# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_ambient_before
_database_code_depnum_ccdc_archive 'CCDC 2208665'
loop_
_audit_author_name
_audit_author_address
'Andrea Cornia'
;University of Modena and Reggio Emilia
Italy
;
_audit_update_record             
;
2022-09-21 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_date             2022-09-17
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Cr5(C15H11N5)4(NCS)2]'
_chemical_formula_moiety         'C62 H44 Cr5 N22 S2'
_chemical_formula_sum            'C62 H44 Cr5 N22 S2'
_chemical_formula_weight         1421.31

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'
Cr Cr 0.3209 0.6236 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   15.2547(4)
_cell_length_b                   26.2195(8)
_cell_length_c                   15.2032(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.0121(16)
_cell_angle_gamma                90
_cell_volume                     6080.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    292.3
_cell_measurement_reflns_used    3444
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      26.32

_exptl_special_details           
;
Crystal mounted with low temperature epoxy resin to a graphite 
fibre to enable conduction cooling inside a vacuum chamber.
;
_exptl_crystal_preparation       
'Et2O vapour diffusion into a CH2Cl2 solution,Magnetic properties'
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.996
_shelx_estimated_absorpt_T_min   0.703
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.421354
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_process_details   
;
TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
Final HKLF 4 output contains 28485 reflections, Rint = 0.0815
(11988 with I > 3sig(I), Rint = 0.0758)
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      292.3
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'rotating anode'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0

_diffrn_reflns_number            5214
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.544
_diffrn_reflns_theta_max         26.382
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measured_fraction_theta_full 0.882
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_Laue_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_point_group_measured_fraction_full 0.882
_reflns_number_total             5214
_reflns_number_gt                3762
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WINGX publication routines v2020.2 (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0786P)²+7.1640P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5214
_refine_ls_number_parameters     417
_refine_ls_number_restraints     466
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1585
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

_refine_special_details          
;Refined as a 2-component twin.
There is a minor instability in the displacement 
parameters of 1 N atom that limits the reduction in shift 
over esd. The model does not significantly change if 
this atom is refined isotropically, but for consistency it 
has been modelled as anisotropic with a small damping
factor on the least squares minimisation.
1. Twinned data refinement with scales 0.558(3) and 0.442(3)
2. Uiso(H) fixed at 1.2 Ueq(C) for all C(H) groups
3. Rigid body (RIGU) restraints for all non-hydrogen atoms with sigma 
   for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Aromatic/amide H refined with riding coordinates:
   C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
   C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), 
   C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),Twin
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.558(3)
2 0.442(3)

_vrf_PLAT029_ambient_before      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.882 Why?
RESPONSE: The sample was measured inside a closed cycle refrigerator
with limited access to reflection geometries. The data were collected 
using a single axis rotation.
;

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
Cr1 Cr 0.500000 0.57558(3) 0.250000 0.0386(2) Uani 1 2 d S T P . .
Cr2 Cr 0.500000 0.66787(3) 0.250000 0.0387(2) Uani 1 2 d S T P . .
Cr3 Cr 0.500000 0.74773(3) 0.250000 0.0343(2) Uani 1 2 d S T P . .
Cr4 Cr 0.500000 0.83928(3) 0.250000 0.0376(2) Uani 1 2 d S T P . .
Cr5 Cr 0.500000 0.92144(3) 0.250000 0.0370(2) Uani 1 2 d S T P . .
S1 S 0.500000 0.38568(7) 0.250000 0.0928(8) Uani 1 2 d S T P . .
S2 S 0.500000 1.11463(7) 0.250000 0.0923(8) Uani 1 2 d S T P . .
N1 N 0.5684(3) 0.58312(19) 0.1294(3) 0.0362(10) Uani 1 1 d . . . . .
N2 N 0.6030(2) 0.66646(12) 0.1662(2) 0.0351(8) Uani 1 1 d . . . . .
N3 N 0.6261(5) 0.75012(10) 0.2034(5) 0.0299(16) Uani 1 1 d . . . . .
N4 N 0.63306(19) 0.83410(12) 0.2471(2) 0.0318(8) Uani 1 1 d . . . . .
N5 N 0.6318(3) 0.9185(2) 0.2889(3) 0.0353(11) Uani 1 1 d . . . . .
N6 N 0.6196(3) 0.5838(2) 0.3171(3) 0.0380(11) Uani 1 1 d . . . . .
N7 N 0.5829(2) 0.66613(12) 0.3541(2) 0.0348(8) Uani 1 1 d . . . . .
N8 N 0.5467(5) 0.75018(10) 0.3775(4) 0.0285(15) Uani 1 1 d . . . . .
N9 N 0.5025(2) 0.83406(12) 0.3836(2) 0.0326(8) Uani 1 1 d . . . . .
N10 N 0.4622(3) 0.91870(19) 0.3819(3) 0.0335(10) Uani 1 1 d . . . . .
N11 N 0.500000 0.49109(19) 0.250000 0.0518(12) Uani 1 2 d S T P . .
N12 N 0.500000 1.0093(2) 0.250000 0.0510(12) Uani 1 2 d S T P . .
C1 C 0.5687(5) 0.5452(3) 0.0720(5) 0.0438(16) Uani 1 1 d . . . . .
H1 H 0.539839 0.515358 0.088143 0.053 Uiso 1 1 calc R U . . .
C2 C 0.6073(6) 0.5460(3) -0.0080(5) 0.0567(19) Uani 1 1 d . . . . .
H2 H 0.606883 0.517450 -0.044222 0.068 Uiso 1 1 calc R U . . .
C3 C 0.6470(5) 0.5905(3) -0.0339(5) 0.065(2) Uani 1 1 d . . . . .
H3 H 0.672817 0.592973 -0.089157 0.078 Uiso 1 1 calc R U . . .
C4 C 0.6484(3) 0.63123(19) 0.0224(3) 0.0543(13) Uani 1 1 d . . . . .
H4 H 0.675241 0.661502 0.005421 0.065 Uiso 1 1 calc R U . . .
C5 C 0.6092(3) 0.62742(17) 0.1063(3) 0.0377(9) Uani 1 1 d . . . . .
C6 C 0.6606(3) 0.70684(18) 0.1666(3) 0.0367(11) Uani 1 1 d . . . . .
C7 C 0.7477(4) 0.7055(2) 0.1396(4) 0.0568(18) Uani 1 1 d . . . . .
H7 H 0.772054 0.675494 0.118251 0.068 Uiso 1 1 calc R U . . .
C8 C 0.7978(7) 0.74968(16) 0.1450(8) 0.066(3) Uani 1 1 d . . . . .
H8 H 0.855937 0.749425 0.126477 0.079 Uiso 1 1 calc R U . . .
C9 C 0.7615(4) 0.7936(3) 0.1777(4) 0.0523(17) Uani 1 1 d . . . . .
H9 H 0.793717 0.823730 0.177989 0.063 Uiso 1 1 calc R U . . .
C10 C 0.6760(3) 0.79315(18) 0.2105(3) 0.0333(10) Uani 1 1 d . . . . .
C11 C 0.6772(2) 0.87399(15) 0.2857(3) 0.0322(9) Uani 1 1 d . . . . .
C12 C 0.7607(3) 0.87106(18) 0.3248(3) 0.0458(11) Uani 1 1 d . . . . .
H12 H 0.791126 0.840327 0.324808 0.055 Uiso 1 1 calc R U . . .
C13 C 0.7973(4) 0.9134(3) 0.3630(4) 0.0516(16) Uani 1 1 d . . . . .
H13 H 0.852301 0.911349 0.389134 0.062 Uiso 1 1 calc R U . . .
C14 C 0.7521(5) 0.9593(3) 0.3626(5) 0.0478(16) Uani 1 1 d . . . . .
H14 H 0.776830 0.988504 0.387002 0.057 Uiso 1 1 calc R U . . .
C15 C 0.6699(4) 0.9609(3) 0.3253(5) 0.0407(14) Uani 1 1 d . . . . .
H15 H 0.639332 0.991592 0.324799 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6774(5) 0.5437(3) 0.3126(5) 0.0510(18) Uani 1 1 d . . . . .
H16 H 0.660615 0.513851 0.284275 0.061 Uiso 1 1 calc R U . . .
C17 C 0.7592(5) 0.5471(3) 0.3489(6) 0.072(3) Uani 1 1 d . . . . .
H17 H 0.797691 0.519642 0.345275 0.086 Uiso 1 1 calc R U . . .
C18 C 0.7843(5) 0.5916(3) 0.3911(5) 0.070(2) Uani 1 1 d . . . . .
H18 H 0.839952 0.594208 0.415589 0.084 Uiso 1 1 calc R U . . .
C19 C 0.7277(3) 0.6315(2) 0.3967(4) 0.0575(14) Uani 1 1 d . . . . .
H19 H 0.744224 0.661286 0.425342 0.069 Uiso 1 1 calc R U . . .
C20 C 0.6432(3) 0.62720(17) 0.3586(3) 0.0381(10) Uani 1 1 d . . . . .
C21 C 0.5830(3) 0.70655(18) 0.4114(3) 0.0374(11) Uani 1 1 d . . . . .
C22 C 0.6102(4) 0.7062(3) 0.4992(4) 0.0601(19) Uani 1 1 d . . . . .
H22 H 0.631054 0.676274 0.524569 0.072 Uiso 1 1 calc R U . . .
C23 C 0.6062(7) 0.74967(17) 0.5473(6) 0.063(3) Uani 1 1 d . . . . .
H23 H 0.627845 0.749708 0.604493 0.076 Uiso 1 1 calc R U . . .
C24 C 0.5706(4) 0.7938(2) 0.5134(4) 0.0504(16) Uani 1 1 d . . . . .
H24 H 0.567828 0.823326 0.547200 0.061 Uiso 1 1 calc R U . . .
C25 C 0.5387(3) 0.79327(18) 0.4269(3) 0.0345(10) Uani 1 1 d . . . . .
C26 C 0.4642(3) 0.87401(16) 0.4276(3) 0.0345(9) Uani 1 1 d . . . . .
C27 C 0.4232(3) 0.87130(18) 0.5110(3) 0.0486(12) Uani 1 1 d . . . . .
H27 H 0.422098 0.840616 0.541694 0.058 Uiso 1 1 calc R U . . .
C28 C 0.3854(4) 0.9135(3) 0.5462(4) 0.0551(17) Uani 1 1 d . . . . .
H28 H 0.358087 0.911779 0.600808 0.066 Uiso 1 1 calc R U . . .
C29 C 0.3876(6) 0.9586(3) 0.5006(5) 0.0587(19) Uani 1 1 d . . . . .
H29 H 0.363620 0.988243 0.524064 0.070 Uiso 1 1 calc R U . . .
C30 C 0.4256(5) 0.9585(3) 0.4212(5) 0.0454(16) Uani 1 1 d . . . . .
H30 H 0.426386 0.989226 0.390666 0.055 Uiso 1 1 calc R U . . .
C31 C 0.500000 0.4475(3) 0.250000 0.0520(14) Uani 1 2 d S T P . .
C32 C 0.500000 1.0529(3) 0.250000 0.0521(15) Uani 1 2 d S T P . .


_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
Cr1 N6 2.101(5) . ?
Cr1 N6 2.101(5) 2_655 ?
Cr1 N1 2.120(5) 2_655 ?
Cr1 N1 2.120(5) . ?
Cr1 N11 2.215(5) . ?
Cr1 Cr2 2.4198(12) . ?
Cr2 N2 2.024(3) 2_655 ?
Cr2 N2 2.024(3) . ?
Cr2 N7 2.025(3) 2_655 ?
Cr2 N7 2.025(3) . ?
Cr2 Cr3 2.0939(13) . ?
Cr3 N3 2.051(7) . ?
Cr3 N3 2.051(7) 2_655 ?
Cr3 N8 2.066(6) . ?
Cr3 N8 2.066(6) 2_655 ?
Cr3 Cr4 2.4005(13) . ?
Cr4 N4 2.035(3) 2_655 ?
Cr4 N4 2.035(3) . ?
Cr4 N9 2.036(3) 2_655 ?
Cr4 N9 2.036(3) . ?
Cr4 Cr5 2.1541(12) . ?
Cr5 N10 2.088(5) 2_655 ?
Cr5 N10 2.088(5) . ?
Cr5 N5 2.097(5) 2_655 ?
Cr5 N5 2.097(5) . ?
Cr5 N12 2.304(5) . ?
S1 C31 1.620(7) . ?
S2 C32 1.619(7) . ?
N1 C1 1.323(8) . ?
N1 C5 1.363(6) . ?
N2 C5 1.373(5) . ?
N2 C6 1.375(5) . ?
N3 C10 1.366(6) . ?
N3 C6 1.370(6) . ?
N4 C11 1.375(5) . ?
N4 C10 1.376(5) . ?
N5 C11 1.358(6) . ?
N5 C15 1.370(8) . ?
N6 C20 1.350(6) . ?
N6 C16 1.373(8) . ?
N7 C21 1.373(6) . ?
N7 C20 1.376(5) . ?
N8 C25 1.363(6) . ?
N8 C21 1.372(6) . ?
N9 C25 1.372(5) . ?
N9 C26 1.374(5) . ?
N10 C30 1.325(8) . ?
N10 C26 1.363(6) . ?
N11 C31 1.144(7) . ?
N12 C32 1.143(7) . ?
C1 C2 1.351(11) . ?
C1 H1 0.9300 . ?
C2 C3 1.373(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.412(6) . ?
C4 H4 0.9300 . ?
C6 C7 1.391(7) . ?
C7 C8 1.390(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.372(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(7) . ?
C9 H9 0.9300 . ?
C11 C12 1.408(6) . ?
C12 C13 1.372(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.367(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.358(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.417(6) . ?
C19 H19 0.9300 . ?
C21 C22 1.398(7) . ?
C22 C23 1.355(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.378(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.402(7) . ?
C24 H24 0.9300 . ?
C26 C27 1.416(6) . ?
C27 C28 1.357(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.372(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.340(11) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cr1 N6 168.2(3) . 2_655 ?
N6 Cr1 N1 89.9(2) . 2_655 ?
N6 Cr1 N1 89.0(2) 2_655 2_655 ?
N6 Cr1 N1 89.0(2) . . ?
N6 Cr1 N1 89.9(2) 2_655 . ?
N1 Cr1 N1 169.3(3) 2_655 . ?
N6 Cr1 N11 95.89(14) . . ?
N6 Cr1 N11 95.89(14) 2_655 . ?
N1 Cr1 N11 95.35(14) 2_655 . ?
N1 Cr1 N11 95.35(14) . . ?
N6 Cr1 Cr2 84.11(14) . . ?
N6 Cr1 Cr2 84.11(14) 2_655 . ?
N1 Cr1 Cr2 84.65(14) 2_655 . ?
N1 Cr1 Cr2 84.65(14) . . ?
N11 Cr1 Cr2 180.0 . . ?
N2 Cr2 N2 177.90(19) 2_655 . ?
N2 Cr2 N7 90.38(15) 2_655 2_655 ?
N2 Cr2 N7 89.57(15) . 2_655 ?
N2 Cr2 N7 89.57(15) 2_655 . ?
N2 Cr2 N7 90.38(15) . . ?
N7 Cr2 N7 177.43(19) 2_655 . ?
N2 Cr2 Cr3 91.05(10) 2_655 . ?
N2 Cr2 Cr3 91.05(10) . . ?
N7 Cr2 Cr3 91.29(9) 2_655 . ?
N7 Cr2 Cr3 91.29(9) . . ?
N2 Cr2 Cr1 88.95(10) 2_655 . ?
N2 Cr2 Cr1 88.95(10) . . ?
N7 Cr2 Cr1 88.71(9) 2_655 . ?
N7 Cr2 Cr1 88.71(9) . . ?
Cr3 Cr2 Cr1 180.0 . . ?
N3 Cr3 N3 176.50(16) . 2_655 ?
N3 Cr3 N8 90.0(4) . . ?
N3 Cr3 N8 89.9(4) 2_655 . ?
N3 Cr3 N8 89.9(4) . 2_655 ?
N3 Cr3 N8 90.0(4) 2_655 2_655 ?
N8 Cr3 N8 176.44(16) . 2_655 ?
N3 Cr3 Cr2 91.75(8) . . ?
N3 Cr3 Cr2 91.75(8) 2_655 . ?
N8 Cr3 Cr2 91.78(8) . . ?
N8 Cr3 Cr2 91.78(8) 2_655 . ?
N3 Cr3 Cr4 88.25(8) . . ?
N3 Cr3 Cr4 88.25(8) 2_655 . ?
N8 Cr3 Cr4 88.22(8) . . ?
N8 Cr3 Cr4 88.22(8) 2_655 . ?
Cr2 Cr3 Cr4 180.0 . . ?
N4 Cr4 N4 172.35(19) 2_655 . ?
N4 Cr4 N9 89.90(14) 2_655 2_655 ?
N4 Cr4 N9 89.59(14) . 2_655 ?
N4 Cr4 N9 89.59(14) 2_655 . ?
N4 Cr4 N9 89.90(14) . . ?
N9 Cr4 N9 172.29(19) 2_655 . ?
N4 Cr4 Cr5 93.83(9) 2_655 . ?
N4 Cr4 Cr5 93.83(9) . . ?
N9 Cr4 Cr5 93.85(9) 2_655 . ?
N9 Cr4 Cr5 93.85(9) . . ?
N4 Cr4 Cr3 86.17(9) 2_655 . ?
N4 Cr4 Cr3 86.17(9) . . ?
N9 Cr4 Cr3 86.15(9) 2_655 . ?
N9 Cr4 Cr3 86.15(9) . . ?
Cr5 Cr4 Cr3 180.0 . . ?
N10 Cr5 N10 176.1(3) 2_655 . ?
N10 Cr5 N5 89.61(19) 2_655 2_655 ?
N10 Cr5 N5 90.3(2) . 2_655 ?
N10 Cr5 N5 90.3(2) 2_655 . ?
N10 Cr5 N5 89.61(19) . . ?
N5 Cr5 N5 175.8(3) 2_655 . ?
N10 Cr5 Cr4 88.03(14) 2_655 . ?
N10 Cr5 Cr4 88.03(14) . . ?
N5 Cr5 Cr4 87.92(14) 2_655 . ?
N5 Cr5 Cr4 87.92(14) . . ?
N10 Cr5 N12 91.97(14) 2_655 . ?
N10 Cr5 N12 91.97(14) . . ?
N5 Cr5 N12 92.08(14) 2_655 . ?
N5 Cr5 N12 92.08(14) . . ?
Cr4 Cr5 N12 180.0 . . ?
C1 N1 C5 118.0(5) . . ?
C1 N1 Cr1 120.1(5) . . ?
C5 N1 Cr1 121.8(3) . . ?
C5 N2 C6 122.3(4) . . ?
C5 N2 Cr2 119.0(3) . . ?
C6 N2 Cr2 118.6(3) . . ?
C10 N3 C6 120.1(6) . . ?
C10 N3 Cr3 121.4(3) . . ?
C6 N3 Cr3 118.4(4) . . ?
C11 N4 C10 122.2(3) . . ?
C11 N4 Cr4 115.4(2) . . ?
C10 N4 Cr4 122.4(3) . . ?
C11 N5 C15 119.7(5) . . ?
C11 N5 Cr5 120.6(3) . . ?
C15 N5 Cr5 119.4(4) . . ?
C20 N6 C16 119.8(5) . . ?
C20 N6 Cr1 123.0(3) . . ?
C16 N6 Cr1 117.0(4) . . ?
C21 N7 C20 122.7(4) . . ?
C21 N7 Cr2 118.7(3) . . ?
C20 N7 Cr2 118.2(3) . . ?
C25 N8 C21 121.4(5) . . ?
C25 N8 Cr3 120.8(3) . . ?
C21 N8 Cr3 117.8(3) . . ?
C25 N9 C26 122.1(4) . . ?
C25 N9 Cr4 122.6(3) . . ?
C26 N9 Cr4 115.3(3) . . ?
C30 N10 C26 117.2(5) . . ?
C30 N10 Cr5 121.4(4) . . ?
C26 N10 Cr5 120.9(3) . . ?
C31 N11 Cr1 180.0 . . ?
C32 N12 Cr5 180.0 . . ?
N1 C1 C2 125.6(7) . . ?
N1 C1 H1 117.2 . . ?
C2 C1 H1 117.2 . . ?
C1 C2 C3 117.7(7) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 119.3(7) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.2(5) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 N2 115.7(4) . . ?
N1 C5 C4 119.0(4) . . ?
N2 C5 C4 125.1(4) . . ?
N3 C6 N2 113.2(4) . . ?
N3 C6 C7 120.5(5) . . ?
N2 C6 C7 126.1(4) . . ?
C8 C7 C6 119.2(6) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 119.9(9) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 120.0(6) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N3 C10 N4 114.2(4) . . ?
N3 C10 C9 120.0(5) . . ?
N4 C10 C9 125.6(4) . . ?
N5 C11 N4 114.8(4) . . ?
N5 C11 C12 119.5(4) . . ?
N4 C11 C12 125.6(4) . . ?
C13 C12 C11 120.2(5) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.9(6) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 118.7(7) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N5 C15 C14 121.9(7) . . ?
N5 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C17 C16 N6 121.1(7) . . ?
C17 C16 H16 119.4 . . ?
N6 C16 H16 119.4 . . ?
C16 C17 C18 119.5(7) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 120.1(6) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 119.4(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
N6 C20 N7 115.0(4) . . ?
N6 C20 C19 120.0(4) . . ?
N7 C20 C19 124.8(4) . . ?
N8 C21 N7 113.8(4) . . ?
N8 C21 C22 119.0(5) . . ?
N7 C21 C22 127.0(5) . . ?
C23 C22 C21 119.7(6) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 121.5(7) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C23 C24 C25 118.6(6) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N8 C25 N9 114.7(4) . . ?
N8 C25 C24 119.6(5) . . ?
N9 C25 C24 125.6(4) . . ?
N10 C26 N9 114.6(4) . . ?
N10 C26 C27 119.3(4) . . ?
N9 C26 C27 125.9(4) . . ?
C28 C27 C26 120.0(5) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.6(6) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 117.6(7) . . ?
C30 C29 H29 121.2 . . ?
C28 C29 H29 121.2 . . ?
N10 C30 C29 126.2(7) . . ?
N10 C30 H30 116.9 . . ?
C29 C30 H30 116.9 . . ?
N11 C31 S1 180.0 . . ?
N12 C32 S2 180.0 . . ?

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
C5 N1 C1 C2 1.0(10) . . . . ?
Cr1 N1 C1 C2 177.7(6) . . . . ?
N1 C1 C2 C3 -2.5(12) . . . . ?
C1 C2 C3 C4 1.9(11) . . . . ?
C2 C3 C4 C5 0.0(10) . . . . ?
C1 N1 C5 N2 176.7(5) . . . . ?
Cr1 N1 C5 N2 0.1(5) . . . . ?
C1 N1 C5 C4 1.0(7) . . . . ?
Cr1 N1 C5 C4 -175.6(3) . . . . ?
C6 N2 C5 N1 159.6(4) . . . . ?
Cr2 N2 C5 N1 -25.7(5) . . . . ?
C6 N2 C5 C4 -25.0(7) . . . . ?
Cr2 N2 C5 C4 149.7(4) . . . . ?
C3 C4 C5 N1 -1.4(8) . . . . ?
C3 C4 C5 N2 -176.7(5) . . . . ?
C10 N3 C6 N2 178.5(5) . . . . ?
Cr3 N3 C6 N2 0.1(7) . . . . ?
C10 N3 C6 C7 2.8(9) . . . . ?
Cr3 N3 C6 C7 -175.6(5) . . . . ?
C5 N2 C6 N3 154.9(5) . . . . ?
Cr2 N2 C6 N3 -19.8(6) . . . . ?
C5 N2 C6 C7 -29.7(7) . . . . ?
Cr2 N2 C6 C7 155.6(5) . . . . ?
N3 C6 C7 C8 -4.2(10) . . . . ?
N2 C6 C7 C8 -179.3(7) . . . . ?
C6 C7 C8 C9 0.8(14) . . . . ?
C7 C8 C9 C10 4.0(13) . . . . ?
C6 N3 C10 N4 178.9(5) . . . . ?
Cr3 N3 C10 N4 -2.8(7) . . . . ?
C6 N3 C10 C9 2.0(9) . . . . ?
Cr3 N3 C10 C9 -179.7(4) . . . . ?
C11 N4 C10 N3 158.1(5) . . . . ?
Cr4 N4 C10 N3 -20.7(6) . . . . ?
C11 N4 C10 C9 -25.2(7) . . . . ?
Cr4 N4 C10 C9 155.9(4) . . . . ?
C8 C9 C10 N3 -5.4(10) . . . . ?
C8 C9 C10 N4 178.1(7) . . . . ?
C15 N5 C11 N4 -179.4(5) . . . . ?
Cr5 N5 C11 N4 6.5(5) . . . . ?
C15 N5 C11 C12 4.0(7) . . . . ?
Cr5 N5 C11 C12 -170.0(3) . . . . ?
C10 N4 C11 N5 156.5(4) . . . . ?
Cr4 N4 C11 N5 -24.5(4) . . . . ?
C10 N4 C11 C12 -27.1(6) . . . . ?
Cr4 N4 C11 C12 151.8(4) . . . . ?
N5 C11 C12 C13 -2.4(7) . . . . ?
N4 C11 C12 C13 -178.6(5) . . . . ?
C11 C12 C13 C14 -0.4(9) . . . . ?
C12 C13 C14 C15 1.6(10) . . . . ?
C11 N5 C15 C14 -2.9(9) . . . . ?
Cr5 N5 C15 C14 171.2(5) . . . . ?
C13 C14 C15 N5 0.0(10) . . . . ?
C20 N6 C16 C17 -0.5(10) . . . . ?
Cr1 N6 C16 C17 175.3(6) . . . . ?
N6 C16 C17 C18 0.0(13) . . . . ?
C16 C17 C18 C19 0.4(13) . . . . ?
C17 C18 C19 C20 -0.4(11) . . . . ?
C16 N6 C20 N7 175.7(5) . . . . ?
Cr1 N6 C20 N7 0.1(6) . . . . ?
C16 N6 C20 C19 0.5(8) . . . . ?
Cr1 N6 C20 C19 -175.1(4) . . . . ?
C21 N7 C20 N6 160.7(4) . . . . ?
Cr2 N7 C20 N6 -26.7(5) . . . . ?
C21 N7 C20 C19 -24.4(7) . . . . ?
Cr2 N7 C20 C19 148.2(4) . . . . ?
C18 C19 C20 N6 0.0(9) . . . . ?
C18 C19 C20 N7 -174.7(6) . . . . ?
C25 N8 C21 N7 177.5(5) . . . . ?
Cr3 N8 C21 N7 -0.2(7) . . . . ?
C25 N8 C21 C22 1.5(9) . . . . ?
Cr3 N8 C21 C22 -176.1(5) . . . . ?
C20 N7 C21 N8 153.5(5) . . . . ?
Cr2 N7 C21 N8 -19.1(6) . . . . ?
C20 N7 C21 C22 -30.9(7) . . . . ?
Cr2 N7 C21 C22 156.5(5) . . . . ?
N8 C21 C22 C23 -4.6(10) . . . . ?
N7 C21 C22 C23 -180.0(7) . . . . ?
C21 C22 C23 C24 4.1(14) . . . . ?
C22 C23 C24 C25 -0.4(13) . . . . ?
C21 N8 C25 N9 178.9(5) . . . . ?
Cr3 N8 C25 N9 -3.5(7) . . . . ?
C21 N8 C25 C24 2.2(8) . . . . ?
Cr3 N8 C25 C24 179.7(4) . . . . ?
C26 N9 C25 N8 158.8(5) . . . . ?
Cr4 N9 C25 N8 -20.2(6) . . . . ?
C26 N9 C25 C24 -24.7(7) . . . . ?
Cr4 N9 C25 C24 156.4(4) . . . . ?
C23 C24 C25 N8 -2.7(9) . . . . ?
C23 C24 C25 N9 -179.1(6) . . . . ?
C30 N10 C26 N9 179.8(5) . . . . ?
Cr5 N10 C26 N9 7.6(5) . . . . ?
C30 N10 C26 C27 3.9(7) . . . . ?
Cr5 N10 C26 C27 -168.3(3) . . . . ?
C25 N9 C26 N10 155.9(4) . . . . ?
Cr4 N9 C26 N10 -25.0(4) . . . . ?
C25 N9 C26 C27 -28.5(6) . . . . ?
Cr4 N9 C26 C27 150.6(4) . . . . ?
N10 C26 C27 C28 -2.6(7) . . . . ?
N9 C26 C27 C28 -178.0(5) . . . . ?
C26 C27 C28 C29 -0.3(9) . . . . ?
C27 C28 C29 C30 1.8(12) . . . . ?
C26 N10 C30 C29 -2.4(10) . . . . ?
Cr5 N10 C30 C29 169.6(6) . . . . ?
C28 C29 C30 N10 -0.5(13) . . . . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.088



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/CH2Cl2'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_15k
_database_code_depnum_ccdc_archive 'CCDC 2208667'
loop_
_audit_author_name
_audit_author_address
'Andrea Cornia'
;University of Modena and Reggio Emilia
Italy
;
_audit_update_record             
;
2022-09-21 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_date             2022-09-17
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Cr5(C15H11N5)4(NCS)2]'
_chemical_formula_moiety         'C62 H44 Cr5 N22 S2'
_chemical_formula_sum            'C62 H44 Cr5 N22 S2'
_chemical_formula_weight         1421.31

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'
Cr Cr 0.3209 0.6236 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   15.0601(4)
_cell_length_b                   26.1633(7)
_cell_length_c                   14.9768(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.0266(16)
_cell_angle_gamma                90
_cell_volume                     5901.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    15.0
_cell_measurement_reflns_used    8267
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      26.38

_exptl_special_details           
;
Crystal mounted with low temperature epoxy resin to a graphite 
fibre to enable conduction cooling inside a vacuum chamber.
;
_exptl_crystal_preparation       
'Et2O vapour diffusion into a CH2Cl2 solution,Magnetic properties'
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.026
_shelx_estimated_absorpt_T_min   0.697
_shelx_estimated_absorpt_T_max   0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.655937
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_process_details   
;
TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
Final HKLF 4 output contains 27585 reflections, Rint = 0.0313
(17654 with I > 3sig(I), Rint = 0.0291)
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      15.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'rotating anode'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0

_diffrn_reflns_number            5069
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.560
_diffrn_reflns_theta_max         26.377
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.883
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.883
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.883
_reflns_number_total             5069
_reflns_number_gt                4298
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WINGX publication routines v2020.2 (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0532P)²+10.2448P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5069
_refine_ls_number_parameters     417
_refine_ls_number_restraints     466
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.1023
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_special_details          
;Refined as a 2-component twin.
1. Twinned data refinement with scales 0.542(2) and 0.458(2)
2. Uiso(H) fixed at 1.2 Ueq(C) for all C(H) groups
3. Rigid body (RIGU) restraints for all non-hydrogen atoms with sigma 
   for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Aromatic/amide H refined with riding coordinates:
   C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
   C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), 
   C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),Twin
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.542(2)
2 0.458(2)

_vrf_PLAT029_15k                 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.883 Why?
RESPONSE: The sample was measured inside a closed cycle refrigerator
with limited access to reflection geometries. The data were collected 
using a single axis rotation.
;

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
Cr1 Cr 0.500000 0.57441(2) 0.250000 0.01278(15) Uani 1 2 d S T P . .
Cr2 Cr 0.500000 0.66984(3) 0.250000 0.01468(16) Uani 1 2 d S T P . .
Cr3 Cr 0.500000 0.74620(3) 0.250000 0.01390(15) Uani 1 2 d S T P . .
Cr4 Cr 0.500000 0.84165(3) 0.250000 0.01626(16) Uani 1 2 d S T P . .
Cr5 Cr 0.500000 0.92035(3) 0.250000 0.01661(16) Uani 1 2 d S T P . .
S1 S 0.500000 0.38332(4) 0.250000 0.0202(2) Uani 1 2 d S T P . .
S2 S 0.500000 1.11563(4) 0.250000 0.0218(2) Uani 1 2 d S T P . .
N1 N 0.56907(18) 0.58268(14) 0.1279(2) 0.0102(7) Uani 1 1 d . . . . .
N2 N 0.60480(15) 0.66614(10) 0.16535(16) 0.0107(6) Uani 1 1 d . . . . .
N3 N 0.6288(4) 0.75024(9) 0.2025(4) 0.0106(13) Uani 1 1 d . . . . .
N4 N 0.63455(15) 0.83429(10) 0.24761(16) 0.0109(5) Uani 1 1 d . . . . .
N5 N 0.6338(2) 0.91878(14) 0.28735(19) 0.0127(7) Uani 1 1 d . . . . .
N6 N 0.6212(2) 0.58388(14) 0.3174(2) 0.0117(7) Uani 1 1 d . . . . .
N7 N 0.58380(15) 0.66607(10) 0.35594(16) 0.0099(5) Uani 1 1 d . . . . .
N8 N 0.5472(3) 0.75022(8) 0.3785(4) 0.0063(12) Uani 1 1 d . . . . .
N9 N 0.50189(15) 0.83421(10) 0.38545(16) 0.0106(5) Uani 1 1 d . . . . .
N10 N 0.46332(19) 0.91949(14) 0.3842(2) 0.0127(7) Uani 1 1 d . . . . .
N11 N 0.500000 0.49068(14) 0.250000 0.0150(7) Uani 1 2 d S T P . .
N12 N 0.500000 1.00875(15) 0.250000 0.0185(7) Uani 1 2 d S T P . .
C1 C 0.5682(3) 0.5446(3) 0.0694(4) 0.0141(11) Uani 1 1 d . . . . .
H1 H 0.537603 0.514165 0.085454 0.017 Uiso 1 1 calc R U . . .
C2 C 0.6088(3) 0.5462(2) -0.0132(4) 0.0163(11) Uani 1 1 d . . . . .
H2 H 0.608234 0.517207 -0.051351 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6496(2) 0.59031(17) -0.0387(2) 0.0177(9) Uani 1 1 d . . . . .
H3 H 0.676955 0.592784 -0.095694 0.021 Uiso 1 1 calc R U . . .
C4 C 0.65083(19) 0.63121(13) 0.01899(19) 0.0143(7) Uani 1 1 d . . . . .
H4 H 0.678424 0.662294 0.001522 0.017 Uiso 1 1 calc R U . . .
C5 C 0.61104(18) 0.62713(12) 0.10438(19) 0.0114(6) Uani 1 1 d . . . . .
C6 C 0.66277(19) 0.70673(13) 0.1657(2) 0.0096(6) Uani 1 1 d . . . . .
C7 C 0.7516(2) 0.70521(15) 0.1382(2) 0.0147(8) Uani 1 1 d . . . . .
H7 H 0.776943 0.674431 0.116283 0.018 Uiso 1 1 calc R U . . .
C8 C 0.8017(5) 0.74938(12) 0.1438(5) 0.0190(16) Uani 1 1 d . . . . .
H8 H 0.861559 0.749176 0.123830 0.023 Uiso 1 1 calc R U . . .
C9 C 0.7657(2) 0.79383(15) 0.1780(2) 0.0146(8) Uani 1 1 d . . . . .
H9 H 0.799650 0.824406 0.179498 0.018 Uiso 1 1 calc R U . . .
C10 C 0.67841(19) 0.79325(13) 0.2104(2) 0.0109(7) Uani 1 1 d . . . . .
C11 C 0.67989(18) 0.87438(12) 0.28544(18) 0.0103(6) Uani 1 1 d . . . . .
C12 C 0.76449(19) 0.87134(13) 0.32621(19) 0.0130(7) Uani 1 1 d . . . . .
H12 H 0.795577 0.839754 0.327343 0.016 Uiso 1 1 calc R U . . .
C13 C 0.8017(2) 0.91417(17) 0.3642(2) 0.0149(8) Uani 1 1 d . . . . .
H13 H 0.858265 0.912152 0.392136 0.018 Uiso 1 1 calc R U . . .
C14 C 0.7560(3) 0.9607(2) 0.3616(3) 0.0145(10) Uani 1 1 d . . . . .
H14 H 0.781838 0.990911 0.385239 0.017 Uiso 1 1 calc R U . . .
C15 C 0.6731(3) 0.9615(3) 0.3241(3) 0.0119(10) Uani 1 1 d . . . . .
H15 H 0.641245 0.992807 0.323455 0.014 Uiso 1 1 calc R U . . .
C16 C 0.6803(3) 0.5440(3) 0.3122(3) 0.0137(11) Uani 1 1 d . . . . .
H16 H 0.662526 0.513603 0.282482 0.016 Uiso 1 1 calc R U . . .
C17 C 0.7637(4) 0.5463(2) 0.3479(3) 0.0180(11) Uani 1 1 d . . . . .
H17 H 0.803548 0.518362 0.342585 0.022 Uiso 1 1 calc R U . . .
C18 C 0.7889(2) 0.59150(18) 0.3930(3) 0.0155(9) Uani 1 1 d . . . . .
H18 H 0.846220 0.594164 0.419002 0.019 Uiso 1 1 calc R U . . .
C19 C 0.73029(19) 0.63151(13) 0.3991(2) 0.0143(7) Uani 1 1 d . . . . .
H19 H 0.747031 0.661970 0.429209 0.017 Uiso 1 1 calc R U . . .
C20 C 0.64471(18) 0.62730(12) 0.36023(18) 0.0106(6) Uani 1 1 d . . . . .
C21 C 0.5837(2) 0.70681(13) 0.4142(2) 0.0105(7) Uani 1 1 d . . . . .
C22 C 0.6115(2) 0.70574(15) 0.5035(2) 0.0153(8) Uani 1 1 d . . . . .
H22 H 0.634222 0.675162 0.528983 0.018 Uiso 1 1 calc R U . . .
C23 C 0.6054(5) 0.74970(11) 0.5539(5) 0.0148(15) Uani 1 1 d . . . . .
H23 H 0.625377 0.749504 0.614071 0.018 Uiso 1 1 calc R U . . .
C24 C 0.5707(2) 0.79393(15) 0.5180(2) 0.0137(8) Uani 1 1 d . . . . .
H24 H 0.568455 0.824406 0.552439 0.016 Uiso 1 1 calc R U . . .
C25 C 0.5386(2) 0.79328(13) 0.4293(2) 0.0099(6) Uani 1 1 d . . . . .
C26 C 0.46401(18) 0.87439(13) 0.4304(2) 0.0122(6) Uani 1 1 d . . . . .
C27 C 0.42260(19) 0.87174(13) 0.5147(2) 0.0153(7) Uani 1 1 d . . . . .
H27 H 0.421458 0.840330 0.546461 0.018 Uiso 1 1 calc R U . . .
C28 C 0.3840(2) 0.91444(19) 0.5507(3) 0.0169(9) Uani 1 1 d . . . . .
H28 H 0.355227 0.912809 0.607086 0.020 Uiso 1 1 calc R U . . .
C29 C 0.3875(3) 0.9595(3) 0.5043(4) 0.0213(12) Uani 1 1 d . . . . .
H29 H 0.362269 0.989834 0.528331 0.026 Uiso 1 1 calc R U . . .
C30 C 0.4281(4) 0.9600(3) 0.4228(4) 0.0192(11) Uani 1 1 d . . . . .
H30 H 0.431137 0.991626 0.391824 0.023 Uiso 1 1 calc R U . . .
C31 C 0.500000 0.44608(19) 0.250000 0.0176(8) Uani 1 2 d S T P . .
C32 C 0.500000 1.05312(18) 0.250000 0.0176(8) Uani 1 2 d S T P . .


_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
Cr1 N6 2.100(3) . ?
Cr1 N6 2.100(3) 2_655 ?
Cr1 N1 2.115(3) 2_655 ?
Cr1 N1 2.115(3) . ?
Cr1 N11 2.191(4) . ?
Cr1 Cr2 2.4969(10) . ?
Cr2 Cr3 1.9978(11) . ?
Cr2 N2 2.027(2) 2_655 ?
Cr2 N2 2.027(2) . ?
Cr2 N7 2.029(2) 2_655 ?
Cr2 N7 2.029(2) . ?
Cr3 N8 2.054(5) . ?
Cr3 N8 2.054(5) 2_655 ?
Cr3 N3 2.069(5) . ?
Cr3 N3 2.069(5) 2_655 ?
Cr3 Cr4 2.4973(11) . ?
Cr4 N4 2.036(2) 2_655 ?
Cr4 N4 2.036(2) . ?
Cr4 N9 2.038(2) 2_655 ?
Cr4 N9 2.038(2) . ?
Cr4 Cr5 2.0589(10) . ?
Cr5 N10 2.084(3) 2_655 ?
Cr5 N10 2.084(3) . ?
Cr5 N5 2.092(3) . ?
Cr5 N5 2.092(3) 2_655 ?
Cr5 N12 2.313(4) . ?
S1 C31 1.642(5) . ?
S2 C32 1.635(5) . ?
N1 C1 1.327(7) . ?
N1 C5 1.370(5) . ?
N2 C5 1.373(4) . ?
N2 C6 1.375(4) . ?
N3 C10 1.356(5) . ?
N3 C6 1.364(5) . ?
N4 C11 1.374(4) . ?
N4 C10 1.378(4) . ?
N5 C11 1.353(5) . ?
N5 C15 1.379(7) . ?
N6 C20 1.352(5) . ?
N6 C16 1.373(7) . ?
N7 C20 1.369(4) . ?
N7 C21 1.378(4) . ?
N8 C25 1.366(5) . ?
N8 C21 1.371(5) . ?
N9 C25 1.372(4) . ?
N9 C26 1.372(4) . ?
N10 C30 1.319(7) . ?
N10 C26 1.368(5) . ?
N11 C31 1.167(5) . ?
N12 C32 1.161(5) . ?
C1 C2 1.381(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.363(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.417(4) . ?
C4 H4 0.9500 . ?
C6 C7 1.400(4) . ?
C7 C8 1.383(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.401(4) . ?
C9 H9 0.9500 . ?
C11 C12 1.415(4) . ?
C12 C13 1.376(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.398(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.369(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.365(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.413(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.372(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.418(4) . ?
C19 H19 0.9500 . ?
C21 C22 1.401(4) . ?
C22 C23 1.378(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.415(4) . ?
C24 H24 0.9500 . ?
C26 C27 1.410(4) . ?
C27 C28 1.371(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.370(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.365(8) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cr1 N6 166.5(2) . 2_655 ?
N6 Cr1 N1 90.03(13) . 2_655 ?
N6 Cr1 N1 88.58(13) 2_655 2_655 ?
N6 Cr1 N1 88.58(13) . . ?
N6 Cr1 N1 90.03(13) 2_655 . ?
N1 Cr1 N1 168.2(2) 2_655 . ?
N6 Cr1 N11 96.77(10) . . ?
N6 Cr1 N11 96.77(10) 2_655 . ?
N1 Cr1 N11 95.88(10) 2_655 . ?
N1 Cr1 N11 95.88(10) . . ?
N6 Cr1 Cr2 83.23(10) . . ?
N6 Cr1 Cr2 83.23(10) 2_655 . ?
N1 Cr1 Cr2 84.12(10) 2_655 . ?
N1 Cr1 Cr2 84.12(10) . . ?
N11 Cr1 Cr2 180.0 . . ?
Cr3 Cr2 N2 92.74(8) . 2_655 ?
Cr3 Cr2 N2 92.74(8) . . ?
N2 Cr2 N2 174.52(15) 2_655 . ?
Cr3 Cr2 N7 92.79(8) . 2_655 ?
N2 Cr2 N7 90.15(11) 2_655 2_655 ?
N2 Cr2 N7 89.59(11) . 2_655 ?
Cr3 Cr2 N7 92.79(8) . . ?
N2 Cr2 N7 89.59(11) 2_655 . ?
N2 Cr2 N7 90.15(11) . . ?
N7 Cr2 N7 174.42(15) 2_655 . ?
Cr3 Cr2 Cr1 180.0 . . ?
N2 Cr2 Cr1 87.26(8) 2_655 . ?
N2 Cr2 Cr1 87.26(8) . . ?
N7 Cr2 Cr1 87.21(8) 2_655 . ?
N7 Cr2 Cr1 87.21(8) . . ?
Cr2 Cr3 N8 92.93(6) . . ?
Cr2 Cr3 N8 92.93(6) . 2_655 ?
N8 Cr3 N8 174.13(13) . 2_655 ?
Cr2 Cr3 N3 92.93(7) . . ?
N8 Cr3 N3 89.7(3) . . ?
N8 Cr3 N3 90.0(3) 2_655 . ?
Cr2 Cr3 N3 92.93(7) . 2_655 ?
N8 Cr3 N3 90.0(3) . 2_655 ?
N8 Cr3 N3 89.7(3) 2_655 2_655 ?
N3 Cr3 N3 174.15(13) . 2_655 ?
Cr2 Cr3 Cr4 180.0 . . ?
N8 Cr3 Cr4 87.07(6) . . ?
N8 Cr3 Cr4 87.07(6) 2_655 . ?
N3 Cr3 Cr4 87.07(7) . . ?
N3 Cr3 Cr4 87.07(7) 2_655 . ?
N4 Cr4 N4 169.14(16) 2_655 . ?
N4 Cr4 N9 89.72(11) 2_655 2_655 ?
N4 Cr4 N9 89.25(11) . 2_655 ?
N4 Cr4 N9 89.25(11) 2_655 . ?
N4 Cr4 N9 89.72(11) . . ?
N9 Cr4 N9 169.04(15) 2_655 . ?
N4 Cr4 Cr5 95.43(8) 2_655 . ?
N4 Cr4 Cr5 95.43(8) . . ?
N9 Cr4 Cr5 95.48(8) 2_655 . ?
N9 Cr4 Cr5 95.48(8) . . ?
N4 Cr4 Cr3 84.57(8) 2_655 . ?
N4 Cr4 Cr3 84.57(8) . . ?
N9 Cr4 Cr3 84.52(8) 2_655 . ?
N9 Cr4 Cr3 84.52(8) . . ?
Cr5 Cr4 Cr3 180.0 . . ?
Cr4 Cr5 N10 89.38(10) . 2_655 ?
Cr4 Cr5 N10 89.38(10) . . ?
N10 Cr5 N10 178.8(2) 2_655 . ?
Cr4 Cr5 N5 88.88(10) . . ?
N10 Cr5 N5 90.10(14) 2_655 . ?
N10 Cr5 N5 89.87(14) . . ?
Cr4 Cr5 N5 88.88(10) . 2_655 ?
N10 Cr5 N5 89.87(14) 2_655 2_655 ?
N10 Cr5 N5 90.10(14) . 2_655 ?
N5 Cr5 N5 177.8(2) . 2_655 ?
Cr4 Cr5 N12 180.0 . . ?
N10 Cr5 N12 90.62(10) 2_655 . ?
N10 Cr5 N12 90.62(10) . . ?
N5 Cr5 N12 91.12(10) . . ?
N5 Cr5 N12 91.12(10) 2_655 . ?
C1 N1 C5 118.2(4) . . ?
C1 N1 Cr1 119.3(3) . . ?
C5 N1 Cr1 122.4(2) . . ?
C5 N2 C6 122.2(2) . . ?
C5 N2 Cr2 120.34(19) . . ?
C6 N2 Cr2 117.1(2) . . ?
C10 N3 C6 121.4(4) . . ?
C10 N3 Cr3 121.9(3) . . ?
C6 N3 Cr3 116.6(3) . . ?
C11 N4 C10 121.5(2) . . ?
C11 N4 Cr4 114.52(19) . . ?
C10 N4 Cr4 123.9(2) . . ?
C11 N5 C15 119.0(3) . . ?
C11 N5 Cr5 120.3(2) . . ?
C15 N5 Cr5 120.3(3) . . ?
C20 N6 C16 119.7(3) . . ?
C20 N6 Cr1 123.7(2) . . ?
C16 N6 Cr1 116.5(3) . . ?
C20 N7 C21 123.0(3) . . ?
C20 N7 Cr2 119.29(19) . . ?
C21 N7 Cr2 117.2(2) . . ?
C25 N8 C21 120.3(4) . . ?
C25 N8 Cr3 122.1(3) . . ?
C21 N8 Cr3 117.5(3) . . ?
C25 N9 C26 122.1(3) . . ?
C25 N9 Cr4 123.8(2) . . ?
C26 N9 Cr4 114.2(2) . . ?
C30 N10 C26 118.3(4) . . ?
C30 N10 Cr5 121.4(4) . . ?
C26 N10 Cr5 119.7(2) . . ?
C31 N11 Cr1 180.0 . . ?
C32 N12 Cr5 180.0 . . ?
N1 C1 C2 124.3(6) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C3 C2 C1 118.5(5) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 N2 115.4(3) . . ?
N1 C5 C4 119.5(3) . . ?
N2 C5 C4 125.0(3) . . ?
N3 C6 N2 114.1(3) . . ?
N3 C6 C7 120.0(3) . . ?
N2 C6 C7 125.7(3) . . ?
C8 C7 C6 118.7(4) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C9 C8 C7 120.8(6) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N3 C10 N4 114.7(3) . . ?
N3 C10 C9 119.7(4) . . ?
N4 C10 C9 125.6(3) . . ?
N5 C11 N4 114.2(3) . . ?
N5 C11 C12 120.0(3) . . ?
N4 C11 C12 125.6(3) . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.8(4) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 118.3(5) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 N5 122.8(5) . . ?
C14 C15 H15 118.6 . . ?
N5 C15 H15 118.6 . . ?
C17 C16 N6 122.7(5) . . ?
C17 C16 H16 118.7 . . ?
N6 C16 H16 118.7 . . ?
C16 C17 C18 118.1(5) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
C19 C18 C17 119.8(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 119.9(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
N6 C20 N7 115.2(3) . . ?
N6 C20 C19 119.8(3) . . ?
N7 C20 C19 124.8(3) . . ?
N8 C21 N7 113.2(3) . . ?
N8 C21 C22 120.6(4) . . ?
N7 C21 C22 126.1(3) . . ?
C23 C22 C21 119.1(4) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 120.8(6) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C25 119.0(4) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N8 C25 N9 114.6(3) . . ?
N8 C25 C24 120.1(3) . . ?
N9 C25 C24 125.3(3) . . ?
N10 C26 N9 114.6(3) . . ?
N10 C26 C27 119.5(3) . . ?
N9 C26 C27 125.8(3) . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 119.0(4) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
C30 C29 C28 118.6(6) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
N10 C30 C29 124.4(6) . . ?
N10 C30 H30 117.8 . . ?
C29 C30 H30 117.8 . . ?
N11 C31 S1 180.0 . . ?
N12 C32 S2 180.0 . . ?

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
C5 N1 C1 C2 1.7(7) . . . . ?
Cr1 N1 C1 C2 178.2(4) . . . . ?
N1 C1 C2 C3 -2.8(8) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
C2 C3 C4 C5 0.9(5) . . . . ?
C1 N1 C5 N2 176.0(3) . . . . ?
Cr1 N1 C5 N2 -0.3(4) . . . . ?
C1 N1 C5 C4 0.7(5) . . . . ?
Cr1 N1 C5 C4 -175.7(2) . . . . ?
C6 N2 C5 N1 160.3(3) . . . . ?
Cr2 N2 C5 N1 -26.8(3) . . . . ?
C6 N2 C5 C4 -24.7(4) . . . . ?
Cr2 N2 C5 C4 148.2(2) . . . . ?
C3 C4 C5 N1 -2.0(4) . . . . ?
C3 C4 C5 N2 -176.8(3) . . . . ?
C10 N3 C6 N2 177.9(4) . . . . ?
Cr3 N3 C6 N2 0.3(5) . . . . ?
C10 N3 C6 C7 2.5(7) . . . . ?
Cr3 N3 C6 C7 -175.1(3) . . . . ?
C5 N2 C6 N3 154.6(4) . . . . ?
Cr2 N2 C6 N3 -18.6(4) . . . . ?
C5 N2 C6 C7 -30.3(5) . . . . ?
Cr2 N2 C6 C7 156.5(3) . . . . ?
N3 C6 C7 C8 -4.3(6) . . . . ?
N2 C6 C7 C8 -179.2(4) . . . . ?
C6 C7 C8 C9 1.8(8) . . . . ?
C7 C8 C9 C10 2.4(8) . . . . ?
C6 N3 C10 N4 179.0(4) . . . . ?
Cr3 N3 C10 N4 -3.5(6) . . . . ?
C6 N3 C10 C9 1.9(7) . . . . ?
Cr3 N3 C10 C9 179.3(3) . . . . ?
C11 N4 C10 N3 159.5(4) . . . . ?
Cr4 N4 C10 N3 -21.5(5) . . . . ?
C11 N4 C10 C9 -23.6(5) . . . . ?
Cr4 N4 C10 C9 155.5(3) . . . . ?
C8 C9 C10 N3 -4.3(6) . . . . ?
C8 C9 C10 N4 178.9(5) . . . . ?
C15 N5 C11 N4 179.8(3) . . . . ?
Cr5 N5 C11 N4 7.5(3) . . . . ?
C15 N5 C11 C12 4.3(5) . . . . ?
Cr5 N5 C11 C12 -168.1(2) . . . . ?
C10 N4 C11 N5 155.7(3) . . . . ?
Cr4 N4 C11 N5 -23.4(3) . . . . ?
C10 N4 C11 C12 -29.0(4) . . . . ?
Cr4 N4 C11 C12 151.9(2) . . . . ?
N5 C11 C12 C13 -3.0(4) . . . . ?
N4 C11 C12 C13 -178.0(3) . . . . ?
C11 C12 C13 C14 -0.6(5) . . . . ?
C12 C13 C14 C15 2.7(7) . . . . ?
C13 C14 C15 N5 -1.4(8) . . . . ?
C11 N5 C15 C14 -2.1(7) . . . . ?
Cr5 N5 C15 C14 170.2(4) . . . . ?
C20 N6 C16 C17 -0.8(7) . . . . ?
Cr1 N6 C16 C17 175.7(4) . . . . ?
N6 C16 C17 C18 0.9(8) . . . . ?
C16 C17 C18 C19 -0.5(7) . . . . ?
C17 C18 C19 C20 0.1(6) . . . . ?
C16 N6 C20 N7 175.3(3) . . . . ?
Cr1 N6 C20 N7 -1.0(4) . . . . ?
C16 N6 C20 C19 0.4(5) . . . . ?
Cr1 N6 C20 C19 -175.9(2) . . . . ?
C21 N7 C20 N6 161.3(3) . . . . ?
Cr2 N7 C20 N6 -27.4(3) . . . . ?
C21 N7 C20 C19 -24.0(4) . . . . ?
Cr2 N7 C20 C19 147.3(2) . . . . ?
C18 C19 C20 N6 0.0(5) . . . . ?
C18 C19 C20 N7 -174.5(3) . . . . ?
C25 N8 C21 N7 177.0(4) . . . . ?
Cr3 N8 C21 N7 0.6(5) . . . . ?
C25 N8 C21 C22 0.9(6) . . . . ?
Cr3 N8 C21 C22 -175.5(3) . . . . ?
C20 N7 C21 N8 152.9(3) . . . . ?
Cr2 N7 C21 N8 -18.5(4) . . . . ?
C20 N7 C21 C22 -31.2(5) . . . . ?
Cr2 N7 C21 C22 157.3(3) . . . . ?
N8 C21 C22 C23 -3.0(6) . . . . ?
N7 C21 C22 C23 -178.6(4) . . . . ?
C21 C22 C23 C24 1.4(7) . . . . ?
C22 C23 C24 C25 2.0(7) . . . . ?
C21 N8 C25 N9 179.4(4) . . . . ?
Cr3 N8 C25 N9 -4.4(5) . . . . ?
C21 N8 C25 C24 2.6(6) . . . . ?
Cr3 N8 C25 C24 178.9(3) . . . . ?
C26 N9 C25 N8 159.9(3) . . . . ?
Cr4 N9 C25 N8 -21.0(4) . . . . ?
C26 N9 C25 C24 -23.5(5) . . . . ?
Cr4 N9 C25 C24 155.5(3) . . . . ?
C23 C24 C25 N8 -4.1(6) . . . . ?
C23 C24 C25 N9 179.5(4) . . . . ?
C30 N10 C26 N9 -180.0(4) . . . . ?
Cr5 N10 C26 N9 8.9(3) . . . . ?
C30 N10 C26 C27 3.9(5) . . . . ?
Cr5 N10 C26 C27 -167.2(2) . . . . ?
C25 N9 C26 N10 154.8(3) . . . . ?
Cr4 N9 C26 N10 -24.3(3) . . . . ?
C25 N9 C26 C27 -29.3(4) . . . . ?
Cr4 N9 C26 C27 151.5(2) . . . . ?
N10 C26 C27 C28 -1.6(4) . . . . ?
N9 C26 C27 C28 -177.3(3) . . . . ?
C26 C27 C28 C29 -0.9(5) . . . . ?
C27 C28 C29 C30 1.2(7) . . . . ?
C26 N10 C30 C29 -3.8(7) . . . . ?
Cr5 N10 C30 C29 167.1(4) . . . . ?
C28 C29 C30 N10 1.2(8) . . . . ?

_refine_diff_density_max         0.795
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.079



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/CH2Cl2'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_3k
_database_code_depnum_ccdc_archive 'CCDC 2208666'
loop_
_audit_author_name
_audit_author_address
'Andrea Cornia'
;University of Modena and Reggio Emilia
Italy
;
_audit_update_record             
;
2022-09-21 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_date             2022-09-17
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Cr5(C15H11N5)4(NCS)2]'
_chemical_formula_moiety         'C62 H44 Cr5 N22 S2'
_chemical_formula_sum            'C62 H44 Cr5 N22 S2'
_chemical_formula_weight         1421.31

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'
Cr Cr 0.3209 0.6236 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   15.0605(4)
_cell_length_b                   26.1672(7)
_cell_length_c                   14.9728(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.023(2)
_cell_angle_gamma                90
_cell_volume                     5900.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    3.0
_cell_measurement_reflns_used    8240
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      26.37

_exptl_special_details           
;
Crystal mounted with low temperature epoxy resin to a graphite 
fibre to enable conduction cooling inside a vacuum chamber.
;
_exptl_crystal_preparation       
'Et2O vapour diffusion into a CH2Cl2 solution,Magnetic properties'
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.026
_shelx_estimated_absorpt_T_min   0.696
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.616768
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_process_details   
;
TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
Final HKLF 4 output contains 27547 reflections, Rint = 0.0302
(17965 with I > 3sig(I), Rint = 0.0282)
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      3.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'rotating anode'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0

_diffrn_reflns_number            5064
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.560
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.883
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.883
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.883
_reflns_number_total             5064
_reflns_number_gt                4336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WINGX publication routines v2020.2 (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0512P)²+10.9668P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5064
_refine_ls_number_parameters     417
_refine_ls_number_restraints     466
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_special_details          
;Refined as a 2-component twin.
1. Twinned data refinement with scales 0.549(2) and 0.451(2)
2. Uiso(H) fixed at 1.2 Ueq(C) for all C(H) groups
3. Rigid body (RIGU) restraints for all non-hydrogen atoms with sigma 
   for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Aromatic/amide H refined with riding coordinates:
   C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
   C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), 
   C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),Twin
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.549(2)
2 0.451(2)

_vrf_PLAT029_3k                  
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.883 Why?
RESPONSE: The sample was measured inside a closed cycle refrigerator
with limited access to reflection geometries. The data were collected 
using a single axis rotation.
;

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
Cr1 Cr 0.500000 0.57425(2) 0.250000 0.01216(15) Uani 1 2 d S T P . .
Cr2 Cr 0.500000 0.67002(3) 0.250000 0.01392(16) Uani 1 2 d S T P . .
Cr3 Cr 0.500000 0.74601(3) 0.250000 0.01319(15) Uani 1 2 d S T P . .
Cr4 Cr 0.500000 0.84183(3) 0.250000 0.01554(16) Uani 1 2 d S T P . .
Cr5 Cr 0.500000 0.92018(3) 0.250000 0.01591(16) Uani 1 2 d S T P . .
S1 S 0.500000 0.38317(4) 0.250000 0.0192(2) Uani 1 2 d S T P . .
S2 S 0.500000 1.11557(4) 0.250000 0.0212(2) Uani 1 2 d S T P . .
N1 N 0.56906(18) 0.58276(14) 0.1279(2) 0.0097(7) Uani 1 1 d . . . . .
N2 N 0.60486(15) 0.66606(10) 0.16539(16) 0.0104(5) Uani 1 1 d . . . . .
N3 N 0.6289(4) 0.75020(9) 0.2025(4) 0.0090(12) Uani 1 1 d . . . . .
N4 N 0.63447(15) 0.83427(10) 0.24778(16) 0.0108(5) Uani 1 1 d . . . . .
N5 N 0.6339(2) 0.91887(14) 0.28751(19) 0.0122(7) Uani 1 1 d . . . . .
N6 N 0.6212(2) 0.58372(14) 0.3173(2) 0.0114(7) Uani 1 1 d . . . . .
N7 N 0.58369(15) 0.66611(10) 0.35601(15) 0.0098(5) Uani 1 1 d . . . . .
N8 N 0.5472(3) 0.75025(8) 0.3784(4) 0.0071(12) Uani 1 1 d . . . . .
N9 N 0.50194(15) 0.83421(10) 0.38539(15) 0.0102(5) Uani 1 1 d . . . . .
N10 N 0.46331(18) 0.91944(14) 0.3840(2) 0.0120(7) Uani 1 1 d . . . . .
N11 N 0.500000 0.49058(14) 0.250000 0.0149(7) Uani 1 2 d S T P . .
N12 N 0.500000 1.00868(14) 0.250000 0.0180(7) Uani 1 2 d S T P . .
C1 C 0.5683(3) 0.5444(2) 0.0688(3) 0.0125(10) Uani 1 1 d . . . . .
H1 H 0.537999 0.513931 0.084785 0.015 Uiso 1 1 calc R U . . .
C2 C 0.6083(3) 0.5463(2) -0.0130(4) 0.0167(11) Uani 1 1 d . . . . .
H2 H 0.607313 0.517376 -0.051446 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6496(2) 0.59024(17) -0.0387(2) 0.0169(9) Uani 1 1 d . . . . .
H3 H 0.677141 0.592563 -0.095679 0.020 Uiso 1 1 calc R U . . .
C4 C 0.65104(19) 0.63125(13) 0.01896(19) 0.0141(7) Uani 1 1 d . . . . .
H4 H 0.678757 0.662302 0.001524 0.017 Uiso 1 1 calc R U . . .
C5 C 0.61109(18) 0.62708(12) 0.10432(19) 0.0113(6) Uani 1 1 d . . . . .
C6 C 0.66277(19) 0.70684(13) 0.1659(2) 0.0095(6) Uani 1 1 d . . . . .
C7 C 0.7516(2) 0.70524(14) 0.1384(2) 0.0144(8) Uani 1 1 d . . . . .
H7 H 0.776951 0.674406 0.116764 0.017 Uiso 1 1 calc R U . . .
C8 C 0.8016(4) 0.74938(12) 0.1435(5) 0.0177(15) Uani 1 1 d . . . . .
H8 H 0.861281 0.749196 0.123069 0.021 Uiso 1 1 calc R U . . .
C9 C 0.7657(2) 0.79387(15) 0.1780(2) 0.0137(8) Uani 1 1 d . . . . .
H9 H 0.799741 0.824427 0.179713 0.016 Uiso 1 1 calc R U . . .
C10 C 0.67823(19) 0.79318(13) 0.2106(2) 0.0107(7) Uani 1 1 d . . . . .
C11 C 0.67986(18) 0.87433(12) 0.28536(18) 0.0100(6) Uani 1 1 d . . . . .
C12 C 0.76452(18) 0.87143(13) 0.32597(19) 0.0123(6) Uani 1 1 d . . . . .
H12 H 0.795741 0.839890 0.326818 0.015 Uiso 1 1 calc R U . . .
C13 C 0.8019(2) 0.91421(17) 0.3643(2) 0.0143(8) Uani 1 1 d . . . . .
H13 H 0.858434 0.912139 0.392159 0.017 Uiso 1 1 calc R U . . .
C14 C 0.7561(3) 0.9607(2) 0.3620(3) 0.0133(10) Uani 1 1 d . . . . .
H14 H 0.781785 0.990952 0.385757 0.016 Uiso 1 1 calc R U . . .
C15 C 0.6726(3) 0.9614(2) 0.3242(3) 0.0122(10) Uani 1 1 d . . . . .
H15 H 0.640509 0.992643 0.323594 0.015 Uiso 1 1 calc R U . . .
C16 C 0.6799(3) 0.5441(2) 0.3120(3) 0.0139(11) Uani 1 1 d . . . . .
H16 H 0.662075 0.513799 0.282139 0.017 Uiso 1 1 calc R U . . .
C17 C 0.7640(4) 0.5463(2) 0.3483(3) 0.0179(11) Uani 1 1 d . . . . .
H17 H 0.803725 0.518266 0.343338 0.021 Uiso 1 1 calc R U . . .
C18 C 0.7890(2) 0.59151(17) 0.3928(3) 0.0149(9) Uani 1 1 d . . . . .
H18 H 0.846456 0.594365 0.418529 0.018 Uiso 1 1 calc R U . . .
C19 C 0.73021(19) 0.63137(13) 0.3990(2) 0.0140(7) Uani 1 1 d . . . . .
H19 H 0.746910 0.661787 0.429315 0.017 Uiso 1 1 calc R U . . .
C20 C 0.64474(18) 0.62731(12) 0.36038(18) 0.0098(6) Uani 1 1 d . . . . .
C21 C 0.5838(2) 0.70674(13) 0.4145(2) 0.0099(7) Uani 1 1 d . . . . .
C22 C 0.6117(2) 0.70572(15) 0.5036(2) 0.0148(8) Uani 1 1 d . . . . .
H22 H 0.634713 0.675199 0.528935 0.018 Uiso 1 1 calc R U . . .
C23 C 0.6052(4) 0.74974(11) 0.5543(5) 0.0140(14) Uani 1 1 d . . . . .
H23 H 0.624728 0.749537 0.614641 0.017 Uiso 1 1 calc R U . . .
C24 C 0.5707(2) 0.79390(14) 0.5181(2) 0.0137(7) Uani 1 1 d . . . . .
H24 H 0.568466 0.824398 0.552425 0.016 Uiso 1 1 calc R U . . .
C25 C 0.5386(2) 0.79338(13) 0.4294(2) 0.0098(6) Uani 1 1 d . . . . .
C26 C 0.46392(18) 0.87442(13) 0.4304(2) 0.0122(6) Uani 1 1 d . . . . .
C27 C 0.42246(18) 0.87173(13) 0.5148(2) 0.0148(7) Uani 1 1 d . . . . .
H27 H 0.421305 0.840344 0.546699 0.018 Uiso 1 1 calc R U . . .
C28 C 0.3839(2) 0.91441(18) 0.5507(3) 0.0170(9) Uani 1 1 d . . . . .
H28 H 0.354799 0.912842 0.606860 0.020 Uiso 1 1 calc R U . . .
C29 C 0.3881(3) 0.9595(3) 0.5041(4) 0.0214(11) Uani 1 1 d . . . . .
H29 H 0.363271 0.989869 0.528369 0.026 Uiso 1 1 calc R U . . .
C30 C 0.4281(3) 0.9602(3) 0.4233(4) 0.0180(11) Uani 1 1 d . . . . .
H30 H 0.431113 0.991884 0.392565 0.022 Uiso 1 1 calc R U . . .
C31 C 0.500000 0.44586(18) 0.250000 0.0171(8) Uani 1 2 d S T P . .
C32 C 0.500000 1.05290(18) 0.250000 0.0173(8) Uani 1 2 d S T P . .


_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
Cr1 N6 2.100(3) . ?
Cr1 N6 2.100(3) 2_655 ?
Cr1 N1 2.115(3) 2_655 ?
Cr1 N1 2.115(3) . ?
Cr1 N11 2.189(4) . ?
Cr1 Cr2 2.5061(10) . ?
Cr2 Cr3 1.9884(10) . ?
Cr2 N2 2.028(2) 2_655 ?
Cr2 N2 2.028(2) . ?
Cr2 N7 2.029(2) 2_655 ?
Cr2 N7 2.029(2) . ?
Cr3 N8 2.053(5) . ?
Cr3 N8 2.053(5) 2_655 ?
Cr3 N3 2.071(5) . ?
Cr3 N3 2.071(5) 2_655 ?
Cr3 Cr4 2.5073(11) . ?
Cr4 N4 2.035(2) 2_655 ?
Cr4 N4 2.035(2) . ?
Cr4 N9 2.037(2) 2_655 ?
Cr4 N9 2.037(2) . ?
Cr4 Cr5 2.0500(10) . ?
Cr5 N10 2.082(3) 2_655 ?
Cr5 N10 2.082(3) . ?
Cr5 N5 2.094(3) . ?
Cr5 N5 2.094(3) 2_655 ?
Cr5 N12 2.316(4) . ?
S1 C31 1.640(5) . ?
S2 C32 1.640(5) . ?
N1 C1 1.338(7) . ?
N1 C5 1.368(5) . ?
N2 C5 1.373(4) . ?
N2 C6 1.378(4) . ?
N3 C10 1.353(5) . ?
N3 C6 1.360(5) . ?
N4 C11 1.372(4) . ?
N4 C10 1.379(4) . ?
N5 C11 1.356(5) . ?
N5 C15 1.371(7) . ?
N6 C20 1.357(5) . ?
N6 C16 1.364(7) . ?
N7 C20 1.371(4) . ?
N7 C21 1.377(4) . ?
N8 C25 1.368(5) . ?
N8 C21 1.375(5) . ?
N9 C25 1.371(4) . ?
N9 C26 1.375(4) . ?
N10 C30 1.328(7) . ?
N10 C26 1.368(5) . ?
N11 C31 1.170(5) . ?
N12 C32 1.157(5) . ?
C1 C2 1.367(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.364(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.417(4) . ?
C4 H4 0.9500 . ?
C6 C7 1.400(4) . ?
C7 C8 1.381(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.384(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.405(4) . ?
C9 H9 0.9500 . ?
C11 C12 1.414(4) . ?
C12 C13 1.378(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.399(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.378(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.409(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.371(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.415(4) . ?
C19 H19 0.9500 . ?
C21 C22 1.399(4) . ?
C22 C23 1.383(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.413(4) . ?
C24 H24 0.9500 . ?
C26 C27 1.412(4) . ?
C27 C28 1.368(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.372(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.352(9) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cr1 N6 166.4(2) . 2_655 ?
N6 Cr1 N1 90.01(13) . 2_655 ?
N6 Cr1 N1 88.56(13) 2_655 2_655 ?
N6 Cr1 N1 88.56(13) . . ?
N6 Cr1 N1 90.01(13) 2_655 . ?
N1 Cr1 N1 167.92(19) 2_655 . ?
N6 Cr1 N11 96.78(10) . . ?
N6 Cr1 N11 96.78(10) 2_655 . ?
N1 Cr1 N11 96.04(10) 2_655 . ?
N1 Cr1 N11 96.04(10) . . ?
N6 Cr1 Cr2 83.22(10) . . ?
N6 Cr1 Cr2 83.22(10) 2_655 . ?
N1 Cr1 Cr2 83.96(10) 2_655 . ?
N1 Cr1 Cr2 83.96(10) . . ?
N11 Cr1 Cr2 180.0 . . ?
Cr3 Cr2 N2 92.93(8) . 2_655 ?
Cr3 Cr2 N2 92.93(8) . . ?
N2 Cr2 N2 174.13(15) 2_655 . ?
Cr3 Cr2 N7 92.90(8) . 2_655 ?
N2 Cr2 N7 90.14(11) 2_655 2_655 ?
N2 Cr2 N7 89.56(11) . 2_655 ?
Cr3 Cr2 N7 92.90(8) . . ?
N2 Cr2 N7 89.56(11) 2_655 . ?
N2 Cr2 N7 90.14(11) . . ?
N7 Cr2 N7 174.21(15) 2_655 . ?
Cr3 Cr2 Cr1 180.0 . . ?
N2 Cr2 Cr1 87.07(8) 2_655 . ?
N2 Cr2 Cr1 87.07(8) . . ?
N7 Cr2 Cr1 87.10(8) 2_655 . ?
N7 Cr2 Cr1 87.10(8) . . ?
Cr2 Cr3 N8 93.09(6) . . ?
Cr2 Cr3 N8 93.09(6) . 2_655 ?
N8 Cr3 N8 173.81(13) . 2_655 ?
Cr2 Cr3 N3 93.03(7) . . ?
N8 Cr3 N3 89.7(3) . . ?
N8 Cr3 N3 90.0(3) 2_655 . ?
Cr2 Cr3 N3 93.03(7) . 2_655 ?
N8 Cr3 N3 90.0(3) . 2_655 ?
N8 Cr3 N3 89.7(3) 2_655 2_655 ?
N3 Cr3 N3 173.93(13) . 2_655 ?
Cr2 Cr3 Cr4 180.0 . . ?
N8 Cr3 Cr4 86.91(6) . . ?
N8 Cr3 Cr4 86.91(6) 2_655 . ?
N3 Cr3 Cr4 86.97(7) . . ?
N3 Cr3 Cr4 86.97(7) 2_655 . ?
N4 Cr4 N4 168.85(16) 2_655 . ?
N4 Cr4 N9 89.59(11) 2_655 2_655 ?
N4 Cr4 N9 89.32(11) . 2_655 ?
N4 Cr4 N9 89.32(11) 2_655 . ?
N4 Cr4 N9 89.59(11) . . ?
N9 Cr4 N9 168.77(15) 2_655 . ?
N4 Cr4 Cr5 95.58(8) 2_655 . ?
N4 Cr4 Cr5 95.58(8) . . ?
N9 Cr4 Cr5 95.62(8) 2_655 . ?
N9 Cr4 Cr5 95.62(8) . . ?
N4 Cr4 Cr3 84.42(8) 2_655 . ?
N4 Cr4 Cr3 84.42(8) . . ?
N9 Cr4 Cr3 84.38(8) 2_655 . ?
N9 Cr4 Cr3 84.38(8) . . ?
Cr5 Cr4 Cr3 180.0 . . ?
Cr4 Cr5 N10 89.47(10) . 2_655 ?
Cr4 Cr5 N10 89.47(10) . . ?
N10 Cr5 N10 178.9(2) 2_655 . ?
Cr4 Cr5 N5 89.06(10) . . ?
N10 Cr5 N5 90.13(14) 2_655 . ?
N10 Cr5 N5 89.85(14) . . ?
Cr4 Cr5 N5 89.06(10) . 2_655 ?
N10 Cr5 N5 89.85(14) 2_655 2_655 ?
N10 Cr5 N5 90.13(14) . 2_655 ?
N5 Cr5 N5 178.1(2) . 2_655 ?
Cr4 Cr5 N12 180.0 . . ?
N10 Cr5 N12 90.53(10) 2_655 . ?
N10 Cr5 N12 90.53(10) . . ?
N5 Cr5 N12 90.94(10) . . ?
N5 Cr5 N12 90.94(10) 2_655 . ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Cr1 119.3(3) . . ?
C5 N1 Cr1 122.7(2) . . ?
C5 N2 C6 122.3(2) . . ?
C5 N2 Cr2 120.50(19) . . ?
C6 N2 Cr2 116.8(2) . . ?
C10 N3 C6 121.6(4) . . ?
C10 N3 Cr3 121.9(3) . . ?
C6 N3 Cr3 116.5(3) . . ?
C11 N4 C10 121.6(2) . . ?
C11 N4 Cr4 114.50(19) . . ?
C10 N4 Cr4 123.9(2) . . ?
C11 N5 C15 119.4(3) . . ?
C11 N5 Cr5 119.9(2) . . ?
C15 N5 Cr5 120.2(3) . . ?
C20 N6 C16 119.8(3) . . ?
C20 N6 Cr1 123.6(2) . . ?
C16 N6 Cr1 116.5(3) . . ?
C20 N7 C21 122.7(2) . . ?
C20 N7 Cr2 119.41(19) . . ?
C21 N7 Cr2 117.3(2) . . ?
C25 N8 C21 120.2(4) . . ?
C25 N8 Cr3 122.3(3) . . ?
C21 N8 Cr3 117.5(3) . . ?
C25 N9 C26 121.9(3) . . ?
C25 N9 Cr4 124.1(2) . . ?
C26 N9 Cr4 114.0(2) . . ?
C30 N10 C26 118.0(4) . . ?
C30 N10 Cr5 121.7(3) . . ?
C26 N10 Cr5 119.7(2) . . ?
C31 N11 Cr1 180.0 . . ?
C32 N12 Cr5 180.0 . . ?
N1 C1 C2 124.3(5) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C3 C2 C1 119.0(5) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 N2 115.2(3) . . ?
N1 C5 C4 119.7(3) . . ?
N2 C5 C4 124.9(3) . . ?
N3 C6 N2 114.2(3) . . ?
N3 C6 C7 120.1(3) . . ?
N2 C6 C7 125.5(3) . . ?
C8 C7 C6 118.7(4) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C7 C8 C9 120.8(5) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C10 119.0(4) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N3 C10 N4 114.9(3) . . ?
N3 C10 C9 119.6(3) . . ?
N4 C10 C9 125.3(3) . . ?
N5 C11 N4 114.4(3) . . ?
N5 C11 C12 119.7(3) . . ?
N4 C11 C12 125.8(3) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 118.1(5) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
N5 C15 C14 122.8(5) . . ?
N5 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
N6 C16 C17 122.8(5) . . ?
N6 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C16 C17 C18 117.8(5) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
C19 C18 C17 119.9(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 120.2(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
N6 C20 N7 115.1(3) . . ?
N6 C20 C19 119.6(3) . . ?
N7 C20 C19 125.0(3) . . ?
N8 C21 N7 113.0(3) . . ?
N8 C21 C22 120.7(3) . . ?
N7 C21 C22 126.3(3) . . ?
C23 C22 C21 119.1(4) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C24 C23 C22 120.6(6) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 119.4(4) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
N8 C25 N9 114.4(3) . . ?
N8 C25 C24 119.9(3) . . ?
N9 C25 C24 125.6(3) . . ?
N10 C26 N9 114.4(3) . . ?
N10 C26 C27 119.7(3) . . ?
N9 C26 C27 125.8(3) . . ?
C28 C27 C26 119.9(3) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 118.9(4) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C30 C29 C28 119.1(6) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
N10 C30 C29 124.4(6) . . ?
N10 C30 H30 117.8 . . ?
C29 C30 H30 117.8 . . ?
N11 C31 S1 180.0 . . ?
N12 C32 S2 180.0 . . ?

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
C5 N1 C1 C2 1.3(6) . . . . ?
Cr1 N1 C1 C2 178.0(4) . . . . ?
N1 C1 C2 C3 -2.2(8) . . . . ?
C1 C2 C3 C4 0.9(7) . . . . ?
C2 C3 C4 C5 1.0(5) . . . . ?
C1 N1 C5 N2 176.1(3) . . . . ?
Cr1 N1 C5 N2 -0.4(3) . . . . ?
C1 N1 C5 C4 0.7(4) . . . . ?
Cr1 N1 C5 C4 -175.8(2) . . . . ?
C6 N2 C5 N1 160.4(3) . . . . ?
Cr2 N2 C5 N1 -26.9(3) . . . . ?
C6 N2 C5 C4 -24.5(4) . . . . ?
Cr2 N2 C5 C4 148.1(2) . . . . ?
C3 C4 C5 N1 -1.9(4) . . . . ?
C3 C4 C5 N2 -176.8(3) . . . . ?
C10 N3 C6 N2 177.9(4) . . . . ?
Cr3 N3 C6 N2 0.4(5) . . . . ?
C10 N3 C6 C7 2.5(7) . . . . ?
Cr3 N3 C6 C7 -175.1(3) . . . . ?
C5 N2 C6 N3 154.4(4) . . . . ?
Cr2 N2 C6 N3 -18.5(4) . . . . ?
C5 N2 C6 C7 -30.4(5) . . . . ?
Cr2 N2 C6 C7 156.7(3) . . . . ?
N3 C6 C7 C8 -4.6(6) . . . . ?
N2 C6 C7 C8 -179.5(4) . . . . ?
C6 C7 C8 C9 2.3(8) . . . . ?
C7 C8 C9 C10 2.0(8) . . . . ?
C6 N3 C10 N4 179.0(4) . . . . ?
Cr3 N3 C10 N4 -3.5(5) . . . . ?
C6 N3 C10 C9 1.9(6) . . . . ?
Cr3 N3 C10 C9 179.4(3) . . . . ?
C11 N4 C10 N3 159.6(4) . . . . ?
Cr4 N4 C10 N3 -21.6(4) . . . . ?
C11 N4 C10 C9 -23.5(5) . . . . ?
Cr4 N4 C10 C9 155.3(3) . . . . ?
C8 C9 C10 N3 -4.1(6) . . . . ?
C8 C9 C10 N4 179.1(4) . . . . ?
C15 N5 C11 N4 179.5(3) . . . . ?
Cr5 N5 C11 N4 7.2(3) . . . . ?
C15 N5 C11 C12 4.0(5) . . . . ?
Cr5 N5 C11 C12 -168.3(2) . . . . ?
C10 N4 C11 N5 155.8(3) . . . . ?
Cr4 N4 C11 N5 -23.1(3) . . . . ?
C10 N4 C11 C12 -29.0(4) . . . . ?
Cr4 N4 C11 C12 152.1(2) . . . . ?
N5 C11 C12 C13 -2.7(4) . . . . ?
N4 C11 C12 C13 -177.7(3) . . . . ?
C11 C12 C13 C14 -0.7(5) . . . . ?
C12 C13 C14 C15 2.7(6) . . . . ?
C11 N5 C15 C14 -2.0(7) . . . . ?
Cr5 N5 C15 C14 170.3(4) . . . . ?
C13 C14 C15 N5 -1.4(8) . . . . ?
C20 N6 C16 C17 -0.6(7) . . . . ?
Cr1 N6 C16 C17 175.9(4) . . . . ?
N6 C16 C17 C18 0.4(8) . . . . ?
C16 C17 C18 C19 0.1(7) . . . . ?
C17 C18 C19 C20 -0.3(6) . . . . ?
C16 N6 C20 N7 175.2(3) . . . . ?
Cr1 N6 C20 N7 -1.0(4) . . . . ?
C16 N6 C20 C19 0.3(5) . . . . ?
Cr1 N6 C20 C19 -175.9(2) . . . . ?
C21 N7 C20 N6 161.3(3) . . . . ?
Cr2 N7 C20 N6 -27.5(3) . . . . ?
C21 N7 C20 C19 -24.1(4) . . . . ?
Cr2 N7 C20 C19 147.1(2) . . . . ?
C18 C19 C20 N6 0.1(5) . . . . ?
C18 C19 C20 N7 -174.2(3) . . . . ?
C25 N8 C21 N7 177.0(4) . . . . ?
Cr3 N8 C21 N7 0.7(5) . . . . ?
C25 N8 C21 C22 0.7(6) . . . . ?
Cr3 N8 C21 C22 -175.5(3) . . . . ?
C20 N7 C21 N8 152.9(3) . . . . ?
Cr2 N7 C21 N8 -18.5(4) . . . . ?
C20 N7 C21 C22 -31.1(5) . . . . ?
Cr2 N7 C21 C22 157.5(3) . . . . ?
N8 C21 C22 C23 -2.5(6) . . . . ?
N7 C21 C22 C23 -178.2(4) . . . . ?
C21 C22 C23 C24 0.9(7) . . . . ?
C22 C23 C24 C25 2.4(7) . . . . ?
C21 N8 C25 N9 179.4(4) . . . . ?
Cr3 N8 C25 N9 -4.5(5) . . . . ?
C21 N8 C25 C24 2.7(6) . . . . ?
Cr3 N8 C25 C24 178.7(3) . . . . ?
C26 N9 C25 N8 159.9(3) . . . . ?
Cr4 N9 C25 N8 -21.0(4) . . . . ?
C26 N9 C25 C24 -23.6(5) . . . . ?
Cr4 N9 C25 C24 155.5(3) . . . . ?
C23 C24 C25 N8 -4.2(6) . . . . ?
C23 C24 C25 N9 179.4(4) . . . . ?
C30 N10 C26 N9 -179.7(3) . . . . ?
Cr5 N10 C26 N9 9.0(3) . . . . ?
C30 N10 C26 C27 4.2(5) . . . . ?
Cr5 N10 C26 C27 -167.2(2) . . . . ?
C25 N9 C26 N10 154.8(3) . . . . ?
Cr4 N9 C26 N10 -24.3(3) . . . . ?
C25 N9 C26 C27 -29.3(4) . . . . ?
Cr4 N9 C26 C27 151.6(2) . . . . ?
N10 C26 C27 C28 -1.6(4) . . . . ?
N9 C26 C27 C28 -177.3(3) . . . . ?
C26 C27 C28 C29 -1.3(5) . . . . ?
C27 C28 C29 C30 1.7(7) . . . . ?
C26 N10 C30 C29 -4.0(7) . . . . ?
Cr5 N10 C30 C29 167.2(4) . . . . ?
C28 C29 C30 N10 1.0(8) . . . . ?

_refine_diff_density_max         0.754
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.079



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/CH2Cl2'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_100k
_database_code_depnum_ccdc_archive 'CCDC 2208668'
loop_
_audit_author_name
_audit_author_address
'Andrea Cornia'
;University of Modena and Reggio Emilia
Italy
;
_audit_update_record             
;
2022-09-21 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_date             2022-09-17
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Cr5(C15H11N5)4(NCS)2]'
_chemical_formula_moiety         'C62 H44 Cr5 N22 S2'
_chemical_formula_sum            'C62 H44 Cr5 N22 S2'
_chemical_formula_weight         1421.31

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'
Cr Cr 0.3209 0.6236 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   15.1037(4)
_cell_length_b                   26.1632(8)
_cell_length_c                   15.0198(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.0189(16)
_cell_angle_gamma                90
_cell_volume                     5935.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0
_cell_measurement_reflns_used    8387
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      26.36

_exptl_special_details           
;
Crystal mounted with low temperature epoxy resin to a graphite 
fibre to enable conduction cooling inside a vacuum chamber.
;
_exptl_crystal_preparation       
'Et2O vapour diffusion into a CH2Cl2 solution,Magnetic properties'
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.020
_shelx_estimated_absorpt_T_min   0.698
_shelx_estimated_absorpt_T_max   0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.601956
_exptl_absorpt_correction_T_max  0.745371
_exptl_absorpt_process_details   
;
TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
Final HKLF 4 output contains 27671 reflections, Rint = 0.0301
(17418 with I > 3sig(I), Rint = 0.0280)
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'rotating anode'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0

_diffrn_reflns_number            5092
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.557
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measured_fraction_theta_full 0.883
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_Laue_measured_fraction_full 0.883
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_point_group_measured_fraction_full 0.883
_reflns_number_total             5092
_reflns_number_gt                4198
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WINGX publication routines v2020.2 (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0493P)²+9.5071P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5092
_refine_ls_number_parameters     417
_refine_ls_number_restraints     466
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_special_details          
;Refined as a 2-component twin.
1. Twinned data refinement with scales 0.570(2) and 0.430(2)
2. Uiso(H) fixed at 1.2 Ueq(C) for all C(H) groups
3. Rigid body (RIGU) restraints for all non-hydrogen atoms with sigma 
   for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Aromatic/amide H refined with riding coordinates:
   C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
   C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), 
   C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),Twin
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.570(2)
2 0.430(2)

_vrf_PLAT029_100k                
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.883 Why?
RESPONSE: The sample was measured inside a closed cycle refrigerator
with limited access to reflection geometries. The data were collected 
using a single axis rotation.
;

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
Cr1 Cr 0.500000 0.57439(2) 0.250000 0.01859(15) Uani 1 2 d S T P . .
Cr2 Cr 0.500000 0.66976(3) 0.250000 0.01979(16) Uani 1 2 d S T P . .
Cr3 Cr 0.500000 0.74618(3) 0.250000 0.01820(15) Uani 1 2 d S T P . .
Cr4 Cr 0.500000 0.84151(3) 0.250000 0.02080(16) Uani 1 2 d S T P . .
Cr5 Cr 0.500000 0.92028(3) 0.250000 0.02121(16) Uani 1 2 d S T P . .
S1 S 0.500000 0.38368(4) 0.250000 0.0384(3) Uani 1 2 d S T P . .
S2 S 0.500000 1.11525(5) 0.250000 0.0393(3) Uani 1 2 d S T P . .
N1 N 0.56899(19) 0.58285(14) 0.1282(2) 0.0160(7) Uani 1 1 d . . . . .
N2 N 0.60456(15) 0.66609(10) 0.16562(16) 0.0163(6) Uani 1 1 d . . . . .
N3 N 0.6276(4) 0.75024(9) 0.2032(4) 0.0146(12) Uani 1 1 d . . . . .
N4 N 0.63410(15) 0.83431(10) 0.24787(16) 0.0157(6) Uani 1 1 d . . . . .
N5 N 0.6332(2) 0.91890(15) 0.28757(19) 0.0178(7) Uani 1 1 d . . . . .
N6 N 0.6207(2) 0.58364(15) 0.3174(2) 0.0181(7) Uani 1 1 d . . . . .
N7 N 0.58329(16) 0.66609(10) 0.35569(16) 0.0161(6) Uani 1 1 d . . . . .
N8 N 0.5473(4) 0.75017(9) 0.3790(3) 0.0118(11) Uani 1 1 d . . . . .
N9 N 0.50203(16) 0.83418(10) 0.38487(16) 0.0151(5) Uani 1 1 d . . . . .
N10 N 0.46288(19) 0.91911(15) 0.3838(2) 0.0173(7) Uani 1 1 d . . . . .
N11 N 0.500000 0.49078(14) 0.250000 0.0233(7) Uani 1 2 d S T P . .
N12 N 0.500000 1.00864(15) 0.250000 0.0259(8) Uani 1 2 d S T P . .
C1 C 0.5683(3) 0.5444(2) 0.0697(3) 0.0193(10) Uani 1 1 d . . . . .
H1 H 0.537791 0.514086 0.086005 0.023 Uiso 1 1 calc R U . . .
C2 C 0.6083(4) 0.5455(3) -0.0125(4) 0.0262(12) Uani 1 1 d . . . . .
H2 H 0.607742 0.516483 -0.050472 0.031 Uiso 1 1 calc R U . . .
C3 C 0.6491(3) 0.59025(19) -0.0377(3) 0.0284(10) Uani 1 1 d . . . . .
H3 H 0.676247 0.592880 -0.094604 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6505(2) 0.63108(14) 0.0198(2) 0.0244(8) Uani 1 1 d . . . . .
H4 H 0.678307 0.662093 0.002463 0.029 Uiso 1 1 calc R U . . .
C5 C 0.61064(19) 0.62709(13) 0.10496(19) 0.0176(7) Uani 1 1 d . . . . .
C6 C 0.6623(2) 0.70682(13) 0.1657(2) 0.0163(7) Uani 1 1 d . . . . .
C7 C 0.7508(2) 0.70538(16) 0.1386(3) 0.0256(9) Uani 1 1 d . . . . .
H7 H 0.775888 0.674574 0.116610 0.031 Uiso 1 1 calc R U . . .
C8 C 0.8014(5) 0.74947(13) 0.1441(5) 0.0286(18) Uani 1 1 d . . . . .
H8 H 0.861241 0.749174 0.124542 0.034 Uiso 1 1 calc R U . . .
C9 C 0.7651(2) 0.79384(16) 0.1782(2) 0.0222(9) Uani 1 1 d . . . . .
H9 H 0.798823 0.824470 0.179542 0.027 Uiso 1 1 calc R U . . .
C10 C 0.6779(2) 0.79331(14) 0.2107(2) 0.0162(7) Uani 1 1 d . . . . .
C11 C 0.67942(19) 0.87433(13) 0.28540(19) 0.0158(6) Uani 1 1 d . . . . .
C12 C 0.76359(19) 0.87146(13) 0.3257(2) 0.0200(7) Uani 1 1 d . . . . .
H12 H 0.794711 0.839907 0.326618 0.024 Uiso 1 1 calc R U . . .
C13 C 0.8007(3) 0.91411(18) 0.3636(2) 0.0237(9) Uani 1 1 d . . . . .
H13 H 0.857430 0.912215 0.390694 0.028 Uiso 1 1 calc R U . . .
C14 C 0.7548(3) 0.9600(3) 0.3620(3) 0.0224(11) Uani 1 1 d . . . . .
H14 H 0.780287 0.990091 0.386377 0.027 Uiso 1 1 calc R U . . .
C15 C 0.6719(3) 0.9613(3) 0.3247(3) 0.0205(10) Uani 1 1 d . . . . .
H15 H 0.640124 0.992615 0.324521 0.025 Uiso 1 1 calc R U . . .
C16 C 0.6793(3) 0.5441(3) 0.3124(4) 0.0242(12) Uani 1 1 d . . . . .
H16 H 0.661961 0.513629 0.282828 0.029 Uiso 1 1 calc R U . . .
C17 C 0.7622(4) 0.5470(3) 0.3486(4) 0.0308(13) Uani 1 1 d . . . . .
H17 H 0.802053 0.519060 0.343596 0.037 Uiso 1 1 calc R U . . .
C18 C 0.7875(3) 0.5916(2) 0.3929(3) 0.0293(11) Uani 1 1 d . . . . .
H18 H 0.844715 0.594153 0.418823 0.035 Uiso 1 1 calc R U . . .
C19 C 0.7294(2) 0.63140(14) 0.3987(2) 0.0250(8) Uani 1 1 d . . . . .
H19 H 0.746139 0.661884 0.428636 0.030 Uiso 1 1 calc R U . . .
C20 C 0.64439(19) 0.62724(13) 0.36001(19) 0.0168(6) Uani 1 1 d . . . . .
C21 C 0.5833(2) 0.70683(14) 0.4138(2) 0.0169(7) Uani 1 1 d . . . . .
C22 C 0.6113(3) 0.70587(17) 0.5027(2) 0.0256(9) Uani 1 1 d . . . . .
H22 H 0.633965 0.675344 0.528272 0.031 Uiso 1 1 calc R U . . .
C23 C 0.6055(5) 0.74985(12) 0.5520(5) 0.0284(18) Uani 1 1 d . . . . .
H23 H 0.626011 0.749806 0.611770 0.034 Uiso 1 1 calc R U . . .
C24 C 0.5706(2) 0.79394(16) 0.5169(2) 0.0233(9) Uani 1 1 d . . . . .
H24 H 0.568057 0.824325 0.551430 0.028 Uiso 1 1 calc R U . . .
C25 C 0.5387(2) 0.79328(13) 0.4285(2) 0.0154(7) Uani 1 1 d . . . . .
C26 C 0.46386(18) 0.87434(13) 0.42981(19) 0.0170(7) Uani 1 1 d . . . . .
C27 C 0.4226(2) 0.87165(14) 0.5141(2) 0.0224(7) Uani 1 1 d . . . . .
H27 H 0.421500 0.840234 0.545734 0.027 Uiso 1 1 calc R U . . .
C28 C 0.3844(3) 0.9142(2) 0.5500(3) 0.0254(10) Uani 1 1 d . . . . .
H28 H 0.355626 0.912454 0.606162 0.031 Uiso 1 1 calc R U . . .
C29 C 0.3879(4) 0.9598(3) 0.5041(4) 0.0301(12) Uani 1 1 d . . . . .
H29 H 0.363408 0.990181 0.528528 0.036 Uiso 1 1 calc R U . . .
C30 C 0.4275(4) 0.9599(3) 0.4228(4) 0.0234(11) Uani 1 1 d . . . . .
H30 H 0.430117 0.991489 0.391568 0.028 Uiso 1 1 calc R U . . .
C31 C 0.500000 0.44624(19) 0.250000 0.0263(9) Uani 1 2 d S T P . .
C32 C 0.500000 1.05286(19) 0.250000 0.0259(9) Uani 1 2 d S T P . .


_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
Cr1 N6 2.098(3) . ?
Cr1 N6 2.098(3) 2_655 ?
Cr1 N1 2.117(3) . ?
Cr1 N1 2.117(3) 2_655 ?
Cr1 N11 2.188(4) . ?
Cr1 Cr2 2.4954(10) . ?
Cr2 Cr3 1.9994(11) . ?
Cr2 N7 2.027(2) 2_655 ?
Cr2 N7 2.027(2) . ?
Cr2 N2 2.027(2) 2_655 ?
Cr2 N2 2.027(2) . ?
Cr3 N3 2.054(6) . ?
Cr3 N3 2.054(6) 2_655 ?
Cr3 N8 2.067(5) . ?
Cr3 N8 2.067(5) 2_655 ?
Cr3 Cr4 2.4940(11) . ?
Cr4 N4 2.034(2) 2_655 ?
Cr4 N4 2.034(2) . ?
Cr4 N9 2.035(2) 2_655 ?
Cr4 N9 2.035(2) . ?
Cr4 Cr5 2.0609(10) . ?
Cr5 N10 2.086(3) 2_655 ?
Cr5 N10 2.086(3) . ?
Cr5 N5 2.090(3) . ?
Cr5 N5 2.090(3) 2_655 ?
Cr5 N12 2.312(4) . ?
S1 C31 1.637(5) . ?
S2 C32 1.632(5) . ?
N1 C1 1.336(7) . ?
N1 C5 1.363(5) . ?
N2 C5 1.371(4) . ?
N2 C6 1.377(4) . ?
N3 C10 1.364(5) . ?
N3 C6 1.372(5) . ?
N4 C11 1.372(4) . ?
N4 C10 1.379(4) . ?
N5 C11 1.359(5) . ?
N5 C15 1.371(7) . ?
N6 C20 1.356(5) . ?
N6 C16 1.363(7) . ?
N7 C20 1.374(4) . ?
N7 C21 1.377(4) . ?
N8 C25 1.357(5) . ?
N8 C21 1.361(5) . ?
N9 C25 1.372(4) . ?
N9 C26 1.375(4) . ?
N10 C30 1.330(7) . ?
N10 C26 1.361(5) . ?
N11 C31 1.165(5) . ?
N12 C32 1.157(5) . ?
C1 C2 1.375(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.376(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.418(4) . ?
C4 H4 0.9500 . ?
C6 C7 1.398(5) . ?
C7 C8 1.387(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.405(5) . ?
C9 H9 0.9500 . ?
C11 C12 1.410(4) . ?
C12 C13 1.372(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.367(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.396(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.365(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.413(4) . ?
C19 H19 0.9500 . ?
C21 C22 1.401(5) . ?
C22 C23 1.371(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.412(5) . ?
C24 H24 0.9500 . ?
C26 C27 1.412(4) . ?
C27 C28 1.366(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.378(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.361(8) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cr1 N6 166.8(2) . 2_655 ?
N6 Cr1 N1 88.69(14) . . ?
N6 Cr1 N1 89.93(14) 2_655 . ?
N6 Cr1 N1 89.93(14) . 2_655 ?
N6 Cr1 N1 88.69(14) 2_655 2_655 ?
N1 Cr1 N1 168.0(2) . 2_655 ?
N6 Cr1 N11 96.62(11) . . ?
N6 Cr1 N11 96.62(11) 2_655 . ?
N1 Cr1 N11 96.01(10) . . ?
N1 Cr1 N11 96.01(10) 2_655 . ?
N6 Cr1 Cr2 83.38(11) . . ?
N6 Cr1 Cr2 83.38(11) 2_655 . ?
N1 Cr1 Cr2 83.99(10) . . ?
N1 Cr1 Cr2 83.99(10) 2_655 . ?
N11 Cr1 Cr2 180.0 . . ?
Cr3 Cr2 N7 92.72(8) . 2_655 ?
Cr3 Cr2 N7 92.72(8) . . ?
N7 Cr2 N7 174.56(16) 2_655 . ?
Cr3 Cr2 N2 92.71(8) . 2_655 ?
N7 Cr2 N2 90.23(11) 2_655 2_655 ?
N7 Cr2 N2 89.51(11) . 2_655 ?
Cr3 Cr2 N2 92.71(8) . . ?
N7 Cr2 N2 89.51(11) 2_655 . ?
N7 Cr2 N2 90.23(11) . . ?
N2 Cr2 N2 174.57(16) 2_655 . ?
Cr3 Cr2 Cr1 180.0 . . ?
N7 Cr2 Cr1 87.28(8) 2_655 . ?
N7 Cr2 Cr1 87.28(8) . . ?
N2 Cr2 Cr1 87.29(8) 2_655 . ?
N2 Cr2 Cr1 87.29(8) . . ?
Cr2 Cr3 N3 92.96(7) . . ?
Cr2 Cr3 N3 92.96(7) . 2_655 ?
N3 Cr3 N3 174.07(13) . 2_655 ?
Cr2 Cr3 N8 92.89(7) . . ?
N3 Cr3 N8 89.7(3) . . ?
N3 Cr3 N8 90.0(3) 2_655 . ?
Cr2 Cr3 N8 92.89(7) . 2_655 ?
N3 Cr3 N8 90.0(3) . 2_655 ?
N3 Cr3 N8 89.7(3) 2_655 2_655 ?
N8 Cr3 N8 174.22(13) . 2_655 ?
Cr2 Cr3 Cr4 180.0 . . ?
N3 Cr3 Cr4 87.04(7) . . ?
N3 Cr3 Cr4 87.04(7) 2_655 . ?
N8 Cr3 Cr4 87.11(7) . . ?
N8 Cr3 Cr4 87.11(7) 2_655 . ?
N4 Cr4 N4 169.37(16) 2_655 . ?
N4 Cr4 N9 89.56(11) 2_655 2_655 ?
N4 Cr4 N9 89.45(11) . 2_655 ?
N4 Cr4 N9 89.45(11) 2_655 . ?
N4 Cr4 N9 89.56(11) . . ?
N9 Cr4 N9 169.19(15) 2_655 . ?
N4 Cr4 Cr5 95.31(8) 2_655 . ?
N4 Cr4 Cr5 95.31(8) . . ?
N9 Cr4 Cr5 95.40(8) 2_655 . ?
N9 Cr4 Cr5 95.40(8) . . ?
N4 Cr4 Cr3 84.69(8) 2_655 . ?
N4 Cr4 Cr3 84.69(8) . . ?
N9 Cr4 Cr3 84.60(8) 2_655 . ?
N9 Cr4 Cr3 84.60(8) . . ?
Cr5 Cr4 Cr3 180.0 . . ?
Cr4 Cr5 N10 89.16(11) . 2_655 ?
Cr4 Cr5 N10 89.16(11) . . ?
N10 Cr5 N10 178.3(2) 2_655 . ?
Cr4 Cr5 N5 89.01(11) . . ?
N10 Cr5 N5 90.04(14) 2_655 . ?
N10 Cr5 N5 89.93(14) . . ?
Cr4 Cr5 N5 89.01(11) . 2_655 ?
N10 Cr5 N5 89.93(14) 2_655 2_655 ?
N10 Cr5 N5 90.04(14) . 2_655 ?
N5 Cr5 N5 178.0(2) . 2_655 ?
Cr4 Cr5 N12 180.0 . . ?
N10 Cr5 N12 90.84(11) 2_655 . ?
N10 Cr5 N12 90.84(11) . . ?
N5 Cr5 N12 90.99(11) . . ?
N5 Cr5 N12 90.99(11) 2_655 . ?
C1 N1 C5 118.3(4) . . ?
C1 N1 Cr1 119.1(3) . . ?
C5 N1 Cr1 122.5(2) . . ?
C5 N2 C6 122.3(3) . . ?
C5 N2 Cr2 120.2(2) . . ?
C6 N2 Cr2 117.1(2) . . ?
C10 N3 C6 120.3(5) . . ?
C10 N3 Cr3 122.5(3) . . ?
C6 N3 Cr3 117.1(3) . . ?
C11 N4 C10 121.4(3) . . ?
C11 N4 Cr4 114.8(2) . . ?
C10 N4 Cr4 123.8(2) . . ?
C11 N5 C15 119.0(4) . . ?
C11 N5 Cr5 120.2(3) . . ?
C15 N5 Cr5 120.4(3) . . ?
C20 N6 C16 119.5(4) . . ?
C20 N6 Cr1 123.6(3) . . ?
C16 N6 Cr1 116.8(3) . . ?
C20 N7 C21 122.9(3) . . ?
C20 N7 Cr2 119.2(2) . . ?
C21 N7 Cr2 117.3(2) . . ?
C25 N8 C21 121.3(4) . . ?
C25 N8 Cr3 121.5(3) . . ?
C21 N8 Cr3 117.1(3) . . ?
C25 N9 C26 122.0(3) . . ?
C25 N9 Cr4 123.7(2) . . ?
C26 N9 Cr4 114.2(2) . . ?
C30 N10 C26 118.1(4) . . ?
C30 N10 Cr5 121.4(3) . . ?
C26 N10 Cr5 120.0(2) . . ?
C31 N11 Cr1 180.0 . . ?
C32 N12 Cr5 180.0 . . ?
N1 C1 C2 124.9(6) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C1 C2 C3 117.5(5) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 N2 115.5(3) . . ?
N1 C5 C4 119.3(3) . . ?
N2 C5 C4 125.0(3) . . ?
N3 C6 N2 113.5(3) . . ?
N3 C6 C7 120.5(4) . . ?
N2 C6 C7 125.8(3) . . ?
C8 C7 C6 119.2(4) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.5(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N3 C10 N4 114.1(3) . . ?
N3 C10 C9 120.1(4) . . ?
N4 C10 C9 125.7(3) . . ?
N5 C11 N4 114.1(3) . . ?
N5 C11 C12 119.9(3) . . ?
N4 C11 C12 125.8(3) . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.5(4) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 119.0(6) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N5 C15 C14 122.3(6) . . ?
N5 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N6 C16 C17 122.1(6) . . ?
N6 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C16 C17 C18 119.1(5) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
N6 C20 N7 115.0(3) . . ?
N6 C20 C19 119.9(3) . . ?
N7 C20 C19 124.9(3) . . ?
N8 C21 N7 113.7(3) . . ?
N8 C21 C22 120.1(4) . . ?
N7 C21 C22 126.1(3) . . ?
C23 C22 C21 118.7(4) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 121.5(6) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C23 C24 C25 118.8(4) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
N8 C25 N9 115.1(3) . . ?
N8 C25 C24 119.5(4) . . ?
N9 C25 C24 125.3(3) . . ?
N10 C26 N9 114.4(3) . . ?
N10 C26 C27 119.6(3) . . ?
N9 C26 C27 125.9(3) . . ?
C28 C27 C26 120.0(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.4(4) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C30 C29 C28 117.9(6) . . ?
C30 C29 H29 121.0 . . ?
C28 C29 H29 121.0 . . ?
N10 C30 C29 124.8(6) . . ?
N10 C30 H30 117.6 . . ?
C29 C30 H30 117.6 . . ?
N11 C31 S1 180.0 . . ?
N12 C32 S2 180.0 . . ?

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
C5 N1 C1 C2 1.5(7) . . . . ?
Cr1 N1 C1 C2 178.2(4) . . . . ?
N1 C1 C2 C3 -2.7(8) . . . . ?
C1 C2 C3 C4 1.6(7) . . . . ?
C2 C3 C4 C5 0.4(6) . . . . ?
C1 N1 C5 N2 176.2(3) . . . . ?
Cr1 N1 C5 N2 -0.4(4) . . . . ?
C1 N1 C5 C4 0.7(5) . . . . ?
Cr1 N1 C5 C4 -175.9(2) . . . . ?
C6 N2 C5 N1 160.5(3) . . . . ?
Cr2 N2 C5 N1 -26.8(3) . . . . ?
C6 N2 C5 C4 -24.3(5) . . . . ?
Cr2 N2 C5 C4 148.4(3) . . . . ?
C3 C4 C5 N1 -1.7(5) . . . . ?
C3 C4 C5 N2 -176.7(3) . . . . ?
C10 N3 C6 N2 177.9(4) . . . . ?
Cr3 N3 C6 N2 -0.2(5) . . . . ?
C10 N3 C6 C7 3.0(7) . . . . ?
Cr3 N3 C6 C7 -175.1(3) . . . . ?
C5 N2 C6 N3 154.8(4) . . . . ?
Cr2 N2 C6 N3 -18.1(4) . . . . ?
C5 N2 C6 C7 -30.7(5) . . . . ?
Cr2 N2 C6 C7 156.4(3) . . . . ?
N3 C6 C7 C8 -4.5(7) . . . . ?
N2 C6 C7 C8 -178.7(5) . . . . ?
C6 C7 C8 C9 1.5(9) . . . . ?
C7 C8 C9 C10 2.8(9) . . . . ?
C6 N3 C10 N4 178.8(4) . . . . ?
Cr3 N3 C10 N4 -3.3(5) . . . . ?
C6 N3 C10 C9 1.5(7) . . . . ?
Cr3 N3 C10 C9 179.4(3) . . . . ?
C11 N4 C10 N3 159.5(4) . . . . ?
Cr4 N4 C10 N3 -21.7(4) . . . . ?
C11 N4 C10 C9 -23.4(5) . . . . ?
Cr4 N4 C10 C9 155.4(3) . . . . ?
C8 C9 C10 N3 -4.4(7) . . . . ?
C8 C9 C10 N4 178.6(5) . . . . ?
C15 N5 C11 N4 179.2(3) . . . . ?
Cr5 N5 C11 N4 7.0(3) . . . . ?
C15 N5 C11 C12 3.8(5) . . . . ?
Cr5 N5 C11 C12 -168.4(2) . . . . ?
C10 N4 C11 N5 155.8(3) . . . . ?
Cr4 N4 C11 N5 -23.1(3) . . . . ?
C10 N4 C11 C12 -29.0(4) . . . . ?
Cr4 N4 C11 C12 152.1(2) . . . . ?
N5 C11 C12 C13 -2.9(5) . . . . ?
N4 C11 C12 C13 -177.8(3) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C12 C13 C14 C15 1.9(7) . . . . ?
C11 N5 C15 C14 -1.8(7) . . . . ?
Cr5 N5 C15 C14 170.4(4) . . . . ?
C13 C14 C15 N5 -1.0(8) . . . . ?
C20 N6 C16 C17 -0.5(7) . . . . ?
Cr1 N6 C16 C17 175.6(4) . . . . ?
N6 C16 C17 C18 0.7(9) . . . . ?
C16 C17 C18 C19 -0.5(8) . . . . ?
C17 C18 C19 C20 0.1(6) . . . . ?
C16 N6 C20 N7 175.4(4) . . . . ?
Cr1 N6 C20 N7 -0.5(4) . . . . ?
C16 N6 C20 C19 0.1(5) . . . . ?
Cr1 N6 C20 C19 -175.8(2) . . . . ?
C21 N7 C20 N6 161.2(3) . . . . ?
Cr2 N7 C20 N6 -27.8(3) . . . . ?
C21 N7 C20 C19 -23.8(5) . . . . ?
Cr2 N7 C20 C19 147.3(3) . . . . ?
C18 C19 C20 N6 0.1(5) . . . . ?
C18 C19 C20 N7 -174.7(3) . . . . ?
C25 N8 C21 N7 177.3(4) . . . . ?
Cr3 N8 C21 N7 0.5(5) . . . . ?
C25 N8 C21 C22 0.9(6) . . . . ?
Cr3 N8 C21 C22 -175.9(3) . . . . ?
C20 N7 C21 N8 152.8(4) . . . . ?
Cr2 N7 C21 N8 -18.4(4) . . . . ?
C20 N7 C21 C22 -31.1(5) . . . . ?
Cr2 N7 C21 C22 157.7(3) . . . . ?
N8 C21 C22 C23 -3.0(7) . . . . ?
N7 C21 C22 C23 -178.9(5) . . . . ?
C21 C22 C23 C24 1.9(9) . . . . ?
C22 C23 C24 C25 1.3(9) . . . . ?
C21 N8 C25 N9 179.5(4) . . . . ?
Cr3 N8 C25 N9 -4.0(5) . . . . ?
C21 N8 C25 C24 2.3(6) . . . . ?
Cr3 N8 C25 C24 178.9(3) . . . . ?
C26 N9 C25 N8 159.4(4) . . . . ?
Cr4 N9 C25 N8 -21.2(4) . . . . ?
C26 N9 C25 C24 -23.7(5) . . . . ?
Cr4 N9 C25 C24 155.7(3) . . . . ?
C23 C24 C25 N8 -3.4(6) . . . . ?
C23 C24 C25 N9 179.8(5) . . . . ?
C30 N10 C26 N9 -179.6(3) . . . . ?
Cr5 N10 C26 N9 8.6(3) . . . . ?
C30 N10 C26 C27 4.2(5) . . . . ?
Cr5 N10 C26 C27 -167.6(2) . . . . ?
C25 N9 C26 N10 155.1(3) . . . . ?
Cr4 N9 C26 N10 -24.4(3) . . . . ?
C25 N9 C26 C27 -29.0(4) . . . . ?
Cr4 N9 C26 C27 151.6(2) . . . . ?
N10 C26 C27 C28 -1.9(5) . . . . ?
N9 C26 C27 C28 -177.7(3) . . . . ?
C26 C27 C28 C29 -1.2(6) . . . . ?
C27 C28 C29 C30 2.0(7) . . . . ?
C26 N10 C30 C29 -3.5(7) . . . . ?
Cr5 N10 C30 C29 168.1(4) . . . . ?
C28 C29 C30 N10 0.4(8) . . . . ?

_refine_diff_density_max         0.789
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.072



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/CH2Cl2'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_ambient_after
_database_code_depnum_ccdc_archive 'CCDC 2208669'
loop_
_audit_author_name
_audit_author_address
'Andrea Cornia'
;University of Modena and Reggio Emilia
Italy
;
_audit_update_record             
;
2022-09-21 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_date             2022-09-17
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Cr5(C15H11N5)4(NCS)2]'
_chemical_formula_moiety         'C62 H44 Cr5 N22 S2'
_chemical_formula_sum            'C62 H44 Cr5 N22 S2'
_chemical_formula_weight         1421.31

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'
Cr Cr 0.3209 0.6236 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   15.2426(3)
_cell_length_b                   26.2039(7)
_cell_length_c                   15.2056(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.0060(10)
_cell_angle_gamma                90
_cell_volume                     6073.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    291.8
_cell_measurement_reflns_used    9538
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      26.35

_exptl_special_details           
;
Crystal mounted with low temperature epoxy resin to a graphite 
fibre to enable conduction cooling inside a vacuum chamber.
;
_exptl_crystal_preparation       
'Et2O vapour diffusion into a CH2Cl2 solution,Magnetic properties'
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_F_000             2888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.997
_shelx_estimated_absorpt_T_min   0.703
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.639976
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_process_details   
;
TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
Final HKLF 4 output contains 28556 reflections, Rint = 0.0347
(12553 with I > 3sig(I), Rint = 0.0303)
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      291.8
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'rotating anode'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0

_diffrn_reflns_number            5213
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.546
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.884
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_point_group_measured_fraction_full 0.884
_reflns_number_total             5213
_reflns_number_gt                3680
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WINGX publication routines v2020.2 (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²+6.2666P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5213
_refine_ls_number_parameters     417
_refine_ls_number_restraints     466
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.1159
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_special_details          
;Refined as a 2-component twin.
There is a minor instability in the displacement 
parameters of 1 N atom that limits the reduction in shift 
over esd. The model does not significantly change if 
this atom is refined isotropically, but for consistency it 
has been modelled as anisotropic with a small damping
factor on the least squares minimisation.
1. Twinned data refinement with scales 0.575(3) and 0.425(3)
2. Uiso(H) fixed at 1.2 Ueq(C) for all C(H) groups
3. Rigid body (RIGU) restraints for all non-hydrogen atoms with sigma 
   for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Aromatic/amide H refined with riding coordinates:
   C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
   C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), 
   C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),Twin
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.575(3)
2 0.425(3)

_vrf_PLAT029_ambient_after       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.884 Why?
RESPONSE: The sample was measured inside a closed cycle refrigerator
with limited access to reflection geometries. The data were collected 
using a single axis rotation.
;

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
Cr1 Cr 0.500000 0.57559(3) 0.250000 0.03940(19) Uani 1 2 d S T P . .
Cr2 Cr 0.500000 0.66782(3) 0.250000 0.03935(19) Uani 1 2 d S T P . .
Cr3 Cr 0.500000 0.74773(3) 0.250000 0.03508(17) Uani 1 2 d S T P . .
Cr4 Cr 0.500000 0.83928(3) 0.250000 0.03849(19) Uani 1 2 d S T P . .
Cr5 Cr 0.500000 0.92139(3) 0.250000 0.03804(19) Uani 1 2 d S T P . .
S1 S 0.500000 0.38562(6) 0.250000 0.0935(7) Uani 1 2 d S T P . .
S2 S 0.500000 1.11473(6) 0.250000 0.0929(6) Uani 1 2 d S T P . .
N1 N 0.5684(2) 0.58305(17) 0.1299(3) 0.0366(10) Uani 1 1 d . . . . .
N2 N 0.60314(18) 0.66627(11) 0.1662(2) 0.0361(7) Uani 1 1 d . . . . .
N3 N 0.6268(4) 0.75012(10) 0.2030(4) 0.0310(14) Uani 1 1 d . . . . .
N4 N 0.63285(18) 0.83417(11) 0.24706(19) 0.0328(7) Uani 1 1 d . . . . .
N5 N 0.6321(3) 0.91838(17) 0.2887(2) 0.0343(9) Uani 1 1 d . . . . .
N6 N 0.6200(3) 0.58372(18) 0.3169(3) 0.0382(10) Uani 1 1 d . . . . .
N7 N 0.58310(19) 0.66609(11) 0.35406(19) 0.0355(7) Uani 1 1 d . . . . .
N8 N 0.5464(4) 0.75011(10) 0.3771(4) 0.0295(13) Uani 1 1 d . . . . .
N9 N 0.50244(18) 0.83404(11) 0.38360(18) 0.0323(7) Uani 1 1 d . . . . .
N10 N 0.4621(2) 0.91866(17) 0.3817(3) 0.0348(9) Uani 1 1 d . . . . .
N11 N 0.500000 0.49135(17) 0.250000 0.0528(10) Uani 1 2 d S T P . .
N12 N 0.500000 1.00931(17) 0.250000 0.0515(10) Uani 1 2 d S T P . .
C1 C 0.5687(4) 0.5445(3) 0.0716(4) 0.0460(15) Uani 1 1 d . . . . .
H1 H 0.540066 0.514527 0.087337 0.055 Uiso 1 1 calc R U . . .
C2 C 0.6074(5) 0.5462(3) -0.0084(5) 0.0579(17) Uani 1 1 d . . . . .
H2 H 0.607385 0.517776 -0.045084 0.069 Uiso 1 1 calc R U . . .
C3 C 0.6467(4) 0.5907(3) -0.0339(4) 0.0682(19) Uani 1 1 d . . . . .
H3 H 0.672257 0.593295 -0.089289 0.082 Uiso 1 1 calc R U . . .
C4 C 0.6482(3) 0.63127(17) 0.0222(3) 0.0544(11) Uani 1 1 d . . . . .
H4 H 0.675029 0.661592 0.005226 0.065 Uiso 1 1 calc R U . . .
C5 C 0.6091(2) 0.62727(15) 0.1062(2) 0.0391(9) Uani 1 1 d . . . . .
C6 C 0.6604(3) 0.70683(16) 0.1667(3) 0.0368(10) Uani 1 1 d . . . . .
C7 C 0.7478(3) 0.7054(2) 0.1397(4) 0.0570(16) Uani 1 1 d . . . . .
H7 H 0.772348 0.675188 0.118981 0.068 Uiso 1 1 calc R U . . .
C8 C 0.7972(6) 0.74949(15) 0.1444(7) 0.068(3) Uani 1 1 d . . . . .
H8 H 0.855028 0.749238 0.124839 0.082 Uiso 1 1 calc R U . . .
C9 C 0.7617(3) 0.7939(2) 0.1777(4) 0.0507(15) Uani 1 1 d . . . . .
H9 H 0.794263 0.823940 0.178458 0.061 Uiso 1 1 calc R U . . .
C10 C 0.6758(2) 0.79305(17) 0.2102(3) 0.0334(9) Uani 1 1 d . . . . .
C11 C 0.6772(2) 0.87407(14) 0.2854(2) 0.0327(8) Uani 1 1 d . . . . .
C12 C 0.7606(2) 0.87089(16) 0.3251(3) 0.0451(10) Uani 1 1 d . . . . .
H12 H 0.790766 0.840039 0.325494 0.054 Uiso 1 1 calc R U . . .
C13 C 0.7974(4) 0.9135(2) 0.3634(4) 0.0524(15) Uani 1 1 d . . . . .
H13 H 0.852382 0.911507 0.389792 0.063 Uiso 1 1 calc R U . . .
C14 C 0.7523(4) 0.9592(3) 0.3623(4) 0.0479(14) Uani 1 1 d . . . . .
H14 H 0.777123 0.988569 0.385851 0.058 Uiso 1 1 calc R U . . .
C15 C 0.6699(4) 0.9603(3) 0.3258(4) 0.0412(13) Uani 1 1 d . . . . .
H15 H 0.638808 0.990870 0.326279 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6769(4) 0.5443(3) 0.3124(4) 0.0498(16) Uani 1 1 d . . . . .
H16 H 0.659887 0.514506 0.283781 0.060 Uiso 1 1 calc R U . . .
C17 C 0.7585(5) 0.5468(3) 0.3487(5) 0.072(2) Uani 1 1 d . . . . .
H17 H 0.796594 0.519100 0.344903 0.086 Uiso 1 1 calc R U . . .
C18 C 0.7843(4) 0.5914(3) 0.3916(5) 0.070(2) Uani 1 1 d . . . . .
H18 H 0.839737 0.593756 0.416829 0.084 Uiso 1 1 calc R U . . .
C19 C 0.7277(3) 0.63128(18) 0.3963(3) 0.0584(12) Uani 1 1 d . . . . .
H19 H 0.744539 0.661272 0.424339 0.070 Uiso 1 1 calc R U . . .
C20 C 0.6432(2) 0.62725(15) 0.3587(2) 0.0373(8) Uani 1 1 d . . . . .
C21 C 0.5830(3) 0.70675(17) 0.4116(3) 0.0383(10) Uani 1 1 d . . . . .
C22 C 0.6102(4) 0.7063(2) 0.4994(4) 0.0606(17) Uani 1 1 d . . . . .
H22 H 0.631774 0.676401 0.524394 0.073 Uiso 1 1 calc R U . . .
C23 C 0.6049(7) 0.74959(16) 0.5482(6) 0.062(3) Uani 1 1 d . . . . .
H23 H 0.624818 0.749403 0.606008 0.075 Uiso 1 1 calc R U . . .
C24 C 0.5709(3) 0.7934(2) 0.5136(4) 0.0518(14) Uani 1 1 d . . . . .
H24 H 0.569065 0.823069 0.547094 0.062 Uiso 1 1 calc R U . . .
C25 C 0.5388(3) 0.79334(17) 0.4272(3) 0.0355(9) Uani 1 1 d . . . . .
C26 C 0.4641(2) 0.87396(14) 0.4277(2) 0.0342(8) Uani 1 1 d . . . . .
C27 C 0.4233(3) 0.87139(17) 0.5112(3) 0.0477(10) Uani 1 1 d . . . . .
H27 H 0.422255 0.840711 0.541950 0.057 Uiso 1 1 calc R U . . .
C28 C 0.3861(4) 0.9134(3) 0.5462(4) 0.0548(15) Uani 1 1 d . . . . .
H28 H 0.359381 0.911716 0.601115 0.066 Uiso 1 1 calc R U . . .
C29 C 0.3877(5) 0.9584(3) 0.5010(5) 0.0588(17) Uani 1 1 d . . . . .
H29 H 0.363170 0.987843 0.524737 0.071 Uiso 1 1 calc R U . . .
C30 C 0.4257(4) 0.9589(3) 0.4213(4) 0.0471(15) Uani 1 1 d . . . . .
H30 H 0.426815 0.989829 0.391268 0.057 Uiso 1 1 calc R U . . .
C31 C 0.500000 0.4477(2) 0.250000 0.0529(13) Uani 1 2 d S T P . .
C32 C 0.500000 1.0529(2) 0.250000 0.0509(12) Uani 1 2 d S T P . .


_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
Cr1 N6 2.103(4) . ?
Cr1 N6 2.103(4) 2_655 ?
Cr1 N1 2.112(4) . ?
Cr1 N1 2.112(4) 2_655 ?
Cr1 N11 2.207(4) . ?
Cr1 Cr2 2.4167(10) . ?
Cr2 N2 2.024(3) 2_655 ?
Cr2 N2 2.024(3) . ?
Cr2 N7 2.027(3) 2_655 ?
Cr2 N7 2.027(3) . ?
Cr2 Cr3 2.0940(11) . ?
Cr3 N8 2.058(6) . ?
Cr3 N8 2.058(6) 2_655 ?
Cr3 N3 2.062(6) . ?
Cr3 N3 2.062(6) 2_655 ?
Cr3 Cr4 2.3990(11) . ?
Cr4 N4 2.030(3) 2_655 ?
Cr4 N4 2.030(3) . ?
Cr4 N9 2.036(3) 2_655 ?
Cr4 N9 2.036(3) . ?
Cr4 Cr5 2.1517(10) . ?
Cr5 N10 2.086(4) 2_655 ?
Cr5 N10 2.086(4) . ?
Cr5 N5 2.099(4) 2_655 ?
Cr5 N5 2.099(4) . ?
Cr5 N12 2.304(4) . ?
S1 C31 1.627(6) . ?
S2 C32 1.621(6) . ?
N1 C1 1.344(8) . ?
N1 C5 1.363(6) . ?
N2 C5 1.373(5) . ?
N2 C6 1.376(5) . ?
N3 C10 1.354(6) . ?
N3 C6 1.362(5) . ?
N4 C11 1.375(4) . ?
N4 C10 1.379(5) . ?
N5 C11 1.351(5) . ?
N5 C15 1.363(8) . ?
N6 C16 1.352(8) . ?
N6 C20 1.353(6) . ?
N7 C20 1.371(4) . ?
N7 C21 1.379(5) . ?
N8 C25 1.370(6) . ?
N8 C21 1.371(6) . ?
N9 C25 1.372(5) . ?
N9 C26 1.373(4) . ?
N10 C30 1.335(8) . ?
N10 C26 1.364(6) . ?
N11 C31 1.144(6) . ?
N12 C32 1.142(6) . ?
C1 C2 1.353(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.368(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.364(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.413(5) . ?
C4 H4 0.9300 . ?
C6 C7 1.394(6) . ?
C7 C8 1.382(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.381(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.400(6) . ?
C9 H9 0.9300 . ?
C11 C12 1.409(5) . ?
C12 C13 1.379(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.381(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.362(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.357(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.414(5) . ?
C19 H19 0.9300 . ?
C21 C22 1.398(7) . ?
C22 C23 1.358(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.365(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.402(6) . ?
C24 H24 0.9300 . ?
C26 C27 1.415(5) . ?
C27 C28 1.348(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.365(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.344(9) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cr1 N6 168.4(3) . 2_655 ?
N6 Cr1 N1 88.80(18) . . ?
N6 Cr1 N1 90.12(18) 2_655 . ?
N6 Cr1 N1 90.12(18) . 2_655 ?
N6 Cr1 N1 88.80(18) 2_655 2_655 ?
N1 Cr1 N1 169.4(2) . 2_655 ?
N6 Cr1 N11 95.81(13) . . ?
N6 Cr1 N11 95.81(13) 2_655 . ?
N1 Cr1 N11 95.31(12) . . ?
N1 Cr1 N11 95.31(12) 2_655 . ?
N6 Cr1 Cr2 84.19(13) . . ?
N6 Cr1 Cr2 84.19(13) 2_655 . ?
N1 Cr1 Cr2 84.69(12) . . ?
N1 Cr1 Cr2 84.69(12) 2_655 . ?
N11 Cr1 Cr2 180.0 . . ?
N2 Cr2 N2 177.70(17) 2_655 . ?
N2 Cr2 N7 90.32(14) 2_655 2_655 ?
N2 Cr2 N7 89.63(14) . 2_655 ?
N2 Cr2 N7 89.63(14) 2_655 . ?
N2 Cr2 N7 90.32(14) . . ?
N7 Cr2 N7 177.44(17) 2_655 . ?
N2 Cr2 Cr3 91.15(9) 2_655 . ?
N2 Cr2 Cr3 91.15(9) . . ?
N7 Cr2 Cr3 91.28(9) 2_655 . ?
N7 Cr2 Cr3 91.28(9) . . ?
N2 Cr2 Cr1 88.85(9) 2_655 . ?
N2 Cr2 Cr1 88.85(9) . . ?
N7 Cr2 Cr1 88.72(9) 2_655 . ?
N7 Cr2 Cr1 88.72(9) . . ?
Cr3 Cr2 Cr1 180.0 . . ?
N8 Cr3 N8 176.52(15) . 2_655 ?
N8 Cr3 N3 90.1(3) . . ?
N8 Cr3 N3 89.8(3) 2_655 . ?
N8 Cr3 N3 89.8(3) . 2_655 ?
N8 Cr3 N3 90.1(3) 2_655 2_655 ?
N3 Cr3 N3 176.51(15) . 2_655 ?
N8 Cr3 Cr2 91.74(7) . . ?
N8 Cr3 Cr2 91.74(7) 2_655 . ?
N3 Cr3 Cr2 91.75(7) . . ?
N3 Cr3 Cr2 91.75(7) 2_655 . ?
N8 Cr3 Cr4 88.26(7) . . ?
N8 Cr3 Cr4 88.26(7) 2_655 . ?
N3 Cr3 Cr4 88.25(7) . . ?
N3 Cr3 Cr4 88.25(7) 2_655 . ?
Cr2 Cr3 Cr4 180.0 . . ?
N4 Cr4 N4 172.43(17) 2_655 . ?
N4 Cr4 N9 89.96(13) 2_655 2_655 ?
N4 Cr4 N9 89.53(13) . 2_655 ?
N4 Cr4 N9 89.53(13) 2_655 . ?
N4 Cr4 N9 89.96(13) . . ?
N9 Cr4 N9 172.27(17) 2_655 . ?
N4 Cr4 Cr5 93.78(9) 2_655 . ?
N4 Cr4 Cr5 93.78(9) . . ?
N9 Cr4 Cr5 93.86(8) 2_655 . ?
N9 Cr4 Cr5 93.86(8) . . ?
N4 Cr4 Cr3 86.22(9) 2_655 . ?
N4 Cr4 Cr3 86.22(9) . . ?
N9 Cr4 Cr3 86.14(8) 2_655 . ?
N9 Cr4 Cr3 86.14(8) . . ?
Cr5 Cr4 Cr3 180.0 . . ?
N10 Cr5 N10 176.1(3) 2_655 . ?
N10 Cr5 N5 89.70(18) 2_655 2_655 ?
N10 Cr5 N5 90.15(18) . 2_655 ?
N10 Cr5 N5 90.15(18) 2_655 . ?
N10 Cr5 N5 89.70(18) . . ?
N5 Cr5 N5 175.7(2) 2_655 . ?
N10 Cr5 Cr4 88.03(13) 2_655 . ?
N10 Cr5 Cr4 88.03(13) . . ?
N5 Cr5 Cr4 87.85(12) 2_655 . ?
N5 Cr5 Cr4 87.85(12) . . ?
N10 Cr5 N12 91.97(13) 2_655 . ?
N10 Cr5 N12 91.97(13) . . ?
N5 Cr5 N12 92.15(12) 2_655 . ?
N5 Cr5 N12 92.15(12) . . ?
Cr4 Cr5 N12 180.0 . . ?
C1 N1 C5 117.6(5) . . ?
C1 N1 Cr1 120.1(4) . . ?
C5 N1 Cr1 122.2(3) . . ?
C5 N2 C6 122.5(3) . . ?
C5 N2 Cr2 119.0(2) . . ?
C6 N2 Cr2 118.3(2) . . ?
C10 N3 C6 121.2(5) . . ?
C10 N3 Cr3 120.9(3) . . ?
C6 N3 Cr3 117.9(3) . . ?
C11 N4 C10 122.2(3) . . ?
C11 N4 Cr4 115.5(2) . . ?
C10 N4 Cr4 122.3(2) . . ?
C11 N5 C15 119.6(4) . . ?
C11 N5 Cr5 120.7(3) . . ?
C15 N5 Cr5 119.4(4) . . ?
C16 N6 C20 120.0(5) . . ?
C16 N6 Cr1 117.2(4) . . ?
C20 N6 Cr1 122.7(3) . . ?
C20 N7 C21 122.8(3) . . ?
C20 N7 Cr2 118.3(2) . . ?
C21 N7 Cr2 118.5(2) . . ?
C25 N8 C21 120.4(5) . . ?
C25 N8 Cr3 121.2(3) . . ?
C21 N8 Cr3 118.3(3) . . ?
C25 N9 C26 121.9(3) . . ?
C25 N9 Cr4 122.8(2) . . ?
C26 N9 Cr4 115.4(2) . . ?
C30 N10 C26 117.2(5) . . ?
C30 N10 Cr5 121.4(4) . . ?
C26 N10 Cr5 121.0(3) . . ?
C31 N11 Cr1 180.0 . . ?
C32 N12 Cr5 180.0 . . ?
N1 C1 C2 124.8(7) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C1 C2 C3 118.3(6) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 119.7(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.0(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 N2 115.3(3) . . ?
N1 C5 C4 119.6(4) . . ?
N2 C5 C4 125.0(4) . . ?
N3 C6 N2 114.0(4) . . ?
N3 C6 C7 120.1(4) . . ?
N2 C6 C7 125.7(4) . . ?
C8 C7 C6 118.9(5) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C9 C8 C7 120.7(8) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 118.9(6) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N3 C10 N4 114.9(4) . . ?
N3 C10 C9 120.0(4) . . ?
N4 C10 C9 125.1(4) . . ?
N5 C11 N4 114.8(3) . . ?
N5 C11 C12 119.6(4) . . ?
N4 C11 C12 125.5(3) . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.6(5) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
N5 C15 C14 122.4(6) . . ?
N5 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N6 C16 C17 122.0(6) . . ?
N6 C16 H16 119.0 . . ?
C17 C16 H16 119.0 . . ?
C16 C17 C18 119.1(7) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C19 C18 C17 119.4(6) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 120.0(5) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
N6 C20 N7 115.3(3) . . ?
N6 C20 C19 119.4(4) . . ?
N7 C20 C19 125.0(4) . . ?
N8 C21 N7 113.4(4) . . ?
N8 C21 C22 119.6(5) . . ?
N7 C21 C22 126.8(4) . . ?
C23 C22 C21 119.8(6) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 121.0(8) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C25 119.5(6) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N8 C25 N9 114.1(4) . . ?
N8 C25 C24 119.5(5) . . ?
N9 C25 C24 126.3(4) . . ?
N10 C26 N9 114.4(3) . . ?
N10 C26 C27 119.4(4) . . ?
N9 C26 C27 126.1(4) . . ?
C28 C27 C26 120.0(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0(6) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 118.1(7) . . ?
C30 C29 H29 121.0 . . ?
C28 C29 H29 121.0 . . ?
N10 C30 C29 125.3(7) . . ?
N10 C30 H30 117.4 . . ?
C29 C30 H30 117.4 . . ?
N11 C31 S1 180.0 . . ?
N12 C32 S2 180.0 . . ?

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
C5 N1 C1 C2 1.0(9) . . . . ?
Cr1 N1 C1 C2 177.3(5) . . . . ?
N1 C1 C2 C3 -2.6(11) . . . . ?
C1 C2 C3 C4 2.0(10) . . . . ?
C2 C3 C4 C5 -0.2(9) . . . . ?
C1 N1 C5 N2 176.8(4) . . . . ?
Cr1 N1 C5 N2 0.6(5) . . . . ?
C1 N1 C5 C4 0.9(6) . . . . ?
Cr1 N1 C5 C4 -175.2(3) . . . . ?
C6 N2 C5 N1 159.6(4) . . . . ?
Cr2 N2 C5 N1 -26.2(4) . . . . ?
C6 N2 C5 C4 -24.8(6) . . . . ?
Cr2 N2 C5 C4 149.4(3) . . . . ?
C3 C4 C5 N1 -1.3(7) . . . . ?
C3 C4 C5 N2 -176.8(5) . . . . ?
C10 N3 C6 N2 178.5(5) . . . . ?
Cr3 N3 C6 N2 0.2(6) . . . . ?
C10 N3 C6 C7 2.9(8) . . . . ?
Cr3 N3 C6 C7 -175.4(4) . . . . ?
C5 N2 C6 N3 154.6(4) . . . . ?
Cr2 N2 C6 N3 -19.7(5) . . . . ?
C5 N2 C6 C7 -30.1(6) . . . . ?
Cr2 N2 C6 C7 155.6(4) . . . . ?
N3 C6 C7 C8 -4.8(9) . . . . ?
N2 C6 C7 C8 -179.9(7) . . . . ?
C6 C7 C8 C9 2.0(13) . . . . ?
C7 C8 C9 C10 2.7(13) . . . . ?
C6 N3 C10 N4 179.0(5) . . . . ?
Cr3 N3 C10 N4 -2.7(6) . . . . ?
C6 N3 C10 C9 1.9(8) . . . . ?
Cr3 N3 C10 C9 -179.8(4) . . . . ?
C11 N4 C10 N3 158.2(4) . . . . ?
Cr4 N4 C10 N3 -20.8(5) . . . . ?
C11 N4 C10 C9 -24.9(6) . . . . ?
Cr4 N4 C10 C9 156.1(4) . . . . ?
C8 C9 C10 N3 -4.7(9) . . . . ?
C8 C9 C10 N4 178.5(6) . . . . ?
C15 N5 C11 N4 179.8(4) . . . . ?
Cr5 N5 C11 N4 6.3(4) . . . . ?
C15 N5 C11 C12 4.0(6) . . . . ?
Cr5 N5 C11 C12 -169.5(3) . . . . ?
C10 N4 C11 N5 156.6(3) . . . . ?
Cr4 N4 C11 N5 -24.4(4) . . . . ?
C10 N4 C11 C12 -27.9(5) . . . . ?
Cr4 N4 C11 C12 151.2(3) . . . . ?
N5 C11 C12 C13 -3.1(6) . . . . ?
N4 C11 C12 C13 -178.4(4) . . . . ?
C11 C12 C13 C14 -0.2(8) . . . . ?
C12 C13 C14 C15 2.4(9) . . . . ?
C11 N5 C15 C14 -1.7(8) . . . . ?
Cr5 N5 C15 C14 171.8(5) . . . . ?
C13 C14 C15 N5 -1.6(10) . . . . ?
C20 N6 C16 C17 -0.4(9) . . . . ?
Cr1 N6 C16 C17 175.9(6) . . . . ?
N6 C16 C17 C18 -0.1(12) . . . . ?
C16 C17 C18 C19 -0.1(12) . . . . ?
C17 C18 C19 C20 0.6(10) . . . . ?
C16 N6 C20 N7 175.6(5) . . . . ?
Cr1 N6 C20 N7 -0.3(5) . . . . ?
C16 N6 C20 C19 0.9(7) . . . . ?
Cr1 N6 C20 C19 -175.1(3) . . . . ?
C21 N7 C20 N6 160.9(4) . . . . ?
Cr2 N7 C20 N6 -26.3(4) . . . . ?
C21 N7 C20 C19 -24.7(6) . . . . ?
Cr2 N7 C20 C19 148.1(4) . . . . ?
C18 C19 C20 N6 -1.0(7) . . . . ?
C18 C19 C20 N7 -175.2(5) . . . . ?
C25 N8 C21 N7 177.8(4) . . . . ?
Cr3 N8 C21 N7 -0.3(6) . . . . ?
C25 N8 C21 C22 2.0(7) . . . . ?
Cr3 N8 C21 C22 -176.1(4) . . . . ?
C20 N7 C21 N8 153.7(4) . . . . ?
Cr2 N7 C21 N8 -19.0(5) . . . . ?
C20 N7 C21 C22 -30.9(6) . . . . ?
Cr2 N7 C21 C22 156.4(4) . . . . ?
N8 C21 C22 C23 -3.9(9) . . . . ?
N7 C21 C22 C23 -179.1(6) . . . . ?
C21 C22 C23 C24 2.1(12) . . . . ?
C22 C23 C24 C25 1.7(12) . . . . ?
C21 N8 C25 N9 178.8(4) . . . . ?
Cr3 N8 C25 N9 -3.1(6) . . . . ?
C21 N8 C25 C24 1.7(7) . . . . ?
Cr3 N8 C25 C24 179.8(4) . . . . ?
C26 N9 C25 N8 158.6(4) . . . . ?
Cr4 N9 C25 N8 -20.5(5) . . . . ?
C26 N9 C25 C24 -24.5(6) . . . . ?
Cr4 N9 C25 C24 156.3(4) . . . . ?
C23 C24 C25 N8 -3.6(8) . . . . ?
C23 C24 C25 N9 179.7(6) . . . . ?
C30 N10 C26 N9 -179.9(4) . . . . ?
Cr5 N10 C26 N9 7.6(4) . . . . ?
C30 N10 C26 C27 4.0(6) . . . . ?
Cr5 N10 C26 C27 -168.6(3) . . . . ?
C25 N9 C26 N10 155.8(3) . . . . ?
Cr4 N9 C26 N10 -24.9(4) . . . . ?
C25 N9 C26 C27 -28.4(6) . . . . ?
Cr4 N9 C26 C27 150.9(3) . . . . ?
N10 C26 C27 C28 -2.7(6) . . . . ?
N9 C26 C27 C28 -178.3(4) . . . . ?
C26 C27 C28 C29 0.0(8) . . . . ?
C27 C28 C29 C30 1.1(10) . . . . ?
C26 N10 C30 C29 -3.0(9) . . . . ?
Cr5 N10 C30 C29 169.5(6) . . . . ?
C28 C29 C30 N10 0.4(11) . . . . ?

_refine_diff_density_max         0.299
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.064



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/CH2Cl2'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
