# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1523199'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H14 Fe N2 O2'
_chemical_formula_sum            'C16 H14 Fe N2 O2'
_chemical_formula_weight         322.14

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'
Fe Fe 0.3463 0.8444 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   13.66(3)
_cell_length_b                   19.02(4)
_cell_length_c                   10.88(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2825(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4151
_cell_measurement_theta_min      2.630
_cell_measurement_theta_max      24.904

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.164
_exptl_absorpt_coefficient_mu    1.072
_shelx_estimated_absorpt_T_min   0.731
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17776
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.836
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_point_group_measured_fraction_full 0.949
_reflns_number_total             6214
_reflns_number_gt                4628
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_max     0.796
_reflns_Friedel_fraction_full    0.892

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0379P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6214
_refine_ls_number_parameters     387
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.0898
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_restrained_S_all      0.921
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.66261(4) 0.19274(3) 0.77031(7) 0.03640(16) Uani 1 1 d . . . . .
O1 O 0.6568(3) 0.38321(19) 0.9412(3) 0.0599(10) Uani 1 1 d . . . . .
O2 O 0.4710(3) 0.38474(19) 0.5665(3) 0.0570(9) Uani 1 1 d . . . . .
N1 N 0.5773(3) 0.3739(2) 0.7559(5) 0.0455(10) Uani 1 1 d . . . . .
N2 N 0.4534(3) 0.4311(2) 0.6552(4) 0.0412(9) Uani 1 1 d . . . . .
C1 C 0.6465(4) 0.3540(2) 0.8429(5) 0.0420(12) Uani 1 1 d . . . . .
C2 C 0.7090(4) 0.2943(2) 0.8011(4) 0.0422(13) Uani 1 1 d . . . . .
C3 C 0.7609(4) 0.2471(3) 0.8795(6) 0.0471(14) Uani 1 1 d . . . . .
H3 H 0.7602 0.2483 0.9696 0.057 Uiso 1 1 calc R U . . .
C4 C 0.8115(4) 0.1969(3) 0.8063(5) 0.0516(17) Uani 1 1 d . . . . .
H4 H 0.8521 0.1582 0.8366 0.062 Uiso 1 1 calc R U . . .
C5 C 0.7911(4) 0.2131(3) 0.6785(6) 0.0508(15) Uani 1 1 d . . . . .
H5 H 0.8161 0.1874 0.6069 0.061 Uiso 1 1 calc R U . . .
C6 C 0.7279(4) 0.2724(3) 0.6754(5) 0.0447(13) Uani 1 1 d . . . . .
H6 H 0.7021 0.2950 0.6011 0.054 Uiso 1 1 calc R U . . .
C7 C 0.5174(4) 0.1815(3) 0.8168(6) 0.0515(17) Uani 1 1 d . . . . .
H7 H 0.4768 0.2175 0.8564 0.062 Uiso 1 1 calc R U . . .
C8 C 0.5298(4) 0.1728(4) 0.6875(7) 0.0588(18) Uani 1 1 d . . . . .
H8 H 0.4988 0.2009 0.6228 0.071 Uiso 1 1 calc R U . . .
C9 C 0.5942(5) 0.1155(3) 0.6702(6) 0.0637(18) Uani 1 1 d . . . . .
H9 H 0.6161 0.0970 0.5907 0.076 Uiso 1 1 calc R U . . .
C10 C 0.6224(4) 0.0892(3) 0.7888(6) 0.0587(16) Uani 1 1 d . . . . .
H10 H 0.6666 0.0496 0.8045 0.070 Uiso 1 1 calc R U . . .
C11 C 0.5744(5) 0.1304(3) 0.8789(6) 0.0565(16) Uani 1 1 d . . . . .
H11 H 0.5797 0.1246 0.9682 0.068 Uiso 1 1 calc R U . . .
C12 C 0.5101(3) 0.4279(2) 0.7611(6) 0.0388(10) Uani 1 1 d . . . . .
C13 C 0.4943(4) 0.4758(3) 0.8540(5) 0.0473(13) Uani 1 1 d . . . . .
H13 H 0.5314 0.4735 0.9256 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4229(4) 0.5279(3) 0.8411(5) 0.0507(14) Uani 1 1 d . . . . .
H14 H 0.4130 0.5610 0.9027 0.061 Uiso 1 1 calc R U . . .
C15 C 0.3673(4) 0.5293(3) 0.7355(5) 0.0543(15) Uani 1 1 d . . . . .
H15 H 0.3195 0.5636 0.7256 0.065 Uiso 1 1 calc R U . . .
C16 C 0.3822(4) 0.4801(3) 0.6446(5) 0.0524(13) Uani 1 1 d . . . . .
H16 H 0.3427 0.4806 0.5749 0.063 Uiso 1 1 calc R U . . .
Fe2 Fe 0.47459(4) 0.19066(3) 0.25999(7) 0.03712(17) Uani 1 1 d . . . . .
O3 O 0.4173(3) 0.3516(2) 0.0619(4) 0.0684(11) Uani 1 1 d . . . . .
O4 O 0.2519(3) 0.4167(2) 0.4308(4) 0.0650(11) Uani 1 1 d . . . . .
N3 N 0.3689(3) 0.3798(2) 0.2570(5) 0.0438(10) Uani 1 1 d . . . . .
N4 N 0.2437(3) 0.4512(2) 0.3270(4) 0.0486(11) Uani 1 1 d . . . . .
C17 C 0.4268(4) 0.3436(2) 0.1728(5) 0.0414(12) Uani 1 1 d . . . . .
C18 C 0.5007(4) 0.2947(2) 0.2250(5) 0.0379(13) Uani 1 1 d . . . . .
C19 C 0.5259(4) 0.2782(3) 0.3499(5) 0.0443(13) Uani 1 1 d . . . . .
H19 H 0.4972 0.2995 0.4236 0.053 Uiso 1 1 calc R U . . .
C20 C 0.5990(4) 0.2248(3) 0.3480(5) 0.0483(14) Uani 1 1 d . . . . .
H20 H 0.6294 0.2029 0.4200 0.058 Uiso 1 1 calc R U . . .
C21 C 0.6203(4) 0.2092(3) 0.2228(6) 0.0506(16) Uani 1 1 d . . . . .
H21 H 0.6677 0.1742 0.1939 0.061 Uiso 1 1 calc R U . . .
C22 C 0.5604(4) 0.2520(2) 0.1469(5) 0.0425(12) Uani 1 1 d . . . . .
H22 H 0.5595 0.2518 0.0569 0.051 Uiso 1 1 calc R U . . .
C23 C 0.3279(4) 0.1721(3) 0.2419(10) 0.080(3) Uani 1 1 d . . . . .
H23 H 0.2777 0.2076 0.2248 0.096 Uiso 1 1 calc R U . . .
C24 C 0.3797(5) 0.1326(3) 0.1526(7) 0.0653(19) Uani 1 1 d . . . . .
H24 H 0.3721 0.1358 0.0632 0.078 Uiso 1 1 calc R U . . .
C25 C 0.4438(5) 0.0875(3) 0.2169(7) 0.065(2) Uani 1 1 d . . . . .
H25 H 0.4896 0.0541 0.1792 0.078 Uiso 1 1 calc R U . . .
C26 C 0.4329(5) 0.0993(3) 0.3439(7) 0.070(2) Uani 1 1 d . . . . .
H26 H 0.4683 0.0749 0.4098 0.084 Uiso 1 1 calc R U . . .
C27 C 0.3604(6) 0.1516(4) 0.3592(7) 0.078(2) Uani 1 1 d . . . . .
H27 H 0.3365 0.1700 0.4379 0.094 Uiso 1 1 calc R U . . .
C28 C 0.3028(4) 0.4329(2) 0.2285(4) 0.0417(13) Uani 1 1 d . . . . .
C29 C 0.2921(4) 0.4670(3) 0.1179(6) 0.0632(16) Uani 1 1 d . . . . .
H29 H 0.3306 0.4539 0.0512 0.076 Uiso 1 1 calc R U . . .
C30 C 0.2245(5) 0.5206(3) 0.1050(7) 0.0755(19) Uani 1 1 d . . . . .
H30 H 0.2177 0.5437 0.0301 0.091 Uiso 1 1 calc R U . . .
C31 C 0.1674(5) 0.5394(3) 0.2035(7) 0.074(2) Uani 1 1 d . . . . .
H31 H 0.1215 0.5753 0.1958 0.088 Uiso 1 1 calc R U . . .
C32 C 0.1784(4) 0.5054(3) 0.3123(6) 0.0639(19) Uani 1 1 d . . . . .
H32 H 0.1404 0.5192 0.3790 0.077 Uiso 1 1 calc R U . . .
H3A H 0.373(3) 0.372(2) 0.327(3) 0.013(12) Uiso 1 1 d . . . . .
H1 H 0.567(3) 0.353(2) 0.695(4) 0.034(14) Uiso 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
Fe1 C6 2.039(6) . ?
Fe1 C9 2.054(6) . ?
Fe1 C10 2.053(6) . ?
Fe1 C7 2.058(7) . ?
Fe1 C5 2.057(6) . ?
Fe1 C8 2.061(7) . ?
Fe1 C11 2.062(6) . ?
Fe1 C2 2.061(6) . ?
Fe1 C3 2.069(6) . ?
Fe1 C4 2.072(7) . ?
O1 C1 1.213(6) . ?
O2 N2 1.329(5) . ?
N1 C12 1.380(6) . ?
N1 C1 1.390(7) . ?
N1 H1 0.78(4) . ?
N2 C16 1.352(6) . ?
N2 C12 1.389(7) . ?
C1 C2 1.491(7) . ?
C2 C3 1.426(7) . ?
C2 C6 1.452(8) . ?
C3 C4 1.422(7) . ?
C3 H3 0.9800 . ?
C4 C5 1.451(9) . ?
C4 H4 0.9800 . ?
C5 C6 1.421(8) . ?
C5 H5 0.9800 . ?
C6 H6 0.9800 . ?
C7 C11 1.417(8) . ?
C7 C8 1.426(8) . ?
C7 H7 0.9800 . ?
C8 C9 1.414(9) . ?
C8 H8 0.9800 . ?
C9 C10 1.436(9) . ?
C9 H9 0.9800 . ?
C10 C11 1.415(8) . ?
C10 H10 0.9800 . ?
C11 H11 0.9800 . ?
C12 C13 1.378(7) . ?
C13 C14 1.397(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.377(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.376(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
Fe2 C27 2.037(7) . ?
Fe2 C26 2.044(7) . ?
Fe2 C23 2.045(7) . ?
Fe2 C18 2.046(6) . ?
Fe2 C20 2.055(6) . ?
Fe2 C19 2.054(6) . ?
Fe2 C25 2.060(7) . ?
Fe2 C22 2.060(5) . ?
Fe2 C21 2.062(7) . ?
Fe2 C24 2.065(7) . ?
O3 C17 1.222(6) . ?
O4 N4 1.310(6) . ?
N3 C28 1.390(6) . ?
N3 C17 1.392(7) . ?
N3 H3A 0.78(4) . ?
N4 C32 1.373(7) . ?
N4 C28 1.385(6) . ?
C17 C18 1.485(7) . ?
C18 C22 1.431(7) . ?
C18 C19 1.437(8) . ?
C19 C20 1.423(7) . ?
C19 H19 0.9800 . ?
C20 C21 1.423(8) . ?
C20 H20 0.9800 . ?
C21 C22 1.418(7) . ?
C21 H21 0.9800 . ?
C22 H22 0.9800 . ?
C23 C27 1.406(11) . ?
C23 C24 1.416(10) . ?
C23 H23 0.9800 . ?
C24 C25 1.412(9) . ?
C24 H24 0.9800 . ?
C25 C26 1.407(8) . ?
C25 H25 0.9800 . ?
C26 C27 1.414(10) . ?
C26 H26 0.9800 . ?
C27 H27 0.9800 . ?
C28 C29 1.375(7) . ?
C29 C30 1.383(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.373(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.357(8) . ?
C31 H31 0.9300 . ?
C32 H32 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
C6 Fe1 C9 117.5(3) . . ?
C6 Fe1 C10 151.5(2) . . ?
C9 Fe1 C10 40.9(3) . . ?
C6 Fe1 C7 128.5(2) . . ?
C9 Fe1 C7 67.5(3) . . ?
C10 Fe1 C7 67.6(2) . . ?
C6 Fe1 C5 40.6(2) . . ?
C9 Fe1 C5 105.4(3) . . ?
C10 Fe1 C5 117.2(2) . . ?
C7 Fe1 C5 164.1(3) . . ?
C6 Fe1 C8 107.5(3) . . ?
C9 Fe1 C8 40.2(3) . . ?
C10 Fe1 C8 68.4(3) . . ?
C7 Fe1 C8 40.5(2) . . ?
C5 Fe1 C8 125.0(3) . . ?
C6 Fe1 C11 166.6(2) . . ?
C9 Fe1 C11 68.1(3) . . ?
C10 Fe1 C11 40.2(2) . . ?
C7 Fe1 C11 40.2(2) . . ?
C5 Fe1 C11 152.3(2) . . ?
C8 Fe1 C11 68.3(3) . . ?
C6 Fe1 C2 41.5(2) . . ?
C9 Fe1 C2 153.8(3) . . ?
C10 Fe1 C2 164.8(2) . . ?
C7 Fe1 C2 110.7(2) . . ?
C5 Fe1 C2 68.9(2) . . ?
C8 Fe1 C2 121.0(3) . . ?
C11 Fe1 C2 128.7(2) . . ?
C6 Fe1 C3 68.6(2) . . ?
C9 Fe1 C3 163.1(3) . . ?
C10 Fe1 C3 126.6(3) . . ?
C7 Fe1 C3 122.4(3) . . ?
C5 Fe1 C3 68.3(3) . . ?
C8 Fe1 C3 156.0(3) . . ?
C11 Fe1 C3 109.7(3) . . ?
C2 Fe1 C3 40.4(2) . . ?
C6 Fe1 C4 68.8(2) . . ?
C9 Fe1 C4 125.0(3) . . ?
C10 Fe1 C4 106.3(2) . . ?
C7 Fe1 C4 154.6(3) . . ?
C5 Fe1 C4 41.1(3) . . ?
C8 Fe1 C4 162.5(3) . . ?
C11 Fe1 C4 119.2(3) . . ?
C2 Fe1 C4 68.4(2) . . ?
C3 Fe1 C4 40.2(2) . . ?
C12 N1 C1 128.9(5) . . ?
C12 N1 H1 107(4) . . ?
C1 N1 H1 124(4) . . ?
O2 N2 C16 121.7(4) . . ?
O2 N2 C12 118.2(4) . . ?
C16 N2 C12 120.1(4) . . ?
O1 C1 N1 123.6(5) . . ?
O1 C1 C2 123.5(5) . . ?
N1 C1 C2 112.9(4) . . ?
C3 C2 C6 107.1(5) . . ?
C3 C2 C1 125.5(5) . . ?
C6 C2 C1 127.4(4) . . ?
C3 C2 Fe1 70.1(3) . . ?
C6 C2 Fe1 68.4(3) . . ?
C1 C2 Fe1 125.9(4) . . ?
C4 C3 C2 109.2(5) . . ?
C4 C3 Fe1 70.0(3) . . ?
C2 C3 Fe1 69.5(3) . . ?
C4 C3 H3 125.4 . . ?
C2 C3 H3 125.4 . . ?
Fe1 C3 H3 125.4 . . ?
C3 C4 C5 107.5(5) . . ?
C3 C4 Fe1 69.8(3) . . ?
C5 C4 Fe1 68.9(4) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 H4 126.2 . . ?
Fe1 C4 H4 126.2 . . ?
C6 C5 C4 107.9(5) . . ?
C6 C5 Fe1 69.0(3) . . ?
C4 C5 Fe1 70.0(4) . . ?
C6 C5 H5 126.0 . . ?
C4 C5 H5 126.0 . . ?
Fe1 C5 H5 126.0 . . ?
C5 C6 C2 108.3(5) . . ?
C5 C6 Fe1 70.4(3) . . ?
C2 C6 Fe1 70.1(3) . . ?
C5 C6 H6 125.9 . . ?
C2 C6 H6 125.9 . . ?
Fe1 C6 H6 125.9 . . ?
C11 C7 C8 109.0(6) . . ?
C11 C7 Fe1 70.0(3) . . ?
C8 C7 Fe1 69.8(4) . . ?
C11 C7 H7 125.5 . . ?
C8 C7 H7 125.5 . . ?
Fe1 C7 H7 125.5 . . ?
C9 C8 C7 107.1(7) . . ?
C9 C8 Fe1 69.7(4) . . ?
C7 C8 Fe1 69.6(4) . . ?
C9 C8 H8 126.4 . . ?
C7 C8 H8 126.4 . . ?
Fe1 C8 H8 126.4 . . ?
C8 C9 C10 108.4(6) . . ?
C8 C9 Fe1 70.2(4) . . ?
C10 C9 Fe1 69.5(3) . . ?
C8 C9 H9 125.8 . . ?
C10 C9 H9 125.8 . . ?
Fe1 C9 H9 125.8 . . ?
C11 C10 C9 107.8(5) . . ?
C11 C10 Fe1 70.2(3) . . ?
C9 C10 Fe1 69.6(3) . . ?
C11 C10 H10 126.1 . . ?
C9 C10 H10 126.1 . . ?
Fe1 C10 H10 126.1 . . ?
C7 C11 C10 107.7(6) . . ?
C7 C11 Fe1 69.7(3) . . ?
C10 C11 Fe1 69.6(3) . . ?
C7 C11 H11 126.1 . . ?
C10 C11 H11 126.1 . . ?
Fe1 C11 H11 126.1 . . ?
C13 C12 N1 128.8(6) . . ?
C13 C12 N2 119.5(4) . . ?
N1 C12 N2 111.7(5) . . ?
C12 C13 C14 120.3(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 118.8(5) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 120.3(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
N2 C16 C15 120.9(5) . . ?
N2 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C27 Fe2 C26 40.6(3) . . ?
C27 Fe2 C23 40.3(3) . . ?
C26 Fe2 C23 67.9(3) . . ?
C27 Fe2 C18 125.8(3) . . ?
C26 Fe2 C18 162.5(3) . . ?
C23 Fe2 C18 108.7(2) . . ?
C27 Fe2 C20 120.1(3) . . ?
C26 Fe2 C20 106.9(3) . . ?
C23 Fe2 C20 155.5(3) . . ?
C18 Fe2 C20 68.7(2) . . ?
C27 Fe2 C19 107.7(3) . . ?
C26 Fe2 C19 124.9(3) . . ?
C23 Fe2 C19 121.4(3) . . ?
C18 Fe2 C19 41.0(2) . . ?
C20 Fe2 C19 40.5(2) . . ?
C27 Fe2 C25 67.5(3) . . ?
C26 Fe2 C25 40.1(2) . . ?
C23 Fe2 C25 67.3(3) . . ?
C18 Fe2 C25 156.1(3) . . ?
C20 Fe2 C25 125.1(3) . . ?
C19 Fe2 C25 161.7(2) . . ?
C27 Fe2 C22 163.4(3) . . ?
C26 Fe2 C22 155.0(3) . . ?
C23 Fe2 C22 126.7(3) . . ?
C18 Fe2 C22 40.78(19) . . ?
C20 Fe2 C22 68.2(3) . . ?
C19 Fe2 C22 68.4(2) . . ?
C25 Fe2 C22 121.3(3) . . ?
C27 Fe2 C21 154.9(3) . . ?
C26 Fe2 C21 120.1(3) . . ?
C23 Fe2 C21 163.2(3) . . ?
C18 Fe2 C21 68.3(2) . . ?
C20 Fe2 C21 40.4(2) . . ?
C19 Fe2 C21 68.0(2) . . ?
C25 Fe2 C21 108.4(3) . . ?
C22 Fe2 C21 40.2(2) . . ?
C27 Fe2 C24 67.9(3) . . ?
C26 Fe2 C24 67.9(3) . . ?
C23 Fe2 C24 40.3(3) . . ?
C18 Fe2 C24 121.4(2) . . ?
C20 Fe2 C24 162.1(3) . . ?
C19 Fe2 C24 156.5(2) . . ?
C25 Fe2 C24 40.0(2) . . ?
C22 Fe2 C24 108.8(3) . . ?
C21 Fe2 C24 125.9(3) . . ?
C28 N3 C17 125.5(5) . . ?
C28 N3 H3A 113(3) . . ?
C17 N3 H3A 121(3) . . ?
O4 N4 C32 122.1(5) . . ?
O4 N4 C28 119.4(4) . . ?
C32 N4 C28 118.5(5) . . ?
O3 C17 N3 121.8(5) . . ?
O3 C17 C18 121.8(5) . . ?
N3 C17 C18 116.3(5) . . ?
C22 C18 C19 107.4(5) . . ?
C22 C18 C17 121.1(5) . . ?
C19 C18 C17 131.4(5) . . ?
C22 C18 Fe2 70.1(3) . . ?
C19 C18 Fe2 69.8(3) . . ?
C17 C18 Fe2 124.0(4) . . ?
C20 C19 C18 108.1(5) . . ?
C20 C19 Fe2 69.8(3) . . ?
C18 C19 Fe2 69.2(3) . . ?
C20 C19 H19 126.0 . . ?
C18 C19 H19 126.0 . . ?
Fe2 C19 H19 126.0 . . ?
C19 C20 C21 107.8(5) . . ?
C19 C20 Fe2 69.7(3) . . ?
C21 C20 Fe2 70.0(4) . . ?
C19 C20 H20 126.1 . . ?
C21 C20 H20 126.1 . . ?
Fe2 C20 H20 126.1 . . ?
C22 C21 C20 108.6(5) . . ?
C22 C21 Fe2 69.8(3) . . ?
C20 C21 Fe2 69.5(4) . . ?
C22 C21 H21 125.7 . . ?
C20 C21 H21 125.7 . . ?
Fe2 C21 H21 125.7 . . ?
C21 C22 C18 108.0(5) . . ?
C21 C22 Fe2 69.9(3) . . ?
C18 C22 Fe2 69.1(3) . . ?
C21 C22 H22 126.0 . . ?
C18 C22 H22 126.0 . . ?
Fe2 C22 H22 126.0 . . ?
C27 C23 C24 108.5(6) . . ?
C27 C23 Fe2 69.6(4) . . ?
C24 C23 Fe2 70.6(4) . . ?
C27 C23 H23 125.7 . . ?
C24 C23 H23 125.7 . . ?
Fe2 C23 H23 125.7 . . ?
C25 C24 C23 107.0(7) . . ?
C25 C24 Fe2 69.8(4) . . ?
C23 C24 Fe2 69.1(4) . . ?
C25 C24 H24 126.5 . . ?
C23 C24 H24 126.5 . . ?
Fe2 C24 H24 126.5 . . ?
C26 C25 C24 108.9(7) . . ?
C26 C25 Fe2 69.3(4) . . ?
C24 C25 Fe2 70.1(4) . . ?
C26 C25 H25 125.5 . . ?
C24 C25 H25 125.5 . . ?
Fe2 C25 H25 125.5 . . ?
C25 C26 C27 107.6(7) . . ?
C25 C26 Fe2 70.6(4) . . ?
C27 C26 Fe2 69.5(4) . . ?
C25 C26 H26 126.2 . . ?
C27 C26 H26 126.2 . . ?
Fe2 C26 H26 126.2 . . ?
C26 C27 C23 108.0(7) . . ?
C26 C27 Fe2 70.0(4) . . ?
C23 C27 Fe2 70.1(4) . . ?
C26 C27 H27 126.0 . . ?
C23 C27 H27 126.0 . . ?
Fe2 C27 H27 126.0 . . ?
C29 C28 N4 119.8(5) . . ?
C29 C28 N3 127.4(5) . . ?
N4 C28 N3 112.8(4) . . ?
C28 C29 C30 120.5(6) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C31 C30 C29 119.5(6) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 C30 119.5(6) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C31 C32 N4 122.1(6) . . ?
C31 C32 H32 118.9 . . ?
N4 C32 H32 118.9 . . ?

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.066

####################################################################### 
# 
# 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_5b
_database_code_depnum_ccdc_archive 'CCDC 1523205'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H33 Co N2 O Pd S, C2 H4 O2, C H2 Cl2'
_chemical_formula_sum            'C46 H39 Cl2 Co N2 O3 Pd S'
_chemical_formula_weight         936.08

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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.285(19)
_cell_length_b                   13.21(2)
_cell_length_c                   15.82(3)
_cell_angle_alpha                98.50(2)
_cell_angle_beta                 97.19(4)
_cell_angle_gamma                107.13(3)
_cell_volume                     2192(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2632
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      24.724

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.148
_exptl_absorpt_coefficient_mu    0.999
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8928
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.645
_diffrn_reflns_theta_max         24.534
_diffrn_reflns_theta_full        24.534
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             6500
_reflns_number_gt                5210
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²+0.5041P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6500
_refine_ls_number_parameters     509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.50411(3) 0.49648(2) 0.39382(2) 0.03735(13) Uani 1 1 d . . . . .
Co1 Co 0.19038(5) 0.45531(4) 0.26644(3) 0.03551(16) Uani 1 1 d . . . . .
S1 S 0.70061(11) 0.45966(10) 0.39136(7) 0.0501(3) Uani 1 1 d . . . . .
Cl2 Cl 0.8064(2) 0.13066(16) 0.60558(14) 0.1466(10) Uani 1 1 d . . . . .
Cl1 Cl 1.0338(3) 0.26819(19) 0.55750(14) 0.1586(11) Uani 1 1 d . . . . .
N1 N 0.4236(3) 0.3318(2) 0.37006(19) 0.0372(8) Uani 1 1 d . . . . .
O1 O 0.2289(3) 0.1955(2) 0.3562(2) 0.0579(8) Uani 1 1 d . . . . .
C23 C 0.0051(4) 0.5429(3) 0.1489(2) 0.0363(9) Uani 1 1 d . . . . .
C8 C 0.2437(4) 0.5240(3) 0.1650(2) 0.0362(10) Uani 1 1 d . . . . .
N2 N 0.5740(4) 0.6610(3) 0.4168(2) 0.0510(10) Uani 1 1 d . . . . .
C10 C 0.0997(4) 0.3747(3) 0.1450(2) 0.0370(10) Uani 1 1 d . . . . .
C11 C 0.3266(4) 0.3461(3) 0.1308(2) 0.0388(10) Uani 1 1 d . . . . .
C7 C 0.2399(4) 0.4085(3) 0.1510(2) 0.0381(10) Uani 1 1 d . . . . .
C17 C 0.3413(4) 0.6304(3) 0.1681(2) 0.0410(10) Uani 1 1 d . . . . .
O2 O 0.9945(4) 0.0928(3) 0.3551(3) 0.0849(13) Uani 1 1 d . . . . .
H2 H 1.0651 0.1273 0.3487 0.127 Uiso 1 1 calc R U . . .
C1 C 0.2945(4) 0.2942(3) 0.3642(2) 0.0404(10) Uani 1 1 d . . . . .
O4 O 0.8409(4) -0.0553(3) 0.2876(3) 0.0989(14) Uani 1 1 d . . . . .
C18 C 0.4705(4) 0.6493(4) 0.2015(3) 0.0471(11) Uani 1 1 d . . . . .
H18 H 0.4950 0.5947 0.2221 0.056 Uiso 1 1 calc R U . . .
C16 C 0.4261(4) 0.3850(4) 0.0863(3) 0.0496(11) Uani 1 1 d . . . . .
H16 H 0.4435 0.4540 0.0738 0.060 Uiso 1 1 calc R U . . .
C28 C -0.1017(4) 0.4965(4) 0.0815(3) 0.0451(11) Uani 1 1 d . . . . .
H28 H -0.1123 0.4303 0.0464 0.054 Uiso 1 1 calc R U . . .
C9 C 0.1030(4) 0.4893(3) 0.1592(2) 0.0345(9) Uani 1 1 d . . . . .
C29 C -0.0067(4) 0.2702(3) 0.1158(3) 0.0397(10) Uani 1 1 d . . . . .
C2 C 0.2382(4) 0.3835(3) 0.3709(2) 0.0386(10) Uani 1 1 d . . . . .
C35 C 0.5013(4) 0.2635(3) 0.3641(2) 0.0420(10) Uani 1 1 d . . . . .
C5 C 0.1157(5) 0.4973(4) 0.3761(3) 0.0520(12) Uani 1 1 d . . . . .
H5 H 0.0434 0.5240 0.3761 0.062 Uiso 1 1 calc R U . . .
C6 C 0.1096(4) 0.3855(4) 0.3662(3) 0.0466(11) Uani 1 1 d . . . . .
H6 H 0.0335 0.3230 0.3587 0.056 Uiso 1 1 calc R U . . .
C4 C 0.2472(5) 0.5643(4) 0.3876(3) 0.0514(12) Uani 1 1 d . . . . .
H4 H 0.2777 0.6433 0.3959 0.062 Uiso 1 1 calc R U . . .
C3 C 0.3246(4) 0.4948(3) 0.3839(2) 0.0367(10) Uani 1 1 d . . . . .
C24 C 0.0154(4) 0.6437(3) 0.2024(3) 0.0497(11) Uani 1 1 d . . . . .
H24 H 0.0837 0.6758 0.2476 0.060 Uiso 1 1 calc R U . . .
C40 C 0.6341(4) 0.3146(4) 0.3747(3) 0.0475(11) Uani 1 1 d . . . . .
C12 C 0.3044(5) 0.2417(3) 0.1497(3) 0.0491(11) Uani 1 1 d . . . . .
H12 H 0.2392 0.2147 0.1791 0.059 Uiso 1 1 calc R U . . .
C30 C -0.0064(5) 0.1941(4) 0.0424(3) 0.0544(12) Uani 1 1 d . . . . .
H30 H 0.0615 0.2075 0.0132 0.065 Uiso 1 1 calc R U . . .
C34 C -0.1120(4) 0.2462(3) 0.1579(3) 0.0484(11) Uani 1 1 d . . . . .
H34 H -0.1144 0.2950 0.2060 0.058 Uiso 1 1 calc R U . . .
C22 C 0.3058(5) 0.7145(3) 0.1360(3) 0.0505(12) Uani 1 1 d . . . . .
H22 H 0.2221 0.7037 0.1130 0.061 Uiso 1 1 calc R U . . .
C19 C 0.5616(5) 0.7489(4) 0.2041(3) 0.0592(14) Uani 1 1 d . . . . .
H19 H 0.6457 0.7599 0.2261 0.071 Uiso 1 1 calc R U . . .
C27 C -0.1917(4) 0.5495(4) 0.0672(3) 0.0550(13) Uani 1 1 d . . . . .
H27 H -0.2606 0.5183 0.0223 0.066 Uiso 1 1 calc R U . . .
C21 C 0.3988(6) 0.8144(4) 0.1393(3) 0.0661(15) Uani 1 1 d . . . . .
H21 H 0.3757 0.8695 0.1186 0.079 Uiso 1 1 calc R U . . .
C31 C -0.1084(5) 0.0989(4) 0.0142(3) 0.0667(15) Uani 1 1 d . . . . .
H31 H -0.1076 0.0500 -0.0344 0.080 Uiso 1 1 calc R U . . .
C33 C -0.2125(4) 0.1506(4) 0.1285(3) 0.0599(13) Uani 1 1 d . . . . .
H33 H -0.2812 0.1368 0.1569 0.072 Uiso 1 1 calc R U . . .
C25 C -0.0757(5) 0.6941(4) 0.1876(3) 0.0591(13) Uani 1 1 d . . . . .
H25 H -0.0679 0.7590 0.2234 0.071 Uiso 1 1 calc R U . . .
C45 C 0.9424(5) 0.0106(4) 0.2875(3) 0.0617(14) Uani 1 1 d . . . . .
C20 C 0.5259(5) 0.8317(4) 0.1734(3) 0.0669(16) Uani 1 1 d . . . . .
H20 H 0.5862 0.8980 0.1756 0.080 Uiso 1 1 calc R U . . .
C26 C -0.1787(5) 0.6483(4) 0.1194(3) 0.0615(14) Uani 1 1 d . . . . .
H26 H -0.2379 0.6834 0.1091 0.074 Uiso 1 1 calc R U . . .
C36 C 0.4580(5) 0.1482(4) 0.3467(3) 0.0576(13) Uani 1 1 d . . . . .
H36 H 0.3721 0.1120 0.3399 0.069 Uiso 1 1 calc R U . . .
C13 C 0.3784(6) 0.1777(4) 0.1253(3) 0.0648(14) Uani 1 1 d . . . . .
H13 H 0.3625 0.1095 0.1392 0.078 Uiso 1 1 calc R U . . .
C39 C 0.7164(5) 0.2519(5) 0.3681(4) 0.0722(15) Uani 1 1 d . . . . .
H39 H 0.8028 0.2864 0.3758 0.087 Uiso 1 1 calc R U . . .
C32 C -0.2113(5) 0.0754(4) 0.0570(3) 0.0659(15) Uani 1 1 d . . . . .
H32 H -0.2776 0.0111 0.0382 0.079 Uiso 1 1 calc R U . . .
C15 C 0.4998(5) 0.3193(5) 0.0606(3) 0.0666(14) Uani 1 1 d . . . . .
H15 H 0.5647 0.3451 0.0306 0.080 Uiso 1 1 calc R U . . .
C14 C 0.4754(6) 0.2154(5) 0.0803(3) 0.0693(15) Uani 1 1 d . . . . .
H14 H 0.5237 0.1724 0.0634 0.083 Uiso 1 1 calc R U . . .
C46 C 1.0135(5) 0.0059(4) 0.2137(3) 0.0704(15) Uani 1 1 d . . . . .
H46A H 0.9646 -0.0533 0.1678 0.106 Uiso 1 1 calc R U . . .
H46B H 1.0923 -0.0043 0.2336 0.106 Uiso 1 1 calc R U . . .
H46C H 1.0290 0.0722 0.1926 0.106 Uiso 1 1 calc R U . . .
C41 C 0.7247(5) 0.4772(5) 0.2804(3) 0.0723(16) Uani 1 1 d . . . . .
H41A H 0.7891 0.4477 0.2651 0.108 Uiso 1 1 calc R U . . .
H41B H 0.7501 0.5527 0.2783 0.108 Uiso 1 1 calc R U . . .
H41C H 0.6475 0.4402 0.2402 0.108 Uiso 1 1 calc R U . . .
C42 C 0.6128(5) 0.7534(4) 0.4291(3) 0.0592(14) Uani 1 1 d . . . . .
C38 C 0.6695(7) 0.1388(6) 0.3503(4) 0.0874(19) Uani 1 1 d . . . . .
H38 H 0.7241 0.0983 0.3457 0.105 Uiso 1 1 calc R U . . .
C37 C 0.5409(6) 0.0881(5) 0.3396(4) 0.0730(16) Uani 1 1 d . . . . .
H37 H 0.5093 0.0130 0.3275 0.088 Uiso 1 1 calc R U . . .
C43 C 0.6624(7) 0.8721(4) 0.4454(4) 0.102(2) Uani 1 1 d . . . . .
H43A H 0.5944 0.9012 0.4497 0.154 Uiso 1 1 calc R U . . .
H43B H 0.7029 0.8947 0.3984 0.154 Uiso 1 1 calc R U . . .
H43C H 0.7224 0.8978 0.4987 0.154 Uiso 1 1 calc R U . . .
C44 C 0.9301(9) 0.1363(7) 0.5486(5) 0.170(5) Uani 1 1 d . . . . .
H44A H 0.8954 0.1058 0.4877 0.205 Uiso 1 1 calc R U . . .
H44B H 0.9776 0.0920 0.5700 0.205 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C3 2.006(5) . ?
Pd1 N2 2.040(5) . ?
Pd1 N1 2.050(5) . ?
Pd1 S1 2.410(4) . ?
Co1 C8 2.027(5) . ?
Co1 C9 2.029(5) . ?
Co1 C10 2.033(5) . ?
Co1 C7 2.039(5) . ?
Co1 C5 2.093(5) . ?
Co1 C2 2.113(5) . ?
Co1 C6 2.113(5) . ?
Co1 C4 2.119(5) . ?
Co1 C3 2.136(5) . ?
S1 C40 1.805(5) . ?
S1 C41 1.847(5) . ?
Cl2 C44 1.744(9) . ?
Cl1 C44 1.762(8) . ?
N1 C1 1.380(6) . ?
N1 C35 1.433(6) . ?
O1 C1 1.273(5) . ?
C23 C28 1.420(6) . ?
C23 C24 1.432(6) . ?
C23 C9 1.483(6) . ?
C8 C7 1.496(6) . ?
C8 C17 1.497(6) . ?
C8 C9 1.504(6) . ?
N2 C42 1.145(6) . ?
C10 C9 1.486(6) . ?
C10 C7 1.499(6) . ?
C10 C29 1.502(6) . ?
C11 C16 1.409(6) . ?
C11 C12 1.411(6) . ?
C11 C7 1.488(6) . ?
C17 C18 1.422(6) . ?
C17 C22 1.425(6) . ?
O2 C45 1.339(6) . ?
O2 H2 0.8200 . ?
C1 C2 1.492(6) . ?
O4 C45 1.218(6) . ?
C18 C19 1.402(6) . ?
C18 H18 0.9300 . ?
C16 C15 1.420(7) . ?
C16 H16 0.9300 . ?
C28 C27 1.407(7) . ?
C28 H28 0.9300 . ?
C29 C34 1.411(6) . ?
C29 C30 1.420(6) . ?
C2 C6 1.452(7) . ?
C2 C3 1.473(6) . ?
C35 C40 1.426(6) . ?
C35 C36 1.427(6) . ?
C5 C6 1.441(7) . ?
C5 C4 1.459(7) . ?
C5 H5 0.9800 . ?
C6 H6 0.9800 . ?
C4 C3 1.442(6) . ?
C4 H4 0.9800 . ?
C24 C25 1.394(7) . ?
C24 H24 0.9300 . ?
C40 C39 1.419(7) . ?
C12 C13 1.400(7) . ?
C12 H12 0.9300 . ?
C30 C31 1.399(6) . ?
C30 H30 0.9300 . ?
C34 C33 1.396(6) . ?
C34 H34 0.9300 . ?
C22 C21 1.413(6) . ?
C22 H22 0.9300 . ?
C19 C20 1.400(8) . ?
C19 H19 0.9300 . ?
C27 C26 1.395(7) . ?
C27 H27 0.9300 . ?
C21 C20 1.407(8) . ?
C21 H21 0.9300 . ?
C31 C32 1.397(7) . ?
C31 H31 0.9300 . ?
C33 C32 1.394(7) . ?
C33 H33 0.9300 . ?
C25 C26 1.400(7) . ?
C25 H25 0.9300 . ?
C45 C46 1.500(7) . ?
C20 H20 0.9300 . ?
C26 H26 0.9300 . ?
C36 C37 1.399(7) . ?
C36 H36 0.9300 . ?
C13 C14 1.390(8) . ?
C13 H13 0.9300 . ?
C39 C38 1.401(8) . ?
C39 H39 0.9300 . ?
C32 H32 0.9300 . ?
C15 C14 1.408(8) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.471(7) . ?
C38 C37 1.384(8) . ?
C38 H38 0.9300 . ?
C37 H37 0.9300 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?

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
C3 Pd1 N2 93.40(17) . . ?
C3 Pd1 N1 83.29(16) . . ?
N2 Pd1 N1 176.69(15) . . ?
C3 Pd1 S1 168.09(11) . . ?
N2 Pd1 S1 98.03(14) . . ?
N1 Pd1 S1 85.26(13) . . ?
C8 Co1 C9 43.53(18) . . ?
C8 Co1 C10 62.45(19) . . ?
C9 Co1 C10 42.91(17) . . ?
C8 Co1 C7 43.16(18) . . ?
C9 Co1 C7 63.0(2) . . ?
C10 Co1 C7 43.20(18) . . ?
C8 Co1 C5 136.2(2) . . ?
C9 Co1 C5 111.1(2) . . ?
C10 Co1 C5 129.5(2) . . ?
C7 Co1 C5 172.60(18) . . ?
C8 Co1 C2 147.83(18) . . ?
C9 Co1 C2 164.77(15) . . ?
C10 Co1 C2 125.60(19) . . ?
C7 Co1 C2 117.3(2) . . ?
C5 Co1 C2 67.0(2) . . ?
C8 Co1 C6 171.94(17) . . ?
C9 Co1 C6 128.6(2) . . ?
C10 Co1 C6 113.5(2) . . ?
C7 Co1 C6 139.16(19) . . ?
C5 Co1 C6 40.07(19) . . ?
C2 Co1 C6 40.21(18) . . ?
C8 Co1 C4 113.9(2) . . ?
C9 Co1 C4 122.3(2) . . ?
C10 Co1 C4 163.30(18) . . ?
C7 Co1 C4 145.89(19) . . ?
C5 Co1 C4 40.52(19) . . ?
C2 Co1 C4 66.9(2) . . ?
C6 Co1 C4 67.8(2) . . ?
C8 Co1 C3 118.34(18) . . ?
C9 Co1 C3 154.18(16) . . ?
C10 Co1 C3 157.09(17) . . ?
C7 Co1 C3 119.6(2) . . ?
C5 Co1 C3 67.7(2) . . ?
C2 Co1 C3 40.56(16) . . ?
C6 Co1 C3 68.3(2) . . ?
C4 Co1 C3 39.61(17) . . ?
C40 S1 C41 100.8(2) . . ?
C40 S1 Pd1 96.06(18) . . ?
C41 S1 Pd1 100.50(19) . . ?
C1 N1 C35 124.0(3) . . ?
C1 N1 Pd1 115.9(3) . . ?
C35 N1 Pd1 120.0(3) . . ?
C28 C23 C24 117.4(4) . . ?
C28 C23 C9 119.9(4) . . ?
C24 C23 C9 122.7(4) . . ?
C7 C8 C17 135.6(4) . . ?
C7 C8 C9 90.3(3) . . ?
C17 C8 C9 133.4(4) . . ?
C7 C8 Co1 68.8(2) . . ?
C17 C8 Co1 127.8(3) . . ?
C9 C8 Co1 68.3(2) . . ?
C42 N2 Pd1 179.5(4) . . ?
C9 C10 C7 90.9(3) . . ?
C9 C10 C29 132.3(4) . . ?
C7 C10 C29 135.4(4) . . ?
C9 C10 Co1 68.4(2) . . ?
C7 C10 Co1 68.6(2) . . ?
C29 C10 Co1 130.4(3) . . ?
C16 C11 C12 118.1(4) . . ?
C16 C11 C7 121.4(4) . . ?
C12 C11 C7 120.2(4) . . ?
C11 C7 C8 137.5(4) . . ?
C11 C7 C10 131.9(4) . . ?
C8 C7 C10 89.3(3) . . ?
C11 C7 Co1 129.9(3) . . ?
C8 C7 Co1 68.0(2) . . ?
C10 C7 Co1 68.2(2) . . ?
C18 C17 C22 118.6(4) . . ?
C18 C17 C8 121.2(4) . . ?
C22 C17 C8 120.1(4) . . ?
C45 O2 H2 109.5 . . ?
O1 C1 N1 125.2(4) . . ?
O1 C1 C2 122.6(4) . . ?
N1 C1 C2 112.2(4) . . ?
C19 C18 C17 121.1(4) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C11 C16 C15 120.2(5) . . ?
C11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C27 C28 C23 120.8(4) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?
C23 C9 C10 133.7(4) . . ?
C23 C9 C8 135.1(4) . . ?
C10 C9 C8 89.5(3) . . ?
C23 C9 Co1 130.9(3) . . ?
C10 C9 Co1 68.7(2) . . ?
C8 C9 Co1 68.2(2) . . ?
C34 C29 C30 117.9(4) . . ?
C34 C29 C10 121.5(4) . . ?
C30 C29 C10 120.5(4) . . ?
C6 C2 C3 109.3(4) . . ?
C6 C2 C1 133.1(4) . . ?
C3 C2 C1 117.6(4) . . ?
C6 C2 Co1 69.9(2) . . ?
C3 C2 Co1 70.6(2) . . ?
C1 C2 Co1 124.9(3) . . ?
C40 C35 C36 116.5(4) . . ?
C40 C35 N1 117.5(4) . . ?
C36 C35 N1 125.9(4) . . ?
C6 C5 C4 109.0(4) . . ?
C6 C5 Co1 70.7(2) . . ?
C4 C5 Co1 70.7(3) . . ?
C6 C5 H5 125.5 . . ?
C4 C5 H5 125.5 . . ?
Co1 C5 H5 125.5 . . ?
C5 C6 C2 106.7(4) . . ?
C5 C6 Co1 69.2(2) . . ?
C2 C6 Co1 69.9(2) . . ?
C5 C6 H6 126.6 . . ?
C2 C6 H6 126.6 . . ?
Co1 C6 H6 126.6 . . ?
C3 C4 C5 108.5(4) . . ?
C3 C4 Co1 70.8(2) . . ?
C5 C4 Co1 68.8(2) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
Co1 C4 H4 125.7 . . ?
C4 C3 C2 106.4(4) . . ?
C4 C3 Pd1 142.7(3) . . ?
C2 C3 Pd1 110.8(3) . . ?
C4 C3 Co1 69.6(2) . . ?
C2 C3 Co1 68.9(2) . . ?
Pd1 C3 Co1 126.2(2) . . ?
C25 C24 C23 120.8(4) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C39 C40 C35 120.5(5) . . ?
C39 C40 S1 118.4(4) . . ?
C35 C40 S1 121.0(3) . . ?
C13 C12 C11 121.5(5) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C33 C34 C29 121.1(4) . . ?
C33 C34 H34 119.4 . . ?
C29 C34 H34 119.4 . . ?
C21 C22 C17 119.5(5) . . ?
C21 C22 H22 120.2 . . ?
C17 C22 H22 120.2 . . ?
C20 C19 C18 120.0(5) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C26 C27 C28 120.8(4) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C20 C21 C22 120.8(5) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C32 C31 C30 121.7(4) . . ?
C32 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C32 C33 C34 120.8(5) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C24 C25 C26 120.9(5) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
O4 C45 O2 119.7(5) . . ?
O4 C45 C46 123.2(5) . . ?
O2 C45 C46 117.1(4) . . ?
C19 C20 C21 119.9(4) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C27 C26 C25 119.3(5) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C37 C36 C35 121.9(5) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C38 C39 C40 121.0(5) . . ?
C38 C39 H39 119.5 . . ?
C40 C39 H39 119.5 . . ?
C33 C32 C31 118.6(4) . . ?
C33 C32 H32 120.7 . . ?
C31 C32 H32 120.7 . . ?
C14 C15 C16 120.4(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C13 C14 C15 119.3(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
S1 C41 H41A 109.5 . . ?
S1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
S1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N2 C42 C43 179.7(6) . . ?
C37 C38 C39 119.2(6) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C38 C37 C36 120.9(5) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Cl2 C44 Cl1 113.6(5) . . ?
Cl2 C44 H44A 108.8 . . ?
Cl1 C44 H44A 108.8 . . ?
Cl2 C44 H44B 108.8 . . ?
Cl1 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?

_refine_diff_density_max         0.595
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1523200'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H30 Co N3 O2 Pd'
_chemical_formula_sum            'C41 H30 Co N3 O2 Pd'
_chemical_formula_weight         762.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.024(11)
_cell_length_b                   20.65(2)
_cell_length_c                   14.762(11)
_cell_angle_alpha                90
_cell_angle_beta                 97.10(3)
_cell_angle_gamma                90
_cell_volume                     3334(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1897
_cell_measurement_theta_min      2.178
_cell_measurement_theta_max      21.342

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.165
_exptl_absorpt_coefficient_mu    1.078
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16351
_diffrn_reflns_av_unetI/netI     0.1707
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.107
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7700
_reflns_number_gt                4772
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0082P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7700
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.0749
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   0.724
_refine_ls_restrained_S_all      0.724
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.31833(3) 0.47415(2) 0.46737(2) 0.03840(11) Uani 1 1 d . . . . .
Co1 Co 0.38122(5) 0.30332(3) 0.46470(4) 0.03179(15) Uani 1 1 d . . . . .
O1 O 0.6000(2) 0.40672(13) 0.3375(2) 0.0497(8) Uani 1 1 d . . . . .
O2 O 0.2632(2) 0.55345(13) 0.3844(2) 0.0500(9) Uani 1 1 d . . . . .
N1 N 0.4391(3) 0.46815(15) 0.3798(2) 0.0301(8) Uani 1 1 d . . . . .
N2 N 0.3391(3) 0.55824(17) 0.3190(3) 0.0405(9) Uani 1 1 d . . . . .
N3 N 0.1928(3) 0.48088(17) 0.5542(3) 0.0478(10) Uani 1 1 d . . . . .
C1 C 0.5228(4) 0.4176(2) 0.3890(3) 0.0374(11) Uani 1 1 d . . . . .
C2 C 0.5022(3) 0.3789(2) 0.4694(3) 0.0340(11) Uani 1 1 d . . . . .
C3 C 0.4030(3) 0.39675(19) 0.5196(3) 0.0344(11) Uani 1 1 d . . . . .
C4 C 0.4023(4) 0.3499(2) 0.5898(3) 0.0426(12) Uani 1 1 d . . . . .
H4 H 0.3439 0.3485 0.6347 0.051 Uiso 1 1 calc R U . . .
C5 C 0.4976(4) 0.3056(2) 0.5844(3) 0.0481(13) Uani 1 1 d . . . . .
H5 H 0.5173 0.2687 0.6254 0.058 Uiso 1 1 calc R U . . .
C6 C 0.5602(3) 0.32260(19) 0.5106(3) 0.0405(12) Uani 1 1 d . . . . .
H6 H 0.6317 0.3005 0.4919 0.049 Uiso 1 1 calc R U . . .
C7 C 0.2925(3) 0.28256(19) 0.3414(3) 0.0327(10) Uani 1 1 d . . . . .
C8 C 0.2155(3) 0.27436(17) 0.4139(3) 0.0291(10) Uani 1 1 d . . . . .
C9 C 0.2919(3) 0.22099(18) 0.4516(3) 0.0305(10) Uani 1 1 d . . . . .
C10 C 0.3710(3) 0.22958(19) 0.3795(3) 0.0329(11) Uani 1 1 d . . . . .
C11 C 0.2817(3) 0.3205(2) 0.2563(3) 0.0374(11) Uani 1 1 d . . . . .
C12 C 0.3140(4) 0.2942(2) 0.1766(3) 0.0580(14) Uani 1 1 d . . . . .
H12 H 0.3458 0.2525 0.1772 0.070 Uiso 1 1 calc R U . . .
C13 C 0.2997(5) 0.3292(3) 0.0957(4) 0.0815(18) Uani 1 1 d . . . . .
H13 H 0.3213 0.3106 0.0426 0.098 Uiso 1 1 calc R U . . .
C14 C 0.2544(5) 0.3902(3) 0.0936(4) 0.0795(19) Uani 1 1 d . . . . .
H14 H 0.2457 0.4134 0.0392 0.095 Uiso 1 1 calc R U . . .
C15 C 0.2215(4) 0.4177(3) 0.1710(4) 0.0691(17) Uani 1 1 d . . . . .
H15 H 0.1910 0.4597 0.1696 0.083 Uiso 1 1 calc R U . . .
C16 C 0.2340(4) 0.3827(2) 0.2513(3) 0.0460(12) Uani 1 1 d . . . . .
H16 H 0.2096 0.4013 0.3035 0.055 Uiso 1 1 calc R U . . .
C17 C 0.0961(4) 0.30078(18) 0.4316(3) 0.0363(11) Uani 1 1 d . . . . .
C18 C 0.0753(4) 0.3175(2) 0.5193(3) 0.0499(13) Uani 1 1 d . . . . .
H18 H 0.1380 0.3131 0.5673 0.060 Uiso 1 1 calc R U . . .
C19 C -0.0370(5) 0.3405(2) 0.5365(4) 0.0667(17) Uani 1 1 d . . . . .
H19 H -0.0503 0.3501 0.5960 0.080 Uiso 1 1 calc R U . . .
C20 C -0.1277(5) 0.3492(2) 0.4675(5) 0.075(2) Uani 1 1 d . . . . .
H20 H -0.2022 0.3664 0.4791 0.090 Uiso 1 1 calc R U . . .
C21 C -0.1102(4) 0.3325(2) 0.3804(5) 0.0721(18) Uani 1 1 d . . . . .
H21 H -0.1735 0.3374 0.3330 0.087 Uiso 1 1 calc R U . . .
C22 C 0.0026(4) 0.3083(2) 0.3627(4) 0.0543(14) Uani 1 1 d . . . . .
H22 H 0.0141 0.2972 0.3033 0.065 Uiso 1 1 calc R U . . .
C23 C 0.2834(4) 0.17387(19) 0.5251(3) 0.0343(11) Uani 1 1 d . . . . .
C24 C 0.1718(4) 0.1595(2) 0.5544(3) 0.0462(13) Uani 1 1 d . . . . .
H24 H 0.1016 0.1795 0.5261 0.055 Uiso 1 1 calc R U . . .
C25 C 0.1620(4) 0.1161(2) 0.6243(3) 0.0624(15) Uani 1 1 d . . . . .
H25 H 0.0864 0.1083 0.6438 0.075 Uiso 1 1 calc R U . . .
C26 C 0.2644(5) 0.0847(2) 0.6650(3) 0.0668(16) Uani 1 1 d . . . . .
H26 H 0.2583 0.0546 0.7112 0.080 Uiso 1 1 calc R U . . .
C27 C 0.3760(4) 0.0983(2) 0.6366(3) 0.0621(15) Uani 1 1 d . . . . .
H27 H 0.4456 0.0776 0.6645 0.075 Uiso 1 1 calc R U . . .
C28 C 0.3860(4) 0.1417(2) 0.5685(3) 0.0450(12) Uani 1 1 d . . . . .
H28 H 0.4624 0.1500 0.5505 0.054 Uiso 1 1 calc R U . . .
C29 C 0.4761(3) 0.1957(2) 0.3501(3) 0.0374(11) Uani 1 1 d . . . . .
C30 C 0.5641(4) 0.2284(2) 0.3087(3) 0.0530(13) Uani 1 1 d . . . . .
H30 H 0.5552 0.2727 0.2982 0.064 Uiso 1 1 calc R U . . .
C31 C 0.6649(4) 0.1969(3) 0.2827(4) 0.0757(18) Uani 1 1 d . . . . .
H31 H 0.7221 0.2198 0.2540 0.091 Uiso 1 1 calc R U . . .
C32 C 0.6804(5) 0.1322(3) 0.2992(4) 0.084(2) Uani 1 1 d . . . . .
H32 H 0.7481 0.1108 0.2818 0.101 Uiso 1 1 calc R U . . .
C33 C 0.5960(5) 0.0989(3) 0.3417(4) 0.0796(18) Uani 1 1 d . . . . .
H33 H 0.6077 0.0551 0.3544 0.095 Uiso 1 1 calc R U . . .
C34 C 0.4932(4) 0.1300(2) 0.3659(3) 0.0552(14) Uani 1 1 d . . . . .
H34 H 0.4353 0.1065 0.3930 0.066 Uiso 1 1 calc R U . . .
C35 C 0.4306(3) 0.51431(19) 0.3149(3) 0.0333(10) Uani 1 1 d . . . . .
C36 C 0.5017(4) 0.5218(2) 0.2427(3) 0.0447(11) Uani 1 1 d . . . . .
H36 H 0.5630 0.4919 0.2357 0.054 Uiso 1 1 calc R U . . .
C37 C 0.4821(4) 0.5721(2) 0.1826(3) 0.0610(14) Uani 1 1 d . . . . .
H37 H 0.5311 0.5766 0.1360 0.073 Uiso 1 1 calc R U . . .
C38 C 0.3902(5) 0.6161(2) 0.1907(3) 0.0630(15) Uani 1 1 d . . . . .
H38 H 0.3763 0.6506 0.1502 0.076 Uiso 1 1 calc R U . . .
C39 C 0.3211(4) 0.6080(2) 0.2590(4) 0.0544(14) Uani 1 1 d . . . . .
H39 H 0.2590 0.6375 0.2651 0.065 Uiso 1 1 calc R U . . .
C40 C 0.1156(4) 0.4903(2) 0.5950(3) 0.0425(12) Uani 1 1 d . . . . .
C41 C 0.0140(3) 0.5041(2) 0.6463(3) 0.0560(14) Uani 1 1 d . . . . .
H41A H -0.0067 0.5492 0.6405 0.084 Uiso 1 1 calc R U . . .
H41B H 0.0371 0.4938 0.7095 0.084 Uiso 1 1 calc R U . . .
H41C H -0.0554 0.4784 0.6228 0.084 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C3 1.960(4) . ?
Pd1 N1 1.972(3) . ?
Pd1 N3 2.005(4) . ?
Pd1 O2 2.090(3) . ?
Co1 C9 1.962(4) . ?
Co1 C10 1.969(4) . ?
Co1 C8 1.980(4) . ?
Co1 C7 2.004(5) . ?
Co1 C6 2.045(4) . ?
Co1 C2 2.049(4) . ?
Co1 C5 2.052(5) . ?
Co1 C4 2.070(4) . ?
Co1 C3 2.094(4) . ?
O1 C1 1.230(4) . ?
O2 N2 1.357(4) . ?
N1 C35 1.346(5) . ?
N1 C1 1.389(5) . ?
N2 C39 1.355(5) . ?
N2 C35 1.363(5) . ?
N3 C40 1.118(5) . ?
C1 C2 1.471(5) . ?
C2 C6 1.426(5) . ?
C2 C3 1.442(5) . ?
C3 C4 1.418(5) . ?
C4 C5 1.403(5) . ?
C4 H4 0.9800 . ?
C5 C6 1.404(5) . ?
C5 H5 0.9800 . ?
C6 H6 0.9800 . ?
C7 C8 1.456(5) . ?
C7 C10 1.464(5) . ?
C7 C11 1.473(5) . ?
C8 C9 1.455(5) . ?
C8 C17 1.477(5) . ?
C9 C10 1.468(5) . ?
C9 C23 1.470(5) . ?
C10 C29 1.464(5) . ?
C11 C12 1.382(6) . ?
C11 C16 1.385(5) . ?
C12 C13 1.388(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.354(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.364(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.381(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.366(5) . ?
C17 C18 1.387(6) . ?
C18 C19 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.348(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.367(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.394(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.385(5) . ?
C23 C28 1.398(5) . ?
C24 C25 1.380(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.374(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.377(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.361(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.384(6) . ?
C29 C30 1.386(5) . ?
C30 C31 1.383(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.365(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.370(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.387(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.407(5) . ?
C36 C37 1.365(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.378(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.346(6) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.456(5) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 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
C3 Pd1 N1 83.06(16) . . ?
C3 Pd1 N3 97.94(16) . . ?
N1 Pd1 N3 178.75(15) . . ?
C3 Pd1 O2 163.58(14) . . ?
N1 Pd1 O2 80.55(13) . . ?
N3 Pd1 O2 98.45(13) . . ?
C9 Co1 C10 43.84(15) . . ?
C9 Co1 C8 43.32(14) . . ?
C10 Co1 C8 63.07(16) . . ?
C9 Co1 C7 62.76(17) . . ?
C10 Co1 C7 43.22(14) . . ?
C8 Co1 C7 42.86(15) . . ?
C9 Co1 C6 130.79(16) . . ?
C10 Co1 C6 109.82(17) . . ?
C8 Co1 C6 172.74(16) . . ?
C7 Co1 C6 133.31(18) . . ?
C9 Co1 C2 168.55(16) . . ?
C10 Co1 C2 126.60(17) . . ?
C8 Co1 C2 144.05(17) . . ?
C7 Co1 C2 115.88(17) . . ?
C6 Co1 C2 40.79(14) . . ?
C9 Co1 C5 110.96(18) . . ?
C10 Co1 C5 123.24(18) . . ?
C8 Co1 C5 141.51(18) . . ?
C7 Co1 C5 166.04(17) . . ?
C6 Co1 C5 40.07(16) . . ?
C2 Co1 C5 67.55(18) . . ?
C9 Co1 C4 119.38(17) . . ?
C10 Co1 C4 157.01(18) . . ?
C8 Co1 C4 118.37(18) . . ?
C7 Co1 C4 153.96(17) . . ?
C6 Co1 C4 67.42(18) . . ?
C2 Co1 C4 67.34(17) . . ?
C5 Co1 C4 39.79(15) . . ?
C9 Co1 C3 150.27(16) . . ?
C10 Co1 C3 162.53(17) . . ?
C8 Co1 C3 118.77(15) . . ?
C7 Co1 C3 124.64(16) . . ?
C6 Co1 C3 68.43(16) . . ?
C2 Co1 C3 40.72(14) . . ?
C5 Co1 C3 67.42(17) . . ?
C4 Co1 C3 39.81(14) . . ?
N2 O2 Pd1 108.3(2) . . ?
C35 N1 C1 126.1(4) . . ?
C35 N1 Pd1 115.4(3) . . ?
C1 N1 Pd1 118.5(3) . . ?
C39 N2 O2 117.8(4) . . ?
C39 N2 C35 121.6(4) . . ?
O2 N2 C35 120.5(4) . . ?
C40 N3 Pd1 171.0(4) . . ?
O1 C1 N1 125.3(4) . . ?
O1 C1 C2 126.0(4) . . ?
N1 C1 C2 108.7(4) . . ?
C6 C2 C3 108.5(4) . . ?
C6 C2 C1 132.9(4) . . ?
C3 C2 C1 118.6(4) . . ?
C6 C2 Co1 69.5(2) . . ?
C3 C2 Co1 71.3(2) . . ?
C1 C2 Co1 123.4(3) . . ?
C4 C3 C2 105.9(4) . . ?
C4 C3 Pd1 142.9(3) . . ?
C2 C3 Pd1 111.1(3) . . ?
C4 C3 Co1 69.2(2) . . ?
C2 C3 Co1 67.9(2) . . ?
Pd1 C3 Co1 124.9(2) . . ?
C5 C4 C3 109.3(4) . . ?
C5 C4 Co1 69.4(3) . . ?
C3 C4 Co1 71.0(2) . . ?
C5 C4 H4 125.3 . . ?
C3 C4 H4 125.3 . . ?
Co1 C4 H4 125.3 . . ?
C4 C5 C6 108.9(4) . . ?
C4 C5 Co1 70.8(2) . . ?
C6 C5 Co1 69.7(3) . . ?
C4 C5 H5 125.5 . . ?
C6 C5 H5 125.5 . . ?
Co1 C5 H5 125.5 . . ?
C5 C6 C2 107.3(4) . . ?
C5 C6 Co1 70.3(2) . . ?
C2 C6 Co1 69.8(2) . . ?
C5 C6 H6 126.3 . . ?
C2 C6 H6 126.3 . . ?
Co1 C6 H6 126.3 . . ?
C8 C7 C10 90.1(3) . . ?
C8 C7 C11 134.1(4) . . ?
C10 C7 C11 135.0(4) . . ?
C8 C7 Co1 67.7(2) . . ?
C10 C7 Co1 67.1(2) . . ?
C11 C7 Co1 129.8(3) . . ?
C7 C8 C9 90.4(3) . . ?
C7 C8 C17 134.4(4) . . ?
C9 C8 C17 134.3(4) . . ?
C7 C8 Co1 69.5(2) . . ?
C9 C8 Co1 67.7(2) . . ?
C17 C8 Co1 128.4(3) . . ?
C8 C9 C10 89.9(3) . . ?
C8 C9 C23 134.2(4) . . ?
C10 C9 C23 135.6(4) . . ?
C8 C9 Co1 69.0(2) . . ?
C10 C9 Co1 68.3(2) . . ?
C23 C9 Co1 125.3(3) . . ?
C7 C10 C29 134.1(4) . . ?
C7 C10 C9 89.6(3) . . ?
C29 C10 C9 136.0(4) . . ?
C7 C10 Co1 69.7(2) . . ?
C29 C10 Co1 125.0(3) . . ?
C9 C10 Co1 67.8(2) . . ?
C12 C11 C16 117.1(5) . . ?
C12 C11 C7 121.0(4) . . ?
C16 C11 C7 121.9(4) . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 120.4(6) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.3(6) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 119.5(5) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C11 121.8(5) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C22 C17 C18 118.1(4) . . ?
C22 C17 C8 121.2(4) . . ?
C18 C17 C8 120.7(4) . . ?
C19 C18 C17 120.9(5) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C18 120.4(5) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 119.9(5) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C22 120.0(5) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C17 C22 C21 120.7(5) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C28 117.1(4) . . ?
C24 C23 C9 120.9(4) . . ?
C28 C23 C9 122.1(4) . . ?
C25 C24 C23 121.8(4) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C26 C25 C24 119.9(4) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 119.1(5) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
C28 C27 C26 121.1(4) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C23 121.0(4) . . ?
C27 C28 H28 119.5 . . ?
C23 C28 H28 119.5 . . ?
C34 C29 C30 117.6(4) . . ?
C34 C29 C10 121.0(4) . . ?
C30 C29 C10 121.3(4) . . ?
C31 C30 C29 121.6(5) . . ?
C31 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
C32 C31 C30 119.9(5) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C33 119.7(5) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C34 120.6(5) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C29 C34 C33 120.5(5) . . ?
C29 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
N1 C35 N2 115.2(4) . . ?
N1 C35 C36 128.3(4) . . ?
N2 C35 C36 116.4(4) . . ?
C37 C36 C35 121.2(4) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 120.3(5) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C39 C38 C37 118.2(5) . . ?
C39 C38 H38 120.9 . . ?
C37 C38 H38 120.9 . . ?
C38 C39 N2 122.2(4) . . ?
C38 C39 H39 118.9 . . ?
N2 C39 H39 118.9 . . ?
N3 C40 C41 178.3(5) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

_refine_diff_density_max         0.577
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1579963'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H29 Co N2 O2'
_chemical_formula_sum            'C39 H29 Co N2 O2'
_chemical_formula_weight         616.57

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.92(4)
_cell_length_b                   14.34(4)
_cell_length_c                   17.16(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.61(3)
_cell_angle_gamma                90
_cell_volume                     3173(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4286
_cell_measurement_theta_min      2.528
_cell_measurement_theta_max      23.841

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.146
_exptl_absorpt_coefficient_mu    0.577
_shelx_estimated_absorpt_T_min   0.840
_shelx_estimated_absorpt_T_max   0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17820
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.579
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             6419
_reflns_number_gt                4134
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6419
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.0924
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_restrained_S_all      0.882
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.28887(2) 0.38112(2) 0.31185(2) 0.03835(11) Uani 1 1 d . . . . .
O1 O 0.00684(14) 0.44465(12) 0.21732(10) 0.0631(5) Uani 1 1 d . . . . .
O2 O 0.25571(13) 0.53194(12) 0.02932(11) 0.0664(5) Uani 1 1 d . . . . .
N2 N 0.16189(16) 0.57236(13) 0.03029(12) 0.0505(5) Uani 1 1 d . . . . .
N1 N 0.13723(17) 0.47177(14) 0.13279(12) 0.0498(5) Uani 1 1 d . . . . .
C17 C 0.49592(17) 0.47860(14) 0.26163(13) 0.0370(5) Uani 1 1 d . . . . .
C7 C 0.31242(16) 0.51954(14) 0.32973(12) 0.0363(5) Uani 1 1 d . . . . .
C11 C 0.25274(16) 0.59850(13) 0.29233(12) 0.0361(5) Uani 1 1 d . . . . .
C10 C 0.30274(16) 0.46855(13) 0.40495(12) 0.0360(5) Uani 1 1 d . . . . .
C8 C 0.41165(16) 0.46901(13) 0.31727(12) 0.0355(5) Uani 1 1 d . . . . .
C29 C 0.23426(16) 0.47688(14) 0.47206(12) 0.0382(5) Uani 1 1 d . . . . .
C9 C 0.40144(16) 0.41877(14) 0.39296(12) 0.0366(5) Uani 1 1 d . . . . .
C12 C 0.14740(17) 0.61176(15) 0.30783(13) 0.0443(6) Uani 1 1 d . . . . .
H12 H 0.1147 0.5687 0.3385 0.053 Uiso 1 1 calc R U . . .
C22 C 0.60115(18) 0.47281(15) 0.28895(14) 0.0476(6) Uani 1 1 d . . . . .
H22 H 0.6180 0.4617 0.3416 0.057 Uiso 1 1 calc R U . . .
C23 C 0.46691(16) 0.35533(14) 0.44483(13) 0.0374(5) Uani 1 1 d . . . . .
C30 C 0.20195(18) 0.56572(16) 0.49688(14) 0.0518(6) Uani 1 1 d . . . . .
H30 H 0.2225 0.6188 0.4708 0.062 Uiso 1 1 calc R U . . .
C16 C 0.29953(17) 0.66341(15) 0.24404(13) 0.0473(6) Uani 1 1 d . . . . .
H16 H 0.3681 0.6550 0.2320 0.057 Uiso 1 1 calc R U . . .
C13 C 0.09176(19) 0.68887(16) 0.27758(14) 0.0535(6) Uani 1 1 d . . . . .
H13 H 0.0225 0.6966 0.2881 0.064 Uiso 1 1 calc R U . . .
C20 C 0.6574(2) 0.50073(16) 0.15804(16) 0.0583(7) Uani 1 1 d . . . . .
H20 H 0.7102 0.5076 0.1240 0.070 Uiso 1 1 calc R U . . .
C24 C 0.46881(18) 0.36746(15) 0.52656(14) 0.0487(6) Uani 1 1 d . . . . .
H24 H 0.4320 0.4163 0.5473 0.058 Uiso 1 1 calc R U . . .
C1 C 0.0941(2) 0.42561(16) 0.19497(14) 0.0477(6) Uani 1 1 d . . . . .
C21 C 0.68113(19) 0.48372(16) 0.23707(16) 0.0562(7) Uani 1 1 d . . . . .
H21 H 0.7501 0.4795 0.2559 0.067 Uiso 1 1 calc R U . . .
C35 C 0.09423(18) 0.54320(15) 0.08582(13) 0.0450(6) Uani 1 1 d . . . . .
C2 C 0.16322(18) 0.35180(16) 0.23175(14) 0.0480(6) Uani 1 1 d . . . . .
C19 C 0.5538(2) 0.50743(16) 0.13027(14) 0.0567(7) Uani 1 1 d . . . . .
H19 H 0.5377 0.5197 0.0777 0.068 Uiso 1 1 calc R U . . .
C18 C 0.47372(19) 0.49580(16) 0.18111(14) 0.0503(6) Uani 1 1 d . . . . .
H18 H 0.4051 0.4995 0.1616 0.060 Uiso 1 1 calc R U . . .
C6 C 0.14687(19) 0.30824(16) 0.30688(15) 0.0530(6) Uani 1 1 d . . . . .
H6 H 0.0886 0.3200 0.3395 0.064 Uiso 1 1 calc R U . . .
C3 C 0.25883(19) 0.31307(16) 0.20376(14) 0.0541(6) Uani 1 1 d . . . . .
H3 H 0.2893 0.3287 0.1546 0.065 Uiso 1 1 calc R U . . .
C28 C 0.52605(18) 0.28207(16) 0.41522(15) 0.0541(6) Uani 1 1 d . . . . .
H28 H 0.5269 0.2736 0.3615 0.065 Uiso 1 1 calc R U . . .
C15 C 0.24338(19) 0.74095(16) 0.21391(15) 0.0573(7) Uani 1 1 d . . . . .
H15 H 0.2750 0.7835 0.1821 0.069 Uiso 1 1 calc R U . . .
C14 C 0.1401(2) 0.75428(16) 0.23162(15) 0.0585(7) Uani 1 1 d . . . . .
H14 H 0.1038 0.8065 0.2129 0.070 Uiso 1 1 calc R U . . .
C31 C 0.1393(2) 0.5748(2) 0.56028(16) 0.0667(8) Uani 1 1 d . . . . .
H31 H 0.1176 0.6338 0.5749 0.080 Uiso 1 1 calc R U . . .
C34 C 0.20470(19) 0.39806(16) 0.51494(14) 0.0539(7) Uani 1 1 d . . . . .
H34 H 0.2258 0.3389 0.5004 0.065 Uiso 1 1 calc R U . . .
C25 C 0.5257(2) 0.30649(19) 0.57679(16) 0.0640(7) Uani 1 1 d . . . . .
H25 H 0.5254 0.3146 0.6306 0.077 Uiso 1 1 calc R U . . .
C4 C 0.2992(2) 0.24740(16) 0.26065(16) 0.0605(7) Uani 1 1 d . . . . .
H4 H 0.3629 0.2109 0.2573 0.073 Uiso 1 1 calc R U . . .
C36 C -0.00362(19) 0.58466(18) 0.08791(15) 0.0575(7) Uani 1 1 d . . . . .
H36 H -0.0493 0.5658 0.1247 0.069 Uiso 1 1 calc R U . . .
C32 C 0.1090(2) 0.4966(2) 0.60181(16) 0.0699(8) Uani 1 1 d . . . . .
H32 H 0.0668 0.5030 0.6434 0.084 Uiso 1 1 calc R U . . .
C5 C 0.2309(2) 0.24443(16) 0.32423(16) 0.0600(7) Uani 1 1 d . . . . .
H5 H 0.2402 0.2054 0.3710 0.072 Uiso 1 1 calc R U . . .
C26 C 0.5825(2) 0.23384(19) 0.54649(19) 0.0684(8) Uani 1 1 d . . . . .
H26 H 0.6198 0.1933 0.5800 0.082 Uiso 1 1 calc R U . . .
C27 C 0.58345(19) 0.22207(17) 0.46563(18) 0.0664(8) Uani 1 1 d . . . . .
H27 H 0.6223 0.1743 0.4453 0.080 Uiso 1 1 calc R U . . .
C38 C 0.0372(2) 0.68342(18) -0.02111(17) 0.0693(8) Uani 1 1 d . . . . .
H38 H 0.0188 0.7305 -0.0566 0.083 Uiso 1 1 calc R U . . .
C39 C 0.1332(2) 0.64110(18) -0.02246(16) 0.0636(7) Uani 1 1 d . . . . .
H39 H 0.1788 0.6594 -0.0594 0.076 Uiso 1 1 calc R U . . .
C33 C 0.1433(2) 0.4084(2) 0.57973(16) 0.0696(8) Uani 1 1 d . . . . .
H33 H 0.1255 0.3561 0.6080 0.084 Uiso 1 1 calc R U . . .
C37 C -0.0321(2) 0.6553(2) 0.03362(17) 0.0687(8) Uani 1 1 d . . . . .
H37 H -0.0971 0.6831 0.0342 0.082 Uiso 1 1 calc R U . . .
H1 H 0.203(2) 0.4628(18) 0.1226(17) 0.086(11) Uiso 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
Co1 C9 2.022(5) . ?
Co1 C8 2.024(5) . ?
Co1 C7 2.029(6) . ?
Co1 C10 2.030(5) . ?
Co1 C2 2.103(5) . ?
Co1 C6 2.109(6) . ?
Co1 C3 2.110(6) . ?
Co1 C5 2.114(6) . ?
Co1 C4 2.117(6) . ?
O1 C1 1.243(4) . ?
O2 N2 1.345(4) . ?
N2 C39 1.373(4) . ?
N2 C35 1.397(4) . ?
N1 C35 1.397(4) . ?
N1 C1 1.401(4) . ?
N1 H1 0.88(3) . ?
C17 C22 1.413(5) . ?
C17 C18 1.415(5) . ?
C17 C8 1.499(4) . ?
C7 C11 1.492(4) . ?
C7 C10 1.496(5) . ?
C7 C8 1.500(5) . ?
C11 C16 1.408(4) . ?
C11 C12 1.416(5) . ?
C10 C9 1.487(5) . ?
C10 C29 1.500(4) . ?
C8 C9 1.498(5) . ?
C29 C34 1.414(4) . ?
C29 C30 1.415(5) . ?
C9 C23 1.497(4) . ?
C12 C13 1.401(4) . ?
C12 H12 0.9300 . ?
C22 C21 1.415(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.412(5) . ?
C23 C28 1.412(4) . ?
C30 C31 1.402(5) . ?
C30 H30 0.9300 . ?
C16 C15 1.408(4) . ?
C16 H16 0.9300 . ?
C13 C14 1.398(4) . ?
C13 H13 0.9300 . ?
C20 C21 1.393(5) . ?
C20 C19 1.395(5) . ?
C20 H20 0.9300 . ?
C24 C25 1.403(4) . ?
C24 H24 0.9300 . ?
C1 C2 1.499(4) . ?
C21 H21 0.9300 . ?
C35 C36 1.400(5) . ?
C2 C6 1.460(5) . ?
C2 C3 1.463(5) . ?
C19 C18 1.405(4) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
C6 C5 1.436(4) . ?
C6 H6 0.9800 . ?
C3 C4 1.431(4) . ?
C3 H3 0.9800 . ?
C28 C27 1.399(4) . ?
C28 H28 0.9300 . ?
C15 C14 1.400(5) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C31 C32 1.399(5) . ?
C31 H31 0.9300 . ?
C34 C33 1.414(5) . ?
C34 H34 0.9300 . ?
C25 C26 1.394(5) . ?
C25 H25 0.9300 . ?
C4 C5 1.447(5) . ?
C4 H4 0.9800 . ?
C36 C37 1.409(5) . ?
C36 H36 0.9300 . ?
C32 C33 1.400(5) . ?
C32 H32 0.9300 . ?
C5 H5 0.9800 . ?
C26 C27 1.398(6) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C38 C39 1.383(5) . ?
C38 C37 1.398(5) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C33 H33 0.9300 . ?
C37 H37 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
C9 Co1 C8 43.47(14) . . ?
C9 Co1 C7 62.62(8) . . ?
C8 Co1 C7 43.44(12) . . ?
C9 Co1 C10 43.06(13) . . ?
C8 Co1 C10 63.19(13) . . ?
C7 Co1 C10 43.25(12) . . ?
C9 Co1 C2 174.65(9) . . ?
C8 Co1 C2 136.51(14) . . ?
C7 Co1 C2 113.38(9) . . ?
C10 Co1 C2 131.63(14) . . ?
C9 Co1 C6 138.29(15) . . ?
C8 Co1 C6 171.17(9) . . ?
C7 Co1 C6 127.80(12) . . ?
C10 Co1 C6 111.81(13) . . ?
C2 Co1 C6 40.56(15) . . ?
C9 Co1 C3 144.39(12) . . ?
C8 Co1 C3 115.39(13) . . ?
C7 Co1 C3 127.09(11) . . ?
C10 Co1 C3 168.44(9) . . ?
C2 Co1 C3 40.64(12) . . ?
C6 Co1 C3 67.90(12) . . ?
C9 Co1 C5 115.00(13) . . ?
C8 Co1 C5 148.73(10) . . ?
C7 Co1 C5 160.53(12) . . ?
C10 Co1 C5 120.53(18) . . ?
C2 Co1 C5 67.43(12) . . ?
C6 Co1 C5 39.77(9) . . ?
C3 Co1 C5 67.22(16) . . ?
C9 Co1 C4 117.78(13) . . ?
C8 Co1 C4 120.90(17) . . ?
C7 Co1 C4 159.44(12) . . ?
C10 Co1 C4 151.81(10) . . ?
C2 Co1 C4 67.28(13) . . ?
C6 Co1 C4 67.15(16) . . ?
C3 Co1 C4 39.57(9) . . ?
C5 Co1 C4 39.99(16) . . ?
O2 N2 C39 120.5(2) . . ?
O2 N2 C35 118.9(2) . . ?
C39 N2 C35 120.7(3) . . ?
C35 N1 C1 128.5(3) . . ?
C35 N1 H1 110.0(18) . . ?
C1 N1 H1 121.0(18) . . ?
C22 C17 C18 117.8(2) . . ?
C22 C17 C8 120.4(3) . . ?
C18 C17 C8 121.8(3) . . ?
C11 C7 C10 132.3(2) . . ?
C11 C7 C8 136.8(2) . . ?
C10 C7 C8 90.31(19) . . ?
C11 C7 Co1 127.5(2) . . ?
C10 C7 Co1 68.42(18) . . ?
C8 C7 Co1 68.11(17) . . ?
C16 C11 C12 118.4(2) . . ?
C16 C11 C7 121.7(3) . . ?
C12 C11 C7 119.9(2) . . ?
C9 C10 C7 89.79(19) . . ?
C9 C10 C29 134.2(2) . . ?
C7 C10 C29 135.1(2) . . ?
C9 C10 Co1 68.20(15) . . ?
C7 C10 Co1 68.3(3) . . ?
C29 C10 Co1 128.8(2) . . ?
C9 C8 C17 134.7(2) . . ?
C9 C8 C7 89.20(19) . . ?
C17 C8 C7 135.1(2) . . ?
C9 C8 Co1 68.21(15) . . ?
C17 C8 Co1 128.80(19) . . ?
C7 C8 Co1 68.4(3) . . ?
C34 C29 C30 117.9(3) . . ?
C34 C29 C10 121.8(2) . . ?
C30 C29 C10 120.2(2) . . ?
C10 C9 C23 131.8(2) . . ?
C10 C9 C8 90.69(19) . . ?
C23 C9 C8 136.9(2) . . ?
C10 C9 Co1 68.7(2) . . ?
C23 C9 Co1 127.0(2) . . ?
C8 C9 Co1 68.3(2) . . ?
C13 C12 C11 120.9(2) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C17 C22 C21 120.7(3) . . ?
C17 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C28 118.2(2) . . ?
C24 C23 C9 119.3(2) . . ?
C28 C23 C9 122.4(3) . . ?
C31 C30 C29 120.9(2) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C11 C16 C15 120.5(3) . . ?
C11 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C21 C20 C19 119.5(2) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C25 C24 C23 120.6(3) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
O1 C1 N1 122.9(2) . . ?
O1 C1 C2 123.6(3) . . ?
N1 C1 C2 113.5(3) . . ?
C20 C21 C22 120.5(3) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
N1 C35 N2 111.7(3) . . ?
N1 C35 C36 128.6(2) . . ?
N2 C35 C36 119.7(3) . . ?
C6 C2 C3 107.4(2) . . ?
C6 C2 C1 123.9(3) . . ?
C3 C2 C1 128.6(3) . . ?
C6 C2 Co1 69.9(2) . . ?
C3 C2 Co1 70.0(2) . . ?
C1 C2 Co1 123.3(2) . . ?
C20 C19 C18 120.5(3) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C5 C6 C2 107.8(2) . . ?
C5 C6 Co1 70.3(3) . . ?
C2 C6 Co1 69.50(15) . . ?
C5 C6 H6 126.1 . . ?
C2 C6 H6 126.1 . . ?
Co1 C6 H6 126.1 . . ?
C4 C3 C2 107.8(3) . . ?
C4 C3 Co1 70.5(3) . . ?
C2 C3 Co1 69.40(18) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
Co1 C3 H3 126.1 . . ?
C27 C28 C23 120.8(3) . . ?
C27 C28 H28 119.6 . . ?
C23 C28 H28 119.6 . . ?
C14 C15 C16 120.3(2) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C13 C14 C15 119.8(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C32 C31 C30 121.0(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C34 C29 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C29 C34 H34 119.7 . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C3 C4 C5 108.7(3) . . ?
C3 C4 Co1 70.0(2) . . ?
C5 C4 Co1 69.90(17) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
Co1 C4 H4 125.7 . . ?
C35 C36 C37 119.2(3) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C31 C32 C33 118.9(3) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C6 C5 C4 108.3(3) . . ?
C6 C5 Co1 69.9(2) . . ?
C4 C5 Co1 70.11(14) . . ?
C6 C5 H5 125.9 . . ?
C4 C5 H5 125.9 . . ?
Co1 C5 H5 125.9 . . ?
C25 C26 C27 119.9(2) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C26 C27 C28 120.1(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C39 C38 C37 119.9(3) . . ?
C39 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
N2 C39 C38 120.6(3) . . ?
N2 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C32 C33 C34 120.7(3) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C38 C37 C36 120.0(3) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?

_refine_diff_density_max         0.310
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.093

####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1523208'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H35 Co N2 O Se'
_chemical_formula_sum            'C49 H35 Co N2 O Se'
_chemical_formula_weight         805.68

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   10.27(2)
_cell_length_b                   16.50(3)
_cell_length_c                   23.24(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3936(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1382
_cell_measurement_theta_min      2.171
_cell_measurement_theta_max      16.405

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.196
_exptl_absorpt_coefficient_mu    1.400
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20113
_diffrn_reflns_av_unetI/netI     0.1586
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.514
_diffrn_reflns_theta_max         27.910
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             8682
_reflns_number_gt                5326
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_max     0.959
_reflns_Friedel_fraction_full    0.991

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0338P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8682
_refine_ls_number_parameters     488
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.0940
_refine_ls_wR_factor_ref         0.1426
_refine_ls_wR_factor_gt          0.1256
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.22786(10) 0.67793(6) 0.53710(4) 0.0434(3) Uani 1 1 d . . . . .
Co1 Co 0.42112(12) 0.51136(7) 0.58893(5) 0.0348(3) Uani 1 1 d . . . . .
C8 C 0.4602(9) 0.4023(6) 0.5545(4) 0.035(2) Uani 1 1 d . . . . .
N1 N 0.1636(9) 0.6413(5) 0.6787(3) 0.047(2) Uani 1 1 d . . . . .
H1 H 0.1520 0.6642 0.6459 0.056 Uiso 1 1 calc R U . . .
C7 C 0.3314(9) 0.4301(5) 0.5395(5) 0.037(2) Uani 1 1 d . . . . .
C29 C 0.1622(10) 0.4269(5) 0.6306(4) 0.035(2) Uani 1 1 d . . . . .
O1 O 0.3180(8) 0.5808(4) 0.7347(3) 0.070(3) Uani 1 1 d . . . . .
C34 C 0.1378(11) 0.3814(7) 0.6790(5) 0.054(3) Uani 1 1 d . . . . .
H34 H 0.2040 0.3492 0.6940 0.064 Uiso 1 1 calc R U . . .
N2 N -0.0575(10) 0.7181(5) 0.6437(4) 0.060(3) Uani 1 1 d . . . . .
C35 C 0.0548(11) 0.6413(6) 0.7169(4) 0.045(3) Uani 1 1 d . . . . .
C3 C 0.3733(9) 0.6335(5) 0.5795(4) 0.036(2) Uani 1 1 d . . . . .
C10 C 0.2899(9) 0.4219(5) 0.6004(4) 0.033(2) Uani 1 1 d . . . . .
C17 C 0.5721(10) 0.3722(5) 0.5215(4) 0.039(2) Uani 1 1 d . . . . .
C42 C -0.0632(12) 0.6811(6) 0.6971(4) 0.049(3) Uani 1 1 d . . . . .
C2 C 0.3844(10) 0.6116(5) 0.6395(5) 0.041(3) Uani 1 1 d . . . . .
C28 C 0.5693(11) 0.2966(6) 0.6647(5) 0.052(3) Uani 1 1 d . . . . .
H28 H 0.5773 0.2694 0.6299 0.062 Uiso 1 1 calc R U . . .
C30 C 0.0591(10) 0.4758(5) 0.6097(4) 0.045(3) Uani 1 1 d . . . . .
H30 H 0.0716 0.5063 0.5765 0.054 Uiso 1 1 calc R U . . .
C5 C 0.5831(11) 0.5887(6) 0.5970(6) 0.058(3) Uani 1 1 d . . . . .
H5 H 0.6742 0.5731 0.5912 0.070 Uiso 1 1 calc R U . . .
C1 C 0.2841(12) 0.6092(5) 0.6885(4) 0.046(3) Uani 1 1 d . . . . .
C9 C 0.4218(9) 0.3963(5) 0.6157(4) 0.034(2) Uani 1 1 d . . . . .
C24 C 0.4742(10) 0.4014(6) 0.7218(4) 0.042(3) Uani 1 1 d . . . . .
H24 H 0.4178 0.4450 0.7261 0.051 Uiso 1 1 calc R U . . .
C31 C -0.0608(10) 0.4790(7) 0.6378(6) 0.063(3) Uani 1 1 d . . . . .
H31 H -0.1262 0.5131 0.6245 0.075 Uiso 1 1 calc R U . . .
C22 C 0.5570(11) 0.3329(6) 0.4681(5) 0.053(3) Uani 1 1 d . . . . .
H22 H 0.4755 0.3318 0.4506 0.064 Uiso 1 1 calc R U . . .
C16 C 0.1508(10) 0.4025(6) 0.4683(5) 0.050(3) Uani 1 1 d . . . . .
H16 H 0.1120 0.3691 0.4957 0.060 Uiso 1 1 calc R U . . .
C44 C 0.2629(11) 0.7927(5) 0.5522(4) 0.044(3) Uani 1 1 d . . . . .
C11 C 0.2647(10) 0.4442(5) 0.4825(4) 0.036(2) Uani 1 1 d . . . . .
C20 C 0.7864(13) 0.2973(7) 0.4654(7) 0.072(4) Uani 1 1 d . . . . .
H20 H 0.8565 0.2723 0.4472 0.086 Uiso 1 1 calc R U . . .
C6 C 0.5146(11) 0.5851(6) 0.6498(5) 0.053(3) Uani 1 1 d . . . . .
H6 H 0.5502 0.5673 0.6868 0.063 Uiso 1 1 calc R U . . .
C12 C 0.3196(10) 0.4940(6) 0.4407(4) 0.051(3) Uani 1 1 d . . . . .
H12 H 0.3960 0.5220 0.4488 0.061 Uiso 1 1 calc R U . . .
C18 C 0.7006(9) 0.3735(6) 0.5446(5) 0.055(3) Uani 1 1 d . . . . .
H18 H 0.7157 0.4001 0.5793 0.066 Uiso 1 1 calc R U . . .
C23 C 0.4878(9) 0.3645(6) 0.6683(4) 0.036(2) Uani 1 1 d . . . . .
C36 C 0.0538(14) 0.6043(7) 0.7699(5) 0.069(4) Uani 1 1 d . . . . .
H36 H 0.1279 0.5774 0.7828 0.083 Uiso 1 1 calc R U . . .
C32 C -0.0816(13) 0.4314(8) 0.6855(6) 0.073(4) Uani 1 1 d . . . . .
H32 H -0.1619 0.4324 0.7040 0.087 Uiso 1 1 calc R U . . .
C48 C 0.1966(14) 0.9201(8) 0.5938(7) 0.088(5) Uani 1 1 d . . . . .
H48 H 0.1376 0.9498 0.6156 0.105 Uiso 1 1 calc R U . . .
C15 C 0.0933(11) 0.4098(7) 0.4136(5) 0.063(3) Uani 1 1 d . . . . .
H15 H 0.0186 0.3806 0.4047 0.076 Uiso 1 1 calc R U . . .
C19 C 0.8035(11) 0.3362(7) 0.5167(6) 0.070(4) Uani 1 1 d . . . . .
H19 H 0.8860 0.3376 0.5333 0.084 Uiso 1 1 calc R U . . .
C13 C 0.2615(14) 0.5026(7) 0.3866(5) 0.071(3) Uani 1 1 d . . . . .
H13 H 0.2990 0.5367 0.3594 0.085 Uiso 1 1 calc R U . . .
C25 C 0.5443(12) 0.3734(6) 0.7688(5) 0.060(3) Uani 1 1 d . . . . .
H25 H 0.5357 0.3996 0.8040 0.072 Uiso 1 1 calc R U . . .
C43 C -0.1765(12) 0.6825(8) 0.7330(5) 0.061(3) Uani 1 1 d . . . . .
C40 C -0.2803(14) 0.7612(8) 0.6586(6) 0.076(4) Uani 1 1 d . . . . .
H40 H -0.3514 0.7899 0.6444 0.092 Uiso 1 1 calc R U . . .
C37 C -0.0577(18) 0.6067(8) 0.8048(6) 0.091(5) Uani 1 1 d . . . . .
H37 H -0.0553 0.5824 0.8409 0.109 Uiso 1 1 calc R U . . .
C41 C -0.1651(13) 0.7549(8) 0.6264(5) 0.067(4) Uani 1 1 d . . . . .
H41 H -0.1643 0.7786 0.5901 0.080 Uiso 1 1 calc R U . . .
C21 C 0.6635(16) 0.2953(7) 0.4406(5) 0.072(4) Uani 1 1 d . . . . .
H21 H 0.6513 0.2690 0.4056 0.087 Uiso 1 1 calc R U . . .
C4 C 0.4970(10) 0.6176(6) 0.5537(5) 0.049(3) Uani 1 1 d . . . . .
H4 H 0.5192 0.6260 0.5131 0.058 Uiso 1 1 calc R U . . .
C27 C 0.6389(12) 0.2691(7) 0.7127(6) 0.065(4) Uani 1 1 d . . . . .
H27 H 0.6936 0.2244 0.7093 0.078 Uiso 1 1 calc R U . . .
C14 C 0.1489(14) 0.4609(8) 0.3731(5) 0.071(4) Uani 1 1 d . . . . .
H14 H 0.1106 0.4670 0.3371 0.085 Uiso 1 1 calc R U . . .
C26 C 0.6268(11) 0.3075(7) 0.7644(5) 0.061(3) Uani 1 1 d . . . . .
H26 H 0.6735 0.2897 0.7963 0.073 Uiso 1 1 calc R U . . .
C49 C 0.1782(11) 0.8366(7) 0.5850(6) 0.068(3) Uani 1 1 d . . . . .
H49 H 0.1071 0.8109 0.6018 0.082 Uiso 1 1 calc R U . . .
C33 C 0.0173(14) 0.3819(8) 0.7060(6) 0.080(4) Uani 1 1 d . . . . .
H33 H 0.0029 0.3491 0.7380 0.096 Uiso 1 1 calc R U . . .
C38 C -0.1700(16) 0.6440(8) 0.7871(6) 0.085(5) Uani 1 1 d . . . . .
H38 H -0.2427 0.6439 0.8110 0.103 Uiso 1 1 calc R U . . .
C45 C 0.3682(12) 0.8302(7) 0.5281(6) 0.088(4) Uani 1 1 d . . . . .
H45 H 0.4261 0.8006 0.5056 0.105 Uiso 1 1 calc R U . . .
C47 C 0.3018(17) 0.9567(8) 0.5699(7) 0.100(5) Uani 1 1 d . . . . .
H47 H 0.3153 1.0119 0.5755 0.120 Uiso 1 1 calc R U . . .
C39 C -0.2859(13) 0.7243(7) 0.7110(6) 0.071(4) Uani 1 1 d . . . . .
H39 H -0.3622 0.7267 0.7325 0.085 Uiso 1 1 calc R U . . .
C46 C 0.3890(17) 0.9126(9) 0.5372(7) 0.120(6) Uani 1 1 d . . . . .
H46 H 0.4615 0.9378 0.5213 0.144 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 C3 1.934(10) . ?
Se1 C44 1.958(10) . ?
Co1 C7 1.992(9) . ?
Co1 C9 1.998(10) . ?
Co1 C8 2.010(10) . ?
Co1 C10 2.016(9) . ?
Co1 C2 2.065(10) . ?
Co1 C4 2.085(10) . ?
Co1 C3 2.086(10) . ?
Co1 C6 2.098(10) . ?
Co1 C5 2.104(11) . ?
C8 C7 1.443(12) . ?
C8 C17 1.467(12) . ?
C8 C9 1.480(12) . ?
N1 C1 1.365(12) . ?
N1 C35 1.427(12) . ?
N1 H1 0.8600 . ?
C7 C10 1.485(13) . ?
C7 C11 1.508(13) . ?
C29 C34 1.375(13) . ?
C29 C30 1.416(12) . ?
C29 C10 1.489(13) . ?
O1 C1 1.221(11) . ?
C34 C33 1.388(15) . ?
C34 H34 0.9300 . ?
N2 C41 1.322(13) . ?
N2 C42 1.385(12) . ?
C35 C36 1.375(14) . ?
C35 C42 1.453(14) . ?
C3 C4 1.430(13) . ?
C3 C2 1.445(13) . ?
C10 C9 1.462(13) . ?
C17 C22 1.410(13) . ?
C17 C18 1.424(13) . ?
C42 C43 1.431(14) . ?
C2 C6 1.426(13) . ?
C2 C1 1.534(14) . ?
C28 C23 1.401(12) . ?
C28 C27 1.401(14) . ?
C28 H28 0.9300 . ?
C30 C31 1.395(14) . ?
C30 H30 0.9300 . ?
C5 C6 1.414(15) . ?
C5 C4 1.422(14) . ?
C5 H5 0.9800 . ?
C9 C23 1.492(12) . ?
C24 C25 1.386(13) . ?
C24 C23 1.392(12) . ?
C24 H24 0.9300 . ?
C31 C32 1.374(16) . ?
C31 H31 0.9300 . ?
C22 C21 1.410(15) . ?
C22 H22 0.9300 . ?
C16 C11 1.397(13) . ?
C16 C15 1.407(14) . ?
C16 H16 0.9300 . ?
C44 C49 1.365(13) . ?
C44 C45 1.366(14) . ?
C11 C12 1.392(12) . ?
C20 C19 1.367(16) . ?
C20 C21 1.387(17) . ?
C20 H20 0.9300 . ?
C6 H6 0.9800 . ?
C12 C13 1.398(14) . ?
C12 H12 0.9300 . ?
C18 C19 1.384(14) . ?
C18 H18 0.9300 . ?
C36 C37 1.404(17) . ?
C36 H36 0.9300 . ?
C32 C33 1.388(16) . ?
C32 H32 0.9300 . ?
C48 C47 1.356(18) . ?
C48 C49 1.405(15) . ?
C48 H48 0.9300 . ?
C15 C14 1.385(15) . ?
C15 H15 0.9300 . ?
C19 H19 0.9300 . ?
C13 C14 1.382(16) . ?
C13 H13 0.9300 . ?
C25 C26 1.382(13) . ?
C25 H25 0.9300 . ?
C43 C38 1.411(17) . ?
C43 C39 1.414(16) . ?
C40 C39 1.364(16) . ?
C40 C41 1.403(16) . ?
C40 H40 0.9300 . ?
C37 C38 1.370(18) . ?
C37 H37 0.9300 . ?
C41 H41 0.9300 . ?
C21 H21 0.9300 . ?
C4 H4 0.9800 . ?
C27 C26 1.364(16) . ?
C27 H27 0.9300 . ?
C14 H14 0.9300 . ?
C26 H26 0.9300 . ?
C49 H49 0.9300 . ?
C33 H33 0.9300 . ?
C38 H38 0.9300 . ?
C45 C46 1.392(17) . ?
C45 H45 0.9300 . ?
C47 C46 1.381(18) . ?
C47 H47 0.9300 . ?
C39 H39 0.9300 . ?
C46 H46 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
C3 Se1 C44 97.7(4) . . ?
C7 Co1 C9 62.7(4) . . ?
C7 Co1 C8 42.3(4) . . ?
C9 Co1 C8 43.3(3) . . ?
C7 Co1 C10 43.5(4) . . ?
C9 Co1 C10 42.7(4) . . ?
C8 Co1 C10 62.0(4) . . ?
C7 Co1 C2 141.6(4) . . ?
C9 Co1 C2 125.8(4) . . ?
C8 Co1 C2 168.8(4) . . ?
C10 Co1 C2 112.9(4) . . ?
C7 Co1 C4 120.8(4) . . ?
C9 Co1 C4 156.9(4) . . ?
C8 Co1 C4 121.4(4) . . ?
C10 Co1 C4 156.4(4) . . ?
C2 Co1 C4 67.6(4) . . ?
C7 Co1 C3 118.7(4) . . ?
C9 Co1 C3 162.1(4) . . ?
C8 Co1 C3 150.5(4) . . ?
C10 Co1 C3 124.3(4) . . ?
C2 Co1 C3 40.7(4) . . ?
C4 Co1 C3 40.1(4) . . ?
C7 Co1 C6 172.3(4) . . ?
C9 Co1 C6 109.9(4) . . ?
C8 Co1 C6 134.2(4) . . ?
C10 Co1 C6 129.9(4) . . ?
C2 Co1 C6 40.1(4) . . ?
C4 Co1 C6 66.8(4) . . ?
C3 Co1 C6 67.5(4) . . ?
C7 Co1 C5 145.6(5) . . ?
C9 Co1 C5 123.1(4) . . ?
C8 Co1 C5 114.9(4) . . ?
C10 Co1 C5 163.8(4) . . ?
C2 Co1 C5 66.9(4) . . ?
C4 Co1 C5 39.7(4) . . ?
C3 Co1 C5 67.0(4) . . ?
C6 Co1 C5 39.3(4) . . ?
C7 C8 C17 134.4(9) . . ?
C7 C8 C9 90.5(8) . . ?
C17 C8 C9 133.4(9) . . ?
C7 C8 Co1 68.2(5) . . ?
C17 C8 Co1 131.9(6) . . ?
C9 C8 Co1 67.9(5) . . ?
C1 N1 C35 127.3(9) . . ?
C1 N1 H1 116.3 . . ?
C35 N1 H1 116.3 . . ?
C8 C7 C10 90.2(8) . . ?
C8 C7 C11 132.6(9) . . ?
C10 C7 C11 136.1(8) . . ?
C8 C7 Co1 69.5(6) . . ?
C10 C7 Co1 69.1(5) . . ?
C11 C7 Co1 127.8(6) . . ?
C34 C29 C30 117.1(10) . . ?
C34 C29 C10 121.0(9) . . ?
C30 C29 C10 121.8(9) . . ?
C29 C34 C33 122.0(12) . . ?
C29 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C41 N2 C42 116.0(10) . . ?
C36 C35 N1 124.2(11) . . ?
C36 C35 C42 118.6(11) . . ?
N1 C35 C42 117.1(9) . . ?
C4 C3 C2 106.9(9) . . ?
C4 C3 Se1 122.8(8) . . ?
C2 C3 Se1 130.4(7) . . ?
C4 C3 Co1 69.9(5) . . ?
C2 C3 Co1 68.9(5) . . ?
Se1 C3 Co1 127.0(4) . . ?
C9 C10 C7 89.6(7) . . ?
C9 C10 C29 135.7(8) . . ?
C7 C10 C29 134.2(8) . . ?
C9 C10 Co1 68.0(5) . . ?
C7 C10 Co1 67.4(5) . . ?
C29 C10 Co1 127.5(6) . . ?
C22 C17 C18 116.2(9) . . ?
C22 C17 C8 121.9(10) . . ?
C18 C17 C8 121.6(9) . . ?
N2 C42 C43 123.3(11) . . ?
N2 C42 C35 116.6(10) . . ?
C43 C42 C35 120.0(10) . . ?
C6 C2 C3 108.1(9) . . ?
C6 C2 C1 119.8(10) . . ?
C3 C2 C1 132.0(9) . . ?
C6 C2 Co1 71.2(6) . . ?
C3 C2 Co1 70.4(5) . . ?
C1 C2 Co1 121.6(6) . . ?
C23 C28 C27 121.2(10) . . ?
C23 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C31 C30 C29 121.3(10) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C6 C5 C4 108.6(10) . . ?
C6 C5 Co1 70.1(6) . . ?
C4 C5 Co1 69.4(6) . . ?
C6 C5 H5 125.7 . . ?
C4 C5 H5 125.7 . . ?
Co1 C5 H5 125.7 . . ?
O1 C1 N1 123.6(11) . . ?
O1 C1 C2 118.0(11) . . ?
N1 C1 C2 118.3(9) . . ?
C10 C9 C8 89.6(7) . . ?
C10 C9 C23 136.2(9) . . ?
C8 C9 C23 133.6(9) . . ?
C10 C9 Co1 69.3(5) . . ?
C8 C9 Co1 68.8(5) . . ?
C23 C9 Co1 126.2(6) . . ?
C25 C24 C23 120.4(10) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C32 C31 C30 119.6(12) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C21 C22 C17 121.1(11) . . ?
C21 C22 H22 119.5 . . ?
C17 C22 H22 119.5 . . ?
C11 C16 C15 121.5(10) . . ?
C11 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C49 C44 C45 119.5(10) . . ?
C49 C44 Se1 119.8(8) . . ?
C45 C44 Se1 120.7(9) . . ?
C12 C11 C16 117.7(9) . . ?
C12 C11 C7 121.3(9) . . ?
C16 C11 C7 120.7(9) . . ?
C19 C20 C21 119.4(11) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C5 C6 C2 108.0(10) . . ?
C5 C6 Co1 70.6(6) . . ?
C2 C6 Co1 68.7(6) . . ?
C5 C6 H6 126.0 . . ?
C2 C6 H6 126.0 . . ?
Co1 C6 H6 126.0 . . ?
C11 C12 C13 121.0(10) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C19 C18 C17 121.6(11) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C24 C23 C28 117.5(9) . . ?
C24 C23 C9 122.2(9) . . ?
C28 C23 C9 120.3(9) . . ?
C35 C36 C37 120.7(13) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C31 C32 C33 120.0(12) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C47 C48 C49 119.0(14) . . ?
C47 C48 H48 120.5 . . ?
C49 C48 H48 120.5 . . ?
C14 C15 C16 119.6(11) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C20 C19 C18 121.3(12) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C14 C13 C12 120.7(11) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C26 C25 C24 121.5(11) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C38 C43 C39 125.4(12) . . ?
C38 C43 C42 118.3(13) . . ?
C39 C43 C42 116.3(12) . . ?
C39 C40 C41 118.6(13) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C38 C37 C36 121.7(13) . . ?
C38 C37 H37 119.1 . . ?
C36 C37 H37 119.1 . . ?
N2 C41 C40 125.3(12) . . ?
N2 C41 H41 117.4 . . ?
C40 C41 H41 117.4 . . ?
C20 C21 C22 120.5(12) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C5 C4 C3 108.4(10) . . ?
C5 C4 Co1 70.9(6) . . ?
C3 C4 Co1 70.0(6) . . ?
C5 C4 H4 125.8 . . ?
C3 C4 H4 125.8 . . ?
Co1 C4 H4 125.8 . . ?
C26 C27 C28 120.2(11) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C13 C14 C15 119.6(12) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C27 C26 C25 119.1(11) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C44 C49 C48 121.1(12) . . ?
C44 C49 H49 119.5 . . ?
C48 C49 H49 119.5 . . ?
C34 C33 C32 120.0(12) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C37 C38 C43 120.6(13) . . ?
C37 C38 H38 119.7 . . ?
C43 C38 H38 119.7 . . ?
C44 C45 C46 120.1(13) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C48 C47 C46 120.4(14) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 H47 119.8 . . ?
C40 C39 C43 120.4(13) . . ?
C40 C39 H39 119.8 . . ?
C43 C39 H39 119.8 . . ?
C47 C46 C45 120.0(14) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?

_refine_diff_density_max         1.047
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.081

####################################################################### 
# 
# 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_6b
_database_code_depnum_ccdc_archive 'CCDC 1523206'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H43 B Co N O3 S, C H Cl3'
_chemical_formula_sum            'C48 H44 B Cl3 Co N O3 S'
_chemical_formula_weight         890.99

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.257(2)
_cell_length_b                   11.746(2)
_cell_length_c                   18.873(4)
_cell_angle_alpha                96.25(3)
_cell_angle_beta                 92.91(3)
_cell_angle_gamma                94.13(3)
_cell_volume                     2250.4(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1608
_cell_measurement_theta_min      2.338
_cell_measurement_theta_max      19.126

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_F_000             924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.195
_exptl_absorpt_coefficient_mu    0.647
_shelx_estimated_absorpt_T_min   0.808
_shelx_estimated_absorpt_T_max   0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14974
_diffrn_reflns_av_unetI/netI     0.1992
_diffrn_reflns_av_R_equivalents  0.1101
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.162
_diffrn_reflns_theta_max         28.466
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             10383
_reflns_number_gt                6758
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0458P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10383
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1506
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   0.776
_refine_ls_restrained_S_all      0.776
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.41001(5) 0.62386(4) 0.78051(3) 0.04104(18) Uani 1 1 d . . . . .
S1 S 0.56831(17) 0.23430(13) 0.51631(8) 0.1026(5) Uani 1 1 d . . . . .
O1 O 0.2653(3) 0.3299(2) 0.70033(17) 0.0797(10) Uani 1 1 d . . . . .
O2 O 0.6516(3) 0.5099(2) 0.61433(16) 0.0683(9) Uani 1 1 d . . . . .
O3 O 0.6721(3) 0.7057(2) 0.64004(16) 0.0701(9) Uani 1 1 d . . . . .
N1 N 0.4636(4) 0.3381(3) 0.6507(2) 0.0595(11) Uani 1 1 d . . . . .
C1 C 0.3586(5) 0.3854(4) 0.6795(2) 0.0555(12) Uani 1 1 d . . . . .
C2 C 0.3590(4) 0.5149(3) 0.6867(2) 0.0454(10) Uani 1 1 d . . . . .
C3 C 0.2467(4) 0.5686(4) 0.7122(2) 0.0516(11) Uani 1 1 d . . . . .
H3 H 0.1658 0.5287 0.7255 0.062 Uiso 1 1 calc R U . . .
C4 C 0.2714(4) 0.6884(4) 0.7140(2) 0.0535(11) Uani 1 1 d . . . . .
H4 H 0.2108 0.7459 0.7291 0.064 Uiso 1 1 calc R U . . .
C5 C 0.3971(4) 0.7120(3) 0.6905(2) 0.0495(11) Uani 1 1 d . . . . .
H5 H 0.4383 0.7890 0.6872 0.059 Uiso 1 1 calc R U . . .
C6 C 0.4570(4) 0.6067(3) 0.67279(19) 0.0439(10) Uani 1 1 d . . . . .
C7 C 0.3870(4) 0.6757(3) 0.88319(19) 0.0423(10) Uani 1 1 d . . . . .
C8 C 0.5161(4) 0.7171(3) 0.86075(19) 0.0431(10) Uani 1 1 d . . . . .
C9 C 0.5534(4) 0.5976(3) 0.85125(19) 0.0439(10) Uani 1 1 d . . . . .
C10 C 0.4249(4) 0.5575(3) 0.8733(2) 0.0443(10) Uani 1 1 d . . . . .
C11 C 0.2714(4) 0.7298(4) 0.9127(2) 0.0485(11) Uani 1 1 d . . . . .
C12 C 0.2025(4) 0.6803(4) 0.9639(2) 0.0622(13) Uani 1 1 d . . . . .
H12 H 0.2299 0.6138 0.9807 0.075 Uiso 1 1 calc R U . . .
C13 C 0.0930(5) 0.7282(5) 0.9907(3) 0.0864(18) Uani 1 1 d . . . . .
H13 H 0.0489 0.6938 1.0257 0.104 Uiso 1 1 calc R U . . .
C14 C 0.0488(5) 0.8247(6) 0.9669(3) 0.0922(19) Uani 1 1 d . . . . .
H14 H -0.0270 0.8542 0.9836 0.111 Uiso 1 1 calc R U . . .
C15 C 0.1186(5) 0.8779(4) 0.9175(3) 0.0827(16) Uani 1 1 d . . . . .
H15 H 0.0917 0.9458 0.9026 0.099 Uiso 1 1 calc R U . . .
C16 C 0.2298(5) 0.8311(4) 0.8894(2) 0.0656(13) Uani 1 1 d . . . . .
H16 H 0.2755 0.8671 0.8556 0.079 Uiso 1 1 calc R U . . .
C17 C 0.5934(4) 0.8292(3) 0.8611(2) 0.0462(10) Uani 1 1 d . . . . .
C18 C 0.5717(4) 0.9242(4) 0.9094(2) 0.0606(13) Uani 1 1 d . . . . .
H18 H 0.5034 0.9199 0.9398 0.073 Uiso 1 1 calc R U . . .
C19 C 0.6530(6) 1.0255(4) 0.9118(3) 0.0786(16) Uani 1 1 d . . . . .
H19 H 0.6382 1.0884 0.9439 0.094 Uiso 1 1 calc R U . . .
C20 C 0.7546(5) 1.0334(4) 0.8672(3) 0.0803(16) Uani 1 1 d . . . . .
H20 H 0.8092 1.1006 0.8695 0.096 Uiso 1 1 calc R U . . .
C21 C 0.7744(5) 0.9397(4) 0.8190(3) 0.0776(15) Uani 1 1 d . . . . .
H21 H 0.8419 0.9444 0.7881 0.093 Uiso 1 1 calc R U . . .
C22 C 0.6957(4) 0.8405(4) 0.8162(2) 0.0606(12) Uani 1 1 d . . . . .
H22 H 0.7110 0.7786 0.7834 0.073 Uiso 1 1 calc R U . . .
C23 C 0.6743(4) 0.5388(3) 0.8374(2) 0.0483(10) Uani 1 1 d . . . . .
C24 C 0.6651(4) 0.4287(4) 0.8001(2) 0.0584(12) Uani 1 1 d . . . . .
H24 H 0.5831 0.3944 0.7835 0.070 Uiso 1 1 calc R U . . .
C25 C 0.7744(5) 0.3696(4) 0.7873(3) 0.0763(15) Uani 1 1 d . . . . .
H25 H 0.7659 0.2967 0.7621 0.092 Uiso 1 1 calc R U . . .
C26 C 0.8959(5) 0.4190(5) 0.8121(3) 0.0877(17) Uani 1 1 d . . . . .
H26 H 0.9703 0.3803 0.8031 0.105 Uiso 1 1 calc R U . . .
C27 C 0.9069(5) 0.5273(5) 0.8507(3) 0.101(2) Uani 1 1 d . . . . .
H27 H 0.9893 0.5600 0.8679 0.122 Uiso 1 1 calc R U . . .
C28 C 0.7976(4) 0.5881(4) 0.8642(3) 0.0770(15) Uani 1 1 d . . . . .
H28 H 0.8063 0.6601 0.8906 0.092 Uiso 1 1 calc R U . . .
C29 C 0.3745(4) 0.4434(3) 0.8924(2) 0.0461(10) Uani 1 1 d . . . . .
C30 C 0.4558(5) 0.3796(4) 0.9306(2) 0.0632(13) Uani 1 1 d . . . . .
H30 H 0.5415 0.4082 0.9440 0.076 Uiso 1 1 calc R U . . .
C31 C 0.4104(6) 0.2737(4) 0.9490(3) 0.0798(15) Uani 1 1 d . . . . .
H31 H 0.4652 0.2329 0.9759 0.096 Uiso 1 1 calc R U . . .
C32 C 0.2857(6) 0.2279(4) 0.9283(3) 0.0767(15) Uani 1 1 d . . . . .
H32 H 0.2571 0.1556 0.9399 0.092 Uiso 1 1 calc R U . . .
C33 C 0.2035(5) 0.2889(4) 0.8905(3) 0.0808(16) Uani 1 1 d . . . . .
H33 H 0.1187 0.2588 0.8765 0.097 Uiso 1 1 calc R U . . .
C34 C 0.2483(4) 0.3963(4) 0.8734(2) 0.0664(13) Uani 1 1 d . . . . .
H34 H 0.1917 0.4380 0.8484 0.080 Uiso 1 1 calc R U . . .
C35 C 0.4930(5) 0.2207(4) 0.6526(3) 0.0625(13) Uani 1 1 d . . . . .
C36 C 0.4722(5) 0.1669(4) 0.7134(3) 0.0793(16) Uani 1 1 d . . . . .
H36 H 0.4323 0.2036 0.7517 0.095 Uiso 1 1 calc R U . . .
C37 C 0.5130(6) 0.0552(5) 0.7157(4) 0.099(2) Uani 1 1 d . . . . .
H37 H 0.4988 0.0172 0.7556 0.119 Uiso 1 1 calc R U . . .
C38 C 0.5743(6) 0.0016(5) 0.6584(4) 0.109(2) Uani 1 1 d . . . . .
H38 H 0.6030 -0.0712 0.6608 0.131 Uiso 1 1 calc R U . . .
C39 C 0.5923(5) 0.0551(5) 0.5997(3) 0.0922(18) Uani 1 1 d . . . . .
H39 H 0.6326 0.0177 0.5617 0.111 Uiso 1 1 calc R U . . .
C40 C 0.5516(5) 0.1660(4) 0.5941(3) 0.0736(15) Uani 1 1 d . . . . .
C41 C 0.6987(6) 0.1639(5) 0.4721(3) 0.136(2) Uani 1 1 d . . . . .
H41A H 0.7761 0.1720 0.5037 0.204 Uiso 1 1 calc R U . . .
H41B H 0.7169 0.1987 0.4296 0.204 Uiso 1 1 calc R U . . .
H41C H 0.6722 0.0839 0.4597 0.204 Uiso 1 1 calc R U . . .
C42 C 0.7696(5) 0.5497(4) 0.5780(3) 0.0694(14) Uani 1 1 d . . . . .
C43 C 0.7987(5) 0.6767(5) 0.6122(3) 0.0798(15) Uani 1 1 d . . . . .
C44 C 0.7264(6) 0.5392(5) 0.4981(2) 0.111(2) Uani 1 1 d . . . . .
H44A H 0.6982 0.4606 0.4817 0.166 Uiso 1 1 calc R U . . .
H44B H 0.7987 0.5638 0.4716 0.166 Uiso 1 1 calc R U . . .
H44C H 0.6555 0.5866 0.4912 0.166 Uiso 1 1 calc R U . . .
C45 C 0.8759(5) 0.4666(5) 0.5907(3) 0.114(2) Uani 1 1 d . . . . .
H45A H 0.8868 0.4594 0.6408 0.172 Uiso 1 1 calc R U . . .
H45B H 0.9572 0.4960 0.5741 0.172 Uiso 1 1 calc R U . . .
H45C H 0.8499 0.3926 0.5651 0.172 Uiso 1 1 calc R U . . .
C46 C 0.8965(5) 0.6890(5) 0.6765(3) 0.125(2) Uani 1 1 d . . . . .
H46A H 0.8895 0.7613 0.7045 0.187 Uiso 1 1 calc R U . . .
H46B H 0.9836 0.6856 0.6605 0.187 Uiso 1 1 calc R U . . .
H46C H 0.8781 0.6276 0.7051 0.187 Uiso 1 1 calc R U . . .
C47 C 0.8376(7) 0.7618(5) 0.5611(4) 0.143(3) Uani 1 1 d . . . . .
H47A H 0.7737 0.7549 0.5216 0.215 Uiso 1 1 calc R U . . .
H47B H 0.9217 0.7462 0.5439 0.215 Uiso 1 1 calc R U . . .
H47C H 0.8420 0.8383 0.5853 0.215 Uiso 1 1 calc R U . . .
B1 B 0.5953(5) 0.6065(5) 0.6431(3) 0.0529(13) Uani 1 1 d . . . . .
Cl1 Cl 0.1054(3) 0.0602(2) 0.58493(14) 0.2283(13) Uani 1 1 d . . . . .
Cl2 Cl -0.0578(2) 0.14022(19) 0.68798(17) 0.2151(13) Uani 1 1 d . . . . .
Cl3 Cl 0.1343(2) -0.0034(2) 0.72207(16) 0.2156(13) Uani 1 1 d . . . . .
C48 C 0.0963(5) 0.1053(4) 0.6732(3) 0.0983(19) Uani 1 1 d . . . . .
H48 H 0.1580 0.1726 0.6870 0.118 Uiso 1 1 calc R U . . .
H1 H 0.522(3) 0.381(3) 0.6347(18) 0.037(12) Uiso 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
Co1 C8 1.994(4) . ?
Co1 C10 1.995(4) . ?
Co1 C7 1.998(4) . ?
Co1 C9 1.999(4) . ?
Co1 C3 2.081(4) . ?
Co1 C4 2.086(4) . ?
Co1 C2 2.088(4) . ?
Co1 C5 2.087(4) . ?
Co1 C6 2.105(4) . ?
S1 C40 1.758(5) . ?
S1 C41 1.814(5) . ?
O1 C1 1.224(5) . ?
O2 B1 1.381(6) . ?
O2 C42 1.491(5) . ?
O3 B1 1.367(5) . ?
O3 C43 1.473(5) . ?
N1 C1 1.357(5) . ?
N1 C35 1.436(5) . ?
N1 H1 0.84(3) . ?
C1 C2 1.513(5) . ?
C2 C3 1.432(5) . ?
C2 C6 1.475(5) . ?
C3 C4 1.409(5) . ?
C3 H3 0.9800 . ?
C4 C5 1.403(5) . ?
C4 H4 0.9800 . ?
C5 C6 1.435(5) . ?
C5 H5 0.9800 . ?
C6 B1 1.552(6) . ?
C7 C10 1.463(5) . ?
C7 C8 1.475(5) . ?
C7 C11 1.490(5) . ?
C8 C9 1.475(5) . ?
C8 C17 1.487(5) . ?
C9 C10 1.463(5) . ?
C9 C23 1.483(5) . ?
C10 C29 1.490(5) . ?
C11 C12 1.380(5) . ?
C11 C16 1.400(5) . ?
C12 C13 1.386(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.363(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.379(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.404(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.389(5) . ?
C17 C18 1.401(5) . ?
C18 C19 1.398(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.376(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.384(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.363(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C28 1.398(5) . ?
C23 C24 1.398(5) . ?
C24 C25 1.378(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.373(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.390(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.392(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.384(5) . ?
C29 C30 1.387(5) . ?
C30 C31 1.383(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.372(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.366(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.389(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.387(6) . ?
C35 C40 1.400(6) . ?
C36 C37 1.410(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.392(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.346(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.410(6) . ?
C39 H39 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C44 1.540(6) . ?
C42 C45 1.542(6) . ?
C42 C43 1.562(6) . ?
C43 C47 1.509(7) . ?
C43 C46 1.522(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
Cl1 C48 1.702(6) . ?
Cl2 C48 1.690(5) . ?
Cl3 C48 1.710(6) . ?
C48 H48 0.9800 . ?

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
C8 Co1 C10 62.70(15) . . ?
C8 Co1 C7 43.38(14) . . ?
C10 Co1 C7 42.97(14) . . ?
C8 Co1 C9 43.37(14) . . ?
C10 Co1 C9 42.97(14) . . ?
C7 Co1 C9 62.71(16) . . ?
C8 Co1 C3 157.79(16) . . ?
C10 Co1 C3 117.55(16) . . ?
C7 Co1 C3 119.76(16) . . ?
C9 Co1 C3 152.56(16) . . ?
C8 Co1 C4 124.59(16) . . ?
C10 Co1 C4 140.43(17) . . ?
C7 Co1 C4 111.30(16) . . ?
C9 Co1 C4 167.67(16) . . ?
C3 Co1 C4 39.51(14) . . ?
C8 Co1 C2 161.54(15) . . ?
C10 Co1 C2 119.36(15) . . ?
C7 Co1 C2 151.50(15) . . ?
C9 Co1 C2 123.77(16) . . ?
C3 Co1 C2 40.17(14) . . ?
C4 Co1 C2 66.98(16) . . ?
C8 Co1 C5 111.39(16) . . ?
C10 Co1 C5 173.31(16) . . ?
C7 Co1 C5 130.74(16) . . ?
C9 Co1 C5 135.31(16) . . ?
C3 Co1 C5 66.53(15) . . ?
C4 Co1 C5 39.28(14) . . ?
C2 Co1 C5 67.27(15) . . ?
C8 Co1 C6 125.65(15) . . ?
C10 Co1 C6 145.49(16) . . ?
C7 Co1 C6 166.85(15) . . ?
C9 Co1 C6 115.80(16) . . ?
C3 Co1 C6 68.17(15) . . ?
C4 Co1 C6 67.32(16) . . ?
C2 Co1 C6 41.19(14) . . ?
C5 Co1 C6 40.02(14) . . ?
C40 S1 C41 104.0(3) . . ?
B1 O2 C42 107.4(3) . . ?
B1 O3 C43 109.0(4) . . ?
C1 N1 C35 124.9(4) . . ?
C1 N1 H1 119(2) . . ?
C35 N1 H1 115(3) . . ?
O1 C1 N1 124.2(4) . . ?
O1 C1 C2 118.5(4) . . ?
N1 C1 C2 117.3(4) . . ?
C3 C2 C6 107.6(3) . . ?
C3 C2 C1 119.5(4) . . ?
C6 C2 C1 132.9(4) . . ?
C3 C2 Co1 69.7(2) . . ?
C6 C2 Co1 70.0(2) . . ?
C1 C2 Co1 125.1(3) . . ?
C4 C3 C2 108.4(4) . . ?
C4 C3 Co1 70.4(2) . . ?
C2 C3 Co1 70.2(2) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
Co1 C3 H3 125.8 . . ?
C5 C4 C3 108.8(4) . . ?
C5 C4 Co1 70.4(2) . . ?
C3 C4 Co1 70.0(2) . . ?
C5 C4 H4 125.6 . . ?
C3 C4 H4 125.6 . . ?
Co1 C4 H4 125.6 . . ?
C4 C5 C6 109.9(3) . . ?
C4 C5 Co1 70.3(2) . . ?
C6 C5 Co1 70.6(2) . . ?
C4 C5 H5 125.0 . . ?
C6 C5 H5 125.0 . . ?
Co1 C5 H5 125.0 . . ?
C5 C6 C2 105.3(3) . . ?
C5 C6 B1 121.2(4) . . ?
C2 C6 B1 133.4(4) . . ?
C5 C6 Co1 69.3(2) . . ?
C2 C6 Co1 68.8(2) . . ?
B1 C6 Co1 127.6(3) . . ?
C10 C7 C8 89.9(3) . . ?
C10 C7 C11 133.8(4) . . ?
C8 C7 C11 135.9(3) . . ?
C10 C7 Co1 68.4(2) . . ?
C8 C7 Co1 68.2(2) . . ?
C11 C7 Co1 126.3(3) . . ?
C9 C8 C7 89.6(3) . . ?
C9 C8 C17 132.0(3) . . ?
C7 C8 C17 137.2(4) . . ?
C9 C8 Co1 68.5(2) . . ?
C7 C8 Co1 68.4(2) . . ?
C17 C8 Co1 129.1(3) . . ?
C10 C9 C8 89.9(3) . . ?
C10 C9 C23 132.5(4) . . ?
C8 C9 C23 136.9(3) . . ?
C10 C9 Co1 68.4(2) . . ?
C8 C9 Co1 68.1(2) . . ?
C23 C9 Co1 127.8(3) . . ?
C7 C10 C9 90.6(3) . . ?
C7 C10 C29 136.9(4) . . ?
C9 C10 C29 131.1(4) . . ?
C7 C10 Co1 68.6(2) . . ?
C9 C10 Co1 68.7(2) . . ?
C29 C10 Co1 130.1(3) . . ?
C12 C11 C16 118.5(4) . . ?
C12 C11 C7 120.3(4) . . ?
C16 C11 C7 121.2(4) . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 121.2(5) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 118.8(5) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C14 C15 C16 121.0(5) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 119.4(5) . . ?
C11 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C22 C17 C18 117.8(4) . . ?
C22 C17 C8 120.5(4) . . ?
C18 C17 C8 121.5(4) . . ?
C19 C18 C17 119.9(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C20 C19 C18 120.9(4) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 119.0(4) . . ?
C19 C20 H20 120.5 . . ?
C21 C20 H20 120.5 . . ?
C22 C21 C20 120.6(4) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C17 121.9(4) . . ?
C21 C22 H22 119.1 . . ?
C17 C22 H22 119.1 . . ?
C28 C23 C24 118.7(4) . . ?
C28 C23 C9 121.6(4) . . ?
C24 C23 C9 119.6(4) . . ?
C25 C24 C23 121.7(4) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C26 C25 C24 119.7(4) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 119.5(4) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C26 C27 C28 121.5(4) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C23 118.8(4) . . ?
C27 C28 H28 120.6 . . ?
C23 C28 H28 120.6 . . ?
C34 C29 C30 117.4(4) . . ?
C34 C29 C10 122.9(4) . . ?
C30 C29 C10 119.7(4) . . ?
C31 C30 C29 120.4(4) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C32 C31 C30 121.0(5) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 119.8(5) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 119.2(5) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C29 C34 C33 122.2(4) . . ?
C29 C34 H34 118.9 . . ?
C33 C34 H34 118.9 . . ?
C36 C35 C40 121.4(5) . . ?
C36 C35 N1 120.1(5) . . ?
C40 C35 N1 118.3(5) . . ?
C35 C36 C37 118.5(5) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 H36 120.8 . . ?
C38 C37 C36 120.3(6) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C39 C38 C37 120.2(6) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 121.8(6) . . ?
C38 C39 H39 119.1 . . ?
C40 C39 H39 119.1 . . ?
C35 C40 C39 117.7(5) . . ?
C35 C40 S1 120.0(4) . . ?
C39 C40 S1 122.3(5) . . ?
S1 C41 H41A 109.5 . . ?
S1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
S1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O2 C42 C44 105.4(4) . . ?
O2 C42 C45 107.4(4) . . ?
C44 C42 C45 110.0(4) . . ?
O2 C42 C43 103.1(3) . . ?
C44 C42 C43 113.2(4) . . ?
C45 C42 C43 116.7(4) . . ?
O3 C43 C47 108.3(5) . . ?
O3 C43 C46 106.2(4) . . ?
C47 C43 C46 110.3(5) . . ?
O3 C43 C42 103.0(4) . . ?
C47 C43 C42 115.4(5) . . ?
C46 C43 C42 113.0(5) . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 B1 O2 112.9(4) . . ?
O3 B1 C6 122.1(4) . . ?
O2 B1 C6 125.0(4) . . ?
Cl2 C48 Cl1 109.0(4) . . ?
Cl2 C48 Cl3 109.7(3) . . ?
Cl1 C48 Cl3 109.0(3) . . ?
Cl2 C48 H48 109.7 . . ?
Cl1 C48 H48 109.7 . . ?
Cl3 C48 H48 109.7 . . ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1523202'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H40 B Co N2 O3'
_chemical_formula_sum            'C45 H40 B Co N2 O3'
_chemical_formula_weight         726.53

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'
B B 0.0013 0.0007 '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'

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

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

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

_cell_length_a                   11.64(5)
_cell_length_b                   13.37(5)
_cell_length_c                   13.68(6)
_cell_angle_alpha                65.93(10)
_cell_angle_beta                 78.53(7)
_cell_angle_gamma                77.94(7)
_cell_volume                     1886(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2332
_cell_measurement_theta_min      2.283
_cell_measurement_theta_max      25.003

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.199
_exptl_absorpt_coefficient_mu    0.498
_shelx_estimated_absorpt_T_min   0.843
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11692
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.851
_diffrn_reflns_theta_max         28.231
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             8470
_reflns_number_gt                4964
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0365P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8470
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1025
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_restrained_S_all      0.832
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.63897(3) 0.16106(3) 0.21915(3) 0.03391(12) Uani 1 1 d . . . . .
O1 O 0.32522(18) 0.15877(17) 0.36569(16) 0.0608(6) Uani 1 1 d . . . . .
O2 O 0.65171(16) 0.16602(15) 0.52563(14) 0.0479(5) Uani 1 1 d . . . . .
O3 O 0.83597(16) 0.09608(14) 0.45989(13) 0.0446(5) Uani 1 1 d . . . . .
N1 N 0.4213(2) 0.20207(18) 0.47155(18) 0.0419(6) Uani 1 1 d . . . . .
N2 N 0.3631(2) 0.2998(2) 0.5835(2) 0.0596(7) Uani 1 1 d . . . . .
C0AA C 0.9925(3) 0.1962(3) -0.1244(3) 0.0678(10) Uani 1 1 d . . . . .
H0AA H 1.0583 0.2316 -0.1601 0.081 Uiso 1 1 calc R U . . .
C1 C 0.4178(3) 0.1540(2) 0.4005(2) 0.0412(7) Uani 1 1 d . . . . .
C1AA C 0.9763(3) 0.1045(3) -0.1412(3) 0.0746(11) Uani 1 1 d . . . . .
H1AA H 1.0313 0.0780 -0.1876 0.089 Uiso 1 1 calc R U . . .
C2 C 0.5326(2) 0.09199(19) 0.36629(18) 0.0333(6) Uani 1 1 d . . . . .
C2AA C 0.8767(3) 0.0527(3) -0.0876(2) 0.0650(9) Uani 1 1 d . . . . .
H2AA H 0.8663 -0.0095 -0.0975 0.078 Uiso 1 1 calc R U . . .
C3 C 0.5330(3) 0.0348(2) 0.2961(2) 0.0430(7) Uani 1 1 d . . . . .
H3 H 0.4631 0.0294 0.2698 0.052 Uiso 1 1 calc R U . . .
C4 C 0.6512(3) -0.0120(2) 0.2710(2) 0.0445(7) Uani 1 1 d . . . . .
H4 H 0.6761 -0.0547 0.2249 0.053 Uiso 1 1 calc R U . . .
C5 C 0.7280(3) 0.01495(19) 0.32480(19) 0.0411(7) Uani 1 1 d . . . . .
H5 H 0.8140 -0.0063 0.3210 0.049 Uiso 1 1 calc R U . . .
C6 C 0.6564(2) 0.07953(19) 0.38548(19) 0.0353(6) Uani 1 1 d . . . . .
C7 C 0.5855(2) 0.32479(19) 0.14132(19) 0.0362(6) Uani 1 1 d . . . . .
C8 C 0.5824(2) 0.2591(2) 0.07690(19) 0.0353(6) Uani 1 1 d . . . . .
C9 C 0.7141(2) 0.23331(19) 0.06616(19) 0.0353(6) Uani 1 1 d . . . . .
C10 C 0.7165(2) 0.2980(2) 0.1319(2) 0.0375(6) Uani 1 1 d . . . . .
C11 C 0.4975(2) 0.39953(19) 0.1845(2) 0.0391(7) Uani 1 1 d . . . . .
C12 C 0.3932(3) 0.4527(2) 0.1375(2) 0.0538(8) Uani 1 1 d . . . . .
H12 H 0.3787 0.4414 0.0785 0.065 Uiso 1 1 calc R U . . .
C13 C 0.3105(3) 0.5231(2) 0.1793(3) 0.0723(11) Uani 1 1 d . . . . .
H13 H 0.2410 0.5569 0.1484 0.087 Uiso 1 1 calc R U . . .
C14 C 0.3307(4) 0.5430(3) 0.2660(3) 0.0790(12) Uani 1 1 d . . . . .
H14 H 0.2754 0.5897 0.2929 0.095 Uiso 1 1 calc R U . . .
C15 C 0.4343(3) 0.4926(2) 0.3117(3) 0.0705(10) Uani 1 1 d . . . . .
H15 H 0.4491 0.5060 0.3693 0.085 Uiso 1 1 calc R U . . .
C16 C 0.5165(3) 0.4217(2) 0.2719(2) 0.0515(8) Uani 1 1 d . . . . .
H16 H 0.5855 0.3883 0.3038 0.062 Uiso 1 1 calc R U . . .
C17 C 0.4869(2) 0.2392(2) 0.0301(2) 0.0388(6) Uani 1 1 d . . . . .
C18 C 0.3716(3) 0.2273(2) 0.0864(2) 0.0475(7) Uani 1 1 d . . . . .
H18 H 0.3538 0.2322 0.1538 0.057 Uiso 1 1 calc R U . . .
C19 C 0.2846(3) 0.2082(2) 0.0420(2) 0.0560(8) Uani 1 1 d . . . . .
H19 H 0.2089 0.2012 0.0797 0.067 Uiso 1 1 calc R U . . .
C20 C 0.3099(3) 0.1996(3) -0.0575(3) 0.0643(9) Uani 1 1 d . . . . .
H20 H 0.2518 0.1859 -0.0865 0.077 Uiso 1 1 calc R U . . .
C21 C 0.4231(3) 0.2115(3) -0.1144(3) 0.0674(10) Uani 1 1 d . . . . .
H21 H 0.4402 0.2059 -0.1815 0.081 Uiso 1 1 calc R U . . .
C22 C 0.5108(3) 0.2317(2) -0.0713(2) 0.0512(8) Uani 1 1 d . . . . .
H22 H 0.5857 0.2403 -0.1103 0.061 Uiso 1 1 calc R U . . .
C23 C 0.8068(2) 0.1852(2) -0.0015(2) 0.0402(7) Uani 1 1 d . . . . .
C24 C 0.9090(2) 0.2355(2) -0.0534(2) 0.0508(8) Uani 1 1 d . . . . .
H24 H 0.9217 0.2954 -0.0407 0.061 Uiso 1 1 calc R U . . .
C28 C 0.7935(3) 0.0925(2) -0.0203(2) 0.0497(8) Uani 1 1 d . . . . .
H28 H 0.7272 0.0573 0.0135 0.060 Uiso 1 1 calc R U . . .
C29 C 0.8132(2) 0.3414(2) 0.1541(2) 0.0399(7) Uani 1 1 d . . . . .
C30 C 0.8034(3) 0.4549(2) 0.1314(2) 0.0616(9) Uani 1 1 d . . . . .
H30 H 0.7357 0.5019 0.1055 0.074 Uiso 1 1 calc R U . . .
C31 C 0.8942(3) 0.4980(3) 0.1475(3) 0.0784(11) Uani 1 1 d . . . . .
H31 H 0.8871 0.5735 0.1315 0.094 Uiso 1 1 calc R U . . .
C32 C 0.9959(3) 0.4278(3) 0.1875(3) 0.0781(11) Uani 1 1 d . . . . .
H32 H 1.0564 0.4565 0.1981 0.094 Uiso 1 1 calc R U . . .
C33 C 1.0062(3) 0.3153(3) 0.2113(2) 0.0630(9) Uani 1 1 d . . . . .
H33 H 1.0734 0.2684 0.2384 0.076 Uiso 1 1 calc R U . . .
C34 C 0.9154(3) 0.2724(2) 0.1945(2) 0.0503(8) Uani 1 1 d . . . . .
H34 H 0.9231 0.1969 0.2105 0.060 Uiso 1 1 calc R U . . .
C35 C 0.3287(3) 0.2684(2) 0.5125(2) 0.0446(7) Uani 1 1 d . . . . .
C36 C 0.2152(3) 0.3007(2) 0.4814(3) 0.0624(9) Uani 1 1 d . . . . .
H36 H 0.1942 0.2784 0.4321 0.075 Uiso 1 1 calc R U . . .
C37 C 0.1337(3) 0.3683(3) 0.5274(3) 0.0807(11) Uani 1 1 d . . . . .
H37 H 0.0574 0.3918 0.5083 0.097 Uiso 1 1 calc R U . . .
C38 C 0.1670(3) 0.3996(3) 0.6005(3) 0.0742(11) Uani 1 1 d . . . . .
H38 H 0.1138 0.4437 0.6320 0.089 Uiso 1 1 calc R U . . .
C39 C 0.2808(3) 0.3643(3) 0.6259(3) 0.0703(10) Uani 1 1 d . . . . .
H39 H 0.3028 0.3858 0.6753 0.084 Uiso 1 1 calc R U . . .
C40 C 0.7391(3) 0.2001(2) 0.5673(2) 0.0447(7) Uani 1 1 d . . . . .
C41 C 0.8547(2) 0.1181(2) 0.5544(2) 0.0424(7) Uani 1 1 d . . . . .
C42 C 0.6906(3) 0.1881(3) 0.6838(2) 0.0608(9) Uani 1 1 d . . . . .
H42A H 0.6186 0.2383 0.6842 0.091 Uiso 1 1 calc R U . . .
H42B H 0.7479 0.2048 0.7146 0.091 Uiso 1 1 calc R U . . .
H42C H 0.6752 0.1135 0.7257 0.091 Uiso 1 1 calc R U . . .
C43 C 0.7479(3) 0.3213(2) 0.4951(3) 0.0695(10) Uani 1 1 d . . . . .
H43A H 0.7795 0.3272 0.4229 0.104 Uiso 1 1 calc R U . . .
H43B H 0.7990 0.3489 0.5223 0.104 Uiso 1 1 calc R U . . .
H43C H 0.6705 0.3640 0.4948 0.104 Uiso 1 1 calc R U . . .
C44 C 0.9694(3) 0.1658(3) 0.5284(2) 0.0638(9) Uani 1 1 d . . . . .
H44A H 1.0349 0.1108 0.5219 0.096 Uiso 1 1 calc R U . . .
H44B H 0.9773 0.1875 0.5852 0.096 Uiso 1 1 calc R U . . .
H44C H 0.9685 0.2291 0.4616 0.096 Uiso 1 1 calc R U . . .
C45 C 0.8631(3) 0.0066(2) 0.6489(2) 0.0575(8) Uani 1 1 d . . . . .
H45A H 0.7915 -0.0245 0.6625 0.086 Uiso 1 1 calc R U . . .
H45B H 0.8739 0.0165 0.7120 0.086 Uiso 1 1 calc R U . . .
H45C H 0.9292 -0.0425 0.6317 0.086 Uiso 1 1 calc R U . . .
B1 B 0.7159(3) 0.1154(2) 0.4564(2) 0.0371(7) Uani 1 1 d . . . . .
H1 H 0.486(2) 0.195(2) 0.4926(19) 0.039(8) Uiso 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
Co1 C8 2.002(7) . ?
Co1 C9 2.014(7) . ?
Co1 C10 2.018(7) . ?
Co1 C7 2.027(8) . ?
Co1 C3 2.094(7) . ?
Co1 C2 2.100(7) . ?
Co1 C5 2.104(6) . ?
Co1 C4 2.107(9) . ?
Co1 C6 2.115(9) . ?
O1 C1 1.243(5) . ?
O2 B1 1.394(5) . ?
O2 C40 1.485(5) . ?
O3 B1 1.374(7) . ?
O3 C41 1.501(6) . ?
N1 C1 1.377(5) . ?
N1 C35 1.424(5) . ?
N1 H1 0.84(2) . ?
N2 C35 1.356(5) . ?
N2 C39 1.356(5) . ?
C0AA C1AA 1.390(7) . ?
C0AA C24 1.412(5) . ?
C0AA H0AA 0.9300 . ?
C1 C2 1.516(6) . ?
C1AA C2AA 1.395(6) . ?
C1AA H1AA 0.9300 . ?
C2 C3 1.450(5) . ?
C2 C6 1.479(7) . ?
C2AA C28 1.378(5) . ?
C2AA H2AA 0.9300 . ?
C3 C4 1.425(6) . ?
C3 H3 0.9800 . ?
C4 C5 1.443(5) . ?
C4 H4 0.9800 . ?
C5 C6 1.462(5) . ?
C5 H5 0.9800 . ?
C6 B1 1.562(6) . ?
C7 C10 1.484(7) . ?
C7 C8 1.485(5) . ?
C7 C11 1.487(5) . ?
C8 C9 1.492(7) . ?
C8 C17 1.505(6) . ?
C9 C10 1.487(5) . ?
C9 C23 1.495(5) . ?
C10 C29 1.500(6) . ?
C11 C12 1.404(6) . ?
C11 C16 1.410(6) . ?
C12 C13 1.408(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.387(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.395(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.400(7) . ?
C17 C18 1.413(6) . ?
C18 C19 1.393(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.382(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.395(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.396(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C28 1.407(6) . ?
C23 C24 1.408(6) . ?
C24 H24 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.401(6) . ?
C29 C30 1.404(7) . ?
C30 C31 1.396(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.399(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.387(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.398(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.396(7) . ?
C36 C37 1.407(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.374(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.374(7) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C43 1.529(7) . ?
C40 C42 1.535(7) . ?
C40 C41 1.579(6) . ?
C41 C44 1.516(7) . ?
C41 C45 1.523(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 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
C8 Co1 C9 43.6(2) . . ?
C8 Co1 C10 62.9(2) . . ?
C9 Co1 C10 43.29(12) . . ?
C8 Co1 C7 43.25(12) . . ?
C9 Co1 C7 62.92(16) . . ?
C10 Co1 C7 43.1(2) . . ?
C8 Co1 C3 108.3(2) . . ?
C9 Co1 C3 133.82(13) . . ?
C10 Co1 C3 170.07(11) . . ?
C7 Co1 C3 127.6(3) . . ?
C8 Co1 C2 126.5(3) . . ?
C9 Co1 C2 169.75(11) . . ?
C10 Co1 C2 140.13(13) . . ?
C7 Co1 C2 112.50(19) . . ?
C3 Co1 C2 40.45(13) . . ?
C8 Co1 C5 153.56(11) . . ?
C9 Co1 C5 119.6(2) . . ?
C10 Co1 C5 122.7(3) . . ?
C7 Co1 C5 159.48(11) . . ?
C3 Co1 C5 67.2(3) . . ?
C2 Co1 C5 68.1(3) . . ?
C8 Co1 C4 119.61(16) . . ?
C9 Co1 C4 113.19(15) . . ?
C10 Co1 C4 147.52(18) . . ?
C7 Co1 C4 160.40(14) . . ?
C3 Co1 C4 39.65(19) . . ?
C2 Co1 C4 67.75(15) . . ?
C5 Co1 C4 40.07(17) . . ?
C8 Co1 C6 164.44(12) . . ?
C9 Co1 C6 149.2(2) . . ?
C10 Co1 C6 118.97(16) . . ?
C7 Co1 C6 126.02(13) . . ?
C3 Co1 C6 68.20(17) . . ?
C2 Co1 C6 41.1(2) . . ?
C5 Co1 C6 40.56(12) . . ?
C4 Co1 C6 68.05(15) . . ?
B1 O2 C40 106.9(3) . . ?
B1 O3 C41 106.8(2) . . ?
C1 N1 C35 128.8(3) . . ?
C1 N1 H1 117.5(17) . . ?
C35 N1 H1 113.7(17) . . ?
C35 N2 C39 116.9(4) . . ?
C1AA C0AA C24 120.1(4) . . ?
C1AA C0AA H0AA 120.0 . . ?
C24 C0AA H0AA 120.0 . . ?
O1 C1 N1 122.6(3) . . ?
O1 C1 C2 120.1(3) . . ?
N1 C1 C2 117.3(3) . . ?
C0AA C1AA C2AA 119.2(4) . . ?
C0AA C1AA H1AA 120.4 . . ?
C2AA C1AA H1AA 120.4 . . ?
C3 C2 C6 107.3(2) . . ?
C3 C2 C1 119.7(3) . . ?
C6 C2 C1 132.8(3) . . ?
C3 C2 Co1 69.6(3) . . ?
C6 C2 Co1 70.0(3) . . ?
C1 C2 Co1 122.9(2) . . ?
C28 C2AA C1AA 120.9(4) . . ?
C28 C2AA H2AA 119.6 . . ?
C1AA C2AA H2AA 119.6 . . ?
C4 C3 C2 109.3(3) . . ?
C4 C3 Co1 70.7(3) . . ?
C2 C3 Co1 70.0(3) . . ?
C4 C3 H3 125.4 . . ?
C2 C3 H3 125.4 . . ?
Co1 C3 H3 125.4 . . ?
C3 C4 C5 108.2(4) . . ?
C3 C4 Co1 69.7(2) . . ?
C5 C4 Co1 69.8(2) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Co1 C4 H4 125.9 . . ?
C4 C5 C6 108.8(4) . . ?
C4 C5 Co1 70.1(3) . . ?
C6 C5 Co1 70.1(3) . . ?
C4 C5 H5 125.6 . . ?
C6 C5 H5 125.6 . . ?
Co1 C5 H5 125.6 . . ?
C5 C6 C2 106.3(3) . . ?
C5 C6 B1 120.0(4) . . ?
C2 C6 B1 133.6(2) . . ?
C5 C6 Co1 69.3(3) . . ?
C2 C6 Co1 68.89(15) . . ?
B1 C6 Co1 128.5(3) . . ?
C10 C7 C8 89.9(2) . . ?
C10 C7 C11 134.1(2) . . ?
C8 C7 C11 135.6(3) . . ?
C10 C7 Co1 68.15(16) . . ?
C8 C7 Co1 67.5(3) . . ?
C11 C7 Co1 127.5(3) . . ?
C7 C8 C9 90.2(2) . . ?
C7 C8 C17 134.6(3) . . ?
C9 C8 C17 134.8(3) . . ?
C7 C8 Co1 69.3(3) . . ?
C9 C8 Co1 68.61(19) . . ?
C17 C8 Co1 125.4(3) . . ?
C10 C9 C8 89.5(2) . . ?
C10 C9 C23 134.0(3) . . ?
C8 C9 C23 135.3(3) . . ?
C10 C9 Co1 68.5(3) . . ?
C8 C9 Co1 67.77(19) . . ?
C23 C9 Co1 130.0(3) . . ?
C7 C10 C9 90.4(2) . . ?
C7 C10 C29 134.5(3) . . ?
C9 C10 C29 133.5(3) . . ?
C7 C10 Co1 68.8(2) . . ?
C9 C10 Co1 68.2(3) . . ?
C29 C10 Co1 131.1(3) . . ?
C12 C11 C16 117.6(3) . . ?
C12 C11 C7 120.7(3) . . ?
C16 C11 C7 121.6(3) . . ?
C11 C12 C13 120.1(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 121.2(4) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 119.1(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 120.4(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 121.5(4) . . ?
C15 C16 H16 119.2 . . ?
C11 C16 H16 119.2 . . ?
C22 C17 C18 118.3(3) . . ?
C22 C17 C8 120.2(3) . . ?
C18 C17 C8 121.5(4) . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 119.7(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C20 C21 C22 120.5(4) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C17 120.5(3) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
C28 C23 C24 117.6(3) . . ?
C28 C23 C9 122.1(3) . . ?
C24 C23 C9 120.2(3) . . ?
C23 C24 C0AA 120.7(4) . . ?
C23 C24 H24 119.6 . . ?
C0AA C24 H24 119.6 . . ?
C2AA C28 C23 121.5(3) . . ?
C2AA C28 H28 119.3 . . ?
C23 C28 H28 119.3 . . ?
C34 C29 C30 118.4(3) . . ?
C34 C29 C10 122.0(4) . . ?
C30 C29 C10 119.6(3) . . ?
C31 C30 C29 120.7(3) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 120.1(4) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 119.9(3) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 120.0(4) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C29 121.0(4) . . ?
C33 C34 H34 119.5 . . ?
C29 C34 H34 119.5 . . ?
N2 C35 C36 123.0(3) . . ?
N2 C35 N1 112.8(4) . . ?
C36 C35 N1 124.2(3) . . ?
C35 C36 C37 117.7(4) . . ?
C35 C36 H36 121.2 . . ?
C37 C36 H36 121.2 . . ?
C38 C37 C36 119.9(4) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C39 C38 C37 118.4(3) . . ?
C39 C38 H38 120.8 . . ?
C37 C38 H38 120.8 . . ?
N2 C39 C38 124.1(4) . . ?
N2 C39 H39 118.0 . . ?
C38 C39 H39 118.0 . . ?
O2 C40 C43 106.4(3) . . ?
O2 C40 C42 107.7(3) . . ?
C43 C40 C42 110.6(3) . . ?
O2 C40 C41 102.1(3) . . ?
C43 C40 C41 113.8(3) . . ?
C42 C40 C41 115.3(2) . . ?
O3 C41 C44 109.3(3) . . ?
O3 C41 C45 106.3(4) . . ?
C44 C41 C45 110.1(3) . . ?
O3 C41 C40 101.8(3) . . ?
C44 C41 C40 114.9(4) . . ?
C45 C41 C40 113.7(3) . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C45 H45A 109.5 . . ?
C41 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C41 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O3 B1 O2 113.6(3) . . ?
O3 B1 C6 123.3(3) . . ?
O2 B1 C6 123.0(4) . . ?

_refine_diff_density_max         0.384
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1523207'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H40 Co N O S Si'
_chemical_formula_sum            'C44 H40 Co N O S Si'
_chemical_formula_weight         717.85

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.00(3)
_cell_length_b                   13.25(3)
_cell_length_c                   23.77(5)
_cell_angle_alpha                84.63(2)
_cell_angle_beta                 86.64(2)
_cell_angle_gamma                72.88(3)
_cell_volume                     3895(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4705
_cell_measurement_theta_min      2.298
_cell_measurement_theta_max      24.317

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.152
_exptl_absorpt_coefficient_mu    0.558
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20295
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.767
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             13544
_reflns_number_gt                7900
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0638P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13544
_refine_ls_number_parameters     899
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1339
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.29314(3) 0.34594(3) 0.42101(2) 0.04041(14) Uani 1 1 d . . . . .
S1 S -0.07927(10) 0.70510(8) 0.36869(5) 0.0832(4) Uani 1 1 d . . . . .
Si1 Si 0.19179(9) 0.11243(8) 0.47103(5) 0.0605(3) Uani 1 1 d . . . . .
O1 O 0.00602(19) 0.28856(19) 0.41273(12) 0.0730(8) Uani 1 1 d . . . . .
N1 N -0.0125(2) 0.4677(2) 0.39726(12) 0.0550(8) Uani 1 1 d . . . . .
H1 H 0.016(2) 0.525(2) 0.4051(13) 0.055(10) Uiso 1 1 d . . . . .
C1 C 0.0377(3) 0.3654(3) 0.41929(14) 0.0514(9) Uani 1 1 d . . . . .
C2 C 0.1355(3) 0.3544(3) 0.45340(13) 0.0470(8) Uani 1 1 d . . . . .
C3 C 0.1723(3) 0.4373(3) 0.47354(14) 0.0539(9) Uani 1 1 d . . . . .
H3 H 0.1374 0.5137 0.4677 0.065 Uiso 1 1 calc R U . . .
C4 C 0.2665(3) 0.3873(3) 0.50527(13) 0.0580(10) Uani 1 1 d . . . . .
H4 H 0.3080 0.4235 0.5249 0.070 Uiso 1 1 calc R U . . .
C5 C 0.2884(3) 0.2751(3) 0.50425(13) 0.0558(10) Uani 1 1 d . . . . .
H5 H 0.3489 0.2219 0.5225 0.067 Uiso 1 1 calc R U . . .
C6 C 0.2074(3) 0.2517(3) 0.47249(13) 0.0490(9) Uani 1 1 d . . . . .
C7 C 0.3884(2) 0.2767(2) 0.35573(12) 0.0418(8) Uani 1 1 d . . . . .
C8 C 0.4415(2) 0.3383(2) 0.38683(12) 0.0394(8) Uani 1 1 d . . . . .
C9 C 0.3600(2) 0.4382(2) 0.36689(12) 0.0387(7) Uani 1 1 d . . . . .
C10 C 0.3066(2) 0.3754(2) 0.33591(12) 0.0400(8) Uani 1 1 d . . . . .
C11 C 0.4212(2) 0.1647(2) 0.33974(13) 0.0402(8) Uani 1 1 d . . . . .
C12 C 0.4016(3) 0.1411(3) 0.28555(14) 0.0508(9) Uani 1 1 d . . . . .
H12 H 0.3660 0.1956 0.2598 0.061 Uiso 1 1 calc R U . . .
C13 C 0.4350(3) 0.0367(3) 0.26978(16) 0.0609(10) Uani 1 1 d . . . . .
H13 H 0.4211 0.0223 0.2339 0.073 Uiso 1 1 calc R U . . .
C14 C 0.4886(3) -0.0448(3) 0.30747(19) 0.0694(11) Uani 1 1 d . . . . .
H14 H 0.5101 -0.1141 0.2972 0.083 Uiso 1 1 calc R U . . .
C15 C 0.5103(3) -0.0230(3) 0.36083(18) 0.0675(11) Uani 1 1 d . . . . .
H15 H 0.5470 -0.0781 0.3860 0.081 Uiso 1 1 calc R U . . .
C16 C 0.4779(3) 0.0806(3) 0.37730(15) 0.0555(9) Uani 1 1 d . . . . .
H16 H 0.4937 0.0940 0.4130 0.067 Uiso 1 1 calc R U . . .
C17 C 0.5467(2) 0.3144(2) 0.41504(13) 0.0403(8) Uani 1 1 d . . . . .
C18 C 0.5580(3) 0.3650(3) 0.46271(14) 0.0534(9) Uani 1 1 d . . . . .
H18 H 0.4974 0.4113 0.4787 0.064 Uiso 1 1 calc R U . . .
C19 C 0.6578(3) 0.3474(3) 0.48669(14) 0.0589(10) Uani 1 1 d . . . . .
H19 H 0.6631 0.3820 0.5182 0.071 Uiso 1 1 calc R U . . .
C20 C 0.7490(3) 0.2783(3) 0.46367(15) 0.0613(10) Uani 1 1 d . . . . .
H20 H 0.8155 0.2662 0.4797 0.074 Uiso 1 1 calc R U . . .
C21 C 0.7400(3) 0.2273(3) 0.41650(16) 0.0607(10) Uani 1 1 d . . . . .
H21 H 0.8010 0.1811 0.4009 0.073 Uiso 1 1 calc R U . . .
C22 C 0.6396(3) 0.2449(3) 0.39205(14) 0.0487(9) Uani 1 1 d . . . . .
H22 H 0.6348 0.2102 0.3605 0.058 Uiso 1 1 calc R U . . .
C23 C 0.3517(3) 0.5522(2) 0.36894(12) 0.0418(8) Uani 1 1 d . . . . .
C24 C 0.4444(3) 0.5840(3) 0.37290(13) 0.0516(9) Uani 1 1 d . . . . .
H24 H 0.5110 0.5329 0.3754 0.062 Uiso 1 1 calc R U . . .
C25 C 0.4393(3) 0.6921(3) 0.37312(16) 0.0666(11) Uani 1 1 d . . . . .
H25 H 0.5019 0.7117 0.3754 0.080 Uiso 1 1 calc R U . . .
C26 C 0.3402(4) 0.7686(3) 0.36994(17) 0.0757(12) Uani 1 1 d . . . . .
H26 H 0.3361 0.8398 0.3702 0.091 Uiso 1 1 calc R U . . .
C27 C 0.2464(3) 0.7387(3) 0.36635(17) 0.0696(11) Uani 1 1 d . . . . .
H27 H 0.1799 0.7901 0.3644 0.084 Uiso 1 1 calc R U . . .
C28 C 0.2523(3) 0.6309(3) 0.36573(14) 0.0562(9) Uani 1 1 d . . . . .
H28 H 0.1896 0.6118 0.3632 0.067 Uiso 1 1 calc R U . . .
C29 C 0.2203(2) 0.4009(2) 0.29303(12) 0.0403(8) Uani 1 1 d . . . . .
C30 C 0.1559(3) 0.3330(3) 0.28840(14) 0.0575(10) Uani 1 1 d . . . . .
H30 H 0.1648 0.2728 0.3133 0.069 Uiso 1 1 calc R U . . .
C31 C 0.0787(3) 0.3555(4) 0.24666(17) 0.0743(12) Uani 1 1 d . . . . .
H31 H 0.0368 0.3102 0.2441 0.089 Uiso 1 1 calc R U . . .
C32 C 0.0643(3) 0.4451(4) 0.20913(18) 0.0789(13) Uani 1 1 d . . . . .
H32 H 0.0127 0.4601 0.1817 0.095 Uiso 1 1 calc R U . . .
C33 C 0.1271(3) 0.5114(3) 0.21299(17) 0.0790(13) Uani 1 1 d . . . . .
H33 H 0.1177 0.5711 0.1877 0.095 Uiso 1 1 calc R U . . .
C34 C 0.2053(3) 0.4904(3) 0.25445(14) 0.0589(10) Uani 1 1 d . . . . .
H34 H 0.2471 0.5361 0.2563 0.071 Uiso 1 1 calc R U . . .
C35 C -0.1059(3) 0.5038(3) 0.36231(14) 0.0528(9) Uani 1 1 d . . . . .
C36 C -0.1584(3) 0.4357(3) 0.34346(17) 0.0710(11) Uani 1 1 d . . . . .
H36 H -0.1348 0.3637 0.3546 0.085 Uiso 1 1 calc R U . . .
C37 C -0.2456(3) 0.4745(4) 0.30828(19) 0.0876(14) Uani 1 1 d . . . . .
H37 H -0.2793 0.4282 0.2957 0.105 Uiso 1 1 calc R U . . .
C38 C -0.2828(4) 0.5827(4) 0.2919(2) 0.0939(15) Uani 1 1 d . . . . .
H38 H -0.3412 0.6087 0.2684 0.113 Uiso 1 1 calc R U . . .
C39 C -0.2326(4) 0.6504(3) 0.31050(19) 0.0862(14) Uani 1 1 d . . . . .
H39 H -0.2576 0.7225 0.2995 0.103 Uiso 1 1 calc R U . . .
C40 C -0.1435(3) 0.6131(3) 0.34605(16) 0.0646(11) Uani 1 1 d . . . . .
C41 C -0.0208(3) 0.7407(4) 0.3018(2) 0.1093(17) Uani 1 1 d . . . . .
H41A H 0.0326 0.6796 0.2889 0.164 Uiso 1 1 calc R U . . .
H41B H 0.0121 0.7953 0.3064 0.164 Uiso 1 1 calc R U . . .
H41C H -0.0761 0.7661 0.2745 0.164 Uiso 1 1 calc R U . . .
C42 C 0.3162(3) 0.0178(3) 0.50469(19) 0.0926(15) Uani 1 1 d . . . . .
H42A H 0.3170 -0.0539 0.5006 0.139 Uiso 1 1 calc R U . . .
H42B H 0.3150 0.0287 0.5441 0.139 Uiso 1 1 calc R U . . .
H42C H 0.3794 0.0306 0.4864 0.139 Uiso 1 1 calc R U . . .
C43 C 0.1794(3) 0.0699(3) 0.39927(17) 0.0782(12) Uani 1 1 d . . . . .
H43A H 0.1742 -0.0012 0.4030 0.117 Uiso 1 1 calc R U . . .
H43B H 0.2417 0.0725 0.3761 0.117 Uiso 1 1 calc R U . . .
H43C H 0.1161 0.1166 0.3820 0.117 Uiso 1 1 calc R U . . .
C44 C 0.0730(3) 0.1032(3) 0.51857(18) 0.0884(14) Uani 1 1 d . . . . .
H44A H 0.0078 0.1483 0.5023 0.133 Uiso 1 1 calc R U . . .
H44B H 0.0805 0.1254 0.5550 0.133 Uiso 1 1 calc R U . . .
H44C H 0.0701 0.0313 0.5226 0.133 Uiso 1 1 calc R U . . .
Co2 Co 0.65194(3) 0.17850(3) 0.09157(2) 0.04614(15) Uani 1 1 d . . . . .
S2 S 1.00729(9) -0.18458(9) 0.14219(6) 0.0877(4) Uani 1 1 d . . . . .
Si2 Si 0.76058(8) 0.41548(8) 0.05750(5) 0.0629(3) Uani 1 1 d . . . . .
O2 O 0.9456(2) 0.2277(2) 0.10687(14) 0.0920(10) Uani 1 1 d . . . . .
N2 N 0.9535(3) 0.0513(3) 0.11973(15) 0.0683(10) Uani 1 1 d . . . . .
H2 H 0.925(3) -0.003(3) 0.1110(19) 0.119(18) Uiso 1 1 d . . . . .
C45 C 0.9087(3) 0.1544(3) 0.09837(17) 0.0608(10) Uani 1 1 d . . . . .
C46 C 0.8115(3) 0.1725(3) 0.06338(14) 0.0505(9) Uani 1 1 d . . . . .
C47 C 0.7753(3) 0.0949(3) 0.03839(14) 0.0564(10) Uani 1 1 d . . . . .
H47 H 0.8095 0.0182 0.0416 0.068 Uiso 1 1 calc R U . . .
C48 C 0.6821(3) 0.1503(3) 0.00580(14) 0.0622(10) Uani 1 1 d . . . . .
H48 H 0.6418 0.1184 -0.0172 0.075 Uiso 1 1 calc R U . . .
C49 C 0.6618(3) 0.2604(3) 0.01222(14) 0.0597(10) Uani 1 1 d . . . . .
H49 H 0.6022 0.3166 -0.0049 0.072 Uiso 1 1 calc R U . . .
C50 C 0.7415(3) 0.2783(3) 0.04727(14) 0.0519(9) Uani 1 1 d . . . . .
C51 C 0.6319(3) 0.1447(2) 0.17605(13) 0.0454(8) Uani 1 1 d . . . . .
C52 C 0.5844(2) 0.0813(3) 0.14205(13) 0.0446(8) Uani 1 1 d . . . . .
C53 C 0.5028(3) 0.1790(2) 0.12101(13) 0.0446(8) Uani 1 1 d . . . . .
C54 C 0.5486(3) 0.2420(3) 0.15545(13) 0.0452(8) Uani 1 1 d . . . . .
C55 C 0.7153(3) 0.1184(3) 0.22022(13) 0.0470(8) Uani 1 1 d . . . . .
C56 C 0.7818(3) 0.1827(3) 0.22518(16) 0.0640(10) Uani 1 1 d . . . . .
H56 H 0.7746 0.2432 0.2007 0.077 Uiso 1 1 calc R U . . .
C57 C 0.8597(3) 0.1564(4) 0.26697(18) 0.0813(13) Uani 1 1 d . . . . .
H57 H 0.9038 0.1996 0.2699 0.098 Uiso 1 1 calc R U . . .
C58 C 0.8711(3) 0.0669(4) 0.30378(18) 0.0809(13) Uani 1 1 d . . . . .
H58 H 0.9244 0.0484 0.3305 0.097 Uiso 1 1 calc R U . . .
C59 C 0.8033(3) 0.0052(3) 0.30076(16) 0.0749(12) Uani 1 1 d . . . . .
H59 H 0.8088 -0.0531 0.3266 0.090 Uiso 1 1 calc R U . . .
C60 C 0.7263(3) 0.0297(3) 0.25916(14) 0.0596(10) Uani 1 1 d . . . . .
H60 H 0.6818 -0.0133 0.2572 0.072 Uiso 1 1 calc R U . . .
C61 C 0.5977(3) -0.0340(3) 0.13953(13) 0.0477(8) Uani 1 1 d . . . . .
C62 C 0.6971(3) -0.1109(3) 0.15125(14) 0.0585(10) Uani 1 1 d . . . . .
H62 H 0.7571 -0.0896 0.1580 0.070 Uiso 1 1 calc R U . . .
C63 C 0.7057(4) -0.2189(3) 0.15277(17) 0.0764(12) Uani 1 1 d . . . . .
H63 H 0.7714 -0.2688 0.1604 0.092 Uiso 1 1 calc R U . . .
C64 C 0.6154(4) -0.2528(3) 0.14276(18) 0.0841(13) Uani 1 1 d . . . . .
H64 H 0.6215 -0.3247 0.1442 0.101 Uiso 1 1 calc R U . . .
C65 C 0.5182(4) -0.1782(3) 0.13080(16) 0.0714(11) Uani 1 1 d . . . . .
H65 H 0.4588 -0.2001 0.1237 0.086 Uiso 1 1 calc R U . . .
C66 C 0.5084(3) -0.0695(3) 0.12923(14) 0.0574(10) Uani 1 1 d . . . . .
H66 H 0.4424 -0.0202 0.1213 0.069 Uiso 1 1 calc R U . . .
C67 C 0.4012(3) 0.2002(3) 0.08922(14) 0.0461(8) Uani 1 1 d . . . . .
C68 C 0.3987(3) 0.1548(3) 0.03836(15) 0.0610(10) Uani 1 1 d . . . . .
H68 H 0.4628 0.1140 0.0225 0.073 Uiso 1 1 calc R U . . .
C69 C 0.3018(3) 0.1696(3) 0.01086(16) 0.0753(12) Uani 1 1 d . . . . .
H69 H 0.3017 0.1390 -0.0228 0.090 Uiso 1 1 calc R U . . .
C70 C 0.2063(4) 0.2307(4) 0.03476(19) 0.0865(14) Uani 1 1 d . . . . .
H70 H 0.1416 0.2409 0.0172 0.104 Uiso 1 1 calc R U . . .
C71 C 0.2073(3) 0.2765(3) 0.08478(18) 0.0798(13) Uani 1 1 d . . . . .
H71 H 0.1430 0.3176 0.1003 0.096 Uiso 1 1 calc R U . . .
C72 C 0.3030(3) 0.2619(3) 0.11222(15) 0.0634(10) Uani 1 1 d . . . . .
H72 H 0.3020 0.2929 0.1458 0.076 Uiso 1 1 calc R U . . .
C73 C 0.5125(3) 0.3541(3) 0.17023(14) 0.0478(8) Uani 1 1 d . . . . .
C74 C 0.4531(3) 0.4353(3) 0.13204(16) 0.0667(11) Uani 1 1 d . . . . .
H74 H 0.4370 0.4188 0.0971 0.080 Uiso 1 1 calc R U . . .
C75 C 0.4184(3) 0.5401(3) 0.1461(2) 0.0797(13) Uani 1 1 d . . . . .
H75 H 0.3792 0.5928 0.1204 0.096 Uiso 1 1 calc R U . . .
C76 C 0.4418(4) 0.5665(3) 0.1981(2) 0.0808(13) Uani 1 1 d . . . . .
H76 H 0.4198 0.6367 0.2070 0.097 Uiso 1 1 calc R U . . .
C77 C 0.4981(3) 0.4875(4) 0.23657(19) 0.0766(12) Uani 1 1 d . . . . .
H77 H 0.5126 0.5047 0.2717 0.092 Uiso 1 1 calc R U . . .
C78 C 0.5332(3) 0.3821(3) 0.22310(15) 0.0593(10) Uani 1 1 d . . . . .
H78 H 0.5707 0.3299 0.2494 0.071 Uiso 1 1 calc R U . . .
C79 C 1.0450(3) 0.0090(3) 0.15453(17) 0.0686(11) Uani 1 1 d . . . . .
C80 C 1.1008(4) 0.0722(4) 0.1765(2) 0.1090(18) Uani 1 1 d . . . . .
H80 H 1.0802 0.1450 0.1675 0.131 Uiso 1 1 calc R U . . .
C81 C 1.1869(4) 0.0250(5) 0.2115(3) 0.133(2) Uani 1 1 d . . . . .
H81 H 1.2220 0.0675 0.2268 0.160 Uiso 1 1 calc R U . . .
C82 C 1.2214(5) -0.0831(6) 0.2242(3) 0.138(2) Uani 1 1 d . . . . .
H82 H 1.2808 -0.1135 0.2465 0.166 Uiso 1 1 calc R U . . .
C83 C 1.1664(4) -0.1459(4) 0.2034(2) 0.1103(18) Uani 1 1 d . . . . .
H83 H 1.1879 -0.2186 0.2128 0.132 Uiso 1 1 calc R U . . .
C84 C 1.0780(3) -0.1012(3) 0.16780(17) 0.0728(12) Uani 1 1 d . . . . .
C85 C 1.0652(5) -0.1950(5) 0.0730(2) 0.163(3) Uani 1 1 d . . . . .
H85A H 1.0440 -0.1269 0.0522 0.245 Uiso 1 1 calc R U . . .
H85B H 1.0408 -0.2445 0.0543 0.245 Uiso 1 1 calc R U . . .
H85C H 1.1422 -0.2192 0.0749 0.245 Uiso 1 1 calc R U . . .
C86 C 0.7701(3) 0.4461(3) 0.13331(16) 0.0732(12) Uani 1 1 d . . . . .
H86A H 0.7843 0.5132 0.1333 0.110 Uiso 1 1 calc R U . . .
H86B H 0.8274 0.3917 0.1513 0.110 Uiso 1 1 calc R U . . .
H86C H 0.7034 0.4489 0.1536 0.110 Uiso 1 1 calc R U . . .
C87 C 0.6414(3) 0.5198(3) 0.02698(18) 0.0891(14) Uani 1 1 d . . . . .
H87A H 0.6574 0.5863 0.0214 0.134 Uiso 1 1 calc R U . . .
H87B H 0.5802 0.5265 0.0526 0.134 Uiso 1 1 calc R U . . .
H87C H 0.6254 0.4999 -0.0086 0.134 Uiso 1 1 calc R U . . .
C88 C 0.8818(3) 0.4331(4) 0.0140(2) 0.1124(18) Uani 1 1 d . . . . .
H88A H 0.8664 0.4409 -0.0255 0.169 Uiso 1 1 calc R U . . .
H88B H 0.9426 0.3722 0.0213 0.169 Uiso 1 1 calc R U . . .
H88C H 0.8979 0.4952 0.0240 0.169 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 C9 2.026(4) . ?
Co1 C8 2.027(5) . ?
Co1 C10 2.031(5) . ?
Co1 C7 2.039(4) . ?
Co1 C3 2.104(4) . ?
Co1 C4 2.108(5) . ?
Co1 C5 2.115(5) . ?
Co1 C2 2.122(5) . ?
Co1 C6 2.162(4) . ?
S1 C40 1.803(5) . ?
S1 C41 1.805(6) . ?
Si1 C43 1.876(5) . ?
Si1 C44 1.887(5) . ?
Si1 C42 1.897(5) . ?
Si1 C6 1.919(5) . ?
O1 C1 1.231(4) . ?
N1 C1 1.387(5) . ?
N1 C35 1.448(5) . ?
N1 H1 0.97(3) . ?
C1 C2 1.512(5) . ?
C2 C3 1.450(5) . ?
C2 C6 1.454(5) . ?
C3 C4 1.430(5) . ?
C3 H3 0.9800 . ?
C4 C5 1.432(5) . ?
C4 H4 0.9800 . ?
C5 C6 1.451(5) . ?
C5 H5 0.9800 . ?
C7 C10 1.479(4) . ?
C7 C8 1.480(4) . ?
C7 C11 1.498(5) . ?
C8 C9 1.488(4) . ?
C8 C17 1.496(5) . ?
C9 C23 1.488(5) . ?
C9 C10 1.494(4) . ?
C10 C29 1.503(5) . ?
C11 C12 1.408(5) . ?
C11 C16 1.411(4) . ?
C12 C13 1.403(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.379(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.398(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.403(4) . ?
C17 C18 1.405(5) . ?
C18 C19 1.395(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.390(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.407(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.401(5) . ?
C23 C28 1.402(5) . ?
C24 C25 1.415(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.387(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.398(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.409(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.402(5) . ?
C29 C30 1.412(5) . ?
C30 C31 1.403(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.389(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.375(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.408(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.398(5) . ?
C35 C40 1.409(5) . ?
C36 C37 1.392(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.398(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.371(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.414(5) . ?
C39 H39 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Co2 C53 2.021(5) . ?
Co2 C52 2.031(4) . ?
Co2 C51 2.035(5) . ?
Co2 C54 2.038(4) . ?
Co2 C47 2.092(4) . ?
Co2 C48 2.101(5) . ?
Co2 C49 2.103(5) . ?
Co2 C46 2.124(5) . ?
Co2 C50 2.172(4) . ?
S2 C85 1.769(6) . ?
S2 C84 1.796(5) . ?
Si2 C87 1.877(4) . ?
Si2 C88 1.895(5) . ?
Si2 C86 1.903(5) . ?
Si2 C50 1.944(5) . ?
O2 C45 1.240(4) . ?
N2 C45 1.379(5) . ?
N2 C79 1.432(5) . ?
N2 H2 0.94(4) . ?
C45 C46 1.501(5) . ?
C46 C47 1.437(5) . ?
C46 C50 1.460(5) . ?
C47 C48 1.445(5) . ?
C47 H47 0.9800 . ?
C48 C49 1.426(6) . ?
C48 H48 0.9800 . ?
C49 C50 1.452(5) . ?
C49 H49 0.9800 . ?
C51 C54 1.482(5) . ?
C51 C52 1.494(5) . ?
C51 C55 1.498(5) . ?
C52 C53 1.478(5) . ?
C52 C61 1.492(5) . ?
C53 C54 1.484(5) . ?
C53 C67 1.502(5) . ?
C54 C73 1.489(5) . ?
C55 C56 1.397(5) . ?
C55 C60 1.404(5) . ?
C56 C57 1.407(5) . ?
C56 H56 0.9300 . ?
C57 C58 1.383(6) . ?
C57 H57 0.9300 . ?
C58 C59 1.375(6) . ?
C58 H58 0.9300 . ?
C59 C60 1.397(5) . ?
C59 H59 0.9300 . ?
C60 H60 0.9300 . ?
C61 C62 1.415(5) . ?
C61 C66 1.416(5) . ?
C62 C63 1.399(6) . ?
C62 H62 0.9300 . ?
C63 C64 1.414(6) . ?
C63 H63 0.9300 . ?
C64 C65 1.382(6) . ?
C64 H64 0.9300 . ?
C65 C66 1.405(5) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C67 C68 1.406(5) . ?
C67 C72 1.409(5) . ?
C68 C69 1.407(5) . ?
C68 H68 0.9300 . ?
C69 C70 1.390(6) . ?
C69 H69 0.9300 . ?
C70 C71 1.387(6) . ?
C70 H70 0.9300 . ?
C71 C72 1.393(5) . ?
C71 H71 0.9300 . ?
C72 H72 0.9300 . ?
C73 C78 1.406(5) . ?
C73 C74 1.410(5) . ?
C74 C75 1.394(6) . ?
C74 H74 0.9300 . ?
C75 C76 1.389(6) . ?
C75 H75 0.9300 . ?
C76 C77 1.385(6) . ?
C76 H76 0.9300 . ?
C77 C78 1.397(6) . ?
C77 H77 0.9300 . ?
C78 H78 0.9300 . ?
C79 C84 1.406(6) . ?
C79 C80 1.409(6) . ?
C80 C81 1.393(6) . ?
C80 H80 0.9300 . ?
C81 C82 1.379(8) . ?
C81 H81 0.9300 . ?
C82 C83 1.385(7) . ?
C82 H82 0.9300 . ?
C83 C84 1.416(6) . ?
C83 H83 0.9300 . ?
C85 H85A 0.9600 . ?
C85 H85B 0.9600 . ?
C85 H85C 0.9600 . ?
C86 H86A 0.9600 . ?
C86 H86B 0.9600 . ?
C86 H86C 0.9600 . ?
C87 H87A 0.9600 . ?
C87 H87B 0.9600 . ?
C87 H87C 0.9600 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 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
C9 Co1 C8 43.08(12) . . ?
C9 Co1 C10 43.19(12) . . ?
C8 Co1 C10 62.34(13) . . ?
C9 Co1 C7 62.23(17) . . ?
C8 Co1 C7 42.71(12) . . ?
C10 Co1 C7 42.61(14) . . ?
C9 Co1 C3 111.60(18) . . ?
C8 Co1 C3 141.17(14) . . ?
C10 Co1 C3 124.66(15) . . ?
C7 Co1 C3 166.93(13) . . ?
C9 Co1 C4 116.42(17) . . ?
C8 Co1 C4 115.62(14) . . ?
C10 Co1 C4 154.92(15) . . ?
C7 Co1 C4 152.76(14) . . ?
C3 Co1 C4 39.70(13) . . ?
C9 Co1 C5 146.28(13) . . ?
C8 Co1 C5 116.06(14) . . ?
C10 Co1 C5 165.45(14) . . ?
C7 Co1 C5 125.38(17) . . ?
C3 Co1 C5 66.55(17) . . ?
C4 Co1 C5 39.64(16) . . ?
C9 Co1 C2 135.70(13) . . ?
C8 Co1 C2 177.64(12) . . ?
C10 Co1 C2 115.34(13) . . ?
C7 Co1 C2 135.44(13) . . ?
C3 Co1 C2 40.12(13) . . ?
C4 Co1 C2 66.63(14) . . ?
C5 Co1 C2 66.06(14) . . ?
C9 Co1 C6 173.72(12) . . ?
C8 Co1 C6 141.30(13) . . ?
C10 Co1 C6 131.76(13) . . ?
C7 Co1 C6 117.33(17) . . ?
C3 Co1 C6 67.41(18) . . ?
C4 Co1 C6 67.11(16) . . ?
C5 Co1 C6 39.66(12) . . ?
C2 Co1 C6 39.68(13) . . ?
C40 S1 C41 99.4(2) . . ?
C43 Si1 C44 110.6(2) . . ?
C43 Si1 C42 108.7(2) . . ?
C44 Si1 C42 106.8(2) . . ?
C43 Si1 C6 115.86(16) . . ?
C44 Si1 C6 108.37(18) . . ?
C42 Si1 C6 106.1(2) . . ?
C1 N1 C35 128.1(3) . . ?
C1 N1 H1 119.3(18) . . ?
C35 N1 H1 112.6(18) . . ?
O1 C1 N1 123.8(4) . . ?
O1 C1 C2 121.4(3) . . ?
N1 C1 C2 114.7(3) . . ?
C3 C2 C6 109.2(3) . . ?
C3 C2 C1 128.4(3) . . ?
C6 C2 C1 122.3(3) . . ?
C3 C2 Co1 69.3(2) . . ?
C6 C2 Co1 71.6(2) . . ?
C1 C2 Co1 126.6(3) . . ?
C4 C3 C2 107.6(3) . . ?
C4 C3 Co1 70.3(2) . . ?
C2 C3 Co1 70.6(2) . . ?
C4 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
Co1 C3 H3 126.2 . . ?
C3 C4 C5 108.0(3) . . ?
C3 C4 Co1 70.0(2) . . ?
C5 C4 Co1 70.4(2) . . ?
C3 C4 H4 126.0 . . ?
C5 C4 H4 126.0 . . ?
Co1 C4 H4 126.0 . . ?
C4 C5 C6 109.9(3) . . ?
C4 C5 Co1 69.95(19) . . ?
C6 C5 Co1 71.9(2) . . ?
C4 C5 H5 125.0 . . ?
C6 C5 H5 125.0 . . ?
Co1 C5 H5 125.0 . . ?
C5 C6 C2 105.3(3) . . ?
C5 C6 Si1 123.7(2) . . ?
C2 C6 Si1 130.1(3) . . ?
C5 C6 Co1 68.4(2) . . ?
C2 C6 Co1 68.7(2) . . ?
Si1 C6 Co1 135.30(19) . . ?
C10 C7 C8 90.4(3) . . ?
C10 C7 C11 134.6(3) . . ?
C8 C7 C11 133.4(3) . . ?
C10 C7 Co1 68.43(19) . . ?
C8 C7 Co1 68.2(2) . . ?
C11 C7 Co1 131.0(2) . . ?
C7 C8 C9 90.1(3) . . ?
C7 C8 C17 134.9(3) . . ?
C9 C8 C17 133.7(3) . . ?
C7 C8 Co1 69.1(2) . . ?
C9 C8 Co1 68.44(19) . . ?
C17 C8 Co1 129.7(2) . . ?
C23 C9 C8 133.3(3) . . ?
C23 C9 C10 136.2(3) . . ?
C8 C9 C10 89.6(3) . . ?
C23 C9 Co1 128.4(2) . . ?
C8 C9 Co1 68.5(2) . . ?
C10 C9 Co1 68.6(2) . . ?
C7 C10 C9 89.9(3) . . ?
C7 C10 C29 133.6(3) . . ?
C9 C10 C29 135.5(3) . . ?
C7 C10 Co1 68.95(17) . . ?
C9 C10 Co1 68.21(18) . . ?
C29 C10 Co1 128.7(2) . . ?
C12 C11 C16 118.1(3) . . ?
C12 C11 C7 120.8(3) . . ?
C16 C11 C7 121.0(3) . . ?
C13 C12 C11 121.1(3) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.8(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C16 121.0(4) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 120.0(4) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C22 C17 C18 117.8(3) . . ?
C22 C17 C8 120.2(3) . . ?
C18 C17 C8 121.9(3) . . ?
C19 C18 C17 121.6(3) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.4(3) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C20 C21 C22 120.8(3) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C17 C22 C21 120.3(3) . . ?
C17 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C24 C23 C28 118.0(3) . . ?
C24 C23 C9 120.3(3) . . ?
C28 C23 C9 121.7(3) . . ?
C23 C24 C25 121.6(3) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 120.1(4) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C23 C28 C27 120.8(4) . . ?
C23 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C34 C29 C30 118.1(3) . . ?
C34 C29 C10 120.6(3) . . ?
C30 C29 C10 121.2(3) . . ?
C31 C30 C29 120.7(4) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C32 C31 C30 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 119.4(4) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C34 121.2(4) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C29 C34 C33 120.2(4) . . ?
C29 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C40 119.1(4) . . ?
C36 C35 N1 123.4(3) . . ?
C40 C35 N1 117.5(3) . . ?
C37 C36 C35 120.8(4) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C36 C37 C38 120.2(4) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C39 C38 C37 119.6(4) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C38 C39 C40 121.4(4) . . ?
C38 C39 H39 119.3 . . ?
C40 C39 H39 119.3 . . ?
C35 C40 C39 118.9(4) . . ?
C35 C40 S1 121.4(3) . . ?
C39 C40 S1 119.7(3) . . ?
S1 C41 H41A 109.5 . . ?
S1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
S1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si1 C42 H42A 109.5 . . ?
Si1 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si1 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si1 C43 H43A 109.5 . . ?
Si1 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si1 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si1 C44 H44A 109.5 . . ?
Si1 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si1 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C53 Co2 C52 42.77(12) . . ?
C53 Co2 C51 62.53(13) . . ?
C52 Co2 C51 43.12(12) . . ?
C53 Co2 C54 42.87(13) . . ?
C52 Co2 C54 61.91(17) . . ?
C51 Co2 C54 42.67(14) . . ?
C53 Co2 C47 139.82(16) . . ?
C52 Co2 C47 112.33(18) . . ?
C51 Co2 C47 126.54(15) . . ?
C54 Co2 C47 169.06(13) . . ?
C53 Co2 C48 114.41(14) . . ?
C52 Co2 C48 118.36(17) . . ?
C51 Co2 C48 157.89(16) . . ?
C54 Co2 C48 150.09(15) . . ?
C47 Co2 C48 40.30(14) . . ?
C53 Co2 C49 116.42(14) . . ?
C52 Co2 C49 148.67(14) . . ?
C51 Co2 C49 162.46(15) . . ?
C54 Co2 C49 123.32(17) . . ?
C47 Co2 C49 66.74(17) . . ?
C48 Co2 C49 39.65(17) . . ?
C53 Co2 C46 177.47(12) . . ?
C52 Co2 C46 134.78(13) . . ?
C51 Co2 C46 115.36(13) . . ?
C54 Co2 C46 136.76(14) . . ?
C47 Co2 C46 39.86(14) . . ?
C48 Co2 C46 66.93(14) . . ?
C49 Co2 C46 66.04(14) . . ?
C53 Co2 C50 142.59(13) . . ?
C52 Co2 C50 171.52(13) . . ?
C51 Co2 C50 129.64(14) . . ?
C54 Co2 C50 116.77(17) . . ?
C47 Co2 C50 67.41(18) . . ?
C48 Co2 C50 67.37(16) . . ?
C49 Co2 C50 39.67(13) . . ?
C46 Co2 C50 39.71(13) . . ?
C85 S2 C84 98.9(3) . . ?
C87 Si2 C88 105.6(2) . . ?
C87 Si2 C86 106.88(19) . . ?
C88 Si2 C86 109.7(2) . . ?
C87 Si2 C50 107.5(2) . . ?
C88 Si2 C50 110.03(19) . . ?
C86 Si2 C50 116.42(16) . . ?
C45 N2 C79 128.8(4) . . ?
C45 N2 H2 120(3) . . ?
C79 N2 H2 111(3) . . ?
O2 C45 N2 122.9(4) . . ?
O2 C45 C46 121.7(3) . . ?
N2 C45 C46 115.3(3) . . ?
C47 C46 C50 109.6(3) . . ?
C47 C46 C45 127.9(3) . . ?
C50 C46 C45 122.4(3) . . ?
C47 C46 Co2 68.9(2) . . ?
C50 C46 Co2 71.9(2) . . ?
C45 C46 Co2 128.1(3) . . ?
C46 C47 C48 107.9(3) . . ?
C46 C47 Co2 71.3(2) . . ?
C48 C47 Co2 70.2(2) . . ?
C46 C47 H47 126.0 . . ?
C48 C47 H47 126.0 . . ?
Co2 C47 H47 126.0 . . ?
C49 C48 C47 107.0(3) . . ?
C49 C48 Co2 70.3(2) . . ?
C47 C48 Co2 69.5(2) . . ?
C49 C48 H48 126.5 . . ?
C47 C48 H48 126.5 . . ?
Co2 C48 H48 126.5 . . ?
C48 C49 C50 110.9(3) . . ?
C48 C49 Co2 70.1(2) . . ?
C50 C49 Co2 72.7(2) . . ?
C48 C49 H49 124.5 . . ?
C50 C49 H49 124.5 . . ?
Co2 C49 H49 124.5 . . ?
C49 C50 C46 104.6(3) . . ?
C49 C50 Si2 125.4(3) . . ?
C46 C50 Si2 129.2(3) . . ?
C49 C50 Co2 67.6(2) . . ?
C46 C50 Co2 68.4(2) . . ?
Si2 C50 Co2 135.45(19) . . ?
C54 C51 C52 89.4(3) . . ?
C54 C51 C55 135.1(3) . . ?
C52 C51 C55 134.7(3) . . ?
C54 C51 Co2 68.79(17) . . ?
C52 C51 Co2 68.3(2) . . ?
C55 C51 Co2 127.8(2) . . ?
C53 C52 C61 133.7(3) . . ?
C53 C52 C51 90.2(3) . . ?
C61 C52 C51 135.0(3) . . ?
C53 C52 Co2 68.3(2) . . ?
C61 C52 Co2 129.4(2) . . ?
C51 C52 Co2 68.6(2) . . ?
C52 C53 C54 90.0(3) . . ?
C52 C53 C67 133.7(3) . . ?
C54 C53 C67 134.9(3) . . ?
C52 C53 Co2 69.0(2) . . ?
C54 C53 Co2 69.2(2) . . ?
C67 C53 Co2 129.3(2) . . ?
C51 C54 C53 90.5(3) . . ?
C51 C54 C73 135.2(3) . . ?
C53 C54 C73 133.6(3) . . ?
C51 C54 Co2 68.5(2) . . ?
C53 C54 Co2 67.9(2) . . ?
C73 C54 Co2 128.3(2) . . ?
C56 C55 C60 118.1(3) . . ?
C56 C55 C51 121.3(3) . . ?
C60 C55 C51 120.5(3) . . ?
C55 C56 C57 120.4(4) . . ?
C55 C56 H56 119.8 . . ?
C57 C56 H56 119.8 . . ?
C58 C57 C56 120.4(4) . . ?
C58 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
C59 C58 C57 119.7(4) . . ?
C59 C58 H58 120.1 . . ?
C57 C58 H58 120.1 . . ?
C58 C59 C60 120.5(4) . . ?
C58 C59 H59 119.8 . . ?
C60 C59 H59 119.8 . . ?
C59 C60 C55 120.8(4) . . ?
C59 C60 H60 119.6 . . ?
C55 C60 H60 119.6 . . ?
C62 C61 C66 118.2(3) . . ?
C62 C61 C52 121.2(3) . . ?
C66 C61 C52 120.4(3) . . ?
C63 C62 C61 120.3(4) . . ?
C63 C62 H62 119.9 . . ?
C61 C62 H62 119.9 . . ?
C62 C63 C64 120.7(4) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 H63 119.6 . . ?
C65 C64 C63 119.4(4) . . ?
C65 C64 H64 120.3 . . ?
C63 C64 H64 120.3 . . ?
C64 C65 C66 120.5(4) . . ?
C64 C65 H65 119.8 . . ?
C66 C65 H65 119.8 . . ?
C65 C66 C61 120.9(4) . . ?
C65 C66 H66 119.5 . . ?
C61 C66 H66 119.5 . . ?
C68 C67 C72 117.9(3) . . ?
C68 C67 C53 122.1(3) . . ?
C72 C67 C53 119.8(3) . . ?
C67 C68 C69 121.7(4) . . ?
C67 C68 H68 119.2 . . ?
C69 C68 H68 119.2 . . ?
C70 C69 C68 119.0(4) . . ?
C70 C69 H69 120.5 . . ?
C68 C69 H69 120.5 . . ?
C71 C70 C69 120.1(4) . . ?
C71 C70 H70 119.9 . . ?
C69 C70 H70 119.9 . . ?
C70 C71 C72 121.1(4) . . ?
C70 C71 H71 119.4 . . ?
C72 C71 H71 119.4 . . ?
C71 C72 C67 120.2(4) . . ?
C71 C72 H72 119.9 . . ?
C67 C72 H72 119.9 . . ?
C78 C73 C74 117.8(3) . . ?
C78 C73 C54 121.4(3) . . ?
C74 C73 C54 120.8(3) . . ?
C75 C74 C73 120.8(4) . . ?
C75 C74 H74 119.6 . . ?
C73 C74 H74 119.6 . . ?
C76 C75 C74 120.5(4) . . ?
C76 C75 H75 119.8 . . ?
C74 C75 H75 119.8 . . ?
C77 C76 C75 119.5(4) . . ?
C77 C76 H76 120.2 . . ?
C75 C76 H76 120.2 . . ?
C76 C77 C78 120.6(4) . . ?
C76 C77 H77 119.7 . . ?
C78 C77 H77 119.7 . . ?
C77 C78 C73 120.8(4) . . ?
C77 C78 H78 119.6 . . ?
C73 C78 H78 119.6 . . ?
C84 C79 C80 119.4(4) . . ?
C84 C79 N2 117.3(4) . . ?
C80 C79 N2 123.3(4) . . ?
C81 C80 C79 119.7(5) . . ?
C81 C80 H80 120.2 . . ?
C79 C80 H80 120.2 . . ?
C82 C81 C80 121.6(5) . . ?
C82 C81 H81 119.2 . . ?
C80 C81 H81 119.2 . . ?
C81 C82 C83 119.2(5) . . ?
C81 C82 H82 120.4 . . ?
C83 C82 H82 120.4 . . ?
C82 C83 C84 121.1(5) . . ?
C82 C83 H83 119.5 . . ?
C84 C83 H83 119.5 . . ?
C79 C84 C83 119.0(4) . . ?
C79 C84 S2 121.0(3) . . ?
C83 C84 S2 120.0(4) . . ?
S2 C85 H85A 109.5 . . ?
S2 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
S2 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
Si2 C86 H86A 109.5 . . ?
Si2 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
Si2 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
Si2 C87 H87A 109.5 . . ?
Si2 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
Si2 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
Si2 C88 H88A 109.5 . . ?
Si2 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
Si2 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?

_refine_diff_density_max         0.802
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_4b
_database_code_depnum_ccdc_archive 'CCDC 1523204'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H32 Co N O S'
_chemical_formula_sum            'C41 H32 Co N O S'
_chemical_formula_weight         645.66

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   11.255(6)
_cell_length_b                   22.409(10)
_cell_length_c                   12.599(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.186(16)
_cell_angle_gamma                90
_cell_volume                     3178(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    304(2)
_cell_measurement_reflns_used    4659
_cell_measurement_theta_min      3.184
_cell_measurement_theta_max      22.448

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.211
_exptl_absorpt_coefficient_mu    0.640
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      304(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13462
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.565
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             6363
_reflns_number_gt                4216
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0611P)²+0.1266P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6363
_refine_ls_number_parameters     412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co01 Co 0.36640(3) 0.34886(2) 0.31338(3) 0.04073(15) Uani 1 1 d . . . . .
S002 S -0.12746(8) 0.26858(4) 0.25724(7) 0.0642(3) Uani 1 1 d . . . . .
N003 N 0.0894(2) 0.31458(12) 0.1449(2) 0.0541(7) Uani 1 1 d . . . . .
O004 O 0.2355(2) 0.33728(12) 0.02504(18) 0.0801(8) Uani 1 1 d . . . . .
C005 C 0.2407(2) 0.37827(11) 0.5271(2) 0.0374(6) Uani 1 1 d . . . . .
C006 C 0.1781(2) 0.44978(11) 0.2823(2) 0.0384(6) Uani 1 1 d . . . . .
C007 C 0.4838(2) 0.46860(12) 0.2369(2) 0.0387(6) Uani 1 1 d . . . . .
C008 C 0.4396(2) 0.40554(11) 0.4164(2) 0.0362(6) Uani 1 1 d . . . . .
C009 C 0.5484(2) 0.39794(11) 0.4801(2) 0.0385(6) Uani 1 1 d . . . . .
C00A C 0.2764(2) 0.39086(12) 0.6312(2) 0.0437(7) Uani 1 1 d . . . . .
H00A H 0.347847 0.410615 0.643122 0.052 Uiso 1 1 calc R U . . .
C00B C 0.3121(2) 0.39748(11) 0.4359(2) 0.0367(6) Uani 1 1 d . . . . .
C00C C 0.4130(2) 0.43429(11) 0.3145(2) 0.0371(6) Uani 1 1 d . . . . .
C00D C 0.2854(2) 0.42731(11) 0.3348(2) 0.0365(6) Uani 1 1 d . . . . .
C00E C 0.1321(2) 0.34895(12) 0.5133(2) 0.0446(7) Uani 1 1 d . . . . .
H00E H 0.106432 0.339731 0.445000 0.053 Uiso 1 1 calc R U . . .
C00F C -0.0161(3) 0.32426(13) 0.0871(2) 0.0495(7) Uani 1 1 d . . . . .
C00G C 0.4539(3) 0.52736(13) 0.2152(2) 0.0499(7) Uani 1 1 d . . . . .
H00G H 0.388635 0.544607 0.248319 0.060 Uiso 1 1 calc R U . . .
C00H C 0.2067(3) 0.37432(13) 0.7167(2) 0.0523(7) Uani 1 1 d . . . . .
H00H H 0.232570 0.382209 0.785444 0.063 Uiso 1 1 calc R U . . .
C00I C 0.1812(3) 0.46426(13) 0.1742(2) 0.0503(7) Uani 1 1 d . . . . .
H00I H 0.249887 0.457218 0.135438 0.060 Uiso 1 1 calc R U . . .
C00J C -0.1241(3) 0.30524(12) 0.1318(2) 0.0514(7) Uani 1 1 d . . . . .
C00K C 0.0729(2) 0.46019(12) 0.3378(2) 0.0475(7) Uani 1 1 d . . . . .
H00K H 0.068234 0.450311 0.409360 0.057 Uiso 1 1 calc R U . . .
C00L C 0.2950(3) 0.29765(13) 0.1915(2) 0.0520(8) Uani 1 1 d . . . . .
C00M C 0.6407(2) 0.43842(13) 0.4703(2) 0.0471(7) Uani 1 1 d . . . . .
H00M H 0.634643 0.469425 0.421516 0.057 Uiso 1 1 calc R U . . .
C00N C 0.0621(2) 0.33337(13) 0.5984(2) 0.0494(7) Uani 1 1 d . . . . .
H00N H -0.010097 0.314204 0.587149 0.059 Uiso 1 1 calc R U . . .
C00O C 0.0991(3) 0.34616(12) 0.7003(2) 0.0528(8) Uani 1 1 d . . . . .
H00O H 0.051765 0.335856 0.757832 0.063 Uiso 1 1 calc R U . . .
C00P C 0.2762(3) 0.26947(12) 0.2916(2) 0.0558(8) Uani 1 1 d . . . . .
H00P H 0.202778 0.260002 0.320804 0.067 Uiso 1 1 calc R U . . .
C00Q C 0.5589(3) 0.35223(13) 0.5553(2) 0.0524(8) Uani 1 1 d . . . . .
H00Q H 0.497804 0.324684 0.563488 0.063 Uiso 1 1 calc R U . . .
C00R C 0.2055(3) 0.31839(14) 0.1117(2) 0.0546(8) Uani 1 1 d . . . . .
C00S C -0.0247(3) 0.48517(14) 0.2869(3) 0.0618(9) Uani 1 1 d . . . . .
H00S H -0.094205 0.492155 0.324642 0.074 Uiso 1 1 calc R U . . .
C00T C -0.0191(3) 0.49963(14) 0.1810(3) 0.0661(9) Uani 1 1 d . . . . .
H00T H -0.084320 0.516697 0.147238 0.079 Uiso 1 1 calc R U . . .
C00U C 0.6170(3) 0.53637(17) 0.0941(2) 0.0660(10) Uani 1 1 d . . . . .
H00U H 0.660665 0.558913 0.046019 0.079 Uiso 1 1 calc R U . . .
C00V C 0.4197(3) 0.30334(14) 0.1772(3) 0.0617(9) Uani 1 1 d . . . . .
H00V H 0.457010 0.319738 0.118305 0.074 Uiso 1 1 calc R U . . .
C00W C 0.5827(2) 0.44538(14) 0.1860(2) 0.0565(8) Uani 1 1 d . . . . .
H00W H 0.605484 0.406259 0.199903 0.068 Uiso 1 1 calc R U . . .
C00X C -0.0177(3) 0.35179(14) -0.0125(2) 0.0631(9) Uani 1 1 d . . . . .
H00X H 0.052623 0.365139 -0.042967 0.076 Uiso 1 1 calc R U . . .
C00Y C 0.5209(3) 0.56051(15) 0.1444(3) 0.0648(9) Uani 1 1 d . . . . .
H00Y H 0.500054 0.599957 0.130925 0.078 Uiso 1 1 calc R U . . .
C00Z C 0.0839(3) 0.48870(15) 0.1251(2) 0.0621(9) Uani 1 1 d . . . . .
H00Z H 0.087273 0.498031 0.053219 0.074 Uiso 1 1 calc R U . . .
C010 C 0.6479(3) 0.47880(17) 0.1153(3) 0.0687(10) Uani 1 1 d . . . . .
H010 H 0.713453 0.461982 0.081956 0.082 Uiso 1 1 calc R U . . .
C011 C 0.7506(3) 0.38815(18) 0.6069(3) 0.0687(10) Uani 1 1 d . . . . .
H011 H 0.817806 0.385209 0.649640 0.082 Uiso 1 1 calc R U . . .
C012 C 0.3884(3) 0.25838(13) 0.3387(3) 0.0666(9) Uani 1 1 d . . . . .
H012 H 0.402111 0.240344 0.404082 0.080 Uiso 1 1 calc R U . . .
C013 C -0.1254(3) 0.35906(15) -0.0657(3) 0.0701(10) Uani 1 1 d . . . . .
H013 H -0.126235 0.377593 -0.131706 0.084 Uiso 1 1 calc R U . . .
C014 C 0.6604(3) 0.34801(15) 0.6176(3) 0.0670(10) Uani 1 1 d . . . . .
H014 H 0.667036 0.317463 0.667245 0.080 Uiso 1 1 calc R U . . .
C015 C 0.7420(3) 0.43312(17) 0.5325(3) 0.0645(9) Uani 1 1 d . . . . .
H015 H 0.804328 0.459952 0.524136 0.077 Uiso 1 1 calc R U . . .
C016 C -0.2295(3) 0.31204(15) 0.0762(3) 0.0678(9) Uani 1 1 d . . . . .
H016 H -0.300247 0.298185 0.105040 0.081 Uiso 1 1 calc R U . . .
C017 C 0.4768(3) 0.28006(14) 0.2671(3) 0.0686(10) Uani 1 1 d . . . . .
H017 H 0.558483 0.278892 0.278293 0.082 Uiso 1 1 calc R U . . .
C018 C -0.2299(4) 0.33961(17) -0.0231(3) 0.0784(11) Uani 1 1 d . . . . .
H018 H -0.300866 0.344713 -0.060050 0.094 Uiso 1 1 calc R U . . .
C019 C -0.1676(3) 0.32802(17) 0.3452(3) 0.0820(11) Uani 1 1 d . . . . .
H01A H -0.108365 0.358792 0.342199 0.123 Uiso 1 1 calc R U . . .
H01B H -0.172833 0.312988 0.416366 0.123 Uiso 1 1 calc R U . . .
H01C H -0.243107 0.344128 0.324110 0.123 Uiso 1 1 calc R U . . .
H1 H 0.074(3) 0.2983(13) 0.212(2) 0.069(10) Uiso 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
Co01 C00C 1.985(3) . ?
Co01 C00B 1.987(3) . ?
Co01 C008 1.992(2) . ?
Co01 C00D 1.999(3) . ?
Co01 C017 2.066(3) . ?
Co01 C00P 2.067(3) . ?
Co01 C012 2.067(3) . ?
Co01 C00L 2.077(3) . ?
Co01 C00V 2.085(3) . ?
S002 C00J 1.781(3) . ?
S002 C019 1.791(3) . ?
N003 C00R 1.376(4) . ?
N003 C00F 1.408(4) . ?
N003 H1 0.94(3) . ?
O004 C00R 1.220(4) . ?
C005 C00E 1.398(4) . ?
C005 C00A 1.399(4) . ?
C005 C00B 1.469(3) . ?
C006 C00K 1.397(4) . ?
C006 C00I 1.400(4) . ?
C006 C00D 1.464(3) . ?
C007 C00G 1.386(4) . ?
C007 C00W 1.388(4) . ?
C007 C00C 1.479(3) . ?
C008 C00C 1.466(3) . ?
C008 C00B 1.468(3) . ?
C008 C009 1.472(3) . ?
C009 C00M 1.385(4) . ?
C009 C00Q 1.400(4) . ?
C00A C00H 1.385(4) . ?
C00A H00A 0.9300 . ?
C00B C00D 1.468(3) . ?
C00C C00D 1.468(3) . ?
C00E C00N 1.377(4) . ?
C00E H00E 0.9300 . ?
C00F C00X 1.398(4) . ?
C00F C00J 1.408(4) . ?
C00G C00Y 1.386(4) . ?
C00G H00G 0.9300 . ?
C00H C00O 1.381(4) . ?
C00H H00H 0.9300 . ?
C00I C00Z 1.371(4) . ?
C00I H00I 0.9300 . ?
C00J C016 1.384(4) . ?
C00K C00S 1.388(4) . ?
C00K H00K 0.9300 . ?
C00L C00V 1.421(4) . ?
C00L C00P 1.426(4) . ?
C00L C00R 1.495(4) . ?
C00M C015 1.387(4) . ?
C00M H00M 0.9300 . ?
C00N C00O 1.378(4) . ?
C00N H00N 0.9300 . ?
C00O H00O 0.9300 . ?
C00P C012 1.416(4) . ?
C00P H00P 0.9300 . ?
C00Q C014 1.387(4) . ?
C00Q H00Q 0.9300 . ?
C00S C00T 1.375(4) . ?
C00S H00S 0.9300 . ?
C00T C00Z 1.380(4) . ?
C00T H00T 0.9300 . ?
C00U C010 1.362(5) . ?
C00U C00Y 1.368(4) . ?
C00U H00U 0.9300 . ?
C00V C017 1.401(4) . ?
C00V H00V 0.9300 . ?
C00W C010 1.377(4) . ?
C00W H00W 0.9300 . ?
C00X C013 1.394(5) . ?
C00X H00X 0.9300 . ?
C00Y H00Y 0.9300 . ?
C00Z H00Z 0.9300 . ?
C010 H010 0.9300 . ?
C011 C014 1.363(5) . ?
C011 C015 1.379(5) . ?
C011 H011 0.9300 . ?
C012 C017 1.430(5) . ?
C012 H012 0.9300 . ?
C013 C018 1.365(5) . ?
C013 H013 0.9300 . ?
C014 H014 0.9300 . ?
C015 H015 0.9300 . ?
C016 C018 1.395(5) . ?
C016 H016 0.9300 . ?
C017 H017 0.9300 . ?
C018 H018 0.9300 . ?
C019 H01A 0.9600 . ?
C019 H01B 0.9600 . ?
C019 H01C 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
C00C Co01 C00B 63.10(10) . . ?
C00C Co01 C008 43.26(10) . . ?
C00B Co01 C008 43.30(10) . . ?
C00C Co01 C00D 43.25(10) . . ?
C00B Co01 C00D 43.23(10) . . ?
C008 Co01 C00D 62.57(10) . . ?
C00C Co01 C017 124.25(13) . . ?
C00B Co01 C017 144.61(13) . . ?
C008 Co01 C017 114.31(12) . . ?
C00D Co01 C017 165.86(13) . . ?
C00C Co01 C00P 163.95(11) . . ?
C00B Co01 C00P 115.03(12) . . ?
C008 Co01 C00P 146.89(11) . . ?
C00D Co01 C00P 123.42(12) . . ?
C017 Co01 C00P 67.39(14) . . ?
C00C Co01 C012 155.96(12) . . ?
C00B Co01 C012 117.05(13) . . ?
C008 Co01 C012 118.40(12) . . ?
C00D Co01 C012 153.64(13) . . ?
C017 Co01 C012 40.49(13) . . ?
C00P Co01 C012 40.07(12) . . ?
C00C Co01 C00L 129.79(11) . . ?
C00B Co01 C00L 139.30(11) . . ?
C008 Co01 C00L 172.82(11) . . ?
C00D Co01 C00L 114.23(11) . . ?
C017 Co01 C00L 67.07(13) . . ?
C00P Co01 C00L 40.27(11) . . ?
C012 Co01 C00L 67.54(13) . . ?
C00C Co01 C00V 113.64(12) . . ?
C00B Co01 C00V 175.58(12) . . ?
C008 Co01 C00V 136.72(11) . . ?
C00D Co01 C00V 132.37(12) . . ?
C017 Co01 C00V 39.44(12) . . ?
C00P Co01 C00V 67.17(13) . . ?
C012 Co01 C00V 67.20(14) . . ?
C00L Co01 C00V 39.93(11) . . ?
C00J S002 C019 102.23(17) . . ?
C00R N003 C00F 129.3(3) . . ?
C00R N003 H1 118.4(19) . . ?
C00F N003 H1 111.7(19) . . ?
C00E C005 C00A 117.4(2) . . ?
C00E C005 C00B 121.4(2) . . ?
C00A C005 C00B 121.2(2) . . ?
C00K C006 C00I 118.1(2) . . ?
C00K C006 C00D 122.0(2) . . ?
C00I C006 C00D 119.8(2) . . ?
C00G C007 C00W 117.4(3) . . ?
C00G C007 C00C 119.6(2) . . ?
C00W C007 C00C 123.0(3) . . ?
C00C C008 C00B 90.20(19) . . ?
C00C C008 C009 134.1(2) . . ?
C00B C008 C009 134.9(2) . . ?
C00C C008 Co01 68.10(14) . . ?
C00B C008 Co01 68.17(14) . . ?
C009 C008 Co01 128.56(18) . . ?
C00M C009 C00Q 118.6(2) . . ?
C00M C009 C008 119.9(2) . . ?
C00Q C009 C008 121.5(2) . . ?
C00H C00A C005 120.9(3) . . ?
C00H C00A H00A 119.6 . . ?
C005 C00A H00A 119.6 . . ?
C008 C00B C00D 89.8(2) . . ?
C008 C00B C005 134.9(2) . . ?
C00D C00B C005 134.4(2) . . ?
C008 C00B Co01 68.53(14) . . ?
C00D C00B Co01 68.81(14) . . ?
C005 C00B Co01 128.12(18) . . ?
C008 C00C C00D 89.9(2) . . ?
C008 C00C C007 134.3(2) . . ?
C00D C00C C007 134.4(2) . . ?
C008 C00C Co01 68.64(14) . . ?
C00D C00C Co01 68.89(14) . . ?
C007 C00C Co01 129.74(18) . . ?
C006 C00D C00C 133.6(2) . . ?
C006 C00D C00B 135.7(2) . . ?
C00C C00D C00B 90.10(19) . . ?
C006 C00D Co01 128.08(18) . . ?
C00C C00D Co01 67.86(14) . . ?
C00B C00D Co01 67.96(14) . . ?
C00N C00E C005 121.6(3) . . ?
C00N C00E H00E 119.2 . . ?
C005 C00E H00E 119.2 . . ?
C00X C00F N003 122.8(3) . . ?
C00X C00F C00J 119.0(3) . . ?
N003 C00F C00J 118.3(3) . . ?
C00Y C00G C007 120.3(3) . . ?
C00Y C00G H00G 119.9 . . ?
C007 C00G H00G 119.9 . . ?
C00O C00H C00A 120.3(3) . . ?
C00O C00H H00H 119.8 . . ?
C00A C00H H00H 119.8 . . ?
C00Z C00I C006 120.7(3) . . ?
C00Z C00I H00I 119.7 . . ?
C006 C00I H00I 119.7 . . ?
C016 C00J C00F 120.2(3) . . ?
C016 C00J S002 118.7(3) . . ?
C00F C00J S002 121.0(2) . . ?
C00S C00K C006 120.5(3) . . ?
C00S C00K H00K 119.8 . . ?
C006 C00K H00K 119.8 . . ?
C00V C00L C00P 107.5(3) . . ?
C00V C00L C00R 123.4(3) . . ?
C00P C00L C00R 129.1(3) . . ?
C00V C00L Co01 70.36(16) . . ?
C00P C00L Co01 69.48(15) . . ?
C00R C00L Co01 125.7(2) . . ?
C009 C00M C015 120.6(3) . . ?
C009 C00M H00M 119.7 . . ?
C015 C00M H00M 119.7 . . ?
C00E C00N C00O 120.1(3) . . ?
C00E C00N H00N 120.0 . . ?
C00O C00N H00N 120.0 . . ?
C00N C00O C00H 119.7(3) . . ?
C00N C00O H00O 120.1 . . ?
C00H C00O H00O 120.1 . . ?
C012 C00P C00L 108.3(3) . . ?
C012 C00P Co01 69.99(17) . . ?
C00L C00P Co01 70.25(16) . . ?
C012 C00P H00P 125.9 . . ?
C00L C00P H00P 125.9 . . ?
Co01 C00P H00P 125.5 . . ?
C014 C00Q C009 120.0(3) . . ?
C014 C00Q H00Q 120.0 . . ?
C009 C00Q H00Q 120.0 . . ?
O004 C00R N003 124.0(3) . . ?
O004 C00R C00L 121.5(3) . . ?
N003 C00R C00L 114.5(3) . . ?
C00T C00S C00K 120.3(3) . . ?
C00T C00S H00S 119.9 . . ?
C00K C00S H00S 119.9 . . ?
C00S C00T C00Z 119.7(3) . . ?
C00S C00T H00T 120.2 . . ?
C00Z C00T H00T 120.2 . . ?
C010 C00U C00Y 119.0(3) . . ?
C010 C00U H00U 120.5 . . ?
C00Y C00U H00U 120.5 . . ?
C017 C00V C00L 108.4(3) . . ?
C017 C00V Co01 69.52(18) . . ?
C00L C00V Co01 69.71(17) . . ?
C017 C00V H00V 125.8 . . ?
C00L C00V H00V 125.8 . . ?
Co01 C00V H00V 126.5 . . ?
C010 C00W C007 121.7(3) . . ?
C010 C00W H00W 119.2 . . ?
C007 C00W H00W 119.2 . . ?
C013 C00X C00F 119.5(3) . . ?
C013 C00X H00X 120.3 . . ?
C00F C00X H00X 120.3 . . ?
C00U C00Y C00G 121.3(3) . . ?
C00U C00Y H00Y 119.4 . . ?
C00G C00Y H00Y 119.4 . . ?
C00I C00Z C00T 120.7(3) . . ?
C00I C00Z H00Z 119.6 . . ?
C00T C00Z H00Z 119.6 . . ?
C00U C010 C00W 120.4(3) . . ?
C00U C010 H010 119.8 . . ?
C00W C010 H010 119.8 . . ?
C014 C011 C015 120.0(3) . . ?
C014 C011 H011 120.0 . . ?
C015 C011 H011 120.0 . . ?
C00P C012 C017 107.3(3) . . ?
C00P C012 Co01 69.93(16) . . ?
C017 C012 Co01 69.68(18) . . ?
C00P C012 H012 126.4 . . ?
C017 C012 H012 126.4 . . ?
Co01 C012 H012 125.6 . . ?
C018 C013 C00X 121.6(3) . . ?
C018 C013 H013 119.2 . . ?
C00X C013 H013 119.2 . . ?
C011 C014 C00Q 120.7(3) . . ?
C011 C014 H014 119.6 . . ?
C00Q C014 H014 119.6 . . ?
C011 C015 C00M 120.1(3) . . ?
C011 C015 H015 119.9 . . ?
C00M C015 H015 119.9 . . ?
C00J C016 C018 120.2(3) . . ?
C00J C016 H016 119.9 . . ?
C018 C016 H016 119.9 . . ?
C00V C017 C012 108.5(3) . . ?
C00V C017 Co01 71.04(18) . . ?
C012 C017 Co01 69.83(18) . . ?
C00V C017 H017 125.7 . . ?
C012 C017 H017 125.7 . . ?
Co01 C017 H017 125.0 . . ?
C013 C018 C016 119.5(3) . . ?
C013 C018 H018 120.2 . . ?
C016 C018 H018 120.2 . . ?
S002 C019 H01A 109.5 . . ?
S002 C019 H01B 109.5 . . ?
H01A C019 H01B 109.5 . . ?
S002 C019 H01C 109.5 . . ?
H01A C019 H01C 109.5 . . ?
H01B C019 H01C 109.5 . . ?

_refine_diff_density_max         0.224
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.047

####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1523201'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C18 H15 Fe N3 O2 Pd), H2 O'
_chemical_formula_sum            'C36 H32 Fe2 N6 O5 Pd2'
_chemical_formula_weight         953.18

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'
Fe Fe 0.3463 0.8444 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.80(3)
_cell_length_b                   11.71(3)
_cell_length_c                   15.37(4)
_cell_angle_alpha                95.62(4)
_cell_angle_beta                 101.53(4)
_cell_angle_gamma                103.73(4)
_cell_volume                     1828(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3659
_cell_measurement_theta_min      2.367
_cell_measurement_theta_max      26.137

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.115
_exptl_absorpt_coefficient_mu    1.795
_shelx_estimated_absorpt_T_min   0.596
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11198
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.368
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             8081
_reflns_number_gt                5484
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0650P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8081
_refine_ls_number_parameters     465
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_restrained_S_all      0.931
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd2 Pd 0.85322(4) 1.00856(3) 0.52111(2) 0.03893(12) Uani 1 1 d . . . . .
Fe1 Fe 0.59708(7) 0.73649(6) 0.46050(5) 0.04148(18) Uani 1 1 d . . . . .
O1 O 0.9199(4) 0.7065(3) 0.6239(3) 0.0579(10) Uani 1 1 d . . . . .
O2 O 0.9602(4) 1.1422(3) 0.6344(2) 0.0508(9) Uani 1 1 d . . . . .
N1 N 0.9145(4) 0.9047(4) 0.6092(3) 0.0411(9) Uani 1 1 d . . . . .
N2 N 1.0179(4) 1.0878(4) 0.7003(3) 0.0431(10) Uani 1 1 d . . . . .
N3 N 0.7922(4) 1.1137(4) 0.4310(3) 0.0465(10) Uani 1 1 d . . . . .
C19 C 0.8834(5) 0.7817(4) 0.5801(3) 0.0405(11) Uani 1 1 d . . . . .
C20 C 0.7976(5) 0.7556(4) 0.4867(3) 0.0415(11) Uani 1 1 d . . . . .
C21 C 0.7276(5) 0.6418(5) 0.4288(4) 0.0465(12) Uani 1 1 d . . . . .
H21 H 0.7289 0.5659 0.4414 0.056 Uiso 1 1 calc R U . . .
C22 C 0.6559(6) 0.6725(5) 0.3480(4) 0.0547(14) Uani 1 1 d . . . . .
H22 H 0.6039 0.6181 0.2985 0.066 Uiso 1 1 calc R U . . .
C23 C 0.6772(5) 0.7994(5) 0.3558(3) 0.0509(13) Uani 1 1 d . . . . .
H23 H 0.6397 0.8404 0.3135 0.061 Uiso 1 1 calc R U . . .
C24 C 0.7673(5) 0.8520(4) 0.4413(3) 0.0401(11) Uani 1 1 d . . . . .
C25 C 0.5038(6) 0.8415(5) 0.5261(4) 0.0568(15) Uani 1 1 d . . . . .
H25 H 0.5287 0.9242 0.5371 0.068 Uiso 1 1 calc R U . . .
C26 C 0.5501(6) 0.7665(5) 0.5845(4) 0.0520(13) Uani 1 1 d . . . . .
H26 H 0.6099 0.7912 0.6397 0.062 Uiso 1 1 calc R U . . .
C27 C 0.4880(6) 0.6455(5) 0.5427(4) 0.0555(14) Uani 1 1 d . . . . .
H27 H 0.5001 0.5778 0.5664 0.067 Uiso 1 1 calc R U . . .
C28 C 0.4040(6) 0.6478(6) 0.4583(4) 0.0624(16) Uani 1 1 d . . . . .
H28 H 0.3526 0.5817 0.4173 0.075 Uiso 1 1 calc R U . . .
C29 C 0.4129(6) 0.7707(6) 0.4476(5) 0.0639(16) Uani 1 1 d . . . . .
H29 H 0.3684 0.7982 0.3992 0.077 Uiso 1 1 calc R U . . .
C30 C 0.9961(5) 0.9640(4) 0.6910(3) 0.0392(11) Uani 1 1 d . . . . .
C31 C 1.0571(5) 0.9157(5) 0.7632(4) 0.0493(13) Uani 1 1 d . . . . .
H31 H 1.0445 0.8337 0.7585 0.059 Uiso 1 1 calc R U . . .
C32 C 1.1365(6) 0.9889(6) 0.8422(4) 0.0608(15) Uani 1 1 d . . . . .
H32 H 1.1751 0.9557 0.8895 0.073 Uiso 1 1 calc R U . . .
C33 C 1.1568(6) 1.1118(6) 0.8491(4) 0.0601(15) Uani 1 1 d . . . . .
H33 H 1.2089 1.1611 0.9011 0.072 Uiso 1 1 calc R U . . .
C34 C 1.0986(5) 1.1604(5) 0.7774(4) 0.0523(13) Uani 1 1 d . . . . .
H34 H 1.1140 1.2425 0.7814 0.063 Uiso 1 1 calc R U . . .
C35 C 0.7671(5) 1.1780(5) 0.3834(3) 0.0434(11) Uani 1 1 d . . . . .
C36 C 0.7367(6) 1.2637(5) 0.3222(4) 0.0623(16) Uani 1 1 d . . . . .
H36A H 0.8046 1.3369 0.3390 0.093 Uiso 1 1 calc R U . . .
H36B H 0.6544 1.2787 0.3266 0.093 Uiso 1 1 calc R U . . .
H36C H 0.7316 1.2307 0.2615 0.093 Uiso 1 1 calc R U . . .
Pd3 Pd 0.04274(4) 0.63559(4) 0.10864(3) 0.04331(13) Uani 1 1 d . . . . .
Fe2 Fe 0.35270(8) 0.84673(7) 0.12189(5) 0.0494(2) Uani 1 1 d . . . . .
O3 O 0.1477(4) 0.7085(4) -0.1305(2) 0.0551(10) Uani 1 1 d . . . . .
O4 O -0.1674(4) 0.6081(4) 0.0667(3) 0.0573(10) Uani 1 1 d . . . . .
N4 N 0.0262(4) 0.6635(4) -0.0203(3) 0.0417(9) Uani 1 1 d . . . . .
N5 N -0.1984(4) 0.6207(4) -0.0224(3) 0.0509(11) Uani 1 1 d . . . . .
N6 N 0.0593(5) 0.6077(4) 0.2389(3) 0.0508(11) Uani 1 1 d . . . . .
C1 C 0.1411(5) 0.6924(4) -0.0518(3) 0.0437(12) Uani 1 1 d . . . . .
C2 C 0.2579(5) 0.6996(5) 0.0226(3) 0.0444(12) Uani 1 1 d . . . . .
C3 C 0.3977(5) 0.7306(5) 0.0292(4) 0.0535(14) Uani 1 1 d . . . . .
H3 H 0.4390 0.7522 -0.0166 0.064 Uiso 1 1 calc R U . . .
C4 C 0.4619(6) 0.7219(5) 0.1193(4) 0.0585(15) Uani 1 1 d . . . . .
H4 H 0.5517 0.7356 0.1413 0.070 Uiso 1 1 calc R U . . .
C5 C 0.3632(6) 0.6885(5) 0.1690(4) 0.0537(14) Uani 1 1 d . . . . .
H5 H 0.3789 0.6786 0.2291 0.064 Uiso 1 1 calc R U . . .
C6 C 0.2339(5) 0.6726(5) 0.1099(3) 0.0483(12) Uani 1 1 d . . . . .
C7 C 0.2841(8) 0.9589(6) 0.2022(6) 0.087(2) Uani 1 1 d . . . . .
H7 H 0.2238 0.9345 0.2366 0.105 Uiso 1 1 calc R U . . .
C8 C 0.2553(8) 0.9801(6) 0.1124(6) 0.087(2) Uani 1 1 d . . . . .
H8 H 0.1716 0.9726 0.0781 0.104 Uiso 1 1 calc R U . . .
C9 C 0.3700(9) 1.0138(6) 0.0830(5) 0.086(2) Uani 1 1 d . . . . .
H9 H 0.3762 1.0306 0.0259 0.103 Uiso 1 1 calc R U . . .
C10 C 0.4765(7) 1.0179(6) 0.1555(6) 0.081(2) Uani 1 1 d . . . . .
H10 H 0.5647 1.0402 0.1544 0.098 Uiso 1 1 calc R U . . .
C11 C 0.4252(8) 0.9821(6) 0.2307(5) 0.078(2) Uani 1 1 d . . . . .
H11 H 0.4729 0.9753 0.2865 0.094 Uiso 1 1 calc R U . . .
C12 C -0.1016(5) 0.6465(4) -0.0707(3) 0.0432(11) Uani 1 1 d . . . . .
C13 C -0.1435(6) 0.6516(5) -0.1641(4) 0.0600(15) Uani 1 1 d . . . . .
H13 H -0.0820 0.6653 -0.1991 0.072 Uiso 1 1 calc R U . . .
C14 C -0.2766(7) 0.6361(6) -0.2037(5) 0.076(2) Uani 1 1 d . . . . .
H14 H -0.3026 0.6398 -0.2646 0.091 Uiso 1 1 calc R U . . .
C15 C -0.3711(6) 0.6151(6) -0.1513(5) 0.0744(19) Uani 1 1 d . . . . .
H15 H -0.4588 0.6079 -0.1768 0.089 Uiso 1 1 calc R U . . .
C16 C -0.3314(6) 0.6053(5) -0.0610(5) 0.0640(16) Uani 1 1 d . . . . .
H16 H -0.3931 0.5887 -0.0264 0.077 Uiso 1 1 calc R U . . .
C17 C 0.0551(5) 0.5977(5) 0.3118(4) 0.0486(13) Uani 1 1 d . . . . .
C18 C 0.0468(6) 0.5830(6) 0.4060(4) 0.0626(16) Uani 1 1 d . . . . .
H18A H 0.0454 0.5027 0.4147 0.094 Uiso 1 1 calc R U . . .
H18B H -0.0319 0.6002 0.4170 0.094 Uiso 1 1 calc R U . . .
H18C H 0.1215 0.6367 0.4470 0.094 Uiso 1 1 calc R U . . .
O5 O 0.7077(6) 0.4616(5) 0.1871(4) 0.0870(15) Uani 1 1 d G . . . .
H5A H 0.7076 0.5140 0.1526 0.131 Uiso 1 1 d G U . . .
H5B H 0.7296 0.4035 0.1625 0.131 Uiso 1 1 d G 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
Pd2 C24 2.006(6) . ?
Pd2 N1 2.024(5) . ?
Pd2 N3 2.055(6) . ?
Pd2 O2 2.149(5) . ?
Fe1 C25 2.072(6) . ?
Fe1 C20 2.074(7) . ?
Fe1 C26 2.086(7) . ?
Fe1 C28 2.088(8) . ?
Fe1 C21 2.088(6) . ?
Fe1 C22 2.089(7) . ?
Fe1 C23 2.089(7) . ?
Fe1 C27 2.094(7) . ?
Fe1 C29 2.095(8) . ?
Fe1 C24 2.100(6) . ?
O1 C19 1.249(6) . ?
O2 N2 1.373(6) . ?
N1 C30 1.390(7) . ?
N1 C19 1.404(7) . ?
N2 C34 1.386(7) . ?
N2 C30 1.402(7) . ?
N3 C35 1.140(6) . ?
C19 C20 1.504(8) . ?
C20 C24 1.451(7) . ?
C20 C21 1.470(8) . ?
C21 C22 1.451(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.439(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.449(8) . ?
C23 H23 0.9300 . ?
C25 C26 1.418(8) . ?
C25 C29 1.432(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.439(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.434(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.447(10) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.413(7) . ?
C31 C32 1.405(8) . ?
C31 H31 0.9300 . ?
C32 C33 1.393(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.396(8) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.489(8) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
Pd3 C6 2.001(8) . ?
Pd3 N4 2.019(6) . ?
Pd3 N6 2.040(7) . ?
Pd3 O4 2.166(7) . ?
Fe2 C11 2.071(7) . ?
Fe2 C5 2.074(7) . ?
Fe2 C7 2.075(7) . ?
Fe2 C9 2.079(9) . ?
Fe2 C10 2.079(8) . ?
Fe2 C3 2.081(6) . ?
Fe2 C8 2.081(8) . ?
Fe2 C4 2.087(7) . ?
Fe2 C2 2.090(6) . ?
Fe2 C6 2.105(7) . ?
O3 C1 1.257(7) . ?
O4 N5 1.374(7) . ?
N4 C12 1.398(7) . ?
N4 C1 1.401(7) . ?
N5 C12 1.393(7) . ?
N5 C16 1.400(8) . ?
N6 C17 1.147(7) . ?
C1 C2 1.502(8) . ?
C2 C3 1.446(8) . ?
C2 C6 1.467(8) . ?
C3 C4 1.444(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.435(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.464(8) . ?
C5 H5 0.9300 . ?
C7 C8 1.412(11) . ?
C7 C11 1.448(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.387(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.420(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.434(11) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.428(8) . ?
C13 C14 1.405(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.413(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.393(10) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.493(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O5 H5A 0.8496 . ?
O5 H5B 0.8502 . ?

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
C24 Pd2 N1 83.1(3) . . ?
C24 Pd2 N3 96.7(3) . . ?
N1 Pd2 N3 179.46(16) . . ?
C24 Pd2 O2 162.99(17) . . ?
N1 Pd2 O2 79.9(3) . . ?
N3 Pd2 O2 100.3(3) . . ?
C25 Fe1 C20 125.6(3) . . ?
C25 Fe1 C26 39.9(2) . . ?
C20 Fe1 C26 106.7(2) . . ?
C25 Fe1 C28 67.3(3) . . ?
C20 Fe1 C28 153.9(2) . . ?
C26 Fe1 C28 67.6(3) . . ?
C25 Fe1 C21 164.2(2) . . ?
C20 Fe1 C21 41.4(2) . . ?
C26 Fe1 C21 127.4(2) . . ?
C28 Fe1 C21 120.5(3) . . ?
C25 Fe1 C22 153.2(2) . . ?
C20 Fe1 C22 67.9(2) . . ?
C26 Fe1 C22 166.7(2) . . ?
C28 Fe1 C22 111.4(3) . . ?
C21 Fe1 C22 40.6(2) . . ?
C25 Fe1 C23 118.1(3) . . ?
C20 Fe1 C23 68.4(2) . . ?
C26 Fe1 C23 150.8(2) . . ?
C28 Fe1 C23 129.2(3) . . ?
C21 Fe1 C23 69.0(3) . . ?
C22 Fe1 C23 40.3(3) . . ?
C25 Fe1 C27 67.2(3) . . ?
C20 Fe1 C27 119.0(2) . . ?
C26 Fe1 C27 40.3(2) . . ?
C28 Fe1 C27 40.1(2) . . ?
C21 Fe1 C27 109.1(3) . . ?
C22 Fe1 C27 130.5(3) . . ?
C23 Fe1 C27 167.4(2) . . ?
C25 Fe1 C29 40.2(3) . . ?
C20 Fe1 C29 163.2(2) . . ?
C26 Fe1 C29 67.8(3) . . ?
C28 Fe1 C29 40.5(3) . . ?
C21 Fe1 C29 154.4(2) . . ?
C22 Fe1 C29 120.8(3) . . ?
C23 Fe1 C29 108.2(3) . . ?
C27 Fe1 C29 67.8(3) . . ?
C25 Fe1 C24 106.4(3) . . ?
C20 Fe1 C24 40.7(2) . . ?
C26 Fe1 C24 116.9(2) . . ?
C28 Fe1 C24 165.2(2) . . ?
C21 Fe1 C24 69.2(3) . . ?
C22 Fe1 C24 67.7(2) . . ?
C23 Fe1 C24 40.5(2) . . ?
C27 Fe1 C24 151.6(2) . . ?
C29 Fe1 C24 126.2(3) . . ?
N2 O2 Pd2 108.5(3) . . ?
C30 N1 C19 125.4(4) . . ?
C30 N1 Pd2 116.1(4) . . ?
C19 N1 Pd2 118.2(4) . . ?
O2 N2 C34 117.3(5) . . ?
O2 N2 C30 121.7(4) . . ?
C34 N2 C30 121.0(4) . . ?
C35 N3 Pd2 174.9(5) . . ?
O1 C19 N1 126.3(5) . . ?
O1 C19 C20 125.6(5) . . ?
N1 C19 C20 108.1(4) . . ?
C24 C20 C21 109.0(5) . . ?
C24 C20 C19 120.2(4) . . ?
C21 C20 C19 130.7(5) . . ?
C24 C20 Fe1 70.6(3) . . ?
C21 C20 Fe1 69.8(3) . . ?
C19 C20 Fe1 123.2(3) . . ?
C22 C21 C20 105.6(5) . . ?
C22 C21 Fe1 69.7(3) . . ?
C20 C21 Fe1 68.8(3) . . ?
C22 C21 H21 127.2 . . ?
C20 C21 H21 127.2 . . ?
Fe1 C21 H21 125.8 . . ?
C23 C22 C21 110.0(5) . . ?
C23 C22 Fe1 69.9(3) . . ?
C21 C22 Fe1 69.6(3) . . ?
C23 C22 H22 125.0 . . ?
C21 C22 H22 125.0 . . ?
Fe1 C22 H22 127.1 . . ?
C22 C23 C24 107.8(5) . . ?
C22 C23 Fe1 69.9(3) . . ?
C24 C23 Fe1 70.2(3) . . ?
C22 C23 H23 126.1 . . ?
C24 C23 H23 126.1 . . ?
Fe1 C23 H23 125.5 . . ?
C23 C24 C20 107.5(5) . . ?
C23 C24 Pd2 142.1(4) . . ?
C20 C24 Pd2 110.2(4) . . ?
C23 C24 Fe1 69.4(3) . . ?
C20 C24 Fe1 68.7(3) . . ?
Pd2 C24 Fe1 121.8(3) . . ?
C26 C25 C29 109.8(6) . . ?
C26 C25 Fe1 70.6(3) . . ?
C29 C25 Fe1 70.8(4) . . ?
C26 C25 H25 125.1 . . ?
C29 C25 H25 125.1 . . ?
Fe1 C25 H25 125.1 . . ?
C25 C26 C27 107.5(6) . . ?
C25 C26 Fe1 69.5(4) . . ?
C27 C26 Fe1 70.2(3) . . ?
C25 C26 H26 126.2 . . ?
C27 C26 H26 126.2 . . ?
Fe1 C26 H26 125.7 . . ?
C28 C27 C26 107.9(5) . . ?
C28 C27 Fe1 69.7(4) . . ?
C26 C27 Fe1 69.6(4) . . ?
C28 C27 H27 126.1 . . ?
C26 C27 H27 126.1 . . ?
Fe1 C27 H27 126.2 . . ?
C27 C28 C29 108.3(5) . . ?
C27 C28 Fe1 70.2(3) . . ?
C29 C28 Fe1 70.0(3) . . ?
C27 C28 H28 125.8 . . ?
C29 C28 H28 125.8 . . ?
Fe1 C28 H28 125.6 . . ?
C25 C29 C28 106.5(5) . . ?
C25 C29 Fe1 69.0(3) . . ?
C28 C29 Fe1 69.5(3) . . ?
C25 C29 H29 126.8 . . ?
C28 C29 H29 126.8 . . ?
Fe1 C29 H29 126.2 . . ?
N1 C30 N2 113.6(4) . . ?
N1 C30 C31 128.6(5) . . ?
N2 C30 C31 117.7(5) . . ?
C32 C31 C30 121.3(5) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C33 C32 C31 119.5(5) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C34 119.6(5) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
N2 C34 C33 120.9(5) . . ?
N2 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
N3 C35 C36 178.9(7) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C6 Pd3 N4 83.0(2) . . ?
C6 Pd3 N6 97.1(2) . . ?
N4 Pd3 N6 179.87(18) . . ?
C6 Pd3 O4 162.73(19) . . ?
N4 Pd3 O4 79.77(17) . . ?
N6 Pd3 O4 100.16(18) . . ?
C11 Fe2 C5 107.6(3) . . ?
C11 Fe2 C7 40.9(3) . . ?
C5 Fe2 C7 114.4(3) . . ?
C11 Fe2 C9 67.9(4) . . ?
C5 Fe2 C9 172.0(3) . . ?
C7 Fe2 C9 67.0(4) . . ?
C11 Fe2 C10 40.4(3) . . ?
C5 Fe2 C10 132.5(3) . . ?
C7 Fe2 C10 67.4(3) . . ?
C9 Fe2 C10 39.9(3) . . ?
C11 Fe2 C3 146.3(3) . . ?
C5 Fe2 C3 68.3(3) . . ?
C7 Fe2 C3 172.4(3) . . ?
C9 Fe2 C3 111.4(3) . . ?
C10 Fe2 C3 116.6(3) . . ?
C11 Fe2 C8 67.4(3) . . ?
C5 Fe2 C8 146.7(3) . . ?
C7 Fe2 C8 39.7(3) . . ?
C9 Fe2 C8 38.9(3) . . ?
C10 Fe2 C8 66.1(4) . . ?
C3 Fe2 C8 134.5(3) . . ?
C11 Fe2 C4 114.3(3) . . ?
C5 Fe2 C4 40.3(2) . . ?
C7 Fe2 C4 145.8(3) . . ?
C9 Fe2 C4 134.4(3) . . ?
C10 Fe2 C4 110.3(3) . . ?
C3 Fe2 C4 40.6(2) . . ?
C8 Fe2 C4 172.8(3) . . ?
C11 Fe2 C2 171.3(3) . . ?
C5 Fe2 C2 68.4(3) . . ?
C7 Fe2 C2 132.7(3) . . ?
C9 Fe2 C2 117.0(3) . . ?
C10 Fe2 C2 147.8(3) . . ?
C3 Fe2 C2 40.6(2) . . ?
C8 Fe2 C2 111.4(3) . . ?
C4 Fe2 C2 68.1(3) . . ?
C11 Fe2 C6 131.1(3) . . ?
C5 Fe2 C6 41.0(2) . . ?
C7 Fe2 C6 108.1(3) . . ?
C9 Fe2 C6 146.9(3) . . ?
C10 Fe2 C6 170.9(3) . . ?
C3 Fe2 C6 68.9(3) . . ?
C8 Fe2 C6 116.0(3) . . ?
C4 Fe2 C6 68.6(3) . . ?
C2 Fe2 C6 40.9(2) . . ?
N5 O4 Pd3 108.7(3) . . ?
C12 N4 C1 126.3(5) . . ?
C12 N4 Pd3 115.8(3) . . ?
C1 N4 Pd3 117.9(3) . . ?
O4 N5 C12 121.0(4) . . ?
O4 N5 C16 116.4(5) . . ?
C12 N5 C16 122.6(5) . . ?
C17 N6 Pd3 171.4(4) . . ?
O3 C1 N4 126.0(5) . . ?
O3 C1 C2 124.1(5) . . ?
N4 C1 C2 109.9(5) . . ?
C3 C2 C6 108.6(5) . . ?
C3 C2 C1 133.6(5) . . ?
C6 C2 C1 117.8(5) . . ?
C3 C2 Fe2 69.4(3) . . ?
C6 C2 Fe2 70.1(3) . . ?
C1 C2 Fe2 125.4(4) . . ?
C4 C3 C2 108.0(5) . . ?
C4 C3 Fe2 69.9(3) . . ?
C2 C3 Fe2 70.1(3) . . ?
C4 C3 H3 126.0 . . ?
C2 C3 H3 126.0 . . ?
Fe2 C3 H3 125.6 . . ?
C5 C4 C3 108.2(5) . . ?
C5 C4 Fe2 69.3(4) . . ?
C3 C4 Fe2 69.5(3) . . ?
C5 C4 H4 125.9 . . ?
C3 C4 H4 125.9 . . ?
Fe2 C4 H4 126.8 . . ?
C4 C5 C6 109.1(5) . . ?
C4 C5 Fe2 70.3(3) . . ?
C6 C5 Fe2 70.6(3) . . ?
C4 C5 H5 125.4 . . ?
C6 C5 H5 125.4 . . ?
Fe2 C5 H5 125.2 . . ?
C5 C6 C2 106.0(5) . . ?
C5 C6 Pd3 142.5(4) . . ?
C2 C6 Pd3 111.4(4) . . ?
C5 C6 Fe2 68.4(3) . . ?
C2 C6 Fe2 69.0(3) . . ?
Pd3 C6 Fe2 123.3(3) . . ?
C8 C7 C11 107.3(7) . . ?
C8 C7 Fe2 70.4(4) . . ?
C11 C7 Fe2 69.4(4) . . ?
C8 C7 H7 126.4 . . ?
C11 C7 H7 126.4 . . ?
Fe2 C7 H7 125.4 . . ?
C9 C8 C7 110.0(7) . . ?
C9 C8 Fe2 70.4(5) . . ?
C7 C8 Fe2 69.9(4) . . ?
C9 C8 H8 125.0 . . ?
C7 C8 H8 125.0 . . ?
Fe2 C8 H8 126.3 . . ?
C8 C9 C10 107.8(8) . . ?
C8 C9 Fe2 70.6(4) . . ?
C10 C9 Fe2 70.0(4) . . ?
C8 C9 H9 126.1 . . ?
C10 C9 H9 126.1 . . ?
Fe2 C9 H9 124.9 . . ?
C9 C10 C11 108.6(7) . . ?
C9 C10 Fe2 70.0(4) . . ?
C11 C10 Fe2 69.5(4) . . ?
C9 C10 H10 125.7 . . ?
C11 C10 H10 125.7 . . ?
Fe2 C10 H10 126.4 . . ?
C10 C11 C7 106.2(7) . . ?
C10 C11 Fe2 70.1(4) . . ?
C7 C11 Fe2 69.7(4) . . ?
C10 C11 H11 126.9 . . ?
C7 C11 H11 126.9 . . ?
Fe2 C11 H11 125.0 . . ?
N5 C12 N4 114.6(5) . . ?
N5 C12 C13 117.2(5) . . ?
N4 C12 C13 128.2(5) . . ?
C14 C13 C12 120.7(6) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 120.2(7) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 119.3(6) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 N5 119.9(6) . . ?
C15 C16 H16 120.1 . . ?
N5 C16 H16 120.1 . . ?
N6 C17 C18 178.8(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
H5A O5 H5B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd2 O2 N2 C34 176.1(4) . . . . ?
Pd2 O2 N2 C30 -4.2(5) . . . . ?
C30 N1 C19 O1 2.8(8) . . . . ?
Pd2 N1 C19 O1 175.6(4) . . . . ?
C30 N1 C19 C20 -177.4(4) . . . . ?
Pd2 N1 C19 C20 -4.6(5) . . . . ?
O1 C19 C20 C24 -177.0(5) . . . . ?
N1 C19 C20 C24 3.3(6) . . . . ?
O1 C19 C20 C21 6.4(8) . . . . ?
N1 C19 C20 C21 -173.3(5) . . . . ?
O1 C19 C20 Fe1 97.5(6) . . . . ?
N1 C19 C20 Fe1 -82.3(5) . . . . ?
C24 C20 C21 C22 0.4(6) . . . . ?
C19 C20 C21 C22 177.3(5) . . . . ?
Fe1 C20 C21 C22 60.4(4) . . . . ?
C24 C20 C21 Fe1 -60.0(3) . . . . ?
C19 C20 C21 Fe1 116.9(5) . . . . ?
C20 C21 C22 C23 -1.5(6) . . . . ?
Fe1 C21 C22 C23 58.3(4) . . . . ?
C20 C21 C22 Fe1 -59.8(4) . . . . ?
C21 C22 C23 C24 2.0(6) . . . . ?
Fe1 C22 C23 C24 60.2(4) . . . . ?
C21 C22 C23 Fe1 -58.1(4) . . . . ?
C22 C23 C24 C20 -1.7(6) . . . . ?
Fe1 C23 C24 C20 58.3(3) . . . . ?
C22 C23 C24 Pd2 -175.6(5) . . . . ?
Fe1 C23 C24 Pd2 -115.6(6) . . . . ?
C22 C23 C24 Fe1 -60.0(4) . . . . ?
C21 C20 C24 C23 0.8(6) . . . . ?
C19 C20 C24 C23 -176.5(4) . . . . ?
Fe1 C20 C24 C23 -58.7(4) . . . . ?
C21 C20 C24 Pd2 176.8(3) . . . . ?
C19 C20 C24 Pd2 -0.4(5) . . . . ?
Fe1 C20 C24 Pd2 117.3(3) . . . . ?
C21 C20 C24 Fe1 59.5(4) . . . . ?
C19 C20 C24 Fe1 -117.8(4) . . . . ?
C29 C25 C26 C27 0.0(6) . . . . ?
Fe1 C25 C26 C27 -60.1(4) . . . . ?
C29 C25 C26 Fe1 60.2(4) . . . . ?
C25 C26 C27 C28 0.3(6) . . . . ?
Fe1 C26 C27 C28 -59.4(4) . . . . ?
C25 C26 C27 Fe1 59.7(4) . . . . ?
C26 C27 C28 C29 -0.5(6) . . . . ?
Fe1 C27 C28 C29 -59.8(4) . . . . ?
C26 C27 C28 Fe1 59.3(4) . . . . ?
C26 C25 C29 C28 -0.3(7) . . . . ?
Fe1 C25 C29 C28 59.7(4) . . . . ?
C26 C25 C29 Fe1 -60.1(4) . . . . ?
C27 C28 C29 C25 0.5(7) . . . . ?
Fe1 C28 C29 C25 -59.4(4) . . . . ?
C27 C28 C29 Fe1 59.9(4) . . . . ?
C19 N1 C30 N2 175.7(4) . . . . ?
Pd2 N1 C30 N2 2.7(5) . . . . ?
C19 N1 C30 C31 -4.6(8) . . . . ?
Pd2 N1 C30 C31 -177.5(4) . . . . ?
O2 N2 C30 N1 1.3(6) . . . . ?
C34 N2 C30 N1 -179.1(4) . . . . ?
O2 N2 C30 C31 -178.5(4) . . . . ?
C34 N2 C30 C31 1.1(7) . . . . ?
N1 C30 C31 C32 -179.4(5) . . . . ?
N2 C30 C31 C32 0.3(8) . . . . ?
C30 C31 C32 C33 -0.8(9) . . . . ?
C31 C32 C33 C34 -0.2(9) . . . . ?
O2 N2 C34 C33 177.5(5) . . . . ?
C30 N2 C34 C33 -2.2(8) . . . . ?
C32 C33 C34 N2 1.7(9) . . . . ?
Pd3 O4 N5 C12 0.2(5) . . . . ?
Pd3 O4 N5 C16 179.8(4) . . . . ?
C12 N4 C1 O3 0.5(8) . . . . ?
Pd3 N4 C1 O3 177.4(4) . . . . ?
C12 N4 C1 C2 -178.5(4) . . . . ?
Pd3 N4 C1 C2 -1.5(5) . . . . ?
O3 C1 C2 C3 4.2(9) . . . . ?
N4 C1 C2 C3 -176.9(5) . . . . ?
O3 C1 C2 C6 -176.9(5) . . . . ?
N4 C1 C2 C6 2.1(6) . . . . ?
O3 C1 C2 Fe2 98.7(6) . . . . ?
N4 C1 C2 Fe2 -82.3(5) . . . . ?
C6 C2 C3 C4 0.7(6) . . . . ?
C1 C2 C3 C4 179.7(5) . . . . ?
Fe2 C2 C3 C4 59.9(4) . . . . ?
C6 C2 C3 Fe2 -59.2(4) . . . . ?
C1 C2 C3 Fe2 119.8(6) . . . . ?
C2 C3 C4 C5 -1.3(7) . . . . ?
Fe2 C3 C4 C5 58.7(4) . . . . ?
C2 C3 C4 Fe2 -60.0(4) . . . . ?
C3 C4 C5 C6 1.4(7) . . . . ?
Fe2 C4 C5 C6 60.2(4) . . . . ?
C3 C4 C5 Fe2 -58.8(4) . . . . ?
C4 C5 C6 C2 -1.0(6) . . . . ?
Fe2 C5 C6 C2 59.0(4) . . . . ?
C4 C5 C6 Pd3 -176.9(5) . . . . ?
Fe2 C5 C6 Pd3 -116.9(6) . . . . ?
C4 C5 C6 Fe2 -60.0(4) . . . . ?
C3 C2 C6 C5 0.2(6) . . . . ?
C1 C2 C6 C5 -179.0(4) . . . . ?
Fe2 C2 C6 C5 -58.6(4) . . . . ?
C3 C2 C6 Pd3 177.5(3) . . . . ?
C1 C2 C6 Pd3 -1.7(6) . . . . ?
Fe2 C2 C6 Pd3 118.7(3) . . . . ?
C3 C2 C6 Fe2 58.8(4) . . . . ?
C1 C2 C6 Fe2 -120.4(4) . . . . ?
C11 C7 C8 C9 0.7(8) . . . . ?
Fe2 C7 C8 C9 -59.2(6) . . . . ?
C11 C7 C8 Fe2 59.9(5) . . . . ?
C7 C8 C9 C10 -1.6(9) . . . . ?
Fe2 C8 C9 C10 -60.4(5) . . . . ?
C7 C8 C9 Fe2 58.8(5) . . . . ?
C8 C9 C10 C11 1.9(8) . . . . ?
Fe2 C9 C10 C11 -59.0(5) . . . . ?
C8 C9 C10 Fe2 60.8(5) . . . . ?
C9 C10 C11 C7 -1.4(8) . . . . ?
Fe2 C10 C11 C7 -60.7(5) . . . . ?
C9 C10 C11 Fe2 59.3(5) . . . . ?
C8 C7 C11 C10 0.4(8) . . . . ?
Fe2 C7 C11 C10 60.9(5) . . . . ?
C8 C7 C11 Fe2 -60.5(5) . . . . ?
O4 N5 C12 N4 -2.9(7) . . . . ?
C16 N5 C12 N4 177.6(5) . . . . ?
O4 N5 C12 C13 176.7(5) . . . . ?
C16 N5 C12 C13 -2.9(7) . . . . ?
C1 N4 C12 N5 -178.7(4) . . . . ?
Pd3 N4 C12 N5 4.2(5) . . . . ?
C1 N4 C12 C13 1.7(8) . . . . ?
Pd3 N4 C12 C13 -175.3(4) . . . . ?
N5 C12 C13 C14 2.7(8) . . . . ?
N4 C12 C13 C14 -177.8(5) . . . . ?
C12 C13 C14 C15 -0.1(10) . . . . ?
C13 C14 C15 C16 -2.5(10) . . . . ?
C14 C15 C16 N5 2.3(10) . . . . ?
O4 N5 C16 C15 -179.2(5) . . . . ?
C12 N5 C16 C15 0.4(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665
C31 H31 O1 0.93 2.38 2.961(9) 120.8 .
C31 H31 O3 0.93 2.61 3.282(9) 129.7 1_656
C34 H34 O4 0.93 2.65 3.272(9) 124.8 2_676
C13 H13 O3 0.93 2.40 2.980(11) 120.2 .
C15 H15 O5 0.93 2.58 3.446(13) 154.3 2_565
C18 H18A O1 0.96 2.59 3.489(12) 155.2 2_666
O5 H5A O4 0.85 2.25 2.951(8) 139.6 1_655
O5 H5B O3 0.85 2.16 2.974(8) 159.3 2_665

_refine_diff_density_max         1.113
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.161

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1523203'
_audit_update_record             
;
2017-10-13 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H17 Fe N O S'
_chemical_formula_sum            'C18 H17 Fe N O S'
_chemical_formula_weight         351.23

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   9.91(3)
_cell_length_b                   12.38(3)
_cell_length_c                   14.01(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1719(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2826
_cell_measurement_theta_min      3.379
_cell_measurement_theta_max      24.455

_exptl_crystal_description       block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.176
_exptl_absorpt_coefficient_mu    0.999
_shelx_estimated_absorpt_T_min   0.716
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3606
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.195
_diffrn_reflns_theta_max         28.121
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.776
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.776
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.780
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             2951
_reflns_number_gt                2196
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_max     0.787
_reflns_Friedel_fraction_full    0.867

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

_computing_data_collection       'Bruker SMART APEX-II'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material  SHELXTL
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0248P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.25(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2951
_refine_ls_number_parameters     205
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0687
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_restrained_S_all      0.864
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe 0.38898(8) 0.05938(5) 0.65238(4) 0.0406(2) Uani 1 1 d . . . . .
S1 S 0.38152(18) 0.53912(9) 0.50440(8) 0.0622(4) Uani 1 1 d . . . . .
O1 O 0.2066(4) 0.3049(2) 0.5327(2) 0.0525(10) Uani 1 1 d . . . . .
N1 N 0.4266(5) 0.2997(3) 0.4794(3) 0.0434(12) Uani 1 1 d D . . . .
C12 C 0.4008(6) 0.3575(4) 0.3901(3) 0.0393(11) Uani 1 1 d . . . . .
C1 C 0.3259(6) 0.2795(3) 0.5462(3) 0.0401(13) Uani 1 1 d . . . . .
C13 C 0.4047(6) 0.3019(4) 0.3023(3) 0.0494(14) Uani 1 1 d . . . . .
H13 H 0.4188 0.2276 0.3022 0.059 Uiso 1 1 calc R U . . .
C2 C 0.3738(6) 0.2253(3) 0.6375(3) 0.0405(12) Uani 1 1 d . . . . .
C4 C 0.3618(6) 0.1345(4) 0.7840(3) 0.0502(16) Uani 1 1 d . . . . .
H4 H 0.3262 0.1002 0.8418 0.060 Uiso 1 1 calc R U . . .
C17 C 0.3786(5) 0.4719(3) 0.3905(3) 0.0385(12) Uani 1 1 d . . . . .
C6 C 0.5093(5) 0.1950(3) 0.6665(3) 0.0418(13) Uani 1 1 d . . . . .
H6 H 0.5923 0.2096 0.6308 0.050 Uiso 1 1 calc R U . . .
C16 C 0.3588(6) 0.5258(4) 0.3030(3) 0.0540(16) Uani 1 1 d . . . . .
H16 H 0.3417 0.5996 0.3029 0.065 Uiso 1 1 calc R U . . .
C3 C 0.2825(6) 0.1880(4) 0.7113(3) 0.0491(15) Uani 1 1 d . . . . .
H3 H 0.1842 0.1965 0.7114 0.059 Uiso 1 1 calc R U . . .
C15 C 0.3645(6) 0.4694(5) 0.2161(3) 0.0631(17) Uani 1 1 d . . . . .
H15 H 0.3530 0.5065 0.1589 0.076 Uiso 1 1 calc R U . . .
C14 C 0.3879(7) 0.3560(5) 0.2151(3) 0.0635(15) Uani 1 1 d . . . . .
H14 H 0.3919 0.3184 0.1577 0.076 Uiso 1 1 calc R U . . .
C5 C 0.5009(6) 0.1398(4) 0.7569(3) 0.0483(14) Uani 1 1 d . . . . .
H5 H 0.5769 0.1097 0.7928 0.058 Uiso 1 1 calc R U . . .
C8 C 0.4748(8) -0.0915(4) 0.6382(5) 0.0735(19) Uani 1 1 d . . . . .
H8 H 0.5524 -0.1185 0.6745 0.088 Uiso 1 1 calc R U . . .
C7 C 0.3401(9) -0.1028(4) 0.6644(6) 0.083(2) Uani 1 1 d . . . . .
H7 H 0.3066 -0.1389 0.7219 0.099 Uiso 1 1 calc R U . . .
C9 C 0.4813(10) -0.0375(5) 0.5512(5) 0.089(2) Uani 1 1 d . . . . .
H9 H 0.5645 -0.0197 0.5168 0.107 Uiso 1 1 calc R U . . .
C10 C 0.3500(12) -0.0100(5) 0.5217(5) 0.110(4) Uani 1 1 d . . . . .
H10 H 0.3248 0.0276 0.4628 0.132 Uiso 1 1 calc R U . . .
C11 C 0.2597(7) -0.0517(6) 0.5933(6) 0.099(3) Uani 1 1 d . . . . .
H11 H 0.1610 -0.0474 0.5925 0.119 Uiso 1 1 calc R U . . .
C18 C 0.3693(9) 0.6806(4) 0.4735(4) 0.101(2) Uani 1 1 d . . . . .
H18A H 0.4292 0.6960 0.4215 0.151 Uiso 1 1 calc R U . . .
H18B H 0.3937 0.7238 0.5277 0.151 Uiso 1 1 calc R U . . .
H18C H 0.2783 0.6970 0.4549 0.151 Uiso 1 1 calc R U . . .
H1 H 0.504(3) 0.274(4) 0.483(3) 0.050(17) Uiso 1 1 d 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
Fe01 C11 2.053(7) . ?
Fe01 C10 2.059(8) . ?
Fe01 C8 2.062(7) . ?
Fe01 C6 2.068(6) . ?
Fe01 C2 2.069(7) . ?
Fe01 C9 2.070(7) . ?
Fe01 C7 2.071(7) . ?
Fe01 C3 2.080(6) . ?
Fe01 C4 2.083(6) . ?
Fe01 C5 2.089(6) . ?
S1 C17 1.801(6) . ?
S1 C18 1.808(7) . ?
O1 C1 1.238(6) . ?
N1 C1 1.391(7) . ?
N1 C12 1.464(6) . ?
N1 H1 0.83(2) . ?
C12 C13 1.410(6) . ?
C12 C17 1.433(7) . ?
C1 C2 1.521(7) . ?
C13 C14 1.404(7) . ?
C13 H13 0.9300 . ?
C2 C3 1.449(7) . ?
C2 C6 1.452(7) . ?
C4 C5 1.431(8) . ?
C4 C3 1.447(7) . ?
C4 H4 0.9800 . ?
C17 C16 1.409(6) . ?
C6 C5 1.442(7) . ?
C6 H6 0.9800 . ?
C16 C15 1.405(7) . ?
C16 H16 0.9300 . ?
C3 H3 0.9800 . ?
C15 C14 1.423(8) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C5 H5 0.9800 . ?
C8 C9 1.392(9) . ?
C8 C7 1.391(9) . ?
C8 H8 0.9800 . ?
C7 C11 1.423(9) . ?
C7 H7 0.9800 . ?
C9 C10 1.407(11) . ?
C9 H9 0.9800 . ?
C10 C11 1.440(10) . ?
C10 H10 0.9800 . ?
C11 H11 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 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
C11 Fe01 C10 41.0(3) . . ?
C11 Fe01 C8 67.2(3) . . ?
C10 Fe01 C8 67.3(3) . . ?
C11 Fe01 C6 160.3(3) . . ?
C10 Fe01 C6 122.1(3) . . ?
C8 Fe01 C6 120.4(3) . . ?
C11 Fe01 C2 125.4(3) . . ?
C10 Fe01 C2 108.1(3) . . ?
C8 Fe01 C2 156.8(3) . . ?
C6 Fe01 C2 41.1(2) . . ?
C11 Fe01 C9 67.2(4) . . ?
C10 Fe01 C9 39.8(3) . . ?
C8 Fe01 C9 39.4(2) . . ?
C6 Fe01 C9 106.3(3) . . ?
C2 Fe01 C9 122.5(3) . . ?
C11 Fe01 C7 40.4(3) . . ?
C10 Fe01 C7 67.9(3) . . ?
C8 Fe01 C7 39.3(3) . . ?
C6 Fe01 C7 156.0(3) . . ?
C2 Fe01 C7 162.3(3) . . ?
C9 Fe01 C7 66.3(3) . . ?
C11 Fe01 C3 110.9(3) . . ?
C10 Fe01 C3 125.2(3) . . ?
C8 Fe01 C3 160.1(2) . . ?
C6 Fe01 C3 68.5(3) . . ?
C2 Fe01 C3 40.9(2) . . ?
C9 Fe01 C3 159.9(3) . . ?
C7 Fe01 C3 126.2(3) . . ?
C11 Fe01 C4 125.1(3) . . ?
C10 Fe01 C4 161.7(4) . . ?
C8 Fe01 C4 122.9(3) . . ?
C6 Fe01 C4 68.2(2) . . ?
C2 Fe01 C4 68.7(2) . . ?
C9 Fe01 C4 157.3(3) . . ?
C7 Fe01 C4 109.3(3) . . ?
C3 Fe01 C4 40.67(18) . . ?
C11 Fe01 C5 158.8(3) . . ?
C10 Fe01 C5 157.2(4) . . ?
C8 Fe01 C5 106.3(3) . . ?
C6 Fe01 C5 40.58(18) . . ?
C2 Fe01 C5 68.7(2) . . ?
C9 Fe01 C5 121.4(4) . . ?
C7 Fe01 C5 121.9(3) . . ?
C3 Fe01 C5 68.1(3) . . ?
C4 Fe01 C5 40.1(2) . . ?
C17 S1 C18 103.5(3) . . ?
C1 N1 C12 122.5(4) . . ?
C1 N1 H1 124(3) . . ?
C12 N1 H1 113(3) . . ?
C13 C12 C17 119.4(4) . . ?
C13 C12 N1 120.1(4) . . ?
C17 C12 N1 120.4(4) . . ?
O1 C1 N1 122.5(5) . . ?
O1 C1 C2 122.6(5) . . ?
N1 C1 C2 114.9(5) . . ?
C14 C13 C12 121.5(5) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C3 C2 C6 107.2(4) . . ?
C3 C2 C1 123.1(5) . . ?
C6 C2 C1 129.6(5) . . ?
C3 C2 Fe01 70.0(2) . . ?
C6 C2 Fe01 69.4(2) . . ?
C1 C2 Fe01 123.1(3) . . ?
C5 C4 C3 108.3(5) . . ?
C5 C4 Fe01 70.2(3) . . ?
C3 C4 Fe01 69.5(3) . . ?
C5 C4 H4 125.8 . . ?
C3 C4 H4 125.8 . . ?
Fe01 C4 H4 125.8 . . ?
C16 C17 C12 119.1(4) . . ?
C16 C17 S1 123.7(4) . . ?
C12 C17 S1 117.2(3) . . ?
C5 C6 C2 108.3(4) . . ?
C5 C6 Fe01 70.5(3) . . ?
C2 C6 Fe01 69.5(3) . . ?
C5 C6 H6 125.8 . . ?
C2 C6 H6 125.8 . . ?
Fe01 C6 H6 125.8 . . ?
C15 C16 C17 120.9(5) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C4 C3 C2 108.0(6) . . ?
C4 C3 Fe01 69.8(3) . . ?
C2 C3 Fe01 69.2(3) . . ?
C4 C3 H3 126.0 . . ?
C2 C3 H3 126.0 . . ?
Fe01 C3 H3 126.0 . . ?
C16 C15 C14 120.3(5) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C13 C14 C15 118.8(5) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C4 C5 C6 108.1(4) . . ?
C4 C5 Fe01 69.7(3) . . ?
C6 C5 Fe01 68.9(3) . . ?
C4 C5 H5 125.9 . . ?
C6 C5 H5 125.9 . . ?
Fe01 C5 H5 125.9 . . ?
C9 C8 C7 108.9(7) . . ?
C9 C8 Fe01 70.6(4) . . ?
C7 C8 Fe01 70.7(3) . . ?
C9 C8 H8 125.6 . . ?
C7 C8 H8 125.6 . . ?
Fe01 C8 H8 125.6 . . ?
C8 C7 C11 108.0(8) . . ?
C8 C7 Fe01 70.0(3) . . ?
C11 C7 Fe01 69.1(3) . . ?
C8 C7 H7 126.0 . . ?
C11 C7 H7 126.0 . . ?
Fe01 C7 H7 126.0 . . ?
C8 C9 C10 109.3(7) . . ?
C8 C9 Fe01 70.0(4) . . ?
C10 C9 Fe01 69.7(4) . . ?
C8 C9 H9 125.3 . . ?
C10 C9 H9 125.3 . . ?
Fe01 C9 H9 125.3 . . ?
C9 C10 C11 106.4(7) . . ?
C9 C10 Fe01 70.5(4) . . ?
C11 C10 Fe01 69.3(4) . . ?
C9 C10 H10 126.8 . . ?
C11 C10 H10 126.8 . . ?
Fe01 C10 H10 126.8 . . ?
C7 C11 C10 107.4(8) . . ?
C7 C11 Fe01 70.5(4) . . ?
C10 C11 Fe01 69.7(4) . . ?
C7 C11 H11 126.3 . . ?
C10 C11 H11 126.3 . . ?
Fe01 C11 H11 126.3 . . ?
S1 C18 H18A 109.5 . . ?
S1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_refine_diff_density_max         0.372
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.047

