1 123.6(10) . 4_575 ? 
N2 N1 Cd1 129.0(9) . 4_575 ? 
C7 N2 N1 107.6(11) . . ? 
C7 N2 Cd1 128.1(10) . . ? 
N1 N2 Cd1 123.6(9) . . ? 
C8 N3 C7 106.3(12) . . ? 
C8 N3 C1 126.3(14) . . ? 
C7 N3 C1 127.2(14) . . ? 
C10 N4 N5 108.2(12) . . ? 
C10 N4 Cd1 124.3(11) . 2_554 ? 
N5 N4 Cd1 124.9(8) . 2_554 ? 
C9 N5 N4 104.9(11) . . ? 
C9 N5 Cd1 128.2(10) . 3_575 ? 
N4 N5 Cd1 126.1(8) . 3_575 ? 
C9 N6 C10 105.7(13) . . ? 
C9 N6 C3 130.3(13) . . ? 
C10 N6 C3 123.7(14) . . ? 
C18 N7 N8 106.1(12) . . ? 
C18 N7 Cd1 128.3(10) . . ? 
N8 N7 Cd1 125.6(9) . . ? 
C17 N8 N7 106.4(13) . . ? 
C17 N8 Cd1 128.6(11) . 4_576 ? 
N7 N8 Cd1 125.0(9) . 4_576 ? 
C18 N9 C17 107.6(12) . . ? 
C18 N9 C11 126.2(13) . . ? 
C17 N9 C11 126.1(12) . . ? 
C20 N10 N11 108.5(16) . . ? 
C19 N11 N10 106.2(17) . . ? 
C20 N12 C19 104.4(16) . . ? 
C20 N12 C13 129.5(16) . . ? 
C19 N12 C13 126.1(16) . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    1.355 
_refine_diff_density_min   -1.379 
_refine_diff_density_rms    0.222 

#END 


 
data_6 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
 'C20 H16 Cd N12, 2(Cl O4)'
_chemical_formula_sum 
 'C20 H16 Cd Cl2 N12 O8' 
_chemical_formula_weight          735.75 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'P 21/c'
_symmetry_space_group_name_Hall    '-P 2ybc'

loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    14.327(3) 
_cell_length_b                    22.105(5) 
_cell_length_c                    8.3039(19) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.790(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2599.0(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used    1064
_cell_measurement_theta_min        2.34
_cell_measurement_theta_max       20.45
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.880 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1464 
_exptl_absorpt_coefficient_mu     1.119 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7301 
_exptl_absorpt_correction_T_max   0.8501 
_exptl_absorpt_process_details    'SADABS (Bruker, 2000)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             12989 
_diffrn_reflns_av_R_equivalents   0.0902 
_diffrn_reflns_av_sigmaI/netI     0.1159 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          1.44 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              4552 
_reflns_number_gt                 2697 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0556P)²+2.0786P] 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          4552 
_refine_ls_number_parameters      378 
_refine_ls_number_restraints      181 
_refine_ls_R_factor_all           0.1165 
_refine_ls_R_factor_gt            0.0573 
_refine_ls_wR_factor_ref          0.1446 
_refine_ls_wR_factor_gt           0.1195 
_refine_ls_goodness_of_fit_ref    1.011 
_refine_ls_restrained_S_all       1.067 
_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 
Cl1 Cl 0.12959(18) -0.00835(12) 0.8006(3) 0.0431(7) Uani 1 1 d D . . 
O1 O 0.0907(5) -0.0691(3) 0.7858(8) 0.0516(19) Uiso 1 1 d D A . 
O2 O 0.0700(9) 0.0266(5) 0.8923(15) 0.065(5) Uiso 0.531(14) 1 d PD A 1 
O3 O 0.1308(11) 0.0171(6) 0.6487(14) 0.089(6) Uiso 0.531(14) 1 d PD A 1 
O4 O 0.2207(8) -0.0131(6) 0.9004(17) 0.078(6) Uiso 0.531(14) 1 d PD A 1 
O2' O 0.0669(10) 0.0320(6) 0.6988(19) 0.090(8) Uiso 0.469(14) 1 d PD A 2 
O3' O 0.2151(9) -0.0085(6) 0.7222(18) 0.069(6) Uiso 0.469(14) 1 d PD A 2 
O4' O 0.1525(13) 0.0122(7) 0.9597(14) 0.097(8) Uiso 0.469(14) 1 d PD A 2 
Cl2 Cl 0.45832(18) 0.66146(11) 0.8633(3) 0.0392(6) Uani 1 1 d D . . 
O5 O 0.4958(7) 0.6763(5) 1.0299(10) 0.047(4) Uiso 0.594(12) 1 d PD B 3 
O6 O 0.4888(9) 0.6068(4) 0.8101(15) 0.063(4) Uiso 0.594(12) 1 d PD B 3 
O7 O 0.3544(6) 0.6624(6) 0.8489(12) 0.048(4) Uiso 0.594(12) 1 d PD B 3 
O8 O 0.4809(9) 0.7123(5) 0.7632(13) 0.065(5) Uiso 0.594(12) 1 d PD B 3 
O5' O 0.4723(12) 0.6348(8) 1.0256(14) 0.064(6) Uiso 0.406(12) 1 d PD B 4 
O6' O 0.4364(12) 0.6084(6) 0.7537(18) 0.061(6) Uiso 0.406(12) 1 d PD B 4 
O7' O 0.3810(9) 0.7000(6) 0.8424(16) 0.033(5) Uiso 0.406(12) 1 d PD B 4 
O8' O 0.5440(9) 0.6868(7) 0.828(2) 0.061(7) Uiso 0.406(12) 1 d PD B 4 
C1 C -0.1790(6) 0.9101(4) -0.3310(10) 0.022(2) Uani 1 1 d . . . 
C2 C -0.1434(5) 0.9666(4) -0.2947(9) 0.0173(18) Uani 1 1 d . . . 
H2 H -0.0800 0.9722 -0.2436 0.021 Uiso 1 1 calc R . . 
C3 C -0.2022(6) 1.0151(4) -0.3346(9) 0.022(2) Uani 1 1 d . . . 
C4 C -0.2950(6) 1.0069(4) -0.4098(11) 0.031(2) Uani 1 1 d . . . 
H4 H -0.3350 1.0407 -0.4376 0.038 Uiso 1 1 calc R . . 
C5 C -0.3277(6) 0.9494(4) -0.4434(11) 0.032(2) Uani 1 1 d . . . 
H5 H -0.3910 0.9436 -0.4950 0.039 Uiso 1 1 calc R . . 
C6 C -0.2706(6) 0.9001(4) -0.4035(11) 0.028(2) Uani 1 1 d . . . 
H6 H -0.2937 0.8602 -0.4253 0.033 Uiso 1 1 calc R . . 
C7 C -0.0696(5) 0.8398(4) -0.1514(9) 0.0207(19) Uani 1 1 d . . . 
H7 H -0.0824 0.8539 -0.0489 0.025 Uiso 1 1 calc R . . 
C8 C -0.0738(6) 0.8282(3) -0.4062(10) 0.022(2) Uani 1 1 d . . . 
H8 H -0.0903 0.8324 -0.5208 0.027 Uiso 1 1 calc R . . 
C9 C -0.1485(6) 1.1084(4) -0.1729(10) 0.028(2) Uani 1 1 d . . . 
H9 H -0.1599 1.0944 -0.0695 0.033 Uiso 1 1 calc R . . 
C10 C -0.1366(6) 1.1123(4) -0.4259(10) 0.026(2) Uani 1 1 d . . . 
H10 H -0.1377 1.1012 -0.5367 0.032 Uiso 1 1 calc R . . 
C11 C 0.4375(6) 0.6305(4) 0.3655(9) 0.023(2) Uani 1 1 d . . . 
C12 C 0.5154(6) 0.6608(4) 0.4410(10) 0.025(2) Uani 1 1 d . . . 
H12 H 0.5118 0.7021 0.4713 0.030 Uiso 1 1 calc R . . 
C13 C 0.5994(6) 0.6291(4) 0.4715(10) 0.026(2) Uani 1 1 d . . . 
C14 C 0.6042(6) 0.5698(4) 0.4246(11) 0.034(2) Uani 1 1 d . . . 
H14 H 0.6627 0.5488 0.4459 0.040 Uiso 1 1 calc R . . 
C15 C 0.5247(6) 0.5402(4) 0.3466(12) 0.041(3) Uani 1 1 d . . . 
H15 H 0.5286 0.4993 0.3131 0.050 Uiso 1 1 calc R . . 
C16 C 0.4396(6) 0.5709(4) 0.3180(11) 0.032(2) Uani 1 1 d . . . 
H16 H 0.3839 0.5513 0.2668 0.038 Uiso 1 1 calc R . . 
C17 C 0.2983(6) 0.6816(4) 0.4547(11) 0.029(2) Uani 1 1 d . . . 
H17 H 0.3168 0.6753 0.5683 0.034 Uiso 1 1 calc R . . 
C18 C 0.2973(6) 0.6805(4) 0.1968(10) 0.023(2) Uani 1 1 d . . . 
H18 H 0.3145 0.6734 0.0924 0.027 Uiso 1 1 calc R . . 
C19 C 0.7040(8) 0.7192(5) 0.5413(14) 0.057(3) Uani 1 1 d . . . 
H19 H 0.6689 0.7472 0.4691 0.068 Uiso 1 1 calc R . . 
C20 C 0.7479(7) 0.6396(5) 0.6670(12) 0.046(3) Uani 1 1 d . . . 
H20 H 0.7504 0.5989 0.7037 0.055 Uiso 1 1 calc R . . 
Cd1 Cd 0.10155(4) 0.75333(3) 0.02740(6) 0.01729(19) Uani 1 1 d . . . 
N1 N -0.0098(5) 0.7915(3) -0.3361(8) 0.0217(16) Uani 1 1 d . . . 
N2 N -0.0071(5) 0.7987(3) -0.1690(8) 0.0194(15) Uani 1 1 d . . . 
N3 N -0.1141(4) 0.8599(3) -0.2962(7) 0.0186(15) Uani 1 1 d . . . 
N4 N -0.1094(5) 1.1647(3) -0.3660(8) 0.0241(17) Uani 1 1 d . . . 
N5 N -0.1164(5) 1.1620(3) -0.2000(8) 0.0249(17) Uani 1 1 d . . . 
N6 N -0.1632(5) 1.0753(3) -0.3109(8) 0.0225(16) Uani 1 1 d . . . 
N7 N 0.2207(5) 0.7086(3) 0.2234(7) 0.0229(16) Uani 1 1 d . . . 
N8 N 0.2216(5) 0.7091(3) 0.3899(8) 0.0210(16) Uani 1 1 d . . . 
N9 N 0.3479(5) 0.6631(3) 0.3389(8) 0.0256(17) Uani 1 1 d . . . 
N10 N 0.8107(6) 0.6802(4) 0.7243(10) 0.044(2) Uani 1 1 d . . . 
N11 N 0.7808(6) 0.7329(4) 0.6410(11) 0.051(2) Uani 1 1 d . . . 
N12 N 0.6806(5) 0.6601(3) 0.5536(8) 0.0288(18) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cl1 O3 1.383(10) . ? 
Cl1 O4' 1.388(11) . ? 
Cl1 O4 1.438(10) . ? 
Cl1 O2' 1.444(11) . ? 
Cl1 O2 1.451(10) . ? 
Cl1 O1 1.452(6) . ? 
Cl1 O3' 1.473(10) . ? 
Cl2 O6 1.380(9) . ? 
Cl2 O7' 1.387(10) . ? 
Cl2 O8' 1.419(10) . ? 
Cl2 O5 1.443(8) . ? 
Cl2 O5' 1.456(10) . ? 
Cl2 O8 1.463(9) . ? 
Cl2 O7 1.475(9) . ? 
Cl2 O6' 1.489(10) . ? 
C1 C2 1.367(11) . ? 
C1 C6 1.376(11) . ? 
C1 N3 1.448(10) . ? 
C2 C3 1.372(11) . ? 
C2 H2 0.9500 . ? 
C3 C4 1.392(11) . ? 
C3 N6 1.444(10) . ? 
C4 C5 1.367(11) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.374(11) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C7 N2 1.299(10) . ? 
C7 N3 1.347(9) . ? 
C7 H7 0.9500 . ? 
C8 N1 1.295(10) . ? 
C8 N3 1.348(10) . ? 
C8 H8 0.9500 . ? 
C9 N5 1.303(10) . ? 
C9 N6 1.349(10) . ? 
C9 H9 0.9500 . ? 
C10 N4 1.298(10) . ? 
C10 N6 1.356(10) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.370(11) . ? 
C11 C16 1.376(12) . ? 
C11 N9 1.459(10) . ? 
C12 C13 1.383(11) . ? 
C12 H12 0.9500 . ? 
C13 C14 1.372(12) . ? 
C13 N12 1.430(11) . ? 
C14 C15 1.386(12) . ? 
C14 H14 0.9500 . ? 
C15 C16 1.384(12) . ? 
C15 H15 0.9500 . ? 
C16 H16 0.9500 . ? 
C17 N8 1.299(10) . ? 
C17 N9 1.344(10) . ? 
C17 H17 0.9500 . ? 
C18 N7 1.309(10) . ? 
C18 N9 1.343(10) . ? 
C18 H18 0.9500 . ? 
C19 N11 1.308(12) . ? 
C19 N12 1.355(12) . ? 
C19 H19 0.9500 . ? 
C20 N10 1.309(11) . ? 
C20 N12 1.321(11) . ? 
C20 H20 0.9500 . ? 
Cd1 N2 2.305(6) . ? 
Cd1 N1 2.316(7) 4_576 ? 
Cd1 N5 2.348(7) 3_575 ? 
Cd1 N8 2.356(7) 4_575 ? 
Cd1 N4 2.385(7) 2_544 ? 
Cd1 N7 2.386(6) . ? 
N1 N2 1.391(9) . ? 
N1 Cd1 2.316(7) 4_575 ? 
N4 N5 1.398(9) . ? 
N4 Cd1 2.386(7) 2_554 ? 
N5 Cd1 2.348(7) 3_575 ? 
N7 N8 1.381(8) . ? 
N8 Cd1 2.356(7) 4_576 ? 
N10 N11 1.389(11) . ? 
 
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 
O3 Cl1 O4' 134.5(9) . . ? 
O3 Cl1 O4 114.7(8) . . ? 
O4' Cl1 O4 54.1(8) . . ? 
O3 Cl1 O2' 46.2(8) . . ? 
O4' Cl1 O2' 113.0(8) . . ? 
O4 Cl1 O2' 144.2(9) . . ? 
O3 Cl1 O2 110.6(7) . . ? 
O4' Cl1 O2 53.0(8) . . ? 
O4 Cl1 O2 106.9(7) . . ? 
O2' Cl1 O2 67.3(8) . . ? 
O3 Cl1 O1 110.9(6) . . ? 
O4' Cl1 O1 114.5(7) . . ? 
O4 Cl1 O1 106.5(6) . . ? 
O2' Cl1 O1 109.0(7) . . ? 
O2 Cl1 O1 106.8(6) . . ? 
O3 Cl1 O3' 58.1(7) . . ? 
O4' Cl1 O3' 109.3(8) . . ? 
O4 Cl1 O3' 60.8(7) . . ? 
O2' Cl1 O3' 103.2(7) . . ? 
O2 Cl1 O3' 146.0(8) . . ? 
O1 Cl1 O3' 107.1(6) . . ? 
O6 Cl2 O7' 141.5(8) . . ? 
O6 Cl2 O8' 87.4(8) . . ? 
O7' Cl2 O8' 115.5(8) . . ? 
O6 Cl2 O5 114.6(6) . . ? 
O7' Cl2 O5 98.8(7) . . ? 
O8' Cl2 O5 84.2(8) . . ? 
O6 Cl2 O5' 86.4(8) . . ? 
O7' Cl2 O5' 111.0(7) . . ? 
O8' Cl2 O5' 110.4(8) . . ? 
O5 Cl2 O5' 39.4(7) . . ? 
O6 Cl2 O8 112.5(6) . . ? 
O7' Cl2 O8 72.5(7) . . ? 
O8' Cl2 O8 46.2(7) . . ? 
O5 Cl2 O8 106.7(6) . . ? 
O5' Cl2 O8 145.7(8) . . ? 
O6 Cl2 O7 110.6(6) . . ? 
O7' Cl2 O7 37.3(6) . . ? 
O8' Cl2 O7 150.6(8) . . ? 
O5 Cl2 O7 107.3(6) . . ? 
O5' Cl2 O7 94.3(8) . . ? 
O8 Cl2 O7 104.5(6) . . ? 
O6 Cl2 O6' 33.1(7) . . ? 
O7' Cl2 O6' 108.5(8) . . ? 
O8' Cl2 O6' 107.1(8) . . ? 
O5 Cl2 O6' 141.1(8) . . ? 
O5' Cl2 O6' 103.5(8) . . ? 
O8 Cl2 O6' 107.6(8) . . ? 
O7 Cl2 O6' 81.1(8) . . ? 
C2 C1 C6 122.8(8) . . ? 
C2 C1 N3 116.8(7) . . ? 
C6 C1 N3 120.3(7) . . ? 
C1 C2 C3 117.8(7) . . ? 
C1 C2 H2 121.1 . . ? 
C3 C2 H2 121.1 . . ? 
C2 C3 C4 121.1(8) . . ? 
C2 C3 N6 118.4(7) . . ? 
C4 C3 N6 120.3(8) . . ? 
C5 C4 C3 119.2(8) . . ? 
C5 C4 H4 120.4 . . ? 
C3 C4 H4 120.4 . . ? 
C4 C5 C6 121.0(8) . . ? 
C4 C5 H5 119.5 . . ? 
C6 C5 H5 119.5 . . ? 
C5 C6 C1 118.2(8) . . ? 
C5 C6 H6 120.9 . . ? 
C1 C6 H6 120.9 . . ? 
N2 C7 N3 111.7(7) . . ? 
N2 C7 H7 124.2 . . ? 
N3 C7 H7 124.2 . . ? 
N1 C8 N3 111.6(7) . . ? 
N1 C8 H8 124.2 . . ? 
N3 C8 H8 124.2 . . ? 
N5 C9 N6 111.1(7) . . ? 
N5 C9 H9 124.5 . . ? 
N6 C9 H9 124.5 . . ? 
N4 C10 N6 111.7(7) . . ? 
N4 C10 H10 124.2 . . ? 
N6 C10 H10 124.2 . . ? 
C12 C11 C16 123.2(8) . . ? 
C12 C11 N9 117.6(8) . . ? 
C16 C11 N9 119.2(8) . . ? 
C11 C12 C13 117.5(8) . . ? 
C11 C12 H12 121.3 . . ? 
C13 C12 H12 121.3 . . ? 
C14 C13 C12 120.8(8) . . ? 
C14 C13 N12 121.4(8) . . ? 
C12 C13 N12 117.8(8) . . ? 
C13 C14 C15 120.7(8) . . ? 
C13 C14 H14 119.6 . . ? 
C15 C14 H14 119.6 . . ? 
C16 C15 C14 119.2(9) . . ? 
C16 C15 H15 120.4 . . ? 
C14 C15 H15 120.4 . . ? 
C11 C16 C15 118.6(8) . . ? 
C11 C16 H16 120.7 . . ? 
C15 C16 H16 120.7 . . ? 
N8 C17 N9 110.7(8) . . ? 
N8 C17 H17 124.7 . . ? 
N9 C17 H17 124.7 . . ? 
N7 C18 N9 110.0(7) . . ? 
N7 C18 H18 125.0 . . ? 
N9 C18 H18 125.0 . . ? 
N11 C19 N12 111.7(9) . . ? 
N11 C19 H19 124.1 . . ? 
N12 C19 H19 124.1 . . ? 
N10 C20 N12 114.2(9) . . ? 
N10 C20 H20 122.9 . . ? 
N12 C20 H20 122.9 . . ? 
N2 Cd1 N1 95.2(2) . 4_576 ? 
N2 Cd1 N5 94.2(2) . 3_575 ? 
N1 Cd1 N5 92.7(2) 4_576 3_575 ? 
N2 Cd1 N8 88.2(2) . 4_575 ? 
N1 Cd1 N8 175.1(2) 4_576 4_575 ? 
N5 Cd1 N8 90.6(2) 3_575 4_575 ? 
N2 Cd1 N4 92.6(2) . 2_544 ? 
N1 Cd1 N4 91.1(2) 4_576 2_544 ? 
N5 Cd1 N4 171.9(2) 3_575 2_544 ? 
N8 Cd1 N4 85.2(2) 4_575 2_544 ? 
N2 Cd1 N7 176.9(2) . . ? 
N1 Cd1 N7 87.9(2) 4_576 . ? 
N5 Cd1 N7 85.7(2) 3_575 . ? 
N8 Cd1 N7 88.7(2) 4_575 . ? 
N4 Cd1 N7 87.3(2) 2_544 . ? 
C8 N1 N2 106.6(7) . . ? 
C8 N1 Cd1 122.8(6) . 4_575 ? 
N2 N1 Cd1 128.4(5) . 4_575 ? 
C7 N2 N1 106.2(6) . . ? 
C7 N2 Cd1 128.8(5) . . ? 
N1 N2 Cd1 124.6(5) . . ? 
C7 N3 C8 103.9(7) . . ? 
C7 N3 C1 129.2(7) . . ? 
C8 N3 C1 126.3(7) . . ? 
C10 N4 N5 106.1(6) . . ? 
C10 N4 Cd1 123.7(5) . 2_554 ? 
N5 N4 Cd1 127.3(5) . 2_554 ? 
C9 N5 N4 106.9(7) . . ? 
C9 N5 Cd1 128.4(6) . 3_575 ? 
N4 N5 Cd1 123.6(5) . 3_575 ? 
C9 N6 C10 104.3(7) . . ? 
C9 N6 C3 128.5(7) . . ? 
C10 N6 C3 127.2(7) . . ? 
C18 N7 N8 107.0(6) . . ? 
C18 N7 Cd1 127.8(5) . . ? 
N8 N7 Cd1 125.2(5) . . ? 
C17 N8 N7 106.8(7) . . ? 
C17 N8 Cd1 126.7(6) . 4_576 ? 
N7 N8 Cd1 126.3(5) . 4_576 ? 
C18 N9 C17 105.5(7) . . ? 
C18 N9 C11 128.3(7) . . ? 
C17 N9 C11 126.2(7) . . ? 
C20 N10 N11 104.5(8) . . ? 
C19 N11 N10 106.7(8) . . ? 
C20 N12 C19 102.8(8) . . ? 
C20 N12 C13 128.8(8) . . ? 
C19 N12 C13 128.2(8) . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    1.079 
_refine_diff_density_min   -0.699 
_refine_diff_density_rms    0.144 

#END

 
data_7 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C60 H48 Cd3 N36' 
_chemical_formula_weight          1610.58
 
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' 
 'Cd'  'Cd'  -0.8075   1.2024 
 '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            'trigonal'
_symmetry_space_group_name_H-M    'R -3 m'
_symmetry_space_group_name_Hall    '-R 3 2"'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 'y, x, -z' 
 '-x, -x+y, -z' 
 'x-y, -y, -z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 'y+2/3, x+1/3, -z+1/3' 
 '-x+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, -y+1/3, -z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 'y+1/3, x+2/3, -z+2/3' 
 '-x+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, -y+2/3, -z+2/3' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 '-y, -x, z' 
 'x, x-y, z' 
 '-x+y, y, z' 
 '-x+2/3, -y+1/3, -z+1/3' 
 'y+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, x+1/3, -z+1/3' 
 '-y+2/3, -x+1/3, z+1/3' 
 'x+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, y+1/3, z+1/3' 
 '-x+1/3, -y+2/3, -z+2/3' 
 'y+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, x+2/3, -z+2/3' 
 '-y+1/3, -x+2/3, z+2/3' 
 'x+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, y+2/3, z+2/3' 
 
_cell_length_a                    20.5262(16) 
_cell_length_b                    20.5262(16) 
_cell_length_c                    20.152(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      7353.0(15) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     2557
_cell_measurement_theta_min       2.32
_cell_measurement_theta_max       22.10
 
_exptl_crystal_description        BLOCK 
_exptl_crystal_colour             COLORLESS 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.22 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       NONE 
_exptl_crystal_density_diffrn     1.091
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2969 
_exptl_absorpt_coefficient_mu     0.721 
_exptl_absorpt_correction_type    MULTI-SCAN 
_exptl_absorpt_correction_T_min   0.8403 
_exptl_absorpt_correction_T_max   0.8692 
_exptl_absorpt_process_details    SADABS
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             9469 
_diffrn_reflns_av_R_equivalents   0.0615 
_diffrn_reflns_av_sigmaI/netI     0.0502 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          1.53 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              1739 
_reflns_number_gt                 1431 
_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, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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)+(0.0805P)²+1.0180P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1756 
_refine_ls_number_parameters      142 
_refine_ls_number_restraints      120 
_refine_ls_R_factor_all           0.0490 
_refine_ls_R_factor_gt            0.0428 
_refine_ls_wR_factor_ref          0.1285 
_refine_ls_wR_factor_gt           0.1254 
_refine_ls_goodness_of_fit_ref    1.082 
_refine_ls_restrained_S_all       1.135 
_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 
Cd1 Cd 0.0000 0.0000 0.0000 0.02136(13) Uani 1 12 d S . . 
Cd2 Cd 0.0000 0.0000 0.205423(16) 0.02007(11) Uani 1 6 d S . . 
C1 C 0.1677(5) 0.3015(3) 0.1111(2) 0.089(2) Uani 0.50 1 d PDU . . 
C2 C 0.1775(6) 0.3445(2) 0.0562(2) 0.0702(18) Uani 0.50 1 d PDU . . 
H2A H 0.1466 0.3234 0.0173 0.084 Uiso 0.50 1 d PR . . 
C3 C 0.2293(5) 0.4204(3) 0.0600(2) 0.095(2) Uani 0.50 1 d PDU . . 
C4 C 0.2722(6) 0.4540(4) 0.1167(3) 0.135(3) Uani 0.50 1 d PDU . . 
H4A H 0.3134 0.5051 0.1158 0.162 Uiso 0.50 1 d PR . . 
C5 C 0.2588(7) 0.4082(4) 0.1700(4) 0.155(3) Uani 0.50 1 d PDU . . 
H5A H 0.2815 0.4309 0.2118 0.186 Uiso 0.50 1 d PR . . 
C6 C 0.2031(6) 0.3319(4) 0.1678(3) 0.143(3) Uani 0.50 1 d PDU . . 
H6A H 0.2030 0.2994 0.2024 0.172 Uiso 0.50 1 d PR . . 
N3 N 0.1225(4) 0.22178(19) 0.10658(15) 0.0580(17) Uani 0.50 1 d PDU . . 
C7 C 0.1004(4) 0.1732(2) 0.15763(19) 0.046(2) Uani 0.50 1 d PDU . . 
H7A H 0.1112 0.1880 0.2035 0.055 Uiso 0.50 1 d PR . . 
N2 N 0.0621(4) 0.10472(19) 0.13619(14) 0.0408(15) Uani 0.50 1 d PDU . . 
N1 N 0.05375(8) 0.10749(17) 0.06792(12) 0.0352(8) Uani 1 2 d SDU . . 
C8 C 0.0972(6) 0.1769(2) 0.05158(18) 0.052(2) Uani 0.50 1 d PDU . . 
H8A H 0.1124 0.1940 0.0067 0.062 Uiso 0.50 1 d PR . . 
N6 N 0.2460(5) 0.4647(2) 0.0011(2) 0.084(2) Uani 0.50 1 d PDU . . 
C9 C 0.2489(5) 0.4377(4) -0.0628(3) 0.094(3) Uani 0.50 1 d PDU . . 
H9A H 0.2422 0.3889 -0.0729 0.113 Uiso 0.50 1 d PR . . 
N5 N 0.2708(3) 0.4921(3) -0.1067(2) 0.081(2) Uani 0.50 1 d PDU . . 
N4 N 0.27891(10) 0.5578(2) -0.06736(17) 0.0625(12) Uani 1 2 d SDU . . 
C10 C 0.26801(12) 0.5360(2) -0.00904(19) 0.0669(15) Uani 1 2 d SDU . . 
H10A H 0.2654 0.5672 0.0260 0.080 Uiso 0.50 1 d PR . . 
 
 
_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 2.350(3) . ? 
Cd1 N1 2.350(3) 19 ? 
Cd1 N1 2.350(3) 3 ? 
Cd1 N1 2.350(3) 2 ? 
Cd1 N1 2.350(3) 21 ? 
Cd1 N1 2.350(3) 20 ? 
Cd2 N4 2.288(3) 8 ? 
Cd2 N4 2.288(3) 7_445 ? 
Cd2 N4 2.288(3) 9_455 ? 
Cd2 N2 2.335(3) 22 ? 
Cd2 N2 2.335(3) 2 ? 
Cd2 N2 2.335(3) 3 ? 
Cd2 N2 2.335(3) . ? 
Cd2 N2 2.335(3) 23 ? 
Cd2 N2 2.335(3) 24 ? 
C1 C1 0.70(2) 24 ? 
C1 C6 1.329(8) . ? 
C1 C2 1.367(6) . ? 
C1 C2 1.421(8) 24 ? 
C1 N3 1.424(6) . ? 
C1 N3 1.536(7) 24 ? 
C1 C6 1.681(12) 24 ? 
C2 C2 0.22(2) 24 ? 
C2 C3 1.381(7) . ? 
C2 C1 1.421(8) 24 ? 
C2 C3 1.441(8) 24 ? 
C2 H2A 0.9638 . ? 
C3 C3 0.78(2) 24 ? 
C3 C4 1.397(10) . ? 
C3 N6 1.427(6) . ? 
C3 C2 1.441(8) 24 ? 
C3 N6 1.573(8) 24 ? 
C3 C4 1.844(13) 24 ? 
C4 C5 1.361(11) . ? 
C4 C3 1.844(13) 24 ? 
C4 C4 1.85(3) 24 ? 
C4 H4A 0.9643 . ? 
C5 C6 1.405(10) . ? 
C5 H5A 0.9637 . ? 
C6 C6 1.53(3) 24 ? 
C6 C1 1.681(12) 24 ? 
C6 H6A 0.9639 . ? 
N3 N3 0.475(17) 24 ? 
N3 C7 1.343(5) . ? 
N3 C8 1.367(5) . ? 
N3 C8 1.428(7) 24 ? 
N3 C7 1.440(6) 24 ? 
N3 C1 1.536(7) 24 ? 
C7 C7 0.565(15) 24 ? 
C7 N2 1.295(5) . ? 
C7 N2 1.380(6) 24 ? 
C7 N3 1.440(6) 24 ? 
C7 H7A 0.9635 . ? 
N2 N2 0.400(15) 24 ? 
N2 C7 1.380(6) 24 ? 
N2 N1 1.391(4) . ? 
N1 C8 1.290(5) 24 ? 
N1 C8 1.290(5) . ? 
N1 N2 1.391(4) 24 ? 
C8 C8 0.36(2) 24 ? 
C8 N3 1.428(7) 24 ? 
C8 H8A 0.9636 . ? 
N6 N6 0.559(19) 24 ? 
N6 C10 1.314(6) . ? 
N6 C9 1.415(9) . ? 
N6 C3 1.573(8) 24 ? 
N6 C9 1.641(10) 24 ? 
C9 C9 1.23(2) 24 ? 
C9 N5 1.315(8) . ? 
C9 N6 1.641(10) 24 ? 
C9 N5 1.727(10) 24 ? 
C9 H9A 0.9643 . ? 
N5 N5 1.017(14) 24 ? 
N5 N4 1.501(6) . ? 
N5 C9 1.727(10) 24 ? 
N4 C10 1.237(5) . ? 
N4 N5 1.501(6) 24 ? 
N4 Cd2 2.288(3) 13_554 ? 
C10 N6 1.314(6) 24 ? 
C10 H10A 0.9728 . ? 
 
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 N1 180.00(10) . 19 ? 
N1 Cd1 N1 89.50(9) . 3 ? 
N1 Cd1 N1 90.50(9) 19 3 ? 
N1 Cd1 N1 89.50(9) . 2 ? 
N1 Cd1 N1 90.50(9) 19 2 ? 
N1 Cd1 N1 89.50(9) 3 2 ? 
N1 Cd1 N1 90.50(9) . 21 ? 
N1 Cd1 N1 89.50(9) 19 21 ? 
N1 Cd1 N1 180.00(15) 3 21 ? 
N1 Cd1 N1 90.50(9) 2 21 ? 
N1 Cd1 N1 90.50(9) . 20 ? 
N1 Cd1 N1 89.50(9) 19 20 ? 
N1 Cd1 N1 90.50(9) 3 20 ? 
N1 Cd1 N1 180.00(15) 2 20 ? 
N1 Cd1 N1 89.50(9) 21 20 ? 
N4 Cd2 N4 94.20(12) 8 7_445 ? 
N4 Cd2 N4 94.19(12) 8 9_455 ? 
N4 Cd2 N4 94.19(12) 7_445 9_455 ? 
N4 Cd2 N2 173.26(16) 8 22 ? 
N4 Cd2 N2 85.34(16) 7_445 22 ? 
N4 Cd2 N2 92.54(16) 9_455 22 ? 
N4 Cd2 N2 173.26(17) 8 2 ? 
N4 Cd2 N2 92.54(16) 7_445 2 ? 
N4 Cd2 N2 85.34(16) 9_455 2 ? 
N2 Cd2 N2 9.8(4) 22 2 ? 
N4 Cd2 N2 92.54(16) 8 3 ? 
N4 Cd2 N2 85.35(16) 7_445 3 ? 
N4 Cd2 N2 173.26(16) 9_455 3 ? 
N2 Cd2 N2 80.7(3) 22 3 ? 
N2 Cd2 N2 87.96(11) 2 3 ? 
N4 Cd2 N2 85.34(16) 8 . ? 
N4 Cd2 N2 173.26(16) 7_445 . ? 
N4 Cd2 N2 92.54(16) 9_455 . ? 
N2 Cd2 N2 94.3(3) 22 . ? 
N2 Cd2 N2 87.96(11) 2 . ? 
N2 Cd2 N2 87.96(11) 3 . ? 
N4 Cd2 N2 85.35(16) 8 23 ? 
N4 Cd2 N2 92.54(16) 7_445 23 ? 
N4 Cd2 N2 173.26(16) 9_455 23 ? 
N2 Cd2 N2 87.96(11) 22 23 ? 
N2 Cd2 N2 94.3(3) 2 23 ? 
N2 Cd2 N2 9.8(4) 3 23 ? 
N2 Cd2 N2 80.7(3) . 23 ? 
N4 Cd2 N2 92.54(16) 8 24 ? 
N4 Cd2 N2 173.26(16) 7_445 24 ? 
N4 Cd2 N2 85.34(16) 9_455 24 ? 
N2 Cd2 N2 87.96(11) 22 24 ? 
N2 Cd2 N2 80.7(3) 2 24 ? 
N2 Cd2 N2 94.3(3) 3 24 ? 
N2 Cd2 N2 9.8(4) . 24 ? 
N2 Cd2 N2 87.96(11) 23 24 ? 
C1 C1 C6 108.2(7) 24 . ? 
C1 C1 C2 79.9(5) 24 . ? 
C6 C1 C2 121.5(5) . . ? 
C1 C1 C2 71.3(6) 24 24 ? 
C6 C1 C2 123.4(5) . 24 ? 
C2 C1 C2 8.6(9) . 24 ? 
C1 C1 N3 85.6(5) 24 . ? 
C6 C1 N3 118.9(5) . . ? 
C2 C1 N3 119.4(4) . . ? 
C2 C1 N3 117.4(5) 24 . ? 
C1 C1 N3 67.6(5) 24 24 ? 
C6 C1 N3 123.0(4) . 24 ? 
C2 C1 N3 113.6(5) . 24 ? 
C2 C1 N3 109.1(6) 24 24 ? 
N3 C1 N3 18.0(6) . 24 ? 
C1 C1 C6 48.7(5) 24 24 ? 
C6 C1 C6 59.5(9) . 24 ? 
C2 C1 C6 104.7(6) . 24 ? 
C2 C1 C6 98.3(7) 24 24 ? 
N3 C1 C6 108.2(6) . 24 ? 
N3 C1 C6 94.9(6) 24 24 ? 
C2 C2 C1 100.1(5) 24 . ? 
C2 C2 C3 101.8(6) 24 . ? 
C1 C2 C3 117.8(5) . . ? 
C2 C2 C1 71.3(6) 24 24 ? 
C1 C2 C1 28.8(8) . 24 ? 
C3 C2 C1 123.3(4) . 24 ? 
C2 C2 C3 69.7(6) 24 24 ? 
C1 C2 C3 122.8(4) . 24 ? 
C3 C2 C3 32.1(8) . 24 ? 
C1 C2 C3 110.6(7) 24 24 ? 
C2 C2 H2A 64.3 24 . ? 
C1 C2 H2A 121.1 . . ? 
C3 C2 H2A 120.9 . . ? 
C1 C2 H2A 106.5 24 . ? 
C3 C2 H2A 104.9 24 . ? 
C3 C3 C2 78.2(6) 24 . ? 
C3 C3 C4 112.6(6) 24 . ? 
C2 C3 C4 122.8(5) . . ? 
C3 C3 N6 85.5(5) 24 . ? 
C2 C3 N6 118.5(5) . . ? 
C4 C3 N6 118.3(5) . . ? 
C3 C3 C2 69.7(6) 24 24 ? 
C2 C3 C2 8.5(9) . 24 ? 
C4 C3 C2 125.2(5) . 24 ? 
N6 C3 C2 116.5(5) . 24 ? 
C3 C3 N6 64.8(5) 24 24 ? 
C2 C3 N6 111.1(5) . 24 ? 
C4 C3 N6 124.5(5) . 24 ? 
N6 C3 N6 20.8(7) . 24 ? 
C2 C3 N6 106.3(6) 24 24 ? 
C3 C3 C4 44.4(4) 24 24 ? 
C2 C3 C4 101.8(6) . 24 ? 
C4 C3 C4 68.2(9) . 24 ? 
N6 C3 C4 106.3(6) . 24 ? 
C2 C3 C4 95.1(7) 24 24 ? 
N6 C3 C4 90.0(6) 24 24 ? 
C5 C4 C3 116.5(7) . . ? 
C5 C4 C3 113.5(7) . 24 ? 
C3 C4 C3 23.0(6) . 24 ? 
C5 C4 C4 98.3(8) . 24 ? 
C3 C4 C4 67.4(6) . 24 ? 
C3 C4 C4 44.4(4) 24 24 ? 
C5 C4 H4A 122.0 . . ? 
C3 C4 H4A 121.0 . . ? 
C3 C4 H4A 122.2 24 . ? 
C4 C4 H4A 109.5 24 . ? 
C4 C5 C6 121.0(7) . . ? 
C4 C5 H5A 118.4 . . ? 
C6 C5 H5A 119.6 . . ? 
C1 C6 C5 120.0(6) . . ? 
C1 C6 C6 71.8(7) . 24 ? 
C5 C6 C6 104.8(8) . 24 ? 
C1 C6 C1 23.1(7) . 24 ? 
C5 C6 C1 120.1(7) . 24 ? 
C6 C6 C1 48.7(5) 24 24 ? 
C1 C6 H6A 119.1 . . ? 
C5 C6 H6A 117.9 . . ? 
C6 C6 H6A 110.1 24 . ? 
C1 C6 H6A 121.7 24 . ? 
N3 N3 C7 91.9(5) 24 . ? 
N3 N3 C8 87.6(6) 24 . ? 
C7 N3 C8 104.3(3) . . ? 
N3 N3 C1 94.4(5) 24 . ? 
C7 N3 C1 125.9(3) . . ? 
C8 N3 C1 129.5(3) . . ? 
N3 N3 C8 73.0(6) 24 24 ? 
C7 N3 C8 104.2(3) . 24 ? 
C8 N3 C8 14.6(10) . 24 ? 
C1 N3 C8 128.9(4) . 24 ? 
N3 N3 C7 68.8(4) 24 24 ? 
C7 N3 C7 23.1(6) . 24 ? 
C8 N3 C7 102.4(4) . 24 ? 
C1 N3 C7 125.3(4) . 24 ? 
C8 N3 C7 96.6(4) 24 24 ? 
N3 N3 C1 67.6(5) 24 24 ? 
C7 N3 C1 124.0(4) . 24 ? 
C8 N3 C1 124.8(5) . 24 ? 
C1 N3 C1 26.8(7) . 24 ? 
C8 N3 C1 116.8(6) 24 24 ? 
C7 N3 C1 111.9(5) 24 24 ? 
C7 C7 N2 86.3(5) 24 . ? 
C7 C7 N3 88.1(5) 24 . ? 
N2 C7 N3 110.3(3) . . ? 
C7 C7 N2 69.5(4) 24 24 ? 
N2 C7 N2 16.8(6) . 24 ? 
N3 C7 N2 108.4(4) . 24 ? 
C7 C7 N3 68.8(4) 24 24 ? 
N2 C7 N3 107.6(4) . 24 ? 
N3 C7 N3 19.3(7) . 24 ? 
N2 C7 N3 100.3(4) 24 24 ? 
C7 C7 H7A 94.2 24 . ? 
N2 C7 H7A 125.6 . . ? 
N3 C7 H7A 124.2 . . ? 
N2 C7 H7A 124.6 24 . ? 
N3 C7 H7A 123.2 24 . ? 
N2 N2 C7 93.7(4) 24 . ? 
N2 N2 C7 69.5(4) 24 24 ? 
C7 N2 C7 24.1(6) . 24 ? 
N2 N2 N1 81.7(3) 24 . ? 
C7 N2 N1 107.8(3) . . ? 
C7 N2 N1 103.2(4) 24 . ? 
N2 N2 Cd2 85.09(19) 24 . ? 
C7 N2 Cd2 123.8(2) . . ? 
C7 N2 Cd2 119.1(3) 24 . ? 
N1 N2 Cd2 127.4(2) . . ? 
C8 N1 C8 16.0(11) 24 . ? 
C8 N1 N2 105.4(3) 24 24 ? 
C8 N1 N2 107.8(3) . 24 ? 
C8 N1 N2 107.8(3) 24 . ? 
C8 N1 N2 105.4(3) . . ? 
N2 N1 N2 16.5(6) 24 . ? 
C8 N1 Cd1 129.0(2) 24 . ? 
C8 N1 Cd1 129.0(2) . . ? 
N2 N1 Cd1 123.2(2) 24 . ? 
N2 N1 Cd1 123.2(2) . . ? 
C8 C8 N1 82.0(5) 24 . ? 
C8 C8 N3 92.4(6) 24 . ? 
N1 C8 N3 110.9(3) . . ? 
C8 C8 N3 73.0(6) 24 24 ? 
N1 C8 N3 107.2(4) . 24 ? 
N3 C8 N3 19.4(7) . 24 ? 
C8 C8 H8A 98.1 24 . ? 
N1 C8 H8A 124.1 . . ? 
N3 C8 H8A 124.8 . . ? 
N3 C8 H8A 126.4 24 . ? 
N6 N6 C10 77.7(4) 24 . ? 
N6 N6 C9 103.8(5) 24 . ? 
C10 N6 C9 103.6(4) . . ? 
N6 N6 C3 94.5(5) 24 . ? 
C10 N6 C3 132.7(5) . . ? 
C9 N6 C3 123.4(5) . . ? 
N6 N6 C3 64.8(5) 24 24 ? 
C10 N6 C3 120.6(6) . 24 ? 
C9 N6 C3 128.1(4) . 24 ? 
C3 N6 C3 29.7(7) . 24 ? 
N6 N6 C9 56.9(4) 24 24 ? 
C10 N6 C9 92.5(5) . 24 ? 
C9 N6 C9 46.8(7) . 24 ? 
C3 N6 C9 122.2(5) . 24 ? 
C3 N6 C9 102.3(6) 24 24 ? 
C9 C9 N5 85.3(5) 24 . ? 
C9 C9 N6 76.2(5) 24 . ? 
N5 C9 N6 110.1(6) . . ? 
C9 C9 N6 56.9(4) 24 24 ? 
N5 C9 N6 105.6(6) . 24 ? 
N6 C9 N6 19.3(7) . 24 ? 
C9 C9 N5 49.4(3) 24 24 ? 
N5 C9 N5 35.9(5) . 24 ? 
N6 C9 N5 97.0(6) . 24 ? 
N6 C9 N5 83.3(5) 24 24 ? 
C9 C9 H9A 112.3 24 . ? 
N5 C9 H9A 123.4 . . ? 
N6 C9 H9A 126.1 . . ? 
N6 C9 H9A 129.6 24 . ? 
N5 C9 H9A 129.9 24 . ? 
N5 N5 C9 94.7(5) 24 . ? 
N5 N5 N4 70.2(3) 24 . ? 
C9 N5 N4 104.1(5) . . ? 
N5 N5 C9 49.4(3) 24 24 ? 
C9 N5 C9 45.3(7) . 24 ? 
N4 N5 C9 86.8(4) . 24 ? 
C10 N4 N5 105.0(3) . . ? 
C10 N4 N5 105.0(3) . 24 ? 
N5 N4 N5 39.6(5) . 24 ? 
C10 N4 Cd2 140.5(3) . 13_554 ? 
N5 N4 Cd2 112.1(2) . 13_554 ? 
N5 N4 Cd2 112.1(2) 24 13_554 ? 
N4 C10 N6 116.8(4) . 24 ? 
N4 C10 N6 116.8(4) . . ? 
N6 C10 N6 24.6(8) 24 . ? 
N4 C10 H10A 120.7 . . ? 
N6 C10 H10A 110.8 24 . ? 
N6 C10 H10A 121.3 . . ? 

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.005     0.297    -0.008    2343.7       1.0
         2     0.333     0.667     0.167      44.6      32.8
         3     0.000     0.000     0.500      44.2      32.7
         4     0.667     0.333     0.833      44.6      32.7
_platon_squeeze_details
; ?
;
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.697 
_refine_diff_density_min   -0.586 
_refine_diff_density_rms    0.093 

# END
  
  
