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

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

data_q12-2
_database_code_depnum_ccdc_archive 'CCDC 987758'
_audit_update_record             
;
2015-01-24 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H17 Co N9 O4'
_chemical_formula_weight         590.43

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'
Co Co 0.3494 0.9721 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pcma

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

_cell_length_a                   19.4254(7)
_cell_length_b                   21.878(2)
_cell_length_c                   15.5780(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6620.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5598
_cell_measurement_theta_min      3.4180
_cell_measurement_theta_max      24.9680

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1204
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0892
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6003
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.02
_reflns_number_total             6003
_reflns_number_gt                4012
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Siemens, 1996)'
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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.
The structure was twinned. The solvent molecule in the structure was highly 
disordered and was impossible to refine using conventional discrete-atom models, 
thus the contribution of partial solvent electron densities were removed by 
the SQUEEZE routine in PLATON. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6003
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0996
_refine_ls_wR_factor_ref         0.3010
_refine_ls_wR_factor_gt          0.2818
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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
Co1 Co 0.43996(3) 0.5000 0.59942(4) 0.0434(3) Uani 1 2 d S . .
O3 O 0.03646(19) 0.5000 0.8472(4) 0.0946(18) Uani 1 2 d S . .
N1 N 0.44043(12) 0.59959(17) 0.59947(17) 0.0459(8) Uani 1 1 d . . .
C5 C 0.0878(3) 0.5000 0.8982(4) 0.0552(14) Uani 1 2 d S . .
C11 C 0.4437(2) 0.7266(3) 0.5960(3) 0.0739(14) Uani 1 1 d . . .
O4 O 0.0844(3) 0.5000 0.9791(3) 0.0978(18) Uani 1 2 d S . .
O2 O 0.3969(3) 0.5000 0.7410(5) 0.114(2) Uani 1 2 d S . .
C14 C 0.4465(4) 0.7942(3) 0.5991(4) 0.095(2) Uani 1 1 d . . .
C8 C 0.2793(2) 0.5000 0.8559(5) 0.071(2) Uani 1 2 d S . .
H8 H 0.3209 0.5000 0.8855 0.085 Uiso 1 2 calc SR . .
C2 C 0.2800(3) 0.5000 0.7659(4) 0.0569(14) Uani 1 2 d S . .
C3 C 0.2189(3) 0.5000 0.7282(4) 0.082(2) Uani 1 2 d S . .
H3 H 0.2181 0.5000 0.6685 0.098 Uiso 1 2 calc SR . .
C13 C 0.3949(3) 0.6299(3) 0.5548(3) 0.0835(15) Uani 1 1 d . . .
H13 H 0.3610 0.6084 0.5254 0.100 Uiso 1 1 calc R . .
C7 C 0.2165(3) 0.5000 0.9035(4) 0.0612(15) Uani 1 2 d S . .
H7 H 0.2167 0.5000 0.9632 0.073 Uiso 1 2 calc SR . .
N4 N 0.3999(3) 0.82994(19) 0.5625(4) 0.0980(14) Uani 1 1 d . . .
H4 H 0.3617 0.8187 0.5395 0.118 Uiso 1 1 calc R . .
C6 C 0.1549(2) 0.5000 0.8575(3) 0.0436(11) Uani 1 2 d S . .
N2 N 0.4963(2) 0.82601(19) 0.6320(3) 0.0941(14) Uani 1 1 d . . .
C9 C 0.4873(2) 0.6313(2) 0.6419(4) 0.0801(14) Uani 1 1 d . . .
H9 H 0.5211 0.6100 0.6720 0.096 Uiso 1 1 calc R . .
C12 C 0.3955(3) 0.6949(2) 0.5496(4) 0.0902(16) Uani 1 1 d . . .
H12 H 0.3638 0.7154 0.5154 0.108 Uiso 1 1 calc R . .
C10 C 0.4887(3) 0.6923(2) 0.6438(4) 0.0949(17) Uani 1 1 d . . .
H10 H 0.5209 0.7120 0.6783 0.114 Uiso 1 1 calc R . .
C4 C 0.1588(3) 0.5000 0.7686(5) 0.100(3) Uani 1 2 d S . .
H4A H 0.1184 0.5000 0.7366 0.120 Uiso 1 2 calc SR . .
N3 N 0.4851(3) 0.8853(2) 0.6270(4) 0.127(2) Uani 1 1 d . . .
C16 C 0.4224(6) 1.0000 0.5756(7) 0.120(3) Uani 1 2 d S . .
H16 H 0.4656 1.0000 0.6014 0.143 Uiso 1 2 calc SR . .
C15 C 0.4245(5) 0.8883(3) 0.5687(4) 0.122(3) Uani 1 1 d . . .
C25 C 0.3958(5) 0.9468(2) 0.5597(5) 0.111(2) Uani 1 1 d . . .
N5 N 0.2999(7) 1.0000 0.4948(7) 0.211(7) Uani 1 2 d S . .
C17 C 0.3289(6) 0.9478(3) 0.5233(6) 0.162(4) Uani 1 1 d . . .
H17 H 0.3044 0.9114 0.5189 0.195 Uiso 1 1 calc R . .
O1 O 0.3311(3) 0.5000 0.6236(4) 0.1026(17) Uani 1 2 d S . .
C1 C 0.3462(5) 0.5000 0.7134(7) 0.092(2) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O4 1.933(5) 2_564 ?
Co1 O3 2.051(4) 6_657 ?
Co1 O1 2.148(6) . ?
Co1 N1 2.179(4) . ?
Co1 N1 2.179(4) 8_565 ?
Co1 O2 2.360(7) . ?
O3 C5 1.275(8) . ?
O3 Co1 2.051(4) 6_557 ?
N1 C13 1.306(5) . ?
N1 C9 1.322(5) . ?
C5 O4 1.263(7) . ?
C5 C6 1.448(8) . ?
C11 C12 1.371(7) . ?
C11 C10 1.372(7) . ?
C11 C14 1.481(8) . ?
O4 Co1 1.933(5) 2_565 ?
O2 C1 1.074(10) . ?
C14 N2 1.298(7) . ?
C14 N4 1.324(7) . ?
C8 C2 1.403(9) . ?
C8 C7 1.428(9) . ?
C8 H8 0.9300 . ?
C2 C3 1.324(9) . ?
C2 C1 1.522(10) . ?
C3 C4 1.327(9) . ?
C3 H3 0.9300 . ?
C13 C12 1.424(7) . ?
C13 H13 0.9300 . ?
C7 C6 1.396(7) . ?
C7 H7 0.9300 . ?
N4 C15 1.367(7) . ?
N4 H4 0.8600 . ?
C6 C4 1.386(9) . ?
N2 N3 1.318(6) . ?
C9 C10 1.336(7) . ?
C9 H9 0.9300 . ?
C12 H12 0.9300 . ?
C10 H10 0.9300 . ?
C4 H4A 0.9300 . ?
N3 C15 1.487(9) . ?
C16 C25 1.298(7) . ?
C16 C25 1.298(7) 8_575 ?
C16 H16 0.9300 . ?
C15 C25 1.402(8) . ?
C25 C17 1.418(11) . ?
N5 C17 1.349(9) . ?
N5 C17 1.349(9) 8_575 ?
C17 H17 0.9300 . ?
O1 C1 1.430(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
O4 Co1 O3 128.1(3) 2_564 6_657 ?
O4 Co1 O1 85.9(3) 2_564 . ?
O3 Co1 O1 146.0(3) 6_657 . ?
O4 Co1 N1 90.08(7) 2_564 . ?
O3 Co1 N1 89.77(6) 6_657 . ?
O1 Co1 N1 90.23(6) . . ?
O4 Co1 N1 90.08(7) 2_564 8_565 ?
O3 Co1 N1 89.77(6) 6_657 8_565 ?
O1 Co1 N1 90.23(6) . 8_565 ?
N1 Co1 N1 179.52(13) . 8_565 ?
O4 Co1 O2 145.1(3) 2_564 . ?
O3 Co1 O2 86.9(2) 6_657 . ?
O1 Co1 O2 59.1(2) . . ?
N1 Co1 O2 90.07(7) . . ?
N1 Co1 O2 90.07(7) 8_565 . ?
C5 O3 Co1 117.6(5) . 6_557 ?
C13 N1 C9 117.8(4) . . ?
C13 N1 Co1 120.3(3) . . ?
C9 N1 Co1 121.8(3) . . ?
O4 C5 O3 125.5(6) . . ?
O4 C5 C6 119.0(6) . . ?
O3 C5 C6 115.5(5) . . ?
C12 C11 C10 116.4(5) . . ?
C12 C11 C14 123.2(5) . . ?
C10 C11 C14 120.3(4) . . ?
C5 O4 Co1 168.9(6) . 2_565 ?
C1 O2 Co1 87.2(7) . . ?
N2 C14 N4 111.3(5) . . ?
N2 C14 C11 125.1(5) . . ?
N4 C14 C11 123.4(6) . . ?
C2 C8 C7 121.8(5) . . ?
C2 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C3 C2 C8 115.7(4) . . ?
C3 C2 C1 121.3(7) . . ?
C8 C2 C1 123.0(6) . . ?
C2 C3 C4 125.4(6) . . ?
C2 C3 H3 117.3 . . ?
C4 C3 H3 117.3 . . ?
N1 C13 C12 122.1(4) . . ?
N1 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C6 C7 C8 117.8(5) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
C14 N4 C15 106.4(5) . . ?
C14 N4 H4 126.8 . . ?
C15 N4 H4 126.8 . . ?
C4 C6 C7 117.7(5) . . ?
C4 C6 C5 119.1(5) . . ?
C7 C6 C5 123.1(5) . . ?
C14 N2 N3 112.4(5) . . ?
N1 C9 C10 123.3(4) . . ?
N1 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
C11 C12 C13 118.7(5) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C9 C10 C11 121.4(4) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C3 C4 C6 121.5(6) . . ?
C3 C4 H4A 119.2 . . ?
C6 C4 H4A 119.2 . . ?
N2 N3 C15 102.2(4) . . ?
C25 C16 C25 127.6(12) . 8_575 ?
C25 C16 H16 116.2 . . ?
C25 C16 H16 116.2 8_575 . ?
N4 C15 C25 134.9(8) . . ?
N4 C15 N3 106.2(5) . . ?
C25 C15 N3 114.6(6) . . ?
C16 C25 C15 129.8(9) . . ?
C16 C25 C17 115.3(7) . . ?
C15 C25 C17 114.7(6) . . ?
C17 N5 C17 115.8(10) . 8_575 ?
N5 C17 C25 121.8(7) . . ?
N5 C17 H17 119.1 . . ?
C25 C17 H17 119.1 . . ?
C1 O1 Co1 88.3(5) . . ?
O2 C1 O1 125.4(9) . . ?
O2 C1 C2 124.0(10) . . ?
O1 C1 C2 110.6(7) . . ?

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
_platon_squeeze_void_content
1 0.288 0.155 -0.035 4646 1023 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.089
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_13410d
_database_code_depnum_ccdc_archive 'CCDC 987759'
_audit_update_record             
;
2014-02-19 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H42 Cd N12 O7'
_chemical_formula_weight         939.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.1597(5)
_cell_length_b                   22.0750(9)
_cell_length_c                   17.4340(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.424(4)
_cell_angle_gamma                90.00
_cell_volume                     4236.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5974
_cell_measurement_theta_min      3.2150
_cell_measurement_theta_max      28.5390

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15268
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7399
_reflns_number_gt                5925
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Siemens, 1996)'
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0355P)²+21.1107P] 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         7399
_refine_ls_number_parameters     565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1463
_refine_ls_wR_factor_gt          0.1369
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_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 0.36763(3) 0.442613(19) 0.47128(2) 0.02460(13) Uani 1 1 d . . .
O1 O 0.3460(4) 0.5435(2) 0.4602(2) 0.0465(12) Uani 1 1 d . . .
O3 O -0.1770(3) 0.92834(17) 0.1201(2) 0.0287(9) Uani 1 1 d . . .
O2 O 0.4970(4) 0.6039(2) 0.4446(3) 0.0481(12) Uani 1 1 d . . .
O4 O -0.2786(4) 0.84997(18) 0.0637(2) 0.0356(10) Uani 1 1 d . . .
N8 N 0.9322(4) 0.5025(2) -0.2589(3) 0.0264(10) Uani 1 1 d . . .
N6 N 1.0561(4) 0.4418(2) -0.1846(2) 0.0257(10) Uani 1 1 d . . .
H6 H 1.1159 0.4185 -0.1665 0.031 Uiso 1 1 calc R . .
N1 N 0.4636(4) 0.4469(2) 0.3633(3) 0.0293(11) Uani 1 1 d . . .
N2 N 0.7251(4) 0.4356(2) 0.1466(3) 0.0287(11) Uani 1 1 d . . .
H2 H 0.7631 0.4068 0.1736 0.034 Uiso 1 1 calc R . .
N3 N 0.5898(4) 0.5100(2) 0.1085(3) 0.0340(12) Uani 1 1 d . . .
N9 N 1.2562(4) 0.4535(2) -0.4279(2) 0.0279(11) Uani 1 1 d . . .
N7 N 0.8823(4) 0.4954(2) -0.1933(3) 0.0285(11) Uani 1 1 d . . .
N4 N 0.6666(4) 0.5033(2) 0.0560(3) 0.0335(12) Uani 1 1 d . . .
O5 O 0.6422(5) 0.5915(2) 0.9486(3) 0.0593(14) Uani 1 1 d . . .
C3 C 0.5711(5) 0.4600(3) 0.2313(3) 0.0279(13) Uani 1 1 d . . .
C5 C 0.4125(5) 0.4813(3) 0.3031(3) 0.0296(13) Uani 1 1 d . . .
H5 H 0.3398 0.5009 0.3065 0.036 Uiso 1 1 calc R . .
N5 N 1.0327(5) 0.3858(2) 0.0450(3) 0.0385(13) Uani 1 1 d . . .
C6 C 0.6281(5) 0.4682(3) 0.1617(3) 0.0287(13) Uani 1 1 d . . .
C15 C 1.1114(5) 0.4649(3) -0.3132(3) 0.0268(12) Uani 1 1 d . . .
C16 C 1.2090(5) 0.4250(3) -0.3039(3) 0.0301(13) Uani 1 1 d . . .
H16 H 1.2272 0.4017 -0.2591 0.036 Uiso 1 1 calc R . .
C14 C 1.0356(5) 0.4698(3) -0.2522(3) 0.0256(12) Uani 1 1 d . . .
C4 C 0.4627(5) 0.4889(3) 0.2371(3) 0.0314(13) Uani 1 1 d . . .
H4 H 0.4245 0.5131 0.1967 0.038 Uiso 1 1 calc R . .
C11 C 0.9471(5) 0.4392(3) -0.0717(3) 0.0273(12) Uani 1 1 d . . .
C19 C 1.0882(5) 0.4984(3) -0.3815(3) 0.0311(13) Uani 1 1 d . . .
H19 H 1.0229 0.5251 -0.3901 0.037 Uiso 1 1 calc R . .
C13 C 0.9605(5) 0.4583(2) -0.1505(3) 0.0256(12) Uani 1 1 d . . .
C1 C 0.5676(5) 0.4190(3) 0.3578(3) 0.0315(13) Uani 1 1 d . . .
H1 H 0.6042 0.3952 0.3991 0.038 Uiso 1 1 calc R . .
C2 C 0.6234(5) 0.4241(3) 0.2926(3) 0.0318(14) Uani 1 1 d . . .
H2A H 0.6954 0.4036 0.2902 0.038 Uiso 1 1 calc R . .
C18 C 1.1632(5) 0.4917(3) -0.4362(3) 0.0312(13) Uani 1 1 d . . .
H18 H 1.1479 0.5150 -0.4812 0.037 Uiso 1 1 calc R . .
C8 C 0.8440(5) 0.4394(3) 0.0385(3) 0.0276(12) Uani 1 1 d . . .
C10 C 1.0357(5) 0.4037(3) -0.0282(3) 0.0322(14) Uani 1 1 d . . .
H10 H 1.1013 0.3916 -0.0512 0.039 Uiso 1 1 calc R . .
C12 C 0.8488(5) 0.4573(2) -0.0370(3) 0.0272(13) Uani 1 1 d . . .
H12 H 0.7873 0.4811 -0.0642 0.033 Uiso 1 1 calc R . .
C30 C -0.0997(5) 0.8295(3) 0.1525(3) 0.0307(13) Uani 1 1 d . . .
C7 C 0.7464(5) 0.4589(3) 0.0806(3) 0.0265(13) Uani 1 1 d . . .
C17 C 1.2785(5) 0.4206(3) -0.3626(3) 0.0293(13) Uani 1 1 d . . .
H17 H 1.3435 0.3937 -0.3563 0.035 Uiso 1 1 calc R . .
C20 C 0.3879(5) 0.5862(3) 0.4327(3) 0.0309(14) Uani 1 1 d . . .
C9 C 0.9375(5) 0.4040(3) 0.0767(3) 0.0343(14) Uani 1 1 d . . .
H9 H 0.9340 0.3922 0.1275 0.041 Uiso 1 1 calc R . .
C42 C -0.0781(10) 0.7258(5) 0.4430(7) 0.099(4) Uani 1 1 d . . .
H42A H -0.1120 0.7568 0.4717 0.149 Uiso 1 1 calc R . .
H42B H -0.1320 0.6916 0.4360 0.149 Uiso 1 1 calc R . .
H42C H -0.0677 0.7414 0.3931 0.149 Uiso 1 1 calc R . .
N10 N 0.6634(6) 0.6557(3) 0.8516(4) 0.067(2) Uani 1 1 d . . .
C24 C 0.1488(6) 0.7040(3) 0.2792(4) 0.0393(15) Uani 1 1 d . . .
C33 C -0.1891(5) 0.8715(3) 0.1098(3) 0.0305(13) Uani 1 1 d . . .
N12 N 0.0391(9) 0.7071(3) 0.4856(5) 0.083(3) Uani 1 1 d . . .
C28 C 0.0888(6) 0.8085(3) 0.2370(4) 0.0367(15) Uani 1 1 d . . .
H28 H 0.1597 0.8228 0.2671 0.044 Uiso 1 1 calc R . .
C27 C 0.0643(6) 0.7465(3) 0.2332(3) 0.0370(15) Uani 1 1 d . . .
C22 C 0.3503(6) 0.6743(3) 0.3367(4) 0.0464(17) Uani 1 1 d . . .
H22 H 0.4338 0.6806 0.3428 0.056 Uiso 1 1 calc R . .
O6 O 0.6159(7) 0.8083(3) 0.7322(4) 0.095(2) Uani 1 1 d . . .
N11 N 0.4899(7) 0.8114(3) 0.6156(4) 0.072(2) Uani 1 1 d . . .
C29 C 0.0062(6) 0.8489(3) 0.1956(4) 0.0390(15) Uani 1 1 d . . .
H29 H 0.0240 0.8901 0.1974 0.047 Uiso 1 1 calc R . .
C32 C -0.0429(6) 0.7258(3) 0.1878(4) 0.0422(16) Uani 1 1 d . . .
H32 H -0.0599 0.6845 0.1844 0.051 Uiso 1 1 calc R . .
C23 C 0.2732(6) 0.7122(3) 0.2884(4) 0.0480(18) Uani 1 1 d . . .
H23 H 0.3052 0.7434 0.2620 0.058 Uiso 1 1 calc R . .
C21 C 0.3051(6) 0.6270(3) 0.3764(3) 0.0348(14) Uani 1 1 d . . .
C25 C 0.1036(6) 0.6556(3) 0.3163(4) 0.0444(16) Uani 1 1 d . . .
H25 H 0.0204 0.6484 0.3085 0.053 Uiso 1 1 calc R . .
C26 C 0.1818(6) 0.6174(3) 0.3652(4) 0.0400(15) Uani 1 1 d . . .
H26 H 0.1503 0.5853 0.3903 0.048 Uiso 1 1 calc R . .
C34 C 0.6884(6) 0.6057(3) 0.8925(4) 0.0486(18) Uani 1 1 d . . .
H34 H 0.7454 0.5794 0.8775 0.058 Uiso 1 1 calc R . .
C31 C -0.1235(6) 0.7668(3) 0.1480(4) 0.0419(16) Uani 1 1 d . . .
H31 H -0.1946 0.7529 0.1178 0.050 Uiso 1 1 calc R . .
C36 C 0.7251(8) 0.6678(4) 0.7876(5) 0.071(2) Uani 1 1 d . . .
H36A H 0.7911 0.6398 0.7885 0.107 Uiso 1 1 calc R . .
H36B H 0.7560 0.7085 0.7915 0.107 Uiso 1 1 calc R . .
H36C H 0.6694 0.6633 0.7398 0.107 Uiso 1 1 calc R . .
C35 C 0.5763(13) 0.6992(5) 0.8687(8) 0.150(7) Uani 1 1 d . . .
H35A H 0.5709 0.6975 0.9230 0.224 Uiso 1 1 calc R . .
H35B H 0.4984 0.6902 0.8386 0.224 Uiso 1 1 calc R . .
H35C H 0.6012 0.7390 0.8558 0.224 Uiso 1 1 calc R . .
C37 C 0.5545(9) 0.8359(4) 0.6783(6) 0.084(3) Uani 1 1 d . . .
H37 H 0.5534 0.8780 0.6820 0.100 Uiso 1 1 calc R . .
C41 C 0.1325(11) 0.7511(5) 0.4954(8) 0.118(4) Uani 1 1 d . . .
H41A H 0.1548 0.7604 0.4459 0.177 Uiso 1 1 calc R . .
H41B H 0.2018 0.7356 0.5296 0.177 Uiso 1 1 calc R . .
H41C H 0.1041 0.7872 0.5174 0.177 Uiso 1 1 calc R . .
C38 C 0.4132(9) 0.8497(5) 0.5570(6) 0.094(3) Uani 1 1 d . . .
H38A H 0.3292 0.8438 0.5609 0.141 Uiso 1 1 calc R . .
H38B H 0.4266 0.8386 0.5058 0.141 Uiso 1 1 calc R . .
H38C H 0.4342 0.8915 0.5663 0.141 Uiso 1 1 calc R . .
O7 O 0.1607(17) 0.6371(6) 0.5512(7) 0.229(8) Uani 1 1 d . . .
C40 C 0.0483(17) 0.6466(9) 0.5096(9) 0.161(8) Uani 1 1 d . . .
H40 H -0.0125 0.6176 0.4989 0.193 Uiso 1 1 calc R . .
C39 C 0.4782(11) 0.7461(4) 0.6064(7) 0.117(5) Uani 1 1 d . . .
H39A H 0.5069 0.7340 0.5597 0.176 Uiso 1 1 calc R . .
H39B H 0.3944 0.7348 0.6031 0.176 Uiso 1 1 calc R . .
H39C H 0.5255 0.7264 0.6503 0.176 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 O2 2.182(4) 3_666 ?
Cd1 O1 2.246(5) . ?
Cd1 N1 2.315(4) . ?
Cd1 O4 2.311(4) 2_545 ?
Cd1 N9 2.326(4) 1_456 ?
Cd1 O3 2.460(4) 2_545 ?
Cd1 C33 2.741(6) 2_545 ?
O1 C20 1.187(7) . ?
O3 C33 1.272(7) . ?
O3 Cd1 2.460(4) 2 ?
O2 C20 1.262(7) . ?
O2 Cd1 2.182(4) 3_666 ?
O4 C33 1.268(7) . ?
O4 Cd1 2.311(4) 2 ?
N8 C14 1.350(7) . ?
N8 N7 1.361(6) . ?
N6 C14 1.317(7) . ?
N6 C13 1.353(7) . ?
N6 H6 0.8600 . ?
N1 C1 1.332(7) . ?
N1 C5 1.345(7) . ?
N2 C7 1.318(7) . ?
N2 C6 1.361(7) . ?
N2 H2 0.8600 . ?
N3 C6 1.328(7) . ?
N3 N4 1.361(6) . ?
N9 C18 1.327(7) . ?
N9 C17 1.338(7) . ?
N9 Cd1 2.326(4) 1_654 ?
N7 C13 1.332(7) . ?
N4 C7 1.347(7) . ?
O5 C34 1.218(8) . ?
C3 C2 1.379(8) . ?
C3 C4 1.387(8) . ?
C3 C6 1.472(7) . ?
C5 C4 1.370(7) . ?
C5 H5 0.9300 . ?
N5 C9 1.337(7) . ?
N5 C10 1.342(7) . ?
C15 C19 1.389(8) . ?
C15 C16 1.390(8) . ?
C15 C14 1.468(7) . ?
C16 C17 1.385(7) . ?
C16 H16 0.9300 . ?
C4 H4 0.9300 . ?
C11 C10 1.386(8) . ?
C11 C12 1.396(7) . ?
C11 C13 1.467(7) . ?
C19 C18 1.376(8) . ?
C19 H19 0.9300 . ?
C1 C2 1.386(8) . ?
C1 H1 0.9300 . ?
C2 H2A 0.9300 . ?
C18 H18 0.9300 . ?
C8 C12 1.384(7) . ?
C8 C9 1.384(8) . ?
C8 C7 1.473(7) . ?
C10 H10 0.9300 . ?
C12 H12 0.9300 . ?
C30 C29 1.362(9) . ?
C30 C31 1.409(9) . ?
C30 C33 1.472(8) . ?
C17 H17 0.9300 . ?
C20 C21 1.527(9) . ?
C9 H9 0.9300 . ?
C42 N12 1.455(13) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
N10 C34 1.319(9) . ?
N10 C35 1.431(11) . ?
N10 C36 1.429(9) . ?
C24 C23 1.384(9) . ?
C24 C25 1.386(9) . ?
C24 C27 1.470(9) . ?
C33 Cd1 2.741(6) 2 ?
N12 C40 1.397(18) . ?
N12 C41 1.415(13) . ?
C28 C29 1.396(8) . ?
C28 C27 1.395(9) . ?
C28 H28 0.9300 . ?
C27 C32 1.399(9) . ?
C22 C23 1.382(9) . ?
C22 C21 1.392(9) . ?
C22 H22 0.9300 . ?
O6 C37 1.229(10) . ?
N11 C37 1.323(11) . ?
N11 C39 1.454(11) . ?
N11 C38 1.485(11) . ?
C29 H29 0.9300 . ?
C32 C31 1.381(9) . ?
C32 H32 0.9300 . ?
C23 H23 0.9300 . ?
C21 C26 1.375(8) . ?
C25 C26 1.399(9) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C34 H34 0.9300 . ?
C31 H31 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C37 H37 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
O7 C40 1.36(2) . ?
C40 H40 0.9300 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 O1 125.26(18) 3_666 . ?
O2 Cd1 N1 101.76(17) 3_666 . ?
O1 Cd1 N1 86.96(17) . . ?
O2 Cd1 O4 88.95(17) 3_666 2_545 ?
O1 Cd1 O4 145.03(16) . 2_545 ?
N1 Cd1 O4 93.29(16) . 2_545 ?
O2 Cd1 N9 86.43(16) 3_666 1_456 ?
O1 Cd1 N9 84.25(17) . 1_456 ?
N1 Cd1 N9 170.44(17) . 1_456 ?
O4 Cd1 N9 91.77(15) 2_545 1_456 ?
O2 Cd1 O3 143.62(16) 3_666 2_545 ?
O1 Cd1 O3 90.11(15) . 2_545 ?
N1 Cd1 O3 86.85(14) . 2_545 ?
O4 Cd1 O3 55.05(13) 2_545 2_545 ?
N9 Cd1 O3 89.41(14) 1_456 2_545 ?
O2 Cd1 C33 116.25(19) 3_666 2_545 ?
O1 Cd1 C33 117.71(18) . 2_545 ?
N1 Cd1 C33 89.89(16) . 2_545 ?
O4 Cd1 C33 27.42(16) 2_545 2_545 ?
N9 Cd1 C33 90.87(16) 1_456 2_545 ?
O3 Cd1 C33 27.63(15) 2_545 2_545 ?
C20 O1 Cd1 141.1(4) . . ?
C33 O3 Cd1 88.6(3) . 2 ?
C20 O2 Cd1 120.6(4) . 3_666 ?
C33 O4 Cd1 95.5(3) . 2 ?
C14 N8 N7 109.1(4) . . ?
C14 N6 C13 103.5(5) . . ?
C14 N6 H6 128.3 . . ?
C13 N6 H6 128.3 . . ?
C1 N1 C5 117.9(5) . . ?
C1 N1 Cd1 124.4(4) . . ?
C5 N1 Cd1 117.6(3) . . ?
C7 N2 C6 103.0(5) . . ?
C7 N2 H2 128.5 . . ?
C6 N2 H2 128.5 . . ?
C6 N3 N4 103.2(5) . . ?
C18 N9 C17 118.1(5) . . ?
C18 N9 Cd1 119.3(4) . 1_654 ?
C17 N9 Cd1 122.6(4) . 1_654 ?
C13 N7 N8 102.8(4) . . ?
C7 N4 N3 108.7(5) . . ?
C2 C3 C4 118.1(5) . . ?
C2 C3 C6 121.7(5) . . ?
C4 C3 C6 120.2(5) . . ?
N1 C5 C4 123.0(5) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C9 N5 C10 116.7(5) . . ?
N3 C6 N2 114.1(5) . . ?
N3 C6 C3 121.9(5) . . ?
N2 C6 C3 123.9(5) . . ?
C19 C15 C16 118.0(5) . . ?
C19 C15 C14 122.3(5) . . ?
C16 C15 C14 119.7(5) . . ?
C17 C16 C15 118.8(5) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
N6 C14 N8 110.4(4) . . ?
N6 C14 C15 125.4(5) . . ?
N8 C14 C15 124.2(5) . . ?
C5 C4 C3 119.1(5) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C10 C11 C12 117.7(5) . . ?
C10 C11 C13 120.1(5) . . ?
C12 C11 C13 122.2(5) . . ?
C18 C19 C15 119.2(5) . . ?
C18 C19 H19 120.4 . . ?
C15 C19 H19 120.4 . . ?
N7 C13 N6 114.3(5) . . ?
N7 C13 C11 122.9(5) . . ?
N6 C13 C11 122.8(5) . . ?
N1 C1 C2 122.3(5) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 119.5(5) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
N9 C18 C19 123.1(5) . . ?
N9 C18 H18 118.4 . . ?
C19 C18 H18 118.4 . . ?
C12 C8 C9 118.3(5) . . ?
C12 C8 C7 122.5(5) . . ?
C9 C8 C7 119.1(5) . . ?
N5 C10 C11 124.1(5) . . ?
N5 C10 H10 118.0 . . ?
C11 C10 H10 118.0 . . ?
C8 C12 C11 119.1(5) . . ?
C8 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C29 C30 C31 118.7(6) . . ?
C29 C30 C33 122.4(6) . . ?
C31 C30 C33 119.0(6) . . ?
N2 C7 N4 111.0(5) . . ?
N2 C7 C8 125.1(5) . . ?
N4 C7 C8 123.9(5) . . ?
N9 C17 C16 122.8(5) . . ?
N9 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
O1 C20 O2 127.7(6) . . ?
O1 C20 C21 119.4(5) . . ?
O2 C20 C21 112.9(6) . . ?
N5 C9 C8 124.0(5) . . ?
N5 C9 H9 118.0 . . ?
C8 C9 H9 118.0 . . ?
N12 C42 H42A 109.5 . . ?
N12 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N12 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C34 N10 C35 122.7(7) . . ?
C34 N10 C36 119.5(7) . . ?
C35 N10 C36 117.8(7) . . ?
C23 C24 C25 118.8(6) . . ?
C23 C24 C27 121.5(6) . . ?
C25 C24 C27 119.7(6) . . ?
O4 C33 O3 120.9(5) . . ?
O4 C33 C30 118.9(5) . . ?
O3 C33 C30 120.2(5) . . ?
O4 C33 Cd1 57.1(3) . 2 ?
O3 C33 Cd1 63.8(3) . 2 ?
C30 C33 Cd1 175.7(5) . 2 ?
C40 N12 C41 127.1(13) . . ?
C40 N12 C42 116.2(12) . . ?
C41 N12 C42 116.7(8) . . ?
C29 C28 C27 119.7(6) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C27 C32 119.3(6) . . ?
C28 C27 C24 119.8(6) . . ?
C32 C27 C24 120.9(6) . . ?
C23 C22 C21 121.1(6) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C37 N11 C39 121.6(8) . . ?
C37 N11 C38 120.7(8) . . ?
C39 N11 C38 117.2(8) . . ?
C30 C29 C28 121.6(6) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C31 C32 C27 119.8(6) . . ?
C31 C32 H32 120.1 . . ?
C27 C32 H32 120.1 . . ?
C24 C23 C22 120.3(6) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C26 C21 C22 118.8(6) . . ?
C26 C21 C20 119.1(5) . . ?
C22 C21 C20 122.1(5) . . ?
C24 C25 C26 120.7(6) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 120.2(6) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
O5 C34 N10 124.7(7) . . ?
O5 C34 H34 117.7 . . ?
N10 C34 H34 117.7 . . ?
C32 C31 C30 121.0(6) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
N10 C36 H36A 109.5 . . ?
N10 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N10 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N10 C35 H35A 109.5 . . ?
N10 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N10 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O6 C37 N11 126.1(9) . . ?
O6 C37 H37 117.0 . . ?
N11 C37 H37 117.0 . . ?
N12 C41 H41A 109.5 . . ?
N12 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N12 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N11 C38 H38A 109.5 . . ?
N11 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N11 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O7 C40 N12 108.9(19) . . ?
O7 C40 H40 125.6 . . ?
N12 C40 H40 125.6 . . ?
N11 C39 H39A 109.5 . . ?
N11 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N11 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.100

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

data_130318
_database_code_depnum_ccdc_archive 'CCDC 1044074'
_audit_update_record             
;
2015-01-18 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H28 Co N10 O5'
_chemical_formula_weight         739.61

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'
Co Co 0.3494 0.9721 '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           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   11.0020(6)
_cell_length_b                   22.1547(17)
_cell_length_c                   16.9957(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.697(5)
_cell_angle_gamma                90.00
_cell_volume                     4070.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3262
_cell_measurement_theta_min      3.4220
_cell_measurement_theta_max      26.5240

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7130
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7130
_reflns_number_gt                4947
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0827P)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         7130
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1645
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.003
_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
Co1 Co 0.14436(4) 0.557404(19) 0.53059(3) 0.01591(16) Uani 1 1 d . . .
O2 O 0.00072(19) 0.59090(11) 0.45246(14) 0.0241(6) Uani 1 1 d . . .
O3 O -0.7860(2) 0.85308(11) 0.06017(15) 0.0278(6) Uani 1 1 d . . .
O4 O -0.6736(2) 0.92857(10) 0.11576(14) 0.0230(6) Uani 1 1 d . . .
O1 O -0.1626(2) 0.53315(11) 0.46079(14) 0.0237(6) Uani 1 1 d . . .
N1 N 0.2442(2) 0.55154(12) 0.43341(16) 0.0185(6) Uani 1 1 d . . .
N9 N 1.0529(2) 0.55536(13) -0.36778(17) 0.0214(7) Uani 1 1 d . . .
N2 N 0.4411(3) 0.56201(15) 0.18218(19) 0.0329(8) Uani 1 1 d . . .
H2 H 0.3828 0.5869 0.1636 0.039 Uiso 1 1 calc R . .
N3 N 0.5603(3) 0.49748(14) 0.25744(19) 0.0301(8) Uani 1 1 d . . .
N4 N 0.6118(3) 0.50443(15) 0.1913(2) 0.0366(8) Uani 1 1 d . . .
C30 C -0.6001(3) 0.82887(16) 0.1492(2) 0.0246(8) Uani 1 1 d . . .
N7 N 0.8345(3) 0.49663(16) -0.0601(2) 0.0403(9) Uani 1 1 d . . .
N6 N 0.7811(3) 0.56514(15) -0.15156(19) 0.0344(8) Uani 1 1 d . . .
H6 H 0.7442 0.5945 -0.1794 0.041 Uiso 1 1 calc R . .
C33 C -0.6908(3) 0.87251(16) 0.1067(2) 0.0231(8) Uani 1 1 d . . .
C4 C 0.4110(3) 0.50414(16) 0.3830(2) 0.0260(9) Uani 1 1 d . . .
H4 H 0.4764 0.4769 0.3911 0.031 Uiso 1 1 calc R . .
C18 C 1.0997(3) 0.51942(17) -0.3061(2) 0.0275(9) Uani 1 1 d . . .
H18 H 1.1734 0.4993 -0.3079 0.033 Uiso 1 1 calc R . .
N8 N 0.9132(3) 0.48914(16) -0.1127(2) 0.0412(9) Uani 1 1 d . . .
C6 C 0.4583(3) 0.53298(17) 0.2505(2) 0.0273(9) Uani 1 1 d . . .
C3 C 0.3835(3) 0.53810(17) 0.3131(2) 0.0241(8) Uani 1 1 d . . .
C17 C 0.9481(3) 0.58442(17) -0.3626(2) 0.0276(9) Uani 1 1 d . . .
H17 H 0.9135 0.6097 -0.4045 0.033 Uiso 1 1 calc R . .
C16 C 0.8887(3) 0.57878(18) -0.2985(2) 0.0314(9) Uani 1 1 d . . .
H16 H 0.8166 0.6003 -0.2971 0.038 Uiso 1 1 calc R . .
C2 C 0.2851(3) 0.57812(18) 0.3049(2) 0.0295(9) Uani 1 1 d . . .
H2A H 0.2639 0.6010 0.2585 0.035 Uiso 1 1 calc R . .
C7 C 0.5360(3) 0.54376(19) 0.1477(2) 0.0328(10) Uani 1 1 d . . .
N5 N 0.4799(4) 0.6247(3) -0.0475(3) 0.0864(18) Uani 1 1 d . . .
C5 C 0.3376(3) 0.51239(16) 0.4403(2) 0.0257(9) Uani 1 1 d . . .
H5 H 0.3547 0.4891 0.4865 0.031 Uiso 1 1 calc R . .
C8 C 0.6484(3) 0.5423(2) 0.0328(2) 0.0343(10) Uani 1 1 d . . .
H8 H 0.7035 0.5138 0.0591 0.041 Uiso 1 1 calc R . .
C1 C 0.2187(3) 0.58384(16) 0.3660(2) 0.0259(8) Uani 1 1 d . . .
H1 H 0.1537 0.6113 0.3599 0.031 Uiso 1 1 calc R . .
C23 C -0.2219(4) 0.70689(19) 0.2956(3) 0.0408(11) Uani 1 1 d . . .
H23 H -0.1876 0.7368 0.2682 0.049 Uiso 1 1 calc R . .
C20 C -0.1123(3) 0.57861(16) 0.4367(2) 0.0221(8) Uani 1 1 d . . .
C21 C -0.1933(3) 0.62226(16) 0.3838(2) 0.0254(8) Uani 1 1 d . . .
C24 C -0.3497(3) 0.70263(17) 0.2864(2) 0.0325(10) Uani 1 1 d . . .
C27 C -0.4340(3) 0.74642(17) 0.2367(2) 0.0303(9) Uani 1 1 d . . .
C15 C 0.9376(3) 0.54066(17) -0.2358(2) 0.0300(9) Uani 1 1 d . . .
C22 C -0.1447(3) 0.66780(19) 0.3443(2) 0.0368(11) Uani 1 1 d . . .
H22 H -0.0594 0.6722 0.3505 0.044 Uiso 1 1 calc R . .
C28 C -0.4040(3) 0.80676(17) 0.2357(2) 0.0300(9) Uani 1 1 d . . .
H28 H -0.3286 0.8202 0.2644 0.036 Uiso 1 1 calc R . .
C19 C 1.0457(4) 0.51049(18) -0.2406(2) 0.0333(10) Uani 1 1 d . . .
H19 H 1.0814 0.4844 -0.1999 0.040 Uiso 1 1 calc R . .
C12 C 0.6598(4) 0.5623(2) -0.0423(3) 0.0403(11) Uani 1 1 d . . .
C25 C -0.3962(4) 0.6576(2) 0.3262(3) 0.0547(15) Uani 1 1 d . . .
H25 H -0.4816 0.6540 0.3210 0.066 Uiso 1 1 calc R . .
C13 C 0.7565(3) 0.5422(2) -0.0843(2) 0.0339(10) Uani 1 1 d . . .
C14 C 0.8759(4) 0.53256(19) -0.1662(2) 0.0330(9) Uani 1 1 d . . .
C29 C -0.4859(3) 0.84783(18) 0.1919(2) 0.0311(9) Uani 1 1 d . . .
H29 H -0.4640 0.8884 0.1911 0.037 Uiso 1 1 calc R . .
C9 C 0.5555(4) 0.5643(2) 0.0688(2) 0.0368(10) Uani 1 1 d . . .
C31 C -0.6277(4) 0.76741(18) 0.1491(3) 0.0378(11) Uani 1 1 d . . .
H31 H -0.7021 0.7536 0.1194 0.045 Uiso 1 1 calc R . .
C26 C -0.3213(3) 0.61710(19) 0.3741(3) 0.0464(13) Uani 1 1 d . . .
H26 H -0.3562 0.5864 0.3998 0.056 Uiso 1 1 calc R . .
C11 C 0.5721(5) 0.6028(3) -0.0787(3) 0.0667(16) Uani 1 1 d . . .
H11 H 0.5783 0.6158 -0.1298 0.080 Uiso 1 1 calc R . .
C32 C -0.5472(4) 0.72704(18) 0.1921(3) 0.0422(12) Uani 1 1 d . . .
H32 H -0.5680 0.6863 0.1916 0.051 Uiso 1 1 calc R . .
N10 N 0.9765(7) 0.6932(3) 0.1067(5) 0.1290(15) Uani 1 1 d . . .
C10 C 0.4741(5) 0.6044(3) 0.0261(3) 0.0662(16) Uani 1 1 d . . .
H10 H 0.4100 0.6185 0.0499 0.079 Uiso 1 1 calc R . .
C36 C 0.8997(8) 0.6521(4) 0.0537(5) 0.1290(15) Uani 1 1 d . . .
H36A H 0.8162 0.6546 0.0626 0.193 Uiso 1 1 calc R . .
H36B H 0.9298 0.6117 0.0640 0.193 Uiso 1 1 calc R . .
H36C H 0.9017 0.6626 -0.0008 0.193 Uiso 1 1 calc R . .
C35 C 0.9695(9) 0.7564(4) 0.0968(7) 0.156(4) Uani 1 1 d . . .
H35A H 1.0459 0.7711 0.0844 0.188 Uiso 1 1 calc R . .
H35B H 0.9553 0.7748 0.1454 0.188 Uiso 1 1 calc R . .
H35C H 0.9027 0.7663 0.0538 0.188 Uiso 1 1 calc R . .
O5 O 1.1055(5) 0.6958(2) 0.2256(4) 0.1290(15) Uani 1 1 d . . .
C34 C 1.0485(8) 0.6669(4) 0.1716(6) 0.132(3) Uani 1 1 d . . .
H34 H 1.0535 0.6250 0.1739 0.158 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
Co1 O2 2.008(2) . ?
Co1 O1 2.019(2) 3_566 ?
Co1 N1 2.150(3) . ?
Co1 O3 2.152(2) 4_676 ?
Co1 N9 2.155(3) 1_456 ?
Co1 O4 2.264(2) 4_676 ?
O2 C20 1.252(4) . ?
O3 C33 1.265(4) . ?
O3 Co1 2.152(2) 4_475 ?
O4 C33 1.261(4) . ?
O4 Co1 2.264(2) 4_475 ?
O1 C20 1.254(4) . ?
O1 Co1 2.019(2) 3_566 ?
N1 C5 1.333(4) . ?
N1 C1 1.336(4) . ?
N9 C17 1.338(5) . ?
N9 C18 1.341(5) . ?
N9 Co1 2.155(3) 1_654 ?
N2 C6 1.310(5) . ?
N2 C7 1.351(5) . ?
N2 H2 0.8600 . ?
N3 C6 1.357(5) . ?
N3 N4 1.359(4) . ?
N4 C7 1.332(5) . ?
C30 C29 1.394(5) . ?
C30 C31 1.395(5) . ?
C30 C33 1.478(5) . ?
N7 C13 1.339(5) . ?
N7 N8 1.366(5) . ?
N6 C13 1.324(5) . ?
N6 C14 1.330(5) . ?
N6 H6 0.8600 . ?
C4 C5 1.387(5) . ?
C4 C3 1.391(5) . ?
C4 H4 0.9300 . ?
C18 C19 1.370(5) . ?
C18 H18 0.9300 . ?
N8 C14 1.336(5) . ?
C6 C3 1.465(5) . ?
C3 C2 1.386(5) . ?
C17 C16 1.376(5) . ?
C17 H17 0.9300 . ?
C16 C15 1.387(5) . ?
C16 H16 0.9300 . ?
C2 C1 1.382(5) . ?
C2 H2A 0.9300 . ?
C7 C9 1.470(5) . ?
N5 C11 1.322(6) . ?
N5 C10 1.342(6) . ?
C5 H5 0.9300 . ?
C8 C9 1.374(6) . ?
C8 C12 1.378(6) . ?
C8 H8 0.9300 . ?
C1 H1 0.9300 . ?
C23 C22 1.377(5) . ?
C23 C24 1.389(5) . ?
C23 H23 0.9300 . ?
C20 C21 1.496(5) . ?
C21 C22 1.374(5) . ?
C21 C26 1.391(5) . ?
C24 C25 1.357(6) . ?
C24 C27 1.492(5) . ?
C27 C28 1.378(5) . ?
C27 C32 1.400(5) . ?
C15 C19 1.380(5) . ?
C15 C14 1.479(5) . ?
C22 H22 0.9300 . ?
C28 C29 1.395(5) . ?
C28 H28 0.9300 . ?
C19 H19 0.9300 . ?
C12 C11 1.377(6) . ?
C12 C13 1.457(6) . ?
C25 C26 1.378(5) . ?
C25 H25 0.9300 . ?
C29 H29 0.9300 . ?
C9 C10 1.369(6) . ?
C31 C32 1.370(5) . ?
C31 H31 0.9300 . ?
C26 H26 0.9300 . ?
C11 H11 0.9300 . ?
C32 H32 0.9300 . ?
N10 C34 1.363(10) . ?
N10 C35 1.412(9) . ?
N10 C36 1.439(8) . ?
C10 H10 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
O5 C34 1.197(9) . ?
C34 H34 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O1 118.08(9) . 3_566 ?
O2 Co1 N1 88.04(10) . . ?
O1 Co1 N1 86.42(10) 3_566 . ?
O2 Co1 O3 90.93(9) . 4_676 ?
O1 Co1 O3 150.77(9) 3_566 4_676 ?
N1 Co1 O3 91.41(10) . 4_676 ?
O2 Co1 N9 96.35(10) . 1_456 ?
O1 Co1 N9 88.62(11) 3_566 1_456 ?
N1 Co1 N9 174.52(11) . 1_456 ?
O3 Co1 N9 91.78(11) 4_676 1_456 ?
O2 Co1 O4 150.01(9) . 4_676 ?
O1 Co1 O4 91.48(9) 3_566 4_676 ?
N1 Co1 O4 88.98(9) . 4_676 ?
O3 Co1 O4 59.32(8) 4_676 4_676 ?
N9 Co1 O4 88.83(10) 1_456 4_676 ?
C20 O2 Co1 133.6(2) . . ?
C33 O3 Co1 92.9(2) . 4_475 ?
C33 O4 Co1 87.84(19) . 4_475 ?
C20 O1 Co1 141.0(2) . 3_566 ?
C5 N1 C1 117.3(3) . . ?
C5 N1 Co1 117.9(2) . . ?
C1 N1 Co1 124.8(2) . . ?
C17 N9 C18 116.4(3) . . ?
C17 N9 Co1 125.4(2) . 1_654 ?
C18 N9 Co1 118.1(2) . 1_654 ?
C6 N2 C7 104.0(3) . . ?
C6 N2 H2 128.0 . . ?
C7 N2 H2 128.0 . . ?
C6 N3 N4 109.1(3) . . ?
C7 N4 N3 102.7(3) . . ?
C29 C30 C31 118.0(3) . . ?
C29 C30 C33 121.2(3) . . ?
C31 C30 C33 120.7(3) . . ?
C13 N7 N8 109.7(3) . . ?
C13 N6 C14 104.3(3) . . ?
C13 N6 H6 127.9 . . ?
C14 N6 H6 127.9 . . ?
O4 C33 O3 120.0(3) . . ?
O4 C33 C30 120.8(3) . . ?
O3 C33 C30 119.2(3) . . ?
C5 C4 C3 117.7(3) . . ?
C5 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
N9 C18 C19 124.0(3) . . ?
N9 C18 H18 118.0 . . ?
C19 C18 H18 118.0 . . ?
C14 N8 N7 101.9(3) . . ?
N2 C6 N3 110.1(3) . . ?
N2 C6 C3 126.7(3) . . ?
N3 C6 C3 123.3(3) . . ?
C2 C3 C4 118.3(3) . . ?
C2 C3 C6 120.7(3) . . ?
C4 C3 C6 121.0(3) . . ?
N9 C17 C16 123.3(3) . . ?
N9 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C17 C16 C15 119.4(4) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
N4 C7 N2 114.1(4) . . ?
N4 C7 C9 121.9(4) . . ?
N2 C7 C9 124.0(4) . . ?
C11 N5 C10 115.1(4) . . ?
N1 C5 C4 124.3(3) . . ?
N1 C5 H5 117.8 . . ?
C4 C5 H5 117.8 . . ?
C9 C8 C12 120.0(4) . . ?
C9 C8 H8 120.0 . . ?
C12 C8 H8 120.0 . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C22 C23 C24 121.6(4) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
O2 C20 O1 125.9(3) . . ?
O2 C20 C21 116.4(3) . . ?
O1 C20 C21 117.7(3) . . ?
C22 C21 C26 118.6(3) . . ?
C22 C21 C20 121.7(3) . . ?
C26 C21 C20 119.7(3) . . ?
C25 C24 C23 117.5(4) . . ?
C25 C24 C27 120.5(3) . . ?
C23 C24 C27 121.9(4) . . ?
C28 C27 C32 118.8(3) . . ?
C28 C27 C24 120.9(3) . . ?
C32 C27 C24 120.3(3) . . ?
C19 C15 C16 117.7(4) . . ?
C19 C15 C14 121.1(4) . . ?
C16 C15 C14 121.2(3) . . ?
C21 C22 C23 120.2(3) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C27 C28 C29 120.5(3) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C18 C19 C15 119.1(4) . . ?
C18 C19 H19 120.4 . . ?
C15 C19 H19 120.4 . . ?
C11 C12 C8 116.7(4) . . ?
C11 C12 C13 119.5(4) . . ?
C8 C12 C13 123.8(4) . . ?
C24 C25 C26 122.2(4) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
N6 C13 N7 109.5(4) . . ?
N6 C13 C12 126.2(4) . . ?
N7 C13 C12 124.3(4) . . ?
N6 C14 N8 114.5(4) . . ?
N6 C14 C15 125.2(4) . . ?
N8 C14 C15 120.3(4) . . ?
C30 C29 C28 120.8(4) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C10 C9 C8 117.5(4) . . ?
C10 C9 C7 119.5(4) . . ?
C8 C9 C7 122.8(4) . . ?
C32 C31 C30 121.2(3) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C25 C26 C21 119.9(4) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
N5 C11 C12 125.8(5) . . ?
N5 C11 H11 117.1 . . ?
C12 C11 H11 117.1 . . ?
C31 C32 C27 120.7(4) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
C34 N10 C35 122.1(8) . . ?
C34 N10 C36 114.9(8) . . ?
C35 N10 C36 122.7(8) . . ?
N5 C10 C9 124.9(4) . . ?
N5 C10 H10 117.6 . . ?
C9 C10 H10 117.6 . . ?
N10 C36 H36A 109.5 . . ?
N10 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N10 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N10 C35 H35A 109.5 . . ?
N10 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N10 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O5 C34 N10 122.4(8) . . ?
O5 C34 H34 118.8 . . ?
N10 C34 H34 118.8 . . ?

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
_platon_squeeze_void_content
1 -0.323 0.277 0.074 245 18 ' '
2 0.322 0.777 0.426 245 18 ' '
3 -0.323 0.223 0.574 245 17 ' '
4 0.322 0.723 0.926 245 18 ' '
5 0.217 0.102 0.309 7 0 ' '
6 0.217 0.398 0.809 7 0 ' '
7 0.783 0.602 0.190 7 0 ' '
8 0.783 0.898 0.690 7 0 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.076
