# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_pbad150616
_database_code_depnum_ccdc_archive 'CCDC 1469264'
_audit_update_record             
;
2016-03-17 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H54 Fe N3 Si2'
_chemical_formula_sum            'C33 H54 Fe N3 Si2'
_chemical_formula_weight         604.82

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'
Si Si 0.0817 0.0704 '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'

_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                   12.844(3)
_cell_length_b                   13.622(3)
_cell_length_c                   22.059(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.821(11)
_cell_angle_gamma                90
_cell_volume                     3653.4(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9968
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      27.99

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.502
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5913
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34373
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.495
_diffrn_reflns_theta_max         28.204
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8950
_reflns_number_gt                6788
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component 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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8950
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.1115
_refine_ls_wR_factor_ref         0.3378
_refine_ls_wR_factor_gt          0.3021
_refine_ls_goodness_of_fit_ref   1.342
_refine_ls_restrained_S_all      1.342
_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
C1 C 0.7071(5) 0.7533(4) 0.1541(3) 0.0188(10) Uani 1 1 d . . . . .
C2 C 0.6924(6) 0.7173(6) 0.0511(3) 0.0320(15) Uani 1 1 d . . . . .
H2 H 0.7065 0.6884 0.0153 0.038 Uiso 1 1 calc R U . . .
C3 C 0.6172(6) 0.7860(6) 0.0491(3) 0.0329(15) Uani 1 1 d . . . . .
H3 H 0.5668 0.8144 0.0118 0.040 Uiso 1 1 calc R U . . .
C4 C 0.8284(4) 0.6217(4) 0.1356(3) 0.0191(11) Uani 1 1 d . . . . .
C5 C 0.7937(5) 0.5243(5) 0.1357(3) 0.0265(13) Uani 1 1 d . . . . .
C6 C 0.8755(6) 0.4524(5) 0.1527(3) 0.0320(15) Uani 1 1 d . . . . .
H6 H 0.8550 0.3857 0.1543 0.038 Uiso 1 1 calc R U . . .
C7 C 0.9850(6) 0.4755(5) 0.1671(4) 0.0352(16) Uani 1 1 d . . . . .
H7 H 1.0392 0.4254 0.1779 0.042 Uiso 1 1 calc R U . . .
C8 C 1.0149(5) 0.5717(5) 0.1656(3) 0.0296(14) Uani 1 1 d . . . . .
H8 H 1.0907 0.5874 0.1760 0.036 Uiso 1 1 calc R U . . .
C9 C 0.9383(5) 0.6472(4) 0.1495(3) 0.0220(12) Uani 1 1 d . . . . .
C10 C 0.6728(6) 0.4969(5) 0.1200(4) 0.0370(16) Uani 1 1 d . . . . .
H10 H 0.6292 0.5585 0.1060 0.044 Uiso 1 1 calc R U . . .
C11 C 0.6378(8) 0.4256(9) 0.0632(5) 0.067(3) Uani 1 1 d . . . . .
H11A H 0.6683 0.3604 0.0773 0.101 Uiso 1 1 calc R U . . .
H11B H 0.6653 0.4492 0.0292 0.101 Uiso 1 1 calc R U . . .
H11C H 0.5573 0.4216 0.0468 0.101 Uiso 1 1 calc R U . . .
C12 C 0.6461(9) 0.4586(12) 0.1779(5) 0.085(4) Uani 1 1 d . . . . .
H12A H 0.6713 0.3905 0.1862 0.128 Uiso 1 1 calc R U . . .
H12B H 0.5665 0.4613 0.1695 0.128 Uiso 1 1 calc R U . . .
H12C H 0.6833 0.4992 0.2153 0.128 Uiso 1 1 calc R U . . .
C13 C 0.9776(6) 0.7540(5) 0.1490(3) 0.0292(13) Uani 1 1 d . . . . .
H13 H 0.9114 0.7967 0.1314 0.035 Uiso 1 1 calc R U . . .
C14 C 1.0399(10) 0.7886(7) 0.2165(4) 0.057(3) Uani 1 1 d . . . . .
H14A H 1.0069 0.7596 0.2467 0.086 Uiso 1 1 calc R U . . .
H14B H 1.0360 0.8603 0.2184 0.086 Uiso 1 1 calc R U . . .
H14C H 1.1170 0.7683 0.2279 0.086 Uiso 1 1 calc R U . . .
C15 C 1.0496(8) 0.7648(6) 0.1060(4) 0.050(2) Uani 1 1 d . . . . .
H15A H 1.1187 0.7290 0.1249 0.075 Uiso 1 1 calc R U . . .
H15B H 1.0656 0.8344 0.1021 0.075 Uiso 1 1 calc R U . . .
H15C H 1.0107 0.7379 0.0635 0.075 Uiso 1 1 calc R U . . .
C16 C 0.5646(4) 0.8832(4) 0.1303(3) 0.0190(11) Uani 1 1 d . . . . .
C17 C 0.5971(5) 0.9822(5) 0.1282(3) 0.0257(13) Uani 1 1 d . . . . .
C18 C 0.5328(6) 1.0523(5) 0.1439(3) 0.0316(15) Uani 1 1 d . . . . .
H18 H 0.5535 1.1193 0.1440 0.038 Uiso 1 1 calc R U . . .
C19 C 0.4404(6) 1.0300(5) 0.1594(4) 0.0300(15) Uani 1 1 d . . . . .
H19 H 0.3974 1.0808 0.1688 0.036 Uiso 1 1 calc R U . . .
C20 C 0.4104(5) 0.9326(4) 0.1612(3) 0.0291(14) Uani 1 1 d . . . . .
H20 H 0.3473 0.9172 0.1729 0.035 Uiso 1 1 calc R U . . .
C21 C 0.4706(5) 0.8568(5) 0.1462(3) 0.0233(12) Uani 1 1 d . . . . .
C22 C 0.6983(6) 1.0088(6) 0.1122(4) 0.0353(16) Uani 1 1 d . . . . .
H22 H 0.7332 0.9465 0.1045 0.042 Uiso 1 1 calc R U . . .
C23 C 0.7820(8) 1.0638(9) 0.1651(5) 0.066(2) Uani 1 1 d . . . . .
H23A H 0.7505 1.1264 0.1726 0.099 Uiso 1 1 calc R U . . .
H23B H 0.8474 1.0764 0.1527 0.099 Uiso 1 1 calc R U . . .
H23C H 0.8025 1.0244 0.2044 0.099 Uiso 1 1 calc R U . . .
C24 C 0.6697(8) 1.0717(9) 0.0498(5) 0.066(2) Uani 1 1 d . . . . .
H24A H 0.6638 1.1410 0.0604 0.099 Uiso 1 1 calc R U . . .
H24B H 0.5995 1.0496 0.0196 0.099 Uiso 1 1 calc R U . . .
H24C H 0.7279 1.0641 0.0303 0.099 Uiso 1 1 calc R U . . .
C25 C 0.4361(6) 0.7511(5) 0.1467(4) 0.0333(15) Uani 1 1 d . . . . .
H25 H 0.5004 0.7084 0.1486 0.040 Uiso 1 1 calc R U . . .
C26 C 0.3422(11) 0.7274(7) 0.0847(4) 0.066(3) Uani 1 1 d . . . . .
H26A H 0.2812 0.7731 0.0800 0.099 Uiso 1 1 calc R U . . .
H26B H 0.3168 0.6600 0.0867 0.099 Uiso 1 1 calc R U . . .
H26C H 0.3688 0.7340 0.0480 0.099 Uiso 1 1 calc R U . . .
C27 C 0.3990(9) 0.7271(6) 0.2040(4) 0.052(2) Uani 1 1 d . . . . .
H27A H 0.4549 0.7494 0.2434 0.078 Uiso 1 1 calc R U . . .
H27B H 0.3890 0.6560 0.2062 0.078 Uiso 1 1 calc R U . . .
H27C H 0.3292 0.7604 0.1993 0.078 Uiso 1 1 calc R U . . .
C28 C 1.0354(6) 0.7187(6) 0.4196(4) 0.0397(17) Uani 1 1 d . . . . .
H28A H 1.0652 0.7369 0.3855 0.060 Uiso 1 1 calc R U . . .
H28B H 1.0823 0.6683 0.4468 0.060 Uiso 1 1 calc R U . . .
H28C H 1.0334 0.7766 0.4455 0.060 Uiso 1 1 calc R U . . .
C29 C 0.9058(7) 0.5632(5) 0.3328(4) 0.0421(19) Uani 1 1 d . . . . .
H29A H 0.8345 0.5302 0.3155 0.063 Uiso 1 1 calc R U . . .
H29B H 0.9603 0.5168 0.3589 0.063 Uiso 1 1 calc R U . . .
H29C H 0.9297 0.5868 0.2974 0.063 Uiso 1 1 calc R U . . .
C30 C 0.8514(6) 0.6163(6) 0.4509(4) 0.0398(18) Uani 1 1 d . . . . .
H30A H 0.8540 0.6679 0.4823 0.060 Uiso 1 1 calc R U . . .
H30B H 0.9023 0.5634 0.4715 0.060 Uiso 1 1 calc R U . . .
H30C H 0.7765 0.5901 0.4341 0.060 Uiso 1 1 calc R U . . .
C31 C 0.6158(5) 0.7932(5) 0.3900(3) 0.0296(13) Uani 1 1 d . . . . .
H31A H 0.5556 0.7829 0.3498 0.044 Uiso 1 1 calc R U . . .
H31B H 0.5925 0.8397 0.4169 0.044 Uiso 1 1 calc R U . . .
H31C H 0.6354 0.7305 0.4126 0.044 Uiso 1 1 calc R U . . .
C32 C 0.8348(6) 0.9006(5) 0.4462(3) 0.0313(15) Uani 1 1 d . . . . .
H32A H 0.8656 0.8493 0.4781 0.047 Uiso 1 1 calc R U . . .
H32B H 0.7944 0.9481 0.4635 0.047 Uiso 1 1 calc R U . . .
H32C H 0.8945 0.9342 0.4360 0.047 Uiso 1 1 calc R U . . .
C33 C 0.6853(7) 0.9481(5) 0.3171(3) 0.0353(16) Uani 1 1 d . . . . .
H33A H 0.7447 0.9764 0.3039 0.053 Uiso 1 1 calc R U . . .
H33B H 0.6561 0.9983 0.3392 0.053 Uiso 1 1 calc R U . . .
H33C H 0.6264 0.9251 0.2793 0.053 Uiso 1 1 calc R U . . .
N1 N 0.7460(4) 0.6961(4) 0.1151(2) 0.0190(10) Uani 1 1 d . . . . .
N2 N 0.6267(4) 0.8079(4) 0.1119(2) 0.0228(10) Uani 1 1 d . . . . .
N3 N 0.8015(4) 0.7557(3) 0.3406(2) 0.0195(9) Uani 1 1 d . . . . .
Si1 Si 0.89259(14) 0.66912(12) 0.38325(8) 0.0233(4) Uani 1 1 d . . . . .
Si2 Si 0.73903(14) 0.84389(11) 0.37183(8) 0.0200(4) Uani 1 1 d . . . . .
Fe1 Fe 0.75649(7) 0.75243(7) 0.25052(4) 0.0226(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.366(7) . ?
C1 N1 1.368(7) . ?
C1 Fe1 2.015(6) . ?
C2 C3 1.336(10) . ?
C2 N1 1.388(8) . ?
C2 H2 0.9500 . ?
C3 N2 1.383(8) . ?
C3 H3 0.9500 . ?
C4 C9 1.389(8) . ?
C4 C5 1.399(9) . ?
C4 N1 1.429(7) . ?
C5 C6 1.397(9) . ?
C5 C10 1.525(9) . ?
C6 C7 1.374(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.369(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(8) . ?
C8 H8 0.9500 . ?
C9 C13 1.542(9) . ?
C10 C12 1.518(13) . ?
C10 C11 1.533(11) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.520(11) . ?
C13 C15 1.530(11) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.408(8) . ?
C16 C17 1.417(8) . ?
C16 N2 1.436(7) . ?
C17 C18 1.377(10) . ?
C17 C22 1.497(9) . ?
C18 C19 1.371(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(9) . ?
C20 H20 0.9500 . ?
C21 C25 1.508(9) . ?
C22 C23 1.506(12) . ?
C22 C24 1.561(12) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.525(11) . ?
C25 C26 1.537(12) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 Si1 1.875(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 Si1 1.863(7) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 Si1 1.879(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 Si2 1.884(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 Si2 1.871(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 Si2 1.847(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N3 Si2 1.708(5) . ?
N3 Si1 1.714(5) . ?
N3 Fe1 1.882(5) . ?

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
N2 C1 N1 103.4(5) . . ?
N2 C1 Fe1 129.3(4) . . ?
N1 C1 Fe1 127.3(4) . . ?
C3 C2 N1 107.1(6) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 106.8(6) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
C9 C4 C5 122.5(5) . . ?
C9 C4 N1 119.3(5) . . ?
C5 C4 N1 118.0(5) . . ?
C6 C5 C4 117.0(6) . . ?
C6 C5 C10 120.8(6) . . ?
C4 C5 C10 122.2(6) . . ?
C7 C6 C5 121.7(6) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C8 C7 C6 119.2(6) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C7 C8 C9 122.2(6) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C4 117.3(6) . . ?
C8 C9 C13 119.6(6) . . ?
C4 C9 C13 123.1(5) . . ?
C12 C10 C5 112.5(7) . . ?
C12 C10 C11 112.5(8) . . ?
C5 C10 C11 110.5(6) . . ?
C12 C10 H10 107.0 . . ?
C5 C10 H10 107.0 . . ?
C11 C10 H10 107.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 110.2(7) . . ?
C14 C13 C9 110.9(6) . . ?
C15 C13 C9 111.1(6) . . ?
C14 C13 H13 108.2 . . ?
C15 C13 H13 108.2 . . ?
C9 C13 H13 108.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 122.4(5) . . ?
C21 C16 N2 119.2(5) . . ?
C17 C16 N2 118.3(5) . . ?
C18 C17 C16 116.4(6) . . ?
C18 C17 C22 121.8(6) . . ?
C16 C17 C22 121.7(6) . . ?
C19 C18 C17 123.1(6) . . ?
C19 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
C18 C19 C20 119.4(6) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 121.4(6) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 117.2(6) . . ?
C20 C21 C25 121.3(6) . . ?
C16 C21 C25 121.5(6) . . ?
C17 C22 C23 113.3(7) . . ?
C17 C22 C24 111.5(6) . . ?
C23 C22 C24 108.4(7) . . ?
C17 C22 H22 107.8 . . ?
C23 C22 H22 107.8 . . ?
C24 C22 H22 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 C27 112.4(6) . . ?
C21 C25 C26 110.0(6) . . ?
C27 C25 C26 109.1(7) . . ?
C21 C25 H25 108.4 . . ?
C27 C25 H25 108.4 . . ?
C26 C25 H25 108.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si2 C31 H31A 109.5 . . ?
Si2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si2 C33 H33A 109.5 . . ?
Si2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C1 N1 C2 111.1(5) . . ?
C1 N1 C4 126.1(5) . . ?
C2 N1 C4 122.8(5) . . ?
C1 N2 C3 111.6(5) . . ?
C1 N2 C16 124.3(5) . . ?
C3 N2 C16 124.0(5) . . ?
Si2 N3 Si1 126.0(3) . . ?
Si2 N3 Fe1 114.8(3) . . ?
Si1 N3 Fe1 119.1(3) . . ?
N3 Si1 C29 112.5(3) . . ?
N3 Si1 C28 112.8(3) . . ?
C29 Si1 C28 105.6(4) . . ?
N3 Si1 C30 112.5(3) . . ?
C29 Si1 C30 106.3(4) . . ?
C28 Si1 C30 106.6(4) . . ?
N3 Si2 C33 113.7(3) . . ?
N3 Si2 C32 112.5(3) . . ?
C33 Si2 C32 104.9(3) . . ?
N3 Si2 C31 111.3(3) . . ?
C33 Si2 C31 105.0(3) . . ?
C32 Si2 C31 109.0(3) . . ?
N3 Fe1 C1 178.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 1.2(9) . . . . ?
C9 C4 C5 C6 2.0(10) . . . . ?
N1 C4 C5 C6 176.8(6) . . . . ?
C9 C4 C5 C10 -179.7(6) . . . . ?
N1 C4 C5 C10 -4.9(9) . . . . ?
C4 C5 C6 C7 -1.6(10) . . . . ?
C10 C5 C6 C7 -180.0(7) . . . . ?
C5 C6 C7 C8 0.9(11) . . . . ?
C6 C7 C8 C9 -0.5(12) . . . . ?
C7 C8 C9 C4 0.9(11) . . . . ?
C7 C8 C9 C13 179.8(7) . . . . ?
C5 C4 C9 C8 -1.7(10) . . . . ?
N1 C4 C9 C8 -176.4(6) . . . . ?
C5 C4 C9 C13 179.5(6) . . . . ?
N1 C4 C9 C13 4.7(9) . . . . ?
C6 C5 C10 C12 67.1(10) . . . . ?
C4 C5 C10 C12 -111.2(10) . . . . ?
C6 C5 C10 C11 -59.6(10) . . . . ?
C4 C5 C10 C11 122.1(8) . . . . ?
C8 C9 C13 C14 -68.2(9) . . . . ?
C4 C9 C13 C14 110.7(8) . . . . ?
C8 C9 C13 C15 54.7(9) . . . . ?
C4 C9 C13 C15 -126.5(7) . . . . ?
C21 C16 C17 C18 1.2(9) . . . . ?
N2 C16 C17 C18 177.6(6) . . . . ?
C21 C16 C17 C22 179.0(6) . . . . ?
N2 C16 C17 C22 -4.6(9) . . . . ?
C16 C17 C18 C19 -1.5(10) . . . . ?
C22 C17 C18 C19 -179.3(7) . . . . ?
C17 C18 C19 C20 1.7(11) . . . . ?
C18 C19 C20 C21 -1.5(11) . . . . ?
C19 C20 C21 C16 1.2(10) . . . . ?
C19 C20 C21 C25 -178.5(7) . . . . ?
C17 C16 C21 C20 -1.1(9) . . . . ?
N2 C16 C21 C20 -177.4(6) . . . . ?
C17 C16 C21 C25 178.6(6) . . . . ?
N2 C16 C21 C25 2.2(9) . . . . ?
C18 C17 C22 C23 58.1(9) . . . . ?
C16 C17 C22 C23 -119.5(8) . . . . ?
C18 C17 C22 C24 -64.4(10) . . . . ?
C16 C17 C22 C24 117.9(8) . . . . ?
C20 C21 C25 C27 -42.4(9) . . . . ?
C16 C21 C25 C27 137.9(7) . . . . ?
C20 C21 C25 C26 79.4(9) . . . . ?
C16 C21 C25 C26 -100.3(8) . . . . ?
N2 C1 N1 C2 1.4(7) . . . . ?
Fe1 C1 N1 C2 -179.9(5) . . . . ?
N2 C1 N1 C4 -176.8(5) . . . . ?
Fe1 C1 N1 C4 1.9(8) . . . . ?
C3 C2 N1 C1 -1.7(8) . . . . ?
C3 C2 N1 C4 176.6(6) . . . . ?
C9 C4 N1 C1 -88.5(7) . . . . ?
C5 C4 N1 C1 96.5(7) . . . . ?
C9 C4 N1 C2 93.4(8) . . . . ?
C5 C4 N1 C2 -81.5(8) . . . . ?
N1 C1 N2 C3 -0.7(7) . . . . ?
Fe1 C1 N2 C3 -179.3(5) . . . . ?
N1 C1 N2 C16 -176.9(5) . . . . ?
Fe1 C1 N2 C16 4.5(9) . . . . ?
C2 C3 N2 C1 -0.3(9) . . . . ?
C2 C3 N2 C16 175.9(6) . . . . ?
C21 C16 N2 C1 -85.0(7) . . . . ?
C17 C16 N2 C1 98.5(7) . . . . ?
C21 C16 N2 C3 99.2(8) . . . . ?
C17 C16 N2 C3 -77.3(8) . . . . ?
Si2 N3 Si1 C29 160.8(4) . . . . ?
Fe1 N3 Si1 C29 -15.2(5) . . . . ?
Si2 N3 Si1 C28 -79.8(5) . . . . ?
Fe1 N3 Si1 C28 104.1(4) . . . . ?
Si2 N3 Si1 C30 40.8(5) . . . . ?
Fe1 N3 Si1 C30 -135.2(4) . . . . ?
Si1 N3 Si2 C33 160.3(4) . . . . ?
Fe1 N3 Si2 C33 -23.6(5) . . . . ?
Si1 N3 Si2 C32 41.2(5) . . . . ?
Fe1 N3 Si2 C32 -142.6(3) . . . . ?
Si1 N3 Si2 C31 -81.4(4) . . . . ?
Fe1 N3 Si2 C31 94.7(4) . . . . ?

_refine_diff_density_max         2.183
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.160

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_pbad150115
_database_code_depnum_ccdc_archive 'CCDC 1469263'
_audit_update_record             
;
2016-03-17 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H54 Co N3 Si2'
_chemical_formula_sum            'C33 H54 Co N3 Si2'
_chemical_formula_weight         607.90

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'
Si Si 0.0817 0.0704 '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                   12.8532(6)
_cell_length_b                   13.6697(6)
_cell_length_c                   21.9596(9)
_cell_angle_alpha                90
_cell_angle_beta                 108.401(2)
_cell_angle_gamma                90
_cell_volume                     3661.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9894
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.85

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.557
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49305
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.670
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9782
_reflns_number_gt                7012
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+1.8187P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9782
_refine_ls_number_parameters     366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1018
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
C1 C 0.29247(14) 0.24594(12) 0.84497(8) 0.0231(3) Uani 1 1 d . . . . .
C2 C 0.30755(16) 0.28276(16) 0.94854(9) 0.0355(5) Uani 1 1 d . . . . .
H2 H 0.2944 0.3127 0.9844 0.043 Uiso 1 1 calc R U . . .
C3 C 0.38204(17) 0.21312(17) 0.95009(10) 0.0370(5) Uani 1 1 d . . . . .
H3 H 0.4318 0.1844 0.9874 0.044 Uiso 1 1 calc R U . . .
C4 C 0.17128(14) 0.37735(13) 0.86452(8) 0.0239(4) Uani 1 1 d . . . . .
C5 C 0.06097(15) 0.35144(13) 0.84962(9) 0.0281(4) Uani 1 1 d . . . . .
C6 C -0.01564(16) 0.42701(15) 0.83395(11) 0.0361(5) Uani 1 1 d . . . . .
H6 H -0.0915 0.4120 0.8232 0.043 Uiso 1 1 calc R U . . .
C7 C 0.01649(18) 0.52332(15) 0.83369(11) 0.0399(5) Uani 1 1 d . . . . .
H7 H -0.0370 0.5738 0.8231 0.048 Uiso 1 1 calc R U . . .
C8 C 0.12585(19) 0.54632(15) 0.84875(11) 0.0389(5) Uani 1 1 d . . . . .
H8 H 0.1469 0.6129 0.8482 0.047 Uiso 1 1 calc R U . . .
C9 C 0.20623(16) 0.47442(14) 0.86471(9) 0.0305(4) Uani 1 1 d . . . . .
C10 C 0.02298(16) 0.24611(14) 0.85018(11) 0.0357(4) Uani 1 1 d . . . . .
H10 H 0.0895 0.2040 0.8670 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0476(2) 0.23306(19) 0.89385(13) 0.0543(6) Uani 1 1 d . . . . .
H11A H -0.0083 0.2585 0.9367 0.081 Uiso 1 1 calc R U . . .
H11B H -0.0632 0.1634 0.8970 0.081 Uiso 1 1 calc R U . . .
H11C H -0.1166 0.2689 0.8760 0.081 Uiso 1 1 calc R U . . .
C12 C -0.0390(3) 0.2122(2) 0.78278(13) 0.0636(8) Uani 1 1 d . . . . .
H12A H -0.1043 0.2530 0.7651 0.095 Uiso 1 1 calc R U . . .
H12B H -0.0612 0.1438 0.7840 0.095 Uiso 1 1 calc R U . . .
H12C H 0.0084 0.2178 0.7557 0.095 Uiso 1 1 calc R U . . .
C13 C 0.32688(18) 0.50160(17) 0.88144(11) 0.0429(5) Uani 1 1 d . . . . .
H13 H 0.3705 0.4404 0.8954 0.051 Uiso 1 1 calc R U . . .
C14 C 0.3613(2) 0.5730(3) 0.93715(15) 0.0787(10) Uani 1 1 d . . . . .
H14A H 0.3267 0.6366 0.9234 0.118 Uiso 1 1 calc R U . . .
H14B H 0.4412 0.5805 0.9513 0.118 Uiso 1 1 calc R U . . .
H14C H 0.3383 0.5480 0.9727 0.118 Uiso 1 1 calc R U . . .
C15 C 0.3527(3) 0.5402(3) 0.82300(14) 0.0880(12) Uani 1 1 d . . . . .
H15A H 0.3131 0.6017 0.8090 0.132 Uiso 1 1 calc R U . . .
H15B H 0.3299 0.4921 0.7882 0.132 Uiso 1 1 calc R U . . .
H15C H 0.4317 0.5519 0.8340 0.132 Uiso 1 1 calc R U . . .
C16 C 0.43600(14) 0.11573(13) 0.86946(9) 0.0252(4) Uani 1 1 d . . . . .
C17 C 0.52877(15) 0.14277(13) 0.85290(9) 0.0285(4) Uani 1 1 d . . . . .
C18 C 0.58957(16) 0.06702(15) 0.83825(11) 0.0353(5) Uani 1 1 d . . . . .
H18 H 0.6531 0.0824 0.8269 0.042 Uiso 1 1 calc R U . . .
C19 C 0.55975(17) -0.02955(15) 0.83983(11) 0.0381(5) Uani 1 1 d . . . . .
H19 H 0.6026 -0.0798 0.8296 0.046 Uiso 1 1 calc R U . . .
C20 C 0.46779(17) -0.05331(14) 0.85625(11) 0.0364(5) Uani 1 1 d . . . . .
H20 H 0.4478 -0.1201 0.8571 0.044 Uiso 1 1 calc R U . . .
C21 C 0.40369(15) 0.01874(14) 0.87165(9) 0.0300(4) Uani 1 1 d . . . . .
C22 C 0.56455(17) 0.24840(14) 0.85234(11) 0.0379(5) Uani 1 1 d . . . . .
H22 H 0.4999 0.2911 0.8492 0.045 Uiso 1 1 calc R U . . .
C23 C 0.6544(3) 0.2734(2) 0.91438(13) 0.0705(9) Uani 1 1 d . . . . .
H23A H 0.6271 0.2635 0.9508 0.106 Uiso 1 1 calc R U . . .
H23B H 0.6761 0.3420 0.9132 0.106 Uiso 1 1 calc R U . . .
H23C H 0.7180 0.2310 0.9191 0.106 Uiso 1 1 calc R U . . .
C24 C 0.6037(3) 0.27092(19) 0.79524(12) 0.0652(8) Uani 1 1 d . . . . .
H24A H 0.6731 0.2369 0.8004 0.098 Uiso 1 1 calc R U . . .
H24B H 0.6146 0.3416 0.7929 0.098 Uiso 1 1 calc R U . . .
H24C H 0.5485 0.2488 0.7557 0.098 Uiso 1 1 calc R U . . .
C25 C 0.30230(17) -0.00974(17) 0.88934(11) 0.0418(5) Uani 1 1 d . . . . .
H25 H 0.2670 0.0520 0.8974 0.050 Uiso 1 1 calc R U . . .
C26 C 0.3319(2) -0.0704(2) 0.95077(14) 0.0695(9) Uani 1 1 d . . . . .
H26A H 0.3614 -0.1338 0.9433 0.104 Uiso 1 1 calc R U . . .
H26B H 0.2662 -0.0808 0.9635 0.104 Uiso 1 1 calc R U . . .
H26C H 0.3873 -0.0356 0.9850 0.104 Uiso 1 1 calc R U . . .
C27 C 0.2199(2) -0.0627(3) 0.83461(15) 0.0893(12) Uani 1 1 d . . . . .
H27A H 0.1990 -0.0207 0.7965 0.134 Uiso 1 1 calc R U . . .
H27B H 0.1547 -0.0784 0.8467 0.134 Uiso 1 1 calc R U . . .
H27C H 0.2526 -0.1232 0.8251 0.134 Uiso 1 1 calc R U . . .
C28 C 0.15065(19) 0.38529(17) 0.55210(11) 0.0443(5) Uani 1 1 d . . . . .
H28A H 0.2216 0.4183 0.5695 0.066 Uiso 1 1 calc R U . . .
H28B H 0.0951 0.4328 0.5290 0.066 Uiso 1 1 calc R U . . .
H28C H 0.1566 0.3334 0.5226 0.066 Uiso 1 1 calc R U . . .
C29 C -0.03216(17) 0.28044(17) 0.58317(12) 0.0422(5) Uani 1 1 d . . . . .
H29A H -0.0291 0.2216 0.5583 0.063 Uiso 1 1 calc R U . . .
H29B H -0.0783 0.3298 0.5549 0.063 Uiso 1 1 calc R U . . .
H29C H -0.0632 0.2638 0.6173 0.063 Uiso 1 1 calc R U . . .
C30 C 0.0989(2) 0.43517(16) 0.67243(12) 0.0476(6) Uani 1 1 d . . . . .
H30A H 0.0750 0.4108 0.7078 0.071 Uiso 1 1 calc R U . . .
H30B H 0.0454 0.4827 0.6472 0.071 Uiso 1 1 calc R U . . .
H30C H 0.1706 0.4668 0.6898 0.071 Uiso 1 1 calc R U . . .
C31 C 0.16496(17) 0.09957(15) 0.55430(10) 0.0364(5) Uani 1 1 d . . . . .
H31A H 0.1046 0.0667 0.5643 0.055 Uiso 1 1 calc R U . . .
H31B H 0.2051 0.0518 0.5370 0.055 Uiso 1 1 calc R U . . .
H31C H 0.1354 0.1510 0.5224 0.055 Uiso 1 1 calc R U . . .
C32 C 0.38308(16) 0.20622(15) 0.61095(10) 0.0327(4) Uani 1 1 d . . . . .
H32A H 0.3611 0.2638 0.5833 0.049 Uiso 1 1 calc R U . . .
H32B H 0.4126 0.1564 0.5888 0.049 Uiso 1 1 calc R U . . .
H32C H 0.4394 0.2249 0.6510 0.049 Uiso 1 1 calc R U . . .
C33 C 0.31444(19) 0.05093(15) 0.68578(11) 0.0405(5) Uani 1 1 d . . . . .
H33A H 0.3691 0.0751 0.7249 0.061 Uiso 1 1 calc R U . . .
H33B H 0.3485 0.0027 0.6650 0.061 Uiso 1 1 calc R U . . .
H33C H 0.2538 0.0202 0.6968 0.061 Uiso 1 1 calc R U . . .
N1 N 0.25386(12) 0.30237(11) 0.88462(7) 0.0256(3) Uani 1 1 d . . . . .
N2 N 0.37253(12) 0.19123(12) 0.88707(7) 0.0278(3) Uani 1 1 d . . . . .
N3 N 0.19955(12) 0.24340(11) 0.66190(7) 0.0262(3) Uani 1 1 d . . . . .
Si1 Si 0.10975(4) 0.33049(4) 0.61979(3) 0.02801(12) Uani 1 1 d . . . . .
Si2 Si 0.26073(4) 0.15565(4) 0.62957(2) 0.02474(11) Uani 1 1 d . . . . .
Co1 Co 0.24512(2) 0.24607(2) 0.75177(2) 0.02530(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.368(2) . ?
C1 N1 1.368(2) . ?
C1 Co1 1.9423(18) . ?
C2 C3 1.343(3) . ?
C2 N1 1.381(2) . ?
C2 H2 0.9500 . ?
C3 N2 1.383(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(3) . ?
C4 C9 1.400(3) . ?
C4 N1 1.441(2) . ?
C5 C6 1.393(3) . ?
C5 C10 1.522(3) . ?
C6 C7 1.380(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.375(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(3) . ?
C8 H8 0.9500 . ?
C9 C13 1.523(3) . ?
C10 C12 1.515(3) . ?
C10 C11 1.524(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.518(3) . ?
C13 C15 1.518(4) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.395(3) . ?
C16 C17 1.402(3) . ?
C16 N2 1.442(2) . ?
C17 C18 1.395(3) . ?
C17 C22 1.517(3) . ?
C18 C19 1.378(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.379(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(3) . ?
C20 H20 0.9500 . ?
C21 C25 1.523(3) . ?
C22 C23 1.521(3) . ?
C22 C24 1.522(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.512(4) . ?
C25 C26 1.526(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 Si1 1.882(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 Si1 1.875(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 Si1 1.872(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 Si2 1.884(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 Si2 1.877(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 Si2 1.874(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N3 Si2 1.7072(15) . ?
N3 Si1 1.7119(15) . ?
N3 Co1 1.8734(15) . ?

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
N2 C1 N1 102.98(15) . . ?
N2 C1 Co1 129.14(12) . . ?
N1 C1 Co1 127.88(12) . . ?
C3 C2 N1 106.68(17) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 106.91(17) . . ?
C2 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
C5 C4 C9 122.82(16) . . ?
C5 C4 N1 119.11(16) . . ?
C9 C4 N1 117.94(16) . . ?
C6 C5 C4 117.12(17) . . ?
C6 C5 C10 120.00(17) . . ?
C4 C5 C10 122.87(16) . . ?
C7 C6 C5 121.28(19) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C8 C7 C6 120.11(19) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 121.44(19) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C4 117.23(18) . . ?
C8 C9 C13 120.55(19) . . ?
C4 C9 C13 122.22(18) . . ?
C12 C10 C5 110.66(18) . . ?
C12 C10 C11 110.2(2) . . ?
C5 C10 C11 111.84(18) . . ?
C12 C10 H10 108.0 . . ?
C5 C10 H10 108.0 . . ?
C11 C10 H10 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 111.8(2) . . ?
C14 C13 C9 111.54(19) . . ?
C15 C13 C9 111.0(2) . . ?
C14 C13 H13 107.4 . . ?
C15 C13 H13 107.4 . . ?
C9 C13 H13 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 123.13(16) . . ?
C21 C16 N2 118.11(16) . . ?
C17 C16 N2 118.72(16) . . ?
C18 C17 C16 116.66(17) . . ?
C18 C17 C22 120.76(17) . . ?
C16 C17 C22 122.56(17) . . ?
C19 C18 C17 121.66(18) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 120.02(18) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 121.24(18) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C20 C21 C16 117.30(17) . . ?
C20 C21 C25 120.03(18) . . ?
C16 C21 C25 122.67(18) . . ?
C17 C22 C23 110.70(19) . . ?
C17 C22 C24 112.28(18) . . ?
C23 C22 C24 109.7(2) . . ?
C17 C22 H22 108.0 . . ?
C23 C22 H22 108.0 . . ?
C24 C22 H22 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C25 C21 111.1(2) . . ?
C27 C25 C26 111.1(2) . . ?
C21 C25 C26 111.69(18) . . ?
C27 C25 H25 107.6 . . ?
C21 C25 H25 107.6 . . ?
C26 C25 H25 107.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si2 C31 H31A 109.5 . . ?
Si2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si2 C33 H33A 109.5 . . ?
Si2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C1 N1 C2 111.85(15) . . ?
C1 N1 C4 125.88(15) . . ?
C2 N1 C4 122.21(15) . . ?
C1 N2 C3 111.59(15) . . ?
C1 N2 C16 125.33(15) . . ?
C3 N2 C16 122.99(15) . . ?
Si2 N3 Si1 125.77(9) . . ?
Si2 N3 Co1 114.83(8) . . ?
Si1 N3 Co1 119.27(8) . . ?
N3 Si1 C30 111.52(9) . . ?
N3 Si1 C29 112.13(9) . . ?
C30 Si1 C29 106.96(11) . . ?
N3 Si1 C28 113.25(9) . . ?
C30 Si1 C28 106.10(11) . . ?
C29 Si1 C28 106.44(11) . . ?
N3 Si2 C33 112.64(9) . . ?
N3 Si2 C32 111.06(9) . . ?
C33 Si2 C32 105.37(10) . . ?
N3 Si2 C31 113.05(9) . . ?
C33 Si2 C31 105.66(10) . . ?
C32 Si2 C31 108.60(9) . . ?
N3 Co1 C1 178.83(7) . . ?

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
N1 C2 C3 N2 -0.1(3) . . . . ?
C9 C4 C5 C6 0.6(3) . . . . ?
N1 C4 C5 C6 176.44(17) . . . . ?
C9 C4 C5 C10 -179.24(18) . . . . ?
N1 C4 C5 C10 -3.4(3) . . . . ?
C4 C5 C6 C7 -0.5(3) . . . . ?
C10 C5 C6 C7 179.3(2) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C6 C7 C8 C9 -0.3(3) . . . . ?
C7 C8 C9 C4 0.3(3) . . . . ?
C7 C8 C9 C13 -179.8(2) . . . . ?
C5 C4 C9 C8 -0.5(3) . . . . ?
N1 C4 C9 C8 -176.40(17) . . . . ?
C5 C4 C9 C13 179.63(18) . . . . ?
N1 C4 C9 C13 3.7(3) . . . . ?
C6 C5 C10 C12 68.0(3) . . . . ?
C4 C5 C10 C12 -112.2(2) . . . . ?
C6 C5 C10 C11 -55.3(3) . . . . ?
C4 C5 C10 C11 124.6(2) . . . . ?
C8 C9 C13 C14 57.2(3) . . . . ?
C4 C9 C13 C14 -122.9(2) . . . . ?
C8 C9 C13 C15 -68.2(3) . . . . ?
C4 C9 C13 C15 111.7(3) . . . . ?
C21 C16 C17 C18 0.0(3) . . . . ?
N2 C16 C17 C18 177.97(17) . . . . ?
C21 C16 C17 C22 -178.43(19) . . . . ?
N2 C16 C17 C22 -0.4(3) . . . . ?
C16 C17 C18 C19 0.2(3) . . . . ?
C22 C17 C18 C19 178.6(2) . . . . ?
C17 C18 C19 C20 -0.1(3) . . . . ?
C18 C19 C20 C21 -0.2(3) . . . . ?
C19 C20 C21 C16 0.3(3) . . . . ?
C19 C20 C21 C25 179.8(2) . . . . ?
C17 C16 C21 C20 -0.2(3) . . . . ?
N2 C16 C21 C20 -178.20(17) . . . . ?
C17 C16 C21 C25 -179.64(18) . . . . ?
N2 C16 C21 C25 2.4(3) . . . . ?
C18 C17 C22 C23 -80.7(3) . . . . ?
C16 C17 C22 C23 97.6(2) . . . . ?
C18 C17 C22 C24 42.2(3) . . . . ?
C16 C17 C22 C24 -139.4(2) . . . . ?
C20 C21 C25 C27 -60.9(3) . . . . ?
C16 C21 C25 C27 118.5(3) . . . . ?
C20 C21 C25 C26 63.7(3) . . . . ?
C16 C21 C25 C26 -116.9(2) . . . . ?
N2 C1 N1 C2 -0.3(2) . . . . ?
Co1 C1 N1 C2 -179.62(14) . . . . ?
N2 C1 N1 C4 176.75(16) . . . . ?
Co1 C1 N1 C4 -2.5(3) . . . . ?
C3 C2 N1 C1 0.3(2) . . . . ?
C3 C2 N1 C4 -176.95(18) . . . . ?
C5 C4 N1 C1 87.4(2) . . . . ?
C9 C4 N1 C1 -96.5(2) . . . . ?
C5 C4 N1 C2 -95.8(2) . . . . ?
C9 C4 N1 C2 80.3(2) . . . . ?
N1 C1 N2 C3 0.3(2) . . . . ?
Co1 C1 N2 C3 179.56(15) . . . . ?
N1 C1 N2 C16 176.92(16) . . . . ?
Co1 C1 N2 C16 -3.8(3) . . . . ?
C2 C3 N2 C1 -0.1(3) . . . . ?
C2 C3 N2 C16 -176.86(18) . . . . ?
C21 C16 N2 C1 -98.1(2) . . . . ?
C17 C16 N2 C1 83.8(2) . . . . ?
C21 C16 N2 C3 78.1(2) . . . . ?
C17 C16 N2 C3 -100.0(2) . . . . ?
Si2 N3 Si1 C30 -160.92(12) . . . . ?
Co1 N3 Si1 C30 14.63(14) . . . . ?
Si2 N3 Si1 C29 79.16(14) . . . . ?
Co1 N3 Si1 C29 -105.29(12) . . . . ?
Si2 N3 Si1 C28 -41.33(15) . . . . ?
Co1 N3 Si1 C28 134.23(11) . . . . ?
Si1 N3 Si2 C33 -160.84(12) . . . . ?
Co1 N3 Si2 C33 23.44(13) . . . . ?
Si1 N3 Si2 C32 81.23(13) . . . . ?
Co1 N3 Si2 C32 -94.50(10) . . . . ?
Si1 N3 Si2 C31 -41.15(14) . . . . ?
Co1 N3 Si2 C31 143.13(10) . . . . ?

_refine_diff_density_max         0.366
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.052

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_pbad150623
_database_code_depnum_ccdc_archive 'CCDC 1469265'
_audit_update_record             
;
2016-03-17 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H96 Co2 N6'
_chemical_formula_sum            'C72 H96 Co2 N6'
_chemical_formula_weight         1163.40

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'
Co Co 0.3494 0.9721 '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                   12.1174(5)
_cell_length_b                   12.5086(5)
_cell_length_c                   13.6791(5)
_cell_angle_alpha                102.2490(10)
_cell_angle_beta                 113.9150(10)
_cell_angle_gamma                99.5290(10)
_cell_volume                     1777.26(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9341
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      30.00

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.508
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38385
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.713
_diffrn_reflns_theta_max         30.024
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10340
_reflns_number_gt                8633
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0835P)²+0.1635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10340
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1359
_refine_ls_wR_factor_gt          0.1300
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.140
_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
C1 C 0.48026(13) 0.07753(12) 0.28820(11) 0.0211(3) Uani 1 1 d . . . . .
C2 C 0.39974(16) 0.11542(17) 0.11818(13) 0.0361(4) Uani 1 1 d . . . . .
H2 H 0.3404 0.1200 0.0489 0.043 Uiso 1 1 calc R U . . .
C3 C 0.52510(16) 0.15066(17) 0.16166(14) 0.0357(4) Uani 1 1 d . . . . .
H3 H 0.5718 0.1848 0.1292 0.043 Uiso 1 1 calc R U . . .
C4 C 0.24551(14) 0.01575(14) 0.16690(12) 0.0273(3) Uani 1 1 d . . . . .
C5 C 0.18447(14) 0.07419(14) 0.21786(13) 0.0277(3) Uani 1 1 d . . . . .
C6 C 0.06015(16) 0.01952(17) 0.18833(16) 0.0382(4) Uani 1 1 d . . . . .
H6 H 0.0162 0.0566 0.2221 0.046 Uiso 1 1 calc R U . . .
C7 C 0.00017(17) -0.08817(19) 0.11031(19) 0.0474(5) Uani 1 1 d . . . . .
H7 H -0.0842 -0.1246 0.0915 0.057 Uiso 1 1 calc R U . . .
C8 C 0.06230(18) -0.14290(18) 0.0597(2) 0.0517(5) Uani 1 1 d . . . . .
H8 H 0.0200 -0.2169 0.0067 0.062 Uiso 1 1 calc R U . . .
C9 C 0.18654(16) -0.09127(17) 0.08517(16) 0.0410(4) Uani 1 1 d . . . . .
C10 C 0.25149(16) 0.19311(15) 0.30187(14) 0.0330(3) Uani 1 1 d . . . . .
H10 H 0.3407 0.1951 0.3483 0.040 Uiso 1 1 calc R U . . .
C11 C 0.1951(2) 0.2229(2) 0.38220(19) 0.0526(5) Uani 1 1 d . . . . .
H11A H 0.1098 0.2282 0.3400 0.079 Uiso 1 1 calc R U . . .
H11B H 0.2475 0.2963 0.4398 0.079 Uiso 1 1 calc R U . . .
H11C H 0.1918 0.1635 0.4183 0.079 Uiso 1 1 calc R U . . .
C12 C 0.2538(3) 0.28323(19) 0.2431(2) 0.0562(6) Uani 1 1 d . . . . .
H12A H 0.2904 0.2637 0.1919 0.084 Uiso 1 1 calc R U . . .
H12B H 0.3048 0.3577 0.2993 0.084 Uiso 1 1 calc R U . . .
H12C H 0.1678 0.2864 0.2001 0.084 Uiso 1 1 calc R U . . .
C13 C 0.2561(2) -0.14807(19) 0.02558(17) 0.0481(5) Uani 1 1 d . . . . .
H13 H 0.3248 -0.0853 0.0332 0.058 Uiso 1 1 calc R U . . .
C14 C 0.3184(4) -0.2239(4) 0.0852(3) 0.1097(16) Uani 1 1 d . . . . .
H14A H 0.2552 -0.2825 0.0868 0.165 Uiso 1 1 calc R U . . .
H14B H 0.3805 -0.1788 0.1623 0.165 Uiso 1 1 calc R U . . .
H14C H 0.3608 -0.2603 0.0458 0.165 Uiso 1 1 calc R U . . .
C15 C 0.1747(2) -0.2043(2) -0.09690(19) 0.0523(5) Uani 1 1 d . . . . .
H15A H 0.2211 -0.2439 -0.1294 0.078 Uiso 1 1 calc R U . . .
H15B H 0.1500 -0.1467 -0.1333 0.078 Uiso 1 1 calc R U . . .
H15C H 0.0993 -0.2595 -0.1088 0.078 Uiso 1 1 calc R U . . .
C16 C 0.70638(13) 0.16575(14) 0.33860(12) 0.0262(3) Uani 1 1 d . . . . .
C17 C 0.77525(14) 0.08493(14) 0.35109(13) 0.0269(3) Uani 1 1 d . . . . .
C18 C 0.90450(15) 0.12577(16) 0.42188(15) 0.0355(4) Uani 1 1 d . . . . .
H18 H 0.9538 0.0736 0.4317 0.043 Uiso 1 1 calc R U . . .
C19 C 0.96193(16) 0.24050(18) 0.47780(17) 0.0436(4) Uani 1 1 d . . . . .
H19 H 1.0500 0.2662 0.5261 0.052 Uiso 1 1 calc R U . . .
C20 C 0.89258(17) 0.31860(17) 0.46430(17) 0.0419(4) Uani 1 1 d . . . . .
H20 H 0.9334 0.3973 0.5037 0.050 Uiso 1 1 calc R U . . .
C21 C 0.76272(15) 0.28262(15) 0.39307(15) 0.0326(3) Uani 1 1 d . . . . .
C22 C 0.71080(16) -0.04115(14) 0.28866(13) 0.0304(3) Uani 1 1 d . . . . .
H22 H 0.6285 -0.0595 0.2909 0.036 Uiso 1 1 calc R U . . .
C23 C 0.7855(2) -0.11866(18) 0.34139(18) 0.0447(4) Uani 1 1 d . . . . .
H23A H 0.8628 -0.1086 0.3330 0.067 Uiso 1 1 calc R U . . .
H23B H 0.7345 -0.1983 0.3035 0.067 Uiso 1 1 calc R U . . .
H23C H 0.8072 -0.0988 0.4215 0.067 Uiso 1 1 calc R U . . .
C24 C 0.6826(2) -0.06806(19) 0.16488(16) 0.0463(5) Uani 1 1 d . . . . .
H24A H 0.6324 -0.0201 0.1305 0.070 Uiso 1 1 calc R U . . .
H24B H 0.6356 -0.1485 0.1250 0.070 Uiso 1 1 calc R U . . .
H24C H 0.7619 -0.0528 0.1599 0.070 Uiso 1 1 calc R U . . .
C25 C 0.68871(18) 0.36994(16) 0.37864(17) 0.0395(4) Uani 1 1 d . . . . .
H25 H 0.6040 0.3299 0.3132 0.047 Uiso 1 1 calc R U . . .
C26 C 0.6674(5) 0.4118(4) 0.4791(3) 0.130(2) Uani 1 1 d . . . . .
H26A H 0.7487 0.4495 0.5459 0.195 Uiso 1 1 calc R U . . .
H26B H 0.6223 0.3471 0.4909 0.195 Uiso 1 1 calc R U . . .
H26C H 0.6175 0.4662 0.4662 0.195 Uiso 1 1 calc R U . . .
C27 C 0.7464(4) 0.4667(3) 0.3507(4) 0.1081(15) Uani 1 1 d . . . . .
H27A H 0.6915 0.5169 0.3361 0.162 Uiso 1 1 calc R U . . .
H27B H 0.7567 0.4368 0.2836 0.162 Uiso 1 1 calc R U . . .
H27C H 0.8287 0.5099 0.4140 0.162 Uiso 1 1 calc R U . . .
C28 C 0.63321(15) 0.21813(13) 0.63743(12) 0.0270(3) Uani 1 1 d . . . . .
C29 C 0.75014(16) 0.20096(14) 0.65284(14) 0.0306(3) Uani 1 1 d . . . . .
C30 C 0.85973(18) 0.28916(17) 0.72065(17) 0.0437(4) Uani 1 1 d . . . . .
H30 H 0.9381 0.2764 0.7302 0.052 Uiso 1 1 calc R U . . .
C31 C 0.8579(2) 0.39614(18) 0.77526(19) 0.0538(6) Uani 1 1 d . . . . .
C32 C 0.7432(2) 0.41154(16) 0.76044(18) 0.0496(5) Uani 1 1 d . . . . .
H32 H 0.7406 0.4836 0.7979 0.060 Uiso 1 1 calc R U . . .
C33 C 0.63055(19) 0.32582(14) 0.69279(15) 0.0372(4) Uani 1 1 d . . . . .
C34 C 0.75564(16) 0.08693(15) 0.59579(14) 0.0327(3) Uani 1 1 d . . . . .
H34A H 0.8435 0.0889 0.6158 0.049 Uiso 1 1 calc R U . . .
H34B H 0.7079 0.0691 0.5141 0.049 Uiso 1 1 calc R U . . .
H34C H 0.7191 0.0283 0.6202 0.049 Uiso 1 1 calc R U . . .
C35 C 0.9782(3) 0.4932(2) 0.8462(3) 0.0911(11) Uani 1 1 d . . . . .
H35A H 1.0100 0.5188 0.7972 0.137 Uiso 1 1 calc R U . . .
H35B H 1.0415 0.4667 0.8994 0.137 Uiso 1 1 calc R U . . .
H35C H 0.9608 0.5566 0.8879 0.137 Uiso 1 1 calc R U . . .
C36 C 0.5078(2) 0.34819(18) 0.6788(2) 0.0566(6) Uani 1 1 d . . . . .
H36A H 0.5232 0.4281 0.7191 0.085 Uiso 1 1 calc R U . . .
H36B H 0.4684 0.2986 0.7093 0.085 Uiso 1 1 calc R U . . .
H36C H 0.4518 0.3324 0.5987 0.085 Uiso 1 1 calc R U . . .
N1 N 0.37249(11) 0.07088(12) 0.19346(10) 0.0258(3) Uani 1 1 d . . . . .
N2 N 0.57407(11) 0.12747(12) 0.26399(10) 0.0249(3) Uani 1 1 d . . . . .
N3 N 0.52260(12) 0.12772(10) 0.56748(10) 0.0232(2) Uani 1 1 d . . . . .
Co1 Co 0.49298(2) 0.03110(2) 0.41421(2) 0.02093(7) Uani 1 1 d . . . . .
H3N H 0.4587(18) 0.1495(16) 0.5626(16) 0.026(5) 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
C1 N1 1.3921(17) . ?
C1 N2 1.3965(18) . ?
C1 Co1 1.8897(14) . ?
C2 C3 1.338(2) . ?
C2 N1 1.392(2) . ?
C2 H2 0.9500 . ?
C3 N2 1.3971(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(2) . ?
C4 C9 1.397(2) . ?
C4 N1 1.4368(19) . ?
C5 C6 1.396(2) . ?
C5 C10 1.520(2) . ?
C6 C7 1.385(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.380(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.401(3) . ?
C8 H8 0.9500 . ?
C9 C13 1.546(3) . ?
C10 C12 1.520(3) . ?
C10 C11 1.527(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.483(3) . ?
C13 C15 1.485(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.398(2) . ?
C16 C17 1.409(2) . ?
C16 N2 1.4328(18) . ?
C17 C18 1.395(2) . ?
C17 C22 1.519(2) . ?
C18 C19 1.379(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.402(2) . ?
C20 H20 0.9500 . ?
C21 C25 1.519(2) . ?
C22 C23 1.529(2) . ?
C22 C24 1.532(2) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.495(3) . ?
C25 C26 1.502(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.406(2) . ?
C28 N3 1.411(2) . ?
C28 C33 1.411(2) . ?
C29 C30 1.387(2) . ?
C29 C34 1.500(2) . ?
C30 C31 1.396(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(4) . ?
C31 C35 1.519(3) . ?
C32 C33 1.393(3) . ?
C32 H32 0.9500 . ?
C33 C36 1.502(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N3 Co1 2.0387(12) . ?
N3 Co1 2.0421(12) 2_656 ?
N3 H3N 0.84(2) . ?
Co1 N3 2.0421(12) 2_656 ?
Co1 Co1 2.5765(4) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 100.93(11) . . ?
N1 C1 Co1 128.74(10) . . ?
N2 C1 Co1 130.33(10) . . ?
C3 C2 N1 107.21(13) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 106.67(14) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
C5 C4 C9 123.22(15) . . ?
C5 C4 N1 118.82(14) . . ?
C9 C4 N1 117.82(14) . . ?
C4 C5 C6 117.50(16) . . ?
C4 C5 C10 120.86(14) . . ?
C6 C5 C10 121.63(15) . . ?
C7 C6 C5 120.72(17) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C6 120.42(17) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 121.20(19) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C8 116.85(18) . . ?
C4 C9 C13 120.88(17) . . ?
C8 C9 C13 122.27(18) . . ?
C12 C10 C5 111.52(15) . . ?
C12 C10 C11 109.92(17) . . ?
C5 C10 C11 112.80(16) . . ?
C12 C10 H10 107.4 . . ?
C5 C10 H10 107.4 . . ?
C11 C10 H10 107.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 113.7(2) . . ?
C14 C13 C9 110.3(2) . . ?
C15 C13 C9 112.79(17) . . ?
C14 C13 H13 106.5 . . ?
C15 C13 H13 106.5 . . ?
C9 C13 H13 106.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 122.61(14) . . ?
C21 C16 N2 118.45(14) . . ?
C17 C16 N2 118.90(14) . . ?
C18 C17 C16 117.27(15) . . ?
C18 C17 C22 121.76(15) . . ?
C16 C17 C22 120.97(14) . . ?
C19 C18 C17 121.18(16) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 120.66(16) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C21 120.64(18) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C16 C21 C20 117.63(16) . . ?
C16 C21 C25 122.63(15) . . ?
C20 C21 C25 119.74(17) . . ?
C17 C22 C23 113.46(15) . . ?
C17 C22 C24 110.87(15) . . ?
C23 C22 C24 109.53(15) . . ?
C17 C22 H22 107.6 . . ?
C23 C22 H22 107.6 . . ?
C24 C22 H22 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C25 C26 111.4(3) . . ?
C27 C25 C21 112.83(18) . . ?
C26 C25 C21 111.56(18) . . ?
C27 C25 H25 106.9 . . ?
C26 C25 H25 106.9 . . ?
C21 C25 H25 106.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 N3 119.26(14) . . ?
C29 C28 C33 118.64(16) . . ?
N3 C28 C33 122.11(15) . . ?
C30 C29 C28 120.02(17) . . ?
C30 C29 C34 120.30(16) . . ?
C28 C29 C34 119.68(15) . . ?
C29 C30 C31 121.7(2) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C32 C31 C30 117.71(18) . . ?
C32 C31 C35 121.1(2) . . ?
C30 C31 C35 121.2(2) . . ?
C31 C32 C33 122.70(19) . . ?
C31 C32 H32 118.6 . . ?
C33 C32 H32 118.6 . . ?
C32 C33 C28 119.19(18) . . ?
C32 C33 C36 120.27(17) . . ?
C28 C33 C36 120.54(17) . . ?
C29 C34 H34A 109.5 . . ?
C29 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C29 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C2 N1 C1 112.62(12) . . ?
C2 N1 C4 121.33(12) . . ?
C1 N1 C4 125.82(12) . . ?
C1 N2 C3 112.56(12) . . ?
C1 N2 C16 125.82(11) . . ?
C3 N2 C16 121.18(13) . . ?
C28 N3 Co1 121.25(10) . . ?
C28 N3 Co1 121.46(9) . 2_656 ?
Co1 N3 Co1 78.30(4) . 2_656 ?
C28 N3 H3N 110.2(13) . . ?
Co1 N3 H3N 110.8(13) . . ?
Co1 N3 H3N 111.3(13) 2_656 . ?
C1 Co1 N3 128.64(5) . . ?
C1 Co1 N3 129.65(6) . 2_656 ?
N3 Co1 N3 101.70(4) . 2_656 ?
C1 Co1 Co1 179.03(4) . 2_656 ?
N3 Co1 Co1 50.91(3) . 2_656 ?
N3 Co1 Co1 50.79(3) 2_656 2_656 ?

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
N1 C2 C3 N2 -0.1(2) . . . . ?
C9 C4 C5 C6 2.9(2) . . . . ?
N1 C4 C5 C6 178.48(14) . . . . ?
C9 C4 C5 C10 -176.80(16) . . . . ?
N1 C4 C5 C10 -1.2(2) . . . . ?
C4 C5 C6 C7 -0.7(3) . . . . ?
C10 C5 C6 C7 179.01(17) . . . . ?
C5 C6 C7 C8 -0.5(3) . . . . ?
C6 C7 C8 C9 -0.4(4) . . . . ?
C5 C4 C9 C8 -3.7(3) . . . . ?
N1 C4 C9 C8 -179.33(17) . . . . ?
C5 C4 C9 C13 175.60(17) . . . . ?
N1 C4 C9 C13 0.0(3) . . . . ?
C7 C8 C9 C4 2.4(3) . . . . ?
C7 C8 C9 C13 -176.9(2) . . . . ?
C4 C5 C10 C12 79.3(2) . . . . ?
C6 C5 C10 C12 -100.4(2) . . . . ?
C4 C5 C10 C11 -156.39(16) . . . . ?
C6 C5 C10 C11 23.9(2) . . . . ?
C4 C9 C13 C14 93.0(3) . . . . ?
C8 C9 C13 C14 -87.7(3) . . . . ?
C4 C9 C13 C15 -138.5(2) . . . . ?
C8 C9 C13 C15 40.8(3) . . . . ?
C21 C16 C17 C18 0.5(2) . . . . ?
N2 C16 C17 C18 178.14(13) . . . . ?
C21 C16 C17 C22 -178.83(14) . . . . ?
N2 C16 C17 C22 -1.2(2) . . . . ?
C16 C17 C18 C19 0.5(2) . . . . ?
C22 C17 C18 C19 179.79(16) . . . . ?
C17 C18 C19 C20 -0.5(3) . . . . ?
C18 C19 C20 C21 -0.3(3) . . . . ?
C17 C16 C21 C20 -1.3(2) . . . . ?
N2 C16 C21 C20 -178.99(15) . . . . ?
C17 C16 C21 C25 179.33(15) . . . . ?
N2 C16 C21 C25 1.7(2) . . . . ?
C19 C20 C21 C16 1.2(3) . . . . ?
C19 C20 C21 C25 -179.40(18) . . . . ?
C18 C17 C22 C23 21.3(2) . . . . ?
C16 C17 C22 C23 -159.43(15) . . . . ?
C18 C17 C22 C24 -102.48(18) . . . . ?
C16 C17 C22 C24 76.81(19) . . . . ?
C16 C21 C25 C27 -129.9(3) . . . . ?
C20 C21 C25 C27 50.7(3) . . . . ?
C16 C21 C25 C26 103.7(3) . . . . ?
C20 C21 C25 C26 -75.6(3) . . . . ?
N3 C28 C29 C30 179.52(15) . . . . ?
C33 C28 C29 C30 -0.5(2) . . . . ?
N3 C28 C29 C34 -0.6(2) . . . . ?
C33 C28 C29 C34 179.43(15) . . . . ?
C28 C29 C30 C31 0.1(3) . . . . ?
C34 C29 C30 C31 -179.76(18) . . . . ?
C29 C30 C31 C32 0.5(3) . . . . ?
C29 C30 C31 C35 -178.0(2) . . . . ?
C30 C31 C32 C33 -0.8(3) . . . . ?
C35 C31 C32 C33 177.7(3) . . . . ?
C31 C32 C33 C28 0.5(3) . . . . ?
C31 C32 C33 C36 -179.3(2) . . . . ?
C29 C28 C33 C32 0.2(2) . . . . ?
N3 C28 C33 C32 -179.82(16) . . . . ?
C29 C28 C33 C36 179.94(18) . . . . ?
N3 C28 C33 C36 -0.1(3) . . . . ?
C3 C2 N1 C1 0.6(2) . . . . ?
C3 C2 N1 C4 -174.13(16) . . . . ?
N2 C1 N1 C2 -0.85(17) . . . . ?
Co1 C1 N1 C2 179.02(12) . . . . ?
N2 C1 N1 C4 173.62(14) . . . . ?
Co1 C1 N1 C4 -6.5(2) . . . . ?
C5 C4 N1 C2 -104.51(18) . . . . ?
C9 C4 N1 C2 71.3(2) . . . . ?
C5 C4 N1 C1 81.46(19) . . . . ?
C9 C4 N1 C1 -102.74(19) . . . . ?
N1 C1 N2 C3 0.80(17) . . . . ?
Co1 C1 N2 C3 -179.07(12) . . . . ?
N1 C1 N2 C16 173.20(14) . . . . ?
Co1 C1 N2 C16 -6.7(2) . . . . ?
C2 C3 N2 C1 -0.5(2) . . . . ?
C2 C3 N2 C16 -173.27(16) . . . . ?
C21 C16 N2 C1 -102.66(18) . . . . ?
C17 C16 N2 C1 79.59(19) . . . . ?
C21 C16 N2 C3 69.1(2) . . . . ?
C17 C16 N2 C3 -108.62(17) . . . . ?
C29 C28 N3 Co1 -45.45(17) . . . . ?
C33 C28 N3 Co1 134.56(13) . . . . ?
C29 C28 N3 Co1 49.90(17) . . . 2_656 ?
C33 C28 N3 Co1 -130.09(14) . . . 2_656 ?
N1 C1 Co1 N3 -98.10(14) . . . . ?
N2 C1 Co1 N3 81.74(15) . . . . ?
N1 C1 Co1 N3 80.50(14) . . . 2_656 ?
N2 C1 Co1 N3 -99.66(14) . . . 2_656 ?

_refine_diff_density_max         1.455
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.075

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.033 0.393 0.347 9.1 0.8
2 0.500 0.500 1.000 239.9 53.5
3 0.967 0.607 0.653 9.1 0.8
_platon_squeeze_details          
;
 The residual electron density was assigned to half a molecule of the
 pentane solvent [55/2 = 28 e per asymmetric unit; half a molecule of
 C5H12 would give 21e].
;

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_pbad150611
_database_code_depnum_ccdc_archive 'CCDC 1469268'
_audit_update_record             
;
2016-03-17 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H124 Fe2 K2 N6 Si4'
_chemical_formula_sum            'C80 H124 Fe2 K2 N6 Si4'
_chemical_formula_weight         1472.10

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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                   11.0494(5)
_cell_length_b                   14.3909(7)
_cell_length_c                   28.2527(13)
_cell_angle_alpha                90
_cell_angle_beta                 108.870(2)
_cell_angle_gamma                90
_cell_volume                     4251.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6559
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.22

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.538
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6582
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42438
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.523
_diffrn_reflns_theta_max         28.052
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10281
_reflns_number_gt                6330
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0775P)²+3.9273P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10281
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1773
_refine_ls_wR_factor_gt          0.1527
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
C1 C 0.1152(3) 0.43042(19) 0.82617(11) 0.0229(6) Uani 1 1 d . . . . .
C2 C 0.0612(3) 0.5296(2) 0.75982(12) 0.0294(7) Uani 1 1 d . . . . .
H2 H 0.0112 0.5691 0.7339 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1857(3) 0.5104(2) 0.77031(12) 0.0297(7) Uani 1 1 d . . . . .
H3 H 0.2411 0.5337 0.7535 0.036 Uiso 1 1 calc R U . . .
C4 C -0.1097(3) 0.4855(2) 0.79545(11) 0.0236(6) Uani 1 1 d . . . . .
C5 C -0.1337(3) 0.5395(2) 0.83302(12) 0.0317(7) Uani 1 1 d . . . . .
C6 C -0.2591(4) 0.5444(3) 0.83261(15) 0.0414(9) Uani 1 1 d . . . . .
H6 H -0.2787 0.5795 0.8577 0.050 Uiso 1 1 calc R U . . .
C7 C -0.3569(4) 0.4992(3) 0.79633(15) 0.0429(9) Uani 1 1 d . . . . .
H7 H -0.4425 0.5042 0.7965 0.052 Uiso 1 1 calc R U . . .
C8 C -0.3301(3) 0.4472(3) 0.76033(14) 0.0378(8) Uani 1 1 d . . . . .
H8 H -0.3979 0.4165 0.7357 0.045 Uiso 1 1 calc R U . . .
C9 C -0.2055(3) 0.4384(2) 0.75904(12) 0.0300(7) Uani 1 1 d . . . . .
C10 C -0.0288(4) 0.5934(3) 0.87120(14) 0.0454(10) Uani 1 1 d . . . . .
H10 H 0.0538 0.5604 0.8756 0.055 Uiso 1 1 calc R U . . .
C11 C -0.0468(5) 0.5992(3) 0.92271(16) 0.0636(13) Uani 1 1 d . . . . .
H11A H -0.1200 0.6393 0.9206 0.095 Uiso 1 1 calc R U . . .
H11B H 0.0305 0.6252 0.9470 0.095 Uiso 1 1 calc R U . . .
H11C H -0.0623 0.5368 0.9334 0.095 Uiso 1 1 calc R U . . .
C12 C -0.0169(5) 0.6904(3) 0.85218(18) 0.0700(15) Uani 1 1 d . . . . .
H12A H -0.0042 0.6863 0.8195 0.105 Uiso 1 1 calc R U . . .
H12B H 0.0564 0.7221 0.8759 0.105 Uiso 1 1 calc R U . . .
H12C H -0.0951 0.7256 0.8489 0.105 Uiso 1 1 calc R U . . .
C13 C -0.1783(4) 0.3769(3) 0.71995(14) 0.0401(8) Uani 1 1 d . . . . .
H13 H -0.0844 0.3795 0.7252 0.048 Uiso 1 1 calc R U . . .
C14 C -0.2484(6) 0.4099(4) 0.66735(16) 0.0796(16) Uani 1 1 d . . . . .
H14A H -0.3408 0.4078 0.6614 0.119 Uiso 1 1 calc R U . . .
H14B H -0.2270 0.3694 0.6433 0.119 Uiso 1 1 calc R U . . .
H14C H -0.2227 0.4738 0.6633 0.119 Uiso 1 1 calc R U . . .
C15 C -0.2139(6) 0.2757(3) 0.7265(2) 0.0774(16) Uani 1 1 d . . . . .
H15A H -0.1651 0.2543 0.7602 0.116 Uiso 1 1 calc R U . . .
H15B H -0.1938 0.2365 0.7017 0.116 Uiso 1 1 calc R U . . .
H15C H -0.3056 0.2717 0.7218 0.116 Uiso 1 1 calc R U . . .
C16 C 0.3465(3) 0.4215(2) 0.83822(12) 0.0270(7) Uani 1 1 d . . . . .
C17 C 0.3953(3) 0.3401(2) 0.82379(13) 0.0343(8) Uani 1 1 d . . . . .
C18 C 0.5178(3) 0.3141(3) 0.85289(15) 0.0430(9) Uani 1 1 d . . . . .
H18 H 0.5545 0.2595 0.8444 0.052 Uiso 1 1 calc R U . . .
C19 C 0.5877(4) 0.3655(3) 0.89389(15) 0.0451(9) Uani 1 1 d . . . . .
H19 H 0.6705 0.3452 0.9136 0.054 Uiso 1 1 calc R U . . .
C20 C 0.5380(3) 0.4463(3) 0.90631(14) 0.0400(9) Uani 1 1 d . . . . .
H20 H 0.5874 0.4815 0.9343 0.048 Uiso 1 1 calc R U . . .
C21 C 0.4164(3) 0.4768(2) 0.87842(12) 0.0315(7) Uani 1 1 d . . . . .
C22 C 0.3203(4) 0.2832(3) 0.77843(15) 0.0444(9) Uani 1 1 d . . . . .
H22 H 0.2407 0.3184 0.7603 0.053 Uiso 1 1 calc R U . . .
C23 C 0.2812(6) 0.1908(4) 0.79330(19) 0.093(2) Uani 1 1 d . . . . .
H23A H 0.2442 0.1526 0.7634 0.139 Uiso 1 1 calc R U . . .
H23B H 0.2175 0.2001 0.8103 0.139 Uiso 1 1 calc R U . . .
H23C H 0.3563 0.1593 0.8160 0.139 Uiso 1 1 calc R U . . .
C24 C 0.3928(6) 0.2671(4) 0.74261(18) 0.090(2) Uani 1 1 d . . . . .
H24A H 0.4664 0.2268 0.7583 0.135 Uiso 1 1 calc R U . . .
H24B H 0.4228 0.3268 0.7339 0.135 Uiso 1 1 calc R U . . .
H24C H 0.3367 0.2373 0.7123 0.135 Uiso 1 1 calc R U . . .
C25 C 0.3656(4) 0.5677(2) 0.89152(13) 0.0389(8) Uani 1 1 d . . . . .
H25 H 0.2791 0.5777 0.8664 0.047 Uiso 1 1 calc R U . . .
C26 C 0.3479(5) 0.5632(3) 0.94290(16) 0.0570(11) Uani 1 1 d . . . . .
H26A H 0.2918 0.5109 0.9438 0.086 Uiso 1 1 calc R U . . .
H26B H 0.3092 0.6212 0.9492 0.086 Uiso 1 1 calc R U . . .
H26C H 0.4312 0.5546 0.9687 0.086 Uiso 1 1 calc R U . . .
C27 C 0.4486(5) 0.6492(3) 0.88709(19) 0.0615(12) Uani 1 1 d . . . . .
H27A H 0.5346 0.6417 0.9113 0.092 Uiso 1 1 calc R U . . .
H27B H 0.4109 0.7071 0.8940 0.092 Uiso 1 1 calc R U . . .
H27C H 0.4540 0.6512 0.8532 0.092 Uiso 1 1 calc R U . . .
C28 C 0.2142(4) 0.2839(3) 0.94781(14) 0.0466(10) Uani 1 1 d . . . . .
C29 C 0.1168(5) 0.3326(3) 0.95836(16) 0.0570(12) Uani 1 1 d . . . . .
H29 H 0.1368 0.3712 0.9872 0.068 Uiso 1 1 calc R U . . .
C30 C -0.0086(5) 0.3254(3) 0.92737(19) 0.0611(13) Uani 1 1 d . . . . .
H30 H -0.0736 0.3609 0.9342 0.073 Uiso 1 1 calc R U . . .
C31 C -0.0400(5) 0.2651(3) 0.88543(18) 0.0602(12) Uani 1 1 d . . . . .
H31 H -0.1261 0.2585 0.8643 0.072 Uiso 1 1 calc R U . . .
C32 C 0.0601(5) 0.2147(3) 0.87557(16) 0.0569(12) Uani 1 1 d . . . . .
H32 H 0.0407 0.1742 0.8476 0.068 Uiso 1 1 calc R U . . .
C33 C 0.1866(4) 0.2242(3) 0.90670(14) 0.0467(10) Uani 1 1 d . . . . .
H33 H 0.2531 0.1905 0.9000 0.056 Uiso 1 1 calc R U . . .
C34 C 0.3400(7) 0.2955(5) 0.9786(3) 0.121(3) Uani 1 1 d . . . . .
H34A H 0.3474 0.3535 0.9975 0.181 Uiso 1 1 calc R U . . .
H34B H 0.3964 0.2981 0.9581 0.181 Uiso 1 1 calc R U . . .
H34C H 0.3648 0.2431 1.0018 0.181 Uiso 1 1 calc R U . . .
C35 C 0.2917(4) -0.0148(3) 0.96548(16) 0.0549(11) Uani 1 1 d . . . . .
H35A H 0.2088 -0.0079 0.9392 0.082 Uiso 1 1 calc R U . . .
H35B H 0.3502 -0.0493 0.9522 0.082 Uiso 1 1 calc R U . . .
H35C H 0.3276 0.0468 0.9766 0.082 Uiso 1 1 calc R U . . .
C36 C 0.1926(4) -0.1941(3) 0.99274(17) 0.0545(11) Uani 1 1 d . . . . .
H36A H 0.1825 -0.2333 1.0196 0.082 Uiso 1 1 calc R U . . .
H36B H 0.2469 -0.2261 0.9765 0.082 Uiso 1 1 calc R U . . .
H36C H 0.1085 -0.1820 0.9681 0.082 Uiso 1 1 calc R U . . .
C37 C 0.4369(4) -0.1113(4) 1.05980(19) 0.0645(13) Uani 1 1 d . . . . .
H37A H 0.4853 -0.0545 1.0725 0.097 Uiso 1 1 calc R U . . .
H37B H 0.4790 -0.1460 1.0397 0.097 Uiso 1 1 calc R U . . .
H37C H 0.4335 -0.1498 1.0880 0.097 Uiso 1 1 calc R U . . .
C38 C 0.2875(6) 0.1534(4) 1.0982(2) 0.088(2) Uani 1 1 d . . . . .
H38A H 0.3606 0.1487 1.0859 0.132 Uiso 1 1 calc R U . . .
H38B H 0.3149 0.1824 1.1314 0.132 Uiso 1 1 calc R U . . .
H38C H 0.2206 0.1914 1.0751 0.132 Uiso 1 1 calc R U . . .
C39 C 0.0809(4) 0.0506(3) 1.12489(15) 0.0546(11) Uani 1 1 d . . . . .
H39A H 0.0150 0.0865 1.1000 0.082 Uiso 1 1 calc R U . . .
H39B H 0.1079 0.0844 1.1567 0.082 Uiso 1 1 calc R U . . .
H39C H 0.0460 -0.0100 1.1296 0.082 Uiso 1 1 calc R U . . .
C40 C 0.3431(5) -0.0258(4) 1.15745(16) 0.0733(15) Uani 1 1 d . . . . .
H40A H 0.3140 -0.0890 1.1610 0.110 Uiso 1 1 calc R U . . .
H40B H 0.3518 0.0095 1.1880 0.110 Uiso 1 1 calc R U . . .
H40C H 0.4260 -0.0286 1.1518 0.110 Uiso 1 1 calc R U . . .
N1 N 0.0188(2) 0.48110(17) 0.79388(9) 0.0227(5) Uani 1 1 d . . . . .
N2 N 0.2177(2) 0.44986(17) 0.81062(9) 0.0237(5) Uani 1 1 d . . . . .
N3 N 0.1807(3) -0.02288(19) 1.04806(10) 0.0323(6) Uani 1 1 d . . . . .
Si1 Si 0.26993(10) -0.08005(7) 1.02003(4) 0.0358(2) Uani 1 1 d . . . . .
Si2 Si 0.22251(10) 0.03322(7) 1.10253(4) 0.0383(3) Uani 1 1 d . . . . .
K1 K 0.05110(8) 0.11080(5) 0.97416(3) 0.03676(19) Uani 1 1 d . . . . .
Fe1 Fe 0.11032(6) 0.35804(4) 0.88546(2) 0.04150(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.368(4) . ?
C1 N2 1.370(4) . ?
C1 Fe1 1.988(3) . ?
C2 C3 1.339(5) . ?
C2 N1 1.387(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C9 1.391(4) . ?
C4 C5 1.407(4) . ?
C4 N1 1.436(4) . ?
C5 C6 1.384(5) . ?
C5 C10 1.517(5) . ?
C6 C7 1.387(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.370(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.394(5) . ?
C8 H8 0.9500 . ?
C9 C13 1.519(5) . ?
C10 C12 1.517(6) . ?
C10 C11 1.533(6) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.513(6) . ?
C13 C15 1.536(6) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.398(5) . ?
C16 C17 1.404(5) . ?
C16 N2 1.442(4) . ?
C17 C18 1.389(5) . ?
C17 C22 1.521(5) . ?
C18 C19 1.381(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.391(5) . ?
C20 H20 0.9500 . ?
C21 C25 1.515(5) . ?
C22 C24 1.498(6) . ?
C22 C23 1.499(6) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.519(5) . ?
C25 C26 1.528(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C34 1.390(8) . ?
C28 C29 1.395(6) . ?
C28 C33 1.397(6) . ?
C28 Fe1 2.061(4) . ?
C28 K1 3.298(4) . ?
C29 C30 1.382(7) . ?
C29 Fe1 2.070(4) . ?
C29 K1 3.336(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.419(7) . ?
C30 Fe1 2.087(4) . ?
C30 K1 3.341(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.423(7) . ?
C31 Fe1 2.132(4) . ?
C31 K1 3.255(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.397(6) . ?
C32 Fe1 2.131(4) . ?
C32 K1 3.191(4) . ?
C32 H32 0.9500 . ?
C33 Fe1 2.110(4) . ?
C33 K1 3.222(4) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 Si1 1.886(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 Si1 1.895(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 Si1 1.878(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 Si2 1.892(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 Si2 1.885(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 Si2 1.889(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N3 Si2 1.665(3) . ?
N3 Si1 1.668(3) . ?
N3 K1 2.742(3) 3_557 ?
N3 K1 2.860(3) . ?
Si1 K1 3.6115(13) . ?
Si1 K1 3.6306(13) 3_557 ?
Si2 K1 3.6802(13) . ?
Si2 K1 3.7274(13) 3_557 ?
K1 N3 2.742(3) 3_557 ?
K1 C36 3.346(4) 3_557 ?
K1 Si1 3.6306(13) 3_557 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 102.9(2) . . ?
N1 C1 Fe1 127.9(2) . . ?
N2 C1 Fe1 128.9(2) . . ?
C3 C2 N1 107.2(3) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 106.4(3) . . ?
C2 C3 H3 126.8 . . ?
N2 C3 H3 126.8 . . ?
C9 C4 C5 122.8(3) . . ?
C9 C4 N1 118.6(3) . . ?
C5 C4 N1 118.5(3) . . ?
C6 C5 C4 117.0(3) . . ?
C6 C5 C10 120.8(3) . . ?
C4 C5 C10 122.1(3) . . ?
C5 C6 C7 121.4(3) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 121.4(3) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C4 C9 C8 117.3(3) . . ?
C4 C9 C13 122.6(3) . . ?
C8 C9 C13 120.1(3) . . ?
C12 C10 C5 110.7(3) . . ?
C12 C10 C11 109.8(3) . . ?
C5 C10 C11 113.5(3) . . ?
C12 C10 H10 107.5 . . ?
C5 C10 H10 107.5 . . ?
C11 C10 H10 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C9 111.9(3) . . ?
C14 C13 C15 110.2(4) . . ?
C9 C13 C15 110.2(3) . . ?
C14 C13 H13 108.1 . . ?
C9 C13 H13 108.1 . . ?
C15 C13 H13 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 123.2(3) . . ?
C21 C16 N2 117.8(3) . . ?
C17 C16 N2 118.9(3) . . ?
C18 C17 C16 116.5(3) . . ?
C18 C17 C22 121.0(3) . . ?
C16 C17 C22 122.5(3) . . ?
C19 C18 C17 121.7(3) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 120.9(3) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C16 117.3(3) . . ?
C20 C21 C25 120.1(3) . . ?
C16 C21 C25 122.6(3) . . ?
C24 C22 C23 108.6(4) . . ?
C24 C22 C17 112.8(3) . . ?
C23 C22 C17 111.7(4) . . ?
C24 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C17 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 C27 111.4(3) . . ?
C21 C25 C26 111.5(3) . . ?
C27 C25 C26 112.2(3) . . ?
C21 C25 H25 107.1 . . ?
C27 C25 H25 107.1 . . ?
C26 C25 H25 107.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C34 C28 C29 119.4(5) . . ?
C34 C28 C33 119.9(5) . . ?
C29 C28 C33 120.7(4) . . ?
C34 C28 Fe1 129.8(4) . . ?
C29 C28 Fe1 70.6(2) . . ?
C33 C28 Fe1 72.3(2) . . ?
C34 C28 K1 117.2(3) . . ?
C29 C28 K1 79.4(2) . . ?
C33 C28 K1 74.6(2) . . ?
Fe1 C28 K1 112.94(16) . . ?
C30 C29 C28 120.8(4) . . ?
C30 C29 Fe1 71.2(2) . . ?
C28 C29 Fe1 69.9(2) . . ?
C30 C29 K1 78.3(3) . . ?
C28 C29 K1 76.4(2) . . ?
Fe1 C29 K1 111.30(17) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
Fe1 C29 H29 132.3 . . ?
K1 C29 H29 116.4 . . ?
C29 C30 C31 119.9(4) . . ?
C29 C30 Fe1 69.9(2) . . ?
C31 C30 Fe1 72.1(2) . . ?
C29 C30 K1 77.8(3) . . ?
C31 C30 K1 74.2(2) . . ?
Fe1 C30 K1 110.64(18) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
Fe1 C30 H30 130.5 . . ?
K1 C30 H30 118.8 . . ?
C30 C31 C32 118.7(5) . . ?
C30 C31 Fe1 68.6(3) . . ?
C32 C31 Fe1 70.5(2) . . ?
C30 C31 K1 81.0(3) . . ?
C32 C31 K1 74.7(2) . . ?
Fe1 C31 K1 112.39(19) . . ?
C30 C31 H31 120.7 . . ?
C32 C31 H31 120.7 . . ?
Fe1 C31 H31 133.2 . . ?
K1 C31 H31 114.3 . . ?
C33 C32 C31 120.6(4) . . ?
C33 C32 Fe1 70.0(2) . . ?
C31 C32 Fe1 70.5(2) . . ?
C33 C32 K1 78.7(2) . . ?
C31 C32 K1 79.8(2) . . ?
Fe1 C32 K1 114.80(16) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
Fe1 C32 H32 133.0 . . ?
K1 C32 H32 112.2 . . ?
C32 C33 C28 119.3(4) . . ?
C32 C33 Fe1 71.6(2) . . ?
C28 C33 Fe1 68.6(2) . . ?
C32 C33 K1 76.2(2) . . ?
C28 C33 K1 80.7(2) . . ?
Fe1 C33 K1 114.28(16) . . ?
C32 C33 H33 120.4 . . ?
C28 C33 H33 120.4 . . ?
Fe1 C33 H33 132.4 . . ?
K1 C33 H33 113.4 . . ?
C28 C34 H34A 109.5 . . ?
C28 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C28 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si1 C35 H35A 109.5 . . ?
Si1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
Si1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si1 C37 H37A 109.5 . . ?
Si1 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si1 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si2 C38 H38A 109.5 . . ?
Si2 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si2 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si2 C39 H39A 109.5 . . ?
Si2 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Si2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Si2 C40 H40A 109.5 . . ?
Si2 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
Si2 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C1 N1 C2 111.5(3) . . ?
C1 N1 C4 124.6(2) . . ?
C2 N1 C4 123.9(2) . . ?
C1 N2 C3 111.9(2) . . ?
C1 N2 C16 122.8(2) . . ?
C3 N2 C16 124.6(3) . . ?
Si2 N3 Si1 130.42(18) . . ?
Si2 N3 K1 113.24(14) . 3_557 ?
Si1 N3 K1 108.39(13) . 3_557 ?
Si2 N3 K1 105.79(13) . . ?
Si1 N3 K1 102.62(12) . . ?
K1 N3 K1 86.16(8) 3_557 . ?
N3 Si1 C37 116.8(2) . . ?
N3 Si1 C35 113.19(17) . . ?
C37 Si1 C35 104.4(2) . . ?
N3 Si1 C36 111.27(17) . . ?
C37 Si1 C36 105.2(2) . . ?
C35 Si1 C36 105.0(2) . . ?
N3 Si1 K1 50.60(10) . . ?
C37 Si1 K1 144.19(17) . . ?
C35 Si1 K1 64.89(14) . . ?
C36 Si1 K1 110.58(14) . . ?
N3 Si1 K1 45.77(10) . 3_557 ?
C37 Si1 K1 136.77(16) . 3_557 ?
C35 Si1 K1 118.86(15) . 3_557 ?
C36 Si1 K1 66.08(13) . 3_557 ?
K1 Si1 K1 63.79(3) . 3_557 ?
N3 Si2 C39 111.23(18) . . ?
N3 Si2 C40 116.9(2) . . ?
C39 Si2 C40 103.1(2) . . ?
N3 Si2 C38 112.42(19) . . ?
C39 Si2 C38 105.9(3) . . ?
C40 Si2 C38 106.4(3) . . ?
N3 Si2 K1 48.39(10) . . ?
C39 Si2 K1 94.10(14) . . ?
C40 Si2 K1 161.35(16) . . ?
C38 Si2 K1 75.18(18) . . ?
C39 Si2 K1 70.33(14) . 3_557 ?
C40 Si2 K1 116.84(19) . 3_557 ?
C38 Si2 K1 136.4(2) . 3_557 ?
K1 Si2 K1 62.20(2) . 3_557 ?
N3 K1 N3 93.84(8) 3_557 . ?
N3 K1 C32 107.87(11) 3_557 . ?
N3 K1 C32 143.40(11) . . ?
N3 K1 C33 132.58(10) 3_557 . ?
N3 K1 C33 123.63(10) . . ?
C32 K1 C33 25.15(11) . . ?
N3 K1 C31 96.04(10) 3_557 . ?
N3 K1 C31 168.03(11) . . ?
C32 K1 C31 25.48(12) . . ?
C33 K1 C31 44.43(11) . . ?
N3 K1 C28 146.64(9) 3_557 . ?
N3 K1 C28 119.46(10) . . ?
C32 K1 C28 43.57(11) . . ?
C33 K1 C28 24.71(10) . . ?
C31 K1 C28 50.67(11) . . ?
N3 K1 C29 129.69(11) 3_557 . ?
N3 K1 C29 131.48(11) . . ?
C32 K1 C29 50.60(11) . . ?
C33 K1 C29 43.39(10) . . ?
C31 K1 C29 43.16(12) . . ?
C28 K1 C29 24.27(11) . . ?
N3 K1 C30 106.61(11) 3_557 . ?
N3 K1 C30 154.04(12) . . ?
C32 K1 C30 43.88(12) . . ?
C33 K1 C30 50.77(11) . . ?
C31 K1 C30 24.80(12) . . ?
C28 K1 C30 42.65(12) . . ?
C29 K1 C30 23.90(12) . . ?
N3 K1 C36 56.81(9) 3_557 3_557 ?
N3 K1 C36 107.19(10) . 3_557 ?
C32 K1 C36 109.34(12) . 3_557 ?
C33 K1 C36 123.62(11) . 3_557 ?
C31 K1 C36 83.95(12) . 3_557 ?
C28 K1 C36 109.90(11) . 3_557 ?
C29 K1 C36 85.64(11) . 3_557 ?
C30 K1 C36 72.87(11) . 3_557 ?
N3 K1 Si1 101.46(6) 3_557 . ?
N3 K1 Si1 26.78(6) . . ?
C32 K1 Si1 117.59(10) . . ?
C33 K1 Si1 102.25(8) . . ?
C31 K1 Si1 143.07(10) . . ?
C28 K1 Si1 107.71(8) . . ?
C29 K1 Si1 128.79(10) . . ?
C30 K1 Si1 150.31(9) . . ?
C36 K1 Si1 132.72(8) 3_557 . ?
N3 K1 Si1 25.84(6) 3_557 3_557 ?
N3 K1 Si1 98.68(6) . 3_557 ?
C32 K1 Si1 113.78(10) . 3_557 ?
C33 K1 Si1 137.40(8) . 3_557 ?
C31 K1 Si1 93.14(9) . 3_557 ?
C28 K1 Si1 135.68(8) . 3_557 ?
C29 K1 Si1 112.38(9) . 3_557 ?
C30 K1 Si1 93.44(9) . 3_557 ?
C36 K1 Si1 31.19(7) 3_557 3_557 ?
Si1 K1 Si1 116.21(3) . 3_557 ?
N3 K1 Si2 103.34(6) 3_557 . ?
N3 K1 Si2 25.81(6) . . ?
C32 K1 Si2 148.31(10) . . ?
C33 K1 Si2 123.17(8) . . ?
C31 K1 Si2 153.93(9) . . ?
C28 K1 Si2 107.88(7) . . ?
C29 K1 Si2 110.94(9) . . ?
C30 K1 Si2 130.04(10) . . ?
C36 K1 Si2 92.15(8) 3_557 . ?
Si1 K1 Si2 49.02(3) . . ?
Si1 K1 Si2 96.74(3) 3_557 . ?
C1 Fe1 C28 146.26(15) . . ?
C1 Fe1 C29 158.32(15) . . ?
C28 Fe1 C29 39.47(17) . . ?
C1 Fe1 C30 142.15(17) . . ?
C28 Fe1 C30 71.19(19) . . ?
C29 Fe1 C30 38.84(19) . . ?
C1 Fe1 C33 126.91(14) . . ?
C28 Fe1 C33 39.11(16) . . ?
C29 Fe1 C33 70.96(16) . . ?
C30 Fe1 C33 84.28(17) . . ?
C1 Fe1 C32 118.27(14) . . ?
C28 Fe1 C32 70.17(17) . . ?
C29 Fe1 C32 83.29(16) . . ?
C30 Fe1 C32 70.84(18) . . ?
C33 Fe1 C32 38.45(17) . . ?
C1 Fe1 C31 124.18(16) . . ?
C28 Fe1 C31 83.93(17) . . ?
C29 Fe1 C31 70.48(19) . . ?
C30 Fe1 C31 39.29(19) . . ?
C33 Fe1 C31 70.54(18) . . ?
C32 Fe1 C31 39.00(18) . . ?

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
N1 C2 C3 N2 0.3(4) . . . . ?
C9 C4 C5 C6 -0.1(5) . . . . ?
N1 C4 C5 C6 178.2(3) . . . . ?
C9 C4 C5 C10 -177.6(3) . . . . ?
N1 C4 C5 C10 0.7(5) . . . . ?
C4 C5 C6 C7 -0.8(5) . . . . ?
C10 C5 C6 C7 176.7(3) . . . . ?
C5 C6 C7 C8 0.9(6) . . . . ?
C6 C7 C8 C9 -0.1(6) . . . . ?
C5 C4 C9 C8 0.9(5) . . . . ?
N1 C4 C9 C8 -177.4(3) . . . . ?
C5 C4 C9 C13 -177.3(3) . . . . ?
N1 C4 C9 C13 4.5(4) . . . . ?
C7 C8 C9 C4 -0.8(5) . . . . ?
C7 C8 C9 C13 177.4(3) . . . . ?
C6 C5 C10 C12 -87.9(4) . . . . ?
C4 C5 C10 C12 89.5(4) . . . . ?
C6 C5 C10 C11 36.2(5) . . . . ?
C4 C5 C10 C11 -146.5(4) . . . . ?
C4 C9 C13 C14 -120.6(4) . . . . ?
C8 C9 C13 C14 61.3(5) . . . . ?
C4 C9 C13 C15 116.3(4) . . . . ?
C8 C9 C13 C15 -61.8(5) . . . . ?
C21 C16 C17 C18 2.3(5) . . . . ?
N2 C16 C17 C18 -177.5(3) . . . . ?
C21 C16 C17 C22 -177.0(3) . . . . ?
N2 C16 C17 C22 3.3(5) . . . . ?
C16 C17 C18 C19 0.1(5) . . . . ?
C22 C17 C18 C19 179.3(4) . . . . ?
C17 C18 C19 C20 -1.6(6) . . . . ?
C18 C19 C20 C21 0.9(6) . . . . ?
C19 C20 C21 C16 1.3(5) . . . . ?
C19 C20 C21 C25 -177.7(3) . . . . ?
C17 C16 C21 C20 -3.0(5) . . . . ?
N2 C16 C21 C20 176.8(3) . . . . ?
C17 C16 C21 C25 176.0(3) . . . . ?
N2 C16 C21 C25 -4.2(5) . . . . ?
C18 C17 C22 C24 -53.2(5) . . . . ?
C16 C17 C22 C24 126.0(4) . . . . ?
C18 C17 C22 C23 69.3(5) . . . . ?
C16 C17 C22 C23 -111.5(4) . . . . ?
C20 C21 C25 C27 61.0(4) . . . . ?
C16 C21 C25 C27 -117.9(4) . . . . ?
C20 C21 C25 C26 -65.1(4) . . . . ?
C16 C21 C25 C26 116.0(4) . . . . ?
C34 C28 C29 C30 177.4(5) . . . . ?
C33 C28 C29 C30 -2.4(6) . . . . ?
Fe1 C28 C29 C30 51.9(3) . . . . ?
K1 C28 C29 C30 -67.2(4) . . . . ?
C34 C28 C29 Fe1 125.5(5) . . . . ?
C33 C28 C29 Fe1 -54.3(3) . . . . ?
K1 C28 C29 Fe1 -119.12(14) . . . . ?
C34 C28 C29 K1 -115.4(4) . . . . ?
C33 C28 C29 K1 64.8(3) . . . . ?
Fe1 C28 C29 K1 119.12(14) . . . . ?
C28 C29 C30 C31 2.6(6) . . . . ?
Fe1 C29 C30 C31 54.0(3) . . . . ?
K1 C29 C30 C31 -63.6(3) . . . . ?
C28 C29 C30 Fe1 -51.4(3) . . . . ?
K1 C29 C30 Fe1 -117.56(13) . . . . ?
C28 C29 C30 K1 66.2(3) . . . . ?
Fe1 C29 C30 K1 117.56(13) . . . . ?
C29 C30 C31 C32 -1.5(6) . . . . ?
Fe1 C30 C31 C32 51.4(3) . . . . ?
K1 C30 C31 C32 -67.0(3) . . . . ?
C29 C30 C31 Fe1 -53.0(3) . . . . ?
K1 C30 C31 Fe1 -118.45(15) . . . . ?
C29 C30 C31 K1 65.5(4) . . . . ?
Fe1 C30 C31 K1 118.45(15) . . . . ?
C30 C31 C32 C33 0.2(6) . . . . ?
Fe1 C31 C32 C33 50.8(3) . . . . ?
K1 C31 C32 C33 -70.2(3) . . . . ?
C30 C31 C32 Fe1 -50.6(3) . . . . ?
K1 C31 C32 Fe1 -121.05(14) . . . . ?
C30 C31 C32 K1 70.4(3) . . . . ?
Fe1 C31 C32 K1 121.05(14) . . . . ?
C31 C32 C33 C28 0.0(6) . . . . ?
Fe1 C32 C33 C28 51.1(3) . . . . ?
K1 C32 C33 C28 -70.8(3) . . . . ?
C31 C32 C33 Fe1 -51.1(3) . . . . ?
K1 C32 C33 Fe1 -121.89(12) . . . . ?
C31 C32 C33 K1 70.8(3) . . . . ?
Fe1 C32 C33 K1 121.89(12) . . . . ?
C34 C28 C33 C32 -178.8(4) . . . . ?
C29 C28 C33 C32 1.0(5) . . . . ?
Fe1 C28 C33 C32 -52.5(3) . . . . ?
K1 C28 C33 C32 68.3(3) . . . . ?
C34 C28 C33 Fe1 -126.3(5) . . . . ?
C29 C28 C33 Fe1 53.5(3) . . . . ?
K1 C28 C33 Fe1 120.80(13) . . . . ?
C34 C28 C33 K1 112.9(4) . . . . ?
C29 C28 C33 K1 -67.3(3) . . . . ?
Fe1 C28 C33 K1 -120.80(13) . . . . ?
N2 C1 N1 C2 0.1(3) . . . . ?
Fe1 C1 N1 C2 174.1(2) . . . . ?
N2 C1 N1 C4 -178.7(3) . . . . ?
Fe1 C1 N1 C4 -4.6(4) . . . . ?
C3 C2 N1 C1 -0.2(4) . . . . ?
C3 C2 N1 C4 178.5(3) . . . . ?
C9 C4 N1 C1 -106.4(3) . . . . ?
C5 C4 N1 C1 75.3(4) . . . . ?
C9 C4 N1 C2 75.1(4) . . . . ?
C5 C4 N1 C2 -103.3(4) . . . . ?
N1 C1 N2 C3 0.1(3) . . . . ?
Fe1 C1 N2 C3 -173.8(2) . . . . ?
N1 C1 N2 C16 171.3(3) . . . . ?
Fe1 C1 N2 C16 -2.7(4) . . . . ?
C2 C3 N2 C1 -0.3(4) . . . . ?
C2 C3 N2 C16 -171.2(3) . . . . ?
C21 C16 N2 C1 -82.3(4) . . . . ?
C17 C16 N2 C1 97.5(4) . . . . ?
C21 C16 N2 C3 87.7(4) . . . . ?
C17 C16 N2 C3 -92.5(4) . . . . ?
Si2 N3 Si1 C37 15.7(3) . . . . ?
K1 N3 Si1 C37 -130.35(19) 3_557 . . . ?
K1 N3 Si1 C37 139.53(19) . . . . ?
Si2 N3 Si1 C35 -105.6(3) . . . . ?
K1 N3 Si1 C35 108.41(19) 3_557 . . . ?
K1 N3 Si1 C35 18.3(2) . . . . ?
Si2 N3 Si1 C36 136.5(2) . . . . ?
K1 N3 Si1 C36 -9.6(2) 3_557 . . . ?
K1 N3 Si1 C36 -99.69(18) . . . . ?
Si2 N3 Si1 K1 -123.9(3) . . . . ?
K1 N3 Si1 K1 90.12(12) 3_557 . . . ?
Si2 N3 Si1 K1 146.0(3) . . . 3_557 ?
K1 N3 Si1 K1 -90.12(12) . . . 3_557 ?
Si1 N3 Si2 C39 -161.4(2) . . . . ?
K1 N3 Si2 C39 -16.7(2) 3_557 . . . ?
K1 N3 Si2 C39 75.97(19) . . . . ?
Si1 N3 Si2 C40 -43.4(3) . . . . ?
K1 N3 Si2 C40 101.3(2) 3_557 . . . ?
K1 N3 Si2 C40 -166.1(2) . . . . ?
Si1 N3 Si2 C38 80.1(3) . . . . ?
K1 N3 Si2 C38 -135.2(3) 3_557 . . . ?
K1 N3 Si2 C38 -42.6(3) . . . . ?
Si1 N3 Si2 K1 122.6(3) . . . . ?
K1 N3 Si2 K1 -92.62(14) 3_557 . . . ?
Si1 N3 Si2 K1 -144.8(3) . . . 3_557 ?
K1 N3 Si2 K1 92.62(14) . . . 3_557 ?

_refine_diff_density_max         1.951
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-4

