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

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

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H16 Cd N0 O8'
_chemical_formula_sum            'C23 H16 Cd N0 O8'
_chemical_formula_weight         532.76

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           Orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   19.0064(19)
_cell_length_b                   24.517(2)
_cell_length_c                   4.6956(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2188.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3308
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      24.63

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7113
_exptl_absorpt_correction_T_max  0.8591
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11049
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3730
_reflns_number_gt                3297
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.1810P)²+16.8915P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(9)
_refine_ls_number_reflns         3730
_refine_ls_number_parameters     290
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0680
_refine_ls_wR_factor_ref         0.2400
_refine_ls_wR_factor_gt          0.2271
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4613(5) 0.6346(3) -0.236(3) 0.030(2) Uani 1 1 d . . .
C2 C 0.4638(5) 0.6960(4) -0.162(2) 0.024(2) Uani 1 1 d . . .
C3 C 0.4144(5) 0.7305(3) -0.288(2) 0.030(2) Uani 1 1 d . . .
H3 H 0.3824 0.7174 -0.4216 0.036 Uiso 1 1 calc R . .
C4 C 0.4144(5) 0.7856(4) -0.207(2) 0.031(2) Uani 1 1 d . . .
C5 C 0.4637(5) 0.8047(4) -0.019(2) 0.032(2) Uani 1 1 d . . .
H5 H 0.4641 0.8415 0.0296 0.038 Uiso 1 1 calc R . .
C6 C 0.5101(5) 0.7719(4) 0.094(2) 0.033(2) Uani 1 1 d . . .
C7 C 0.5108(5) 0.7158(4) 0.038(2) 0.029(2) Uani 1 1 d . . .
H7 H 0.5418 0.6926 0.1319 0.035 Uiso 1 1 calc R . .
C8 C 0.3092(6) 0.7989(5) -0.479(3) 0.047(3) Uani 1 1 d . . .
H8A H 0.2863 0.7704 -0.3696 0.056 Uiso 1 1 calc R . .
H8B H 0.3265 0.7830 -0.6551 0.056 Uiso 1 1 calc R . .
C9 C 0.2579(6) 0.8442(4) -0.543(3) 0.039(3) Uani 1 1 d . . .
C10 C 0.1960(7) 0.8492(5) -0.401(3) 0.049(3) Uani 1 1 d . . .
H10 H 0.1856 0.8242 -0.2581 0.059 Uiso 1 1 calc R . .
C11 C 0.1477(6) 0.8902(4) -0.459(3) 0.039(3) Uani 1 1 d . . .
H11 H 0.1060 0.8925 -0.3558 0.047 Uiso 1 1 calc R . .
C12 C 0.1626(5) 0.9287(4) -0.678(2) 0.029(3) Uani 1 1 d . . .
C13 C 0.2267(6) 0.9258(5) -0.815(2) 0.046(3) Uani 1 1 d . . .
H13 H 0.2379 0.9521 -0.9503 0.055 Uiso 1 1 calc R . .
C14 C 0.2748(5) 0.8850(5) -0.756(4) 0.055(3) Uani 1 1 d . . .
H14 H 0.3176 0.8838 -0.8517 0.066 Uiso 1 1 calc R . .
C15 C 0.1093(5) 0.9686(3) -0.769(3) 0.028(2) Uani 1 1 d . . .
C16 C 0.5667(6) 0.8423(5) 0.347(3) 0.039(3) Uani 1 1 d . . .
H16A H 0.5243 0.8547 0.4424 0.047 Uiso 1 1 calc R . .
H16B H 0.5720 0.8629 0.1723 0.047 Uiso 1 1 calc R . .
C17 C 0.6299(5) 0.8515(5) 0.538(2) 0.041(3) Uani 1 1 d . . .
C18 C 0.6561(6) 0.8113(4) 0.708(3) 0.046(3) Uani 1 1 d . . .
H18 H 0.6357 0.7768 0.7041 0.056 Uiso 1 1 calc R . .
C19 C 0.7124(6) 0.8212(5) 0.886(3) 0.044(3) Uani 1 1 d . . .
H19 H 0.7299 0.7935 1.0012 0.053 Uiso 1 1 calc R . .
C20 C 0.7436(5) 0.8739(4) 0.892(2) 0.033(2) Uani 1 1 d . . .
C21 C 0.7184(6) 0.9145(4) 0.715(3) 0.048(3) Uani 1 1 d . . .
H21 H 0.7397 0.9487 0.7095 0.058 Uiso 1 1 calc R . .
C22 C 0.6611(6) 0.9029(4) 0.549(3) 0.045(3) Uani 1 1 d . . .
H22 H 0.6421 0.9307 0.4377 0.053 Uiso 1 1 calc R . .
C23 C 0.8060(5) 0.8849(4) 1.071(2) 0.033(2) Uani 1 1 d . . .
Cd1 Cd 0.44712(3) 0.54590(2) 0.2515(3) 0.02368(18) Uani 1 1 d . . .
O1 O 0.4330(4) 0.6221(3) -0.4668(17) 0.0310(16) Uani 1 1 d . . .
O2 O 0.4934(7) 0.6027(12) -0.084(4) 0.799(9) Uani 1 1 d . . .
O3 O 0.5614(4) 0.7866(3) 0.286(3) 0.050(2) Uani 1 1 d . . .
O4 O 0.3668(4) 0.8218(3) -0.3187(17) 0.044(2) Uani 1 1 d . . .
O5 O 0.1210(4) 0.9922(3) -0.9913(17) 0.044(2) Uani 1 1 d . . .
O6 O 0.0565(3) 0.9781(3) -0.6093(18) 0.0292(17) Uani 1 1 d . . .
O7 O 0.8379(4) 0.9276(3) 1.0673(18) 0.0389(19) Uani 1 1 d . . .
O8 O 0.8263(4) 0.8440(3) 1.229(2) 0.0468(19) Uani 1 1 d . . .
H8 H 0.8647 0.8509 1.2998 0.070 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
C1 O1 1.246(15) . ?
C1 O2 1.22(3) . ?
C1 C2 1.547(12) . ?
C2 C7 1.382(14) . ?
C2 C3 1.397(13) . ?
C3 C4 1.405(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(14) . ?
C4 O4 1.372(11) . ?
C5 C6 1.305(15) . ?
C5 H5 0.9300 . ?
C6 O3 1.374(13) . ?
C6 C7 1.402(14) . ?
C7 H7 0.9300 . ?
C8 O4 1.443(13) . ?
C8 C9 1.508(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.359(17) . ?
C9 C14 1.449(18) . ?
C10 C11 1.389(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.425(15) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(15) . ?
C12 C15 1.471(13) . ?
C13 C14 1.384(15) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O5 1.213(14) . ?
C15 O6 1.275(12) . ?
C16 O3 1.401(13) . ?
C16 C17 1.516(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.362(17) . ?
C17 C22 1.394(16) . ?
C18 C19 1.380(17) . ?
C18 H18 0.9300 . ?
C19 C20 1.422(15) . ?
C19 H19 0.9300 . ?
C20 C21 1.384(16) . ?
C20 C23 1.477(14) . ?
C21 C22 1.371(17) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O7 1.210(12) . ?
C23 O8 1.306(14) . ?
Cd1 O5 2.207(8) 4_546 ?
Cd1 O6 2.257(6) 3_566 ?
Cd1 O2 2.28(2) . ?
Cd1 O1 2.305(7) 1_556 ?
Cd1 O7 2.341(7) 3_464 ?
Cd1 O6 2.375(8) 4_545 ?
O1 Cd1 2.305(7) 1_554 ?
O5 Cd1 2.207(8) 4_553 ?
O6 Cd1 2.257(6) 3_464 ?
O6 Cd1 2.375(8) 4_554 ?
O7 Cd1 2.341(7) 3_566 ?
O8 H8 0.8203 . ?

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 C1 O2 124.5(12) . . ?
O1 C1 C2 116.7(8) . . ?
O2 C1 C2 118.2(12) . . ?
C7 C2 C3 120.7(8) . . ?
C7 C2 C1 121.1(8) . . ?
C3 C2 C1 118.1(8) . . ?
C2 C3 C4 117.8(9) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C5 C4 O4 118.5(8) . . ?
C5 C4 C3 120.2(9) . . ?
O4 C4 C3 121.2(9) . . ?
C6 C5 C4 121.0(9) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 O3 125.7(9) . . ?
C5 C6 C7 122.3(9) . . ?
O3 C6 C7 112.0(9) . . ?
C2 C7 C6 117.8(9) . . ?
C2 C7 H7 121.1 . . ?
C6 C7 H7 121.1 . . ?
O4 C8 C9 107.9(9) . . ?
O4 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 C14 117.9(10) . . ?
C10 C9 C8 121.9(11) . . ?
C14 C9 C8 120.2(10) . . ?
C9 C10 C11 122.8(11) . . ?
C9 C10 H10 118.6 . . ?
C11 C10 H10 118.6 . . ?
C10 C11 C12 119.3(10) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 118.5(9) . . ?
C13 C12 C15 120.4(9) . . ?
C11 C12 C15 120.9(9) . . ?
C12 C13 C14 121.9(11) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C9 119.4(11) . . ?
C13 C14 H14 120.3 . . ?
C9 C14 H14 120.3 . . ?
O5 C15 O6 124.4(9) . . ?
O5 C15 C12 116.2(9) . . ?
O6 C15 C12 119.4(10) . . ?
O3 C16 C17 108.9(9) . . ?
O3 C16 H16A 109.9 . . ?
C17 C16 H16A 109.9 . . ?
O3 C16 H16B 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
C18 C17 C22 118.6(10) . . ?
C18 C17 C16 121.9(11) . . ?
C22 C17 C16 119.5(11) . . ?
C17 C18 C19 120.7(10) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 119.8(11) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 119.8(10) . . ?
C21 C20 C23 119.2(9) . . ?
C19 C20 C23 120.9(10) . . ?
C22 C21 C20 118.0(10) . . ?
C22 C21 H21 121.0 . . ?
C20 C21 H21 121.0 . . ?
C21 C22 C17 123.1(11) . . ?
C21 C22 H22 118.5 . . ?
C17 C22 H22 118.5 . . ?
O7 C23 O8 121.7(9) . . ?
O7 C23 C20 123.5(10) . . ?
O8 C23 C20 114.8(9) . . ?
O5 Cd1 O6 103.1(3) 4_546 3_566 ?
O5 Cd1 O2 165.8(5) 4_546 . ?
O6 Cd1 O2 90.2(6) 3_566 . ?
O5 Cd1 O1 95.8(3) 4_546 1_556 ?
O6 Cd1 O1 98.8(3) 3_566 1_556 ?
O2 Cd1 O1 86.9(5) . 1_556 ?
O5 Cd1 O7 81.2(3) 4_546 3_464 ?
O6 Cd1 O7 174.9(3) 3_566 3_464 ?
O2 Cd1 O7 85.3(6) . 3_464 ?
O1 Cd1 O7 83.3(3) 1_556 3_464 ?
O5 Cd1 O6 87.4(3) 4_546 4_545 ?
O6 Cd1 O6 92.92(18) 3_566 4_545 ?
O2 Cd1 O6 86.9(5) . 4_545 ?
O1 Cd1 O6 166.8(3) 1_556 4_545 ?
O7 Cd1 O6 84.6(2) 3_464 4_545 ?
C1 O1 Cd1 130.3(6) . 1_554 ?
C1 O2 Cd1 127.1(10) . . ?
C6 O3 C16 116.2(8) . . ?
C4 O4 C8 116.6(8) . . ?
C15 O5 Cd1 130.3(7) . 4_553 ?
C15 O6 Cd1 120.5(7) . 3_464 ?
C15 O6 Cd1 124.7(6) . 4_554 ?
Cd1 O6 Cd1 111.2(3) 3_464 4_554 ?
C23 O7 Cd1 132.8(7) . 3_566 ?
C23 O8 H8 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.758
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.351
_database_code_depnum_ccdc_archive 'CCDC 986465'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H26 Cd N4 O8'
_chemical_formula_weight         743.00

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   27.0432(17)
_cell_length_b                   8.0754(5)
_cell_length_c                   27.1949(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5938.9(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5140
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      22.85

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7249
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_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            29097
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5239
_reflns_number_gt                3717
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0148P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5239
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.68494(11) 0.1855(4) 0.96818(11) 0.0300(7) Uani 1 1 d . . .
C2 C 0.64356(11) 0.1479(3) 0.93248(10) 0.0274(7) Uani 1 1 d . . .
C3 C 0.63928(12) 0.2485(3) 0.89139(11) 0.0326(8) Uani 1 1 d . . .
H3 H 0.6619 0.3337 0.8864 0.039 Uiso 1 1 calc R . .
C4 C 0.60182(12) 0.2232(4) 0.85784(11) 0.0351(8) Uani 1 1 d . . .
C5 C 0.56855(12) 0.0975(4) 0.86437(11) 0.0352(8) Uani 1 1 d . . .
H5 H 0.5431 0.0805 0.8419 0.042 Uiso 1 1 calc R . .
C6 C 0.57361(12) -0.0047(4) 0.90553(11) 0.0342(8) Uani 1 1 d . . .
C7 C 0.61077(11) 0.0191(4) 0.93962(11) 0.0304(8) Uani 1 1 d . . .
H7 H 0.6136 -0.0501 0.9668 0.036 Uiso 1 1 calc R . .
C8 C 0.55849(14) 0.3367(4) 0.78790(13) 0.0609(11) Uani 1 1 d . . .
H8A H 0.5285 0.3387 0.8074 0.073 Uiso 1 1 calc R . .
H8B H 0.5579 0.2394 0.7670 0.073 Uiso 1 1 calc R . .
C9 C 0.56258(13) 0.4933(4) 0.75693(13) 0.0493(10) Uani 1 1 d . . .
C10 C 0.55591(14) 0.6468(5) 0.77991(14) 0.0562(11) Uani 1 1 d . . .
H10 H 0.5499 0.6533 0.8135 0.067 Uiso 1 1 calc R . .
C11 C 0.55847(14) 0.7903(5) 0.75112(13) 0.0582(11) Uani 1 1 d . . .
H11 H 0.5533 0.8931 0.7656 0.070 Uiso 1 1 calc R . .
C12 C 0.56865(13) 0.7809(4) 0.70112(12) 0.0453(9) Uani 1 1 d . . .
C13 C 0.57479(13) 0.6298(4) 0.67910(13) 0.0474(10) Uani 1 1 d . . .
H13 H 0.5810 0.6242 0.6455 0.057 Uiso 1 1 calc R . .
C14 C 0.57178(13) 0.4842(4) 0.70645(12) 0.0512(10) Uani 1 1 d . . .
H14 H 0.5759 0.3820 0.6912 0.061 Uiso 1 1 calc R . .
C15 C 0.57106(15) 0.9397(5) 0.67246(15) 0.0548(11) Uani 1 1 d . . .
C16 C 0.54039(13) -0.2353(4) 0.94986(12) 0.0503(10) Uani 1 1 d . . .
H16A H 0.5378 -0.1709 0.9799 0.060 Uiso 1 1 calc R . .
H16B H 0.5715 -0.2952 0.9505 0.060 Uiso 1 1 calc R . .
C17 C 0.49804(13) -0.3548(4) 0.94644(12) 0.0392(9) Uani 1 1 d . . .
C18 C 0.45359(13) -0.3176(4) 0.96810(12) 0.0460(9) Uani 1 1 d . . .
H18 H 0.4493 -0.2152 0.9831 0.055 Uiso 1 1 calc R . .
C19 C 0.41546(13) -0.4293(4) 0.96790(12) 0.0398(9) Uani 1 1 d . . .
H19 H 0.3859 -0.4027 0.9835 0.048 Uiso 1 1 calc R . .
C20 C 0.42034(12) -0.5805(4) 0.94491(10) 0.0320(8) Uani 1 1 d . . .
C21 C 0.46427(13) -0.6182(4) 0.92206(12) 0.0431(9) Uani 1 1 d . . .
H21 H 0.4680 -0.7188 0.9058 0.052 Uiso 1 1 calc R . .
C22 C 0.50297(14) -0.5061(4) 0.92331(12) 0.0453(9) Uani 1 1 d . . .
H22 H 0.5328 -0.5332 0.9083 0.054 Uiso 1 1 calc R . .
C23 C 0.37833(13) -0.7032(4) 0.94728(12) 0.0376(8) Uani 1 1 d . . .
C24 C 0.72452(12) -0.1498(4) 0.88766(11) 0.0366(8) Uani 1 1 d . . .
H24 H 0.7504 -0.0752 0.8921 0.044 Uiso 1 1 calc R . .
C25 C 0.66884(13) -0.3302(4) 0.90136(12) 0.0405(9) Uani 1 1 d . . .
H25 H 0.6483 -0.4051 0.9174 0.049 Uiso 1 1 calc R . .
C26 C 0.66740(13) -0.2951(4) 0.85239(11) 0.0465(9) Uani 1 1 d . . .
H26 H 0.6463 -0.3415 0.8292 0.056 Uiso 1 1 calc R . .
C27 C 0.71645(13) -0.1077(4) 0.79740(11) 0.0374(8) Uani 1 1 d . . .
C28 C 0.68103(13) -0.0425(4) 0.76691(12) 0.0509(10) Uani 1 1 d . . .
H28 H 0.6481 -0.0429 0.7766 0.061 Uiso 1 1 calc R . .
C29 C 0.76471(13) -0.1061(4) 0.78350(12) 0.0458(9) Uani 1 1 d . . .
H29 H 0.7888 -0.1499 0.8042 0.055 Uiso 1 1 calc R . .
C30 C 0.79830(13) -0.1918(5) 1.09911(12) 0.0542(10) Uani 1 1 d . . .
H30 H 0.8241 -0.2357 1.0806 0.065 Uiso 1 1 calc R . .
C31 C 0.80155(14) -0.1469(5) 1.14690(13) 0.0627(12) Uani 1 1 d . . .
H31 H 0.8294 -0.1538 1.1668 0.075 Uiso 1 1 calc R . .
C32 C 0.72779(13) -0.1043(4) 1.11981(11) 0.0444(9) Uani 1 1 d . . .
H32 H 0.6945 -0.0753 1.1189 0.053 Uiso 1 1 calc R . .
C33 C 0.74282(13) -0.0245(4) 1.20731(11) 0.0388(9) Uani 1 1 d . . .
C34 C 0.69401(13) -0.0238(4) 1.22184(12) 0.0518(10) Uani 1 1 d . . .
H34 H 0.6698 -0.0680 1.2014 0.062 Uiso 1 1 calc R . .
C35 C 0.77814(13) 0.0392(4) 1.23837(11) 0.0458(9) Uani 1 1 d . . .
H35 H 0.8112 0.0375 1.2291 0.055 Uiso 1 1 calc R . .
Cd1 Cd 0.722774(8) -0.19789(3) 1.005287(7) 0.02745(8) Uani 1 1 d . . .
N1 N 0.75199(10) -0.1633(3) 1.08206(9) 0.0389(7) Uani 1 1 d . . .
N2 N 0.75650(10) -0.0900(3) 1.16020(9) 0.0394(7) Uani 1 1 d . . .
N3 N 0.70493(10) -0.2386(3) 0.92330(9) 0.0344(7) Uani 1 1 d . . .
N4 N 0.70268(10) -0.1797(3) 0.84405(9) 0.0363(7) Uani 1 1 d . . .
O1 O 0.70356(8) 0.0750(2) 0.99483(7) 0.0391(6) Uani 1 1 d . . .
O2 O 0.69990(8) 0.3326(3) 0.96921(8) 0.0392(6) Uani 1 1 d . . .
O3 O 0.60094(9) 0.3342(3) 0.81902(8) 0.0537(7) Uani 1 1 d . . .
O4 O 0.53882(9) -0.1279(3) 0.90796(8) 0.0531(7) Uani 1 1 d . . .
O5 O 0.55723(13) 1.0705(3) 0.68810(11) 0.0973(12) Uani 1 1 d . . .
O6 O 0.59224(12) 0.9209(3) 0.62927(10) 0.0721(9) Uani 1 1 d . . .
H6 H 0.5953 1.0115 0.6160 0.108 Uiso 1 1 calc R . .
O7 O 0.37955(10) -0.8305(3) 0.92222(10) 0.0760(9) Uani 1 1 d . . .
O8 O 0.34468(9) -0.6667(3) 0.97617(8) 0.0540(7) 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 O1 1.255(3) . ?
C1 O2 1.255(3) . ?
C1 C2 1.512(4) . ?
C2 C7 1.381(4) . ?
C2 C3 1.386(4) . ?
C3 C4 1.379(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(4) . ?
C4 O3 1.385(3) . ?
C5 C6 1.398(4) . ?
C5 H5 0.9300 . ?
C6 O4 1.371(3) . ?
C6 C7 1.381(4) . ?
C7 H7 0.9300 . ?
C8 O3 1.426(4) . ?
C8 C9 1.524(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C14 1.397(4) . ?
C9 C10 1.400(4) . ?
C10 C11 1.400(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.370(4) . ?
C12 C15 1.502(4) . ?
C13 C14 1.393(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O5 1.198(4) . ?
C15 O6 1.316(4) . ?
C16 O4 1.433(3) . ?
C16 C17 1.500(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.372(4) . ?
C17 C22 1.381(4) . ?
C18 C19 1.370(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.378(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.375(4) . ?
C20 C23 1.509(4) . ?
C21 C22 1.384(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O7 1.233(4) . ?
C23 O8 1.238(4) . ?
C24 N3 1.317(3) . ?
C24 N4 1.347(3) . ?
C24 H24 0.9300 . ?
C25 N3 1.362(4) . ?
C25 C26 1.362(4) . ?
C25 H25 0.9300 . ?
C26 N4 1.353(4) . ?
C26 H26 0.9300 . ?
C27 C29 1.359(4) . ?
C27 C28 1.372(4) . ?
C27 N4 1.445(4) . ?
C28 C34 1.383(4) 7 ?
C28 H28 0.9300 . ?
C29 C35 1.389(4) 7 ?
C29 H29 0.9300 . ?
C30 C31 1.352(4) . ?
C30 N1 1.355(4) . ?
C30 H30 0.9300 . ?
C31 N2 1.351(4) . ?
C31 H31 0.9300 . ?
C32 N1 1.307(4) . ?
C32 N2 1.350(4) . ?
C32 H32 0.9300 . ?
C33 C35 1.375(4) . ?
C33 C34 1.378(4) . ?
C33 N2 1.435(4) . ?
C34 C28 1.383(4) 7_556 ?
C34 H34 0.9300 . ?
C35 C29 1.389(4) 7_556 ?
C35 H35 0.9300 . ?
Cd1 O8 2.186(2) 5_647 ?
Cd1 N1 2.250(2) . ?
Cd1 O1 2.282(2) . ?
Cd1 N3 2.305(2) . ?
Cd1 O2 2.323(2) 8_755 ?
O2 Cd1 2.323(2) 8_765 ?
O6 H6 0.8200 . ?
O8 Cd1 2.186(2) 5_647 ?

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 C1 O2 122.0(3) . . ?
O1 C1 C2 121.7(3) . . ?
O2 C1 C2 116.3(3) . . ?
C7 C2 C3 120.1(3) . . ?
C7 C2 C1 122.4(3) . . ?
C3 C2 C1 117.5(3) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 O3 124.6(3) . . ?
C3 C4 O3 114.9(3) . . ?
C4 C5 C6 118.5(3) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
O4 C6 C7 124.6(3) . . ?
O4 C6 C5 113.6(3) . . ?
C7 C6 C5 121.8(3) . . ?
C2 C7 C6 118.6(3) . . ?
C2 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
O3 C8 C9 106.3(3) . . ?
O3 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
O3 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C14 C9 C10 120.5(3) . . ?
C14 C9 C8 120.8(3) . . ?
C10 C9 C8 118.6(3) . . ?
C9 C10 C11 118.5(4) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
C12 C11 C10 120.8(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 C15 121.9(3) . . ?
C11 C12 C15 118.0(3) . . ?
C12 C13 C14 120.7(3) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C9 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C9 C14 H14 120.3 . . ?
O5 C15 O6 123.7(4) . . ?
O5 C15 C12 123.7(4) . . ?
O6 C15 C12 112.6(3) . . ?
O4 C16 C17 108.5(3) . . ?
O4 C16 H16A 110.0 . . ?
C17 C16 H16A 110.0 . . ?
O4 C16 H16B 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
C18 C17 C22 118.3(3) . . ?
C18 C17 C16 120.1(3) . . ?
C22 C17 C16 121.6(3) . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 120.9(3) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C21 C20 C19 119.0(3) . . ?
C21 C20 C23 121.6(3) . . ?
C19 C20 C23 119.4(3) . . ?
C20 C21 C22 119.8(3) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C17 C22 C21 121.1(3) . . ?
C17 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
O7 C23 O8 124.7(3) . . ?
O7 C23 C20 120.2(3) . . ?
O8 C23 C20 115.1(3) . . ?
N3 C24 N4 111.9(3) . . ?
N3 C24 H24 124.0 . . ?
N4 C24 H24 124.0 . . ?
N3 C25 C26 109.6(3) . . ?
N3 C25 H25 125.2 . . ?
C26 C25 H25 125.2 . . ?
N4 C26 C25 106.7(3) . . ?
N4 C26 H26 126.7 . . ?
C25 C26 H26 126.7 . . ?
C29 C27 C28 119.9(3) . . ?
C29 C27 N4 119.7(3) . . ?
C28 C27 N4 120.4(3) . . ?
C27 C28 C34 120.5(3) . 7 ?
C27 C28 H28 119.8 . . ?
C34 C28 H28 119.8 7 . ?
C27 C29 C35 120.0(3) . 7 ?
C27 C29 H29 120.0 . . ?
C35 C29 H29 120.0 7 . ?
C31 C30 N1 110.1(3) . . ?
C31 C30 H30 125.0 . . ?
N1 C30 H30 125.0 . . ?
N2 C31 C30 106.8(3) . . ?
N2 C31 H31 126.6 . . ?
C30 C31 H31 126.6 . . ?
N1 C32 N2 112.5(3) . . ?
N1 C32 H32 123.8 . . ?
N2 C32 H32 123.8 . . ?
C35 C33 C34 119.2(3) . . ?
C35 C33 N2 120.5(3) . . ?
C34 C33 N2 120.3(3) . . ?
C33 C34 C28 119.9(3) . 7_556 ?
C33 C34 H34 120.0 . . ?
C28 C34 H34 120.0 7_556 . ?
C33 C35 C29 120.4(3) . 7_556 ?
C33 C35 H35 119.8 . . ?
C29 C35 H35 119.8 7_556 . ?
O8 Cd1 N1 98.11(9) 5_647 . ?
O8 Cd1 O1 108.76(8) 5_647 . ?
N1 Cd1 O1 94.34(8) . . ?
O8 Cd1 N3 88.68(9) 5_647 . ?
N1 Cd1 N3 171.49(9) . . ?
O1 Cd1 N3 88.26(8) . . ?
O8 Cd1 O2 154.40(8) 5_647 8_755 ?
N1 Cd1 O2 93.59(9) . 8_755 ?
O1 Cd1 O2 92.87(7) . 8_755 ?
N3 Cd1 O2 78.17(8) . 8_755 ?
C32 N1 C30 104.8(3) . . ?
C32 N1 Cd1 126.7(2) . . ?
C30 N1 Cd1 128.4(2) . . ?
C32 N2 C31 105.8(3) . . ?
C32 N2 C33 127.6(3) . . ?
C31 N2 C33 126.6(3) . . ?
C24 N3 C25 105.2(3) . . ?
C24 N3 Cd1 123.4(2) . . ?
C25 N3 Cd1 130.6(2) . . ?
C24 N4 C26 106.6(3) . . ?
C24 N4 C27 126.0(3) . . ?
C26 N4 C27 127.3(3) . . ?
C1 O1 Cd1 148.19(19) . . ?
C1 O2 Cd1 101.50(19) . 8_765 ?
C4 O3 C8 118.4(3) . . ?
C6 O4 C16 117.2(2) . . ?
C15 O6 H6 109.5 . . ?
C23 O8 Cd1 129.9(2) . 5_647 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 986466'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H26 Mn N4 O8'
_chemical_formula_weight         685.54

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   26.780(2)
_cell_length_b                   8.1675(7)
_cell_length_c                   26.928(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5889.9(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2486
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      21.46

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2824
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_T_max  0.9650
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_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            28793
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5188
_reflns_number_gt                2862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0230P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5188
_refine_ls_number_parameters     434
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.20172(17) 0.7999(5) 0.60145(16) 0.0545(12) Uani 1 1 d . . .
H1 H 0.1757 0.7551 0.5831 0.065 Uiso 1 1 calc R . .
C2 C 0.19845(16) 0.8445(6) 0.64925(16) 0.0588(13) Uani 1 1 d . . .
H2 H 0.1705 0.8356 0.6695 0.071 Uiso 1 1 calc R . .
C3 C 0.27225(16) 0.8914(5) 0.62162(14) 0.0432(11) Uani 1 1 d . . .
H3 H 0.3056 0.9227 0.6204 0.052 Uiso 1 1 calc R . .
C4 C 0.25769(15) 0.9741(5) 0.70946(14) 0.0383(10) Uani 1 1 d . . .
C5 C 0.30708(16) 0.9756(5) 0.72460(16) 0.0512(12) Uani 1 1 d . . .
H5 H 0.3317 0.9305 0.7044 0.061 Uiso 1 1 calc R . .
C6 C 0.22179(16) 1.0399(5) 0.74024(14) 0.0449(11) Uani 1 1 d . . .
H6 H 0.1884 1.0376 0.7306 0.054 Uiso 1 1 calc R . .
C7 C 0.33080(15) 0.6657(4) 0.40461(16) 0.0410(11) Uani 1 1 d . . .
H7 H 0.3511 0.5902 0.4208 0.049 Uiso 1 1 calc R . .
C8 C 0.33305(15) 0.6986(5) 0.35543(15) 0.0439(11) Uani 1 1 d . . .
H8 H 0.3545 0.6517 0.3323 0.053 Uiso 1 1 calc R . .
C9 C 0.27589(14) 0.8447(4) 0.39097(13) 0.0344(10) Uani 1 1 d . . .
H9 H 0.2501 0.9195 0.3953 0.041 Uiso 1 1 calc R . .
C10 C 0.28430(15) 0.8872(5) 0.30032(14) 0.0360(10) Uani 1 1 d . . .
C11 C 0.31978(16) 0.9561(5) 0.26962(15) 0.0493(12) Uani 1 1 d . . .
H11 H 0.3530 0.9564 0.2796 0.059 Uiso 1 1 calc R . .
C12 C 0.23490(15) 0.8905(5) 0.28544(15) 0.0438(11) Uani 1 1 d . . .
H12 H 0.2104 0.8459 0.3058 0.053 Uiso 1 1 calc R . .
C13 C 0.18603(14) 0.6692(5) 0.47289(14) 0.0322(9) Uani 1 1 d U . .
C14 C 0.14411(13) 0.6398(4) 0.43654(13) 0.0269(9) Uani 1 1 d . . .
C15 C 0.11033(14) 0.5113(4) 0.44307(14) 0.0340(10) Uani 1 1 d . . .
H15 H 0.1129 0.4409 0.4701 0.041 Uiso 1 1 calc R . .
C16 C 0.07291(14) 0.4920(4) 0.40822(15) 0.0358(10) Uani 1 1 d . . .
C17 C 0.06848(14) 0.5955(4) 0.36750(15) 0.0399(11) Uani 1 1 d . . .
H17 H 0.0431 0.5799 0.3444 0.048 Uiso 1 1 calc R . .
C18 C 0.10227(15) 0.7219(4) 0.36184(14) 0.0361(10) Uani 1 1 d . . .
C19 C 0.13989(14) 0.7429(4) 0.39642(14) 0.0336(10) Uani 1 1 d . . .
H19 H 0.1626 0.8280 0.3925 0.040 Uiso 1 1 calc R . .
C20 C 0.05893(17) 0.8321(6) 0.29039(17) 0.0707(15) Uani 1 1 d U . .
H20A H 0.0281 0.8314 0.3092 0.085 Uiso 1 1 calc R . .
H20B H 0.0597 0.7359 0.2693 0.085 Uiso 1 1 calc R . .
C21 C 0.06274(16) 0.9876(5) 0.2592(2) 0.0568(13) Uani 1 1 d . . .
C22 C 0.07212(16) 0.9795(6) 0.20822(18) 0.0590(13) Uani 1 1 d . . .
H22 H 0.0766 0.8788 0.1927 0.071 Uiso 1 1 calc R . .
C23 C 0.07473(16) 1.1252(5) 0.18077(18) 0.0556(13) Uani 1 1 d . . .
H23 H 0.0810 1.1209 0.1468 0.067 Uiso 1 1 calc R . .
C24 C 0.06814(16) 1.2730(6) 0.20327(17) 0.0527(12) Uani 1 1 d U . .
C25 C 0.05777(17) 1.2827(6) 0.25408(18) 0.0636(13) Uani 1 1 d U . .
H25 H 0.0521 1.3842 0.2687 0.076 Uiso 1 1 calc R . .
C26 C 0.05578(16) 1.1383(6) 0.28339(19) 0.0629(14) Uani 1 1 d . . .
H26 H 0.0501 1.1433 0.3174 0.075 Uiso 1 1 calc R . .
C27 C 0.07017(19) 1.4316(6) 0.1745(2) 0.0615(14) Uani 1 1 d . . .
C28 C 0.03815(16) 0.2649(5) 0.45156(17) 0.0577(13) Uani 1 1 d . . .
H28A H 0.0341 0.3282 0.4818 0.069 Uiso 1 1 calc R . .
H28B H 0.0698 0.2076 0.4533 0.069 Uiso 1 1 calc R . .
C29 C -0.00411(16) 0.1432(5) 0.44656(16) 0.0446(11) Uani 1 1 d . . .
C30 C -0.04944(17) 0.1780(5) 0.46838(16) 0.0538(12) Uani 1 1 d . . .
H30 H -0.0543 0.2783 0.4840 0.065 Uiso 1 1 calc R . .
C31 C -0.08763(16) 0.0646(5) 0.46717(16) 0.0468(11) Uani 1 1 d . . .
H31 H -0.1179 0.0887 0.4824 0.056 Uiso 1 1 calc R . .
C32 C -0.08126(15) -0.0851(5) 0.44351(14) 0.0371(10) Uani 1 1 d . . .
C33 C -0.03584(16) -0.1191(5) 0.42116(16) 0.0505(12) Uani 1 1 d . . .
H33 H -0.0310 -0.2179 0.4047 0.061 Uiso 1 1 calc R . .
C34 C 0.00231(16) -0.0048(5) 0.42347(16) 0.0522(12) Uani 1 1 d . . .
H34 H 0.0330 -0.0290 0.4090 0.063 Uiso 1 1 calc R . .
C35 C -0.12251(16) -0.2110(5) 0.44459(16) 0.0438(11) Uani 1 1 d U . .
Mn1 Mn 0.27735(2) 0.80472(6) 0.507536(19) 0.02861(17) Uani 1 1 d . . .
N1 N 0.24857(12) 0.8294(4) 0.58341(11) 0.0383(8) Uani 1 1 d . . .
N2 N 0.24429(12) 0.9060(4) 0.66264(11) 0.0389(9) Uani 1 1 d . . .
N3 N 0.29483(11) 0.7578(4) 0.42755(11) 0.0345(8) Uani 1 1 d . . .
N4 N 0.29737(12) 0.8152(4) 0.34673(11) 0.0353(8) Uani 1 1 d . . .
O1 O 0.03756(10) 0.3707(3) 0.40963(11) 0.0560(9) Uani 1 1 d . . .
O2 O 0.10136(10) 0.8335(3) 0.32335(10) 0.0544(8) Uani 1 1 d U . .
O3 O -0.11853(12) -0.3367(4) 0.41939(14) 0.0816(12) Uani 1 1 d . . .
O4 O -0.15887(10) -0.1770(3) 0.47300(10) 0.0503(8) Uani 1 1 d U . .
O5 O 0.09075(16) 1.4152(4) 0.13088(14) 0.0820(11) Uani 1 1 d . . .
H5A H 0.0911 1.5041 0.1167 0.123 Uiso 1 1 calc R . .
O6 O 0.05642(16) 1.5615(4) 0.19120(15) 0.1040(14) Uani 1 1 d . . .
O7 O 0.20240(9) 0.8134(3) 0.47606(9) 0.0376(7) Uani 1 1 d . . .
O8 O 0.20408(10) 0.5537(3) 0.49876(9) 0.0428(7) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.341(5) . ?
C1 N1 1.367(5) . ?
C1 H1 0.9300 . ?
C2 N2 1.374(5) . ?
C2 H2 0.9300 . ?
C3 N1 1.311(4) . ?
C3 N2 1.340(4) . ?
C3 H3 0.9300 . ?
C4 C6 1.378(5) . ?
C4 C5 1.384(5) . ?
C4 N2 1.424(4) . ?
C5 C11 1.377(5) 8_576 ?
C5 H5 0.9300 . ?
C6 C12 1.389(5) 8_576 ?
C6 H6 0.9300 . ?
C7 C8 1.353(5) . ?
C7 N3 1.370(4) . ?
C7 H7 0.9300 . ?
C8 N4 1.369(4) . ?
C8 H8 0.9300 . ?
C9 N3 1.316(4) . ?
C9 N4 1.345(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.379(5) . ?
C10 C12 1.382(5) . ?
C10 N4 1.425(4) . ?
C11 C5 1.377(5) 8_575 ?
C11 H11 0.9300 . ?
C12 C6 1.389(5) 8_575 ?
C12 H12 0.9300 . ?
C13 O7 1.260(4) . ?
C13 O8 1.268(4) . ?
C13 C14 1.508(5) . ?
C14 C19 1.375(5) . ?
C14 C15 1.397(5) . ?
C15 C16 1.382(5) . ?
C15 H15 0.9300 . ?
C16 O1 1.371(4) . ?
C16 C17 1.390(5) . ?
C17 C18 1.381(5) . ?
C17 H17 0.9300 . ?
C18 O2 1.380(4) . ?
C18 C19 1.383(5) . ?
C19 H19 0.9300 . ?
C20 O2 1.442(4) . ?
C20 C21 1.526(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.396(6) . ?
C21 C26 1.405(6) . ?
C22 C23 1.403(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.362(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.398(6) . ?
C24 C27 1.511(6) . ?
C25 C26 1.420(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O6 1.210(5) . ?
C27 O5 1.304(5) . ?
C28 O1 1.422(4) . ?
C28 C29 1.512(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C34 1.370(5) . ?
C29 C30 1.378(5) . ?
C30 C31 1.380(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.385(5) . ?
C32 C35 1.509(5) . ?
C33 C34 1.385(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 O3 1.236(4) . ?
C35 O4 1.269(5) . ?
Mn1 O4 2.069(3) 3_556 ?
Mn1 O8 2.107(2) 7_665 ?
Mn1 O7 2.180(2) . ?
Mn1 N1 2.193(3) . ?
Mn1 N3 2.237(3) . ?
O4 Mn1 2.069(3) 3_456 ?
O5 H5A 0.8200 . ?
O8 Mn1 2.107(2) 7_655 ?

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
C2 C1 N1 110.7(4) . . ?
C2 C1 H1 124.7 . . ?
N1 C1 H1 124.7 . . ?
C1 C2 N2 107.0(4) . . ?
C1 C2 H2 126.5 . . ?
N2 C2 H2 126.5 . . ?
N1 C3 N2 114.3(4) . . ?
N1 C3 H3 122.9 . . ?
N2 C3 H3 122.9 . . ?
C6 C4 C5 119.1(4) . . ?
C6 C4 N2 120.6(4) . . ?
C5 C4 N2 120.3(4) . . ?
C11 C5 C4 119.9(4) 8_576 . ?
C11 C5 H5 120.0 8_576 . ?
C4 C5 H5 120.0 . . ?
C4 C6 C12 120.7(4) . 8_576 ?
C4 C6 H6 119.7 . . ?
C12 C6 H6 119.7 8_576 . ?
C8 C7 N3 111.3(4) . . ?
C8 C7 H7 124.3 . . ?
N3 C7 H7 124.3 . . ?
C7 C8 N4 105.9(3) . . ?
C7 C8 H8 127.0 . . ?
N4 C8 H8 127.0 . . ?
N3 C9 N4 113.7(3) . . ?
N3 C9 H9 123.2 . . ?
N4 C9 H9 123.2 . . ?
C11 C10 C12 118.5(4) . . ?
C11 C10 N4 121.6(4) . . ?
C12 C10 N4 119.8(4) . . ?
C5 C11 C10 121.5(4) 8_575 . ?
C5 C11 H11 119.2 8_575 . ?
C10 C11 H11 119.2 . . ?
C10 C12 C6 120.3(4) . 8_575 ?
C10 C12 H12 119.9 . . ?
C6 C12 H12 119.9 8_575 . ?
O7 C13 O8 121.7(3) . . ?
O7 C13 C14 116.9(3) . . ?
O8 C13 C14 121.5(3) . . ?
C19 C14 C15 120.4(3) . . ?
C19 C14 C13 118.3(3) . . ?
C15 C14 C13 121.3(3) . . ?
C16 C15 C14 118.1(3) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
O1 C16 C15 124.4(3) . . ?
O1 C16 C17 113.7(3) . . ?
C15 C16 C17 121.9(4) . . ?
C18 C17 C16 119.1(4) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
O2 C18 C17 124.4(3) . . ?
O2 C18 C19 115.9(3) . . ?
C17 C18 C19 119.7(4) . . ?
C14 C19 C18 120.9(4) . . ?
C14 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
O2 C20 C21 106.3(3) . . ?
O2 C20 H20A 110.5 . . ?
C21 C20 H20A 110.5 . . ?
O2 C20 H20B 110.5 . . ?
C21 C20 H20B 110.5 . . ?
H20A C20 H20B 108.7 . . ?
C22 C21 C26 121.4(5) . . ?
C22 C21 C20 120.9(5) . . ?
C26 C21 C20 117.7(5) . . ?
C21 C22 C23 119.1(5) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 120.7(5) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 120.8(5) . . ?
C23 C24 C27 121.8(5) . . ?
C25 C24 C27 117.4(5) . . ?
C24 C25 C26 120.3(5) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 117.7(5) . . ?
C21 C26 H26 121.2 . . ?
C25 C26 H26 121.2 . . ?
O6 C27 O5 123.6(5) . . ?
O6 C27 C24 123.3(5) . . ?
O5 C27 C24 112.9(5) . . ?
O1 C28 C29 108.7(3) . . ?
O1 C28 H28A 110.0 . . ?
C29 C28 H28A 110.0 . . ?
O1 C28 H28B 110.0 . . ?
C29 C28 H28B 110.0 . . ?
H28A C28 H28B 108.3 . . ?
C34 C29 C30 119.0(4) . . ?
C34 C29 C28 121.8(4) . . ?
C30 C29 C28 119.1(4) . . ?
C29 C30 C31 120.3(4) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 118.9(4) . . ?
C33 C32 C35 121.0(4) . . ?
C31 C32 C35 120.1(4) . . ?
C32 C33 C34 119.6(4) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C29 C34 C33 121.5(4) . . ?
C29 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
O3 C35 O4 125.4(4) . . ?
O3 C35 C32 119.5(4) . . ?
O4 C35 C32 115.1(4) . . ?
O4 Mn1 O8 108.68(11) 3_556 7_665 ?
O4 Mn1 O7 151.04(11) 3_556 . ?
O8 Mn1 O7 98.19(10) 7_665 . ?
O4 Mn1 N1 95.76(11) 3_556 . ?
O8 Mn1 N1 95.68(11) 7_665 . ?
O7 Mn1 N1 92.04(11) . . ?
O4 Mn1 N3 89.13(11) 3_556 . ?
O8 Mn1 N3 90.45(10) 7_665 . ?
O7 Mn1 N3 79.86(10) . . ?
N1 Mn1 N3 170.49(12) . . ?
C3 N1 C1 103.5(3) . . ?
C3 N1 Mn1 126.6(3) . . ?
C1 N1 Mn1 129.6(3) . . ?
C3 N2 C2 104.5(3) . . ?
C3 N2 C4 128.6(4) . . ?
C2 N2 C4 126.9(3) . . ?
C9 N3 C7 103.3(3) . . ?
C9 N3 Mn1 123.2(2) . . ?
C7 N3 Mn1 132.5(3) . . ?
C9 N4 C8 105.8(3) . . ?
C9 N4 C10 126.7(3) . . ?
C8 N4 C10 127.5(3) . . ?
C16 O1 C28 117.0(3) . . ?
C18 O2 C20 118.1(3) . . ?
C35 O4 Mn1 132.5(3) . 3_456 ?
C27 O5 H5A 109.5 . . ?
C13 O7 Mn1 108.5(2) . . ?
C13 O8 Mn1 150.4(2) . 7_655 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 986467'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H26 Fe N4 O8'
_chemical_formula_weight         686.45

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   26.4977(19)
_cell_length_b                   8.1948(6)
_cell_length_c                   26.8556(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5831.5(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4201
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      22.48

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2832
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_T_max  0.8874
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_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            28865
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5189
_reflns_number_gt                3315
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0394P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5189
_refine_ls_number_parameters     434
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.27653(11) 0.1528(4) 0.89213(11) 0.0339(8) Uani 1 1 d . . .
H1 H 0.2513 0.0754 0.8968 0.041 Uiso 1 1 calc R . .
C2 C 0.33108(12) 0.3370(4) 0.90588(12) 0.0384(8) Uani 1 1 d . . .
H2 H 0.3512 0.4132 0.9221 0.046 Uiso 1 1 calc R . .
C3 C 0.33269(12) 0.3044(4) 0.85590(12) 0.0428(9) Uani 1 1 d . . .
H3 H 0.3536 0.3531 0.8324 0.051 Uiso 1 1 calc R . .
C4 C 0.28432(12) 0.1129(4) 0.80013(11) 0.0363(8) Uani 1 1 d . . .
C5 C 0.32008(12) 0.0449(4) 0.76962(12) 0.0469(9) Uani 1 1 d . . .
H5 H 0.3537 0.0458 0.7796 0.056 Uiso 1 1 calc R . .
C6 C 0.23505(12) 0.1108(4) 0.78535(12) 0.0442(9) Uani 1 1 d . . .
H6 H 0.2103 0.1556 0.8057 0.053 Uiso 1 1 calc R . .
C7 C 0.20250(13) 0.2046(5) 1.10063(13) 0.0513(10) Uani 1 1 d . . .
H7 H 0.1765 0.2526 1.0826 0.062 Uiso 1 1 calc R . .
C8 C 0.19929(13) 0.1578(5) 1.14891(13) 0.0535(10) Uani 1 1 d . . .
H8 H 0.1712 0.1679 1.1694 0.064 Uiso 1 1 calc R . .
C9 C 0.27302(12) 0.1060(4) 1.12013(12) 0.0428(9) Uani 1 1 d . . .
H9 H 0.3064 0.0714 1.1185 0.051 Uiso 1 1 calc R . .
C10 C 0.25793(12) 0.0248(4) 1.20910(11) 0.0373(8) Uani 1 1 d . . .
C11 C 0.22185(12) -0.0415(4) 1.23972(11) 0.0432(9) Uani 1 1 d . . .
H11 H 0.1882 -0.0402 1.2299 0.052 Uiso 1 1 calc R . .
C12 C 0.30762(12) 0.0249(4) 1.22443(12) 0.0496(10) Uani 1 1 d . . .
H12 H 0.3325 0.0715 1.2045 0.060 Uiso 1 1 calc R . .
C13 C 0.18768(11) 0.3403(4) 0.97437(11) 0.0298(7) Uani 1 1 d . . .
C14 C 0.14491(10) 0.3657(3) 0.93809(11) 0.0269(7) Uani 1 1 d . . .
C15 C 0.14070(11) 0.2601(4) 0.89792(11) 0.0316(8) Uani 1 1 d . . .
H15 H 0.1640 0.1761 0.8942 0.038 Uiso 1 1 calc R . .
C16 C 0.10239(11) 0.2781(4) 0.86340(11) 0.0337(8) Uani 1 1 d . . .
C17 C 0.06808(11) 0.4022(4) 0.86885(11) 0.0346(8) Uani 1 1 d . . .
H17 H 0.0421 0.4155 0.8459 0.042 Uiso 1 1 calc R . .
C18 C 0.07258(11) 0.5082(4) 0.90933(11) 0.0334(8) Uani 1 1 d . . .
C19 C 0.11062(10) 0.4925(4) 0.94417(11) 0.0316(8) Uani 1 1 d . . .
H19 H 0.1132 0.5644 0.9708 0.038 Uiso 1 1 calc R . .
C20 C 0.03726(13) 0.7352(4) 0.95227(14) 0.0538(10) Uani 1 1 d . . .
H20A H 0.0692 0.7931 0.9536 0.065 Uiso 1 1 calc R . .
H20B H 0.0336 0.6728 0.9827 0.065 Uiso 1 1 calc R . .
C21 C -0.00538(12) 0.8550(4) 0.94772(13) 0.0409(9) Uani 1 1 d . . .
C22 C 0.00124(12) 1.0037(4) 0.92393(13) 0.0460(9) Uani 1 1 d . . .
H22 H 0.0321 1.0274 0.9091 0.055 Uiso 1 1 calc R . .
C23 C -0.03728(12) 1.1176(4) 0.92180(12) 0.0444(9) Uani 1 1 d . . .
H23 H -0.0324 1.2165 0.9055 0.053 Uiso 1 1 calc R . .
C24 C -0.08281(11) 1.0831(4) 0.94395(11) 0.0332(8) Uani 1 1 d . . .
C25 C -0.08921(12) 0.9331(4) 0.96751(12) 0.0416(9) Uani 1 1 d . . .
H25 H -0.1199 0.9091 0.9827 0.050 Uiso 1 1 calc R . .
C26 C -0.05100(13) 0.8202(4) 0.96877(13) 0.0461(9) Uani 1 1 d . . .
H26 H -0.0562 0.7196 0.9840 0.055 Uiso 1 1 calc R . .
C27 C -0.12367(12) 1.2090(4) 0.94560(12) 0.0371(8) Uani 1 1 d . . .
C28 C 0.05944(13) 0.1644(5) 0.79154(14) 0.0618(11) Uani 1 1 d U . .
H28A H 0.0609 0.2601 0.7703 0.074 Uiso 1 1 calc R . .
H28B H 0.0279 0.1665 0.8098 0.074 Uiso 1 1 calc R . .
C29 C 0.06285(12) 0.0106(5) 0.76041(14) 0.0515(10) Uani 1 1 d . . .
C30 C 0.05562(13) -0.1404(5) 0.78431(15) 0.0586(11) Uani 1 1 d . . .
H30 H 0.0494 -0.1457 0.8183 0.070 Uiso 1 1 calc R . .
C31 C 0.05806(13) -0.2833(5) 0.75517(14) 0.0596(11) Uani 1 1 d . . .
H31 H 0.0528 -0.3844 0.7701 0.072 Uiso 1 1 calc R . .
C32 C 0.06833(12) -0.2748(5) 0.70383(13) 0.0473(9) Uani 1 1 d . . .
C33 C 0.07522(12) -0.1273(4) 0.68128(14) 0.0500(10) Uani 1 1 d . . .
H33 H 0.0818 -0.1223 0.6473 0.060 Uiso 1 1 calc R . .
C34 C 0.07245(12) 0.0170(5) 0.70941(14) 0.0534(10) Uani 1 1 d . . .
H34 H 0.0770 0.1174 0.6939 0.064 Uiso 1 1 calc R . .
C35 C 0.07073(14) -0.4324(5) 0.67481(16) 0.0569(11) Uani 1 1 d . . .
Fe1 Fe 0.276903(15) 0.20408(5) 1.007472(15) 0.02695(13) Uani 1 1 d . . .
N1 N 0.29562(9) 0.2413(3) 0.92851(9) 0.0309(6) Uani 1 1 d . . .
N2 N 0.29741(9) 0.1861(3) 0.84736(9) 0.0350(6) Uani 1 1 d . . .
N3 N 0.24935(9) 0.1713(3) 1.08221(9) 0.0347(6) Uani 1 1 d . . .
N4 N 0.24466(10) 0.0934(3) 1.16190(9) 0.0370(7) Uani 1 1 d . . .
O1 O 0.20605(8) 0.4558(3) 0.99952(7) 0.0409(6) Uani 1 1 d . . .
O2 O 0.20452(7) 0.1962(3) 0.97772(7) 0.0343(5) Uani 1 1 d . . .
O3 O 0.10117(8) 0.1638(3) 0.82529(9) 0.0521(7) Uani 1 1 d U . .
O4 O 0.03666(8) 0.6280(3) 0.91034(8) 0.0497(7) Uani 1 1 d . . .
O5 O 0.05685(12) -0.5625(4) 0.69101(12) 0.0938(10) Uani 1 1 d . . .
O6 O 0.09112(12) -0.4151(3) 0.63069(10) 0.0717(8) Uani 1 1 d . . .
H6A H 0.0924 -0.5041 0.6168 0.108 Uiso 1 1 calc R . .
O7 O -0.11905(9) 1.3373(3) 0.92191(11) 0.0694(8) Uani 1 1 d . . .
O8 O -0.16117(8) 1.1731(3) 0.97292(8) 0.0439(6) 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 1.318(4) . ?
C1 N2 1.351(4) . ?
C1 H1 0.9300 . ?
C2 N1 1.366(4) . ?
C2 C3 1.369(4) . ?
C2 H2 0.9300 . ?
C3 N2 1.366(4) . ?
C3 H3 0.9300 . ?
C4 C6 1.365(4) . ?
C4 C5 1.371(4) . ?
C4 N2 1.445(4) . ?
C5 C12 1.382(4) 7 ?
C5 H5 0.9300 . ?
C6 C11 1.395(4) 7 ?
C6 H6 0.9300 . ?
C7 C8 1.355(4) . ?
C7 N3 1.364(4) . ?
C7 H7 0.9300 . ?
C8 N4 1.359(4) . ?
C8 H8 0.9300 . ?
C9 N3 1.310(4) . ?
C9 N4 1.354(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(4) . ?
C10 C12 1.380(4) . ?
C10 N4 1.430(4) . ?
C11 C6 1.395(4) 7_556 ?
C11 H11 0.9300 . ?
C12 C5 1.382(4) 7_556 ?
C12 H12 0.9300 . ?
C13 O1 1.261(3) . ?
C13 O2 1.266(3) . ?
C13 C14 1.509(4) . ?
C14 C15 1.388(4) . ?
C14 C19 1.390(4) . ?
C15 C16 1.383(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.372(4) . ?
C16 O3 1.388(3) . ?
C17 C18 1.397(4) . ?
C17 H17 0.9300 . ?
C18 O4 1.368(3) . ?
C18 C19 1.381(4) . ?
C19 H19 0.9300 . ?
C20 O4 1.429(4) . ?
C20 C21 1.502(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C26 1.364(4) . ?
C21 C22 1.387(4) . ?
C22 C23 1.384(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(4) . ?
C24 C27 1.496(4) . ?
C25 C26 1.372(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O7 1.235(4) . ?
C27 O8 1.270(4) . ?
C28 O3 1.430(4) . ?
C28 C29 1.515(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C34 1.394(5) . ?
C29 C30 1.407(5) . ?
C30 C31 1.410(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.407(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.364(5) . ?
C32 C35 1.510(5) . ?
C33 C34 1.405(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 O5 1.209(4) . ?
C35 O6 1.310(4) . ?
Fe1 O8 1.996(2) 4_567 ?
Fe1 O2 2.0788(19) . ?
Fe1 O1 2.095(2) 8_655 ?
Fe1 N3 2.153(2) . ?
Fe1 N1 2.199(2) . ?
O1 Fe1 2.095(2) 8_665 ?
O6 H6A 0.8200 . ?
O8 Fe1 1.996(2) 4_467 ?

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 N2 113.0(3) . . ?
N1 C1 H1 123.5 . . ?
N2 C1 H1 123.5 . . ?
N1 C2 C3 110.2(3) . . ?
N1 C2 H2 124.9 . . ?
C3 C2 H2 124.9 . . ?
N2 C3 C2 106.4(3) . . ?
N2 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
C6 C4 C5 118.8(3) . . ?
C6 C4 N2 119.3(3) . . ?
C5 C4 N2 121.8(3) . . ?
C4 C5 C12 121.9(3) . 7 ?
C4 C5 H5 119.1 . . ?
C12 C5 H5 119.1 7 . ?
C4 C6 C11 120.0(3) . 7 ?
C4 C6 H6 120.0 . . ?
C11 C6 H6 120.0 7 . ?
C8 C7 N3 110.3(3) . . ?
C8 C7 H7 124.8 . . ?
N3 C7 H7 124.8 . . ?
C7 C8 N4 107.5(3) . . ?
C7 C8 H8 126.3 . . ?
N4 C8 H8 126.3 . . ?
N3 C9 N4 114.2(3) . . ?
N3 C9 H9 122.9 . . ?
N4 C9 H9 122.9 . . ?
C11 C10 C12 119.1(3) . . ?
C11 C10 N4 121.0(3) . . ?
C12 C10 N4 119.9(3) . . ?
C10 C11 C6 120.8(3) . 7_556 ?
C10 C11 H11 119.6 . . ?
C6 C11 H11 119.6 7_556 . ?
C10 C12 C5 119.3(3) . 7_556 ?
C10 C12 H12 120.3 . . ?
C5 C12 H12 120.3 7_556 . ?
O1 C13 O2 121.7(3) . . ?
O1 C13 C14 122.2(3) . . ?
O2 C13 C14 116.1(3) . . ?
C15 C14 C19 120.3(3) . . ?
C15 C14 C13 118.4(3) . . ?
C19 C14 C13 121.2(3) . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C15 119.6(3) . . ?
C17 C16 O3 124.3(3) . . ?
C15 C16 O3 116.1(3) . . ?
C16 C17 C18 119.2(3) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
O4 C18 C19 124.1(3) . . ?
O4 C18 C17 113.7(3) . . ?
C19 C18 C17 122.1(3) . . ?
C18 C19 C14 117.8(3) . . ?
C18 C19 H19 121.1 . . ?
C14 C19 H19 121.1 . . ?
O4 C20 C21 109.2(3) . . ?
O4 C20 H20A 109.8 . . ?
C21 C20 H20A 109.8 . . ?
O4 C20 H20B 109.8 . . ?
C21 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
C26 C21 C22 119.1(3) . . ?
C26 C21 C20 119.7(3) . . ?
C22 C21 C20 121.1(3) . . ?
C23 C22 C21 121.2(3) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 119.0(3) . . ?
C23 C24 C27 120.4(3) . . ?
C25 C24 C27 120.5(3) . . ?
C26 C25 C24 121.1(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C21 C26 C25 120.1(3) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
O7 C27 O8 124.9(3) . . ?
O7 C27 C24 120.0(3) . . ?
O8 C27 C24 115.1(3) . . ?
O3 C28 C29 107.5(3) . . ?
O3 C28 H28A 110.2 . . ?
C29 C28 H28A 110.2 . . ?
O3 C28 H28B 110.2 . . ?
C29 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
C34 C29 C30 120.4(4) . . ?
C34 C29 C28 121.4(4) . . ?
C30 C29 C28 118.2(4) . . ?
C29 C30 C31 118.1(4) . . ?
C29 C30 H30 120.9 . . ?
C31 C30 H30 120.9 . . ?
C32 C31 C30 120.7(4) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C33 C32 C31 120.3(4) . . ?
C33 C32 C35 121.5(3) . . ?
C31 C32 C35 118.1(4) . . ?
C32 C33 C34 120.0(4) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C29 C34 C33 120.4(4) . . ?
C29 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
O5 C35 O6 123.1(4) . . ?
O5 C35 C32 123.8(4) . . ?
O6 C35 C32 113.1(4) . . ?
O8 Fe1 O2 151.13(9) 4_567 . ?
O8 Fe1 O1 109.85(9) 4_567 8_655 ?
O2 Fe1 O1 97.44(8) . 8_655 ?
O8 Fe1 N3 95.50(9) 4_567 . ?
O2 Fe1 N3 92.38(9) . . ?
O1 Fe1 N3 92.68(9) 8_655 . ?
O8 Fe1 N1 89.94(9) 4_567 . ?
O2 Fe1 N1 80.90(8) . . ?
O1 Fe1 N1 89.30(8) 8_655 . ?
N3 Fe1 N1 173.19(9) . . ?
C1 N1 C2 104.5(3) . . ?
C1 N1 Fe1 123.5(2) . . ?
C2 N1 Fe1 131.6(2) . . ?
C1 N2 C3 105.9(3) . . ?
C1 N2 C4 126.8(3) . . ?
C3 N2 C4 127.3(3) . . ?
C9 N3 C7 103.6(3) . . ?
C9 N3 Fe1 127.8(2) . . ?
C7 N3 Fe1 128.4(2) . . ?
C9 N4 C8 104.4(3) . . ?
C9 N4 C10 128.9(3) . . ?
C8 N4 C10 126.7(3) . . ?
C13 O1 Fe1 150.1(2) . 8_665 ?
C13 O2 Fe1 108.88(19) . . ?
C16 O3 C28 118.9(2) . . ?
C18 O4 C20 116.7(2) . . ?
C35 O6 H6A 109.5 . . ?
C27 O8 Fe1 132.8(2) . 4_467 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 986468'
