# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2016

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

data_feaza105kd2
_database_code_depnum_ccdc_archive 'CCDC 1492627'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
          bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0064(8)
_cell_length_b                   14.3397(11)
_cell_length_c                   16.6293(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.918(5)
_cell_angle_gamma                90.00
_cell_volume                     3573.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    7666
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5416
_exptl_absorpt_correction_T_max  0.8924
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
               its'aim being to analyse the evolution of partial collection of data, 
               always carried out over the same part of reciprocal space, 
               and over a large scale of temperature.
               This  explain the poor completness of data as well as the low theta(max) value, 
               the low number of unique reflexions collected.
               In ordre to obtain significant intensities with an exposure time relatively short, 
               a crystal of neutron size was used. As the aim is to compare the diffraction data 
               always obtained from the same part of the crystal at different temperature, 
               problems of intensity scale are not considered to be of prior importance.
               The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
               over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
               these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
               or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
               but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5527
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         22.97
_reflns_number_total             3981
_reflns_number_gt                3481
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0218P)²+2.1134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3981
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0697
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29114(2) 0.28443(2) 0.06843(2) 0.01889(13) Uani 1 1 d . . .
S1 S 0.19511(4) 0.48777(4) -0.14301(4) 0.02431(18) Uani 1 1 d . . .
S2 S 0.42156(4) 0.07410(4) -0.10796(4) 0.02780(19) Uani 1 1 d . . .
N1 N 0.17743(13) 0.21969(12) 0.08034(12) 0.0186(5) Uani 1 1 d . . .
N2 N 0.27129(12) 0.37449(12) 0.15591(12) 0.0173(5) Uani 1 1 d . . .
C1 C 0.19384(15) 0.38081(15) 0.20324(15) 0.0182(6) Uani 1 1 d . . .
C2 C 0.41712(15) 0.18562(15) 0.18896(15) 0.0185(6) Uani 1 1 d . . .
C3 C 0.22325(15) 0.41692(17) -0.06801(17) 0.0205(6) Uani 1 1 d . . .
N3 N 0.32792(13) 0.19621(12) 0.15504(12) 0.0184(5) Uani 1 1 d . . .
C4 C 0.34068(16) 0.42228(15) 0.17950(15) 0.0207(6) Uani 1 1 d . . .
H4 H 0.3405 0.4623 0.2250 0.025 Uiso 1 1 calc R . .
C5 C 0.26330(16) 0.15202(15) 0.18616(15) 0.0197(6) Uani 1 1 d . . .
H5 H 0.2725 0.1138 0.2325 0.024 Uiso 1 1 calc R . .
N4 N 0.40639(12) 0.35062(13) 0.07077(12) 0.0212(5) Uani 1 1 d . . .
N5 N 0.32771(13) 0.19776(14) -0.01291(13) 0.0242(5) Uani 1 1 d . . .
C6 C 0.17554(15) 0.16401(15) 0.14626(15) 0.0195(6) Uani 1 1 d . . .
C7 C 0.03592(16) 0.40211(16) 0.20944(16) 0.0246(6) Uani 1 1 d . . .
H7 H -0.0209 0.4136 0.1835 0.030 Uiso 1 1 calc R . .
C8 C 0.11101(16) 0.39690(15) 0.16458(16) 0.0219(6) Uani 1 1 d . . .
H8 H 0.1059 0.4043 0.1078 0.026 Uiso 1 1 calc R . .
C9 C 0.04365(16) 0.39059(16) 0.29225(16) 0.0236(6) Uani 1 1 d . . .
C10 C 0.10175(17) 0.22834(16) 0.03480(16) 0.0229(6) Uani 1 1 d . . .
H10 H 0.1024 0.2650 -0.0128 0.027 Uiso 1 1 calc R . .
C11 C 0.48345(16) 0.15785(16) 0.13885(16) 0.0247(6) Uani 1 1 d . . .
H11 H 0.4690 0.1427 0.0841 0.030 Uiso 1 1 calc R . .
C12 C 0.36556(16) 0.14597(17) -0.05312(15) 0.0208(6) Uani 1 1 d . . .
C13 C 0.12609(17) 0.37579(17) 0.33004(16) 0.0286(7) Uani 1 1 d . . .
H13 H 0.1313 0.3699 0.3870 0.034 Uiso 1 1 calc R . .
C14 C 0.43809(16) 0.20789(15) 0.26894(15) 0.0217(6) Uani 1 1 d . . .
H14 H 0.3926 0.2276 0.3029 0.026 Uiso 1 1 calc R . .
C15 C 0.41885(15) 0.41157(16) 0.13271(15) 0.0217(6) Uani 1 1 d . . .
C16 C 0.52573(16) 0.20124(16) 0.29904(16) 0.0237(6) Uani 1 1 d . . .
H16 H 0.5404 0.2161 0.3538 0.028 Uiso 1 1 calc R . .
N6 N 0.70020(13) 0.15428(13) 0.34717(14) 0.0252(5) Uani 1 1 d . . .
C17 C 0.96986(17) 0.11410(16) 0.41879(17) 0.0269(6) Uani 1 1 d . . .
H17 H 1.0303 0.1019 0.4353 0.032 Uiso 1 1 calc R . .
N7 N 0.24277(13) 0.36774(14) -0.01442(13) 0.0226(5) Uani 1 1 d . . .
C18 C 0.09830(16) 0.12147(16) 0.16971(16) 0.0241(6) Uani 1 1 d . . .
H18 H 0.0988 0.0845 0.2171 0.029 Uiso 1 1 calc R . .
C19 C 0.59198(16) 0.17278(15) 0.24909(15) 0.0204(6) Uani 1 1 d . . .
N8 N 0.68444(13) 0.16291(13) 0.27283(14) 0.0236(5) Uani 1 1 d . . .
N9 N -0.10311(16) 0.39271(13) 0.30791(14) 0.0293(5) Uani 1 1 d . . .
N10 N -0.02970(16) 0.39782(14) 0.34547(14) 0.0308(6) Uani 1 1 d . . .
C20 C 0.02268(17) 0.18643(16) 0.05386(16) 0.0272(6) Uani 1 1 d . . .
H20 H -0.0295 0.1939 0.0197 0.033 Uiso 1 1 calc R . .
C21 C 0.79342(15) 0.14392(15) 0.36893(16) 0.0217(6) Uani 1 1 d . . .
C22 C 0.57034(16) 0.15245(16) 0.16929(16) 0.0246(6) Uani 1 1 d . . .
H22 H 0.6160 0.1345 0.1349 0.030 Uiso 1 1 calc R . .
C23 C 0.20132(16) 0.36943(16) 0.28597(15) 0.0252(6) Uani 1 1 d . . .
H23 H 0.2578 0.3573 0.3122 0.030 Uiso 1 1 calc R . .
C24 C 0.02043(17) 0.13363(17) 0.12302(16) 0.0272(6) Uani 1 1 d . . .
H24 H -0.0338 0.1061 0.1383 0.033 Uiso 1 1 calc R . .
C25 C 0.86133(16) 0.16315(16) 0.31671(16) 0.0268(6) Uani 1 1 d . . .
H25 H 0.8472 0.1862 0.2640 0.032 Uiso 1 1 calc R . .
C26 C 0.47352(16) 0.34026(17) 0.02132(16) 0.0286(6) Uani 1 1 d . . .
H26 H 0.4654 0.2994 -0.0234 0.034 Uiso 1 1 calc R . .
C27 C 0.90307(17) 0.09760(17) 0.47085(17) 0.0301(7) Uani 1 1 d . . .
H27 H 0.9175 0.0755 0.5238 0.036 Uiso 1 1 calc R . .
C28 C 0.94889(17) 0.14832(17) 0.34257(17) 0.0286(7) Uani 1 1 d . . .
H28 H 0.9953 0.1618 0.3076 0.034 Uiso 1 1 calc R . .
C29 C -0.17852(18) 0.40620(16) 0.35833(17) 0.0280(7) Uani 1 1 d . . .
C30 C 0.81456(16) 0.11335(16) 0.44576(16) 0.0273(6) Uani 1 1 d . . .
H30 H 0.7686 0.1029 0.4819 0.033 Uiso 1 1 calc R . .
C31 C 0.55383(17) 0.38624(18) 0.03244(18) 0.0353(7) Uani 1 1 d . . .
H31 H 0.5994 0.3776 -0.0045 0.042 Uiso 1 1 calc R . .
C32 C 0.49843(16) 0.45866(17) 0.14848(17) 0.0302(7) Uani 1 1 d . . .
H32 H 0.5055 0.4996 0.1933 0.036 Uiso 1 1 calc R . .
C33 C -0.33099(18) 0.43535(17) 0.44053(18) 0.0348(7) Uani 1 1 d . . .
H33 H -0.3838 0.4453 0.4685 0.042 Uiso 1 1 calc R . .
C34 C -0.26038(18) 0.39109(17) 0.32023(18) 0.0311(7) Uani 1 1 d . . .
H34 H -0.2646 0.3709 0.2658 0.037 Uiso 1 1 calc R . .
C35 C -0.33677(18) 0.40548(17) 0.36157(18) 0.0338(7) Uani 1 1 d . . .
H35 H -0.3936 0.3947 0.3354 0.041 Uiso 1 1 calc R . .
C36 C -0.24839(18) 0.45086(18) 0.47910(18) 0.0346(7) Uani 1 1 d . . .
H36 H -0.2445 0.4714 0.5335 0.042 Uiso 1 1 calc R . .
C37 C -0.17097(18) 0.43631(17) 0.43792(18) 0.0336(7) Uani 1 1 d . . .
H37 H -0.1139 0.4468 0.4638 0.040 Uiso 1 1 calc R . .
C38 C 0.56764(17) 0.44484(19) 0.09746(19) 0.0368(7) Uani 1 1 d . . .
H38 H 0.6234 0.4752 0.1072 0.044 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.937(2) . ?
Fe1 N5 1.937(2) . ?
Fe1 N1 1.9614(19) . ?
Fe1 N4 1.9716(19) . ?
Fe1 N3 1.9744(19) . ?
Fe1 N2 1.9791(19) . ?
S1 C3 1.647(3) . ?
S2 C12 1.636(3) . ?
N1 C10 1.338(3) . ?
N1 C6 1.358(3) . ?
N2 C4 1.291(3) . ?
N2 C1 1.439(3) . ?
C1 C23 1.384(3) . ?
C1 C8 1.389(3) . ?
C2 C14 1.388(3) . ?
C2 C11 1.389(3) . ?
C2 N3 1.434(3) . ?
C3 N7 1.162(3) . ?
N3 C5 1.289(3) . ?
C4 C15 1.448(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.454(3) . ?
C5 H5 0.9500 . ?
N4 C26 1.341(3) . ?
N4 C15 1.357(3) . ?
N5 C12 1.166(3) . ?
C6 C18 1.383(3) . ?
C7 C8 1.385(3) . ?
C7 C9 1.386(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.375(3) . ?
C9 N10 1.451(3) . ?
C10 C20 1.381(3) . ?
C10 H10 0.9500 . ?
C11 C22 1.377(3) . ?
C11 H11 0.9500 . ?
C13 C23 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C16 1.387(3) . ?
C14 H14 0.9500 . ?
C15 C32 1.385(3) . ?
C16 C19 1.389(3) . ?
C16 H16 0.9500 . ?
N6 N8 1.253(3) . ?
N6 C21 1.435(3) . ?
C17 C27 1.378(4) . ?
C17 C28 1.381(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.381(3) . ?
C18 H18 0.9500 . ?
C19 C22 1.381(3) . ?
C19 N8 1.430(3) . ?
N9 N10 1.241(3) . ?
N9 C29 1.455(3) . ?
C20 C24 1.379(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.373(4) . ?
C21 C25 1.400(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.378(3) . ?
C25 H25 0.9500 . ?
C26 C31 1.378(3) . ?
C26 H26 0.9500 . ?
C27 C30 1.390(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.370(4) . ?
C29 C37 1.391(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.377(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.388(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.380(4) . ?
C33 C36 1.384(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.394(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.47(8) . . ?
N7 Fe1 N1 93.86(8) . . ?
N5 Fe1 N1 92.63(8) . . ?
N7 Fe1 N4 90.78(8) . . ?
N5 Fe1 N4 92.47(8) . . ?
N1 Fe1 N4 173.07(8) . . ?
N7 Fe1 N3 174.23(8) . . ?
N5 Fe1 N3 91.13(8) . . ?
N1 Fe1 N3 80.53(8) . . ?
N4 Fe1 N3 94.68(8) . . ?
N7 Fe1 N2 93.17(8) . . ?
N5 Fe1 N2 172.17(8) . . ?
N1 Fe1 N2 94.03(8) . . ?
N4 Fe1 N2 80.56(8) . . ?
N3 Fe1 N2 85.92(8) . . ?
C10 N1 C6 117.4(2) . . ?
C10 N1 Fe1 128.07(17) . . ?
C6 N1 Fe1 114.45(16) . . ?
C4 N2 C1 117.5(2) . . ?
C4 N2 Fe1 114.87(15) . . ?
C1 N2 Fe1 126.80(15) . . ?
C23 C1 C8 120.3(2) . . ?
C23 C1 N2 120.6(2) . . ?
C8 C1 N2 119.1(2) . . ?
C14 C2 C11 120.4(2) . . ?
C14 C2 N3 120.9(2) . . ?
C11 C2 N3 118.5(2) . . ?
N7 C3 S1 179.2(2) . . ?
C5 N3 C2 119.8(2) . . ?
C5 N3 Fe1 114.83(16) . . ?
C2 N3 Fe1 125.13(15) . . ?
N2 C4 C15 116.3(2) . . ?
N2 C4 H4 121.8 . . ?
C15 C4 H4 121.8 . . ?
N3 C5 C6 116.2(2) . . ?
N3 C5 H5 121.9 . . ?
C6 C5 H5 121.9 . . ?
C26 N4 C15 117.3(2) . . ?
C26 N4 Fe1 128.34(17) . . ?
C15 N4 Fe1 114.33(15) . . ?
C12 N5 Fe1 166.59(19) . . ?
N1 C6 C18 122.6(2) . . ?
N1 C6 C5 112.5(2) . . ?
C18 C6 C5 124.9(2) . . ?
C8 C7 C9 120.0(2) . . ?
C8 C7 H7 120.0 . . ?
C9 C7 H7 120.0 . . ?
C7 C8 C1 119.5(2) . . ?
C7 C8 H8 120.2 . . ?
C1 C8 H8 120.2 . . ?
C13 C9 C7 120.0(2) . . ?
C13 C9 N10 115.2(2) . . ?
C7 C9 N10 124.7(2) . . ?
N1 C10 C20 123.0(2) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.3(2) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.2(2) . . ?
C9 C13 C23 120.6(2) . . ?
C9 C13 H13 119.7 . . ?
C23 C13 H13 119.7 . . ?
C16 C14 C2 119.6(2) . . ?
C16 C14 H14 120.2 . . ?
C2 C14 H14 120.2 . . ?
N4 C15 C32 122.8(2) . . ?
N4 C15 C4 113.1(2) . . ?
C32 C15 C4 124.1(2) . . ?
C14 C16 C19 119.9(2) . . ?
C14 C16 H16 120.0 . . ?
C19 C16 H16 120.0 . . ?
N8 N6 C21 113.1(2) . . ?
C27 C17 C28 119.9(2) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 172.11(19) . . ?
C24 C18 C6 118.9(2) . . ?
C24 C18 H18 120.6 . . ?
C6 C18 H18 120.6 . . ?
C22 C19 C16 119.7(2) . . ?
C22 C19 N8 114.9(2) . . ?
C16 C19 N8 125.3(2) . . ?
N6 N8 C19 114.4(2) . . ?
N10 N9 C29 113.5(2) . . ?
N9 N10 C9 111.7(2) . . ?
C24 C20 C10 119.2(2) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C30 C21 C25 120.0(2) . . ?
C30 C21 N6 116.4(2) . . ?
C25 C21 N6 123.7(2) . . ?
C11 C22 C19 120.9(2) . . ?
C11 C22 H22 119.6 . . ?
C19 C22 H22 119.6 . . ?
C13 C23 C1 119.5(2) . . ?
C13 C23 H23 120.2 . . ?
C1 C23 H23 120.2 . . ?
C20 C24 C18 118.8(2) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C28 C25 C21 119.3(2) . . ?
C28 C25 H25 120.4 . . ?
C21 C25 H25 120.4 . . ?
N4 C26 C31 123.0(2) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 119.9(3) . . ?
C17 C27 H27 120.1 . . ?
C30 C27 H27 120.1 . . ?
C25 C28 C17 120.7(2) . . ?
C25 C28 H28 119.6 . . ?
C17 C28 H28 119.6 . . ?
C34 C29 C37 121.1(2) . . ?
C34 C29 N9 114.7(3) . . ?
C37 C29 N9 124.2(3) . . ?
C21 C30 C27 120.2(2) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C38 C31 C26 119.5(2) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C15 C32 C38 118.6(3) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C35 C33 C36 120.1(2) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.6(3) . . ?
C29 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C33 C35 C34 120.4(3) . . ?
C33 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C33 C36 C37 119.8(3) . . ?
C33 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C29 C37 C36 119.0(3) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C31 C38 C32 118.7(2) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.802
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.802
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.039
####################################################################### 
# 
# 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_feaza110kd1
_database_code_depnum_ccdc_archive 'CCDC 1492628'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
   bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   14.9984(9)
_cell_length_b                   14.3524(10)
_cell_length_c                   16.6350(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.822(3)
_cell_angle_gamma                90.00
_cell_volume                     3576.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    4842
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5418
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
      its'aim being to analyse the evolution of partial collection of data, 
      always carried out over the same part of reciprocal space, 
      and over a large scale of temperature.
      This  explain the poor completness of data as well as the low theta(max) value, 
      the low number of unique reflexions collected.
      In ordre to obtain significant intensities with an exposure time relatively short, 
      a crystal of neutron size was used. As the aim is to compare the diffraction data 
      always obtained from the same part of the crystal at different temperature, 
      problems of intensity scale are not considered to be of prior importance.
      The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
      over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
      these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
      or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
      but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5635
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         21.27
_reflns_number_total             3366
_reflns_number_gt                3007
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0277P)²+1.8862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3366
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29137(2) 0.28443(3) 0.06835(2) 0.01974(16) Uani 1 1 d . . .
S1 S 0.19518(4) 0.48753(5) -0.14288(4) 0.0256(2) Uani 1 1 d . . .
S2 S 0.42163(4) 0.07421(5) -0.10807(4) 0.0296(2) Uani 1 1 d . . .
N1 N 0.17759(13) 0.21989(14) 0.08001(13) 0.0196(6) Uani 1 1 d . . .
N2 N 0.27123(13) 0.37421(15) 0.15595(12) 0.0175(5) Uani 1 1 d . . .
C1 C 0.19361(16) 0.38080(17) 0.20316(17) 0.0177(7) Uani 1 1 d . . .
C2 C 0.41729(16) 0.18543(18) 0.18918(17) 0.0193(7) Uani 1 1 d . . .
C3 C 0.22307(16) 0.4170(2) -0.06817(18) 0.0196(7) Uani 1 1 d . . .
N3 N 0.32799(13) 0.19621(14) 0.15473(12) 0.0181(5) Uani 1 1 d . . .
C4 C 0.34043(17) 0.42215(19) 0.17902(16) 0.0214(7) Uani 1 1 d . . .
H4 H 0.3400 0.4625 0.2243 0.026 Uiso 1 1 calc R . .
C5 C 0.26337(17) 0.15176(19) 0.18601(15) 0.0216(7) Uani 1 1 d . . .
H5 H 0.2725 0.1134 0.2322 0.026 Uiso 1 1 calc R . .
N4 N 0.40678(13) 0.35075(15) 0.07079(13) 0.0206(5) Uani 1 1 d . . .
N5 N 0.32789(14) 0.19782(17) -0.01300(14) 0.0260(6) Uani 1 1 d . . .
C6 C 0.17589(16) 0.16398(18) 0.14615(15) 0.0192(7) Uani 1 1 d . . .
C7 C 0.03616(17) 0.40185(18) 0.20877(19) 0.0248(7) Uani 1 1 d . . .
H7 H -0.0207 0.4128 0.1827 0.030 Uiso 1 1 calc R . .
C8 C 0.11106(16) 0.39707(18) 0.16444(16) 0.0219(7) Uani 1 1 d . . .
H8 H 0.1063 0.4049 0.1077 0.026 Uiso 1 1 calc R . .
C9 C 0.04385(17) 0.39069(18) 0.29170(19) 0.0244(7) Uani 1 1 d . . .
C10 C 0.10200(17) 0.22848(19) 0.03479(16) 0.0246(7) Uani 1 1 d . . .
H10 H 0.1025 0.2651 -0.0127 0.029 Uiso 1 1 calc R . .
C11 C 0.48374(17) 0.15779(19) 0.13891(16) 0.0254(7) Uani 1 1 d . . .
H11 H 0.4693 0.1428 0.0842 0.030 Uiso 1 1 calc R . .
C12 C 0.36588(16) 0.1463(2) -0.05317(16) 0.0208(7) Uani 1 1 d . . .
C13 C 0.12629(18) 0.3757(2) 0.32965(17) 0.0307(7) Uani 1 1 d . . .
H13 H 0.1315 0.3695 0.3866 0.037 Uiso 1 1 calc R . .
C14 C 0.43797(17) 0.20757(18) 0.26883(17) 0.0229(7) Uani 1 1 d . . .
H14 H 0.3924 0.2270 0.3028 0.027 Uiso 1 1 calc R . .
C15 C 0.41896(16) 0.4115(2) 0.13245(17) 0.0237(7) Uani 1 1 d . . .
C16 C 0.52571(17) 0.20127(19) 0.29894(17) 0.0246(7) Uani 1 1 d . . .
H16 H 0.5404 0.2163 0.3536 0.029 Uiso 1 1 calc R . .
N6 N 0.70006(13) 0.15436(16) 0.34714(16) 0.0265(6) Uani 1 1 d . . .
C17 C 0.96946(17) 0.11437(19) 0.41881(18) 0.0280(7) Uani 1 1 d . . .
H17 H 1.0298 0.1025 0.4356 0.034 Uiso 1 1 calc R . .
N7 N 0.24329(13) 0.36809(17) -0.01431(14) 0.0239(6) Uani 1 1 d . . .
C18 C 0.09866(16) 0.12157(19) 0.16960(16) 0.0246(7) Uani 1 1 d . . .
H18 H 0.0992 0.0848 0.2171 0.030 Uiso 1 1 calc R . .
C19 C 0.59197(16) 0.17287(19) 0.24891(17) 0.0219(7) Uani 1 1 d . . .
N8 N 0.68474(13) 0.16298(15) 0.27269(15) 0.0247(6) Uani 1 1 d . . .
N9 N -0.10262(16) 0.39271(16) 0.30783(14) 0.0318(6) Uani 1 1 d . . .
N10 N -0.02965(16) 0.39808(16) 0.34559(14) 0.0344(6) Uani 1 1 d . . .
C20 C 0.02297(17) 0.1863(2) 0.05416(17) 0.0284(7) Uani 1 1 d . . .
H20 H -0.0293 0.1939 0.0202 0.034 Uiso 1 1 calc R . .
C21 C 0.79391(16) 0.14388(19) 0.36904(17) 0.0227(7) Uani 1 1 d . . .
C22 C 0.57102(17) 0.15239(19) 0.16930(17) 0.0255(7) Uani 1 1 d . . .
H22 H 0.6169 0.1344 0.1351 0.031 Uiso 1 1 calc R . .
C23 C 0.20091(17) 0.36962(19) 0.28550(19) 0.0257(7) Uani 1 1 d . . .
H23 H 0.2575 0.3577 0.3116 0.031 Uiso 1 1 calc R . .
C24 C 0.02061(17) 0.1335(2) 0.12289(17) 0.0285(7) Uani 1 1 d . . .
H24 H -0.0335 0.1056 0.1380 0.034 Uiso 1 1 calc R . .
C25 C 0.86108(17) 0.16310(19) 0.31658(17) 0.0286(7) Uani 1 1 d . . .
H25 H 0.8468 0.1859 0.2639 0.034 Uiso 1 1 calc R . .
C26 C 0.47374(18) 0.3404(2) 0.02159(17) 0.0304(7) Uani 1 1 d . . .
H26 H 0.4657 0.2996 -0.0232 0.036 Uiso 1 1 calc R . .
C27 C 0.90251(18) 0.0976(2) 0.47054(17) 0.0308(8) Uani 1 1 d . . .
H27 H 0.9167 0.0751 0.5233 0.037 Uiso 1 1 calc R . .
C28 C 0.94905(17) 0.1484(2) 0.34264(18) 0.0300(7) Uani 1 1 d . . .
H28 H 0.9957 0.1619 0.3078 0.036 Uiso 1 1 calc R . .
C29 C -0.17882(19) 0.4059(2) 0.3585(2) 0.0308(8) Uani 1 1 d . . .
C30 C 0.81460(17) 0.11359(19) 0.44562(17) 0.0277(7) Uani 1 1 d . . .
H30 H 0.7684 0.1035 0.4818 0.033 Uiso 1 1 calc R . .
C31 C 0.55389(18) 0.3863(2) 0.0330(2) 0.0377(8) Uani 1 1 d . . .
H31 H 0.5996 0.3775 -0.0038 0.045 Uiso 1 1 calc R . .
C32 C 0.49845(17) 0.4584(2) 0.14845(17) 0.0325(8) Uani 1 1 d . . .
H32 H 0.5054 0.4990 0.1934 0.039 Uiso 1 1 calc R . .
C33 C -0.33068(19) 0.4352(2) 0.4404(2) 0.0375(8) Uani 1 1 d . . .
H33 H -0.3837 0.4450 0.4682 0.045 Uiso 1 1 calc R . .
C34 C -0.26005(19) 0.3911(2) 0.32044(18) 0.0338(8) Uani 1 1 d . . .
H34 H -0.2641 0.3710 0.2660 0.041 Uiso 1 1 calc R . .
C35 C -0.33628(19) 0.4056(2) 0.3616(2) 0.0368(8) Uani 1 1 d . . .
H35 H -0.3931 0.3951 0.3354 0.044 Uiso 1 1 calc R . .
C36 C -0.24874(19) 0.4507(2) 0.47910(19) 0.0375(8) Uani 1 1 d . . .
H36 H -0.2452 0.4713 0.5334 0.045 Uiso 1 1 calc R . .
C37 C -0.17082(18) 0.4359(2) 0.4381(2) 0.0359(8) Uani 1 1 d . . .
H37 H -0.1138 0.4461 0.4640 0.043 Uiso 1 1 calc R . .
C38 C 0.56774(18) 0.4447(2) 0.0975(2) 0.0393(8) Uani 1 1 d . . .
H38 H 0.6235 0.4752 0.1071 0.047 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.936(3) . ?
Fe1 N7 1.938(3) . ?
Fe1 N1 1.960(2) . ?
Fe1 N3 1.973(2) . ?
Fe1 N4 1.974(2) . ?
Fe1 N2 1.980(2) . ?
S1 C3 1.641(3) . ?
S2 C12 1.637(3) . ?
N1 C10 1.335(3) . ?
N1 C6 1.363(3) . ?
N2 C4 1.288(3) . ?
N2 C1 1.439(3) . ?
C1 C23 1.378(4) . ?
C1 C8 1.387(3) . ?
C2 C14 1.383(4) . ?
C2 C11 1.390(3) . ?
C2 N3 1.439(3) . ?
C3 N7 1.166(3) . ?
N3 C5 1.291(3) . ?
C4 C15 1.449(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.451(3) . ?
C5 H5 0.9500 . ?
N4 C26 1.335(3) . ?
N4 C15 1.352(3) . ?
N5 C12 1.164(3) . ?
C6 C18 1.382(4) . ?
C7 C8 1.376(4) . ?
C7 C9 1.388(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.377(4) . ?
C9 N10 1.459(3) . ?
C10 C20 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.382(3) . ?
C11 H11 0.9500 . ?
C13 C23 1.371(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.388(3) . ?
C14 H14 0.9500 . ?
C15 C32 1.383(4) . ?
C16 C19 1.388(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.255(3) . ?
N6 C21 1.444(3) . ?
C17 C27 1.376(4) . ?
C17 C28 1.378(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.383(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.378(4) . ?
C19 N8 1.435(3) . ?
N9 N10 1.237(3) . ?
N9 C29 1.465(4) . ?
C20 C24 1.374(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.367(4) . ?
C21 C25 1.393(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.384(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.376(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.382(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.361(4) . ?
C29 C37 1.393(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.369(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.376(4) . ?
C33 C36 1.377(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.398(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N5 Fe1 N7 90.58(9) . . ?
N5 Fe1 N1 92.49(9) . . ?
N7 Fe1 N1 93.88(9) . . ?
N5 Fe1 N3 91.08(9) . . ?
N7 Fe1 N3 174.33(8) . . ?
N1 Fe1 N3 80.63(8) . . ?
N5 Fe1 N4 92.63(9) . . ?
N7 Fe1 N4 90.63(8) . . ?
N1 Fe1 N4 173.13(9) . . ?
N3 Fe1 N4 94.71(8) . . ?
N5 Fe1 N2 172.31(9) . . ?
N7 Fe1 N2 93.10(9) . . ?
N1 Fe1 N2 93.99(8) . . ?
N3 Fe1 N2 85.91(8) . . ?
N4 Fe1 N2 80.59(9) . . ?
C10 N1 C6 117.4(2) . . ?
C10 N1 Fe1 128.32(19) . . ?
C6 N1 Fe1 114.15(15) . . ?
C4 N2 C1 117.6(2) . . ?
C4 N2 Fe1 114.66(17) . . ?
C1 N2 Fe1 126.97(17) . . ?
C23 C1 C8 120.4(2) . . ?
C23 C1 N2 120.5(2) . . ?
C8 C1 N2 119.0(2) . . ?
C14 C2 C11 120.6(2) . . ?
C14 C2 N3 121.2(2) . . ?
C11 C2 N3 118.2(2) . . ?
N7 C3 S1 178.9(3) . . ?
C5 N3 C2 119.3(2) . . ?
C5 N3 Fe1 115.03(17) . . ?
C2 N3 Fe1 125.40(16) . . ?
N2 C4 C15 116.6(2) . . ?
N2 C4 H4 121.7 . . ?
C15 C4 H4 121.7 . . ?
N3 C5 C6 115.8(2) . . ?
N3 C5 H5 122.1 . . ?
C6 C5 H5 122.1 . . ?
C26 N4 C15 117.3(2) . . ?
C26 N4 Fe1 128.3(2) . . ?
C15 N4 Fe1 114.35(16) . . ?
C12 N5 Fe1 166.4(2) . . ?
N1 C6 C18 122.4(2) . . ?
N1 C6 C5 112.8(2) . . ?
C18 C6 C5 124.7(3) . . ?
C8 C7 C9 119.8(2) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
C7 C8 C1 119.6(3) . . ?
C7 C8 H8 120.2 . . ?
C1 C8 H8 120.2 . . ?
C13 C9 C7 120.2(2) . . ?
C13 C9 N10 114.7(3) . . ?
C7 C9 N10 125.0(2) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 119.4(2) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.5(2) . . ?
C23 C13 C9 120.2(3) . . ?
C23 C13 H13 119.9 . . ?
C9 C13 H13 119.9 . . ?
C2 C14 C16 119.7(2) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 122.9(2) . . ?
N4 C15 C4 113.0(2) . . ?
C32 C15 C4 124.1(3) . . ?
C14 C16 C19 119.8(3) . . ?
C14 C16 H16 120.1 . . ?
C19 C16 H16 120.1 . . ?
N8 N6 C21 112.8(2) . . ?
C27 C17 C28 120.1(2) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 172.5(2) . . ?
C6 C18 C24 119.0(3) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.2(2) . . ?
C22 C19 N8 114.6(2) . . ?
C16 C19 N8 125.2(2) . . ?
N6 N8 C19 114.2(2) . . ?
N10 N9 C29 113.3(2) . . ?
N9 N10 C9 111.1(2) . . ?
C24 C20 C10 119.5(2) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C30 C21 C25 120.6(2) . . ?
C30 C21 N6 116.2(2) . . ?
C25 C21 N6 123.2(2) . . ?
C19 C22 C11 120.4(2) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 119.9(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C20 C24 C18 118.7(2) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C28 C25 C21 118.8(3) . . ?
C28 C25 H25 120.6 . . ?
C21 C25 H25 120.6 . . ?
N4 C26 C31 122.7(3) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 119.9(3) . . ?
C17 C27 H27 120.1 . . ?
C30 C27 H27 120.1 . . ?
C17 C28 C25 120.5(3) . . ?
C17 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
C34 C29 C37 121.6(3) . . ?
C34 C29 N9 114.7(3) . . ?
C37 C29 N9 123.6(3) . . ?
C21 C30 C27 120.1(2) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C38 C31 C26 120.0(3) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C15 C32 C38 118.6(3) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C35 C33 C36 120.4(3) . . ?
C35 C33 H33 119.8 . . ?
C36 C33 H33 119.8 . . ?
C29 C34 C35 119.4(3) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C33 C35 C34 120.4(3) . . ?
C33 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C33 C36 C37 119.7(3) . . ?
C33 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C29 C37 C36 118.4(3) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 118.4(3) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.845
_diffrn_reflns_theta_full        21.26
_diffrn_measured_fraction_theta_full 0.845
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.036
####################################################################### 
# 
# 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_feaza145kd2
_database_code_depnum_ccdc_archive 'CCDC 1492629'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
        bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0133(8)
_cell_length_b                   14.3893(11)
_cell_length_c                   16.6664(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.825(4)
_cell_angle_gamma                90.00
_cell_volume                     3596.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    145(2)
_cell_measurement_reflns_used    7237
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5434
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
              its'aim being to analyse the evolution of partial collection of data, 
              always carried out over the same part of reciprocal space, 
              and over a large scale of temperature.
              This  explain the poor completness of data as well as the low theta(max) value, 
              the low number of unique reflexions collected.
              In ordre to obtain significant intensities with an exposure time relatively short, 
              a crystal of neutron size was used. As the aim is to compare the diffraction data 
              always obtained from the same part of the crystal at different temperature, 
              problems of intensity scale are not considered to be of prior importance.
              The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
              over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
              these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
              or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
              but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      145(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5636
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         22.97
_reflns_number_total             4035
_reflns_number_gt                3489
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0180P)²+2.3508P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4035
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0678
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29150(2) 0.28434(2) 0.06805(2) 0.02440(13) Uani 1 1 d . . .
S1 S 0.19529(4) 0.48716(5) -0.14266(4) 0.03172(19) Uani 1 1 d . . .
S2 S 0.42172(5) 0.07450(5) -0.10812(4) 0.0363(2) Uani 1 1 d . . .
N1 N 0.17761(14) 0.21951(13) 0.08034(13) 0.0239(5) Uani 1 1 d . . .
N2 N 0.27160(13) 0.37439(13) 0.15614(12) 0.0219(5) Uani 1 1 d . . .
C1 C 0.19396(16) 0.38076(16) 0.20303(16) 0.0228(6) Uani 1 1 d . . .
C2 C 0.41725(16) 0.18535(16) 0.18885(16) 0.0234(6) Uani 1 1 d . . .
C3 C 0.22329(16) 0.41681(18) -0.06816(17) 0.0259(6) Uani 1 1 d . . .
N3 N 0.32831(13) 0.19593(13) 0.15480(12) 0.0232(5) Uani 1 1 d . . .
C4 C 0.34061(17) 0.42190(17) 0.17923(16) 0.0267(6) Uani 1 1 d . . .
H4 H 0.3403 0.4619 0.2246 0.032 Uiso 1 1 calc R . .
C5 C 0.26357(17) 0.15203(16) 0.18547(16) 0.0247(6) Uani 1 1 d . . .
H5 H 0.2726 0.1138 0.2316 0.030 Uiso 1 1 calc R . .
N4 N 0.40710(13) 0.35077(14) 0.07107(13) 0.0271(5) Uani 1 1 d . . .
N5 N 0.32859(14) 0.19792(15) -0.01346(14) 0.0325(6) Uani 1 1 d . . .
C6 C 0.17590(16) 0.16388(16) 0.14585(15) 0.0241(6) Uani 1 1 d . . .
C7 C 0.03619(17) 0.40199(17) 0.20919(17) 0.0313(7) Uani 1 1 d . . .
H7 H -0.0206 0.4133 0.1833 0.038 Uiso 1 1 calc R . .
C8 C 0.11147(17) 0.39690(16) 0.16425(16) 0.0273(7) Uani 1 1 d . . .
H8 H 0.1066 0.4044 0.1076 0.033 Uiso 1 1 calc R . .
C9 C 0.04378(18) 0.39059(17) 0.29171(17) 0.0304(7) Uani 1 1 d . . .
C10 C 0.10198(18) 0.22815(17) 0.03519(17) 0.0301(7) Uani 1 1 d . . .
H10 H 0.1027 0.2647 -0.0122 0.036 Uiso 1 1 calc R . .
C11 C 0.48354(17) 0.15758(17) 0.13913(17) 0.0309(7) Uani 1 1 d . . .
H11 H 0.4692 0.1424 0.0845 0.037 Uiso 1 1 calc R . .
C12 C 0.36624(17) 0.14630(18) -0.05334(16) 0.0270(6) Uani 1 1 d . . .
C13 C 0.12577(18) 0.37539(19) 0.32950(17) 0.0371(7) Uani 1 1 d . . .
H13 H 0.1309 0.3691 0.3863 0.045 Uiso 1 1 calc R . .
C14 C 0.43798(17) 0.20745(17) 0.26865(17) 0.0292(7) Uani 1 1 d . . .
H14 H 0.3924 0.2269 0.3025 0.035 Uiso 1 1 calc R . .
C15 C 0.41898(16) 0.41147(17) 0.13266(17) 0.0272(6) Uani 1 1 d . . .
C16 C 0.52546(17) 0.20093(17) 0.29875(17) 0.0311(7) Uani 1 1 d . . .
H16 H 0.5401 0.2158 0.3534 0.037 Uiso 1 1 calc R . .
N6 N 0.69958(14) 0.15424(14) 0.34655(15) 0.0321(6) Uani 1 1 d . . .
C17 C 0.96907(18) 0.11456(18) 0.41880(18) 0.0340(7) Uani 1 1 d . . .
H17 H 1.0294 0.1026 0.4355 0.041 Uiso 1 1 calc R . .
N7 N 0.24285(13) 0.36794(15) -0.01445(14) 0.0297(5) Uani 1 1 d . . .
C18 C 0.09885(17) 0.12159(17) 0.16936(17) 0.0311(7) Uani 1 1 d . . .
H18 H 0.0995 0.0846 0.2166 0.037 Uiso 1 1 calc R . .
C19 C 0.59170(17) 0.17257(17) 0.24886(17) 0.0271(6) Uani 1 1 d . . .
N8 N 0.68446(14) 0.16277(14) 0.27261(15) 0.0312(6) Uani 1 1 d . . .
N9 N -0.10225(18) 0.39275(15) 0.30793(15) 0.0394(6) Uani 1 1 d . . .
N10 N -0.02980(17) 0.39784(15) 0.34541(16) 0.0408(6) Uani 1 1 d . . .
C20 C 0.02292(18) 0.18646(18) 0.05419(18) 0.0362(7) Uani 1 1 d . . .
H20 H -0.0293 0.1939 0.0202 0.043 Uiso 1 1 calc R . .
C21 C 0.79343(16) 0.14387(17) 0.36872(17) 0.0289(7) Uani 1 1 d . . .
C22 C 0.57053(17) 0.15204(17) 0.16939(17) 0.0319(7) Uani 1 1 d . . .
H22 H 0.6162 0.1339 0.1352 0.038 Uiso 1 1 calc R . .
C23 C 0.20080(18) 0.36920(18) 0.28520(17) 0.0333(7) Uani 1 1 d . . .
H23 H 0.2572 0.3570 0.3114 0.040 Uiso 1 1 calc R . .
C24 C 0.02085(18) 0.13389(18) 0.12307(18) 0.0361(7) Uani 1 1 d . . .
H24 H -0.0333 0.1065 0.1385 0.043 Uiso 1 1 calc R . .
C25 C 0.86090(18) 0.16274(18) 0.31651(18) 0.0355(7) Uani 1 1 d . . .
H25 H 0.8468 0.1851 0.2638 0.043 Uiso 1 1 calc R . .
C26 C 0.47450(18) 0.34052(19) 0.02216(18) 0.0373(7) Uani 1 1 d . . .
H26 H 0.4668 0.2996 -0.0223 0.045 Uiso 1 1 calc R . .
C27 C 0.90238(18) 0.09823(19) 0.47024(19) 0.0393(7) Uani 1 1 d . . .
H27 H 0.9166 0.0763 0.5231 0.047 Uiso 1 1 calc R . .
C28 C 0.94854(18) 0.14838(18) 0.34266(19) 0.0372(7) Uani 1 1 d . . .
H28 H 0.9951 0.1619 0.3079 0.045 Uiso 1 1 calc R . .
C29 C -0.1781(2) 0.40574(18) 0.3587(2) 0.0370(8) Uani 1 1 d . . .
C30 C 0.81419(18) 0.11362(18) 0.44535(18) 0.0364(7) Uani 1 1 d . . .
H30 H 0.7681 0.1032 0.4814 0.044 Uiso 1 1 calc R . .
C31 C 0.55436(19) 0.3866(2) 0.0335(2) 0.0474(8) Uani 1 1 d . . .
H31 H 0.6001 0.3782 -0.0033 0.057 Uiso 1 1 calc R . .
C32 C 0.49814(18) 0.45845(19) 0.14883(19) 0.0408(8) Uani 1 1 d . . .
H32 H 0.5048 0.4992 0.1936 0.049 Uiso 1 1 calc R . .
C33 C -0.3304(2) 0.4349(2) 0.4410(2) 0.0464(8) Uani 1 1 d . . .
H33 H -0.3834 0.4444 0.4687 0.056 Uiso 1 1 calc R . .
C34 C -0.2594(2) 0.39101(18) 0.3210(2) 0.0412(8) Uani 1 1 d . . .
H34 H -0.2638 0.3711 0.2665 0.049 Uiso 1 1 calc R . .
C35 C -0.3354(2) 0.40522(19) 0.3624(2) 0.0453(8) Uani 1 1 d . . .
H35 H -0.3921 0.3944 0.3364 0.054 Uiso 1 1 calc R . .
C36 C -0.2481(2) 0.4508(2) 0.4797(2) 0.0474(8) Uani 1 1 d . . .
H36 H -0.2444 0.4716 0.5339 0.057 Uiso 1 1 calc R . .
C37 C -0.17017(19) 0.43587(19) 0.4383(2) 0.0450(8) Uani 1 1 d . . .
H37 H -0.1131 0.4461 0.4640 0.054 Uiso 1 1 calc R . .
C38 C 0.56761(19) 0.4448(2) 0.0982(2) 0.0483(9) Uani 1 1 d . . .
H38 H 0.6233 0.4752 0.1082 0.058 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.942(2) . ?
Fe1 N5 1.943(3) . ?
Fe1 N1 1.967(2) . ?
Fe1 N4 1.980(2) . ?
Fe1 N3 1.984(2) . ?
Fe1 N2 1.992(2) . ?
S1 C3 1.641(3) . ?
S2 C12 1.634(3) . ?
N1 C10 1.337(3) . ?
N1 C6 1.355(3) . ?
N2 C4 1.284(3) . ?
N2 C1 1.438(3) . ?
C1 C23 1.378(4) . ?
C1 C8 1.388(3) . ?
C2 C11 1.385(3) . ?
C2 C14 1.388(4) . ?
C2 N3 1.433(3) . ?
C3 N7 1.164(3) . ?
N3 C5 1.286(3) . ?
C4 C15 1.449(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.453(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.338(3) . ?
N4 C15 1.353(3) . ?
N5 C12 1.162(3) . ?
C6 C18 1.381(3) . ?
C7 C9 1.384(4) . ?
C7 C8 1.388(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.372(4) . ?
C9 N10 1.459(3) . ?
C10 C20 1.381(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.379(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.380(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.382(3) . ?
C16 C19 1.389(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.248(3) . ?
N6 C21 1.447(3) . ?
C17 C27 1.370(4) . ?
C17 C28 1.380(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.382(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.379(4) . ?
C19 N8 1.436(3) . ?
N9 N10 1.230(3) . ?
N9 C29 1.463(4) . ?
C20 C24 1.376(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.370(4) . ?
C21 C25 1.394(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.381(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.375(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.386(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.363(4) . ?
C29 C37 1.395(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.373(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.376(4) . ?
C33 C36 1.383(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.405(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.69(9) . . ?
N7 Fe1 N1 93.96(9) . . ?
N5 Fe1 N1 92.86(8) . . ?
N7 Fe1 N4 91.01(8) . . ?
N5 Fe1 N4 92.61(9) . . ?
N1 Fe1 N4 172.57(9) . . ?
N7 Fe1 N3 174.10(9) . . ?
N5 Fe1 N3 91.14(8) . . ?
N1 Fe1 N3 80.35(9) . . ?
N4 Fe1 N3 94.51(8) . . ?
N7 Fe1 N2 93.10(8) . . ?
N5 Fe1 N2 171.95(9) . . ?
N1 Fe1 N2 93.96(8) . . ?
N4 Fe1 N2 80.23(8) . . ?
N3 Fe1 N2 85.79(8) . . ?
C10 N1 C6 117.3(2) . . ?
C10 N1 Fe1 128.01(18) . . ?
C6 N1 Fe1 114.52(17) . . ?
C4 N2 C1 117.8(2) . . ?
C4 N2 Fe1 114.77(16) . . ?
C1 N2 Fe1 126.67(16) . . ?
C23 C1 C8 120.3(2) . . ?
C23 C1 N2 120.6(2) . . ?
C8 C1 N2 119.1(2) . . ?
C11 C2 C14 120.4(2) . . ?
C11 C2 N3 118.5(2) . . ?
C14 C2 N3 121.1(2) . . ?
N7 C3 S1 179.0(2) . . ?
C5 N3 C2 119.9(2) . . ?
C5 N3 Fe1 114.56(16) . . ?
C2 N3 Fe1 125.27(16) . . ?
N2 C4 C15 116.7(2) . . ?
N2 C4 H4 121.7 . . ?
C15 C4 H4 121.7 . . ?
N3 C5 C6 116.6(2) . . ?
N3 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C26 N4 C15 117.2(2) . . ?
C26 N4 Fe1 128.28(19) . . ?
C15 N4 Fe1 114.43(16) . . ?
C12 N5 Fe1 166.7(2) . . ?
N1 C6 C18 122.6(2) . . ?
N1 C6 C5 112.5(2) . . ?
C18 C6 C5 124.9(2) . . ?
C9 C7 C8 120.0(2) . . ?
C9 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C1 C8 C7 119.3(3) . . ?
C1 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C13 C9 C7 120.2(2) . . ?
C13 C9 N10 114.8(3) . . ?
C7 C9 N10 125.0(2) . . ?
N1 C10 C20 123.1(3) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
N5 C12 S2 178.4(2) . . ?
C9 C13 C23 120.1(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C16 C14 C2 119.7(2) . . ?
C16 C14 H14 120.2 . . ?
C2 C14 H14 120.2 . . ?
N4 C15 C32 122.9(2) . . ?
N4 C15 C4 113.2(2) . . ?
C32 C15 C4 123.9(3) . . ?
C14 C16 C19 119.8(3) . . ?
C14 C16 H16 120.1 . . ?
C19 C16 H16 120.1 . . ?
N8 N6 C21 112.9(2) . . ?
C27 C17 C28 119.9(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 171.9(2) . . ?
C6 C18 C24 118.9(3) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.0(2) . . ?
C22 C19 N8 114.7(2) . . ?
C16 C19 N8 125.3(2) . . ?
N6 N8 C19 114.1(2) . . ?
N10 N9 C29 113.1(3) . . ?
N9 N10 C9 111.2(3) . . ?
C24 C20 C10 119.0(3) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.3(2) . . ?
C30 C21 N6 116.4(2) . . ?
C25 C21 N6 123.3(3) . . ?
C19 C22 C11 120.5(3) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C1 C23 C13 120.1(2) . . ?
C1 C23 H23 120.0 . . ?
C13 C23 H23 120.0 . . ?
C20 C24 C18 118.9(3) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C28 C25 C21 118.9(3) . . ?
C28 C25 H25 120.5 . . ?
C21 C25 H25 120.5 . . ?
N4 C26 C31 122.9(3) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 120.1(3) . . ?
C17 C27 H27 119.9 . . ?
C30 C27 H27 119.9 . . ?
C17 C28 C25 120.6(3) . . ?
C17 C28 H28 119.7 . . ?
C25 C28 H28 119.7 . . ?
C34 C29 C37 121.3(3) . . ?
C34 C29 N9 114.7(3) . . ?
C37 C29 N9 123.9(3) . . ?
C21 C30 C27 120.0(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 119.6(3) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C15 C32 C38 118.5(3) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C35 C33 C36 120.1(3) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.4(3) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C33 C35 C34 121.1(3) . . ?
C33 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C33 C36 C37 119.4(3) . . ?
C33 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C29 C37 C36 118.8(3) . . ?
C29 C37 H37 120.6 . . ?
C36 C37 H37 120.6 . . ?
C31 C38 C32 118.7(3) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.809
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.809
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_feaza115km2
_database_code_depnum_ccdc_archive 'CCDC 1492630'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0068(9)
_cell_length_b                   14.3500(12)
_cell_length_c                   16.6364(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.859(5)
_cell_angle_gamma                90.00
_cell_volume                     3578.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    8865
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5419
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                its'aim being to analyse the evolution of partial collection of data, 
                always carried out over the same part of reciprocal space, 
                and over a large scale of temperature.
                This  explain the poor completness of data as well as the low theta(max) value, 
                the low number of unique reflexions collected.
                In ordre to obtain significant intensities with an exposure time relatively short, 
                a crystal of neutron size was used. As the aim is to compare the diffraction data 
                always obtained from the same part of the crystal at different temperature, 
                problems of intensity scale are not considered to be of prior importance.
                The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      115(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5529
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         23.00
_reflns_number_total             3980
_reflns_number_gt                3441
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0244P)²+2.1464P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3980
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0702
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29120(2) 0.28438(2) 0.06842(2) 0.02043(14) Uani 1 1 d . . .
S1 S 0.19523(4) 0.48753(5) -0.14291(4) 0.02628(19) Uani 1 1 d . . .
S2 S 0.42148(5) 0.07423(5) -0.10799(4) 0.0301(2) Uani 1 1 d . . .
N1 N 0.17755(14) 0.21978(13) 0.08039(13) 0.0206(5) Uani 1 1 d . . .
N2 N 0.27119(13) 0.37441(13) 0.15593(12) 0.0188(5) Uani 1 1 d . . .
C1 C 0.19380(16) 0.38077(16) 0.20316(16) 0.0201(6) Uani 1 1 d . . .
C2 C 0.41704(16) 0.18553(16) 0.18917(16) 0.0192(6) Uani 1 1 d . . .
C3 C 0.22336(16) 0.41670(18) -0.06793(17) 0.0218(6) Uani 1 1 d . . .
N3 N 0.32803(14) 0.19620(13) 0.15490(13) 0.0208(5) Uani 1 1 d . . .
C4 C 0.34064(17) 0.42211(16) 0.17916(16) 0.0228(6) Uani 1 1 d . . .
H4 H 0.3404 0.4623 0.2245 0.027 Uiso 1 1 calc R . .
C5 C 0.26355(17) 0.15195(16) 0.18603(16) 0.0215(6) Uani 1 1 d . . .
H5 H 0.2727 0.1137 0.2323 0.026 Uiso 1 1 calc R . .
N4 N 0.40659(13) 0.35055(13) 0.07058(13) 0.0223(5) Uani 1 1 d . . .
N5 N 0.32783(14) 0.19773(15) -0.01302(14) 0.0264(5) Uani 1 1 d . . .
C6 C 0.17575(16) 0.16404(16) 0.14611(16) 0.0217(6) Uani 1 1 d . . .
C7 C 0.03597(17) 0.40228(16) 0.20938(17) 0.0265(7) Uani 1 1 d . . .
H7 H -0.0207 0.4139 0.1834 0.032 Uiso 1 1 calc R . .
C8 C 0.11111(17) 0.39683(16) 0.16448(17) 0.0234(6) Uani 1 1 d . . .
H8 H 0.1061 0.4040 0.1077 0.028 Uiso 1 1 calc R . .
C9 C 0.04348(18) 0.39074(17) 0.29211(17) 0.0252(7) Uani 1 1 d . . .
C10 C 0.10178(18) 0.22840(17) 0.03495(17) 0.0258(7) Uani 1 1 d . . .
H10 H 0.1024 0.2650 -0.0126 0.031 Uiso 1 1 calc R . .
C11 C 0.48359(17) 0.15756(17) 0.13873(17) 0.0267(7) Uani 1 1 d . . .
H11 H 0.4691 0.1423 0.0841 0.032 Uiso 1 1 calc R . .
C12 C 0.36565(17) 0.14587(18) -0.05308(16) 0.0230(6) Uani 1 1 d . . .
C13 C 0.12593(18) 0.37569(18) 0.32996(17) 0.0312(7) Uani 1 1 d . . .
H13 H 0.1311 0.3697 0.3869 0.037 Uiso 1 1 calc R . .
C14 C 0.43817(17) 0.20780(17) 0.26882(17) 0.0243(7) Uani 1 1 d . . .
H14 H 0.3928 0.2275 0.3028 0.029 Uiso 1 1 calc R . .
C15 C 0.41879(16) 0.41129(17) 0.13272(17) 0.0233(6) Uani 1 1 d . . .
C16 C 0.52568(17) 0.20123(17) 0.29884(17) 0.0262(7) Uani 1 1 d . . .
H16 H 0.5403 0.2162 0.3535 0.031 Uiso 1 1 calc R . .
N6 N 0.70007(14) 0.15429(14) 0.34700(15) 0.0268(6) Uani 1 1 d . . .
C17 C 0.96965(17) 0.11443(17) 0.41874(18) 0.0289(7) Uani 1 1 d . . .
H17 H 1.0301 0.1027 0.4354 0.035 Uiso 1 1 calc R . .
N7 N 0.24300(13) 0.36765(15) -0.01427(14) 0.0246(5) Uani 1 1 d . . .
C18 C 0.09856(17) 0.12168(17) 0.16977(17) 0.0254(7) Uani 1 1 d . . .
H18 H 0.0991 0.0851 0.2174 0.031 Uiso 1 1 calc R . .
C19 C 0.59207(17) 0.17280(17) 0.24904(17) 0.0228(6) Uani 1 1 d . . .
N8 N 0.68443(14) 0.16280(14) 0.27269(15) 0.0264(5) Uani 1 1 d . . .
N9 N -0.10308(17) 0.39265(14) 0.30782(15) 0.0320(6) Uani 1 1 d . . .
N10 N -0.02974(17) 0.39794(15) 0.34539(15) 0.0334(6) Uani 1 1 d . . .
C20 C 0.02265(18) 0.18643(18) 0.05408(18) 0.0302(7) Uani 1 1 d . . .
H20 H -0.0296 0.1940 0.0201 0.036 Uiso 1 1 calc R . .
C21 C 0.79332(16) 0.14404(17) 0.36872(17) 0.0237(6) Uani 1 1 d . . .
C22 C 0.57047(17) 0.15233(17) 0.16916(17) 0.0260(7) Uani 1 1 d . . .
H22 H 0.6162 0.1344 0.1348 0.031 Uiso 1 1 calc R . .
C23 C 0.20115(17) 0.36924(18) 0.28570(17) 0.0273(7) Uani 1 1 d . . .
H23 H 0.2576 0.3570 0.3119 0.033 Uiso 1 1 calc R . .
C24 C 0.02056(18) 0.13348(18) 0.12299(18) 0.0302(7) Uani 1 1 d . . .
H24 H -0.0335 0.1056 0.1381 0.036 Uiso 1 1 calc R . .
C25 C 0.86100(17) 0.16288(17) 0.31678(17) 0.0292(7) Uani 1 1 d . . .
H25 H 0.8468 0.1856 0.2640 0.035 Uiso 1 1 calc R . .
C26 C 0.47373(17) 0.34018(19) 0.02141(17) 0.0314(7) Uani 1 1 d . . .
H26 H 0.4657 0.2992 -0.0232 0.038 Uiso 1 1 calc R . .
C27 C 0.90285(18) 0.09752(18) 0.47059(18) 0.0318(7) Uani 1 1 d . . .
H27 H 0.9172 0.0749 0.5233 0.038 Uiso 1 1 calc R . .
C28 C 0.94884(18) 0.14840(18) 0.34242(18) 0.0309(7) Uani 1 1 d . . .
H28 H 0.9952 0.1619 0.3074 0.037 Uiso 1 1 calc R . .
C29 C -0.17837(19) 0.40604(17) 0.35828(19) 0.0305(7) Uani 1 1 d . . .
C30 C 0.81440(18) 0.11346(17) 0.44575(18) 0.0300(7) Uani 1 1 d . . .
H30 H 0.7684 0.1032 0.4820 0.036 Uiso 1 1 calc R . .
C31 C 0.55397(18) 0.3862(2) 0.0324(2) 0.0384(8) Uani 1 1 d . . .
H31 H 0.5995 0.3776 -0.0046 0.046 Uiso 1 1 calc R . .
C32 C 0.49824(17) 0.45859(18) 0.14837(18) 0.0326(7) Uani 1 1 d . . .
H32 H 0.5051 0.4997 0.1930 0.039 Uiso 1 1 calc R . .
C33 C -0.3309(2) 0.43518(19) 0.4408(2) 0.0389(8) Uani 1 1 d . . .
H33 H -0.3837 0.4449 0.4688 0.047 Uiso 1 1 calc R . .
C34 C -0.26025(19) 0.39106(18) 0.32025(19) 0.0335(7) Uani 1 1 d . . .
H34 H -0.2644 0.3709 0.2658 0.040 Uiso 1 1 calc R . .
C35 C -0.33652(19) 0.40548(18) 0.3615(2) 0.0371(8) Uani 1 1 d . . .
H35 H -0.3933 0.3950 0.3353 0.045 Uiso 1 1 calc R . .
C36 C -0.24840(19) 0.45067(19) 0.4792(2) 0.0387(8) Uani 1 1 d . . .
H36 H -0.2445 0.4713 0.5336 0.046 Uiso 1 1 calc R . .
C37 C -0.17084(19) 0.43594(18) 0.43795(19) 0.0363(8) Uani 1 1 d . . .
H37 H -0.1138 0.4462 0.4638 0.044 Uiso 1 1 calc R . .
C38 C 0.56770(18) 0.4447(2) 0.0975(2) 0.0407(8) Uani 1 1 d . . .
H38 H 0.6235 0.4750 0.1074 0.049 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.935(2) . ?
Fe1 N5 1.939(2) . ?
Fe1 N1 1.960(2) . ?
Fe1 N4 1.974(2) . ?
Fe1 N3 1.974(2) . ?
Fe1 N2 1.980(2) . ?
S1 C3 1.648(3) . ?
S2 C12 1.634(3) . ?
N1 C10 1.339(3) . ?
N1 C6 1.356(3) . ?
N2 C4 1.290(3) . ?
N2 C1 1.437(3) . ?
C1 C23 1.382(4) . ?
C1 C8 1.388(3) . ?
C2 C14 1.384(4) . ?
C2 C11 1.395(3) . ?
C2 N3 1.434(3) . ?
C3 N7 1.163(3) . ?
N3 C5 1.288(3) . ?
C4 C15 1.445(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.456(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.337(3) . ?
N4 C15 1.358(3) . ?
N5 C12 1.165(3) . ?
C6 C18 1.383(3) . ?
C7 C9 1.385(4) . ?
C7 C8 1.386(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.377(4) . ?
C9 N10 1.449(3) . ?
C10 C20 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.377(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.385(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.385(3) . ?
C16 C19 1.388(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.253(3) . ?
N6 C21 1.435(3) . ?
C17 C27 1.376(4) . ?
C17 C28 1.381(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.383(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.384(4) . ?
C19 N8 1.429(3) . ?
N9 N10 1.241(3) . ?
N9 C29 1.454(3) . ?
C20 C24 1.377(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.376(4) . ?
C21 C25 1.392(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.381(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.378(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.389(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.371(4) . ?
C29 C37 1.392(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.377(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.389(4) . ?
C32 H32 0.9500 . ?
C33 C36 1.382(4) . ?
C33 C35 1.386(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.397(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.47(9) . . ?
N7 Fe1 N1 93.90(9) . . ?
N5 Fe1 N1 92.65(8) . . ?
N7 Fe1 N4 90.71(8) . . ?
N5 Fe1 N4 92.42(9) . . ?
N1 Fe1 N4 173.12(9) . . ?
N7 Fe1 N3 174.32(9) . . ?
N5 Fe1 N3 91.11(8) . . ?
N1 Fe1 N3 80.57(9) . . ?
N4 Fe1 N3 94.68(8) . . ?
N7 Fe1 N2 93.14(8) . . ?
N5 Fe1 N2 172.23(9) . . ?
N1 Fe1 N2 93.97(8) . . ?
N4 Fe1 N2 80.67(8) . . ?
N3 Fe1 N2 85.96(8) . . ?
C10 N1 C6 117.3(2) . . ?
C10 N1 Fe1 128.13(18) . . ?
C6 N1 Fe1 114.41(17) . . ?
C4 N2 C1 117.7(2) . . ?
C4 N2 Fe1 114.62(16) . . ?
C1 N2 Fe1 126.84(16) . . ?
C23 C1 C8 120.4(2) . . ?
C23 C1 N2 120.6(2) . . ?
C8 C1 N2 119.0(2) . . ?
C14 C2 C11 120.4(2) . . ?
C14 C2 N3 121.3(2) . . ?
C11 C2 N3 118.2(2) . . ?
N7 C3 S1 179.1(2) . . ?
C5 N3 C2 119.4(2) . . ?
C5 N3 Fe1 114.87(17) . . ?
C2 N3 Fe1 125.41(16) . . ?
N2 C4 C15 116.6(2) . . ?
N2 C4 H4 121.7 . . ?
C15 C4 H4 121.7 . . ?
N3 C5 C6 116.0(2) . . ?
N3 C5 H5 122.0 . . ?
C6 C5 H5 122.0 . . ?
C26 N4 C15 117.4(2) . . ?
C26 N4 Fe1 128.49(19) . . ?
C15 N4 Fe1 114.06(16) . . ?
C12 N5 Fe1 166.5(2) . . ?
N1 C6 C18 122.6(2) . . ?
N1 C6 C5 112.6(2) . . ?
C18 C6 C5 124.7(2) . . ?
C9 C7 C8 120.1(2) . . ?
C9 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C1 119.5(3) . . ?
C7 C8 H8 120.3 . . ?
C1 C8 H8 120.3 . . ?
C13 C9 C7 120.0(2) . . ?
C13 C9 N10 115.0(3) . . ?
C7 C9 N10 124.9(2) . . ?
N1 C10 C20 123.0(3) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.2(3) . . ?
C22 C11 H11 120.4 . . ?
C2 C11 H11 120.4 . . ?
N5 C12 S2 178.3(2) . . ?
C9 C13 C23 120.4(3) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C2 C14 C16 119.8(2) . . ?
C2 C14 H14 120.1 . . ?
C16 C14 H14 120.1 . . ?
N4 C15 C32 122.7(2) . . ?
N4 C15 C4 113.2(2) . . ?
C32 C15 C4 124.1(3) . . ?
C14 C16 C19 120.0(3) . . ?
C14 C16 H16 120.0 . . ?
C19 C16 H16 120.0 . . ?
N8 N6 C21 113.0(2) . . ?
C27 C17 C28 120.0(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 172.2(2) . . ?
C6 C18 C24 118.9(2) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 119.7(2) . . ?
C22 C19 N8 114.9(2) . . ?
C16 C19 N8 125.5(2) . . ?
N6 N8 C19 114.4(2) . . ?
N10 N9 C29 113.4(3) . . ?
N9 N10 C9 111.6(2) . . ?
C24 C20 C10 119.2(3) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C30 C21 C25 119.9(2) . . ?
C30 C21 N6 116.3(2) . . ?
C25 C21 N6 123.8(2) . . ?
C11 C22 C19 120.9(2) . . ?
C11 C22 H22 119.5 . . ?
C19 C22 H22 119.5 . . ?
C13 C23 C1 119.7(2) . . ?
C13 C23 H23 120.2 . . ?
C1 C23 H23 120.2 . . ?
C20 C24 C18 118.8(2) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C28 C25 C21 119.6(3) . . ?
C28 C25 H25 120.2 . . ?
C21 C25 H25 120.2 . . ?
N4 C26 C31 123.1(3) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 120.0(3) . . ?
C17 C27 H27 120.0 . . ?
C30 C27 H27 120.0 . . ?
C25 C28 C17 120.4(3) . . ?
C25 C28 H28 119.8 . . ?
C17 C28 H28 119.8 . . ?
C34 C29 C37 121.1(3) . . ?
C34 C29 N9 114.7(3) . . ?
C37 C29 N9 124.2(3) . . ?
C21 C30 C27 120.1(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 119.5(3) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.2 . . ?
C15 C32 C38 118.7(3) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C36 C33 C35 120.1(3) . . ?
C36 C33 H33 120.0 . . ?
C35 C33 H33 120.0 . . ?
C29 C34 C35 119.6(3) . . ?
C29 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C33 120.4(3) . . ?
C34 C35 H35 119.8 . . ?
C33 C35 H35 119.8 . . ?
C33 C36 C37 119.8(3) . . ?
C33 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C29 C37 C36 119.0(3) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C31 C38 C32 118.6(3) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.799
_diffrn_reflns_theta_full        23.00
_diffrn_measured_fraction_theta_full 0.799
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_feaza125kd2
_database_code_depnum_ccdc_archive 'CCDC 1492631'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
         bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0070(8)
_cell_length_b                   14.3657(10)
_cell_length_c                   16.6511(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.856(4)
_cell_angle_gamma                90.00
_cell_volume                     3585.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    125(2)
_cell_measurement_reflns_used    7184
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
               its'aim being to analyse the evolution of partial collection of data, 
               always carried out over the same part of reciprocal space, 
               and over a large scale of temperature.
               This  explain the poor completness of data as well as the low theta(max) value, 
               the low number of unique reflexions collected.
               In ordre to obtain significant intensities with an exposure time relatively short, 
               a crystal of neutron size was used. As the aim is to compare the diffraction data 
               always obtained from the same part of the crystal at different temperature, 
               problems of intensity scale are not considered to be of prior importance.
               The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
               over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
               these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
               or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
               but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      125(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5597
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         22.96
_reflns_number_total             4010
_reflns_number_gt                3482
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0185P)²+2.2854P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4010
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0699
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29119(2) 0.28431(2) 0.06839(2) 0.02110(13) Uani 1 1 d . . .
S1 S 0.19525(4) 0.48735(4) -0.14277(4) 0.02755(18) Uani 1 1 d . . .
S2 S 0.42129(4) 0.07424(5) -0.10801(4) 0.03138(19) Uani 1 1 d . . .
N1 N 0.17751(13) 0.21968(12) 0.08022(12) 0.0213(5) Uani 1 1 d . . .
N2 N 0.27122(12) 0.37420(13) 0.15589(12) 0.0195(5) Uani 1 1 d . . .
C1 C 0.19370(16) 0.38062(15) 0.20315(15) 0.0211(6) Uani 1 1 d . . .
C2 C 0.41719(16) 0.18555(15) 0.18902(16) 0.0210(6) Uani 1 1 d . . .
C3 C 0.22338(15) 0.41665(17) -0.06796(17) 0.0223(6) Uani 1 1 d . . .
N3 N 0.32792(13) 0.19617(13) 0.15496(12) 0.0209(5) Uani 1 1 d . . .
C4 C 0.34036(16) 0.42207(16) 0.17921(16) 0.0236(6) Uani 1 1 d . . .
H4 H 0.3399 0.4622 0.2245 0.028 Uiso 1 1 calc R . .
C5 C 0.26325(16) 0.15204(16) 0.18577(15) 0.0224(6) Uani 1 1 d . . .
H5 H 0.2723 0.1138 0.2320 0.027 Uiso 1 1 calc R . .
N4 N 0.40658(13) 0.35065(13) 0.07077(12) 0.0239(5) Uani 1 1 d . . .
N5 N 0.32785(14) 0.19772(14) -0.01302(13) 0.0275(5) Uani 1 1 d . . .
C6 C 0.17561(16) 0.16398(16) 0.14599(15) 0.0218(6) Uani 1 1 d . . .
C7 C 0.03596(17) 0.40186(16) 0.20933(17) 0.0276(6) Uani 1 1 d . . .
H7 H -0.0208 0.4132 0.1834 0.033 Uiso 1 1 calc R . .
C8 C 0.11115(16) 0.39667(15) 0.16441(16) 0.0237(6) Uani 1 1 d . . .
H8 H 0.1062 0.4040 0.1077 0.028 Uiso 1 1 calc R . .
C9 C 0.04365(17) 0.39053(16) 0.29203(16) 0.0255(6) Uani 1 1 d . . .
C10 C 0.10159(17) 0.22833(17) 0.03499(16) 0.0262(6) Uani 1 1 d . . .
H10 H 0.1022 0.2650 -0.0125 0.031 Uiso 1 1 calc R . .
C11 C 0.48353(17) 0.15744(17) 0.13897(17) 0.0286(7) Uani 1 1 d . . .
H11 H 0.4691 0.1420 0.0844 0.034 Uiso 1 1 calc R . .
C12 C 0.36540(16) 0.14584(18) -0.05314(16) 0.0233(6) Uani 1 1 d . . .
C13 C 0.12592(18) 0.37520(18) 0.32996(17) 0.0322(7) Uani 1 1 d . . .
H13 H 0.1310 0.3687 0.3868 0.039 Uiso 1 1 calc R . .
C14 C 0.43795(17) 0.20773(16) 0.26884(16) 0.0255(6) Uani 1 1 d . . .
H14 H 0.3924 0.2273 0.3027 0.031 Uiso 1 1 calc R . .
C15 C 0.41867(16) 0.41152(16) 0.13286(16) 0.0239(6) Uani 1 1 d . . .
C16 C 0.52565(17) 0.20119(16) 0.29895(16) 0.0264(6) Uani 1 1 d . . .
H16 H 0.5404 0.2162 0.3536 0.032 Uiso 1 1 calc R . .
N6 N 0.69984(13) 0.15424(14) 0.34689(14) 0.0280(5) Uani 1 1 d . . .
C17 C 0.96921(17) 0.11426(17) 0.41880(17) 0.0297(7) Uani 1 1 d . . .
H17 H 1.0296 0.1023 0.4354 0.036 Uiso 1 1 calc R . .
N7 N 0.24277(13) 0.36771(14) -0.01429(13) 0.0247(5) Uani 1 1 d . . .
C18 C 0.09863(16) 0.12154(17) 0.16977(16) 0.0266(6) Uani 1 1 d . . .
H18 H 0.0992 0.0849 0.2173 0.032 Uiso 1 1 calc R . .
C19 C 0.59182(16) 0.17261(16) 0.24895(16) 0.0239(6) Uani 1 1 d . . .
N8 N 0.68439(13) 0.16264(13) 0.27276(14) 0.0267(5) Uani 1 1 d . . .
N9 N -0.10311(16) 0.39267(14) 0.30776(15) 0.0337(6) Uani 1 1 d . . .
N10 N -0.02974(16) 0.39783(14) 0.34518(15) 0.0341(6) Uani 1 1 d . . .
C20 C 0.02257(17) 0.18658(17) 0.05399(17) 0.0310(7) Uani 1 1 d . . .
H20 H -0.0297 0.1943 0.0201 0.037 Uiso 1 1 calc R . .
C21 C 0.79340(16) 0.14381(16) 0.36862(16) 0.0250(6) Uani 1 1 d . . .
C22 C 0.57051(17) 0.15219(17) 0.16931(17) 0.0279(7) Uani 1 1 d . . .
H22 H 0.6163 0.1343 0.1350 0.033 Uiso 1 1 calc R . .
C23 C 0.20107(17) 0.36930(17) 0.28555(16) 0.0280(6) Uani 1 1 d . . .
H23 H 0.2577 0.3575 0.3117 0.034 Uiso 1 1 calc R . .
C24 C 0.02060(17) 0.13356(17) 0.12280(17) 0.0311(7) Uani 1 1 d . . .
H24 H -0.0335 0.1056 0.1378 0.037 Uiso 1 1 calc R . .
C25 C 0.86095(17) 0.16270(17) 0.31691(17) 0.0301(7) Uani 1 1 d . . .
H25 H 0.8469 0.1855 0.2642 0.036 Uiso 1 1 calc R . .
C26 C 0.47385(17) 0.34001(18) 0.02154(17) 0.0327(7) Uani 1 1 d . . .
H26 H 0.4660 0.2988 -0.0229 0.039 Uiso 1 1 calc R . .
C27 C 0.90256(17) 0.09777(18) 0.47072(18) 0.0340(7) Uani 1 1 d . . .
H27 H 0.9169 0.0758 0.5236 0.041 Uiso 1 1 calc R . .
C28 C 0.94868(17) 0.14810(17) 0.34270(18) 0.0317(7) Uani 1 1 d . . .
H28 H 0.9952 0.1615 0.3078 0.038 Uiso 1 1 calc R . .
C29 C -0.17851(18) 0.40585(17) 0.35843(18) 0.0310(7) Uani 1 1 d . . .
C30 C 0.81423(17) 0.11338(17) 0.44543(17) 0.0312(7) Uani 1 1 d . . .
H30 H 0.7681 0.1030 0.4814 0.037 Uiso 1 1 calc R . .
C31 C 0.55393(18) 0.38633(19) 0.03268(19) 0.0398(8) Uani 1 1 d . . .
H31 H 0.5995 0.3780 -0.0042 0.048 Uiso 1 1 calc R . .
C32 C 0.49810(17) 0.45846(18) 0.14841(18) 0.0351(7) Uani 1 1 d . . .
H32 H 0.5051 0.4994 0.1931 0.042 Uiso 1 1 calc R . .
C33 C -0.33093(19) 0.43498(19) 0.44061(19) 0.0401(8) Uani 1 1 d . . .
H33 H -0.3838 0.4447 0.4686 0.048 Uiso 1 1 calc R . .
C34 C -0.26033(18) 0.39103(17) 0.32029(18) 0.0350(7) Uani 1 1 d . . .
H34 H -0.2645 0.3711 0.2658 0.042 Uiso 1 1 calc R . .
C35 C -0.33649(18) 0.40523(18) 0.36169(19) 0.0382(7) Uani 1 1 d . . .
H35 H -0.3933 0.3944 0.3357 0.046 Uiso 1 1 calc R . .
C36 C -0.24835(19) 0.45059(19) 0.47904(19) 0.0401(8) Uani 1 1 d . . .
H36 H -0.2445 0.4713 0.5333 0.048 Uiso 1 1 calc R . .
C37 C -0.17104(18) 0.43592(18) 0.43798(19) 0.0382(7) Uani 1 1 d . . .
H37 H -0.1140 0.4463 0.4638 0.046 Uiso 1 1 calc R . .
C38 C 0.56733(18) 0.4446(2) 0.0976(2) 0.0411(8) Uani 1 1 d . . .
H38 H 0.6231 0.4749 0.1075 0.049 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.939(2) . ?
Fe1 N5 1.940(2) . ?
Fe1 N1 1.961(2) . ?
Fe1 N4 1.9753(19) . ?
Fe1 N3 1.976(2) . ?
Fe1 N2 1.981(2) . ?
S1 C3 1.646(3) . ?
S2 C12 1.635(3) . ?
N1 C10 1.340(3) . ?
N1 C6 1.358(3) . ?
N2 C4 1.288(3) . ?
N2 C1 1.440(3) . ?
C1 C23 1.381(3) . ?
C1 C8 1.387(3) . ?
C2 C14 1.387(3) . ?
C2 C11 1.390(3) . ?
C2 N3 1.437(3) . ?
C3 N7 1.163(3) . ?
N3 C5 1.287(3) . ?
C4 C15 1.446(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.453(3) . ?
C5 H5 0.9500 . ?
N4 C26 1.340(3) . ?
N4 C15 1.359(3) . ?
N5 C12 1.165(3) . ?
C6 C18 1.382(3) . ?
C7 C9 1.386(4) . ?
C7 C8 1.386(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.376(4) . ?
C9 N10 1.451(3) . ?
C10 C20 1.380(3) . ?
C10 H10 0.9500 . ?
C11 C22 1.378(3) . ?
C11 H11 0.9500 . ?
C13 C23 1.382(3) . ?
C13 H13 0.9500 . ?
C14 C16 1.388(3) . ?
C14 H14 0.9500 . ?
C15 C32 1.383(3) . ?
C16 C19 1.389(3) . ?
C16 H16 0.9500 . ?
N6 N8 1.250(3) . ?
N6 C21 1.440(3) . ?
C17 C27 1.375(4) . ?
C17 C28 1.378(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.386(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.380(4) . ?
C19 N8 1.433(3) . ?
N9 N10 1.240(3) . ?
N9 C29 1.457(3) . ?
C20 C24 1.377(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.373(4) . ?
C21 C25 1.389(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.380(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.378(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.389(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.371(4) . ?
C29 C37 1.392(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.374(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.380(4) . ?
C33 C36 1.384(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.392(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.53(9) . . ?
N7 Fe1 N1 93.83(8) . . ?
N5 Fe1 N1 92.58(8) . . ?
N7 Fe1 N4 90.76(8) . . ?
N5 Fe1 N4 92.55(9) . . ?
N1 Fe1 N4 173.08(9) . . ?
N7 Fe1 N3 174.19(8) . . ?
N5 Fe1 N3 91.17(8) . . ?
N1 Fe1 N3 80.55(8) . . ?
N4 Fe1 N3 94.71(8) . . ?
N7 Fe1 N2 93.12(8) . . ?
N5 Fe1 N2 172.20(8) . . ?
N1 Fe1 N2 94.05(8) . . ?
N4 Fe1 N2 80.52(8) . . ?
N3 Fe1 N2 85.88(8) . . ?
C10 N1 C6 117.2(2) . . ?
C10 N1 Fe1 128.27(17) . . ?
C6 N1 Fe1 114.42(16) . . ?
C4 N2 C1 117.5(2) . . ?
C4 N2 Fe1 114.88(16) . . ?
C1 N2 Fe1 126.86(15) . . ?
C23 C1 C8 120.5(2) . . ?
C23 C1 N2 120.6(2) . . ?
C8 C1 N2 118.9(2) . . ?
C14 C2 C11 120.5(2) . . ?
C14 C2 N3 121.0(2) . . ?
C11 C2 N3 118.4(2) . . ?
N7 C3 S1 178.9(2) . . ?
C5 N3 C2 119.8(2) . . ?
C5 N3 Fe1 114.71(16) . . ?
C2 N3 Fe1 125.22(16) . . ?
N2 C4 C15 116.5(2) . . ?
N2 C4 H4 121.7 . . ?
C15 C4 H4 121.7 . . ?
N3 C5 C6 116.3(2) . . ?
N3 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C26 N4 C15 117.5(2) . . ?
C26 N4 Fe1 128.24(18) . . ?
C15 N4 Fe1 114.16(15) . . ?
C12 N5 Fe1 166.7(2) . . ?
N1 C6 C18 122.9(2) . . ?
N1 C6 C5 112.5(2) . . ?
C18 C6 C5 124.6(2) . . ?
C9 C7 C8 120.0(2) . . ?
C9 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C1 119.3(2) . . ?
C7 C8 H8 120.3 . . ?
C1 C8 H8 120.3 . . ?
C13 C9 C7 120.2(2) . . ?
C13 C9 N10 115.0(2) . . ?
C7 C9 N10 124.7(2) . . ?
N1 C10 C20 123.2(2) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
C22 C11 C2 119.3(3) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.1(2) . . ?
C9 C13 C23 120.1(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C2 C14 C16 119.6(2) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 122.5(2) . . ?
N4 C15 C4 113.1(2) . . ?
C32 C15 C4 124.4(2) . . ?
C14 C16 C19 119.8(2) . . ?
C14 C16 H16 120.1 . . ?
C19 C16 H16 120.1 . . ?
N8 N6 C21 112.9(2) . . ?
C27 C17 C28 120.2(2) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 171.9(2) . . ?
C6 C18 C24 118.6(2) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 120.0(2) . . ?
C22 C19 N8 114.8(2) . . ?
C16 C19 N8 125.2(2) . . ?
N6 N8 C19 114.3(2) . . ?
N10 N9 C29 113.4(2) . . ?
N9 N10 C9 111.8(2) . . ?
C24 C20 C10 119.0(2) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.0(2) . . ?
C30 C21 N6 116.2(2) . . ?
C25 C21 N6 123.8(2) . . ?
C11 C22 C19 120.7(2) . . ?
C11 C22 H22 119.7 . . ?
C19 C22 H22 119.7 . . ?
C1 C23 C13 119.8(2) . . ?
C1 C23 H23 120.1 . . ?
C13 C23 H23 120.1 . . ?
C20 C24 C18 119.1(2) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C28 C25 C21 119.5(3) . . ?
C28 C25 H25 120.3 . . ?
C21 C25 H25 120.3 . . ?
N4 C26 C31 122.7(3) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 119.7(3) . . ?
C17 C27 H27 120.2 . . ?
C30 C27 H27 120.2 . . ?
C17 C28 C25 120.4(3) . . ?
C17 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
C34 C29 C37 121.1(2) . . ?
C34 C29 N9 114.5(3) . . ?
C37 C29 N9 124.3(3) . . ?
C21 C30 C27 120.2(3) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C38 C31 C26 119.5(3) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C15 C32 C38 118.7(3) . . ?
C15 C32 H32 120.6 . . ?
C38 C32 H32 120.6 . . ?
C35 C33 C36 120.0(3) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.4(3) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 120.6(3) . . ?
C34 C35 H35 119.7 . . ?
C33 C35 H35 119.7 . . ?
C33 C36 C37 119.8(3) . . ?
C33 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C36 C37 C29 119.0(3) . . ?
C36 C37 H37 120.5 . . ?
C29 C37 H37 120.5 . . ?
C31 C38 C32 118.9(3) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.807
_diffrn_reflns_theta_full        22.96
_diffrn_measured_fraction_theta_full 0.807
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_feaza135km2
_database_code_depnum_ccdc_archive 'CCDC 1492632'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0091(9)
_cell_length_b                   14.3725(12)
_cell_length_c                   16.6495(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.839(5)
_cell_angle_gamma                90.00
_cell_volume                     3587.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    8934
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986


_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5427
_exptl_absorpt_correction_T_max  0.8928
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                   its'aim being to analyse the evolution of partial collection of data, 
                   always carried out over the same part of reciprocal space, 
                   and over a large scale of temperature.
                   This  explain the poor completness of data as well as the low theta(max) value, 
                   the low number of unique reflexions collected.
                   In ordre to obtain significant intensities with an exposure time relatively short, 
                   a crystal of neutron size was used. As the aim is to compare the diffraction data 
                   always obtained from the same part of the crystal at different temperature, 
                   problems of intensity scale are not considered to be of prior importance.
                   The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                   over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                   these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                   or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                   but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5543
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         22.99
_reflns_number_total             3987
_reflns_number_gt                3440
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0220P)²+2.1005P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3987
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0725
_refine_ls_wR_factor_gt          0.0682
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29133(2) 0.28431(2) 0.06832(2) 0.02302(13) Uani 1 1 d . . .
S1 S 0.19528(4) 0.48723(5) -0.14272(4) 0.02980(19) Uani 1 1 d . . .
S2 S 0.42145(5) 0.07440(5) -0.10795(4) 0.0342(2) Uani 1 1 d . . .
N1 N 0.17764(13) 0.21973(13) 0.08023(13) 0.0225(5) Uani 1 1 d . . .
N2 N 0.27136(13) 0.37423(13) 0.15597(12) 0.0212(5) Uani 1 1 d . . .
C1 C 0.19373(16) 0.38048(15) 0.20311(16) 0.0214(6) Uani 1 1 d . . .
C2 C 0.41713(16) 0.18545(16) 0.18912(16) 0.0220(6) Uani 1 1 d . . .
C3 C 0.22348(16) 0.41674(18) -0.06785(17) 0.0237(6) Uani 1 1 d . . .
N3 N 0.32815(13) 0.19608(13) 0.15486(13) 0.0226(5) Uani 1 1 d . . .
C4 C 0.34044(17) 0.42198(16) 0.17922(16) 0.0242(6) Uani 1 1 d . . .
H4 H 0.3400 0.4622 0.2245 0.029 Uiso 1 1 calc R . .
C5 C 0.26353(17) 0.15187(16) 0.18568(16) 0.0240(6) Uani 1 1 d . . .
H5 H 0.2727 0.1134 0.2318 0.029 Uiso 1 1 calc R . .
N4 N 0.40674(13) 0.35080(13) 0.07101(13) 0.0255(5) Uani 1 1 d . . .
N5 N 0.32824(14) 0.19775(15) -0.01306(14) 0.0306(6) Uani 1 1 d . . .
C6 C 0.17570(16) 0.16403(16) 0.14608(15) 0.0228(6) Uani 1 1 d . . .
C7 C 0.03606(17) 0.40190(16) 0.20929(17) 0.0293(7) Uani 1 1 d . . .
H7 H -0.0207 0.4132 0.1834 0.035 Uiso 1 1 calc R . .
C8 C 0.11111(16) 0.39677(16) 0.16437(17) 0.0259(6) Uani 1 1 d . . .
H8 H 0.1061 0.4043 0.1076 0.031 Uiso 1 1 calc R . .
C9 C 0.04379(17) 0.39057(17) 0.29201(17) 0.0278(7) Uani 1 1 d . . .
C10 C 0.10173(18) 0.22812(17) 0.03535(17) 0.0289(7) Uani 1 1 d . . .
H10 H 0.1022 0.2648 -0.0121 0.035 Uiso 1 1 calc R . .
C11 C 0.48344(17) 0.15767(17) 0.13904(17) 0.0310(7) Uani 1 1 d . . .
H11 H 0.4690 0.1426 0.0844 0.037 Uiso 1 1 calc R . .
C12 C 0.36600(17) 0.14605(18) -0.05332(16) 0.0248(6) Uani 1 1 d . . .
C13 C 0.12590(18) 0.37557(19) 0.32963(17) 0.0351(7) Uani 1 1 d . . .
H13 H 0.1311 0.3694 0.3865 0.042 Uiso 1 1 calc R . .
C14 C 0.43816(17) 0.20783(16) 0.26882(17) 0.0271(7) Uani 1 1 d . . .
H14 H 0.3927 0.2277 0.3026 0.033 Uiso 1 1 calc R . .
C15 C 0.41868(16) 0.41123(16) 0.13292(16) 0.0252(6) Uani 1 1 d . . .
C16 C 0.52570(17) 0.20115(17) 0.29905(17) 0.0289(7) Uani 1 1 d . . .
H16 H 0.5403 0.2160 0.3537 0.035 Uiso 1 1 calc R . .
N6 N 0.69974(14) 0.15420(14) 0.34686(15) 0.0303(6) Uani 1 1 d . . .
C17 C 0.96917(17) 0.11435(17) 0.41891(18) 0.0321(7) Uani 1 1 d . . .
H17 H 1.0295 0.1025 0.4357 0.039 Uiso 1 1 calc R . .
N7 N 0.24287(13) 0.36755(15) -0.01438(14) 0.0279(5) Uani 1 1 d . . .
C18 C 0.09863(17) 0.12152(17) 0.16961(17) 0.0286(7) Uani 1 1 d . . .
H18 H 0.0992 0.0847 0.2170 0.034 Uiso 1 1 calc R . .
C19 C 0.59190(16) 0.17273(16) 0.24913(17) 0.0254(6) Uani 1 1 d . . .
N8 N 0.68443(14) 0.16277(14) 0.27294(15) 0.0289(5) Uani 1 1 d . . .
N9 N -0.10281(17) 0.39272(14) 0.30781(15) 0.0367(6) Uani 1 1 d . . .
N10 N -0.02999(17) 0.39771(15) 0.34526(15) 0.0373(6) Uani 1 1 d . . .
C20 C 0.02277(18) 0.18632(18) 0.05426(18) 0.0335(7) Uani 1 1 d . . .
H20 H -0.0295 0.1939 0.0203 0.040 Uiso 1 1 calc R . .
C21 C 0.79331(16) 0.14377(16) 0.36865(17) 0.0263(6) Uani 1 1 d . . .
C22 C 0.57059(17) 0.15218(17) 0.16932(17) 0.0301(7) Uani 1 1 d . . .
H22 H 0.6163 0.1341 0.1351 0.036 Uiso 1 1 calc R . .
C23 C 0.20085(17) 0.36932(18) 0.28548(17) 0.0310(7) Uani 1 1 d . . .
H23 H 0.2573 0.3573 0.3117 0.037 Uiso 1 1 calc R . .
C24 C 0.02084(18) 0.13357(18) 0.12302(18) 0.0342(7) Uani 1 1 d . . .
H24 H -0.0332 0.1058 0.1383 0.041 Uiso 1 1 calc R . .
C25 C 0.86086(18) 0.16288(18) 0.31651(18) 0.0332(7) Uani 1 1 d . . .
H25 H 0.8468 0.1856 0.2638 0.040 Uiso 1 1 calc R . .
C26 C 0.47405(18) 0.34016(19) 0.02185(17) 0.0348(7) Uani 1 1 d . . .
H26 H 0.4662 0.2989 -0.0225 0.042 Uiso 1 1 calc R . .
C27 C 0.90239(18) 0.09785(18) 0.47048(19) 0.0371(7) Uani 1 1 d . . .
H27 H 0.9166 0.0757 0.5233 0.044 Uiso 1 1 calc R . .
C28 C 0.94872(18) 0.14813(18) 0.34276(19) 0.0347(7) Uani 1 1 d . . .
H28 H 0.9953 0.1614 0.3079 0.042 Uiso 1 1 calc R . .
C29 C -0.17813(19) 0.40566(17) 0.35842(19) 0.0342(7) Uani 1 1 d . . .
C30 C 0.81420(18) 0.11356(18) 0.44541(18) 0.0339(7) Uani 1 1 d . . .
H30 H 0.7681 0.1034 0.4815 0.041 Uiso 1 1 calc R . .
C31 C 0.55415(18) 0.3864(2) 0.0328(2) 0.0439(8) Uani 1 1 d . . .
H31 H 0.5997 0.3780 -0.0041 0.053 Uiso 1 1 calc R . .
C32 C 0.49825(18) 0.45860(19) 0.14879(18) 0.0378(7) Uani 1 1 d . . .
H32 H 0.5051 0.4995 0.1935 0.045 Uiso 1 1 calc R . .
C33 C -0.3305(2) 0.43521(19) 0.4407(2) 0.0449(8) Uani 1 1 d . . .
H33 H -0.3834 0.4451 0.4685 0.054 Uiso 1 1 calc R . .
C34 C -0.25979(19) 0.39069(18) 0.32060(19) 0.0378(8) Uani 1 1 d . . .
H34 H -0.2641 0.3703 0.2663 0.045 Uiso 1 1 calc R . .
C35 C -0.33593(19) 0.40539(19) 0.3619(2) 0.0415(8) Uani 1 1 d . . .
H35 H -0.3928 0.3949 0.3358 0.050 Uiso 1 1 calc R . .
C36 C -0.2482(2) 0.4507(2) 0.4792(2) 0.0452(8) Uani 1 1 d . . .
H36 H -0.2443 0.4714 0.5335 0.054 Uiso 1 1 calc R . .
C37 C -0.17067(19) 0.43585(18) 0.4380(2) 0.0406(8) Uani 1 1 d . . .
H37 H -0.1137 0.4462 0.4638 0.049 Uiso 1 1 calc R . .
C38 C 0.56753(19) 0.4449(2) 0.0979(2) 0.0465(8) Uani 1 1 d . . .
H38 H 0.6232 0.4753 0.1077 0.056 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.938(2) . ?
Fe1 N5 1.940(2) . ?
Fe1 N1 1.961(2) . ?
Fe1 N4 1.977(2) . ?
Fe1 N3 1.978(2) . ?
Fe1 N2 1.983(2) . ?
S1 C3 1.645(3) . ?
S2 C12 1.630(3) . ?
N1 C10 1.337(3) . ?
N1 C6 1.359(3) . ?
N2 C4 1.287(3) . ?
N2 C1 1.440(3) . ?
C1 C23 1.380(4) . ?
C1 C8 1.389(3) . ?
C2 C14 1.386(4) . ?
C2 C11 1.388(3) . ?
C2 N3 1.434(3) . ?
C3 N7 1.162(3) . ?
N3 C5 1.287(3) . ?
C4 C15 1.445(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.455(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.340(3) . ?
N4 C15 1.353(3) . ?
N5 C12 1.166(3) . ?
C6 C18 1.382(3) . ?
C7 C8 1.385(3) . ?
C7 C9 1.386(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.372(4) . ?
C9 N10 1.456(3) . ?
C10 C20 1.379(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.381(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.377(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.387(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.389(3) . ?
C16 C19 1.388(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.247(3) . ?
N6 C21 1.441(3) . ?
C17 C27 1.372(4) . ?
C17 C28 1.378(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.380(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.383(4) . ?
C19 N8 1.432(3) . ?
N9 N10 1.233(3) . ?
N9 C29 1.455(3) . ?
C20 C24 1.375(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.371(4) . ?
C21 C25 1.394(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.385(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.378(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.387(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.367(4) . ?
C29 C37 1.393(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.378(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.388(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.378(4) . ?
C33 C36 1.382(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.396(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.56(9) . . ?
N7 Fe1 N1 93.79(9) . . ?
N5 Fe1 N1 92.70(8) . . ?
N7 Fe1 N4 90.87(8) . . ?
N5 Fe1 N4 92.62(9) . . ?
N1 Fe1 N4 172.89(9) . . ?
N7 Fe1 N3 174.20(9) . . ?
N5 Fe1 N3 91.06(8) . . ?
N1 Fe1 N3 80.56(9) . . ?
N4 Fe1 N3 94.62(8) . . ?
N7 Fe1 N2 93.18(8) . . ?
N5 Fe1 N2 172.08(8) . . ?
N1 Fe1 N2 94.02(8) . . ?
N4 Fe1 N2 80.36(8) . . ?
N3 Fe1 N2 85.91(8) . . ?
C10 N1 C6 116.9(2) . . ?
C10 N1 Fe1 128.51(18) . . ?
C6 N1 Fe1 114.45(17) . . ?
C4 N2 C1 117.7(2) . . ?
C4 N2 Fe1 114.83(16) . . ?
C1 N2 Fe1 126.71(15) . . ?
C23 C1 C8 120.3(2) . . ?
C23 C1 N2 120.7(2) . . ?
C8 C1 N2 119.0(2) . . ?
C14 C2 C11 120.4(2) . . ?
C14 C2 N3 121.3(2) . . ?
C11 C2 N3 118.2(2) . . ?
N7 C3 S1 179.2(3) . . ?
C5 N3 C2 119.6(2) . . ?
C5 N3 Fe1 114.72(17) . . ?
C2 N3 Fe1 125.40(16) . . ?
N2 C4 C15 116.5(2) . . ?
N2 C4 H4 121.7 . . ?
C15 C4 H4 121.7 . . ?
N3 C5 C6 116.3(2) . . ?
N3 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C26 N4 C15 117.6(2) . . ?
C26 N4 Fe1 128.12(19) . . ?
C15 N4 Fe1 114.23(16) . . ?
C12 N5 Fe1 166.8(2) . . ?
N1 C6 C18 122.7(2) . . ?
N1 C6 C5 112.4(2) . . ?
C18 C6 C5 124.8(2) . . ?
C8 C7 C9 120.0(2) . . ?
C8 C7 H7 120.0 . . ?
C9 C7 H7 120.0 . . ?
C7 C8 C1 119.3(3) . . ?
C7 C8 H8 120.3 . . ?
C1 C8 H8 120.3 . . ?
C13 C9 C7 120.1(2) . . ?
C13 C9 N10 115.2(3) . . ?
C7 C9 N10 124.6(2) . . ?
N1 C10 C20 123.5(3) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
C22 C11 C2 119.4(3) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.3(2) . . ?
C9 C13 C23 120.4(3) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C2 C14 C16 119.9(2) . . ?
C2 C14 H14 120.1 . . ?
C16 C14 H14 120.1 . . ?
N4 C15 C32 122.7(2) . . ?
N4 C15 C4 113.3(2) . . ?
C32 C15 C4 124.1(3) . . ?
C14 C16 C19 119.8(3) . . ?
C14 C16 H16 120.1 . . ?
C19 C16 H16 120.1 . . ?
N8 N6 C21 112.9(2) . . ?
C27 C17 C28 120.0(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 172.0(2) . . ?
C24 C18 C6 118.8(2) . . ?
C24 C18 H18 120.6 . . ?
C6 C18 H18 120.6 . . ?
C22 C19 C16 120.0(2) . . ?
C22 C19 N8 114.8(2) . . ?
C16 C19 N8 125.2(2) . . ?
N6 N8 C19 114.3(2) . . ?
N10 N9 C29 113.2(3) . . ?
N9 N10 C9 111.7(2) . . ?
C24 C20 C10 119.0(3) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.2(2) . . ?
C30 C21 N6 116.3(2) . . ?
C25 C21 N6 123.5(2) . . ?
C11 C22 C19 120.6(3) . . ?
C11 C22 H22 119.7 . . ?
C19 C22 H22 119.7 . . ?
C13 C23 C1 119.9(2) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C20 C24 C18 119.0(3) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C28 C25 C21 118.9(3) . . ?
C28 C25 H25 120.5 . . ?
C21 C25 H25 120.5 . . ?
N4 C26 C31 122.9(3) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 120.0(3) . . ?
C17 C27 H27 120.0 . . ?
C30 C27 H27 120.0 . . ?
C17 C28 C25 120.6(3) . . ?
C17 C28 H28 119.7 . . ?
C25 C28 H28 119.7 . . ?
C34 C29 C37 121.0(3) . . ?
C34 C29 N9 114.7(3) . . ?
C37 C29 N9 124.2(3) . . ?
C21 C30 C27 120.2(3) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C26 C31 C38 119.4(3) . . ?
C26 C31 H31 120.3 . . ?
C38 C31 H31 120.3 . . ?
C38 C32 C15 118.5(3) . . ?
C38 C32 H32 120.7 . . ?
C15 C32 H32 120.7 . . ?
C35 C33 C36 120.1(3) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.5(3) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C33 C35 C34 120.7(3) . . ?
C33 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C33 C36 C37 119.6(3) . . ?
C33 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C29 C37 C36 119.1(3) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C31 C38 C32 118.8(3) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.800
_diffrn_reflns_theta_full        22.99
_diffrn_measured_fraction_theta_full 0.800
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_feaza150kd1
_database_code_depnum_ccdc_archive 'CCDC 1492633'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0119(11)
_cell_length_b                   14.3903(11)
_cell_length_c                   16.6678(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.793(4)
_cell_angle_gamma                90.00
_cell_volume                     3596.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5559
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5434
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
    its'aim being to analyse the evolution of partial collection of data, 
    always carried out over the same part of reciprocal space, 
    and over a large scale of temperature.
    This  explain the poor completness of data as well as the low theta(max) value, 
    the low number of unique reflexions collected.
    In ordre to obtain significant intensities with an exposure time relatively short, 
    a crystal of neutron size was used. As the aim is to compare the diffraction data 
    always obtained from the same part of the crystal at different temperature, 
    problems of intensity scale are not considered to be of prior importance.
    The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
    over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
    these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
    or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
    but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5650
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         21.25
_reflns_number_total             3378
_reflns_number_gt                2956
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0284P)²+1.8750P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3378
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29163(2) 0.28440(3) 0.06777(2) 0.02594(16) Uani 1 1 d . . .
S1 S 0.19520(4) 0.48732(5) -0.14264(4) 0.0337(2) Uani 1 1 d . . .
S2 S 0.42211(5) 0.07453(5) -0.10817(4) 0.0384(2) Uani 1 1 d . . .
N1 N 0.17757(13) 0.21947(15) 0.08000(13) 0.0243(6) Uani 1 1 d . . .
N2 N 0.27141(13) 0.37435(15) 0.15619(12) 0.0224(5) Uani 1 1 d . . .
C1 C 0.19369(16) 0.38067(18) 0.20330(18) 0.0233(7) Uani 1 1 d . . .
C2 C 0.41752(17) 0.18540(18) 0.18924(18) 0.0252(7) Uani 1 1 d . . .
C3 C 0.22301(16) 0.4167(2) -0.06790(18) 0.0266(7) Uani 1 1 d . . .
N3 N 0.32821(13) 0.19594(14) 0.15465(12) 0.0238(6) Uani 1 1 d . . .
C4 C 0.34081(18) 0.42175(19) 0.17928(16) 0.0274(7) Uani 1 1 d . . .
H4 H 0.3406 0.4616 0.2247 0.033 Uiso 1 1 calc R . .
C5 C 0.26344(17) 0.15183(19) 0.18567(16) 0.0271(7) Uani 1 1 d . . .
H5 H 0.2724 0.1136 0.2318 0.032 Uiso 1 1 calc R . .
N4 N 0.40746(13) 0.35113(15) 0.07123(14) 0.0269(6) Uani 1 1 d . . .
N5 N 0.32885(15) 0.19819(17) -0.01352(14) 0.0342(6) Uani 1 1 d . . .
C6 C 0.17584(16) 0.16415(19) 0.14578(16) 0.0249(7) Uani 1 1 d . . .
C7 C 0.03642(17) 0.40186(19) 0.2086(2) 0.0319(8) Uani 1 1 d . . .
H7 H -0.0202 0.4132 0.1826 0.038 Uiso 1 1 calc R . .
C8 C 0.11175(17) 0.39674(18) 0.16474(17) 0.0282(7) Uani 1 1 d . . .
H8 H 0.1073 0.4043 0.1081 0.034 Uiso 1 1 calc R . .
C9 C 0.04435(18) 0.39033(19) 0.2911(2) 0.0319(8) Uani 1 1 d . . .
C10 C 0.10185(18) 0.22820(19) 0.03517(17) 0.0316(7) Uani 1 1 d . . .
H10 H 0.1022 0.2649 -0.0122 0.038 Uiso 1 1 calc R . .
C11 C 0.48362(17) 0.1578(2) 0.13930(17) 0.0315(7) Uani 1 1 d . . .
H11 H 0.4693 0.1429 0.0847 0.038 Uiso 1 1 calc R . .
C12 C 0.36672(17) 0.1467(2) -0.05347(17) 0.0277(7) Uani 1 1 d . . .
C13 C 0.12631(19) 0.3756(2) 0.32938(18) 0.0386(8) Uani 1 1 d . . .
H13 H 0.1313 0.3699 0.3862 0.046 Uiso 1 1 calc R . .
C14 C 0.43781(17) 0.20729(19) 0.26867(17) 0.0295(7) Uani 1 1 d . . .
H14 H 0.3922 0.2267 0.3025 0.035 Uiso 1 1 calc R . .
C15 C 0.41911(16) 0.41141(19) 0.13278(17) 0.0279(7) Uani 1 1 d . . .
C16 C 0.52559(18) 0.20067(19) 0.29871(17) 0.0314(7) Uani 1 1 d . . .
H16 H 0.5401 0.2154 0.3533 0.038 Uiso 1 1 calc R . .
N6 N 0.69972(14) 0.15419(16) 0.34688(16) 0.0334(6) Uani 1 1 d . . .
C17 C 0.96875(18) 0.11451(19) 0.41868(19) 0.0348(8) Uani 1 1 d . . .
H17 H 1.0290 0.1025 0.4356 0.042 Uiso 1 1 calc R . .
N7 N 0.24298(14) 0.36794(17) -0.01439(15) 0.0320(6) Uani 1 1 d . . .
C18 C 0.09921(17) 0.12164(19) 0.16955(17) 0.0313(7) Uani 1 1 d . . .
H18 H 0.1001 0.0847 0.2168 0.038 Uiso 1 1 calc R . .
C19 C 0.59153(17) 0.17280(19) 0.24934(18) 0.0280(7) Uani 1 1 d . . .
N8 N 0.68468(14) 0.16277(16) 0.27278(16) 0.0325(6) Uani 1 1 d . . .
N9 N -0.10141(18) 0.39274(16) 0.30790(15) 0.0421(7) Uani 1 1 d . . .
N10 N -0.02960(18) 0.39820(17) 0.34578(15) 0.0454(7) Uani 1 1 d . . .
C20 C 0.02316(18) 0.1862(2) 0.05470(18) 0.0370(8) Uani 1 1 d . . .
H20 H -0.0292 0.1936 0.0210 0.044 Uiso 1 1 calc R . .
C21 C 0.79372(17) 0.14386(19) 0.36887(18) 0.0290(7) Uani 1 1 d . . .
C22 C 0.57091(17) 0.15219(19) 0.16981(18) 0.0322(8) Uani 1 1 d . . .
H22 H 0.6168 0.1341 0.1358 0.039 Uiso 1 1 calc R . .
C23 C 0.20054(18) 0.3692(2) 0.28558(19) 0.0341(8) Uani 1 1 d . . .
H23 H 0.2569 0.3568 0.3117 0.041 Uiso 1 1 calc R . .
C24 C 0.02124(18) 0.1337(2) 0.12344(19) 0.0377(8) Uani 1 1 d . . .
H24 H -0.0328 0.1061 0.1389 0.045 Uiso 1 1 calc R . .
C25 C 0.86074(18) 0.1625(2) 0.31664(18) 0.0362(8) Uani 1 1 d . . .
H25 H 0.8465 0.1847 0.2639 0.043 Uiso 1 1 calc R . .
C26 C 0.47430(19) 0.3409(2) 0.02224(18) 0.0404(8) Uani 1 1 d . . .
H26 H 0.4665 0.3003 -0.0225 0.048 Uiso 1 1 calc R . .
C27 C 0.90192(19) 0.0983(2) 0.46996(18) 0.0404(8) Uani 1 1 d . . .
H27 H 0.9160 0.0766 0.5229 0.048 Uiso 1 1 calc R . .
C28 C 0.94858(18) 0.1482(2) 0.34264(19) 0.0382(8) Uani 1 1 d . . .
H28 H 0.9952 0.1618 0.3079 0.046 Uiso 1 1 calc R . .
C29 C -0.1782(2) 0.4057(2) 0.3589(2) 0.0400(8) Uani 1 1 d . . .
C30 C 0.81390(18) 0.1134(2) 0.44477(18) 0.0359(8) Uani 1 1 d . . .
H30 H 0.7676 0.1024 0.4805 0.043 Uiso 1 1 calc R . .
C31 C 0.5541(2) 0.3869(2) 0.0342(2) 0.0500(9) Uani 1 1 d . . .
H31 H 0.6001 0.3781 -0.0023 0.060 Uiso 1 1 calc R . .
C32 C 0.49821(18) 0.4585(2) 0.14924(18) 0.0415(8) Uani 1 1 d . . .
H32 H 0.5049 0.4989 0.1942 0.050 Uiso 1 1 calc R . .
C33 C -0.3297(2) 0.4352(2) 0.4412(2) 0.0486(9) Uani 1 1 d . . .
H33 H -0.3828 0.4451 0.4688 0.058 Uiso 1 1 calc R . .
C34 C -0.2592(2) 0.3910(2) 0.3213(2) 0.0441(8) Uani 1 1 d . . .
H34 H -0.2635 0.3711 0.2669 0.053 Uiso 1 1 calc R . .
C35 C -0.3349(2) 0.4053(2) 0.3629(2) 0.0477(9) Uani 1 1 d . . .
H35 H -0.3917 0.3943 0.3371 0.057 Uiso 1 1 calc R . .
C36 C -0.2479(2) 0.4508(2) 0.4798(2) 0.0497(9) Uani 1 1 d . . .
H36 H -0.2442 0.4717 0.5339 0.060 Uiso 1 1 calc R . .
C37 C -0.16966(19) 0.4355(2) 0.4382(2) 0.0468(9) Uani 1 1 d . . .
H37 H -0.1125 0.4453 0.4638 0.056 Uiso 1 1 calc R . .
C38 C 0.56748(19) 0.4452(2) 0.0985(2) 0.0516(9) Uani 1 1 d . . .
H38 H 0.6230 0.4759 0.1081 0.062 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.938(3) . ?
Fe1 N5 1.939(3) . ?
Fe1 N1 1.970(2) . ?
Fe1 N4 1.985(2) . ?
Fe1 N3 1.985(2) . ?
Fe1 N2 1.996(2) . ?
S1 C3 1.646(3) . ?
S2 C12 1.635(3) . ?
N1 C10 1.335(3) . ?
N1 C6 1.356(3) . ?
N2 C4 1.288(3) . ?
N2 C1 1.441(3) . ?
C1 C8 1.379(3) . ?
C1 C23 1.380(4) . ?
C2 C14 1.380(4) . ?
C2 C11 1.384(4) . ?
C2 N3 1.441(3) . ?
C3 N7 1.162(3) . ?
N3 C5 1.290(3) . ?
C4 C15 1.447(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.455(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.332(3) . ?
N4 C15 1.348(3) . ?
N5 C12 1.163(3) . ?
C6 C18 1.378(4) . ?
C7 C8 1.378(4) . ?
C7 C9 1.384(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.375(4) . ?
C9 N10 1.475(4) . ?
C10 C20 1.380(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.385(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.365(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.383(4) . ?
C16 C19 1.377(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.251(3) . ?
N6 C21 1.448(3) . ?
C17 C27 1.369(4) . ?
C17 C28 1.377(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.379(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.379(4) . ?
C19 N8 1.441(3) . ?
N9 N10 1.225(3) . ?
N9 C29 1.478(4) . ?
C20 C24 1.375(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.359(4) . ?
C21 C25 1.388(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.375(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.384(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.356(4) . ?
C29 C37 1.390(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.368(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.386(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.372(4) . ?
C33 C36 1.377(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.409(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.83(10) . . ?
N7 Fe1 N1 93.88(9) . . ?
N5 Fe1 N1 92.88(9) . . ?
N7 Fe1 N4 91.14(9) . . ?
N5 Fe1 N4 92.75(10) . . ?
N1 Fe1 N4 172.40(9) . . ?
N7 Fe1 N3 173.92(9) . . ?
N5 Fe1 N3 91.18(9) . . ?
N1 Fe1 N3 80.29(9) . . ?
N4 Fe1 N3 94.49(9) . . ?
N7 Fe1 N2 93.09(9) . . ?
N5 Fe1 N2 171.97(9) . . ?
N1 Fe1 N2 93.84(8) . . ?
N4 Fe1 N2 80.18(9) . . ?
N3 Fe1 N2 85.64(8) . . ?
C10 N1 C6 117.3(2) . . ?
C10 N1 Fe1 128.2(2) . . ?
C6 N1 Fe1 114.40(16) . . ?
C4 N2 C1 117.9(2) . . ?
C4 N2 Fe1 114.47(17) . . ?
C1 N2 Fe1 126.85(17) . . ?
C8 C1 C23 120.3(2) . . ?
C8 C1 N2 119.0(3) . . ?
C23 C1 N2 120.7(2) . . ?
C14 C2 C11 120.7(2) . . ?
C14 C2 N3 121.1(2) . . ?
C11 C2 N3 118.0(2) . . ?
N7 C3 S1 179.0(3) . . ?
C5 N3 C2 119.5(2) . . ?
C5 N3 Fe1 114.88(17) . . ?
C2 N3 Fe1 125.31(17) . . ?
N2 C4 C15 116.9(3) . . ?
N2 C4 H4 121.6 . . ?
C15 C4 H4 121.6 . . ?
N3 C5 C6 116.0(2) . . ?
N3 C5 H5 122.0 . . ?
C6 C5 H5 122.0 . . ?
C26 N4 C15 117.6(2) . . ?
C26 N4 Fe1 127.8(2) . . ?
C15 N4 Fe1 114.47(16) . . ?
C12 N5 Fe1 166.7(2) . . ?
N1 C6 C18 122.8(2) . . ?
N1 C6 C5 112.8(2) . . ?
C18 C6 C5 124.3(3) . . ?
C8 C7 C9 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C9 C7 H7 120.4 . . ?
C7 C8 C1 119.9(3) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
C13 C9 C7 120.7(2) . . ?
C13 C9 N10 114.1(3) . . ?
C7 C9 N10 125.0(3) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C2 C11 C22 119.3(3) . . ?
C2 C11 H11 120.4 . . ?
C22 C11 H11 120.4 . . ?
N5 C12 S2 178.6(3) . . ?
C23 C13 C9 119.9(3) . . ?
C23 C13 H13 120.1 . . ?
C9 C13 H13 120.1 . . ?
C2 C14 C16 119.4(2) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
N4 C15 C32 123.0(3) . . ?
N4 C15 C4 113.3(2) . . ?
C32 C15 C4 123.7(3) . . ?
C19 C16 C14 120.1(3) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 112.8(2) . . ?
C27 C17 C28 120.0(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 172.1(2) . . ?
C6 C18 C24 118.8(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C16 C19 C22 120.2(2) . . ?
C16 C19 N8 125.7(3) . . ?
C22 C19 N8 114.1(2) . . ?
N6 N8 C19 113.8(2) . . ?
N10 N9 C29 112.8(3) . . ?
N9 N10 C9 110.3(3) . . ?
C24 C20 C10 119.4(3) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 120.7(2) . . ?
C30 C21 N6 116.0(2) . . ?
C25 C21 N6 123.3(3) . . ?
C19 C22 C11 120.3(2) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.0(3) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C20 C24 C18 118.8(3) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C28 C25 C21 118.9(3) . . ?
C28 C25 H25 120.5 . . ?
C21 C25 H25 120.5 . . ?
N4 C26 C31 122.4(3) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 120.1(3) . . ?
C17 C27 H27 119.9 . . ?
C30 C27 H27 119.9 . . ?
C17 C28 C25 120.3(3) . . ?
C17 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
C34 C29 C37 121.8(3) . . ?
C34 C29 N9 114.9(3) . . ?
C37 C29 N9 123.2(3) . . ?
C21 C30 C27 119.9(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 120.1(3) . . ?
C38 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?
C15 C32 C38 118.3(3) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C35 C33 C36 120.2(3) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.1(3) . . ?
C29 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C33 C35 C34 121.1(3) . . ?
C33 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C33 C36 C37 119.4(3) . . ?
C33 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C29 C37 C36 118.3(3) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 118.5(3) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.846
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.846
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza155km2
_database_code_depnum_ccdc_archive 'CCDC 1492634'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   15.0171(9)
_cell_length_b                   14.3939(12)
_cell_length_c                   16.6705(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.807(5)
_cell_angle_gamma                90.00
_cell_volume                     3599.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    155(2)
_cell_measurement_reflns_used    8806
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5436
_exptl_absorpt_correction_T_max  0.8931
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                   its'aim being to analyse the evolution of partial collection of data, 
                   always carried out over the same part of reciprocal space, 
                   and over a large scale of temperature.
                   This  explain the poor completness of data as well as the low theta(max) value, 
                   the low number of unique reflexions collected.
                   In ordre to obtain significant intensities with an exposure time relatively short, 
                   a crystal of neutron size was used. As the aim is to compare the diffraction data 
                   always obtained from the same part of the crystal at different temperature, 
                   problems of intensity scale are not considered to be of prior importance.
                   The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                   over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                   these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                   or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                   but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      155(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5570
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         22.97
_reflns_number_total             4005
_reflns_number_gt                3411
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0212P)²+2.5484P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4005
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0773
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29167(2) 0.28443(2) 0.06768(2) 0.02710(15) Uani 1 1 d . . .
S1 S 0.19518(5) 0.48739(5) -0.14270(5) 0.0352(2) Uani 1 1 d . . .
S2 S 0.42228(5) 0.07457(5) -0.10813(5) 0.0400(2) Uani 1 1 d . . .
N1 N 0.17770(15) 0.21941(14) 0.08004(14) 0.0260(6) Uani 1 1 d . . .
N2 N 0.27154(14) 0.37446(14) 0.15614(13) 0.0243(5) Uani 1 1 d . . .
C1 C 0.19402(17) 0.38080(17) 0.20302(17) 0.0254(7) Uani 1 1 d . . .
C2 C 0.41727(18) 0.18524(17) 0.18909(17) 0.0256(7) Uani 1 1 d . . .
C3 C 0.22325(17) 0.41685(19) -0.06818(19) 0.0283(7) Uani 1 1 d . . .
N3 N 0.32842(15) 0.19588(14) 0.15464(14) 0.0253(6) Uani 1 1 d . . .
C4 C 0.34071(18) 0.42182(18) 0.17974(18) 0.0289(7) Uani 1 1 d . . .
H4 H 0.3404 0.4615 0.2253 0.035 Uiso 1 1 calc R . .
C5 C 0.26381(18) 0.15196(17) 0.18539(17) 0.0273(7) Uani 1 1 d . . .
H5 H 0.2729 0.1136 0.2315 0.033 Uiso 1 1 calc R . .
N4 N 0.40741(14) 0.35121(15) 0.07129(14) 0.0290(6) Uani 1 1 d . . .
N5 N 0.32934(16) 0.19817(17) -0.01380(16) 0.0360(6) Uani 1 1 d . . .
C6 C 0.17620(18) 0.16406(17) 0.14586(17) 0.0260(7) Uani 1 1 d . . .
C7 C 0.03652(19) 0.40211(18) 0.20917(19) 0.0338(7) Uani 1 1 d . . .
H7 H -0.0201 0.4135 0.1832 0.041 Uiso 1 1 calc R . .
C8 C 0.11180(18) 0.39695(17) 0.16433(18) 0.0285(7) Uani 1 1 d . . .
H8 H 0.1070 0.4044 0.1077 0.034 Uiso 1 1 calc R . .
C9 C 0.04377(19) 0.39068(18) 0.29156(19) 0.0330(8) Uani 1 1 d . . .
C10 C 0.1019(2) 0.22805(19) 0.03522(19) 0.0334(7) Uani 1 1 d . . .
H10 H 0.1024 0.2646 -0.0122 0.040 Uiso 1 1 calc R . .
C11 C 0.48376(19) 0.15744(19) 0.13919(19) 0.0342(7) Uani 1 1 d . . .
H11 H 0.4695 0.1422 0.0846 0.041 Uiso 1 1 calc R . .
C12 C 0.36711(18) 0.1464(2) -0.05366(18) 0.0293(7) Uani 1 1 d . . .
C13 C 0.1257(2) 0.3757(2) 0.32944(19) 0.0401(8) Uani 1 1 d . . .
H13 H 0.1308 0.3696 0.3862 0.048 Uiso 1 1 calc R . .
C14 C 0.43827(19) 0.20741(18) 0.26850(18) 0.0317(7) Uani 1 1 d . . .
H14 H 0.3928 0.2273 0.3023 0.038 Uiso 1 1 calc R . .
C15 C 0.41905(17) 0.41141(18) 0.13309(18) 0.0293(7) Uani 1 1 d . . .
C16 C 0.52575(19) 0.20061(18) 0.29876(19) 0.0332(7) Uani 1 1 d . . .
H16 H 0.5403 0.2152 0.3534 0.040 Uiso 1 1 calc R . .
N6 N 0.69951(15) 0.15419(15) 0.34643(17) 0.0346(6) Uani 1 1 d . . .
C17 C 0.9687(2) 0.11482(19) 0.4188(2) 0.0376(8) Uani 1 1 d . . .
H17 H 1.0290 0.1032 0.4358 0.045 Uiso 1 1 calc R . .
N7 N 0.24274(15) 0.36798(16) -0.01479(16) 0.0338(6) Uani 1 1 d . . .
C18 C 0.09912(19) 0.12187(19) 0.16984(19) 0.0336(8) Uani 1 1 d . . .
H18 H 0.0997 0.0853 0.2173 0.040 Uiso 1 1 calc R . .
C19 C 0.59182(18) 0.17239(18) 0.24893(19) 0.0300(7) Uani 1 1 d . . .
N8 N 0.68469(15) 0.16271(15) 0.27281(17) 0.0336(6) Uani 1 1 d . . .
N9 N -0.1012(2) 0.39300(16) 0.30824(17) 0.0433(7) Uani 1 1 d . . .
N10 N -0.02965(19) 0.39809(16) 0.34577(18) 0.0448(7) Uani 1 1 d . . .
C20 C 0.0233(2) 0.1865(2) 0.0545(2) 0.0402(8) Uani 1 1 d . . .
H20 H -0.0289 0.1941 0.0206 0.048 Uiso 1 1 calc R . .
C21 C 0.79338(18) 0.14381(18) 0.36826(19) 0.0309(7) Uani 1 1 d . . .
C22 C 0.57057(19) 0.15214(19) 0.16976(19) 0.0340(8) Uani 1 1 d . . .
H22 H 0.6164 0.1342 0.1356 0.041 Uiso 1 1 calc R . .
C23 C 0.20070(19) 0.36948(19) 0.28506(18) 0.0357(7) Uani 1 1 d . . .
H23 H 0.2571 0.3574 0.3112 0.043 Uiso 1 1 calc R . .
C24 C 0.0209(2) 0.1340(2) 0.1233(2) 0.0395(8) Uani 1 1 d . . .
H24 H -0.0332 0.1065 0.1386 0.047 Uiso 1 1 calc R . .
C25 C 0.86080(19) 0.16253(19) 0.3165(2) 0.0381(8) Uani 1 1 d . . .
H25 H 0.8469 0.1847 0.2637 0.046 Uiso 1 1 calc R . .
C26 C 0.4747(2) 0.3410(2) 0.0222(2) 0.0417(8) Uani 1 1 d . . .
H26 H 0.4669 0.3004 -0.0225 0.050 Uiso 1 1 calc R . .
C27 C 0.9021(2) 0.0981(2) 0.4700(2) 0.0426(8) Uani 1 1 d . . .
H27 H 0.9163 0.0760 0.5228 0.051 Uiso 1 1 calc R . .
C28 C 0.9485(2) 0.1484(2) 0.3428(2) 0.0404(8) Uani 1 1 d . . .
H28 H 0.9952 0.1619 0.3082 0.048 Uiso 1 1 calc R . .
C29 C -0.1775(2) 0.4058(2) 0.3592(2) 0.0412(8) Uani 1 1 d . . .
C30 C 0.8138(2) 0.1135(2) 0.4451(2) 0.0400(8) Uani 1 1 d . . .
H30 H 0.7677 0.1032 0.4810 0.048 Uiso 1 1 calc R . .
C31 C 0.5546(2) 0.3867(2) 0.0337(2) 0.0533(10) Uani 1 1 d . . .
H31 H 0.6004 0.3782 -0.0030 0.064 Uiso 1 1 calc R . .
C32 C 0.49837(19) 0.4584(2) 0.1493(2) 0.0433(8) Uani 1 1 d . . .
H32 H 0.5052 0.4989 0.1942 0.052 Uiso 1 1 calc R . .
C33 C -0.3293(2) 0.4351(2) 0.4415(2) 0.0511(10) Uani 1 1 d . . .
H33 H -0.3823 0.4448 0.4691 0.061 Uiso 1 1 calc R . .
C34 C -0.2588(2) 0.3909(2) 0.3215(2) 0.0450(9) Uani 1 1 d . . .
H34 H -0.2630 0.3707 0.2672 0.054 Uiso 1 1 calc R . .
C35 C -0.3344(2) 0.4052(2) 0.3628(2) 0.0494(9) Uani 1 1 d . . .
H35 H -0.3912 0.3943 0.3368 0.059 Uiso 1 1 calc R . .
C36 C -0.2472(2) 0.4509(2) 0.4804(2) 0.0523(9) Uani 1 1 d . . .
H36 H -0.2435 0.4716 0.5346 0.063 Uiso 1 1 calc R . .
C37 C -0.1695(2) 0.4360(2) 0.4386(2) 0.0487(9) Uani 1 1 d . . .
H37 H -0.1124 0.4464 0.4641 0.058 Uiso 1 1 calc R . .
C38 C 0.5676(2) 0.4448(2) 0.0984(2) 0.0546(10) Uani 1 1 d . . .
H38 H 0.6232 0.4753 0.1082 0.065 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.944(3) . ?
Fe1 N5 1.945(3) . ?
Fe1 N1 1.970(2) . ?
Fe1 N4 1.984(2) . ?
Fe1 N3 1.988(2) . ?
Fe1 N2 1.997(2) . ?
S1 C3 1.643(3) . ?
S2 C12 1.629(3) . ?
N1 C10 1.336(3) . ?
N1 C6 1.357(3) . ?
N2 C4 1.288(3) . ?
N2 C1 1.436(3) . ?
C1 C23 1.376(4) . ?
C1 C8 1.384(4) . ?
C2 C14 1.383(4) . ?
C2 C11 1.389(4) . ?
C2 N3 1.435(3) . ?
C3 N7 1.161(3) . ?
N3 C5 1.286(3) . ?
C4 C15 1.449(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.453(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.339(4) . ?
N4 C15 1.351(4) . ?
N5 C12 1.164(3) . ?
C6 C18 1.383(4) . ?
C7 C9 1.382(4) . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.372(4) . ?
C9 N10 1.463(4) . ?
C10 C20 1.375(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.378(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.387(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.385(4) . ?
C16 C19 1.386(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.242(3) . ?
N6 C21 1.446(3) . ?
C17 C27 1.367(4) . ?
C17 C28 1.376(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.386(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.374(4) . ?
C19 N8 1.438(4) . ?
N9 N10 1.218(3) . ?
N9 C29 1.472(4) . ?
C20 C24 1.375(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.373(4) . ?
C21 C25 1.389(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.373(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.388(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.362(4) . ?
C29 C37 1.393(5) . ?
C30 H30 0.9500 . ?
C31 C38 1.371(5) . ?
C31 H31 0.9500 . ?
C32 C38 1.389(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.379(5) . ?
C33 C36 1.383(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.373(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.404(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 90.79(10) . . ?
N7 Fe1 N1 93.87(9) . . ?
N5 Fe1 N1 93.08(9) . . ?
N7 Fe1 N4 91.26(9) . . ?
N5 Fe1 N4 92.65(10) . . ?
N1 Fe1 N4 172.26(10) . . ?
N7 Fe1 N3 173.91(9) . . ?
N5 Fe1 N3 91.16(9) . . ?
N1 Fe1 N3 80.26(9) . . ?
N4 Fe1 N3 94.42(9) . . ?
N7 Fe1 N2 93.16(9) . . ?
N5 Fe1 N2 171.77(9) . . ?
N1 Fe1 N2 93.86(9) . . ?
N4 Fe1 N2 80.06(9) . . ?
N3 Fe1 N2 85.65(9) . . ?
C10 N1 C6 117.3(2) . . ?
C10 N1 Fe1 128.15(19) . . ?
C6 N1 Fe1 114.34(18) . . ?
C4 N2 C1 117.6(2) . . ?
C4 N2 Fe1 114.83(18) . . ?
C1 N2 Fe1 126.80(17) . . ?
C23 C1 C8 120.2(3) . . ?
C23 C1 N2 120.8(2) . . ?
C8 C1 N2 119.0(3) . . ?
C14 C2 C11 120.2(3) . . ?
C14 C2 N3 121.5(2) . . ?
C11 C2 N3 118.2(3) . . ?
N7 C3 S1 179.0(3) . . ?
C5 N3 C2 119.5(2) . . ?
C5 N3 Fe1 114.71(18) . . ?
C2 N3 Fe1 125.44(17) . . ?
N2 C4 C15 116.4(3) . . ?
N2 C4 H4 121.8 . . ?
C15 C4 H4 121.8 . . ?
N3 C5 C6 116.4(2) . . ?
N3 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C26 N4 C15 117.6(2) . . ?
C26 N4 Fe1 127.9(2) . . ?
C15 N4 Fe1 114.47(17) . . ?
C12 N5 Fe1 166.8(2) . . ?
N1 C6 C18 122.6(2) . . ?
N1 C6 C5 112.8(2) . . ?
C18 C6 C5 124.6(3) . . ?
C9 C7 C8 120.2(3) . . ?
C9 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C1 C8 C7 119.3(3) . . ?
C1 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C13 C9 C7 120.1(3) . . ?
C13 C9 N10 114.4(3) . . ?
C7 C9 N10 125.4(3) . . ?
N1 C10 C20 123.1(3) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.3(3) . . ?
C22 C11 H11 120.4 . . ?
C2 C11 H11 120.4 . . ?
N5 C12 S2 178.6(3) . . ?
C9 C13 C23 120.0(3) . . ?
C9 C13 H13 120.0 . . ?
C23 C13 H13 120.0 . . ?
C2 C14 C16 119.9(3) . . ?
C2 C14 H14 120.0 . . ?
C16 C14 H14 120.0 . . ?
N4 C15 C32 122.7(3) . . ?
N4 C15 C4 113.4(2) . . ?
C32 C15 C4 123.9(3) . . ?
C19 C16 C14 119.7(3) . . ?
C19 C16 H16 120.1 . . ?
C14 C16 H16 120.1 . . ?
N8 N6 C21 112.6(2) . . ?
C27 C17 C28 120.1(3) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 171.8(2) . . ?
C6 C18 C24 118.7(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 119.9(3) . . ?
C22 C19 N8 115.0(3) . . ?
C16 C19 N8 125.1(3) . . ?
N6 N8 C19 114.0(2) . . ?
N10 N9 C29 112.8(3) . . ?
N9 N10 C9 110.5(3) . . ?
C10 C20 C24 119.5(3) . . ?
C10 C20 H20 120.3 . . ?
C24 C20 H20 120.3 . . ?
C30 C21 C25 120.3(3) . . ?
C30 C21 N6 116.0(3) . . ?
C25 C21 N6 123.7(3) . . ?
C19 C22 C11 121.0(3) . . ?
C19 C22 H22 119.5 . . ?
C11 C22 H22 119.5 . . ?
C1 C23 C13 120.2(3) . . ?
C1 C23 H23 119.9 . . ?
C13 C23 H23 119.9 . . ?
C20 C24 C18 118.7(3) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C28 C25 C21 119.0(3) . . ?
C28 C25 H25 120.5 . . ?
C21 C25 H25 120.5 . . ?
N4 C26 C31 122.9(3) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 120.1(3) . . ?
C17 C27 H27 119.9 . . ?
C30 C27 H27 119.9 . . ?
C17 C28 C25 120.5(3) . . ?
C17 C28 H28 119.7 . . ?
C25 C28 H28 119.7 . . ?
C34 C29 C37 121.4(3) . . ?
C34 C29 N9 114.8(3) . . ?
C37 C29 N9 123.7(3) . . ?
C21 C30 C27 119.8(3) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.5(3) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C15 C32 C38 118.3(3) . . ?
C15 C32 H32 120.8 . . ?
C38 C32 H32 120.8 . . ?
C35 C33 C36 120.4(3) . . ?
C35 C33 H33 119.8 . . ?
C36 C33 H33 119.8 . . ?
C29 C34 C35 119.4(3) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 120.9(3) . . ?
C34 C35 H35 119.5 . . ?
C33 C35 H35 119.5 . . ?
C33 C36 C37 119.0(3) . . ?
C33 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C29 C37 C36 119.0(3) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C31 C38 C32 119.0(3) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.803
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.803
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.039
####################################################################### 
# 
# 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_feaza130kd1
_database_code_depnum_ccdc_archive 'CCDC 1492635'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
   bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0090(11)
_cell_length_b                   14.3641(11)
_cell_length_c                   16.6475(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.803(4)
_cell_angle_gamma                90.00
_cell_volume                     3584.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    5168
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
     its'aim being to analyse the evolution of partial collection of data, 
     always carried out over the same part of reciprocal space, 
     and over a large scale of temperature.
     This  explain the poor completness of data as well as the low theta(max) value, 
     the low number of unique reflexions collected.
     In ordre to obtain significant intensities with an exposure time relatively short, 
     a crystal of neutron size was used. As the aim is to compare the diffraction data 
     always obtained from the same part of the crystal at different temperature, 
     problems of intensity scale are not considered to be of prior importance.
     The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
     over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
     these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
     or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
     but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5624
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         21.28
_reflns_number_total             3376
_reflns_number_gt                2986
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0227P)²+1.9377P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3376
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0650
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29135(2) 0.28433(3) 0.06825(2) 0.02223(15) Uani 1 1 d . . .
S1 S 0.19527(4) 0.48723(5) -0.14275(4) 0.0290(2) Uani 1 1 d . . .
S2 S 0.42153(4) 0.07433(5) -0.10802(4) 0.0332(2) Uani 1 1 d . . .
N1 N 0.17755(13) 0.21984(14) 0.08013(13) 0.0212(5) Uani 1 1 d . . .
N2 N 0.27121(13) 0.37409(14) 0.15610(12) 0.0199(5) Uani 1 1 d . . .
C1 C 0.19363(15) 0.38045(17) 0.20323(18) 0.0199(7) Uani 1 1 d . . .
C2 C 0.41723(15) 0.18557(18) 0.18919(17) 0.0216(7) Uani 1 1 d . . .
C3 C 0.22311(16) 0.4168(2) -0.06809(18) 0.0229(7) Uani 1 1 d . . .
N3 N 0.32782(13) 0.19602(14) 0.15470(12) 0.0206(5) Uani 1 1 d . . .
C4 C 0.34063(17) 0.42191(18) 0.17919(16) 0.0240(7) Uani 1 1 d . . .
H4 H 0.3403 0.4620 0.2246 0.029 Uiso 1 1 calc R . .
C5 C 0.26332(16) 0.15173(18) 0.18590(15) 0.0237(7) Uani 1 1 d . . .
H5 H 0.2724 0.1133 0.2320 0.028 Uiso 1 1 calc R . .
N4 N 0.40685(13) 0.35063(15) 0.07102(13) 0.0237(5) Uani 1 1 d . . .
N5 N 0.32799(14) 0.19806(16) -0.01292(14) 0.0288(6) Uani 1 1 d . . .
C6 C 0.17566(16) 0.16431(18) 0.14596(16) 0.0224(7) Uani 1 1 d . . .
C7 C 0.03621(17) 0.40169(18) 0.20889(19) 0.0286(7) Uani 1 1 d . . .
H7 H -0.0205 0.4128 0.1829 0.034 Uiso 1 1 calc R . .
C8 C 0.11115(16) 0.39671(18) 0.16470(16) 0.0245(7) Uani 1 1 d . . .
H8 H 0.1064 0.4044 0.1080 0.029 Uiso 1 1 calc R . .
C9 C 0.04393(17) 0.39042(18) 0.29145(19) 0.0269(7) Uani 1 1 d . . .
C10 C 0.10176(17) 0.22862(19) 0.03508(16) 0.0275(7) Uani 1 1 d . . .
H10 H 0.1021 0.2655 -0.0122 0.033 Uiso 1 1 calc R . .
C11 C 0.48356(16) 0.15762(19) 0.13919(16) 0.0286(7) Uani 1 1 d . . .
H11 H 0.4691 0.1424 0.0846 0.034 Uiso 1 1 calc R . .
C12 C 0.36585(17) 0.1464(2) -0.05298(16) 0.0242(7) Uani 1 1 d . . .
C13 C 0.12624(18) 0.3756(2) 0.32967(17) 0.0338(8) Uani 1 1 d . . .
H13 H 0.1314 0.3696 0.3865 0.041 Uiso 1 1 calc R . .
C14 C 0.43795(16) 0.20761(18) 0.26886(17) 0.0255(7) Uani 1 1 d . . .
H14 H 0.3925 0.2273 0.3028 0.031 Uiso 1 1 calc R . .
C15 C 0.41897(16) 0.41146(19) 0.13261(16) 0.0242(7) Uani 1 1 d . . .
C16 C 0.52579(16) 0.20076(18) 0.29887(16) 0.0269(7) Uani 1 1 d . . .
H16 H 0.5405 0.2153 0.3536 0.032 Uiso 1 1 calc R . .
N6 N 0.69982(13) 0.15424(15) 0.34696(16) 0.0295(6) Uani 1 1 d . . .
C17 C 0.96913(17) 0.11459(19) 0.41861(19) 0.0313(7) Uani 1 1 d . . .
H17 H 1.0295 0.1029 0.4353 0.038 Uiso 1 1 calc R . .
N7 N 0.24318(13) 0.36806(16) -0.01439(14) 0.0267(6) Uani 1 1 d . . .
C18 C 0.09882(16) 0.12174(19) 0.16965(16) 0.0269(7) Uani 1 1 d . . .
H18 H 0.0995 0.0850 0.2172 0.032 Uiso 1 1 calc R . .
C19 C 0.59173(16) 0.17271(18) 0.24896(17) 0.0242(7) Uani 1 1 d . . .
N8 N 0.68468(13) 0.16269(15) 0.27273(16) 0.0280(6) Uani 1 1 d . . .
N9 N -0.10241(16) 0.39274(15) 0.30786(14) 0.0351(6) Uani 1 1 d . . .
N10 N -0.02962(16) 0.39788(16) 0.34551(14) 0.0379(6) Uani 1 1 d . . .
C20 C 0.02306(17) 0.1863(2) 0.05443(17) 0.0323(8) Uani 1 1 d . . .
H20 H -0.0292 0.1937 0.0205 0.039 Uiso 1 1 calc R . .
C21 C 0.79370(16) 0.14376(18) 0.36912(17) 0.0259(7) Uani 1 1 d . . .
C22 C 0.57079(16) 0.15204(19) 0.16946(17) 0.0286(7) Uani 1 1 d . . .
H22 H 0.6166 0.1339 0.1353 0.034 Uiso 1 1 calc R . .
C23 C 0.20070(17) 0.36948(19) 0.28537(19) 0.0292(7) Uani 1 1 d . . .
H23 H 0.2573 0.3577 0.3115 0.035 Uiso 1 1 calc R . .
C24 C 0.02090(17) 0.1334(2) 0.12309(18) 0.0327(7) Uani 1 1 d . . .
H24 H -0.0331 0.1054 0.1382 0.039 Uiso 1 1 calc R . .
C25 C 0.86077(17) 0.16285(19) 0.31663(17) 0.0316(7) Uani 1 1 d . . .
H25 H 0.8464 0.1855 0.2640 0.038 Uiso 1 1 calc R . .
C26 C 0.47397(18) 0.3401(2) 0.02175(17) 0.0348(8) Uani 1 1 d . . .
H26 H 0.4661 0.2992 -0.0229 0.042 Uiso 1 1 calc R . .
C27 C 0.90251(18) 0.0979(2) 0.47030(17) 0.0348(8) Uani 1 1 d . . .
H27 H 0.9168 0.0757 0.5231 0.042 Uiso 1 1 calc R . .
C28 C 0.94862(17) 0.1482(2) 0.34253(18) 0.0331(8) Uani 1 1 d . . .
H28 H 0.9951 0.1615 0.3076 0.040 Uiso 1 1 calc R . .
C29 C -0.17878(18) 0.40584(19) 0.3581(2) 0.0330(8) Uani 1 1 d . . .
C30 C 0.81422(17) 0.1135(2) 0.44542(17) 0.0318(7) Uani 1 1 d . . .
H30 H 0.7681 0.1030 0.4815 0.038 Uiso 1 1 calc R . .
C31 C 0.55390(18) 0.3863(2) 0.0333(2) 0.0424(8) Uani 1 1 d . . .
H31 H 0.5997 0.3774 -0.0034 0.051 Uiso 1 1 calc R . .
C32 C 0.49822(17) 0.4583(2) 0.14844(17) 0.0359(8) Uani 1 1 d . . .
H32 H 0.5051 0.4990 0.1933 0.043 Uiso 1 1 calc R . .
C33 C -0.33047(19) 0.4351(2) 0.4407(2) 0.0420(8) Uani 1 1 d . . .
H33 H -0.3833 0.4452 0.4686 0.050 Uiso 1 1 calc R . .
C34 C -0.26011(19) 0.39099(19) 0.32030(18) 0.0359(8) Uani 1 1 d . . .
H34 H -0.2644 0.3710 0.2658 0.043 Uiso 1 1 calc R . .
C35 C -0.33613(19) 0.4053(2) 0.3620(2) 0.0411(8) Uani 1 1 d . . .
H35 H -0.3930 0.3944 0.3361 0.049 Uiso 1 1 calc R . .
C36 C -0.24833(19) 0.4504(2) 0.47913(19) 0.0425(8) Uani 1 1 d . . .
H36 H -0.2445 0.4708 0.5335 0.051 Uiso 1 1 calc R . .
C37 C -0.17061(18) 0.4356(2) 0.4377(2) 0.0393(8) Uani 1 1 d . . .
H37 H -0.1135 0.4458 0.4633 0.047 Uiso 1 1 calc R . .
C38 C 0.56753(18) 0.4449(2) 0.0976(2) 0.0436(8) Uani 1 1 d . . .
H38 H 0.6231 0.4756 0.1071 0.052 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.933(2) . ?
Fe1 N7 1.940(3) . ?
Fe1 N1 1.962(2) . ?
Fe1 N3 1.976(2) . ?
Fe1 N4 1.976(2) . ?
Fe1 N2 1.984(2) . ?
S1 C3 1.641(3) . ?
S2 C12 1.639(3) . ?
N1 C10 1.337(3) . ?
N1 C6 1.357(3) . ?
N2 C4 1.291(3) . ?
N2 C1 1.438(3) . ?
C1 C23 1.376(4) . ?
C1 C8 1.386(3) . ?
C2 C14 1.384(3) . ?
C2 C11 1.388(3) . ?
C2 N3 1.441(3) . ?
C3 N7 1.163(3) . ?
N3 C5 1.289(3) . ?
C4 C15 1.448(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.456(3) . ?
C5 H5 0.9500 . ?
N4 C26 1.338(3) . ?
N4 C15 1.353(3) . ?
N5 C12 1.164(3) . ?
C6 C18 1.380(3) . ?
C7 C8 1.376(3) . ?
C7 C9 1.383(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.378(4) . ?
C9 N10 1.462(3) . ?
C10 C20 1.380(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.382(3) . ?
C11 H11 0.9500 . ?
C13 C23 1.371(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.390(3) . ?
C14 H14 0.9500 . ?
C15 C32 1.381(4) . ?
C16 C19 1.383(3) . ?
C16 H16 0.9500 . ?
N6 N8 1.251(3) . ?
N6 C21 1.447(3) . ?
C17 C27 1.372(4) . ?
C17 C28 1.376(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.381(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.378(3) . ?
C19 N8 1.439(3) . ?
N9 N10 1.235(3) . ?
N9 C29 1.464(3) . ?
C20 C24 1.374(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.364(4) . ?
C21 C25 1.392(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.376(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.387(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.363(4) . ?
C29 C37 1.391(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.369(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.377(4) . ?
C33 C36 1.379(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.400(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N5 Fe1 N7 90.60(9) . . ?
N5 Fe1 N1 92.67(9) . . ?
N7 Fe1 N1 93.90(9) . . ?
N5 Fe1 N3 91.11(9) . . ?
N7 Fe1 N3 174.22(8) . . ?
N1 Fe1 N3 80.50(8) . . ?
N5 Fe1 N4 92.64(9) . . ?
N7 Fe1 N4 90.80(8) . . ?
N1 Fe1 N4 172.87(9) . . ?
N3 Fe1 N4 94.64(8) . . ?
N5 Fe1 N2 172.20(8) . . ?
N7 Fe1 N2 93.15(9) . . ?
N1 Fe1 N2 93.89(8) . . ?
N3 Fe1 N2 85.82(8) . . ?
N4 Fe1 N2 80.49(9) . . ?
C10 N1 C6 117.2(2) . . ?
C10 N1 Fe1 128.31(19) . . ?
C6 N1 Fe1 114.31(15) . . ?
C4 N2 C1 117.8(2) . . ?
C4 N2 Fe1 114.56(17) . . ?
C1 N2 Fe1 126.86(16) . . ?
C23 C1 C8 120.2(2) . . ?
C23 C1 N2 120.7(2) . . ?
C8 C1 N2 119.1(2) . . ?
C14 C2 C11 120.4(2) . . ?
C14 C2 N3 121.3(2) . . ?
C11 C2 N3 118.2(2) . . ?
N7 C3 S1 178.9(3) . . ?
C5 N3 C2 119.4(2) . . ?
C5 N3 Fe1 115.07(17) . . ?
C2 N3 Fe1 125.20(16) . . ?
N2 C4 C15 116.8(2) . . ?
N2 C4 H4 121.6 . . ?
C15 C4 H4 121.6 . . ?
N3 C5 C6 115.8(2) . . ?
N3 C5 H5 122.1 . . ?
C6 C5 H5 122.1 . . ?
C26 N4 C15 117.4(2) . . ?
C26 N4 Fe1 128.09(19) . . ?
C15 N4 Fe1 114.47(16) . . ?
C12 N5 Fe1 166.5(2) . . ?
N1 C6 C18 122.8(2) . . ?
N1 C6 C5 112.8(2) . . ?
C18 C6 C5 124.3(3) . . ?
C8 C7 C9 119.6(2) . . ?
C8 C7 H7 120.2 . . ?
C9 C7 H7 120.2 . . ?
C7 C8 C1 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
C13 C9 C7 120.4(2) . . ?
C13 C9 N10 114.5(3) . . ?
C7 C9 N10 125.0(2) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 119.5(2) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
N5 C12 S2 178.5(2) . . ?
C23 C13 C9 119.8(3) . . ?
C23 C13 H13 120.1 . . ?
C9 C13 H13 120.1 . . ?
C2 C14 C16 119.5(2) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 122.8(2) . . ?
N4 C15 C4 113.0(2) . . ?
C32 C15 C4 124.2(3) . . ?
C19 C16 C14 119.9(2) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 112.9(2) . . ?
C27 C17 C28 120.1(3) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 172.4(2) . . ?
C6 C18 C24 118.8(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.2(2) . . ?
C22 C19 N8 114.5(2) . . ?
C16 C19 N8 125.2(2) . . ?
N6 N8 C19 114.1(2) . . ?
N10 N9 C29 113.6(2) . . ?
N9 N10 C9 111.0(2) . . ?
C24 C20 C10 119.5(2) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C30 C21 C25 120.7(2) . . ?
C30 C21 N6 116.3(2) . . ?
C25 C21 N6 123.0(2) . . ?
C19 C22 C11 120.4(2) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.1(2) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C20 C24 C18 118.7(2) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C28 C25 C21 118.8(3) . . ?
C28 C25 H25 120.6 . . ?
C21 C25 H25 120.6 . . ?
N4 C26 C31 122.5(3) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 120.0(3) . . ?
C17 C27 H27 120.0 . . ?
C30 C27 H27 120.0 . . ?
C17 C28 C25 120.5(3) . . ?
C17 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
C34 C29 C37 121.5(3) . . ?
C34 C29 N9 115.1(3) . . ?
C37 C29 N9 123.3(3) . . ?
C21 C30 C27 119.9(2) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 120.1(3) . . ?
C38 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?
C15 C32 C38 118.7(3) . . ?
C15 C32 H32 120.6 . . ?
C38 C32 H32 120.6 . . ?
C35 C33 C36 120.2(3) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.3(3) . . ?
C29 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C33 C35 C34 120.7(3) . . ?
C33 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C33 C36 C37 119.6(3) . . ?
C33 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C29 C37 C36 118.6(3) . . ?
C29 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C31 C38 C32 118.4(3) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.844
_diffrn_reflns_theta_full        21.28
_diffrn_measured_fraction_theta_full 0.844
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.033
####################################################################### 
# 
# 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_feaza160km1
_database_code_depnum_ccdc_archive 'CCDC 1492636'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
     bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0178(10)
_cell_length_b                   14.4001(10)
_cell_length_c                   16.6809(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.794(4)
_cell_angle_gamma                90.00
_cell_volume                     3603.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    4518
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5439
_exptl_absorpt_correction_T_max  0.8932
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
       its'aim being to analyse the evolution of partial collection of data, 
       always carried out over the same part of reciprocal space, 
       and over a large scale of temperature.
       This  explain the poor completness of data as well as the low theta(max) value, 
       the low number of unique reflexions collected.
       In ordre to obtain significant intensities with an exposure time relatively short, 
       a crystal of neutron size was used. As the aim is to compare the diffraction data 
       always obtained from the same part of the crystal at different temperature, 
       problems of intensity scale are not considered to be of prior importance.
       The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
       over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
       these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
       or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
       but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5688
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         21.28
_reflns_number_total             3396
_reflns_number_gt                2941
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0227P)²+2.2940P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3396
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29183(2) 0.28453(3) 0.06721(2) 0.02833(16) Uani 1 1 d . . .
S1 S 0.19504(5) 0.48764(6) -0.14276(4) 0.0369(2) Uani 1 1 d . . .
S2 S 0.42294(5) 0.07460(6) -0.10820(5) 0.0416(2) Uani 1 1 d . . .
N1 N 0.17757(14) 0.21934(15) 0.08001(14) 0.0264(6) Uani 1 1 d . . .
N2 N 0.27165(14) 0.37443(15) 0.15631(12) 0.0238(6) Uani 1 1 d . . .
C1 C 0.19406(17) 0.38079(19) 0.20325(19) 0.0246(7) Uani 1 1 d . . .
C2 C 0.41736(17) 0.18515(19) 0.18904(18) 0.0258(7) Uani 1 1 d . . .
C3 C 0.22266(17) 0.4170(2) -0.06832(19) 0.0287(7) Uani 1 1 d . . .
N3 N 0.32848(14) 0.19561(15) 0.15471(13) 0.0253(6) Uani 1 1 d . . .
C4 C 0.34097(18) 0.4217(2) 0.17951(17) 0.0286(7) Uani 1 1 d . . .
H4 H 0.3405 0.4616 0.2249 0.034 Uiso 1 1 calc R . .
C5 C 0.26363(18) 0.15180(19) 0.18545(17) 0.0277(7) Uani 1 1 d . . .
H5 H 0.2725 0.1135 0.2315 0.033 Uiso 1 1 calc R . .
N4 N 0.40791(14) 0.35177(16) 0.07146(14) 0.0291(6) Uani 1 1 d . . .
N5 N 0.32961(16) 0.19856(19) -0.01420(16) 0.0387(7) Uani 1 1 d . . .
C6 C 0.17627(17) 0.1641(2) 0.14591(17) 0.0264(7) Uani 1 1 d . . .
C7 C 0.03668(18) 0.4020(2) 0.2085(2) 0.0345(8) Uani 1 1 d . . .
H7 H -0.0200 0.4131 0.1825 0.041 Uiso 1 1 calc R . .
C8 C 0.11184(18) 0.39704(19) 0.16467(17) 0.0294(7) Uani 1 1 d . . .
H8 H 0.1073 0.4047 0.1081 0.035 Uiso 1 1 calc R . .
C9 C 0.04444(19) 0.3908(2) 0.2909(2) 0.0348(8) Uani 1 1 d . . .
C10 C 0.10205(19) 0.2280(2) 0.03543(17) 0.0333(8) Uani 1 1 d . . .
H10 H 0.1023 0.2645 -0.0120 0.040 Uiso 1 1 calc R . .
C11 C 0.48372(18) 0.1576(2) 0.13936(18) 0.0344(8) Uani 1 1 d . . .
H11 H 0.4696 0.1425 0.0848 0.041 Uiso 1 1 calc R . .
C12 C 0.36741(18) 0.1468(2) -0.05388(18) 0.0308(8) Uani 1 1 d . . .
C13 C 0.1260(2) 0.3757(2) 0.32923(19) 0.0422(9) Uani 1 1 d . . .
H13 H 0.1309 0.3693 0.3860 0.051 Uiso 1 1 calc R . .
C14 C 0.43779(18) 0.2069(2) 0.26866(18) 0.0312(8) Uani 1 1 d . . .
H14 H 0.3922 0.2261 0.3025 0.037 Uiso 1 1 calc R . .
C15 C 0.41958(17) 0.4116(2) 0.13346(18) 0.0302(7) Uani 1 1 d . . .
C16 C 0.52568(18) 0.2004(2) 0.29885(18) 0.0333(8) Uani 1 1 d . . .
H16 H 0.5403 0.2149 0.3535 0.040 Uiso 1 1 calc R . .
N6 N 0.69932(15) 0.15429(17) 0.34645(18) 0.0370(7) Uani 1 1 d . . .
C17 C 0.96848(19) 0.1150(2) 0.4186(2) 0.0382(8) Uani 1 1 d . . .
H17 H 1.0288 0.1032 0.4355 0.046 Uiso 1 1 calc R . .
N7 N 0.24270(15) 0.36839(18) -0.01493(16) 0.0353(6) Uani 1 1 d . . .
C18 C 0.09938(18) 0.1220(2) 0.16966(18) 0.0345(8) Uani 1 1 d . . .
H18 H 0.1001 0.0854 0.2171 0.041 Uiso 1 1 calc R . .
C19 C 0.59147(18) 0.1727(2) 0.24908(18) 0.0291(8) Uani 1 1 d . . .
N8 N 0.68466(15) 0.16285(16) 0.27258(17) 0.0350(6) Uani 1 1 d . . .
N9 N -0.1004(2) 0.39309(17) 0.30809(16) 0.0462(7) Uani 1 1 d . . .
N10 N -0.02945(19) 0.39837(18) 0.34651(17) 0.0499(8) Uani 1 1 d . . .
C20 C 0.0236(2) 0.1862(2) 0.0551(2) 0.0414(9) Uani 1 1 d . . .
H20 H -0.0288 0.1938 0.0214 0.050 Uiso 1 1 calc R . .
C21 C 0.79349(17) 0.1438(2) 0.36847(19) 0.0318(8) Uani 1 1 d . . .
C22 C 0.57067(18) 0.1524(2) 0.17006(19) 0.0355(8) Uani 1 1 d . . .
H22 H 0.6166 0.1346 0.1360 0.043 Uiso 1 1 calc R . .
C23 C 0.20061(19) 0.3697(2) 0.2853(2) 0.0367(8) Uani 1 1 d . . .
H23 H 0.2570 0.3580 0.3116 0.044 Uiso 1 1 calc R . .
C24 C 0.02121(19) 0.1337(2) 0.1236(2) 0.0404(8) Uani 1 1 d . . .
H24 H -0.0328 0.1061 0.1390 0.048 Uiso 1 1 calc R . .
C25 C 0.86073(19) 0.1628(2) 0.31632(19) 0.0399(8) Uani 1 1 d . . .
H25 H 0.8467 0.1851 0.2636 0.048 Uiso 1 1 calc R . .
C26 C 0.4751(2) 0.3416(2) 0.02257(19) 0.0440(9) Uani 1 1 d . . .
H26 H 0.4675 0.3011 -0.0222 0.053 Uiso 1 1 calc R . .
C27 C 0.9020(2) 0.0986(2) 0.46984(19) 0.0433(9) Uani 1 1 d . . .
H27 H 0.9161 0.0767 0.5227 0.052 Uiso 1 1 calc R . .
C28 C 0.9484(2) 0.1485(2) 0.3428(2) 0.0416(9) Uani 1 1 d . . .
H28 H 0.9951 0.1619 0.3082 0.050 Uiso 1 1 calc R . .
C29 C -0.1778(2) 0.4057(2) 0.3595(2) 0.0440(9) Uani 1 1 d . . .
C30 C 0.81392(19) 0.1138(2) 0.44473(19) 0.0387(8) Uani 1 1 d . . .
H30 H 0.7677 0.1034 0.4806 0.046 Uiso 1 1 calc R . .
C31 C 0.5547(2) 0.3874(3) 0.0347(2) 0.0550(10) Uani 1 1 d . . .
H31 H 0.6007 0.3790 -0.0017 0.066 Uiso 1 1 calc R . .
C32 C 0.49856(19) 0.4583(2) 0.1497(2) 0.0447(9) Uani 1 1 d . . .
H32 H 0.5053 0.4986 0.1946 0.054 Uiso 1 1 calc R . .
C33 C -0.3288(2) 0.4352(2) 0.4419(2) 0.0520(10) Uani 1 1 d . . .
H33 H -0.3820 0.4448 0.4694 0.062 Uiso 1 1 calc R . .
C34 C -0.2582(2) 0.3910(2) 0.3221(2) 0.0490(9) Uani 1 1 d . . .
H34 H -0.2625 0.3712 0.2677 0.059 Uiso 1 1 calc R . .
C35 C -0.3335(2) 0.4051(2) 0.3637(3) 0.0521(10) Uani 1 1 d . . .
H35 H -0.3902 0.3938 0.3378 0.062 Uiso 1 1 calc R . .
C36 C -0.2472(2) 0.4513(2) 0.4805(2) 0.0535(10) Uani 1 1 d . . .
H36 H -0.2436 0.4725 0.5345 0.064 Uiso 1 1 calc R . .
C37 C -0.1691(2) 0.4359(2) 0.4388(2) 0.0515(10) Uani 1 1 d . . .
H37 H -0.1119 0.4460 0.4641 0.062 Uiso 1 1 calc R . .
C38 C 0.5678(2) 0.4452(3) 0.0991(2) 0.0551(10) Uani 1 1 d . . .
H38 H 0.6233 0.4758 0.1090 0.066 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.943(3) . ?
Fe1 N7 1.945(3) . ?
Fe1 N1 1.977(2) . ?
Fe1 N4 1.992(2) . ?
Fe1 N3 1.999(2) . ?
Fe1 N2 2.005(2) . ?
S1 C3 1.643(4) . ?
S2 C12 1.635(4) . ?
N1 C10 1.331(3) . ?
N1 C6 1.358(3) . ?
N2 C4 1.288(3) . ?
N2 C1 1.438(3) . ?
C1 C23 1.377(4) . ?
C1 C8 1.384(4) . ?
C2 C14 1.384(4) . ?
C2 C11 1.385(4) . ?
C2 N3 1.435(3) . ?
C3 N7 1.161(3) . ?
N3 C5 1.288(3) . ?
C4 C15 1.447(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.450(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.337(3) . ?
N4 C15 1.351(3) . ?
N5 C12 1.163(3) . ?
C6 C18 1.379(4) . ?
C7 C8 1.377(4) . ?
C7 C9 1.383(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.372(4) . ?
C9 N10 1.485(4) . ?
C10 C20 1.377(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.381(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.370(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.393(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.379(4) . ?
C16 C19 1.380(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.247(3) . ?
N6 C21 1.452(3) . ?
C17 C27 1.367(4) . ?
C17 C28 1.374(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.382(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.371(4) . ?
C19 N8 1.442(3) . ?
N9 N10 1.219(3) . ?
N9 C29 1.489(4) . ?
C20 C24 1.371(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.364(4) . ?
C21 C25 1.392(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.372(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.385(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.349(5) . ?
C29 C37 1.392(5) . ?
C30 H30 0.9500 . ?
C31 C38 1.366(5) . ?
C31 H31 0.9500 . ?
C32 C38 1.383(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.374(4) . ?
C33 C36 1.375(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.371(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.411(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N5 Fe1 N7 90.97(10) . . ?
N5 Fe1 N1 93.30(10) . . ?
N7 Fe1 N1 93.99(10) . . ?
N5 Fe1 N4 92.85(10) . . ?
N7 Fe1 N4 91.41(9) . . ?
N1 Fe1 N4 171.75(10) . . ?
N5 Fe1 N3 91.31(10) . . ?
N7 Fe1 N3 173.69(9) . . ?
N1 Fe1 N3 80.01(9) . . ?
N4 Fe1 N3 94.36(9) . . ?
N5 Fe1 N2 171.66(9) . . ?
N7 Fe1 N2 93.18(9) . . ?
N1 Fe1 N2 93.62(9) . . ?
N4 Fe1 N2 79.83(10) . . ?
N3 Fe1 N2 85.32(9) . . ?
C10 N1 C6 117.5(2) . . ?
C10 N1 Fe1 128.0(2) . . ?
C6 N1 Fe1 114.37(17) . . ?
C4 N2 C1 117.9(2) . . ?
C4 N2 Fe1 114.52(18) . . ?
C1 N2 Fe1 126.90(18) . . ?
C23 C1 C8 120.0(3) . . ?
C23 C1 N2 120.9(2) . . ?
C8 C1 N2 119.1(3) . . ?
C14 C2 C11 120.4(2) . . ?
C14 C2 N3 121.2(2) . . ?
C11 C2 N3 118.3(3) . . ?
N7 C3 S1 178.8(3) . . ?
C5 N3 C2 119.8(2) . . ?
C5 N3 Fe1 114.71(18) . . ?
C2 N3 Fe1 125.22(18) . . ?
N2 C4 C15 117.1(3) . . ?
N2 C4 H4 121.4 . . ?
C15 C4 H4 121.4 . . ?
N3 C5 C6 116.4(3) . . ?
N3 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C26 N4 C15 117.6(2) . . ?
C26 N4 Fe1 127.6(2) . . ?
C15 N4 Fe1 114.70(17) . . ?
C12 N5 Fe1 166.8(2) . . ?
N1 C6 C18 122.4(2) . . ?
N1 C6 C5 113.0(2) . . ?
C18 C6 C5 124.6(3) . . ?
C8 C7 C9 119.4(3) . . ?
C8 C7 H7 120.3 . . ?
C9 C7 H7 120.3 . . ?
C7 C8 C1 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
C13 C9 C7 120.8(3) . . ?
C13 C9 N10 113.5(3) . . ?
C7 C9 N10 125.6(3) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 119.3(3) . . ?
C22 C11 H11 120.4 . . ?
C2 C11 H11 120.4 . . ?
N5 C12 S2 178.5(3) . . ?
C23 C13 C9 119.7(3) . . ?
C23 C13 H13 120.1 . . ?
C9 C13 H13 120.1 . . ?
C2 C14 C16 119.6(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 122.6(3) . . ?
N4 C15 C4 113.1(2) . . ?
C32 C15 C4 124.3(3) . . ?
C19 C16 C14 119.7(3) . . ?
C19 C16 H16 120.1 . . ?
C14 C16 H16 120.1 . . ?
N8 N6 C21 112.5(2) . . ?
C27 C17 C28 120.2(3) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 172.0(2) . . ?
C6 C18 C24 119.1(3) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C22 C19 C16 120.2(3) . . ?
C22 C19 N8 114.4(3) . . ?
C16 C19 N8 125.4(3) . . ?
N6 N8 C19 113.6(2) . . ?
N10 N9 C29 112.1(3) . . ?
N9 N10 C9 109.1(3) . . ?
C24 C20 C10 119.8(3) . . ?
C24 C20 H20 120.1 . . ?
C10 C20 H20 120.1 . . ?
C30 C21 C25 120.5(3) . . ?
C30 C21 N6 116.2(3) . . ?
C25 C21 N6 123.3(3) . . ?
C19 C22 C11 120.8(3) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C13 C23 C1 120.2(3) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C20 C24 C18 118.4(3) . . ?
C20 C24 H24 120.8 . . ?
C18 C24 H24 120.8 . . ?
C28 C25 C21 118.7(3) . . ?
C28 C25 H25 120.7 . . ?
C21 C25 H25 120.7 . . ?
N4 C26 C31 122.4(3) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 120.0(3) . . ?
C17 C27 H27 120.0 . . ?
C30 C27 H27 120.0 . . ?
C17 C28 C25 120.6(3) . . ?
C17 C28 H28 119.7 . . ?
C25 C28 H28 119.7 . . ?
C34 C29 C37 122.0(3) . . ?
C34 C29 N9 114.8(3) . . ?
C37 C29 N9 123.1(3) . . ?
C21 C30 C27 120.0(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 120.0(3) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C15 C32 C38 118.7(3) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C35 C33 C36 120.0(3) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.0(3) . . ?
C29 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C34 C35 C33 121.5(3) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 119.1(3) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C29 C37 C36 118.4(3) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 118.6(3) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.845
_diffrn_reflns_theta_full        21.27
_diffrn_measured_fraction_theta_full 0.845
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.035
####################################################################### 
# 
# 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_feaza185kd2
_database_code_depnum_ccdc_archive 'CCDC 1492637'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
      bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0534(8)
_cell_length_b                   14.4184(10)
_cell_length_c                   16.7682(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.865(4)
_cell_angle_gamma                90.00
_cell_volume                     3634.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    5813
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5465
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
            its'aim being to analyse the evolution of partial collection of data, 
            always carried out over the same part of reciprocal space, 
            and over a large scale of temperature.
            This  explain the poor completness of data as well as the low theta(max) value, 
            the low number of unique reflexions collected.
            In ordre to obtain significant intensities with an exposure time relatively short, 
            a crystal of neutron size was used. As the aim is to compare the diffraction data 
            always obtained from the same part of the crystal at different temperature, 
            problems of intensity scale are not considered to be of prior importance.
            The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
            over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
            these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
            or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
            but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5705
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         22.97
_reflns_number_total             4090
_reflns_number_gt                3346
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0242P)²+2.9116P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4090
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29191(3) 0.28539(3) 0.06385(3) 0.03857(17) Uani 1 1 d . . .
S1 S 0.19365(5) 0.49088(6) -0.14394(5) 0.0499(3) Uani 1 1 d . . .
S2 S 0.42752(6) 0.07431(6) -0.10811(6) 0.0540(3) Uani 1 1 d . . .
N1 N 0.17634(16) 0.21817(15) 0.08003(15) 0.0360(6) Uani 1 1 d . . .
N2 N 0.27219(15) 0.37638(15) 0.15734(14) 0.0302(6) Uani 1 1 d . . .
C1 C 0.19528(19) 0.38252(18) 0.20425(18) 0.0314(7) Uani 1 1 d . . .
C2 C 0.41692(19) 0.18426(19) 0.18931(19) 0.0338(8) Uani 1 1 d . . .
C3 C 0.2204(2) 0.4196(2) -0.0704(2) 0.0410(8) Uani 1 1 d . . .
N3 N 0.32849(16) 0.19413(16) 0.15456(14) 0.0325(6) Uani 1 1 d . . .
C4 C 0.3418(2) 0.42128(19) 0.18139(19) 0.0355(8) Uani 1 1 d . . .
H4 H 0.3420 0.4592 0.2277 0.043 Uiso 1 1 calc R . .
C5 C 0.2635(2) 0.15214(19) 0.18490(18) 0.0346(8) Uani 1 1 d . . .
H5 H 0.2721 0.1147 0.2312 0.042 Uiso 1 1 calc R . .
N4 N 0.40985(15) 0.35442(17) 0.07206(16) 0.0387(6) Uani 1 1 d . . .
N5 N 0.33374(19) 0.1995(2) -0.01825(19) 0.0548(8) Uani 1 1 d . . .
C6 C 0.1759(2) 0.16398(19) 0.14574(18) 0.0334(8) Uani 1 1 d . . .
C7 C 0.0382(2) 0.4027(2) 0.2095(2) 0.0450(9) Uani 1 1 d . . .
H7 H -0.0184 0.4135 0.1836 0.054 Uiso 1 1 calc R . .
C8 C 0.11343(19) 0.39818(19) 0.1652(2) 0.0379(8) Uani 1 1 d . . .
H8 H 0.1089 0.4057 0.1088 0.045 Uiso 1 1 calc R . .
C9 C 0.0455(2) 0.3915(2) 0.2914(2) 0.0458(9) Uani 1 1 d . . .
C10 C 0.0998(2) 0.2270(2) 0.0367(2) 0.0453(9) Uani 1 1 d . . .
H10 H 0.0996 0.2629 -0.0108 0.054 Uiso 1 1 calc R . .
C11 C 0.4839(2) 0.1579(2) 0.1402(2) 0.0439(8) Uani 1 1 d . . .
H11 H 0.4701 0.1432 0.0858 0.053 Uiso 1 1 calc R . .
C12 C 0.3717(2) 0.1474(2) -0.0559(2) 0.0413(8) Uani 1 1 d . . .
C13 C 0.1269(2) 0.3767(2) 0.3293(2) 0.0535(9) Uani 1 1 d . . .
H13 H 0.1316 0.3702 0.3857 0.064 Uiso 1 1 calc R . .
C14 C 0.4372(2) 0.2053(2) 0.2686(2) 0.0414(8) Uani 1 1 d . . .
H14 H 0.3916 0.2238 0.3023 0.050 Uiso 1 1 calc R . .
C15 C 0.42059(19) 0.4121(2) 0.1352(2) 0.0373(8) Uani 1 1 d . . .
C16 C 0.5246(2) 0.1993(2) 0.2985(2) 0.0436(8) Uani 1 1 d . . .
H16 H 0.5390 0.2140 0.3528 0.052 Uiso 1 1 calc R . .
N6 N 0.69823(17) 0.15380(18) 0.34565(19) 0.0481(7) Uani 1 1 d . . .
C17 C 0.9675(2) 0.1162(2) 0.4181(2) 0.0478(9) Uani 1 1 d . . .
H17 H 1.0276 0.1049 0.4354 0.057 Uiso 1 1 calc R . .
N7 N 0.23911(19) 0.3706(2) -0.01769(19) 0.0534(8) Uani 1 1 d . . .
C18 C 0.0997(2) 0.1229(2) 0.1713(2) 0.0447(9) Uani 1 1 d . . .
H18 H 0.1014 0.0867 0.2186 0.054 Uiso 1 1 calc R . .
C19 C 0.5904(2) 0.1721(2) 0.2494(2) 0.0395(8) Uani 1 1 d . . .
N8 N 0.68451(18) 0.16315(17) 0.27306(19) 0.0459(7) Uani 1 1 d . . .
N9 N -0.0948(3) 0.39376(19) 0.3104(2) 0.0625(9) Uani 1 1 d . . .
N10 N -0.0286(2) 0.39989(19) 0.3496(2) 0.0677(10) Uani 1 1 d . . .
C20 C 0.0217(2) 0.1869(2) 0.0573(2) 0.0560(10) Uani 1 1 d . . .
H20 H -0.0310 0.1945 0.0243 0.067 Uiso 1 1 calc R . .
C21 C 0.79284(19) 0.1436(2) 0.3677(2) 0.0409(8) Uani 1 1 d . . .
C22 C 0.5704(2) 0.1530(2) 0.1705(2) 0.0456(9) Uani 1 1 d . . .
H22 H 0.6164 0.1362 0.1366 0.055 Uiso 1 1 calc R . .
C23 C 0.2015(2) 0.3711(2) 0.2861(2) 0.0455(8) Uani 1 1 d . . .
H23 H 0.2577 0.3595 0.3125 0.055 Uiso 1 1 calc R . .
C24 C 0.0206(2) 0.1353(2) 0.1265(2) 0.0545(10) Uani 1 1 d . . .
H24 H -0.0333 0.1089 0.1432 0.065 Uiso 1 1 calc R . .
C25 C 0.8600(2) 0.1629(2) 0.3162(2) 0.0517(9) Uani 1 1 d . . .
H25 H 0.8461 0.1851 0.2637 0.062 Uiso 1 1 calc R . .
C26 C 0.4781(2) 0.3455(3) 0.0243(2) 0.0578(10) Uani 1 1 d . . .
H26 H 0.4710 0.3060 -0.0209 0.069 Uiso 1 1 calc R . .
C27 C 0.9008(2) 0.0994(2) 0.4683(2) 0.0565(10) Uani 1 1 d . . .
H27 H 0.9148 0.0779 0.5210 0.068 Uiso 1 1 calc R . .
C28 C 0.9479(2) 0.1492(2) 0.3429(2) 0.0526(9) Uani 1 1 d . . .
H28 H 0.9946 0.1629 0.3087 0.063 Uiso 1 1 calc R . .
C29 C -0.1731(3) 0.4068(2) 0.3639(3) 0.0622(12) Uani 1 1 d . . .
C30 C 0.8126(2) 0.1135(2) 0.4432(2) 0.0527(9) Uani 1 1 d . . .
H30 H 0.7664 0.1022 0.4786 0.063 Uiso 1 1 calc R . .
C31 C 0.5571(3) 0.3901(3) 0.0375(3) 0.0742(12) Uani 1 1 d . . .
H31 H 0.6033 0.3826 0.0014 0.089 Uiso 1 1 calc R . .
C32 C 0.4993(2) 0.4583(2) 0.1536(2) 0.0590(10) Uani 1 1 d . . .
H32 H 0.5055 0.4972 0.1992 0.071 Uiso 1 1 calc R . .
C33 C -0.3239(3) 0.4361(3) 0.4457(3) 0.0659(11) Uani 1 1 d . . .
H33 H -0.3772 0.4456 0.4727 0.079 Uiso 1 1 calc R . .
C34 C -0.2529(3) 0.3903(2) 0.3273(3) 0.0683(12) Uani 1 1 d . . .
H34 H -0.2570 0.3689 0.2736 0.082 Uiso 1 1 calc R . .
C35 C -0.3280(3) 0.4045(2) 0.3679(3) 0.0665(11) Uani 1 1 d . . .
H35 H -0.3844 0.3923 0.3420 0.080 Uiso 1 1 calc R . .
C36 C -0.2430(3) 0.4538(3) 0.4841(3) 0.0705(12) Uani 1 1 d . . .
H36 H -0.2397 0.4760 0.5376 0.085 Uiso 1 1 calc R . .
C37 C -0.1646(2) 0.4384(3) 0.4427(3) 0.0692(12) Uani 1 1 d . . .
H37 H -0.1076 0.4493 0.4679 0.083 Uiso 1 1 calc R . .
C38 C 0.5693(2) 0.4462(3) 0.1034(3) 0.0753(13) Uani 1 1 d . . .
H38 H 0.6248 0.4762 0.1146 0.090 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.975(3) . ?
Fe1 N5 1.978(3) . ?
Fe1 N1 2.022(3) . ?
Fe1 N4 2.034(2) . ?
Fe1 N3 2.065(2) . ?
Fe1 N2 2.077(2) . ?
S1 C3 1.639(4) . ?
S2 C12 1.630(4) . ?
N1 C10 1.337(4) . ?
N1 C6 1.351(4) . ?
N2 C4 1.280(3) . ?
N2 C1 1.435(3) . ?
C1 C23 1.380(4) . ?
C1 C8 1.385(4) . ?
C2 C14 1.383(4) . ?
C2 C11 1.387(4) . ?
C2 N3 1.433(4) . ?
C3 N7 1.156(4) . ?
N3 C5 1.277(3) . ?
C4 C15 1.454(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.454(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.340(4) . ?
N4 C15 1.350(4) . ?
N5 C12 1.151(4) . ?
C6 C18 1.378(4) . ?
C7 C9 1.382(5) . ?
C7 C8 1.388(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.368(5) . ?
C9 N10 1.522(4) . ?
C10 C20 1.370(5) . ?
C10 H10 0.9500 . ?
C11 C22 1.375(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.370(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.380(4) . ?
C16 C19 1.378(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.232(4) . ?
N6 C21 1.461(4) . ?
C17 C27 1.364(5) . ?
C17 C28 1.366(5) . ?
C17 H17 0.9500 . ?
C18 C24 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.370(4) . ?
C19 N8 1.457(4) . ?
N9 N10 1.170(4) . ?
N9 C29 1.528(5) . ?
C20 C24 1.379(5) . ?
C20 H20 0.9500 . ?
C21 C30 1.358(5) . ?
C21 C25 1.390(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.390(5) . ?
C25 H25 0.9500 . ?
C26 C31 1.360(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.387(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.342(6) . ?
C29 C37 1.398(6) . ?
C30 H30 0.9500 . ?
C31 C38 1.375(6) . ?
C31 H31 0.9500 . ?
C32 C38 1.393(5) . ?
C32 H32 0.9500 . ?
C33 C36 1.373(5) . ?
C33 C35 1.381(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.364(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.417(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 92.23(12) . . ?
N7 Fe1 N1 94.12(11) . . ?
N5 Fe1 N1 95.69(11) . . ?
N7 Fe1 N4 93.57(11) . . ?
N5 Fe1 N4 92.66(11) . . ?
N1 Fe1 N4 168.41(10) . . ?
N7 Fe1 N3 171.64(11) . . ?
N5 Fe1 N3 91.78(10) . . ?
N1 Fe1 N3 78.18(10) . . ?
N4 Fe1 N3 93.57(10) . . ?
N7 Fe1 N2 93.55(10) . . ?
N5 Fe1 N2 169.54(10) . . ?
N1 Fe1 N2 92.59(9) . . ?
N4 Fe1 N2 78.29(10) . . ?
N3 Fe1 N2 83.65(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 127.2(2) . . ?
C6 N1 Fe1 115.2(2) . . ?
C4 N2 C1 117.8(3) . . ?
C4 N2 Fe1 114.31(19) . . ?
C1 N2 Fe1 127.06(18) . . ?
C23 C1 C8 120.3(3) . . ?
C23 C1 N2 121.4(3) . . ?
C8 C1 N2 118.3(3) . . ?
C14 C2 C11 119.9(3) . . ?
C14 C2 N3 121.7(3) . . ?
C11 C2 N3 118.3(3) . . ?
N7 C3 S1 178.9(3) . . ?
C5 N3 C2 120.3(3) . . ?
C5 N3 Fe1 114.47(19) . . ?
C2 N3 Fe1 124.80(19) . . ?
N2 C4 C15 117.6(3) . . ?
N2 C4 H4 121.2 . . ?
C15 C4 H4 121.2 . . ?
N3 C5 C6 117.4(3) . . ?
N3 C5 H5 121.3 . . ?
C6 C5 H5 121.3 . . ?
C26 N4 C15 117.6(3) . . ?
C26 N4 Fe1 127.2(2) . . ?
C15 N4 Fe1 115.11(19) . . ?
C12 N5 Fe1 166.9(3) . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 113.3(3) . . ?
C18 C6 C5 124.0(3) . . ?
C9 C7 C8 120.1(3) . . ?
C9 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C1 C8 C7 119.0(3) . . ?
C1 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C13 C9 C7 120.3(3) . . ?
C13 C9 N10 112.5(3) . . ?
C7 C9 N10 127.1(3) . . ?
N1 C10 C20 123.3(3) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
C22 C11 C2 119.9(3) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
N5 C12 S2 178.7(3) . . ?
C9 C13 C23 120.2(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C2 C14 C16 119.6(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 122.7(3) . . ?
N4 C15 C4 113.9(3) . . ?
C32 C15 C4 123.4(3) . . ?
C19 C16 C14 120.0(3) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 112.0(3) . . ?
C27 C17 C28 120.0(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 169.8(3) . . ?
C6 C18 C24 118.8(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.2(3) . . ?
C22 C19 N8 114.2(3) . . ?
C16 C19 N8 125.6(3) . . ?
N6 N8 C19 113.0(3) . . ?
N10 N9 C29 108.8(4) . . ?
N9 N10 C9 105.4(4) . . ?
C10 C20 C24 119.1(3) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C30 C21 C25 120.8(3) . . ?
C30 C21 N6 115.7(3) . . ?
C25 C21 N6 123.6(3) . . ?
C19 C22 C11 120.4(3) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.2(3) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C20 C24 C18 118.6(3) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C28 C25 C21 118.8(3) . . ?
C28 C25 H25 120.6 . . ?
C21 C25 H25 120.6 . . ?
N4 C26 C31 123.2(4) . . ?
N4 C26 H26 118.4 . . ?
C31 C26 H26 118.4 . . ?
C17 C27 C30 120.6(4) . . ?
C17 C27 H27 119.7 . . ?
C30 C27 H27 119.7 . . ?
C17 C28 C25 120.3(3) . . ?
C17 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
C34 C29 C37 121.8(3) . . ?
C34 C29 N9 114.1(4) . . ?
C37 C29 N9 123.9(4) . . ?
C21 C30 C27 119.4(3) . . ?
C21 C30 H30 120.3 . . ?
C27 C30 H30 120.3 . . ?
C26 C31 C38 119.3(4) . . ?
C26 C31 H31 120.3 . . ?
C38 C31 H31 120.3 . . ?
C15 C32 C38 118.2(4) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C36 C33 C35 120.1(4) . . ?
C36 C33 H33 119.9 . . ?
C35 C33 H33 119.9 . . ?
C29 C34 C35 119.4(4) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 121.5(4) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.8(4) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C29 C37 C36 118.4(4) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 119.0(3) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.811
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.811
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.039
####################################################################### 
# 
# 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_feaza205kd2
_database_code_depnum_ccdc_archive 'CCDC 1492638'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
      bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0800(7)
_cell_length_b                   14.4253(9)
_cell_length_c                   16.8673(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.994(3)
_cell_angle_gamma                90.00
_cell_volume                     3664.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    205(2)
_cell_measurement_reflns_used    4242
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      21.261

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5488
_exptl_absorpt_correction_T_max  0.8948
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
           its'aim being to analyse the evolution of partial collection of data, 
           always carried out over the same part of reciprocal space, 
           and over a large scale of temperature.
           This  explain the poor completness of data as well as the low theta(max) value, 
           the low number of unique reflexions collected.
           In ordre to obtain significant intensities with an exposure time relatively short, 
           a crystal of neutron size was used. As the aim is to compare the diffraction data 
           always obtained from the same part of the crystal at different temperature, 
           problems of intensity scale are not considered to be of prior importance.
           The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
           over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
           these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
           or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
           but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      205(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5359
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         21.25
_reflns_number_total             3732
_reflns_number_gt                3074
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0224P)²+2.5135P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3732
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29134(3) 0.28643(3) 0.05991(3) 0.04438(18) Uani 1 1 d . . .
S1 S 0.19163(5) 0.49507(7) -0.14566(6) 0.0576(3) Uani 1 1 d . . .
S2 S 0.43242(6) 0.07356(6) -0.10747(6) 0.0611(3) Uani 1 1 d . . .
N1 N 0.17378(17) 0.21703(16) 0.07967(16) 0.0416(7) Uani 1 1 d . . .
N2 N 0.27252(16) 0.37825(15) 0.15879(14) 0.0335(6) Uani 1 1 d . . .
C1 C 0.19618(19) 0.38395(19) 0.20522(19) 0.0351(8) Uani 1 1 d . . .
C2 C 0.4155(2) 0.18267(19) 0.1901(2) 0.0383(8) Uani 1 1 d . . .
C3 C 0.2168(2) 0.4232(2) -0.0730(2) 0.0488(9) Uani 1 1 d . . .
N3 N 0.32810(17) 0.19250(16) 0.15445(15) 0.0371(6) Uani 1 1 d . . .
C4 C 0.3430(2) 0.4210(2) 0.18328(19) 0.0405(8) Uani 1 1 d . . .
H4 H 0.3440 0.4573 0.2296 0.049 Uiso 1 1 calc R . .
C5 C 0.2626(2) 0.1521(2) 0.18465(19) 0.0401(8) Uani 1 1 d . . .
H5 H 0.2708 0.1156 0.2306 0.048 Uiso 1 1 calc R . .
N4 N 0.41160(15) 0.35759(18) 0.07289(16) 0.0452(7) Uani 1 1 d . . .
N5 N 0.3374(2) 0.2008(2) -0.0226(2) 0.0646(9) Uani 1 1 d . . .
C6 C 0.1747(2) 0.1643(2) 0.14572(19) 0.0383(8) Uani 1 1 d . . .
C7 C 0.0394(2) 0.4032(2) 0.2109(2) 0.0514(9) Uani 1 1 d . . .
H7 H -0.0168 0.4133 0.1857 0.062 Uiso 1 1 calc R . .
C8 C 0.1144(2) 0.3990(2) 0.1671(2) 0.0428(8) Uani 1 1 d . . .
H8 H 0.1095 0.4065 0.1116 0.051 Uiso 1 1 calc R . .
C9 C 0.0482(2) 0.3921(2) 0.2920(3) 0.0563(11) Uani 1 1 d . . .
C10 C 0.0968(3) 0.2262(2) 0.0375(2) 0.0529(9) Uani 1 1 d . . .
H10 H 0.0958 0.2610 -0.0096 0.063 Uiso 1 1 calc R . .
C11 C 0.4828(2) 0.1579(2) 0.1415(2) 0.0497(9) Uani 1 1 d . . .
H11 H 0.4696 0.1443 0.0877 0.060 Uiso 1 1 calc R . .
C12 C 0.3766(2) 0.1479(2) -0.0585(2) 0.0482(9) Uani 1 1 d . . .
C13 C 0.1290(3) 0.3768(2) 0.3299(2) 0.0613(10) Uani 1 1 d . . .
H13 H 0.1338 0.3695 0.3853 0.074 Uiso 1 1 calc R . .
C14 C 0.4357(2) 0.2032(2) 0.2689(2) 0.0479(9) Uani 1 1 d . . .
H14 H 0.3905 0.2211 0.3021 0.057 Uiso 1 1 calc R . .
C15 C 0.42166(19) 0.4121(2) 0.1374(2) 0.0424(8) Uani 1 1 d . . .
C16 C 0.5230(2) 0.1974(2) 0.2991(2) 0.0528(9) Uani 1 1 d . . .
H16 H 0.5369 0.2111 0.3528 0.063 Uiso 1 1 calc R . .
N6 N 0.69620(19) 0.15355(19) 0.3450(2) 0.0587(8) Uani 1 1 d . . .
C17 C 0.9656(2) 0.1168(2) 0.4182(3) 0.0540(10) Uani 1 1 d . . .
H17 H 1.0248 0.1060 0.4358 0.065 Uiso 1 1 calc R . .
N7 N 0.2341(2) 0.3731(2) -0.0207(2) 0.0637(9) Uani 1 1 d . . .
C18 C 0.0991(2) 0.1240(2) 0.1726(2) 0.0517(9) Uani 1 1 d . . .
H18 H 0.1015 0.0888 0.2196 0.062 Uiso 1 1 calc R . .
C19 C 0.5891(2) 0.1716(2) 0.2505(2) 0.0471(9) Uani 1 1 d . . .
N8 N 0.68438(19) 0.16307(18) 0.2739(2) 0.0562(8) Uani 1 1 d . . .
N9 N -0.0892(3) 0.39480(19) 0.3123(2) 0.0725(10) Uani 1 1 d . . .
N10 N -0.0271(3) 0.4009(2) 0.3530(2) 0.0848(12) Uani 1 1 d . . .
C20 C 0.0189(3) 0.1869(2) 0.0603(3) 0.0648(11) Uani 1 1 d . . .
H20 H -0.0340 0.1946 0.0290 0.078 Uiso 1 1 calc R . .
C21 C 0.7922(2) 0.1434(2) 0.3670(2) 0.0493(9) Uani 1 1 d . . .
C22 C 0.5692(2) 0.1530(2) 0.1721(2) 0.0532(9) Uani 1 1 d . . .
H22 H 0.6148 0.1368 0.1388 0.064 Uiso 1 1 calc R . .
C23 C 0.2024(2) 0.3723(2) 0.2866(2) 0.0512(9) Uani 1 1 d . . .
H23 H 0.2581 0.3611 0.3124 0.061 Uiso 1 1 calc R . .
C24 C 0.0193(2) 0.1363(2) 0.1291(3) 0.0627(10) Uani 1 1 d . . .
H24 H -0.0335 0.1105 0.1465 0.075 Uiso 1 1 calc R . .
C25 C 0.8591(2) 0.1627(2) 0.3163(2) 0.0613(10) Uani 1 1 d . . .
H25 H 0.8454 0.1844 0.2646 0.074 Uiso 1 1 calc R . .
C26 C 0.4800(2) 0.3501(3) 0.0267(2) 0.0685(11) Uani 1 1 d . . .
H26 H 0.4733 0.3130 -0.0190 0.082 Uiso 1 1 calc R . .
C27 C 0.8991(2) 0.0999(2) 0.4673(2) 0.0641(10) Uani 1 1 d . . .
H27 H 0.9127 0.0784 0.5191 0.077 Uiso 1 1 calc R . .
C28 C 0.9469(2) 0.1494(2) 0.3434(3) 0.0612(10) Uani 1 1 d . . .
H28 H 0.9933 0.1630 0.3102 0.073 Uiso 1 1 calc R . .
C29 C -0.1689(3) 0.4078(3) 0.3682(3) 0.0759(14) Uani 1 1 d . . .
C30 C 0.8121(2) 0.1137(2) 0.4421(3) 0.0640(10) Uani 1 1 d . . .
H30 H 0.7665 0.1026 0.4768 0.077 Uiso 1 1 calc R . .
C31 C 0.5592(3) 0.3936(3) 0.0423(4) 0.0929(15) Uani 1 1 d . . .
H31 H 0.6055 0.3869 0.0075 0.111 Uiso 1 1 calc R . .
C32 C 0.5003(2) 0.4573(2) 0.1583(3) 0.0691(11) Uani 1 1 d . . .
H32 H 0.5061 0.4938 0.2044 0.083 Uiso 1 1 calc R . .
C33 C -0.3191(3) 0.4367(3) 0.4483(3) 0.0715(12) Uani 1 1 d . . .
H33 H -0.3719 0.4460 0.4743 0.086 Uiso 1 1 calc R . .
C34 C -0.2480(3) 0.3901(3) 0.3324(3) 0.0789(13) Uani 1 1 d . . .
H34 H -0.2519 0.3682 0.2798 0.095 Uiso 1 1 calc R . .
C35 C -0.3226(3) 0.4035(3) 0.3719(3) 0.0724(12) Uani 1 1 d . . .
H35 H -0.3781 0.3899 0.3465 0.087 Uiso 1 1 calc R . .
C36 C -0.2387(3) 0.4562(3) 0.4870(3) 0.0792(12) Uani 1 1 d . . .
H36 H -0.2357 0.4790 0.5392 0.095 Uiso 1 1 calc R . .
C37 C -0.1604(2) 0.4408(3) 0.4456(3) 0.0799(14) Uani 1 1 d . . .
H37 H -0.1041 0.4526 0.4700 0.096 Uiso 1 1 calc R . .
C38 C 0.5708(3) 0.4470(3) 0.1088(4) 0.0913(15) Uani 1 1 d . . .
H38 H 0.6255 0.4764 0.1211 0.110 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 2.008(4) . ?
Fe1 N5 2.012(4) . ?
Fe1 N1 2.078(3) . ?
Fe1 N4 2.085(3) . ?
Fe1 N3 2.143(2) . ?
Fe1 N2 2.160(2) . ?
S1 C3 1.634(4) . ?
S2 C12 1.616(4) . ?
N1 C10 1.335(4) . ?
N1 C6 1.348(4) . ?
N2 C4 1.279(3) . ?
N2 C1 1.428(4) . ?
C1 C8 1.379(4) . ?
C1 C23 1.382(4) . ?
C2 C14 1.381(4) . ?
C2 C11 1.384(4) . ?
C2 N3 1.427(4) . ?
C3 N7 1.161(4) . ?
N3 C5 1.275(4) . ?
C4 C15 1.456(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.459(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.328(4) . ?
N4 C15 1.345(4) . ?
N5 C12 1.156(4) . ?
C6 C18 1.379(4) . ?
C7 C9 1.376(5) . ?
C7 C8 1.385(4) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.364(5) . ?
C9 N10 1.577(5) . ?
C10 C20 1.377(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.377(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.359(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.389(4) . ?
C14 H14 0.9400 . ?
C15 C32 1.383(4) . ?
C16 C19 1.373(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.211(4) . ?
N6 C21 1.483(4) . ?
C17 C27 1.356(5) . ?
C17 C28 1.361(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.388(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.367(4) . ?
C19 N8 1.476(4) . ?
N9 N10 1.135(4) . ?
N9 C29 1.577(5) . ?
C20 C24 1.371(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.356(5) . ?
C21 C25 1.384(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.392(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.364(5) . ?
C26 H26 0.9400 . ?
C27 C30 1.372(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.334(6) . ?
C29 C37 1.389(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.365(6) . ?
C31 H31 0.9400 . ?
C32 C38 1.393(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.373(5) . ?
C33 C36 1.375(5) . ?
C33 H33 0.9400 . ?
C34 C35 1.351(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.420(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N7 Fe1 N5 93.76(12) . . ?
N7 Fe1 N1 93.90(11) . . ?
N5 Fe1 N1 98.22(11) . . ?
N7 Fe1 N4 96.07(11) . . ?
N5 Fe1 N4 92.61(11) . . ?
N1 Fe1 N4 164.76(11) . . ?
N7 Fe1 N3 169.23(11) . . ?
N5 Fe1 N3 92.38(11) . . ?
N1 Fe1 N3 76.45(10) . . ?
N4 Fe1 N3 92.49(10) . . ?
N7 Fe1 N2 94.11(10) . . ?
N5 Fe1 N2 167.14(10) . . ?
N1 Fe1 N2 91.38(9) . . ?
N4 Fe1 N2 76.45(10) . . ?
N3 Fe1 N2 81.52(9) . . ?
C10 N1 C6 117.8(3) . . ?
C10 N1 Fe1 126.3(2) . . ?
C6 N1 Fe1 115.6(2) . . ?
C4 N2 C1 118.4(3) . . ?
C4 N2 Fe1 113.89(19) . . ?
C1 N2 Fe1 126.93(19) . . ?
C8 C1 C23 119.7(3) . . ?
C8 C1 N2 118.7(3) . . ?
C23 C1 N2 121.6(3) . . ?
C14 C2 C11 119.6(3) . . ?
C14 C2 N3 122.5(3) . . ?
C11 C2 N3 117.8(3) . . ?
N7 C3 S1 178.9(3) . . ?
C5 N3 C2 120.3(3) . . ?
C5 N3 Fe1 114.2(2) . . ?
C2 N3 Fe1 125.0(2) . . ?
N2 C4 C15 118.2(3) . . ?
N2 C4 H4 120.9 . . ?
C15 C4 H4 120.9 . . ?
N3 C5 C6 118.0(3) . . ?
N3 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C26 N4 C15 117.6(3) . . ?
C26 N4 Fe1 126.6(3) . . ?
C15 N4 Fe1 115.70(19) . . ?
C12 N5 Fe1 166.5(3) . . ?
N1 C6 C18 122.5(3) . . ?
N1 C6 C5 114.2(3) . . ?
C18 C6 C5 123.3(3) . . ?
C9 C7 C8 119.1(3) . . ?
C9 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C1 C8 C7 119.5(3) . . ?
C1 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C13 C9 C7 121.4(3) . . ?
C13 C9 N10 111.3(4) . . ?
C7 C9 N10 127.1(3) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 120.0(3) . . ?
C22 C11 H11 120.0 . . ?
C2 C11 H11 120.0 . . ?
N5 C12 S2 179.1(3) . . ?
C23 C13 C9 119.3(4) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C2 C14 C16 119.8(3) . . ?
C2 C14 H14 120.1 . . ?
C16 C14 H14 120.1 . . ?
N4 C15 C32 122.8(3) . . ?
N4 C15 C4 114.9(3) . . ?
C32 C15 C4 122.3(3) . . ?
C19 C16 C14 120.0(3) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 110.5(3) . . ?
C27 C17 C28 120.3(3) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 167.0(3) . . ?
C6 C18 C24 118.8(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.1(3) . . ?
C22 C19 N8 113.8(3) . . ?
C16 C19 N8 126.1(3) . . ?
N6 N8 C19 111.4(3) . . ?
N10 N9 C29 105.0(4) . . ?
N9 N10 C9 101.4(4) . . ?
C24 C20 C10 119.3(3) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C30 C21 C25 120.5(3) . . ?
C30 C21 N6 115.5(3) . . ?
C25 C21 N6 124.0(4) . . ?
C19 C22 C11 120.5(3) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.9(3) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 118.8(3) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.7(4) . . ?
C21 C25 H25 120.6 . . ?
C28 C25 H25 120.6 . . ?
N4 C26 C31 123.3(4) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C17 C27 C30 120.7(4) . . ?
C17 C27 H27 119.7 . . ?
C30 C27 H27 119.7 . . ?
C17 C28 C25 119.9(3) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C34 C29 C37 121.9(4) . . ?
C34 C29 N9 113.5(5) . . ?
C37 C29 N9 124.5(5) . . ?
C21 C30 C27 119.7(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C26 C31 C38 119.4(4) . . ?
C26 C31 H31 120.3 . . ?
C38 C31 H31 120.3 . . ?
C15 C32 C38 117.9(4) . . ?
C15 C32 H32 121.0 . . ?
C38 C32 H32 121.0 . . ?
C35 C33 C36 120.5(4) . . ?
C35 C33 H33 119.8 . . ?
C36 C33 H33 119.8 . . ?
C29 C34 C35 119.8(5) . . ?
C29 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C33 121.4(4) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.0(4) . . ?
C33 C36 H36 121.0 . . ?
C37 C36 H36 121.0 . . ?
C29 C37 C36 118.5(4) . . ?
C29 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C31 C38 C32 118.9(4) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.916
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza210kd1
_database_code_depnum_ccdc_archive 'CCDC 1492639'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0821(11)
_cell_length_b                   14.4302(11)
_cell_length_c                   16.8916(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.026(4)
_cell_angle_gamma                90.00
_cell_volume                     3671.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    4292
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5494
_exptl_absorpt_correction_T_max  0.8950
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
  its'aim being to analyse the evolution of partial collection of data, 
  always carried out over the same part of reciprocal space, 
  and over a large scale of temperature.
  This  explain the poor completness of data as well as the low theta(max) value, 
  the low number of unique reflexions collected.
  In ordre to obtain significant intensities with an exposure time relatively short, 
  a crystal of neutron size was used. As the aim is to compare the diffraction data 
  always obtained from the same part of the crystal at different temperature, 
  problems of intensity scale are not considered to be of prior importance.
  The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
  over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
  these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
  or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
  but modelling this two conformations is over the scope 
 of this study of partial data collections.
;

_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5776
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         21.24
_reflns_number_total             3449
_reflns_number_gt                2824
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0312P)²+2.3938P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3449
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29115(3) 0.28659(3) 0.05906(3) 0.0457(2) Uani 1 1 d . . .
S1 S 0.19117(6) 0.49592(8) -0.14596(6) 0.0589(3) Uani 1 1 d . . .
S2 S 0.43346(6) 0.07338(7) -0.10719(6) 0.0632(3) Uani 1 1 d . . .
N1 N 0.17318(17) 0.21693(19) 0.07923(17) 0.0426(7) Uani 1 1 d . . .
N2 N 0.27293(16) 0.37864(18) 0.15916(14) 0.0354(7) Uani 1 1 d . . .
C1 C 0.19651(19) 0.3841(2) 0.2060(2) 0.0359(8) Uani 1 1 d . . .
C2 C 0.4154(2) 0.1823(2) 0.1902(2) 0.0397(9) Uani 1 1 d . . .
C3 C 0.2157(2) 0.4241(3) -0.0740(2) 0.0497(10) Uani 1 1 d . . .
N3 N 0.32780(17) 0.19209(18) 0.15446(15) 0.0376(7) Uani 1 1 d . . .
C4 C 0.3435(2) 0.4209(2) 0.1835(2) 0.0421(9) Uani 1 1 d . . .
H4 H 0.3445 0.4567 0.2300 0.051 Uiso 1 1 calc R . .
C5 C 0.2620(2) 0.1521(2) 0.18455(19) 0.0409(9) Uani 1 1 d . . .
H5 H 0.2699 0.1159 0.2306 0.049 Uiso 1 1 calc R . .
N4 N 0.41233(17) 0.3585(2) 0.07353(18) 0.0478(8) Uani 1 1 d . . .
N5 N 0.3381(2) 0.2010(2) -0.0233(2) 0.0666(10) Uani 1 1 d . . .
C6 C 0.1742(2) 0.1643(2) 0.1454(2) 0.0405(9) Uani 1 1 d . . .
C7 C 0.0396(2) 0.4031(2) 0.2106(3) 0.0522(10) Uani 1 1 d . . .
H7 H -0.0164 0.4131 0.1849 0.063 Uiso 1 1 calc R . .
C8 C 0.1148(2) 0.3990(2) 0.1680(2) 0.0436(9) Uani 1 1 d . . .
H8 H 0.1104 0.4065 0.1126 0.052 Uiso 1 1 calc R . .
C9 C 0.0484(3) 0.3922(2) 0.2915(3) 0.0588(12) Uani 1 1 d . . .
C10 C 0.0958(3) 0.2261(3) 0.0381(2) 0.0562(10) Uani 1 1 d . . .
H10 H 0.0942 0.2611 -0.0089 0.067 Uiso 1 1 calc R . .
C11 C 0.4833(2) 0.1580(3) 0.1422(2) 0.0513(10) Uani 1 1 d . . .
H11 H 0.4704 0.1448 0.0883 0.062 Uiso 1 1 calc R . .
C12 C 0.3774(2) 0.1481(3) -0.0588(2) 0.0480(10) Uani 1 1 d . . .
C13 C 0.1291(3) 0.3771(3) 0.3300(2) 0.0633(11) Uani 1 1 d . . .
H13 H 0.1337 0.3701 0.3853 0.076 Uiso 1 1 calc R . .
C14 C 0.4344(2) 0.2027(2) 0.2691(2) 0.0482(10) Uani 1 1 d . . .
H14 H 0.3890 0.2201 0.3021 0.058 Uiso 1 1 calc R . .
C15 C 0.4222(2) 0.4126(2) 0.1381(2) 0.0440(9) Uani 1 1 d . . .
C16 C 0.5223(2) 0.1971(3) 0.2992(2) 0.0547(10) Uani 1 1 d . . .
H16 H 0.5361 0.2108 0.3529 0.066 Uiso 1 1 calc R . .
N6 N 0.6965(2) 0.1534(2) 0.3450(2) 0.0629(9) Uani 1 1 d . . .
C17 C 0.9653(2) 0.1170(3) 0.4183(3) 0.0578(11) Uani 1 1 d . . .
H17 H 1.0245 0.1065 0.4364 0.069 Uiso 1 1 calc R . .
N7 N 0.2329(2) 0.3737(2) -0.0216(2) 0.0638(9) Uani 1 1 d . . .
C18 C 0.0988(2) 0.1241(3) 0.1724(2) 0.0535(10) Uani 1 1 d . . .
H18 H 0.1016 0.0890 0.2194 0.064 Uiso 1 1 calc R . .
C19 C 0.5890(2) 0.1717(2) 0.2510(2) 0.0505(10) Uani 1 1 d . . .
N8 N 0.6843(2) 0.1629(2) 0.2739(2) 0.0600(9) Uani 1 1 d . . .
N9 N -0.0884(3) 0.3949(2) 0.3127(2) 0.0755(11) Uani 1 1 d . . .
N10 N -0.0265(3) 0.4010(2) 0.3539(2) 0.0881(13) Uani 1 1 d . . .
C20 C 0.0176(3) 0.1864(3) 0.0615(3) 0.0687(12) Uani 1 1 d . . .
H20 H -0.0356 0.1941 0.0307 0.082 Uiso 1 1 calc R . .
C21 C 0.7922(2) 0.1434(2) 0.3672(3) 0.0535(10) Uani 1 1 d . . .
C22 C 0.5692(2) 0.1532(3) 0.1728(2) 0.0558(10) Uani 1 1 d . . .
H22 H 0.6149 0.1369 0.1396 0.067 Uiso 1 1 calc R . .
C23 C 0.2028(2) 0.3724(3) 0.2871(2) 0.0524(10) Uani 1 1 d . . .
H23 H 0.2584 0.3610 0.3130 0.063 Uiso 1 1 calc R . .
C24 C 0.0191(2) 0.1360(3) 0.1297(3) 0.0651(11) Uani 1 1 d . . .
H24 H -0.0334 0.1098 0.1474 0.078 Uiso 1 1 calc R . .
C25 C 0.8593(3) 0.1627(3) 0.3161(2) 0.0635(11) Uani 1 1 d . . .
H25 H 0.8455 0.1845 0.2645 0.076 Uiso 1 1 calc R . .
C26 C 0.4810(3) 0.3511(3) 0.0275(2) 0.0727(12) Uani 1 1 d . . .
H26 H 0.4748 0.3146 -0.0186 0.087 Uiso 1 1 calc R . .
C27 C 0.8985(3) 0.1000(3) 0.4669(2) 0.0665(11) Uani 1 1 d . . .
H27 H 0.9118 0.0787 0.5188 0.080 Uiso 1 1 calc R . .
C28 C 0.9472(2) 0.1492(3) 0.3431(3) 0.0645(11) Uani 1 1 d . . .
H28 H 0.9937 0.1622 0.3099 0.077 Uiso 1 1 calc R . .
C29 C -0.1680(3) 0.4082(3) 0.3696(4) 0.0806(15) Uani 1 1 d . . .
C30 C 0.8121(2) 0.1134(3) 0.4415(3) 0.0650(11) Uani 1 1 d . . .
H30 H 0.7663 0.1016 0.4758 0.078 Uiso 1 1 calc R . .
C31 C 0.5604(3) 0.3950(4) 0.0448(4) 0.0963(17) Uani 1 1 d . . .
H31 H 0.6073 0.3887 0.0107 0.116 Uiso 1 1 calc R . .
C32 C 0.5007(2) 0.4567(3) 0.1591(3) 0.0701(12) Uani 1 1 d . . .
H32 H 0.5061 0.4926 0.2056 0.084 Uiso 1 1 calc R . .
C33 C -0.3184(3) 0.4373(3) 0.4493(3) 0.0746(13) Uani 1 1 d . . .
H33 H -0.3712 0.4465 0.4755 0.089 Uiso 1 1 calc R . .
C34 C -0.2475(3) 0.3899(3) 0.3332(3) 0.0808(14) Uani 1 1 d . . .
H34 H -0.2513 0.3675 0.2809 0.097 Uiso 1 1 calc R . .
C35 C -0.3217(3) 0.4041(3) 0.3730(3) 0.0757(13) Uani 1 1 d . . .
H35 H -0.3773 0.3908 0.3477 0.091 Uiso 1 1 calc R . .
C36 C -0.2382(3) 0.4569(3) 0.4871(3) 0.0802(13) Uani 1 1 d . . .
H36 H -0.2354 0.4803 0.5391 0.096 Uiso 1 1 calc R . .
C37 C -0.1599(3) 0.4417(3) 0.4472(3) 0.0807(14) Uani 1 1 d . . .
H37 H -0.1038 0.4537 0.4721 0.097 Uiso 1 1 calc R . .
C38 C 0.5712(3) 0.4477(4) 0.1115(4) 0.0947(16) Uani 1 1 d . . .
H38 H 0.6256 0.4772 0.1246 0.114 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.016(4) . ?
Fe1 N7 2.020(4) . ?
Fe1 N1 2.087(3) . ?
Fe1 N4 2.104(3) . ?
Fe1 N3 2.160(3) . ?
Fe1 N2 2.179(3) . ?
S1 C3 1.626(5) . ?
S2 C12 1.617(5) . ?
N1 C10 1.333(4) . ?
N1 C6 1.351(4) . ?
N2 C4 1.275(4) . ?
N2 C1 1.435(4) . ?
C1 C8 1.376(4) . ?
C1 C23 1.378(4) . ?
C2 C14 1.380(4) . ?
C2 C11 1.385(4) . ?
C2 N3 1.430(4) . ?
C3 N7 1.164(4) . ?
N3 C5 1.277(4) . ?
C4 C15 1.452(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.459(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.332(4) . ?
N4 C15 1.343(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.375(4) . ?
C7 C9 1.376(5) . ?
C7 C8 1.376(4) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.367(5) . ?
C9 N10 1.590(5) . ?
C10 C20 1.387(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.372(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.359(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.397(4) . ?
C14 H14 0.9400 . ?
C15 C32 1.375(5) . ?
C16 C19 1.377(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.213(4) . ?
N6 C21 1.480(4) . ?
C17 C27 1.355(5) . ?
C17 C28 1.367(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.380(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.365(5) . ?
C19 N8 1.475(4) . ?
N9 N10 1.137(4) . ?
N9 C29 1.590(5) . ?
C20 C24 1.362(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.346(5) . ?
C21 C25 1.391(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.393(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.374(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.364(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.344(6) . ?
C29 C37 1.396(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.361(6) . ?
C31 H31 0.9400 . ?
C32 C38 1.372(6) . ?
C32 H32 0.9400 . ?
C33 C36 1.367(5) . ?
C33 C35 1.373(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.352(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.408(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 94.13(13) . . ?
N5 Fe1 N1 98.66(12) . . ?
N7 Fe1 N1 93.76(12) . . ?
N5 Fe1 N4 92.74(13) . . ?
N7 Fe1 N4 96.65(12) . . ?
N1 Fe1 N4 163.95(12) . . ?
N5 Fe1 N3 92.44(12) . . ?
N7 Fe1 N3 168.72(11) . . ?
N1 Fe1 N3 76.17(10) . . ?
N4 Fe1 N3 92.18(10) . . ?
N5 Fe1 N2 166.42(11) . . ?
N7 Fe1 N2 94.34(11) . . ?
N1 Fe1 N2 91.35(10) . . ?
N4 Fe1 N2 75.75(11) . . ?
N3 Fe1 N2 81.01(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 126.7(3) . . ?
C6 N1 Fe1 115.7(2) . . ?
C4 N2 C1 118.5(3) . . ?
C4 N2 Fe1 113.8(2) . . ?
C1 N2 Fe1 126.8(2) . . ?
C8 C1 C23 119.8(3) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.8(3) . . ?
C14 C2 C11 119.8(3) . . ?
C14 C2 N3 121.8(3) . . ?
C11 C2 N3 118.2(3) . . ?
N7 C3 S1 178.9(4) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 114.1(2) . . ?
C2 N3 Fe1 124.9(2) . . ?
N2 C4 C15 118.8(3) . . ?
N2 C4 H4 120.6 . . ?
C15 C4 H4 120.6 . . ?
N3 C5 C6 118.1(3) . . ?
N3 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C26 N4 C15 117.7(3) . . ?
C26 N4 Fe1 126.2(3) . . ?
C15 N4 Fe1 116.0(2) . . ?
C12 N5 Fe1 166.5(3) . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 114.4(3) . . ?
C18 C6 C5 123.0(3) . . ?
C9 C7 C8 118.4(3) . . ?
C9 C7 H7 120.8 . . ?
C8 C7 H7 120.8 . . ?
C1 C8 C7 120.3(3) . . ?
C1 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C13 C9 C7 121.8(3) . . ?
C13 C9 N10 110.1(4) . . ?
C7 C9 N10 127.9(4) . . ?
N1 C10 C20 123.0(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 120.3(3) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
N5 C12 S2 179.0(4) . . ?
C23 C13 C9 119.2(4) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C2 C14 C16 119.0(3) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
N4 C15 C32 122.4(3) . . ?
N4 C15 C4 114.7(3) . . ?
C32 C15 C4 122.9(4) . . ?
C19 C16 C14 120.6(3) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N8 N6 C21 110.8(3) . . ?
C27 C17 C28 120.4(4) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 166.6(3) . . ?
C6 C18 C24 119.1(4) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C22 C19 C16 119.7(3) . . ?
C22 C19 N8 113.4(3) . . ?
C16 C19 N8 126.8(4) . . ?
N6 N8 C19 111.4(3) . . ?
N10 N9 C29 104.0(4) . . ?
N9 N10 C9 100.2(4) . . ?
C24 C20 C10 119.1(3) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.6(3) . . ?
C30 C21 N6 115.6(4) . . ?
C25 C21 N6 123.7(4) . . ?
C19 C22 C11 120.6(3) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.5(3) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C20 C24 C18 118.9(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.7(4) . . ?
C21 C25 H25 120.7 . . ?
C28 C25 H25 120.7 . . ?
N4 C26 C31 122.3(4) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 120.8(4) . . ?
C17 C27 H27 119.6 . . ?
C30 C27 H27 119.6 . . ?
C17 C28 C25 119.4(4) . . ?
C17 C28 H28 120.3 . . ?
C25 C28 H28 120.3 . . ?
C34 C29 C37 122.0(4) . . ?
C34 C29 N9 112.5(5) . . ?
C37 C29 N9 125.3(5) . . ?
C21 C30 C27 120.0(4) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 119.9(4) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C38 C32 C15 119.2(4) . . ?
C38 C32 H32 120.4 . . ?
C15 C32 H32 120.4 . . ?
C36 C33 C35 119.9(4) . . ?
C36 C33 H33 120.1 . . ?
C35 C33 H33 120.1 . . ?
C29 C34 C35 119.0(5) . . ?
C29 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C34 C35 C33 121.9(5) . . ?
C34 C35 H35 119.0 . . ?
C33 C35 H35 119.0 . . ?
C33 C36 C37 119.2(4) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C29 C37 C36 118.0(4) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
C31 C38 C32 118.4(4) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.845
_diffrn_reflns_theta_full        21.24
_diffrn_measured_fraction_theta_full 0.846
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.035
####################################################################### 
# 
# 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_feaza170kd1
_database_code_depnum_ccdc_archive 'CCDC 1492640'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0294(11)
_cell_length_b                   14.4106(11)
_cell_length_c                   16.7098(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.796(4)
_cell_angle_gamma                90.00
_cell_volume                     3614.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    5105
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5449
_exptl_absorpt_correction_T_max  0.8935
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
   its'aim being to analyse the evolution of partial collection of data, 
   always carried out over the same part of reciprocal space, 
   and over a large scale of temperature.
   This  explain the poor completness of data as well as the low theta(max) value, 
   the low number of unique reflexions collected.
   In ordre to obtain significant intensities with an exposure time relatively short, 
   a crystal of neutron size was used. As the aim is to compare the diffraction data 
   always obtained from the same part of the crystal at different temperature, 
   problems of intensity scale are not considered to be of prior importance.
   The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
   over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
   these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
   or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
   but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5700
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         21.25
_reflns_number_total             3408
_reflns_number_gt                2929
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0292P)²+2.0854P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3408
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0743
_refine_ls_wR_factor_gt          0.0700
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29196(3) 0.28480(3) 0.06617(2) 0.03237(18) Uani 1 1 d . . .
S1 S 0.19461(5) 0.48845(6) -0.14299(5) 0.0419(3) Uani 1 1 d . . .
S2 S 0.42434(5) 0.07448(6) -0.10821(5) 0.0465(3) Uani 1 1 d . . .
N1 N 0.17740(14) 0.21895(16) 0.07986(14) 0.0294(6) Uani 1 1 d . . .
N2 N 0.27190(14) 0.37511(16) 0.15660(13) 0.0263(6) Uani 1 1 d . . .
C1 C 0.19451(17) 0.38137(19) 0.20362(19) 0.0271(7) Uani 1 1 d . . .
C2 C 0.41737(18) 0.1850(2) 0.18927(19) 0.0288(8) Uani 1 1 d . . .
C3 C 0.22194(18) 0.4176(2) -0.0688(2) 0.0331(8) Uani 1 1 d . . .
N3 N 0.32853(14) 0.19529(16) 0.15450(13) 0.0278(6) Uani 1 1 d . . .
C4 C 0.34130(19) 0.4215(2) 0.17995(17) 0.0315(7) Uani 1 1 d . . .
H4 H 0.3412 0.4608 0.2256 0.038 Uiso 1 1 calc R . .
C5 C 0.26381(19) 0.1521(2) 0.18542(17) 0.0318(8) Uani 1 1 d . . .
H5 H 0.2727 0.1142 0.2317 0.038 Uiso 1 1 calc R . .
N4 N 0.40862(14) 0.35215(17) 0.07152(15) 0.0329(6) Uani 1 1 d . . .
N5 N 0.33101(17) 0.19891(19) -0.01526(17) 0.0441(7) Uani 1 1 d . . .
C6 C 0.17600(18) 0.1643(2) 0.14569(18) 0.0298(7) Uani 1 1 d . . .
C7 C 0.03707(19) 0.4022(2) 0.2089(2) 0.0389(9) Uani 1 1 d . . .
H7 H -0.0196 0.4130 0.1828 0.047 Uiso 1 1 calc R . .
C8 C 0.11245(19) 0.3972(2) 0.16501(18) 0.0328(8) Uani 1 1 d . . .
H8 H 0.1080 0.4047 0.1085 0.039 Uiso 1 1 calc R . .
C9 C 0.0450(2) 0.3912(2) 0.2910(2) 0.0395(9) Uani 1 1 d . . .
C10 C 0.1016(2) 0.2281(2) 0.03561(18) 0.0384(8) Uani 1 1 d . . .
H10 H 0.1017 0.2647 -0.0117 0.046 Uiso 1 1 calc R . .
C11 C 0.48378(19) 0.1578(2) 0.13956(18) 0.0379(8) Uani 1 1 d . . .
H11 H 0.4697 0.1431 0.0850 0.045 Uiso 1 1 calc R . .
C12 C 0.3687(2) 0.1471(2) -0.05477(19) 0.0349(8) Uani 1 1 d . . .
C13 C 0.1265(2) 0.3760(2) 0.3293(2) 0.0464(9) Uani 1 1 d . . .
H13 H 0.1312 0.3696 0.3859 0.056 Uiso 1 1 calc R . .
C14 C 0.43740(19) 0.2064(2) 0.26860(19) 0.0338(8) Uani 1 1 d . . .
H14 H 0.3918 0.2252 0.3024 0.041 Uiso 1 1 calc R . .
C15 C 0.41995(17) 0.4115(2) 0.13361(19) 0.0325(8) Uani 1 1 d . . .
C16 C 0.52530(19) 0.2000(2) 0.29846(18) 0.0363(8) Uani 1 1 d . . .
H16 H 0.5397 0.2147 0.3530 0.044 Uiso 1 1 calc R . .
N6 N 0.69908(15) 0.15419(17) 0.34640(18) 0.0405(7) Uani 1 1 d . . .
C17 C 0.9678(2) 0.1154(2) 0.4186(2) 0.0417(9) Uani 1 1 d . . .
H17 H 1.0280 0.1038 0.4357 0.050 Uiso 1 1 calc R . .
N7 N 0.24176(16) 0.3690(2) -0.01557(17) 0.0423(7) Uani 1 1 d . . .
C18 C 0.09955(19) 0.1220(2) 0.17014(18) 0.0382(8) Uani 1 1 d . . .
H18 H 0.1007 0.0854 0.2174 0.046 Uiso 1 1 calc R . .
C19 C 0.59162(18) 0.1724(2) 0.2493(2) 0.0340(8) Uani 1 1 d . . .
N8 N 0.68488(16) 0.16292(17) 0.27279(18) 0.0390(7) Uani 1 1 d . . .
N9 N -0.0986(2) 0.39346(18) 0.30887(17) 0.0523(8) Uani 1 1 d . . .
N10 N -0.0290(2) 0.39891(19) 0.34758(18) 0.0577(8) Uani 1 1 d . . .
C20 C 0.0231(2) 0.1864(2) 0.0558(2) 0.0464(9) Uani 1 1 d . . .
H20 H -0.0294 0.1939 0.0223 0.056 Uiso 1 1 calc R . .
C21 C 0.79323(18) 0.1437(2) 0.3685(2) 0.0359(8) Uani 1 1 d . . .
C22 C 0.57088(19) 0.1523(2) 0.1702(2) 0.0390(8) Uani 1 1 d . . .
H22 H 0.6168 0.1345 0.1362 0.047 Uiso 1 1 calc R . .
C23 C 0.2009(2) 0.3701(2) 0.2856(2) 0.0390(8) Uani 1 1 d . . .
H23 H 0.2572 0.3582 0.3119 0.047 Uiso 1 1 calc R . .
C24 C 0.0212(2) 0.1342(2) 0.1244(2) 0.0458(9) Uani 1 1 d . . .
H24 H -0.0328 0.1070 0.1401 0.055 Uiso 1 1 calc R . .
C25 C 0.8605(2) 0.1627(2) 0.3165(2) 0.0448(9) Uani 1 1 d . . .
H25 H 0.8463 0.1846 0.2638 0.054 Uiso 1 1 calc R . .
C26 C 0.4760(2) 0.3429(2) 0.0231(2) 0.0501(9) Uani 1 1 d . . .
H26 H 0.4684 0.3031 -0.0220 0.060 Uiso 1 1 calc R . .
C27 C 0.9012(2) 0.0987(2) 0.4693(2) 0.0480(9) Uani 1 1 d . . .
H27 H 0.9152 0.0768 0.5221 0.058 Uiso 1 1 calc R . .
C28 C 0.9482(2) 0.1490(2) 0.3428(2) 0.0461(9) Uani 1 1 d . . .
H28 H 0.9950 0.1628 0.3084 0.055 Uiso 1 1 calc R . .
C29 C -0.1769(2) 0.4058(2) 0.3609(3) 0.0510(10) Uani 1 1 d . . .
C30 C 0.8138(2) 0.1135(2) 0.4443(2) 0.0436(9) Uani 1 1 d . . .
H30 H 0.7677 0.1026 0.4800 0.052 Uiso 1 1 calc R . .
C31 C 0.5553(2) 0.3880(3) 0.0354(3) 0.0621(11) Uani 1 1 d . . .
H31 H 0.6014 0.3795 -0.0008 0.075 Uiso 1 1 calc R . .
C32 C 0.4989(2) 0.4585(2) 0.1511(2) 0.0494(9) Uani 1 1 d . . .
H32 H 0.5055 0.4982 0.1964 0.059 Uiso 1 1 calc R . .
C33 C -0.3273(2) 0.4357(3) 0.4433(3) 0.0566(10) Uani 1 1 d . . .
H33 H -0.3805 0.4455 0.4705 0.068 Uiso 1 1 calc R . .
C34 C -0.2564(2) 0.3906(2) 0.3238(2) 0.0568(10) Uani 1 1 d . . .
H34 H -0.2607 0.3702 0.2697 0.068 Uiso 1 1 calc R . .
C35 C -0.3316(2) 0.4051(2) 0.3655(3) 0.0568(10) Uani 1 1 d . . .
H35 H -0.3883 0.3936 0.3397 0.068 Uiso 1 1 calc R . .
C36 C -0.2460(2) 0.4521(3) 0.4819(2) 0.0598(10) Uani 1 1 d . . .
H36 H -0.2425 0.4733 0.5357 0.072 Uiso 1 1 calc R . .
C37 C -0.1676(2) 0.4368(2) 0.4401(3) 0.0576(11) Uani 1 1 d . . .
H37 H -0.1104 0.4474 0.4652 0.069 Uiso 1 1 calc R . .
C38 C 0.5681(2) 0.4456(3) 0.1002(3) 0.0637(11) Uani 1 1 d . . .
H38 H 0.6235 0.4763 0.1102 0.076 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.951(3) . ?
Fe1 N5 1.951(3) . ?
Fe1 N1 1.989(2) . ?
Fe1 N4 2.002(2) . ?
Fe1 N3 2.016(2) . ?
Fe1 N2 2.028(2) . ?
S1 C3 1.643(4) . ?
S2 C12 1.633(4) . ?
N1 C10 1.334(4) . ?
N1 C6 1.354(3) . ?
N2 C4 1.284(3) . ?
N2 C1 1.438(3) . ?
C1 C23 1.378(4) . ?
C1 C8 1.383(4) . ?
C2 C14 1.380(4) . ?
C2 C11 1.386(4) . ?
C2 N3 1.438(3) . ?
C3 N7 1.160(4) . ?
N3 C5 1.284(3) . ?
C4 C15 1.452(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.459(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.333(4) . ?
N4 C15 1.349(4) . ?
N5 C12 1.162(4) . ?
C6 C18 1.380(4) . ?
C7 C8 1.381(4) . ?
C7 C9 1.381(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.372(4) . ?
C9 N10 1.500(4) . ?
C10 C20 1.379(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.384(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.368(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.392(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.385(4) . ?
C16 C19 1.381(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.244(3) . ?
N6 C21 1.453(4) . ?
C17 C27 1.365(4) . ?
C17 C28 1.374(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.384(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.374(4) . ?
C19 N8 1.444(4) . ?
N9 N10 1.204(3) . ?
N9 C29 1.507(4) . ?
C20 C24 1.373(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.359(4) . ?
C21 C25 1.393(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.384(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.364(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.376(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.337(5) . ?
C29 C37 1.397(5) . ?
C30 H30 0.9500 . ?
C31 C38 1.371(5) . ?
C31 H31 0.9500 . ?
C32 C38 1.387(5) . ?
C32 H32 0.9500 . ?
C33 C35 1.371(5) . ?
C33 C36 1.373(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.373(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.416(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 91.45(11) . . ?
N7 Fe1 N1 94.00(10) . . ?
N5 Fe1 N1 93.96(10) . . ?
N7 Fe1 N4 92.17(10) . . ?
N5 Fe1 N4 92.65(11) . . ?
N1 Fe1 N4 170.84(10) . . ?
N7 Fe1 N3 173.04(10) . . ?
N5 Fe1 N3 91.39(10) . . ?
N1 Fe1 N3 79.47(9) . . ?
N4 Fe1 N3 94.05(9) . . ?
N7 Fe1 N2 93.22(10) . . ?
N5 Fe1 N2 170.98(10) . . ?
N1 Fe1 N2 93.41(9) . . ?
N4 Fe1 N2 79.47(10) . . ?
N3 Fe1 N2 84.85(9) . . ?
C10 N1 C6 117.4(2) . . ?
C10 N1 Fe1 127.6(2) . . ?
C6 N1 Fe1 114.76(18) . . ?
C4 N2 C1 117.9(2) . . ?
C4 N2 Fe1 114.38(19) . . ?
C1 N2 Fe1 126.95(19) . . ?
C23 C1 C8 120.0(3) . . ?
C23 C1 N2 121.1(2) . . ?
C8 C1 N2 118.8(3) . . ?
C14 C2 C11 120.6(3) . . ?
C14 C2 N3 121.3(2) . . ?
C11 C2 N3 118.0(3) . . ?
N7 C3 S1 178.8(3) . . ?
C5 N3 C2 119.6(2) . . ?
C5 N3 Fe1 114.82(19) . . ?
C2 N3 Fe1 125.22(18) . . ?
N2 C4 C15 117.2(3) . . ?
N2 C4 H4 121.4 . . ?
C15 C4 H4 121.4 . . ?
N3 C5 C6 116.4(3) . . ?
N3 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C26 N4 C15 117.3(3) . . ?
C26 N4 Fe1 127.9(2) . . ?
C15 N4 Fe1 114.79(18) . . ?
C12 N5 Fe1 167.3(2) . . ?
N1 C6 C18 122.9(3) . . ?
N1 C6 C5 113.0(3) . . ?
C18 C6 C5 124.1(3) . . ?
C8 C7 C9 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C9 C7 H7 120.4 . . ?
C7 C8 C1 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
C13 C9 C7 121.0(3) . . ?
C13 C9 N10 113.0(3) . . ?
C7 C9 N10 126.0(3) . . ?
N1 C10 C20 122.6(3) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
C22 C11 C2 119.4(3) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.2(3) . . ?
C23 C13 C9 119.6(3) . . ?
C23 C13 H13 120.2 . . ?
C9 C13 H13 120.2 . . ?
C2 C14 C16 119.2(3) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
N4 C15 C32 123.1(3) . . ?
N4 C15 C4 113.4(3) . . ?
C32 C15 C4 123.5(3) . . ?
C19 C16 C14 120.4(3) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 112.3(2) . . ?
C27 C17 C28 120.3(3) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 171.4(2) . . ?
C6 C18 C24 118.6(3) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 119.8(3) . . ?
C22 C19 N8 114.4(3) . . ?
C16 C19 N8 125.8(3) . . ?
N6 N8 C19 113.3(2) . . ?
N10 N9 C29 111.3(3) . . ?
N9 N10 C9 107.9(3) . . ?
C24 C20 C10 119.7(3) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C30 C21 C25 120.4(3) . . ?
C30 C21 N6 116.4(3) . . ?
C25 C21 N6 123.2(3) . . ?
C19 C22 C11 120.6(3) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.3(3) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C20 C24 C18 118.6(3) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C28 C25 C21 118.9(3) . . ?
C28 C25 H25 120.5 . . ?
C21 C25 H25 120.5 . . ?
N4 C26 C31 123.0(3) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 120.1(3) . . ?
C17 C27 H27 119.9 . . ?
C30 C27 H27 119.9 . . ?
C17 C28 C25 120.0(3) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C34 C29 C37 122.5(3) . . ?
C34 C29 N9 114.7(4) . . ?
C37 C29 N9 122.6(4) . . ?
C21 C30 C27 120.2(3) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C26 C31 C38 119.7(3) . . ?
C26 C31 H31 120.1 . . ?
C38 C31 H31 120.1 . . ?
C15 C32 C38 117.8(3) . . ?
C15 C32 H32 121.1 . . ?
C38 C32 H32 121.1 . . ?
C35 C33 C36 120.1(3) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 118.7(4) . . ?
C29 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
C33 C35 C34 121.8(4) . . ?
C33 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
C33 C36 C37 119.0(4) . . ?
C33 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C29 C37 C36 118.0(3) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
C31 C38 C32 118.9(3) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.848
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.848
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.035
####################################################################### 
# 
# 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_feaza175km2
_database_code_depnum_ccdc_archive 'CCDC 1492641'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0368(9)
_cell_length_b                   14.4119(12)
_cell_length_c                   16.7208(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.815(5)
_cell_angle_gamma                90.00
_cell_volume                     3619.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    7843
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_T_max  0.8936
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                  its'aim being to analyse the evolution of partial collection of data, 
                  always carried out over the same part of reciprocal space, 
                  and over a large scale of temperature.
                  This  explain the poor completness of data as well as the low theta(max) value, 
                  the low number of unique reflexions collected.
                  In ordre to obtain significant intensities with an exposure time relatively short, 
                  a crystal of neutron size was used. As the aim is to compare the diffraction data 
                  always obtained from the same part of the crystal at different temperature, 
                  problems of intensity scale are not considered to be of prior importance.
                  The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                  over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                  these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                  or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                  but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5633
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         22.98
_reflns_number_total             4041
_reflns_number_gt                3343
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0260P)²+2.2080P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4041
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29201(3) 0.28493(3) 0.06578(3) 0.03410(16) Uani 1 1 d . . .
S1 S 0.19450(5) 0.48903(6) -0.14321(5) 0.0442(2) Uani 1 1 d . . .
S2 S 0.42513(6) 0.07451(6) -0.10816(5) 0.0490(3) Uani 1 1 d . . .
N1 N 0.17718(16) 0.21877(14) 0.07994(15) 0.0324(6) Uani 1 1 d . . .
N2 N 0.27201(15) 0.37541(15) 0.15664(14) 0.0281(6) Uani 1 1 d . . .
C1 C 0.19438(18) 0.38171(18) 0.20365(18) 0.0296(7) Uani 1 1 d . . .
C2 C 0.41716(18) 0.18481(18) 0.18917(18) 0.0299(7) Uani 1 1 d . . .
C3 C 0.22180(19) 0.4181(2) -0.0694(2) 0.0360(8) Uani 1 1 d . . .
N3 N 0.32862(15) 0.19495(15) 0.15460(14) 0.0299(6) Uani 1 1 d . . .
C4 C 0.34130(19) 0.42175(18) 0.18045(18) 0.0330(7) Uani 1 1 d . . .
H4 H 0.3411 0.4607 0.2263 0.040 Uiso 1 1 calc R . .
C5 C 0.26380(19) 0.15212(18) 0.18507(18) 0.0321(7) Uani 1 1 d . . .
H5 H 0.2726 0.1142 0.2312 0.039 Uiso 1 1 calc R . .
N4 N 0.40890(15) 0.35292(16) 0.07187(15) 0.0356(6) Uani 1 1 d . . .
N5 N 0.33163(18) 0.19894(18) -0.01583(18) 0.0473(7) Uani 1 1 d . . .
C6 C 0.17594(19) 0.16415(18) 0.14582(18) 0.0306(7) Uani 1 1 d . . .
C7 C 0.0371(2) 0.40239(19) 0.2095(2) 0.0411(8) Uani 1 1 d . . .
H7 H -0.0196 0.4136 0.1837 0.049 Uiso 1 1 calc R . .
C8 C 0.11259(19) 0.39754(18) 0.16450(19) 0.0343(8) Uani 1 1 d . . .
H8 H 0.1080 0.4050 0.1080 0.041 Uiso 1 1 calc R . .
C9 C 0.0448(2) 0.3909(2) 0.2914(2) 0.0410(8) Uani 1 1 d . . .
C10 C 0.1010(2) 0.2276(2) 0.0357(2) 0.0407(8) Uani 1 1 d . . .
H10 H 0.1011 0.2637 -0.0118 0.049 Uiso 1 1 calc R . .
C11 C 0.4836(2) 0.1576(2) 0.1397(2) 0.0405(8) Uani 1 1 d . . .
H11 H 0.4696 0.1427 0.0852 0.049 Uiso 1 1 calc R . .
C12 C 0.3693(2) 0.1469(2) -0.0549(2) 0.0376(8) Uani 1 1 d . . .
C13 C 0.1262(2) 0.3761(2) 0.3289(2) 0.0485(9) Uani 1 1 d . . .
H13 H 0.1312 0.3696 0.3855 0.058 Uiso 1 1 calc R . .
C14 C 0.4377(2) 0.20628(19) 0.2684(2) 0.0384(8) Uani 1 1 d . . .
H14 H 0.3922 0.2254 0.3022 0.046 Uiso 1 1 calc R . .
C15 C 0.41994(18) 0.41200(19) 0.13425(19) 0.0342(7) Uani 1 1 d . . .
C16 C 0.5252(2) 0.1999(2) 0.2984(2) 0.0395(8) Uani 1 1 d . . .
H16 H 0.5395 0.2144 0.3529 0.047 Uiso 1 1 calc R . .
N6 N 0.69906(16) 0.15410(16) 0.34591(18) 0.0426(7) Uani 1 1 d . . .
C17 C 0.9680(2) 0.1156(2) 0.4187(2) 0.0434(9) Uani 1 1 d . . .
H17 H 1.0282 0.1042 0.4359 0.052 Uiso 1 1 calc R . .
N7 N 0.24116(17) 0.36930(18) -0.01622(18) 0.0454(7) Uani 1 1 d . . .
C18 C 0.0995(2) 0.1225(2) 0.1706(2) 0.0409(8) Uani 1 1 d . . .
H18 H 0.1006 0.0862 0.2181 0.049 Uiso 1 1 calc R . .
C19 C 0.59112(19) 0.17254(19) 0.2494(2) 0.0354(8) Uani 1 1 d . . .
N8 N 0.68473(17) 0.16319(16) 0.27281(18) 0.0410(7) Uani 1 1 d . . .
N9 N -0.0976(2) 0.39355(17) 0.30930(19) 0.0559(8) Uani 1 1 d . . .
N10 N -0.0290(2) 0.39915(18) 0.3477(2) 0.0600(9) Uani 1 1 d . . .
C20 C 0.0228(2) 0.1868(2) 0.0560(2) 0.0486(9) Uani 1 1 d . . .
H20 H -0.0298 0.1946 0.0229 0.058 Uiso 1 1 calc R . .
C21 C 0.79320(19) 0.14365(19) 0.3680(2) 0.0368(8) Uani 1 1 d . . .
C22 C 0.5704(2) 0.1525(2) 0.1703(2) 0.0395(8) Uani 1 1 d . . .
H22 H 0.6163 0.1348 0.1363 0.047 Uiso 1 1 calc R . .
C23 C 0.2010(2) 0.3704(2) 0.28530(19) 0.0418(8) Uani 1 1 d . . .
H23 H 0.2573 0.3587 0.3116 0.050 Uiso 1 1 calc R . .
C24 C 0.0213(2) 0.1346(2) 0.1247(2) 0.0489(9) Uani 1 1 d . . .
H24 H -0.0326 0.1072 0.1404 0.059 Uiso 1 1 calc R . .
C25 C 0.8603(2) 0.1628(2) 0.3163(2) 0.0459(9) Uani 1 1 d . . .
H25 H 0.8463 0.1850 0.2637 0.055 Uiso 1 1 calc R . .
C26 C 0.4765(2) 0.3435(2) 0.0233(2) 0.0514(9) Uani 1 1 d . . .
H26 H 0.4691 0.3035 -0.0216 0.062 Uiso 1 1 calc R . .
C27 C 0.9013(2) 0.0991(2) 0.4691(2) 0.0502(9) Uani 1 1 d . . .
H27 H 0.9152 0.0774 0.5219 0.060 Uiso 1 1 calc R . .
C28 C 0.9480(2) 0.1490(2) 0.3428(2) 0.0480(9) Uani 1 1 d . . .
H28 H 0.9946 0.1626 0.3083 0.058 Uiso 1 1 calc R . .
C29 C -0.1751(3) 0.4063(2) 0.3616(3) 0.0535(10) Uani 1 1 d . . .
C30 C 0.8135(2) 0.1136(2) 0.4439(2) 0.0472(9) Uani 1 1 d . . .
H30 H 0.7674 0.1026 0.4796 0.057 Uiso 1 1 calc R . .
C31 C 0.5558(2) 0.3888(3) 0.0356(3) 0.0655(11) Uani 1 1 d . . .
H31 H 0.6017 0.3810 -0.0008 0.079 Uiso 1 1 calc R . .
C32 C 0.4986(2) 0.4583(2) 0.1518(2) 0.0519(9) Uani 1 1 d . . .
H32 H 0.5052 0.4977 0.1972 0.062 Uiso 1 1 calc R . .
C33 C -0.3264(2) 0.4357(2) 0.4438(3) 0.0595(10) Uani 1 1 d . . .
H33 H -0.3796 0.4455 0.4709 0.071 Uiso 1 1 calc R . .
C34 C -0.2555(3) 0.3904(2) 0.3247(3) 0.0593(11) Uani 1 1 d . . .
H34 H -0.2598 0.3694 0.2708 0.071 Uiso 1 1 calc R . .
C35 C -0.3310(2) 0.4048(2) 0.3660(3) 0.0611(10) Uani 1 1 d . . .
H35 H -0.3876 0.3932 0.3402 0.073 Uiso 1 1 calc R . .
C36 C -0.2451(2) 0.4527(2) 0.4830(3) 0.0636(11) Uani 1 1 d . . .
H36 H -0.2417 0.4741 0.5368 0.076 Uiso 1 1 calc R . .
C37 C -0.1667(2) 0.4374(2) 0.4407(3) 0.0615(11) Uani 1 1 d . . .
H37 H -0.1096 0.4481 0.4659 0.074 Uiso 1 1 calc R . .
C38 C 0.5684(2) 0.4457(3) 0.1008(3) 0.0661(12) Uani 1 1 d . . .
H38 H 0.6239 0.4760 0.1112 0.079 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 1.958(3) . ?
Fe1 N7 1.960(3) . ?
Fe1 N1 1.997(2) . ?
Fe1 N4 2.010(2) . ?
Fe1 N3 2.027(2) . ?
Fe1 N2 2.036(2) . ?
S1 C3 1.639(4) . ?
S2 C12 1.630(4) . ?
N1 C10 1.339(4) . ?
N1 C6 1.355(4) . ?
N2 C4 1.284(3) . ?
N2 C1 1.442(3) . ?
C1 C23 1.374(4) . ?
C1 C8 1.384(4) . ?
C2 C14 1.380(4) . ?
C2 C11 1.384(4) . ?
C2 N3 1.433(4) . ?
C3 N7 1.159(4) . ?
N3 C5 1.280(3) . ?
C4 C15 1.451(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.456(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.339(4) . ?
N4 C15 1.351(4) . ?
N5 C12 1.161(4) . ?
C6 C18 1.378(4) . ?
C7 C9 1.379(4) . ?
C7 C8 1.393(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.365(4) . ?
C9 N10 1.494(4) . ?
C10 C20 1.371(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.381(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.371(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.387(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.377(4) . ?
C16 C19 1.375(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.238(3) . ?
N6 C21 1.453(4) . ?
C17 C27 1.363(4) . ?
C17 C28 1.376(5) . ?
C17 H17 0.9500 . ?
C18 C24 1.383(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.374(4) . ?
C19 N8 1.449(4) . ?
N9 N10 1.192(4) . ?
N9 C29 1.502(4) . ?
C20 C24 1.374(5) . ?
C20 H20 0.9500 . ?
C21 C30 1.363(4) . ?
C21 C25 1.387(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.385(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.365(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.380(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.350(5) . ?
C29 C37 1.396(5) . ?
C30 H30 0.9500 . ?
C31 C38 1.369(5) . ?
C31 H31 0.9500 . ?
C32 C38 1.395(5) . ?
C32 H32 0.9500 . ?
C33 C35 1.374(5) . ?
C33 C36 1.379(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.372(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.421(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N5 Fe1 N7 91.53(11) . . ?
N5 Fe1 N1 94.30(10) . . ?
N7 Fe1 N1 93.97(10) . . ?
N5 Fe1 N4 92.78(11) . . ?
N7 Fe1 N4 92.47(10) . . ?
N1 Fe1 N4 170.29(10) . . ?
N5 Fe1 N3 91.42(10) . . ?
N7 Fe1 N3 172.77(10) . . ?
N1 Fe1 N3 79.22(10) . . ?
N4 Fe1 N3 93.98(9) . . ?
N5 Fe1 N2 170.71(10) . . ?
N7 Fe1 N2 93.32(10) . . ?
N1 Fe1 N2 93.27(9) . . ?
N4 Fe1 N2 79.10(10) . . ?
N3 Fe1 N2 84.71(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 127.6(2) . . ?
C6 N1 Fe1 114.86(19) . . ?
C4 N2 C1 117.7(2) . . ?
C4 N2 Fe1 114.65(19) . . ?
C1 N2 Fe1 126.91(18) . . ?
C23 C1 C8 120.6(3) . . ?
C23 C1 N2 120.9(3) . . ?
C8 C1 N2 118.5(3) . . ?
C14 C2 C11 120.1(3) . . ?
C14 C2 N3 121.6(3) . . ?
C11 C2 N3 118.1(3) . . ?
N7 C3 S1 178.7(3) . . ?
C5 N3 C2 120.1(2) . . ?
C5 N3 Fe1 114.54(19) . . ?
C2 N3 Fe1 125.05(18) . . ?
N2 C4 C15 117.0(3) . . ?
N2 C4 H4 121.5 . . ?
C15 C4 H4 121.5 . . ?
N3 C5 C6 117.0(3) . . ?
N3 C5 H5 121.5 . . ?
C6 C5 H5 121.5 . . ?
C26 N4 C15 117.6(3) . . ?
C26 N4 Fe1 127.5(2) . . ?
C15 N4 Fe1 114.86(18) . . ?
C12 N5 Fe1 167.2(3) . . ?
N1 C6 C18 122.9(3) . . ?
N1 C6 C5 112.8(3) . . ?
C18 C6 C5 124.3(3) . . ?
C9 C7 C8 120.0(3) . . ?
C9 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C1 C8 C7 118.8(3) . . ?
C1 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C13 C9 C7 120.3(3) . . ?
C13 C9 N10 113.6(3) . . ?
C7 C9 N10 126.0(3) . . ?
N1 C10 C20 122.9(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 119.4(3) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.2(3) . . ?
C9 C13 C23 120.3(3) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C2 C14 C16 119.7(3) . . ?
C2 C14 H14 120.1 . . ?
C16 C14 H14 120.1 . . ?
N4 C15 C32 122.8(3) . . ?
N4 C15 C4 113.6(2) . . ?
C32 C15 C4 123.7(3) . . ?
C19 C16 C14 120.1(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 112.4(3) . . ?
C27 C17 C28 119.7(3) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C3 N7 Fe1 170.9(3) . . ?
C6 C18 C24 118.5(3) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 119.9(3) . . ?
C22 C19 N8 114.3(3) . . ?
C16 C19 N8 125.8(3) . . ?
N6 N8 C19 113.4(3) . . ?
N10 N9 C29 110.7(3) . . ?
N9 N10 C9 107.8(3) . . ?
C10 C20 C24 119.4(3) . . ?
C10 C20 H20 120.3 . . ?
C24 C20 H20 120.3 . . ?
C30 C21 C25 120.5(3) . . ?
C30 C21 N6 116.2(3) . . ?
C25 C21 N6 123.4(3) . . ?
C19 C22 C11 120.7(3) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.0(3) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C20 C24 C18 118.9(3) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C28 C25 C21 118.8(3) . . ?
C28 C25 H25 120.6 . . ?
C21 C25 H25 120.6 . . ?
N4 C26 C31 122.9(3) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 120.5(3) . . ?
C17 C27 H27 119.8 . . ?
C30 C27 H27 119.8 . . ?
C17 C28 C25 120.5(3) . . ?
C17 C28 H28 119.7 . . ?
C25 C28 H28 119.7 . . ?
C34 C29 C37 121.7(3) . . ?
C34 C29 N9 114.5(4) . . ?
C37 C29 N9 123.7(4) . . ?
C21 C30 C27 120.0(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C26 C31 C38 119.5(3) . . ?
C26 C31 H31 120.3 . . ?
C38 C31 H31 120.3 . . ?
C15 C32 C38 118.1(3) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C35 C33 C36 120.7(3) . . ?
C35 C33 H33 119.7 . . ?
C36 C33 H33 119.7 . . ?
C29 C34 C35 119.2(4) . . ?
C29 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C33 121.4(4) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.2(4) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
C29 C37 C36 118.8(4) . . ?
C29 C37 H37 120.6 . . ?
C36 C37 H37 120.6 . . ?
C31 C38 C32 119.0(3) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.804
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.804
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.039
####################################################################### 
# 
# 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_feaza165kd2
_database_code_depnum_ccdc_archive 'CCDC 1492642'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
       bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0266(8)
_cell_length_b                   14.4078(11)
_cell_length_c                   16.6985(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.813(4)
_cell_angle_gamma                90.00
_cell_volume                     3610.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    165(2)
_cell_measurement_reflns_used    6903
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5446
_exptl_absorpt_correction_T_max  0.8934
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
             its'aim being to analyse the evolution of partial collection of data, 
             always carried out over the same part of reciprocal space, 
             and over a large scale of temperature.
             This  explain the poor completness of data as well as the low theta(max) value, 
             the low number of unique reflexions collected.
             In ordre to obtain significant intensities with an exposure time relatively short, 
             a crystal of neutron size was used. As the aim is to compare the diffraction data 
             always obtained from the same part of the crystal at different temperature, 
             problems of intensity scale are not considered to be of prior importance.
             The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
             over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
             these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
             or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
             but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      165(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5651
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         22.97
_reflns_number_total             4057
_reflns_number_gt                3443
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0250P)²+2.3886P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4057
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29185(2) 0.28462(3) 0.06693(2) 0.02991(15) Uani 1 1 d . . .
S1 S 0.19492(5) 0.48785(5) -0.14287(5) 0.0390(2) Uani 1 1 d . . .
S2 S 0.42332(5) 0.07460(5) -0.10818(5) 0.0434(2) Uani 1 1 d . . .
N1 N 0.17748(15) 0.21906(14) 0.08009(14) 0.0288(6) Uani 1 1 d . . .
N2 N 0.27160(14) 0.37469(14) 0.15638(13) 0.0254(5) Uani 1 1 d . . .
C1 C 0.19409(17) 0.38107(17) 0.20312(17) 0.0266(7) Uani 1 1 d . . .
C2 C 0.41723(18) 0.18504(17) 0.18886(18) 0.0280(7) Uani 1 1 d . . .
C3 C 0.22271(17) 0.41721(19) -0.06882(19) 0.0301(7) Uani 1 1 d . . .
N3 N 0.32840(15) 0.19555(14) 0.15474(13) 0.0266(5) Uani 1 1 d . . .
C4 C 0.34079(18) 0.42149(18) 0.17975(17) 0.0305(7) Uani 1 1 d . . .
H4 H 0.3405 0.4609 0.2254 0.037 Uiso 1 1 calc R . .
C5 C 0.26377(18) 0.15205(18) 0.18532(17) 0.0285(7) Uani 1 1 d . . .
H5 H 0.2727 0.1139 0.2314 0.034 Uiso 1 1 calc R . .
N4 N 0.40800(14) 0.35189(15) 0.07132(14) 0.0316(6) Uani 1 1 d . . .
N5 N 0.33030(16) 0.19836(17) -0.01465(16) 0.0402(6) Uani 1 1 d . . .
C6 C 0.17623(18) 0.16403(17) 0.14582(17) 0.0282(7) Uani 1 1 d . . .
C7 C 0.03682(19) 0.40219(18) 0.2088(2) 0.0380(8) Uani 1 1 d . . .
H7 H -0.0198 0.4133 0.1828 0.046 Uiso 1 1 calc R . .
C8 C 0.11217(18) 0.39725(17) 0.16427(18) 0.0316(7) Uani 1 1 d . . .
H8 H 0.1076 0.4049 0.1077 0.038 Uiso 1 1 calc R . .
C9 C 0.0441(2) 0.39091(19) 0.2914(2) 0.0370(8) Uani 1 1 d . . .
C10 C 0.1017(2) 0.22785(19) 0.03543(19) 0.0362(7) Uani 1 1 d . . .
H10 H 0.1021 0.2644 -0.0119 0.043 Uiso 1 1 calc R . .
C11 C 0.48378(19) 0.15749(19) 0.13936(18) 0.0369(7) Uani 1 1 d . . .
H11 H 0.4697 0.1424 0.0848 0.044 Uiso 1 1 calc R . .
C12 C 0.36791(19) 0.1469(2) -0.05416(18) 0.0320(7) Uani 1 1 d . . .
C13 C 0.1259(2) 0.3756(2) 0.32922(19) 0.0442(8) Uani 1 1 d . . .
H13 H 0.1308 0.3688 0.3859 0.053 Uiso 1 1 calc R . .
C14 C 0.43782(19) 0.20668(18) 0.26830(18) 0.0342(7) Uani 1 1 d . . .
H14 H 0.3922 0.2257 0.3021 0.041 Uiso 1 1 calc R . .
C15 C 0.41953(17) 0.41156(18) 0.13341(18) 0.0312(7) Uani 1 1 d . . .
C16 C 0.52538(19) 0.20054(18) 0.29860(19) 0.0359(7) Uani 1 1 d . . .
H16 H 0.5398 0.2155 0.3531 0.043 Uiso 1 1 calc R . .
N6 N 0.69944(15) 0.15426(15) 0.34626(17) 0.0381(6) Uani 1 1 d . . .
C17 C 0.96846(19) 0.11519(19) 0.4186(2) 0.0395(8) Uani 1 1 d . . .
H17 H 1.0287 0.1037 0.4357 0.047 Uiso 1 1 calc R . .
N7 N 0.24227(15) 0.36856(17) -0.01516(16) 0.0373(6) Uani 1 1 d . . .
C18 C 0.09935(19) 0.12197(19) 0.16990(19) 0.0366(8) Uani 1 1 d . . .
H18 H 0.1002 0.0853 0.2172 0.044 Uiso 1 1 calc R . .
C19 C 0.59157(18) 0.17256(18) 0.24904(19) 0.0325(7) Uani 1 1 d . . .
N8 N 0.68454(16) 0.16273(15) 0.27286(17) 0.0365(6) Uani 1 1 d . . .
N9 N -0.0997(2) 0.39312(16) 0.30862(17) 0.0480(7) Uani 1 1 d . . .
N10 N -0.0293(2) 0.39853(17) 0.34658(18) 0.0508(7) Uani 1 1 d . . .
C20 C 0.0231(2) 0.1865(2) 0.0548(2) 0.0439(8) Uani 1 1 d . . .
H20 H -0.0292 0.1938 0.0211 0.053 Uiso 1 1 calc R . .
C21 C 0.79323(18) 0.14393(18) 0.36812(19) 0.0331(7) Uani 1 1 d . . .
C22 C 0.57050(19) 0.15219(19) 0.16980(19) 0.0384(8) Uani 1 1 d . . .
H22 H 0.6163 0.1343 0.1357 0.046 Uiso 1 1 calc R . .
C23 C 0.20090(19) 0.3699(2) 0.28532(18) 0.0388(8) Uani 1 1 d . . .
H23 H 0.2573 0.3584 0.3116 0.047 Uiso 1 1 calc R . .
C24 C 0.0211(2) 0.1343(2) 0.1238(2) 0.0441(8) Uani 1 1 d . . .
H24 H -0.0330 0.1073 0.1395 0.053 Uiso 1 1 calc R . .
C25 C 0.8606(2) 0.1627(2) 0.3165(2) 0.0426(8) Uani 1 1 d . . .
H25 H 0.8465 0.1849 0.2638 0.051 Uiso 1 1 calc R . .
C26 C 0.4756(2) 0.3422(2) 0.0228(2) 0.0458(8) Uani 1 1 d . . .
H26 H 0.4679 0.3018 -0.0220 0.055 Uiso 1 1 calc R . .
C27 C 0.9018(2) 0.0985(2) 0.4694(2) 0.0459(8) Uani 1 1 d . . .
H27 H 0.9160 0.0764 0.5221 0.055 Uiso 1 1 calc R . .
C28 C 0.9485(2) 0.1487(2) 0.3427(2) 0.0443(8) Uani 1 1 d . . .
H28 H 0.9951 0.1622 0.3081 0.053 Uiso 1 1 calc R . .
C29 C -0.1770(2) 0.4058(2) 0.3600(2) 0.0467(9) Uani 1 1 d . . .
C30 C 0.8136(2) 0.1136(2) 0.4445(2) 0.0429(8) Uani 1 1 d . . .
H30 H 0.7674 0.1030 0.4803 0.051 Uiso 1 1 calc R . .
C31 C 0.5554(2) 0.3875(2) 0.0344(2) 0.0588(10) Uani 1 1 d . . .
H31 H 0.6013 0.3791 -0.0021 0.071 Uiso 1 1 calc R . .
C32 C 0.4986(2) 0.4587(2) 0.1501(2) 0.0489(9) Uani 1 1 d . . .
H32 H 0.5052 0.4990 0.1950 0.059 Uiso 1 1 calc R . .
C33 C -0.3283(2) 0.4355(2) 0.4425(2) 0.0550(10) Uani 1 1 d . . .
H33 H -0.3814 0.4453 0.4699 0.066 Uiso 1 1 calc R . .
C34 C -0.2576(2) 0.3908(2) 0.3227(2) 0.0527(9) Uani 1 1 d . . .
H34 H -0.2619 0.3705 0.2686 0.063 Uiso 1 1 calc R . .
C35 C -0.3331(2) 0.4051(2) 0.3640(2) 0.0548(9) Uani 1 1 d . . .
H35 H -0.3898 0.3939 0.3381 0.066 Uiso 1 1 calc R . .
C36 C -0.2465(2) 0.4516(2) 0.4813(2) 0.0577(10) Uani 1 1 d . . .
H36 H -0.2428 0.4725 0.5353 0.069 Uiso 1 1 calc R . .
C37 C -0.1684(2) 0.4363(2) 0.4393(2) 0.0546(10) Uani 1 1 d . . .
H37 H -0.1112 0.4467 0.4646 0.066 Uiso 1 1 calc R . .
C38 C 0.5681(2) 0.4452(2) 0.0992(3) 0.0597(10) Uani 1 1 d . . .
H38 H 0.6237 0.4756 0.1093 0.072 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.948(3) . ?
Fe1 N5 1.952(3) . ?
Fe1 N1 1.983(2) . ?
Fe1 N4 1.995(2) . ?
Fe1 N3 2.005(2) . ?
Fe1 N2 2.013(2) . ?
S1 C3 1.640(3) . ?
S2 C12 1.632(3) . ?
N1 C10 1.337(4) . ?
N1 C6 1.355(3) . ?
N2 C4 1.284(3) . ?
N2 C1 1.436(3) . ?
C1 C23 1.381(4) . ?
C1 C8 1.383(4) . ?
C2 C14 1.383(4) . ?
C2 C11 1.386(4) . ?
C2 N3 1.433(3) . ?
C3 N7 1.164(3) . ?
N3 C5 1.283(3) . ?
C4 C15 1.452(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.453(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.337(4) . ?
N4 C15 1.351(3) . ?
N5 C12 1.158(3) . ?
C6 C18 1.382(4) . ?
C7 C9 1.387(4) . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.372(4) . ?
C9 N10 1.475(4) . ?
C10 C20 1.375(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.377(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.377(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.389(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.385(4) . ?
C16 C19 1.385(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.241(3) . ?
N6 C21 1.446(3) . ?
C17 C27 1.365(4) . ?
C17 C28 1.376(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.385(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.377(4) . ?
C19 N8 1.441(4) . ?
N9 N10 1.210(3) . ?
N9 C29 1.488(4) . ?
C20 C24 1.377(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.369(4) . ?
C21 C25 1.388(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.387(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.371(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.388(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.351(5) . ?
C29 C37 1.396(5) . ?
C30 H30 0.9500 . ?
C31 C38 1.371(5) . ?
C31 H31 0.9500 . ?
C32 C38 1.392(5) . ?
C32 H32 0.9500 . ?
C33 C36 1.380(5) . ?
C33 C35 1.380(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.372(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.413(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 91.16(10) . . ?
N7 Fe1 N1 94.02(9) . . ?
N5 Fe1 N1 93.55(9) . . ?
N7 Fe1 N4 91.60(9) . . ?
N5 Fe1 N4 92.67(10) . . ?
N1 Fe1 N4 171.53(10) . . ?
N7 Fe1 N3 173.41(9) . . ?
N5 Fe1 N3 91.32(9) . . ?
N1 Fe1 N3 79.73(9) . . ?
N4 Fe1 N3 94.38(9) . . ?
N7 Fe1 N2 93.18(9) . . ?
N5 Fe1 N2 171.43(9) . . ?
N1 Fe1 N2 93.52(9) . . ?
N4 Fe1 N2 79.83(9) . . ?
N3 Fe1 N2 85.18(8) . . ?
C10 N1 C6 117.5(2) . . ?
C10 N1 Fe1 127.8(2) . . ?
C6 N1 Fe1 114.53(18) . . ?
C4 N2 C1 117.9(2) . . ?
C4 N2 Fe1 114.49(18) . . ?
C1 N2 Fe1 126.91(17) . . ?
C23 C1 C8 120.5(3) . . ?
C23 C1 N2 120.7(2) . . ?
C8 C1 N2 118.9(3) . . ?
C14 C2 C11 120.2(3) . . ?
C14 C2 N3 121.2(2) . . ?
C11 C2 N3 118.6(3) . . ?
N7 C3 S1 178.6(3) . . ?
C5 N3 C2 119.9(2) . . ?
C5 N3 Fe1 114.73(18) . . ?
C2 N3 Fe1 125.08(17) . . ?
N2 C4 C15 117.1(3) . . ?
N2 C4 H4 121.5 . . ?
C15 C4 H4 121.5 . . ?
N3 C5 C6 116.6(2) . . ?
N3 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C26 N4 C15 117.3(2) . . ?
C26 N4 Fe1 128.0(2) . . ?
C15 N4 Fe1 114.60(17) . . ?
C12 N5 Fe1 167.0(2) . . ?
N1 C6 C18 122.5(2) . . ?
N1 C6 C5 112.9(2) . . ?
C18 C6 C5 124.6(3) . . ?
C9 C7 C8 120.1(3) . . ?
C9 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C1 C8 C7 119.2(3) . . ?
C1 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C13 C9 C7 120.1(3) . . ?
C13 C9 N10 113.9(3) . . ?
C7 C9 N10 126.0(3) . . ?
N1 C10 C20 123.1(3) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.5(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
N5 C12 S2 178.4(3) . . ?
C9 C13 C23 120.2(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C2 C14 C16 119.9(3) . . ?
C2 C14 H14 120.1 . . ?
C16 C14 H14 120.1 . . ?
N4 C15 C32 122.9(3) . . ?
N4 C15 C4 113.2(2) . . ?
C32 C15 C4 123.9(3) . . ?
C19 C16 C14 119.7(3) . . ?
C19 C16 H16 120.1 . . ?
C14 C16 H16 120.1 . . ?
N8 N6 C21 112.7(2) . . ?
C27 C17 C28 120.1(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 171.4(2) . . ?
C6 C18 C24 118.8(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 119.9(3) . . ?
C22 C19 N8 114.7(3) . . ?
C16 C19 N8 125.4(3) . . ?
N6 N8 C19 114.1(2) . . ?
N10 N9 C29 112.2(3) . . ?
N9 N10 C9 109.3(3) . . ?
C10 C20 C24 119.2(3) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C30 C21 C25 120.4(3) . . ?
C30 C21 N6 116.0(3) . . ?
C25 C21 N6 123.7(3) . . ?
C19 C22 C11 120.8(3) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C13 C23 C1 120.0(3) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C20 C24 C18 118.8(3) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C28 C25 C21 119.2(3) . . ?
C28 C25 H25 120.4 . . ?
C21 C25 H25 120.4 . . ?
N4 C26 C31 123.3(3) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C17 C27 C30 120.4(3) . . ?
C17 C27 H27 119.8 . . ?
C30 C27 H27 119.8 . . ?
C17 C28 C25 120.2(3) . . ?
C17 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
C34 C29 C37 121.7(3) . . ?
C34 C29 N9 115.0(3) . . ?
C37 C29 N9 123.2(3) . . ?
C21 C30 C27 119.7(3) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C26 C31 C38 119.2(3) . . ?
C26 C31 H31 120.4 . . ?
C38 C31 H31 120.4 . . ?
C15 C32 C38 118.1(3) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C36 C33 C35 120.2(3) . . ?
C36 C33 H33 119.9 . . ?
C35 C33 H33 119.9 . . ?
C29 C34 C35 119.3(4) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 121.2(4) . . ?
C34 C35 H35 119.4 . . ?
C33 C35 H35 119.4 . . ?
C33 C36 C37 118.9(4) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C29 C37 C36 118.6(3) . . ?
C29 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C31 C38 C32 119.1(3) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.809
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.809
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_feaza220km1
_database_code_depnum_ccdc_archive 'CCDC 1492643'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
   bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0861(11)
_cell_length_b                   14.4369(11)
_cell_length_c                   16.9270(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.073(4)
_cell_angle_gamma                90.00
_cell_volume                     3681.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    4328
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5502
_exptl_absorpt_correction_T_max  0.8953
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
          its'aim being to analyse the evolution of partial collection of data, 
          always carried out over the same part of reciprocal space, 
          and over a large scale of temperature.
          This  explain the poor completness of data as well as the low theta(max) value, 
          the low number of unique reflexions collected.
          In ordre to obtain significant intensities with an exposure time relatively short, 
          a crystal of neutron size was used. As the aim is to compare the diffraction data 
          always obtained from the same part of the crystal at different temperature, 
          problems of intensity scale are not considered to be of prior importance.
          The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
          over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
          these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
          or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
          but modelling this two conformations is over the scope 
   of this study of partial data collections.
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5805
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         21.27
_reflns_number_total             3470
_reflns_number_gt                2810
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0282P)²+1.9609P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3470
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0809
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29091(3) 0.28694(3) 0.05794(3) 0.0474(2) Uani 1 1 d . . .
S1 S 0.19044(6) 0.49689(7) -0.14636(5) 0.0609(3) Uani 1 1 d . . .
S2 S 0.43475(6) 0.07312(7) -0.10678(6) 0.0657(3) Uani 1 1 d . . .
N1 N 0.17244(16) 0.21647(18) 0.07924(16) 0.0443(7) Uani 1 1 d . . .
N2 N 0.27301(16) 0.37903(17) 0.15972(14) 0.0369(6) Uani 1 1 d . . .
C1 C 0.19668(19) 0.3845(2) 0.2065(2) 0.0365(8) Uani 1 1 d . . .
C2 C 0.4147(2) 0.1817(2) 0.1907(2) 0.0416(9) Uani 1 1 d . . .
C3 C 0.2149(2) 0.4249(3) -0.0747(2) 0.0510(10) Uani 1 1 d . . .
N3 N 0.32773(17) 0.19153(18) 0.15443(14) 0.0415(7) Uani 1 1 d . . .
C4 C 0.3439(2) 0.4205(2) 0.18402(19) 0.0430(8) Uani 1 1 d . . .
H4 H 0.3453 0.4557 0.2308 0.052 Uiso 1 1 calc R . .
C5 C 0.2614(2) 0.1523(2) 0.18435(19) 0.0440(8) Uani 1 1 d . . .
H5 H 0.2691 0.1163 0.2305 0.053 Uiso 1 1 calc R . .
N4 N 0.41284(16) 0.3592(2) 0.07382(18) 0.0504(8) Uani 1 1 d . . .
N5 N 0.3390(2) 0.2015(2) -0.02475(19) 0.0702(10) Uani 1 1 d . . .
C6 C 0.1738(2) 0.1646(2) 0.1454(2) 0.0415(8) Uani 1 1 d . . .
C7 C 0.0404(2) 0.4031(2) 0.2109(3) 0.0548(10) Uani 1 1 d . . .
H7 H -0.0157 0.4131 0.1854 0.066 Uiso 1 1 calc R . .
C8 C 0.1149(2) 0.3993(2) 0.1683(2) 0.0457(9) Uani 1 1 d . . .
H8 H 0.1103 0.4067 0.1131 0.055 Uiso 1 1 calc R . .
C9 C 0.0488(3) 0.3922(2) 0.2916(3) 0.0634(12) Uani 1 1 d . . .
C10 C 0.0951(3) 0.2255(3) 0.0385(2) 0.0593(10) Uani 1 1 d . . .
H10 H 0.0935 0.2600 -0.0087 0.071 Uiso 1 1 calc R . .
C11 C 0.4828(2) 0.1580(2) 0.1427(2) 0.0536(10) Uani 1 1 d . . .
H11 H 0.4701 0.1454 0.0888 0.064 Uiso 1 1 calc R . .
C12 C 0.3787(2) 0.1480(3) -0.0593(2) 0.0489(9) Uani 1 1 d . . .
C13 C 0.1295(3) 0.3770(3) 0.3302(2) 0.0671(11) Uani 1 1 d . . .
H13 H 0.1340 0.3697 0.3855 0.081 Uiso 1 1 calc R . .
C14 C 0.4340(2) 0.2022(2) 0.2694(2) 0.0503(10) Uani 1 1 d . . .
H14 H 0.3886 0.2198 0.3023 0.060 Uiso 1 1 calc R . .
C15 C 0.42274(19) 0.4126(2) 0.1386(2) 0.0458(9) Uani 1 1 d . . .
C16 C 0.5217(2) 0.1964(2) 0.2995(2) 0.0577(10) Uani 1 1 d . . .
H16 H 0.5356 0.2096 0.3531 0.069 Uiso 1 1 calc R . .
N6 N 0.6952(2) 0.1532(2) 0.3446(2) 0.0695(9) Uani 1 1 d . . .
C17 C 0.9648(2) 0.1172(3) 0.4184(3) 0.0603(10) Uani 1 1 d . . .
H17 H 1.0239 0.1069 0.4367 0.072 Uiso 1 1 calc R . .
N7 N 0.2314(2) 0.3743(2) -0.0224(2) 0.0658(9) Uani 1 1 d . . .
C18 C 0.0988(2) 0.1244(2) 0.1728(2) 0.0564(10) Uani 1 1 d . . .
H18 H 0.1018 0.0893 0.2197 0.068 Uiso 1 1 calc R . .
C19 C 0.5879(2) 0.1716(2) 0.2512(3) 0.0542(10) Uani 1 1 d . . .
N8 N 0.6843(2) 0.1629(2) 0.2743(2) 0.0645(9) Uani 1 1 d . . .
N9 N -0.0871(3) 0.3948(2) 0.3130(2) 0.0790(11) Uani 1 1 d . . .
N10 N -0.0261(3) 0.4013(2) 0.3544(2) 0.0917(13) Uani 1 1 d . . .
C20 C 0.0169(3) 0.1866(3) 0.0621(3) 0.0714(12) Uani 1 1 d . . .
H20 H -0.0365 0.1947 0.0316 0.086 Uiso 1 1 calc R . .
C21 C 0.7920(2) 0.1430(2) 0.3669(3) 0.0570(10) Uani 1 1 d . . .
C22 C 0.5683(2) 0.1528(3) 0.1732(2) 0.0582(10) Uani 1 1 d . . .
H22 H 0.6139 0.1362 0.1403 0.070 Uiso 1 1 calc R . .
C23 C 0.2028(2) 0.3726(2) 0.2872(2) 0.0535(10) Uani 1 1 d . . .
H23 H 0.2585 0.3614 0.3130 0.064 Uiso 1 1 calc R . .
C24 C 0.0187(2) 0.1365(3) 0.1301(3) 0.0687(11) Uani 1 1 d . . .
H24 H -0.0337 0.1104 0.1479 0.082 Uiso 1 1 calc R . .
C25 C 0.8591(3) 0.1624(3) 0.3159(2) 0.0686(11) Uani 1 1 d . . .
H25 H 0.8455 0.1838 0.2642 0.082 Uiso 1 1 calc R . .
C26 C 0.4819(3) 0.3524(3) 0.0283(2) 0.0745(12) Uani 1 1 d . . .
H26 H 0.4761 0.3165 -0.0180 0.089 Uiso 1 1 calc R . .
C27 C 0.8979(3) 0.1001(3) 0.4665(2) 0.0714(12) Uani 1 1 d . . .
H27 H 0.9111 0.0783 0.5181 0.086 Uiso 1 1 calc R . .
C28 C 0.9468(2) 0.1492(3) 0.3435(3) 0.0679(11) Uani 1 1 d . . .
H28 H 0.9935 0.1623 0.3106 0.081 Uiso 1 1 calc R . .
C29 C -0.1662(3) 0.4084(3) 0.3710(4) 0.0834(15) Uani 1 1 d . . .
C30 C 0.8118(2) 0.1140(3) 0.4412(3) 0.0697(11) Uani 1 1 d . . .
H30 H 0.7661 0.1032 0.4757 0.084 Uiso 1 1 calc R . .
C31 C 0.5612(3) 0.3961(4) 0.0466(4) 0.1031(17) Uani 1 1 d . . .
H31 H 0.6082 0.3901 0.0127 0.124 Uiso 1 1 calc R . .
C32 C 0.5008(2) 0.4565(3) 0.1605(3) 0.0739(12) Uani 1 1 d . . .
H32 H 0.5058 0.4920 0.2071 0.089 Uiso 1 1 calc R . .
C33 C -0.3172(3) 0.4371(3) 0.4494(3) 0.0774(13) Uani 1 1 d . . .
H33 H -0.3701 0.4467 0.4753 0.093 Uiso 1 1 calc R . .
C34 C -0.2456(3) 0.3899(3) 0.3344(3) 0.0833(14) Uani 1 1 d . . .
H34 H -0.2491 0.3678 0.2821 0.100 Uiso 1 1 calc R . .
C35 C -0.3205(3) 0.4034(3) 0.3736(3) 0.0783(13) Uani 1 1 d . . .
H35 H -0.3759 0.3892 0.3484 0.094 Uiso 1 1 calc R . .
C36 C -0.2369(3) 0.4571(3) 0.4876(3) 0.0849(13) Uani 1 1 d . . .
H36 H -0.2342 0.4805 0.5394 0.102 Uiso 1 1 calc R . .
C37 C -0.1590(3) 0.4420(3) 0.4480(3) 0.0839(14) Uani 1 1 d . . .
H37 H -0.1031 0.4544 0.4729 0.101 Uiso 1 1 calc R . .
C38 C 0.5718(3) 0.4479(4) 0.1134(4) 0.1001(16) Uani 1 1 d . . .
H38 H 0.6261 0.4770 0.1271 0.120 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 2.028(4) . ?
Fe1 N5 2.029(4) . ?
Fe1 N1 2.104(3) . ?
Fe1 N4 2.120(3) . ?
Fe1 N3 2.185(3) . ?
Fe1 N2 2.204(2) . ?
S1 C3 1.625(5) . ?
S2 C12 1.613(4) . ?
N1 C10 1.329(4) . ?
N1 C6 1.347(4) . ?
N2 C4 1.275(4) . ?
N2 C1 1.434(4) . ?
C1 C23 1.375(4) . ?
C1 C8 1.379(4) . ?
C2 C14 1.380(4) . ?
C2 C11 1.387(4) . ?
C2 N3 1.426(4) . ?
C3 N7 1.164(4) . ?
N3 C5 1.277(4) . ?
C4 C15 1.455(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.456(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.332(4) . ?
N4 C15 1.342(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.374(4) . ?
C7 C8 1.369(4) . ?
C7 C9 1.374(5) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.368(5) . ?
C9 N10 1.598(5) . ?
C10 C20 1.385(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.365(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.359(4) . ?
C13 H13 0.9400 . ?
C14 C16 1.395(4) . ?
C14 H14 0.9400 . ?
C15 C32 1.371(5) . ?
C16 C19 1.371(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.201(4) . ?
N6 C21 1.495(4) . ?
C17 C27 1.353(5) . ?
C17 C28 1.362(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.386(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.365(4) . ?
C19 N8 1.491(4) . ?
N9 N10 1.130(4) . ?
N9 C29 1.597(5) . ?
C20 C24 1.360(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.343(5) . ?
C21 C25 1.394(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.394(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.372(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.360(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.346(6) . ?
C29 C37 1.388(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.359(6) . ?
C31 H31 0.9400 . ?
C32 C38 1.374(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.371(5) . ?
C33 C36 1.373(5) . ?
C33 H33 0.9400 . ?
C34 C35 1.355(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.401(5) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N7 Fe1 N5 94.40(13) . . ?
N7 Fe1 N1 93.80(12) . . ?
N5 Fe1 N1 99.39(12) . . ?
N7 Fe1 N4 97.39(11) . . ?
N5 Fe1 N4 92.66(13) . . ?
N1 Fe1 N4 162.87(11) . . ?
N7 Fe1 N3 168.12(11) . . ?
N5 Fe1 N3 92.66(11) . . ?
N1 Fe1 N3 75.61(10) . . ?
N4 Fe1 N3 91.80(10) . . ?
N7 Fe1 N2 94.65(11) . . ?
N5 Fe1 N2 165.75(11) . . ?
N1 Fe1 N2 90.97(10) . . ?
N4 Fe1 N2 75.27(11) . . ?
N3 Fe1 N2 80.38(9) . . ?
C10 N1 C6 117.4(3) . . ?
C10 N1 Fe1 126.4(3) . . ?
C6 N1 Fe1 115.9(2) . . ?
C4 N2 C1 118.8(3) . . ?
C4 N2 Fe1 113.5(2) . . ?
C1 N2 Fe1 126.9(2) . . ?
C23 C1 C8 119.7(3) . . ?
C23 C1 N2 121.9(3) . . ?
C8 C1 N2 118.4(3) . . ?
C14 C2 C11 119.7(3) . . ?
C14 C2 N3 122.4(3) . . ?
C11 C2 N3 117.7(3) . . ?
N7 C3 S1 178.7(4) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.7(2) . . ?
C2 N3 Fe1 125.2(2) . . ?
N2 C4 C15 119.2(3) . . ?
N2 C4 H4 120.4 . . ?
C15 C4 H4 120.4 . . ?
N3 C5 C6 118.6(3) . . ?
N3 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C26 N4 C15 117.3(3) . . ?
C26 N4 Fe1 126.2(3) . . ?
C15 N4 Fe1 116.4(2) . . ?
C12 N5 Fe1 166.0(3) . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 114.6(3) . . ?
C18 C6 C5 122.7(3) . . ?
C8 C7 C9 118.9(3) . . ?
C8 C7 H7 120.5 . . ?
C9 C7 H7 120.5 . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
C13 C9 C7 121.8(3) . . ?
C13 C9 N10 109.8(4) . . ?
C7 C9 N10 128.3(4) . . ?
N1 C10 C20 123.3(3) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
C22 C11 C2 120.4(3) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
N5 C12 S2 179.4(4) . . ?
C23 C13 C9 118.7(4) . . ?
C23 C13 H13 120.6 . . ?
C9 C13 H13 120.6 . . ?
C2 C14 C16 119.0(3) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
N4 C15 C32 122.9(3) . . ?
N4 C15 C4 114.7(3) . . ?
C32 C15 C4 122.4(4) . . ?
C19 C16 C14 120.4(3) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 110.0(3) . . ?
C27 C17 C28 120.3(3) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 165.7(3) . . ?
C6 C18 C24 118.8(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.1(3) . . ?
C22 C19 N8 113.3(3) . . ?
C16 C19 N8 126.6(4) . . ?
N6 N8 C19 110.5(3) . . ?
N10 N9 C29 102.7(4) . . ?
N9 N10 C9 99.4(4) . . ?
C24 C20 C10 118.8(3) . . ?
C24 C20 H20 120.6 . . ?
C10 C20 H20 120.6 . . ?
C30 C21 C25 120.6(3) . . ?
C30 C21 N6 115.6(4) . . ?
C25 C21 N6 123.7(4) . . ?
C19 C22 C11 120.5(3) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.9(3) . . ?
C13 C23 H23 119.5 . . ?
C1 C23 H23 119.5 . . ?
C20 C24 C18 119.1(4) . . ?
C20 C24 H24 120.4 . . ?
C18 C24 H24 120.4 . . ?
C21 C25 C28 118.2(4) . . ?
C21 C25 H25 120.9 . . ?
C28 C25 H25 120.9 . . ?
N4 C26 C31 122.3(4) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 120.9(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C17 C28 C25 119.8(4) . . ?
C17 C28 H28 120.1 . . ?
C25 C28 H28 120.1 . . ?
C34 C29 C37 121.6(4) . . ?
C34 C29 N9 111.6(5) . . ?
C37 C29 N9 126.6(5) . . ?
C21 C30 C27 120.1(4) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C38 C31 C26 120.2(4) . . ?
C38 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?
C15 C32 C38 119.0(4) . . ?
C15 C32 H32 120.5 . . ?
C38 C32 H32 120.5 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.5(5) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 121.3(4) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 119.0(4) . . ?
C33 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C29 C37 C36 118.6(4) . . ?
C29 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C31 C38 C32 118.2(4) . . ?
C31 C38 H38 120.9 . . ?
C32 C38 H38 120.9 . . ?

_diffrn_measured_fraction_theta_max 0.845
_diffrn_reflns_theta_full        21.26
_diffrn_measured_fraction_theta_full 0.845
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza180km1
_database_code_depnum_ccdc_archive 'CCDC 1492644'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
   bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0406(10)
_cell_length_b                   14.4132(10)
_cell_length_c                   16.7432(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.832(3)
_cell_angle_gamma                90.00
_cell_volume                     3625.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    4419
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5457
_exptl_absorpt_correction_T_max  0.8938
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
        its'aim being to analyse the evolution of partial collection of data, 
        always carried out over the same part of reciprocal space, 
        and over a large scale of temperature.
        This  explain the poor completness of data as well as the low theta(max) value, 
        the low number of unique reflexions collected.
        In ordre to obtain significant intensities with an exposure time relatively short, 
        a crystal of neutron size was used. As the aim is to compare the diffraction data 
        always obtained from the same part of the crystal at different temperature, 
        problems of intensity scale are not considered to be of prior importance.
        The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
        over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
        these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
        or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
        but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5728
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         21.26
_reflns_number_total             3416
_reflns_number_gt                2882
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0266P)²+2.2600P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3416
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0749
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29201(3) 0.28523(3) 0.06463(3) 0.03659(18) Uani 1 1 d . . .
S1 S 0.19403(5) 0.48997(7) -0.14349(5) 0.0473(3) Uani 1 1 d . . .
S2 S 0.42648(6) 0.07435(7) -0.10819(5) 0.0517(3) Uani 1 1 d . . .
N1 N 0.17678(15) 0.21837(16) 0.07988(15) 0.0329(6) Uani 1 1 d . . .
N2 N 0.27228(15) 0.37583(16) 0.15697(13) 0.0283(6) Uani 1 1 d . . .
C1 C 0.19485(18) 0.3819(2) 0.2039(2) 0.0292(8) Uani 1 1 d . . .
C2 C 0.41721(18) 0.1842(2) 0.18923(19) 0.0316(8) Uani 1 1 d . . .
C3 C 0.22072(19) 0.4183(2) -0.0694(2) 0.0377(8) Uani 1 1 d . . .
N3 N 0.32870(15) 0.19460(16) 0.15427(14) 0.0312(6) Uani 1 1 d . . .
C4 C 0.3416(2) 0.4213(2) 0.18064(18) 0.0344(8) Uani 1 1 d . . .
H4 H 0.3416 0.4599 0.2267 0.041 Uiso 1 1 calc R . .
C5 C 0.26374(19) 0.1520(2) 0.18493(17) 0.0328(8) Uani 1 1 d . . .
H5 H 0.2725 0.1140 0.2310 0.039 Uiso 1 1 calc R . .
N4 N 0.40932(15) 0.35378(18) 0.07197(16) 0.0367(7) Uani 1 1 d . . .
N5 N 0.33267(18) 0.1994(2) -0.01722(18) 0.0518(8) Uani 1 1 d . . .
C6 C 0.17594(18) 0.1645(2) 0.14568(18) 0.0316(8) Uani 1 1 d . . .
C7 C 0.0376(2) 0.4025(2) 0.2085(2) 0.0407(9) Uani 1 1 d . . .
H7 H -0.0189 0.4134 0.1824 0.049 Uiso 1 1 calc R . .
C8 C 0.11281(19) 0.3976(2) 0.16525(18) 0.0349(8) Uani 1 1 d . . .
H8 H 0.1084 0.4051 0.1088 0.042 Uiso 1 1 calc R . .
C9 C 0.0456(2) 0.3913(2) 0.2902(3) 0.0443(9) Uani 1 1 d . . .
C10 C 0.1008(2) 0.2275(2) 0.03616(19) 0.0430(9) Uani 1 1 d . . .
H10 H 0.1007 0.2637 -0.0113 0.052 Uiso 1 1 calc R . .
C11 C 0.48400(19) 0.1576(2) 0.13995(19) 0.0414(8) Uani 1 1 d . . .
H11 H 0.4702 0.1427 0.0855 0.050 Uiso 1 1 calc R . .
C12 C 0.3709(2) 0.1474(2) -0.0555(2) 0.0390(8) Uani 1 1 d . . .
C13 C 0.1267(2) 0.3764(3) 0.3290(2) 0.0526(10) Uani 1 1 d . . .
H13 H 0.1311 0.3698 0.3855 0.063 Uiso 1 1 calc R . .
C14 C 0.43727(19) 0.2057(2) 0.26861(19) 0.0381(8) Uani 1 1 d . . .
H14 H 0.3916 0.2246 0.3023 0.046 Uiso 1 1 calc R . .
C15 C 0.42035(18) 0.4120(2) 0.1346(2) 0.0362(8) Uani 1 1 d . . .
C16 C 0.5248(2) 0.1994(2) 0.29865(19) 0.0398(8) Uani 1 1 d . . .
H16 H 0.5391 0.2139 0.3531 0.048 Uiso 1 1 calc R . .
N6 N 0.69872(16) 0.15394(18) 0.34602(19) 0.0466(7) Uani 1 1 d . . .
C17 C 0.9678(2) 0.1159(2) 0.4185(2) 0.0460(9) Uani 1 1 d . . .
H17 H 1.0278 0.1046 0.4360 0.055 Uiso 1 1 calc R . .
N7 N 0.24040(18) 0.3699(2) -0.01654(19) 0.0497(8) Uani 1 1 d . . .
C18 C 0.0996(2) 0.1226(2) 0.17075(19) 0.0425(8) Uani 1 1 d . . .
H18 H 0.1011 0.0864 0.2182 0.051 Uiso 1 1 calc R . .
C19 C 0.59097(19) 0.1722(2) 0.2496(2) 0.0362(8) Uani 1 1 d . . .
N8 N 0.68477(16) 0.16313(18) 0.27294(18) 0.0438(7) Uani 1 1 d . . .
N9 N -0.0960(2) 0.3937(2) 0.30971(18) 0.0604(8) Uani 1 1 d . . .
N10 N -0.0284(2) 0.3995(2) 0.3489(2) 0.0673(10) Uani 1 1 d . . .
C20 C 0.0224(2) 0.1866(2) 0.0569(2) 0.0529(10) Uani 1 1 d . . .
H20 H -0.0304 0.1943 0.0240 0.064 Uiso 1 1 calc R . .
C21 C 0.79323(19) 0.1437(2) 0.3681(2) 0.0396(9) Uani 1 1 d . . .
C22 C 0.57054(19) 0.1528(2) 0.1707(2) 0.0425(9) Uani 1 1 d . . .
H22 H 0.6166 0.1358 0.1367 0.051 Uiso 1 1 calc R . .
C23 C 0.2012(2) 0.3711(2) 0.2856(2) 0.0428(9) Uani 1 1 d . . .
H23 H 0.2575 0.3598 0.3120 0.051 Uiso 1 1 calc R . .
C24 C 0.0212(2) 0.1344(2) 0.1256(2) 0.0508(9) Uani 1 1 d . . .
H24 H -0.0325 0.1070 0.1417 0.061 Uiso 1 1 calc R . .
C25 C 0.8604(2) 0.1627(2) 0.3163(2) 0.0497(9) Uani 1 1 d . . .
H25 H 0.8463 0.1848 0.2637 0.060 Uiso 1 1 calc R . .
C26 C 0.4772(2) 0.3445(3) 0.0239(2) 0.0545(10) Uani 1 1 d . . .
H26 H 0.4701 0.3048 -0.0213 0.065 Uiso 1 1 calc R . .
C27 C 0.9008(2) 0.0992(2) 0.4687(2) 0.0520(10) Uani 1 1 d . . .
H27 H 0.9146 0.0774 0.5214 0.062 Uiso 1 1 calc R . .
C28 C 0.9483(2) 0.1489(2) 0.3429(2) 0.0497(9) Uani 1 1 d . . .
H28 H 0.9951 0.1623 0.3086 0.060 Uiso 1 1 calc R . .
C29 C -0.1750(3) 0.4062(3) 0.3631(3) 0.0601(11) Uani 1 1 d . . .
C30 C 0.8135(2) 0.1136(2) 0.4436(2) 0.0483(9) Uani 1 1 d . . .
H30 H 0.7673 0.1025 0.4792 0.058 Uiso 1 1 calc R . .
C31 C 0.5560(2) 0.3899(3) 0.0371(3) 0.0706(12) Uani 1 1 d . . .
H31 H 0.6022 0.3825 0.0009 0.085 Uiso 1 1 calc R . .
C32 C 0.4991(2) 0.4582(2) 0.1527(2) 0.0551(10) Uani 1 1 d . . .
H32 H 0.5055 0.4972 0.1984 0.066 Uiso 1 1 calc R . .
C33 C -0.3253(2) 0.4359(3) 0.4448(3) 0.0623(11) Uani 1 1 d . . .
H33 H -0.3786 0.4456 0.4717 0.075 Uiso 1 1 calc R . .
C34 C -0.2546(3) 0.3900(3) 0.3258(3) 0.0651(11) Uani 1 1 d . . .
H34 H -0.2587 0.3690 0.2720 0.078 Uiso 1 1 calc R . .
C35 C -0.3294(2) 0.4046(3) 0.3672(3) 0.0635(11) Uani 1 1 d . . .
H35 H -0.3860 0.3926 0.3415 0.076 Uiso 1 1 calc R . .
C36 C -0.2444(3) 0.4532(3) 0.4834(2) 0.0662(11) Uani 1 1 d . . .
H36 H -0.2411 0.4750 0.5370 0.079 Uiso 1 1 calc R . .
C37 C -0.1659(2) 0.4378(3) 0.4418(3) 0.0652(12) Uani 1 1 d . . .
H37 H -0.1088 0.4486 0.4668 0.078 Uiso 1 1 calc R . .
C38 C 0.5687(2) 0.4461(3) 0.1025(3) 0.0703(12) Uani 1 1 d . . .
H38 H 0.6241 0.4763 0.1133 0.084 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.958(3) . ?
Fe1 N5 1.967(3) . ?
Fe1 N1 2.010(2) . ?
Fe1 N4 2.021(2) . ?
Fe1 N3 2.045(2) . ?
Fe1 N2 2.056(2) . ?
S1 C3 1.648(4) . ?
S2 C12 1.631(4) . ?
N1 C10 1.332(4) . ?
N1 C6 1.349(4) . ?
N2 C4 1.278(3) . ?
N2 C1 1.440(4) . ?
C1 C23 1.376(4) . ?
C1 C8 1.384(4) . ?
C2 C14 1.383(4) . ?
C2 C11 1.385(4) . ?
C2 N3 1.435(3) . ?
C3 N7 1.155(4) . ?
N3 C5 1.283(3) . ?
C4 C15 1.451(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.457(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.338(4) . ?
N4 C15 1.347(4) . ?
N5 C12 1.157(4) . ?
C6 C18 1.380(4) . ?
C7 C8 1.374(4) . ?
C7 C9 1.376(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.370(5) . ?
C9 N10 1.526(4) . ?
C10 C20 1.379(4) . ?
C10 H10 0.9500 . ?
C11 C22 1.377(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.367(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.389(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.379(4) . ?
C16 C19 1.377(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.238(3) . ?
N6 C21 1.458(4) . ?
C17 C27 1.364(4) . ?
C17 C28 1.370(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.379(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.371(4) . ?
C19 N8 1.451(4) . ?
N9 N10 1.185(4) . ?
N9 C29 1.534(4) . ?
C20 C24 1.376(5) . ?
C20 H20 0.9500 . ?
C21 C30 1.358(4) . ?
C21 C25 1.390(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.389(4) . ?
C25 H25 0.9500 . ?
C26 C31 1.363(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.374(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.343(5) . ?
C29 C37 1.394(5) . ?
C30 H30 0.9500 . ?
C31 C38 1.369(5) . ?
C31 H31 0.9500 . ?
C32 C38 1.385(5) . ?
C32 H32 0.9500 . ?
C33 C36 1.373(5) . ?
C33 C35 1.374(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.367(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.418(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 91.99(12) . . ?
N7 Fe1 N1 94.14(11) . . ?
N5 Fe1 N1 94.97(10) . . ?
N7 Fe1 N4 93.01(10) . . ?
N5 Fe1 N4 92.84(11) . . ?
N1 Fe1 N4 169.22(10) . . ?
N7 Fe1 N3 172.23(10) . . ?
N5 Fe1 N3 91.58(10) . . ?
N1 Fe1 N3 78.67(10) . . ?
N4 Fe1 N3 93.70(10) . . ?
N7 Fe1 N2 93.39(10) . . ?
N5 Fe1 N2 170.08(10) . . ?
N1 Fe1 N2 92.95(9) . . ?
N4 Fe1 N2 78.57(10) . . ?
N3 Fe1 N2 84.12(9) . . ?
C10 N1 C6 117.6(3) . . ?
C10 N1 Fe1 127.2(2) . . ?
C6 N1 Fe1 115.01(18) . . ?
C4 N2 C1 118.0(2) . . ?
C4 N2 Fe1 114.41(19) . . ?
C1 N2 Fe1 126.87(19) . . ?
C23 C1 C8 120.0(3) . . ?
C23 C1 N2 121.2(3) . . ?
C8 C1 N2 118.8(3) . . ?
C14 C2 C11 120.3(3) . . ?
C14 C2 N3 121.5(3) . . ?
C11 C2 N3 118.1(3) . . ?
N7 C3 S1 178.4(3) . . ?
C5 N3 C2 119.8(3) . . ?
C5 N3 Fe1 114.61(19) . . ?
C2 N3 Fe1 125.23(19) . . ?
N2 C4 C15 117.6(3) . . ?
N2 C4 H4 121.2 . . ?
C15 C4 H4 121.2 . . ?
N3 C5 C6 116.9(3) . . ?
N3 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C26 N4 C15 117.6(3) . . ?
C26 N4 Fe1 127.2(2) . . ?
C15 N4 Fe1 115.19(18) . . ?
C12 N5 Fe1 166.8(3) . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 113.3(3) . . ?
C18 C6 C5 123.9(3) . . ?
C8 C7 C9 119.0(3) . . ?
C8 C7 H7 120.5 . . ?
C9 C7 H7 120.5 . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
C13 C9 C7 121.4(3) . . ?
C13 C9 N10 111.5(3) . . ?
C7 C9 N10 127.0(3) . . ?
N1 C10 C20 122.7(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 119.4(3) . . ?
C22 C11 H11 120.3 . . ?
C2 C11 H11 120.3 . . ?
N5 C12 S2 178.8(3) . . ?
C23 C13 C9 119.4(3) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.4(3) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
N4 C15 C32 122.9(3) . . ?
N4 C15 C4 113.5(3) . . ?
C32 C15 C4 123.6(3) . . ?
C19 C16 C14 120.2(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 112.1(3) . . ?
C27 C17 C28 120.0(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 170.7(3) . . ?
C24 C18 C6 118.8(3) . . ?
C24 C18 H18 120.6 . . ?
C6 C18 H18 120.6 . . ?
C22 C19 C16 119.9(3) . . ?
C22 C19 N8 114.2(3) . . ?
C16 C19 N8 125.9(3) . . ?
N6 N8 C19 113.0(3) . . ?
N10 N9 C29 109.7(3) . . ?
N9 N10 C9 105.7(3) . . ?
C24 C20 C10 119.4(3) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 120.5(3) . . ?
C30 C21 N6 116.0(3) . . ?
C25 C21 N6 123.5(3) . . ?
C19 C22 C11 120.8(3) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C13 C23 C1 120.2(3) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C20 C24 C18 118.6(3) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C28 C25 C21 118.8(3) . . ?
C28 C25 H25 120.6 . . ?
C21 C25 H25 120.6 . . ?
N4 C26 C31 122.5(4) . . ?
N4 C26 H26 118.7 . . ?
C31 C26 H26 118.7 . . ?
C17 C27 C30 120.6(3) . . ?
C17 C27 H27 119.7 . . ?
C30 C27 H27 119.7 . . ?
C17 C28 C25 120.1(3) . . ?
C17 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
C34 C29 C37 122.7(3) . . ?
C34 C29 N9 114.0(4) . . ?
C37 C29 N9 123.1(4) . . ?
C21 C30 C27 119.9(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C26 C31 C38 120.0(3) . . ?
C26 C31 H31 120.0 . . ?
C38 C31 H31 120.0 . . ?
C15 C32 C38 118.2(4) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C36 C33 C35 120.2(3) . . ?
C36 C33 H33 119.9 . . ?
C35 C33 H33 119.9 . . ?
C29 C34 C35 118.3(4) . . ?
C29 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
C34 C35 C33 122.0(4) . . ?
C34 C35 H35 119.0 . . ?
C33 C35 H35 119.0 . . ?
C33 C36 C37 118.7(4) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
C29 C37 C36 118.0(4) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
C31 C38 C32 118.8(3) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.846
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.846
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.035
####################################################################### 
# 
# 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_feaza240km1
_database_code_depnum_ccdc_archive 'CCDC 1492645'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
    bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1046(11)
_cell_length_b                   14.4631(11)
_cell_length_c                   16.9754(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.103(4)
_cell_angle_gamma                90.00
_cell_volume                     3703.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    4347
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5519
_exptl_absorpt_correction_T_max  0.8959
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
          its'aim being to analyse the evolution of partial collection of data, 
          always carried out over the same part of reciprocal space, 
          and over a large scale of temperature.
          This  explain the poor completness of data as well as the low theta(max) value, 
          the low number of unique reflexions collected.
          In ordre to obtain significant intensities with an exposure time relatively short, 
          a crystal of neutron size was used. As the aim is to compare the diffraction data 
          always obtained from the same part of the crystal at different temperature, 
          problems of intensity scale are not considered to be of prior importance.
          The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
          over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
          these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
          or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
          but modelling this two conformations is over the scope 
   of this study of partial data collections.
;

_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5833
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         21.23
_reflns_number_total             3476
_reflns_number_gt                2767
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0295P)²+1.9724P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3476
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0775
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29094(3) 0.28727(4) 0.05665(3) 0.0500(2) Uani 1 1 d . . .
S1 S 0.18959(6) 0.49753(8) -0.14670(6) 0.0633(3) Uani 1 1 d . . .
S2 S 0.43609(7) 0.07291(8) -0.10641(6) 0.0703(3) Uani 1 1 d . . .
N1 N 0.17151(17) 0.21601(19) 0.07893(17) 0.0473(7) Uani 1 1 d . . .
N2 N 0.27292(17) 0.37953(18) 0.16021(14) 0.0396(7) Uani 1 1 d . . .
C1 C 0.1972(2) 0.3850(2) 0.2070(2) 0.0399(9) Uani 1 1 d . . .
C2 C 0.4141(2) 0.1812(2) 0.1910(2) 0.0457(9) Uani 1 1 d . . .
C3 C 0.2136(2) 0.4258(3) -0.0752(2) 0.0510(10) Uani 1 1 d . . .
N3 N 0.32749(18) 0.19095(18) 0.15452(15) 0.0443(7) Uani 1 1 d . . .
C4 C 0.3443(2) 0.4200(2) 0.1846(2) 0.0465(9) Uani 1 1 d . . .
H4 H 0.3459 0.4545 0.2316 0.056 Uiso 1 1 calc R . .
C5 C 0.2613(2) 0.1520(2) 0.1839(2) 0.0483(9) Uani 1 1 d . . .
H5 H 0.2689 0.1157 0.2297 0.058 Uiso 1 1 calc R . .
N4 N 0.41392(17) 0.3605(2) 0.07421(19) 0.0551(8) Uani 1 1 d . . .
N5 N 0.3406(2) 0.2019(3) -0.0261(2) 0.0734(10) Uani 1 1 d . . .
C6 C 0.1732(2) 0.1644(2) 0.1453(2) 0.0462(9) Uani 1 1 d . . .
C7 C 0.0408(2) 0.4033(2) 0.2113(3) 0.0592(11) Uani 1 1 d . . .
H7 H -0.0151 0.4133 0.1856 0.071 Uiso 1 1 calc R . .
C8 C 0.1157(2) 0.3995(2) 0.1690(2) 0.0497(9) Uani 1 1 d . . .
H8 H 0.1112 0.4067 0.1139 0.060 Uiso 1 1 calc R . .
C9 C 0.0489(3) 0.3923(3) 0.2917(3) 0.0663(12) Uani 1 1 d . . .
C10 C 0.0938(3) 0.2252(3) 0.0389(2) 0.0614(11) Uani 1 1 d . . .
H10 H 0.0917 0.2595 -0.0082 0.074 Uiso 1 1 calc R . .
C11 C 0.4822(2) 0.1576(3) 0.1437(2) 0.0584(10) Uani 1 1 d . . .
H11 H 0.4696 0.1448 0.0900 0.070 Uiso 1 1 calc R . .
C12 C 0.3803(2) 0.1481(3) -0.0598(2) 0.0523(10) Uani 1 1 d . . .
C13 C 0.1300(3) 0.3775(3) 0.3301(2) 0.0702(12) Uani 1 1 d . . .
H13 H 0.1346 0.3703 0.3852 0.084 Uiso 1 1 calc R . .
C14 C 0.4329(2) 0.2011(2) 0.2697(2) 0.0564(10) Uani 1 1 d . . .
H14 H 0.3874 0.2180 0.3024 0.068 Uiso 1 1 calc R . .
C15 C 0.4234(2) 0.4126(3) 0.1396(2) 0.0512(10) Uani 1 1 d . . .
C16 C 0.5207(3) 0.1957(3) 0.2998(2) 0.0646(11) Uani 1 1 d . . .
H16 H 0.5344 0.2090 0.3532 0.078 Uiso 1 1 calc R . .
N6 N 0.6943(2) 0.1535(2) 0.3440(3) 0.0776(10) Uani 1 1 d . . .
C17 C 0.9639(3) 0.1174(3) 0.4185(3) 0.0670(11) Uani 1 1 d . . .
H17 H 1.0228 0.1073 0.4372 0.080 Uiso 1 1 calc R . .
N7 N 0.2303(2) 0.3752(2) -0.0234(2) 0.0670(10) Uani 1 1 d . . .
C18 C 0.0982(2) 0.1250(3) 0.1729(2) 0.0619(10) Uani 1 1 d . . .
H18 H 0.1014 0.0906 0.2200 0.074 Uiso 1 1 calc R . .
C19 C 0.5871(2) 0.1710(3) 0.2518(3) 0.0614(11) Uani 1 1 d . . .
N8 N 0.6848(2) 0.1626(2) 0.2748(2) 0.0726(10) Uani 1 1 d . . .
N9 N -0.0854(3) 0.3952(2) 0.3133(2) 0.0822(11) Uani 1 1 d . . .
N10 N -0.0261(3) 0.4014(2) 0.3553(3) 0.0985(15) Uani 1 1 d . . .
C20 C 0.0160(3) 0.1868(3) 0.0630(3) 0.0764(13) Uani 1 1 d . . .
H20 H -0.0376 0.1953 0.0331 0.092 Uiso 1 1 calc R . .
C21 C 0.7919(2) 0.1429(3) 0.3664(3) 0.0645(12) Uani 1 1 d . . .
C22 C 0.5682(2) 0.1528(3) 0.1743(3) 0.0653(11) Uani 1 1 d . . .
H22 H 0.6140 0.1369 0.1415 0.078 Uiso 1 1 calc R . .
C23 C 0.2032(2) 0.3733(3) 0.2875(2) 0.0580(10) Uani 1 1 d . . .
H23 H 0.2588 0.3623 0.3134 0.070 Uiso 1 1 calc R . .
C24 C 0.0183(3) 0.1364(3) 0.1309(3) 0.0745(12) Uani 1 1 d . . .
H24 H -0.0338 0.1098 0.1488 0.089 Uiso 1 1 calc R . .
C25 C 0.8585(3) 0.1622(3) 0.3157(3) 0.0747(12) Uani 1 1 d . . .
H25 H 0.8449 0.1835 0.2642 0.090 Uiso 1 1 calc R . .
C26 C 0.4836(3) 0.3544(3) 0.0298(3) 0.0821(13) Uani 1 1 d . . .
H26 H 0.4784 0.3191 -0.0167 0.099 Uiso 1 1 calc R . .
C27 C 0.8972(3) 0.1008(3) 0.4657(3) 0.0783(13) Uani 1 1 d . . .
H27 H 0.9101 0.0800 0.5175 0.094 Uiso 1 1 calc R . .
C28 C 0.9465(3) 0.1489(3) 0.3435(3) 0.0749(12) Uani 1 1 d . . .
H28 H 0.9932 0.1617 0.3108 0.090 Uiso 1 1 calc R . .
C29 C -0.1646(4) 0.4086(3) 0.3723(4) 0.0894(17) Uani 1 1 d . . .
C30 C 0.8115(3) 0.1135(3) 0.4401(3) 0.0786(13) Uani 1 1 d . . .
H30 H 0.7658 0.1017 0.4742 0.094 Uiso 1 1 calc R . .
C31 C 0.5629(3) 0.3975(4) 0.0493(4) 0.1127(19) Uani 1 1 d . . .
H31 H 0.6106 0.3917 0.0163 0.135 Uiso 1 1 calc R . .
C32 C 0.5014(3) 0.4559(3) 0.1626(3) 0.0772(12) Uani 1 1 d . . .
H32 H 0.5061 0.4902 0.2097 0.093 Uiso 1 1 calc R . .
C33 C -0.3159(3) 0.4372(3) 0.4500(3) 0.0826(13) Uani 1 1 d . . .
H33 H -0.3688 0.4466 0.4756 0.099 Uiso 1 1 calc R . .
C34 C -0.2438(4) 0.3901(3) 0.3358(3) 0.0893(15) Uani 1 1 d . . .
H34 H -0.2473 0.3679 0.2837 0.107 Uiso 1 1 calc R . .
C35 C -0.3185(3) 0.4036(3) 0.3748(3) 0.0819(13) Uani 1 1 d . . .
H35 H -0.3737 0.3895 0.3494 0.098 Uiso 1 1 calc R . .
C36 C -0.2360(3) 0.4572(3) 0.4881(3) 0.0897(14) Uani 1 1 d . . .
H36 H -0.2336 0.4802 0.5400 0.108 Uiso 1 1 calc R . .
C37 C -0.1576(3) 0.4429(3) 0.4487(4) 0.0895(15) Uani 1 1 d . . .
H37 H -0.1019 0.4562 0.4735 0.107 Uiso 1 1 calc R . .
C38 C 0.5722(3) 0.4485(4) 0.1164(4) 0.1088(18) Uani 1 1 d . . .
H38 H 0.6261 0.4780 0.1307 0.131 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 2.042(4) . ?
Fe1 N5 2.043(4) . ?
Fe1 N1 2.129(3) . ?
Fe1 N4 2.145(3) . ?
Fe1 N3 2.215(3) . ?
Fe1 N2 2.235(3) . ?
S1 C3 1.623(5) . ?
S2 C12 1.610(5) . ?
N1 C10 1.331(4) . ?
N1 C6 1.351(4) . ?
N2 C4 1.276(4) . ?
N2 C1 1.430(4) . ?
C1 C8 1.375(4) . ?
C1 C23 1.375(4) . ?
C2 C14 1.380(4) . ?
C2 C11 1.382(4) . ?
C2 N3 1.424(4) . ?
C3 N7 1.160(4) . ?
N3 C5 1.273(4) . ?
C4 C15 1.456(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.462(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.330(4) . ?
N4 C15 1.343(4) . ?
N5 C12 1.154(4) . ?
C6 C18 1.372(5) . ?
C7 C8 1.373(5) . ?
C7 C9 1.373(5) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.373(5) . ?
C9 N10 1.612(5) . ?
C10 C20 1.381(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.374(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.355(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.398(5) . ?
C14 H14 0.9400 . ?
C15 C32 1.373(5) . ?
C16 C19 1.372(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.184(4) . ?
N6 C21 1.510(5) . ?
C17 C27 1.343(5) . ?
C17 C28 1.364(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.379(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.356(5) . ?
C19 N8 1.511(5) . ?
N9 N10 1.118(4) . ?
N9 C29 1.614(5) . ?
C20 C24 1.363(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.340(5) . ?
C21 C25 1.387(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.400(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.375(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.355(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.344(7) . ?
C29 C37 1.388(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.358(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.364(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.364(6) . ?
C33 C36 1.368(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.353(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.408(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N7 Fe1 N5 94.95(13) . . ?
N7 Fe1 N1 93.77(12) . . ?
N5 Fe1 N1 100.12(12) . . ?
N7 Fe1 N4 97.98(12) . . ?
N5 Fe1 N4 92.68(13) . . ?
N1 Fe1 N4 161.80(12) . . ?
N7 Fe1 N3 167.32(12) . . ?
N5 Fe1 N3 92.88(12) . . ?
N1 Fe1 N3 75.01(11) . . ?
N4 Fe1 N3 91.58(11) . . ?
N7 Fe1 N2 94.73(11) . . ?
N5 Fe1 N2 165.11(11) . . ?
N1 Fe1 N2 90.50(10) . . ?
N4 Fe1 N2 74.77(11) . . ?
N3 Fe1 N2 79.72(9) . . ?
C10 N1 C6 117.2(3) . . ?
C10 N1 Fe1 126.4(3) . . ?
C6 N1 Fe1 116.0(2) . . ?
C4 N2 C1 118.8(3) . . ?
C4 N2 Fe1 113.1(2) . . ?
C1 N2 Fe1 127.3(2) . . ?
C8 C1 C23 119.6(3) . . ?
C8 C1 N2 118.0(3) . . ?
C23 C1 N2 122.3(3) . . ?
C14 C2 C11 119.5(3) . . ?
C14 C2 N3 122.4(3) . . ?
C11 C2 N3 117.8(3) . . ?
N7 C3 S1 179.2(4) . . ?
C5 N3 C2 120.6(3) . . ?
C5 N3 Fe1 113.8(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 119.9(3) . . ?
N2 C4 H4 120.1 . . ?
C15 C4 H4 120.1 . . ?
N3 C5 C6 119.0(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C26 N4 C15 117.0(3) . . ?
C26 N4 Fe1 126.4(3) . . ?
C15 N4 Fe1 116.4(2) . . ?
C12 N5 Fe1 165.7(3) . . ?
N1 C6 C18 122.4(3) . . ?
N1 C6 C5 114.7(3) . . ?
C18 C6 C5 122.9(4) . . ?
C8 C7 C9 118.9(3) . . ?
C8 C7 H7 120.6 . . ?
C9 C7 H7 120.6 . . ?
C7 C8 C1 120.2(3) . . ?
C7 C8 H8 119.9 . . ?
C1 C8 H8 119.9 . . ?
C13 C9 C7 121.3(3) . . ?
C13 C9 N10 109.6(4) . . ?
C7 C9 N10 128.9(4) . . ?
N1 C10 C20 123.3(4) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
C22 C11 C2 120.7(3) . . ?
C22 C11 H11 119.6 . . ?
C2 C11 H11 119.6 . . ?
N5 C12 S2 179.7(4) . . ?
C23 C13 C9 119.1(4) . . ?
C23 C13 H13 120.5 . . ?
C9 C13 H13 120.5 . . ?
C2 C14 C16 118.9(3) . . ?
C2 C14 H14 120.6 . . ?
C16 C14 H14 120.6 . . ?
N4 C15 C32 122.8(3) . . ?
N4 C15 C4 114.9(3) . . ?
C32 C15 C4 122.3(4) . . ?
C19 C16 C14 120.5(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 108.9(4) . . ?
C27 C17 C28 120.2(4) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 165.5(3) . . ?
C6 C18 C24 119.3(4) . . ?
C6 C18 H18 120.3 . . ?
C24 C18 H18 120.3 . . ?
C22 C19 C16 120.2(3) . . ?
C22 C19 N8 112.7(4) . . ?
C16 C19 N8 127.0(4) . . ?
N6 N8 C19 109.2(4) . . ?
N10 N9 C29 100.9(5) . . ?
N9 N10 C9 97.7(4) . . ?
C24 C20 C10 118.9(4) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.6 . . ?
C30 C21 C25 120.8(4) . . ?
C30 C21 N6 115.5(4) . . ?
C25 C21 N6 123.7(4) . . ?
C19 C22 C11 120.1(4) . . ?
C19 C22 H22 119.9 . . ?
C11 C22 H22 119.9 . . ?
C13 C23 C1 120.9(3) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.1(4) . . ?
C21 C25 H25 120.9 . . ?
C28 C25 H25 120.9 . . ?
N4 C26 C31 122.6(5) . . ?
N4 C26 H26 118.7 . . ?
C31 C26 H26 118.7 . . ?
C17 C27 C30 121.3(4) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C17 C28 C25 119.5(4) . . ?
C17 C28 H28 120.3 . . ?
C25 C28 H28 120.3 . . ?
C34 C29 C37 121.6(4) . . ?
C34 C29 N9 111.2(5) . . ?
C37 C29 N9 126.9(5) . . ?
C21 C30 C27 120.1(4) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C38 C31 C26 119.8(4) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C38 C32 C15 119.3(5) . . ?
C38 C32 H32 120.4 . . ?
C15 C32 H32 120.4 . . ?
C35 C33 C36 119.9(4) . . ?
C35 C33 H33 120.1 . . ?
C36 C33 H33 120.1 . . ?
C29 C34 C35 119.4(5) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 121.8(5) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C33 C36 C37 119.2(5) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C29 C37 C36 118.2(4) . . ?
C29 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?
C31 C38 C32 118.4(5) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.846
_diffrn_reflns_theta_full        21.23
_diffrn_measured_fraction_theta_full 0.846
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza225kd2
_database_code_depnum_ccdc_archive 'CCDC 1492646'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
     bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0984(6)
_cell_length_b                   14.4452(9)
_cell_length_c                   16.9444(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.086(3)
_cell_angle_gamma                90.00
_cell_volume                     3690.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    225(2)
_cell_measurement_reflns_used    4239
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      21.261

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_T_max  0.8955
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
          its'aim being to analyse the evolution of partial collection of data, 
          always carried out over the same part of reciprocal space, 
          and over a large scale of temperature.
          This  explain the poor completness of data as well as the low theta(max) value, 
          the low number of unique reflexions collected.
          In ordre to obtain significant intensities with an exposure time relatively short, 
          a crystal of neutron size was used. As the aim is to compare the diffraction data 
          always obtained from the same part of the crystal at different temperature, 
          problems of intensity scale are not considered to be of prior importance.
          The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
          over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
          these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
          or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
          but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      225(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5402
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         21.25
_reflns_number_total             3759
_reflns_number_gt                3069
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0190P)²+2.6586P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3759
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0818
_refine_ls_wR_factor_gt          0.0750
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29089(3) 0.28703(3) 0.05757(3) 0.04742(18) Uani 1 1 d . . .
S1 S 0.19025(6) 0.49712(7) -0.14656(6) 0.0605(3) Uani 1 1 d . . .
S2 S 0.43509(6) 0.07312(7) -0.10675(6) 0.0661(3) Uani 1 1 d . . .
N1 N 0.17214(18) 0.21635(17) 0.07927(17) 0.0458(7) Uani 1 1 d . . .
N2 N 0.27273(16) 0.37933(16) 0.15978(14) 0.0366(6) Uani 1 1 d . . .
C1 C 0.1970(2) 0.38455(19) 0.20624(19) 0.0378(8) Uani 1 1 d . . .
C2 C 0.4147(2) 0.1817(2) 0.1907(2) 0.0433(8) Uani 1 1 d . . .
C3 C 0.2146(2) 0.4251(3) -0.0746(2) 0.0510(9) Uani 1 1 d . . .
N3 N 0.32748(18) 0.19118(16) 0.15456(15) 0.0409(7) Uani 1 1 d . . .
C4 C 0.3436(2) 0.4205(2) 0.1844(2) 0.0447(8) Uani 1 1 d . . .
H4 H 0.3449 0.4555 0.2312 0.054 Uiso 1 1 calc R . .
C5 C 0.2616(2) 0.1520(2) 0.1844(2) 0.0448(8) Uani 1 1 d . . .
H5 H 0.2693 0.1159 0.2304 0.054 Uiso 1 1 calc R . .
N4 N 0.41307(16) 0.35951(19) 0.07380(17) 0.0501(7) Uani 1 1 d . . .
N5 N 0.3393(2) 0.2017(2) -0.02500(19) 0.0692(9) Uani 1 1 d . . .
C6 C 0.1738(2) 0.1643(2) 0.1455(2) 0.0436(8) Uani 1 1 d . . .
C7 C 0.0404(2) 0.4034(2) 0.2118(3) 0.0568(10) Uani 1 1 d . . .
H7 H -0.0157 0.4138 0.1865 0.068 Uiso 1 1 calc R . .
C8 C 0.1151(2) 0.3993(2) 0.1684(2) 0.0466(9) Uani 1 1 d . . .
H8 H 0.1101 0.4066 0.1132 0.056 Uiso 1 1 calc R . .
C9 C 0.0488(3) 0.3921(2) 0.2926(3) 0.0628(11) Uani 1 1 d . . .
C10 C 0.0946(3) 0.2256(2) 0.0382(2) 0.0590(10) Uani 1 1 d . . .
H10 H 0.0928 0.2598 -0.0091 0.071 Uiso 1 1 calc R . .
C11 C 0.4822(2) 0.1575(2) 0.1425(2) 0.0548(9) Uani 1 1 d . . .
H11 H 0.4694 0.1445 0.0887 0.066 Uiso 1 1 calc R . .
C12 C 0.3791(2) 0.1479(2) -0.0594(2) 0.0497(9) Uani 1 1 d . . .
C13 C 0.1299(3) 0.3770(3) 0.3303(2) 0.0654(10) Uani 1 1 d . . .
H13 H 0.1349 0.3697 0.3855 0.078 Uiso 1 1 calc R . .
C14 C 0.4340(2) 0.2018(2) 0.2693(2) 0.0533(9) Uani 1 1 d . . .
H14 H 0.3886 0.2190 0.3021 0.064 Uiso 1 1 calc R . .
C15 C 0.4228(2) 0.4126(2) 0.1390(2) 0.0478(9) Uani 1 1 d . . .
C16 C 0.5216(3) 0.1963(2) 0.2999(2) 0.0599(10) Uani 1 1 d . . .
H16 H 0.5354 0.2097 0.3534 0.072 Uiso 1 1 calc R . .
N6 N 0.6947(2) 0.1534(2) 0.3447(2) 0.0704(9) Uani 1 1 d . . .
C17 C 0.9645(2) 0.1171(2) 0.4180(3) 0.0616(10) Uani 1 1 d . . .
H17 H 1.0237 0.1064 0.4358 0.074 Uiso 1 1 calc R . .
N7 N 0.2312(2) 0.3747(2) -0.0225(2) 0.0659(9) Uani 1 1 d . . .
C18 C 0.0984(2) 0.1248(2) 0.1733(2) 0.0563(10) Uani 1 1 d . . .
H18 H 0.1014 0.0902 0.2204 0.068 Uiso 1 1 calc R . .
C19 C 0.5875(2) 0.1713(2) 0.2514(3) 0.0550(10) Uani 1 1 d . . .
N8 N 0.6846(2) 0.16274(19) 0.2749(2) 0.0648(9) Uani 1 1 d . . .
N9 N -0.0872(3) 0.3951(2) 0.3135(2) 0.0793(11) Uani 1 1 d . . .
N10 N -0.0266(3) 0.4013(2) 0.3546(3) 0.0911(13) Uani 1 1 d . . .
C20 C 0.0168(3) 0.1868(3) 0.0625(3) 0.0714(12) Uani 1 1 d . . .
H20 H -0.0366 0.1948 0.0322 0.086 Uiso 1 1 calc R . .
C21 C 0.7920(2) 0.1428(2) 0.3672(3) 0.0584(11) Uani 1 1 d . . .
C22 C 0.5681(2) 0.1528(2) 0.1736(3) 0.0616(10) Uani 1 1 d . . .
H22 H 0.6139 0.1367 0.1408 0.074 Uiso 1 1 calc R . .
C23 C 0.2031(2) 0.3727(2) 0.2872(2) 0.0560(9) Uani 1 1 d . . .
H23 H 0.2588 0.3615 0.3129 0.067 Uiso 1 1 calc R . .
C24 C 0.0184(2) 0.1368(3) 0.1309(3) 0.0681(11) Uani 1 1 d . . .
H24 H -0.0340 0.1110 0.1489 0.082 Uiso 1 1 calc R . .
C25 C 0.8582(3) 0.1622(2) 0.3162(3) 0.0699(11) Uani 1 1 d . . .
H25 H 0.8442 0.1834 0.2646 0.084 Uiso 1 1 calc R . .
C26 C 0.4819(3) 0.3523(3) 0.0282(3) 0.0779(12) Uani 1 1 d . . .
H26 H 0.4759 0.3162 -0.0179 0.093 Uiso 1 1 calc R . .
C27 C 0.8983(3) 0.1002(3) 0.4666(3) 0.0718(11) Uani 1 1 d . . .
H27 H 0.9119 0.0790 0.5183 0.086 Uiso 1 1 calc R . .
C28 C 0.9462(3) 0.1494(3) 0.3434(3) 0.0686(11) Uani 1 1 d . . .
H28 H 0.9926 0.1631 0.3105 0.082 Uiso 1 1 calc R . .
C29 C -0.1660(3) 0.4083(3) 0.3706(4) 0.0844(16) Uani 1 1 d . . .
C30 C 0.8118(3) 0.1136(3) 0.4417(3) 0.0745(12) Uani 1 1 d . . .
H30 H 0.7663 0.1026 0.4762 0.089 Uiso 1 1 calc R . .
C31 C 0.5609(3) 0.3957(4) 0.0462(4) 0.1053(17) Uani 1 1 d . . .
H31 H 0.6078 0.3899 0.0121 0.126 Uiso 1 1 calc R . .
C32 C 0.5015(2) 0.4566(3) 0.1614(3) 0.0753(12) Uani 1 1 d . . .
H32 H 0.5068 0.4918 0.2081 0.090 Uiso 1 1 calc R . .
C33 C -0.3166(3) 0.4371(3) 0.4500(3) 0.0778(12) Uani 1 1 d . . .
H33 H -0.3694 0.4462 0.4759 0.093 Uiso 1 1 calc R . .
C34 C -0.2451(3) 0.3899(3) 0.3351(3) 0.0839(14) Uani 1 1 d . . .
H34 H -0.2488 0.3674 0.2830 0.101 Uiso 1 1 calc R . .
C35 C -0.3194(3) 0.4034(3) 0.3741(3) 0.0779(12) Uani 1 1 d . . .
H35 H -0.3747 0.3894 0.3487 0.094 Uiso 1 1 calc R . .
C36 C -0.2360(3) 0.4574(3) 0.4877(3) 0.0863(13) Uani 1 1 d . . .
H36 H -0.2330 0.4810 0.5395 0.104 Uiso 1 1 calc R . .
C37 C -0.1581(3) 0.4421(3) 0.4474(4) 0.0862(14) Uani 1 1 d . . .
H37 H -0.1020 0.4546 0.4720 0.103 Uiso 1 1 calc R . .
C38 C 0.5720(3) 0.4474(4) 0.1135(4) 0.1016(17) Uani 1 1 d . . .
H38 H 0.6265 0.4762 0.1269 0.122 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.030(4) . ?
Fe1 N7 2.031(3) . ?
Fe1 N1 2.113(3) . ?
Fe1 N4 2.126(3) . ?
Fe1 N3 2.197(3) . ?
Fe1 N2 2.214(2) . ?
S1 C3 1.629(4) . ?
S2 C12 1.612(4) . ?
N1 C10 1.336(4) . ?
N1 C6 1.350(4) . ?
N2 C4 1.274(4) . ?
N2 C1 1.425(4) . ?
C1 C8 1.379(4) . ?
C1 C23 1.380(4) . ?
C2 C14 1.379(4) . ?
C2 C11 1.386(4) . ?
C2 N3 1.428(4) . ?
C3 N7 1.162(4) . ?
N3 C5 1.273(4) . ?
C4 C15 1.461(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.459(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.331(4) . ?
N4 C15 1.346(4) . ?
N5 C12 1.159(4) . ?
C6 C18 1.378(4) . ?
C7 C9 1.379(5) . ?
C7 C8 1.380(4) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.367(5) . ?
C9 N10 1.596(5) . ?
C10 C20 1.384(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.375(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.360(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.396(4) . ?
C14 H14 0.9400 . ?
C15 C32 1.382(5) . ?
C16 C19 1.372(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.191(4) . ?
N6 C21 1.505(4) . ?
C17 C27 1.352(5) . ?
C17 C28 1.361(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.383(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.361(5) . ?
C19 N8 1.503(4) . ?
N9 N10 1.124(4) . ?
N9 C29 1.585(5) . ?
C20 C24 1.365(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.348(5) . ?
C21 C25 1.385(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.396(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.368(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.363(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.334(6) . ?
C29 C37 1.389(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.367(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.379(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.373(6) . ?
C33 C36 1.375(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.347(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.409(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 94.65(13) . . ?
N5 Fe1 N1 99.63(11) . . ?
N7 Fe1 N1 93.86(12) . . ?
N5 Fe1 N4 92.63(12) . . ?
N7 Fe1 N4 97.48(11) . . ?
N1 Fe1 N4 162.56(11) . . ?
N5 Fe1 N3 92.73(11) . . ?
N7 Fe1 N3 167.81(11) . . ?
N1 Fe1 N3 75.33(11) . . ?
N4 Fe1 N3 91.84(10) . . ?
N5 Fe1 N2 165.68(11) . . ?
N7 Fe1 N2 94.48(11) . . ?
N1 Fe1 N2 90.73(10) . . ?
N4 Fe1 N2 75.25(10) . . ?
N3 Fe1 N2 80.27(9) . . ?
C10 N1 C6 117.7(3) . . ?
C10 N1 Fe1 126.1(2) . . ?
C6 N1 Fe1 115.9(2) . . ?
C4 N2 C1 118.6(3) . . ?
C4 N2 Fe1 113.6(2) . . ?
C1 N2 Fe1 126.9(2) . . ?
C8 C1 C23 119.5(3) . . ?
C8 C1 N2 118.5(3) . . ?
C23 C1 N2 121.9(3) . . ?
C14 C2 C11 119.9(3) . . ?
C14 C2 N3 122.5(3) . . ?
C11 C2 N3 117.5(3) . . ?
N7 C3 S1 178.9(3) . . ?
C5 N3 C2 120.6(3) . . ?
C5 N3 Fe1 114.0(2) . . ?
C2 N3 Fe1 124.8(2) . . ?
N2 C4 C15 119.2(3) . . ?
N2 C4 H4 120.4 . . ?
C15 C4 H4 120.4 . . ?
N3 C5 C6 118.5(3) . . ?
N3 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C26 N4 C15 117.8(3) . . ?
C26 N4 Fe1 125.8(3) . . ?
C15 N4 Fe1 116.3(2) . . ?
C12 N5 Fe1 165.9(3) . . ?
N1 C6 C18 122.4(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.8(3) . . ?
C9 C7 C8 119.4(3) . . ?
C9 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C1 C8 C7 119.8(3) . . ?
C1 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C13 C9 C7 121.0(3) . . ?
C13 C9 N10 111.0(4) . . ?
C7 C9 N10 127.9(4) . . ?
N1 C10 C20 122.6(3) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
C22 C11 C2 119.7(3) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
N5 C12 S2 179.6(4) . . ?
C23 C13 C9 119.4(4) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.6(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 122.8(3) . . ?
N4 C15 C4 114.9(3) . . ?
C32 C15 C4 122.3(4) . . ?
C19 C16 C14 119.7(3) . . ?
C19 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
N8 N6 C21 109.6(3) . . ?
C27 C17 C28 120.5(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C3 N7 Fe1 165.6(3) . . ?
C6 C18 C24 119.0(3) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.4(3) . . ?
C22 C19 N8 113.4(3) . . ?
C16 C19 N8 126.2(4) . . ?
N6 N8 C19 110.2(3) . . ?
N10 N9 C29 102.9(5) . . ?
N9 N10 C9 99.8(4) . . ?
C24 C20 C10 119.4(3) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 121.1(3) . . ?
C30 C21 N6 115.7(4) . . ?
C25 C21 N6 123.2(4) . . ?
C19 C22 C11 120.7(3) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C13 C23 C1 121.0(3) . . ?
C13 C23 H23 119.5 . . ?
C1 C23 H23 119.5 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.3(4) . . ?
C21 C25 H25 120.9 . . ?
C28 C25 H25 120.9 . . ?
N4 C26 C31 122.3(4) . . ?
N4 C26 H26 118.9 . . ?
C31 C26 H26 118.9 . . ?
C17 C27 C30 120.8(4) . . ?
C17 C27 H27 119.6 . . ?
C30 C27 H27 119.6 . . ?
C17 C28 C25 119.6(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 121.5(4) . . ?
C34 C29 N9 112.5(5) . . ?
C37 C29 N9 125.8(5) . . ?
C21 C30 C27 119.7(4) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C38 C31 C26 120.1(4) . . ?
C38 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?
C38 C32 C15 118.3(4) . . ?
C38 C32 H32 120.9 . . ?
C15 C32 H32 120.9 . . ?
C35 C33 C36 119.5(4) . . ?
C35 C33 H33 120.2 . . ?
C36 C33 H33 120.2 . . ?
C29 C34 C35 119.9(5) . . ?
C29 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C33 121.7(4) . . ?
C34 C35 H35 119.2 . . ?
C33 C35 H35 119.2 . . ?
C33 C36 C37 118.9(5) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C29 C37 C36 118.5(4) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 118.7(4) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.915
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.915
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza195km2
_database_code_depnum_ccdc_archive 'CCDC 1492647'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
   bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0676(7)
_cell_length_b                   14.4217(10)
_cell_length_c                   16.8187(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.929(4)
_cell_angle_gamma                90.00
_cell_volume                     3649.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    195(2)
_cell_measurement_reflns_used    5573
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5477
_exptl_absorpt_correction_T_max  0.8945
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                   its'aim being to analyse the evolution of partial collection of data, 
                   always carried out over the same part of reciprocal space, 
                   and over a large scale of temperature.
                   This  explain the poor completness of data as well as the low theta(max) value, 
                   the low number of unique reflexions collected.
                   In ordre to obtain significant intensities with an exposure time relatively short, 
                   a crystal of neutron size was used. As the aim is to compare the diffraction data 
                   always obtained from the same part of the crystal at different temperature, 
                   problems of intensity scale are not considered to be of prior importance.
                   The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                   over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                   these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                   or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                   but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      195(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5767
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         22.98
_reflns_number_total             4121
_reflns_number_gt                3312
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0207P)²+2.7841P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4121
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0848
_refine_ls_wR_factor_gt          0.0779
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29169(3) 0.28593(3) 0.06181(3) 0.04244(17) Uani 1 1 d . . .
S1 S 0.19263(5) 0.49309(7) -0.14486(5) 0.0550(3) Uani 1 1 d . . .
S2 S 0.43016(6) 0.07388(6) -0.10779(6) 0.0586(3) Uani 1 1 d . . .
N1 N 0.17506(17) 0.21764(16) 0.07952(15) 0.0392(6) Uani 1 1 d . . .
N2 N 0.27251(15) 0.37755(15) 0.15812(14) 0.0319(6) Uani 1 1 d . . .
C1 C 0.19560(18) 0.38345(18) 0.20471(18) 0.0335(7) Uani 1 1 d . . .
C2 C 0.41625(19) 0.18345(19) 0.18964(19) 0.0358(8) Uani 1 1 d . . .
C3 C 0.2188(2) 0.4214(2) -0.0716(2) 0.0468(9) Uani 1 1 d . . .
N3 N 0.32834(16) 0.19323(16) 0.15459(14) 0.0356(6) Uani 1 1 d . . .
C4 C 0.3426(2) 0.4214(2) 0.18214(19) 0.0383(8) Uani 1 1 d . . .
H4 H 0.3432 0.4590 0.2286 0.046 Uiso 1 1 calc R . .
C5 C 0.2630(2) 0.1524(2) 0.18472(19) 0.0381(8) Uani 1 1 d . . .
H5 H 0.2713 0.1154 0.2312 0.046 Uiso 1 1 calc R . .
N4 N 0.41075(15) 0.35616(17) 0.07253(16) 0.0426(7) Uani 1 1 d . . .
N5 N 0.3358(2) 0.2004(2) -0.02043(19) 0.0611(8) Uani 1 1 d . . .
C6 C 0.1752(2) 0.16439(19) 0.14560(19) 0.0372(8) Uani 1 1 d . . .
C7 C 0.0387(2) 0.4031(2) 0.2103(2) 0.0487(9) Uani 1 1 d . . .
H7 H -0.0179 0.4140 0.1846 0.058 Uiso 1 1 calc R . .
C8 C 0.1139(2) 0.39860(19) 0.1660(2) 0.0408(8) Uani 1 1 d . . .
H8 H 0.1091 0.4058 0.1098 0.049 Uiso 1 1 calc R . .
C9 C 0.0465(2) 0.3918(2) 0.2917(2) 0.0519(10) Uani 1 1 d . . .
C10 C 0.0982(2) 0.2267(2) 0.0370(2) 0.0511(9) Uani 1 1 d . . .
H10 H 0.0973 0.2623 -0.0106 0.061 Uiso 1 1 calc R . .
C11 C 0.4834(2) 0.1578(2) 0.1410(2) 0.0479(9) Uani 1 1 d . . .
H11 H 0.4698 0.1435 0.0866 0.057 Uiso 1 1 calc R . .
C12 C 0.3744(2) 0.1475(2) -0.0575(2) 0.0457(8) Uani 1 1 d . . .
C13 C 0.1275(2) 0.3768(2) 0.3297(2) 0.0587(10) Uani 1 1 d . . .
H13 H 0.1323 0.3700 0.3859 0.070 Uiso 1 1 calc R . .
C14 C 0.4364(2) 0.2044(2) 0.2687(2) 0.0447(8) Uani 1 1 d . . .
H14 H 0.3908 0.2227 0.3024 0.054 Uiso 1 1 calc R . .
C15 C 0.42128(19) 0.4121(2) 0.1363(2) 0.0402(8) Uani 1 1 d . . .
C16 C 0.5239(2) 0.1984(2) 0.2987(2) 0.0492(9) Uani 1 1 d . . .
H16 H 0.5381 0.2125 0.3530 0.059 Uiso 1 1 calc R . .
N6 N 0.69747(18) 0.15347(18) 0.3453(2) 0.0534(8) Uani 1 1 d . . .
C17 C 0.9668(2) 0.1167(2) 0.4182(2) 0.0512(9) Uani 1 1 d . . .
H17 H 1.0268 0.1061 0.4359 0.061 Uiso 1 1 calc R . .
N7 N 0.2365(2) 0.3718(2) -0.0194(2) 0.0605(8) Uani 1 1 d . . .
C18 C 0.0995(2) 0.1234(2) 0.1721(2) 0.0480(9) Uani 1 1 d . . .
H18 H 0.1016 0.0875 0.2195 0.058 Uiso 1 1 calc R . .
C19 C 0.5900(2) 0.1721(2) 0.2500(2) 0.0427(8) Uani 1 1 d . . .
N8 N 0.68449(19) 0.16315(18) 0.27330(19) 0.0517(7) Uani 1 1 d . . .
N9 N -0.0920(3) 0.39448(19) 0.3114(2) 0.0696(9) Uani 1 1 d . . .
N10 N -0.0279(2) 0.4006(2) 0.3516(2) 0.0755(11) Uani 1 1 d . . .
C20 C 0.0204(3) 0.1867(2) 0.0591(2) 0.0605(10) Uani 1 1 d . . .
H20 H -0.0329 0.1942 0.0270 0.073 Uiso 1 1 calc R . .
C21 C 0.79261(19) 0.1433(2) 0.3676(2) 0.0463(9) Uani 1 1 d . . .
C22 C 0.5698(2) 0.1529(2) 0.1713(2) 0.0493(9) Uani 1 1 d . . .
H22 H 0.6158 0.1361 0.1375 0.059 Uiso 1 1 calc R . .
C23 C 0.2021(2) 0.3717(2) 0.2860(2) 0.0485(9) Uani 1 1 d . . .
H23 H 0.2583 0.3600 0.3121 0.058 Uiso 1 1 calc R . .
C24 C 0.0204(2) 0.1358(2) 0.1279(2) 0.0596(10) Uani 1 1 d . . .
H24 H -0.0332 0.1094 0.1450 0.072 Uiso 1 1 calc R . .
C25 C 0.8595(2) 0.1627(2) 0.3163(2) 0.0560(10) Uani 1 1 d . . .
H25 H 0.8455 0.1847 0.2639 0.067 Uiso 1 1 calc R . .
C26 C 0.4793(2) 0.3478(3) 0.0256(2) 0.0654(11) Uani 1 1 d . . .
H26 H 0.4726 0.3091 -0.0201 0.079 Uiso 1 1 calc R . .
C27 C 0.9000(2) 0.0995(2) 0.4677(2) 0.0596(10) Uani 1 1 d . . .
H27 H 0.9139 0.0776 0.5202 0.072 Uiso 1 1 calc R . .
C28 C 0.9474(2) 0.1492(2) 0.3432(3) 0.0582(10) Uani 1 1 d . . .
H28 H 0.9941 0.1627 0.3091 0.070 Uiso 1 1 calc R . .
C29 C -0.1704(3) 0.4074(3) 0.3663(3) 0.0711(13) Uani 1 1 d . . .
C30 C 0.8127(2) 0.1134(2) 0.4426(2) 0.0585(10) Uani 1 1 d . . .
H30 H 0.7667 0.1020 0.4779 0.070 Uiso 1 1 calc R . .
C31 C 0.5582(3) 0.3920(3) 0.0400(3) 0.0859(14) Uani 1 1 d . . .
H31 H 0.6047 0.3850 0.0044 0.103 Uiso 1 1 calc R . .
C32 C 0.4999(2) 0.4580(2) 0.1561(2) 0.0637(11) Uani 1 1 d . . .
H32 H 0.5059 0.4959 0.2023 0.076 Uiso 1 1 calc R . .
C33 C -0.3215(3) 0.4366(3) 0.4474(3) 0.0682(11) Uani 1 1 d . . .
H33 H -0.3748 0.4464 0.4739 0.082 Uiso 1 1 calc R . .
C34 C -0.2504(3) 0.3899(3) 0.3300(3) 0.0744(12) Uani 1 1 d . . .
H34 H -0.2545 0.3680 0.2767 0.089 Uiso 1 1 calc R . .
C35 C -0.3251(3) 0.4039(3) 0.3704(3) 0.0721(12) Uani 1 1 d . . .
H35 H -0.3814 0.3908 0.3447 0.087 Uiso 1 1 calc R . .
C36 C -0.2406(3) 0.4552(3) 0.4859(3) 0.0757(12) Uani 1 1 d . . .
H36 H -0.2373 0.4778 0.5390 0.091 Uiso 1 1 calc R . .
C37 C -0.1623(2) 0.4396(3) 0.4444(3) 0.0744(13) Uani 1 1 d . . .
H37 H -0.1054 0.4510 0.4694 0.089 Uiso 1 1 calc R . .
C38 C 0.5699(2) 0.4467(3) 0.1061(3) 0.0842(14) Uani 1 1 d . . .
H38 H 0.6253 0.4766 0.1178 0.101 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.993(4) . ?
Fe1 N5 1.993(3) . ?
Fe1 N1 2.049(3) . ?
Fe1 N4 2.060(2) . ?
Fe1 N3 2.107(2) . ?
Fe1 N2 2.122(2) . ?
S1 C3 1.641(4) . ?
S2 C12 1.619(4) . ?
N1 C10 1.336(4) . ?
N1 C6 1.351(4) . ?
N2 C4 1.278(3) . ?
N2 C1 1.434(3) . ?
C1 C23 1.377(4) . ?
C1 C8 1.381(4) . ?
C2 C14 1.382(4) . ?
C2 C11 1.383(4) . ?
C2 N3 1.429(4) . ?
C3 N7 1.154(4) . ?
N3 C5 1.274(3) . ?
C4 C15 1.453(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.458(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.338(4) . ?
N4 C15 1.345(4) . ?
N5 C12 1.159(4) . ?
C6 C18 1.379(4) . ?
C7 C9 1.378(5) . ?
C7 C8 1.389(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.366(5) . ?
C9 N10 1.549(5) . ?
C10 C20 1.375(5) . ?
C10 H10 0.9500 . ?
C11 C22 1.375(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.375(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.382(4) . ?
C16 C19 1.374(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.224(3) . ?
N6 C21 1.471(4) . ?
C17 C27 1.361(5) . ?
C17 C28 1.365(5) . ?
C17 H17 0.9500 . ?
C18 C24 1.384(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.371(4) . ?
C19 N8 1.463(4) . ?
N9 N10 1.155(4) . ?
N9 C29 1.547(5) . ?
C20 C24 1.370(5) . ?
C20 H20 0.9500 . ?
C21 C30 1.353(5) . ?
C21 C25 1.389(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.390(5) . ?
C25 H25 0.9500 . ?
C26 C31 1.359(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.375(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.347(6) . ?
C29 C37 1.392(6) . ?
C30 H30 0.9500 . ?
C31 C38 1.367(6) . ?
C31 H31 0.9500 . ?
C32 C38 1.393(6) . ?
C32 H32 0.9500 . ?
C33 C35 1.377(5) . ?
C33 C36 1.377(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.360(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.419(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 92.96(12) . . ?
N7 Fe1 N1 93.86(11) . . ?
N5 Fe1 N1 97.02(11) . . ?
N7 Fe1 N4 94.91(11) . . ?
N5 Fe1 N4 92.59(11) . . ?
N1 Fe1 N4 166.63(11) . . ?
N7 Fe1 N3 170.37(11) . . ?
N5 Fe1 N3 92.11(10) . . ?
N1 Fe1 N3 77.39(10) . . ?
N4 Fe1 N3 93.04(10) . . ?
N7 Fe1 N2 93.89(10) . . ?
N5 Fe1 N2 168.17(10) . . ?
N1 Fe1 N2 92.13(9) . . ?
N4 Fe1 N2 77.23(10) . . ?
N3 Fe1 N2 82.56(9) . . ?
C10 N1 C6 117.4(3) . . ?
C10 N1 Fe1 127.0(2) . . ?
C6 N1 Fe1 115.3(2) . . ?
C4 N2 C1 118.4(3) . . ?
C4 N2 Fe1 114.01(19) . . ?
C1 N2 Fe1 126.83(18) . . ?
C23 C1 C8 120.2(3) . . ?
C23 C1 N2 121.2(3) . . ?
C8 C1 N2 118.6(3) . . ?
C14 C2 C11 119.7(3) . . ?
C14 C2 N3 121.9(3) . . ?
C11 C2 N3 118.2(3) . . ?
N7 C3 S1 179.0(3) . . ?
C5 N3 C2 120.6(3) . . ?
C5 N3 Fe1 114.2(2) . . ?
C2 N3 Fe1 124.8(2) . . ?
N2 C4 C15 118.0(3) . . ?
N2 C4 H4 121.0 . . ?
C15 C4 H4 121.0 . . ?
N3 C5 C6 117.9(3) . . ?
N3 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C26 N4 C15 117.5(3) . . ?
C26 N4 Fe1 126.8(3) . . ?
C15 N4 Fe1 115.55(19) . . ?
C12 N5 Fe1 167.0(3) . . ?
N1 C6 C18 122.9(3) . . ?
N1 C6 C5 113.7(3) . . ?
C18 C6 C5 123.4(3) . . ?
C9 C7 C8 119.8(3) . . ?
C9 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C1 C8 C7 119.1(3) . . ?
C1 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C13 C9 C7 120.8(3) . . ?
C13 C9 N10 111.6(3) . . ?
C7 C9 N10 127.5(3) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 120.1(3) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
N5 C12 S2 178.7(3) . . ?
C9 C13 C23 119.6(3) . . ?
C9 C13 H13 120.2 . . ?
C23 C13 H13 120.2 . . ?
C2 C14 C16 119.5(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 123.0(3) . . ?
N4 C15 C4 114.4(3) . . ?
C32 C15 C4 122.7(3) . . ?
C19 C16 C14 120.3(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 111.6(3) . . ?
C27 C17 C28 119.9(3) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C3 N7 Fe1 168.3(3) . . ?
C6 C18 C24 118.4(3) . . ?
C6 C18 H18 120.8 . . ?
C24 C18 H18 120.8 . . ?
C22 C19 C16 119.9(3) . . ?
C22 C19 N8 113.9(3) . . ?
C16 C19 N8 126.1(3) . . ?
N6 N8 C19 112.3(3) . . ?
N10 N9 C29 106.4(4) . . ?
N9 N10 C9 103.0(4) . . ?
C24 C20 C10 119.3(3) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 120.6(3) . . ?
C30 C21 N6 116.1(3) . . ?
C25 C21 N6 123.4(3) . . ?
C19 C22 C11 120.4(3) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.4(3) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C20 C24 C18 119.1(3) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C21 C25 C28 118.7(3) . . ?
C21 C25 H25 120.7 . . ?
C28 C25 H25 120.7 . . ?
N4 C26 C31 123.2(4) . . ?
N4 C26 H26 118.4 . . ?
C31 C26 H26 118.4 . . ?
C17 C27 C30 120.8(4) . . ?
C17 C27 H27 119.6 . . ?
C30 C27 H27 119.6 . . ?
C17 C28 C25 120.3(3) . . ?
C17 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
C34 C29 C37 121.5(4) . . ?
C34 C29 N9 113.5(4) . . ?
C37 C29 N9 124.8(4) . . ?
C21 C30 C27 119.8(3) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C26 C31 C38 119.4(4) . . ?
C26 C31 H31 120.3 . . ?
C38 C31 H31 120.3 . . ?
C15 C32 C38 117.7(4) . . ?
C15 C32 H32 121.1 . . ?
C38 C32 H32 121.1 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.4(4) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 121.7(4) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C33 C36 C37 118.4(4) . . ?
C33 C36 H36 120.8 . . ?
C37 C36 H36 120.8 . . ?
C29 C37 C36 118.9(4) . . ?
C29 C37 H37 120.6 . . ?
C36 C37 H37 120.6 . . ?
C31 C38 C32 119.2(4) . . ?
C31 C38 H38 120.4 . . ?
C32 C38 H38 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.814
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.814
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_feaza235km2
_database_code_depnum_ccdc_archive 'CCDC 1492648'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
    bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1045(7)
_cell_length_b                   14.4584(9)
_cell_length_c                   16.9678(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.103(4)
_cell_angle_gamma                90.00
_cell_volume                     3700.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    235(2)
_cell_measurement_reflns_used    4466
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5517
_exptl_absorpt_correction_T_max  0.8958
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                    its'aim being to analyse the evolution of partial collection of data, 
                    always carried out over the same part of reciprocal space, 
                    and over a large scale of temperature.
                    This  explain the poor completness of data as well as the low theta(max) value, 
                    the low number of unique reflexions collected.
                    In ordre to obtain significant intensities with an exposure time relatively short, 
                    a crystal of neutron size was used. As the aim is to compare the diffraction data 
                    always obtained from the same part of the crystal at different temperature, 
                    problems of intensity scale are not considered to be of prior importance.
                    The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                    over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                    these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                    or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                    but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      235(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5859
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         22.96
_reflns_number_total             4181
_reflns_number_gt                3289
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0154P)²+2.9098P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4181
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0873
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29092(3) 0.28719(3) 0.05696(3) 0.04899(18) Uani 1 1 d . . .
S1 S 0.18978(6) 0.49750(7) -0.14677(6) 0.0621(3) Uani 1 1 d . . .
S2 S 0.43582(6) 0.07295(7) -0.10654(6) 0.0687(3) Uani 1 1 d . . .
N1 N 0.17181(18) 0.21603(17) 0.07890(17) 0.0483(7) Uani 1 1 d . . .
N2 N 0.27307(16) 0.37933(16) 0.15996(15) 0.0386(6) Uani 1 1 d . . .
C1 C 0.1971(2) 0.38501(19) 0.2067(2) 0.0400(8) Uani 1 1 d . . .
C2 C 0.4144(2) 0.1813(2) 0.1911(2) 0.0454(8) Uani 1 1 d . . .
C3 C 0.2140(2) 0.4257(3) -0.0753(2) 0.0514(9) Uani 1 1 d . . .
N3 N 0.32759(18) 0.19096(17) 0.15459(15) 0.0431(7) Uani 1 1 d . . .
C4 C 0.3439(2) 0.4204(2) 0.1848(2) 0.0464(9) Uani 1 1 d . . .
H4 H 0.3454 0.4553 0.2315 0.056 Uiso 1 1 calc R . .
C5 C 0.2613(2) 0.1521(2) 0.1845(2) 0.0471(9) Uani 1 1 d . . .
H5 H 0.2687 0.1164 0.2307 0.057 Uiso 1 1 calc R . .
N4 N 0.41344(17) 0.35994(19) 0.07386(18) 0.0530(7) Uani 1 1 d . . .
N5 N 0.3402(2) 0.2019(2) -0.02577(19) 0.0715(9) Uani 1 1 d . . .
C6 C 0.1734(2) 0.1646(2) 0.1453(2) 0.0462(8) Uani 1 1 d . . .
C7 C 0.0403(2) 0.4037(2) 0.2120(3) 0.0588(10) Uani 1 1 d . . .
H7 H -0.0157 0.4141 0.1867 0.071 Uiso 1 1 calc R . .
C8 C 0.1153(2) 0.3995(2) 0.1686(2) 0.0488(9) Uani 1 1 d . . .
H8 H 0.1104 0.4066 0.1134 0.059 Uiso 1 1 calc R . .
C9 C 0.0488(3) 0.3923(2) 0.2925(3) 0.0645(12) Uani 1 1 d . . .
C10 C 0.0940(3) 0.2251(2) 0.0382(2) 0.0618(10) Uani 1 1 d . . .
H10 H 0.0922 0.2592 -0.0090 0.074 Uiso 1 1 calc R . .
C11 C 0.4822(2) 0.1575(2) 0.1429(2) 0.0579(10) Uani 1 1 d . . .
H11 H 0.4695 0.1447 0.0892 0.070 Uiso 1 1 calc R . .
C12 C 0.3798(2) 0.1480(2) -0.0596(2) 0.0497(9) Uani 1 1 d . . .
C13 C 0.1295(3) 0.3773(3) 0.3303(2) 0.0702(11) Uani 1 1 d . . .
H13 H 0.1343 0.3698 0.3854 0.084 Uiso 1 1 calc R . .
C14 C 0.4339(2) 0.2014(2) 0.2697(2) 0.0572(10) Uani 1 1 d . . .
H14 H 0.3886 0.2188 0.3025 0.069 Uiso 1 1 calc R . .
C15 C 0.4229(2) 0.4122(2) 0.1391(2) 0.0507(9) Uani 1 1 d . . .
C16 C 0.5213(3) 0.1958(2) 0.3000(2) 0.0635(11) Uani 1 1 d . . .
H16 H 0.5351 0.2090 0.3535 0.076 Uiso 1 1 calc R . .
N6 N 0.6942(2) 0.1533(2) 0.3442(2) 0.0749(10) Uani 1 1 d . . .
C17 C 0.9639(2) 0.1174(2) 0.4182(3) 0.0642(11) Uani 1 1 d . . .
H17 H 1.0228 0.1069 0.4365 0.077 Uiso 1 1 calc R . .
N7 N 0.2303(2) 0.3752(2) -0.0233(2) 0.0667(9) Uani 1 1 d . . .
C18 C 0.0983(2) 0.1251(2) 0.1733(2) 0.0595(10) Uani 1 1 d . . .
H18 H 0.1013 0.0906 0.2203 0.071 Uiso 1 1 calc R . .
C19 C 0.5871(2) 0.1712(2) 0.2520(3) 0.0583(10) Uani 1 1 d . . .
N8 N 0.6848(2) 0.1626(2) 0.2750(2) 0.0686(9) Uani 1 1 d . . .
N9 N -0.0861(3) 0.3953(2) 0.3136(2) 0.0821(11) Uani 1 1 d . . .
N10 N -0.0268(3) 0.4016(2) 0.3553(3) 0.0948(14) Uani 1 1 d . . .
C20 C 0.0162(3) 0.1868(3) 0.0624(3) 0.0734(12) Uani 1 1 d . . .
H20 H -0.0372 0.1948 0.0322 0.088 Uiso 1 1 calc R . .
C21 C 0.7919(2) 0.1431(2) 0.3663(3) 0.0617(11) Uani 1 1 d . . .
C22 C 0.5679(2) 0.1525(2) 0.1740(3) 0.0644(11) Uani 1 1 d . . .
H22 H 0.6138 0.1361 0.1414 0.077 Uiso 1 1 calc R . .
C23 C 0.2032(2) 0.3732(2) 0.2874(2) 0.0584(10) Uani 1 1 d . . .
H23 H 0.2589 0.3622 0.3132 0.070 Uiso 1 1 calc R . .
C24 C 0.0184(3) 0.1372(3) 0.1307(3) 0.0712(11) Uani 1 1 d . . .
H24 H -0.0340 0.1114 0.1488 0.085 Uiso 1 1 calc R . .
C25 C 0.8585(3) 0.1623(3) 0.3161(3) 0.0721(11) Uani 1 1 d . . .
H25 H 0.8451 0.1834 0.2644 0.086 Uiso 1 1 calc R . .
C26 C 0.4831(3) 0.3532(3) 0.0290(3) 0.0805(13) Uani 1 1 d . . .
H26 H 0.4778 0.3172 -0.0172 0.097 Uiso 1 1 calc R . .
C27 C 0.8972(3) 0.1006(3) 0.4660(3) 0.0762(12) Uani 1 1 d . . .
H27 H 0.9104 0.0794 0.5177 0.091 Uiso 1 1 calc R . .
C28 C 0.9463(3) 0.1494(3) 0.3440(3) 0.0720(12) Uani 1 1 d . . .
H28 H 0.9930 0.1629 0.3114 0.086 Uiso 1 1 calc R . .
C29 C -0.1646(3) 0.4087(3) 0.3717(4) 0.0875(17) Uani 1 1 d . . .
C30 C 0.8110(3) 0.1138(3) 0.4406(3) 0.0793(12) Uani 1 1 d . . .
H30 H 0.7652 0.1025 0.4747 0.095 Uiso 1 1 calc R . .
C31 C 0.5620(3) 0.3968(4) 0.0477(4) 0.1105(19) Uani 1 1 d . . .
H31 H 0.6091 0.3917 0.0140 0.133 Uiso 1 1 calc R . .
C32 C 0.5014(2) 0.4564(3) 0.1624(3) 0.0777(12) Uani 1 1 d . . .
H32 H 0.5062 0.4914 0.2091 0.093 Uiso 1 1 calc R . .
C33 C -0.3158(3) 0.4371(3) 0.4499(3) 0.0806(13) Uani 1 1 d . . .
H33 H -0.3687 0.4466 0.4756 0.097 Uiso 1 1 calc R . .
C34 C -0.2440(3) 0.3899(3) 0.3358(3) 0.0872(15) Uani 1 1 d . . .
H34 H -0.2476 0.3676 0.2837 0.105 Uiso 1 1 calc R . .
C35 C -0.3188(3) 0.4030(3) 0.3749(3) 0.0822(13) Uani 1 1 d . . .
H35 H -0.3739 0.3883 0.3497 0.099 Uiso 1 1 calc R . .
C36 C -0.2355(3) 0.4576(3) 0.4881(3) 0.0888(14) Uani 1 1 d . . .
H36 H -0.2326 0.4810 0.5399 0.107 Uiso 1 1 calc R . .
C37 C -0.1579(3) 0.4428(3) 0.4477(4) 0.0887(15) Uani 1 1 d . . .
H37 H -0.1020 0.4560 0.4723 0.106 Uiso 1 1 calc R . .
C38 C 0.5721(3) 0.4475(4) 0.1150(4) 0.1068(18) Uani 1 1 d . . .
H38 H 0.6266 0.4761 0.1290 0.128 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.039(4) . ?
Fe1 N7 2.044(3) . ?
Fe1 N1 2.123(3) . ?
Fe1 N4 2.134(3) . ?
Fe1 N3 2.211(3) . ?
Fe1 N2 2.226(3) . ?
S1 C3 1.623(4) . ?
S2 C12 1.612(4) . ?
N1 C10 1.337(4) . ?
N1 C6 1.349(4) . ?
N2 C4 1.275(4) . ?
N2 C1 1.433(4) . ?
C1 C23 1.379(4) . ?
C1 C8 1.379(4) . ?
C2 C14 1.381(4) . ?
C2 C11 1.388(5) . ?
C2 N3 1.426(4) . ?
C3 N7 1.160(4) . ?
N3 C5 1.277(4) . ?
C4 C15 1.462(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.463(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.336(4) . ?
N4 C15 1.342(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.377(4) . ?
C7 C9 1.375(5) . ?
C7 C8 1.386(4) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.364(5) . ?
C9 N10 1.608(5) . ?
C10 C20 1.381(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.374(5) . ?
C11 H11 0.9400 . ?
C13 C23 1.363(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.393(5) . ?
C14 H14 0.9400 . ?
C15 C32 1.384(5) . ?
C16 C19 1.366(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.183(4) . ?
N6 C21 1.510(5) . ?
C17 C27 1.349(5) . ?
C17 C28 1.354(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.384(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.366(5) . ?
C19 N8 1.511(4) . ?
N9 N10 1.115(4) . ?
N9 C29 1.594(5) . ?
C20 C24 1.363(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.346(5) . ?
C21 C25 1.382(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.396(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.371(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.363(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.344(6) . ?
C29 C37 1.380(7) . ?
C30 H30 0.9400 . ?
C31 C38 1.358(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.378(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.364(6) . ?
C33 C36 1.376(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.353(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.406(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 94.86(13) . . ?
N5 Fe1 N1 99.92(12) . . ?
N7 Fe1 N1 93.75(12) . . ?
N5 Fe1 N4 92.53(12) . . ?
N7 Fe1 N4 97.85(12) . . ?
N1 Fe1 N4 162.20(11) . . ?
N5 Fe1 N3 92.83(11) . . ?
N7 Fe1 N3 167.47(11) . . ?
N1 Fe1 N3 75.16(11) . . ?
N4 Fe1 N3 91.67(10) . . ?
N5 Fe1 N2 165.20(11) . . ?
N7 Fe1 N2 94.69(11) . . ?
N1 Fe1 N2 90.72(10) . . ?
N4 Fe1 N2 74.96(10) . . ?
N3 Fe1 N2 79.88(9) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Fe1 126.3(2) . . ?
C6 N1 Fe1 115.9(2) . . ?
C4 N2 C1 118.3(3) . . ?
C4 N2 Fe1 113.7(2) . . ?
C1 N2 Fe1 127.1(2) . . ?
C23 C1 C8 119.7(3) . . ?
C23 C1 N2 122.0(3) . . ?
C8 C1 N2 118.3(3) . . ?
C14 C2 C11 119.6(3) . . ?
C14 C2 N3 122.8(3) . . ?
C11 C2 N3 117.3(3) . . ?
N7 C3 S1 178.8(3) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.8(2) . . ?
C2 N3 Fe1 125.0(2) . . ?
N2 C4 C15 118.8(3) . . ?
N2 C4 H4 120.6 . . ?
C15 C4 H4 120.6 . . ?
N3 C5 C6 118.5(3) . . ?
N3 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C26 N4 C15 117.4(3) . . ?
C26 N4 Fe1 126.3(3) . . ?
C15 N4 Fe1 116.2(2) . . ?
C12 N5 Fe1 165.7(3) . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.4(3) . . ?
C9 C7 C8 119.2(3) . . ?
C9 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C1 C8 C7 119.6(3) . . ?
C1 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C13 C9 C7 121.3(3) . . ?
C13 C9 N10 110.5(4) . . ?
C7 C9 N10 128.1(4) . . ?
N1 C10 C20 123.1(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.8(4) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
N5 C12 S2 179.5(4) . . ?
C23 C13 C9 119.4(4) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.5(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
N4 C15 C32 123.2(3) . . ?
N4 C15 C4 115.4(3) . . ?
C32 C15 C4 121.5(4) . . ?
C19 C16 C14 120.0(4) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 108.6(4) . . ?
C27 C17 C28 120.4(4) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 165.2(3) . . ?
C6 C18 C24 118.6(4) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C16 C19 C22 120.4(3) . . ?
C16 C19 N8 126.8(4) . . ?
C22 C19 N8 112.8(3) . . ?
N6 N8 C19 109.2(4) . . ?
N10 N9 C29 101.3(5) . . ?
N9 N10 C9 98.5(4) . . ?
C24 C20 C10 118.8(4) . . ?
C24 C20 H20 120.6 . . ?
C10 C20 H20 120.6 . . ?
C30 C21 C25 120.9(3) . . ?
C30 C21 N6 114.8(4) . . ?
C25 C21 N6 124.2(4) . . ?
C19 C22 C11 120.5(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.8(3) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 119.3(4) . . ?
C20 C24 H24 120.3 . . ?
C18 C24 H24 120.3 . . ?
C21 C25 C28 118.3(4) . . ?
C21 C25 H25 120.8 . . ?
C28 C25 H25 120.8 . . ?
N4 C26 C31 122.4(4) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 121.1(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C17 C28 C25 119.7(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 121.0(4) . . ?
C34 C29 N9 111.7(5) . . ?
C37 C29 N9 127.1(5) . . ?
C21 C30 C27 119.6(4) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C38 C31 C26 120.0(4) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C38 C32 C15 118.0(5) . . ?
C38 C32 H32 121.0 . . ?
C15 C32 H32 121.0 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.9(5) . . ?
C29 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C33 121.5(5) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.3(5) . . ?
C33 C36 H36 120.8 . . ?
C37 C36 H36 120.8 . . ?
C29 C37 C36 119.3(4) . . ?
C29 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C31 C38 C32 119.1(4) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.816
_diffrn_reflns_theta_full        22.96
_diffrn_measured_fraction_theta_full 0.816
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_feaza250kd1
_database_code_depnum_ccdc_archive 'CCDC 1492649'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1063(11)
_cell_length_b                   14.4809(11)
_cell_length_c                   16.9914(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.085(4)
_cell_angle_gamma                90.00
_cell_volume                     3711.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    4317
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986


_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5525
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
  its'aim being to analyse the evolution of partial collection of data, 
  always carried out over the same part of reciprocal space, 
  and over a large scale of temperature.
  This  explain the poor completness of data as well as the low theta(max) value, 
  the low number of unique reflexions collected.
  In ordre to obtain significant intensities with an exposure time relatively short, 
  a crystal of neutron size was used. As the aim is to compare the diffraction data 
  always obtained from the same part of the crystal at different temperature, 
  problems of intensity scale are not considered to be of prior importance.
  The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
  over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
  these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
  or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
  but modelling this two conformations is over the scope 
 of this study of partial data collections.
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5852
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         21.24
_reflns_number_total             3493
_reflns_number_gt                2769
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0265P)²+2.2447P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3493
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29111(3) 0.28741(4) 0.05624(3) 0.0517(2) Uani 1 1 d . . .
S1 S 0.18930(6) 0.49748(8) -0.14672(6) 0.0655(3) Uani 1 1 d . . .
S2 S 0.43650(7) 0.07278(8) -0.10636(6) 0.0733(4) Uani 1 1 d . . .
N1 N 0.17133(18) 0.2158(2) 0.07896(18) 0.0498(8) Uani 1 1 d . . .
N2 N 0.27331(17) 0.37957(19) 0.16031(15) 0.0421(7) Uani 1 1 d . . .
C1 C 0.1973(2) 0.3850(2) 0.2070(2) 0.0414(9) Uani 1 1 d . . .
C2 C 0.4140(2) 0.1810(2) 0.1913(2) 0.0482(9) Uani 1 1 d . . .
C3 C 0.2134(2) 0.4260(3) -0.0754(2) 0.0521(10) Uani 1 1 d . . .
N3 N 0.32737(18) 0.19054(19) 0.15436(15) 0.0464(8) Uani 1 1 d . . .
C4 C 0.3445(2) 0.4203(2) 0.1849(2) 0.0487(9) Uani 1 1 d . . .
H4 H 0.3458 0.4548 0.2318 0.058 Uiso 1 1 calc R . .
C5 C 0.2611(2) 0.1523(2) 0.1837(2) 0.0503(9) Uani 1 1 d . . .
H5 H 0.2685 0.1165 0.2298 0.060 Uiso 1 1 calc R . .
N4 N 0.41426(18) 0.3607(2) 0.0748(2) 0.0572(8) Uani 1 1 d . . .
N5 N 0.3412(2) 0.2022(3) -0.0265(2) 0.0758(11) Uani 1 1 d . . .
C6 C 0.1732(2) 0.1647(3) 0.1451(2) 0.0488(9) Uani 1 1 d . . .
C7 C 0.0410(2) 0.4031(3) 0.2112(3) 0.0609(11) Uani 1 1 d . . .
H7 H -0.0149 0.4127 0.1854 0.073 Uiso 1 1 calc R . .
C8 C 0.1157(2) 0.3996(2) 0.1691(2) 0.0528(10) Uani 1 1 d . . .
H8 H 0.1113 0.4073 0.1141 0.063 Uiso 1 1 calc R . .
C9 C 0.0489(3) 0.3924(3) 0.2910(3) 0.0694(13) Uani 1 1 d . . .
C10 C 0.0936(3) 0.2253(3) 0.0387(2) 0.0646(11) Uani 1 1 d . . .
H10 H 0.0916 0.2600 -0.0082 0.078 Uiso 1 1 calc R . .
C11 C 0.4826(2) 0.1579(3) 0.1439(2) 0.0603(11) Uani 1 1 d . . .
H11 H 0.4702 0.1455 0.0901 0.072 Uiso 1 1 calc R . .
C12 C 0.3808(2) 0.1482(3) -0.0600(2) 0.0535(10) Uani 1 1 d . . .
C13 C 0.1296(3) 0.3777(3) 0.3302(2) 0.0752(12) Uani 1 1 d . . .
H13 H 0.1338 0.3706 0.3853 0.090 Uiso 1 1 calc R . .
C14 C 0.4325(2) 0.2011(3) 0.2700(2) 0.0586(11) Uani 1 1 d . . .
H14 H 0.3869 0.2183 0.3026 0.070 Uiso 1 1 calc R . .
C15 C 0.4235(2) 0.4129(3) 0.1401(2) 0.0532(10) Uani 1 1 d . . .
C16 C 0.5204(3) 0.1952(3) 0.3001(2) 0.0685(12) Uani 1 1 d . . .
H16 H 0.5342 0.2080 0.3536 0.082 Uiso 1 1 calc R . .
N6 N 0.6936(2) 0.1535(2) 0.3439(3) 0.0833(11) Uani 1 1 d . . .
C17 C 0.9633(3) 0.1173(3) 0.4184(3) 0.0697(12) Uani 1 1 d . . .
H17 H 1.0222 0.1068 0.4371 0.084 Uiso 1 1 calc R . .
N7 N 0.2302(2) 0.3755(3) -0.0237(2) 0.0685(10) Uani 1 1 d . . .
C18 C 0.0981(3) 0.1252(3) 0.1727(2) 0.0639(11) Uani 1 1 d . . .
H18 H 0.1011 0.0905 0.2196 0.077 Uiso 1 1 calc R . .
C19 C 0.5869(2) 0.1708(3) 0.2516(3) 0.0643(12) Uani 1 1 d . . .
N8 N 0.6851(2) 0.1624(2) 0.2751(2) 0.0774(11) Uani 1 1 d . . .
N9 N -0.0847(3) 0.3952(2) 0.3135(2) 0.0866(12) Uani 1 1 d . . .
N10 N -0.0260(3) 0.4018(3) 0.3554(3) 0.1034(16) Uani 1 1 d . . .
C20 C 0.0162(3) 0.1866(3) 0.0626(3) 0.0765(13) Uani 1 1 d . . .
H20 H -0.0372 0.1942 0.0323 0.092 Uiso 1 1 calc R . .
C21 C 0.7918(2) 0.1430(3) 0.3658(3) 0.0676(12) Uani 1 1 d . . .
C22 C 0.5678(3) 0.1529(3) 0.1744(3) 0.0691(12) Uani 1 1 d . . .
H22 H 0.6136 0.1370 0.1416 0.083 Uiso 1 1 calc R . .
C23 C 0.2032(2) 0.3734(3) 0.2875(3) 0.0612(11) Uani 1 1 d . . .
H23 H 0.2588 0.3625 0.3133 0.073 Uiso 1 1 calc R . .
C24 C 0.0182(3) 0.1372(3) 0.1308(3) 0.0759(12) Uani 1 1 d . . .
H24 H -0.0340 0.1116 0.1490 0.091 Uiso 1 1 calc R . .
C25 C 0.8587(3) 0.1619(3) 0.3153(3) 0.0787(13) Uani 1 1 d . . .
H25 H 0.8456 0.1829 0.2636 0.094 Uiso 1 1 calc R . .
C26 C 0.4839(3) 0.3545(3) 0.0304(3) 0.0871(14) Uani 1 1 d . . .
H26 H 0.4788 0.3193 -0.0161 0.104 Uiso 1 1 calc R . .
C27 C 0.8967(3) 0.1011(3) 0.4655(3) 0.0821(13) Uani 1 1 d . . .
H27 H 0.9095 0.0805 0.5174 0.099 Uiso 1 1 calc R . .
C28 C 0.9464(3) 0.1487(3) 0.3438(3) 0.0772(13) Uani 1 1 d . . .
H28 H 0.9934 0.1615 0.3114 0.093 Uiso 1 1 calc R . .
C29 C -0.1645(4) 0.4089(3) 0.3725(4) 0.0923(18) Uani 1 1 d . . .
C30 C 0.8111(3) 0.1141(3) 0.4396(3) 0.0851(14) Uani 1 1 d . . .
H30 H 0.7652 0.1027 0.4735 0.102 Uiso 1 1 calc R . .
C31 C 0.5632(3) 0.3978(5) 0.0502(4) 0.116(2) Uani 1 1 d . . .
H31 H 0.6107 0.3925 0.0170 0.139 Uiso 1 1 calc R . .
C32 C 0.5016(3) 0.4557(3) 0.1634(3) 0.0807(13) Uani 1 1 d . . .
H32 H 0.5060 0.4900 0.2105 0.097 Uiso 1 1 calc R . .
C33 C -0.3149(3) 0.4372(3) 0.4503(3) 0.0856(14) Uani 1 1 d . . .
H33 H -0.3679 0.4467 0.4758 0.103 Uiso 1 1 calc R . .
C34 C -0.2434(4) 0.3902(3) 0.3360(3) 0.0915(15) Uani 1 1 d . . .
H34 H -0.2467 0.3683 0.2838 0.110 Uiso 1 1 calc R . .
C35 C -0.3180(3) 0.4032(3) 0.3750(3) 0.0860(14) Uani 1 1 d . . .
H35 H -0.3731 0.3886 0.3499 0.103 Uiso 1 1 calc R . .
C36 C -0.2351(3) 0.4575(3) 0.4887(3) 0.0942(15) Uani 1 1 d . . .
H36 H -0.2328 0.4806 0.5405 0.113 Uiso 1 1 calc R . .
C37 C -0.1570(3) 0.4432(3) 0.4492(4) 0.0933(15) Uani 1 1 d . . .
H37 H -0.1012 0.4563 0.4738 0.112 Uiso 1 1 calc R . .
C38 C 0.5726(3) 0.4480(4) 0.1175(4) 0.1118(19) Uani 1 1 d . . .
H38 H 0.6268 0.4769 0.1321 0.134 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.046(4) . ?
Fe1 N7 2.046(4) . ?
Fe1 N1 2.139(3) . ?
Fe1 N4 2.150(3) . ?
Fe1 N3 2.225(3) . ?
Fe1 N2 2.243(3) . ?
S1 C3 1.621(5) . ?
S2 C12 1.610(5) . ?
N1 C10 1.334(4) . ?
N1 C6 1.345(4) . ?
N2 C4 1.277(4) . ?
N2 C1 1.433(4) . ?
C1 C8 1.375(4) . ?
C1 C23 1.376(5) . ?
C2 C14 1.382(5) . ?
C2 C11 1.387(5) . ?
C2 N3 1.427(4) . ?
C3 N7 1.160(4) . ?
N3 C5 1.270(4) . ?
C4 C15 1.454(5) . ?
C4 H4 0.9400 . ?
C5 C6 1.460(5) . ?
C5 H5 0.9400 . ?
N4 C26 1.330(4) . ?
N4 C15 1.343(4) . ?
N5 C12 1.154(4) . ?
C6 C18 1.376(5) . ?
C7 C9 1.364(5) . ?
C7 C8 1.369(5) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.374(6) . ?
C9 N10 1.621(6) . ?
C10 C20 1.378(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.363(5) . ?
C11 H11 0.9400 . ?
C13 C23 1.362(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.400(5) . ?
C14 H14 0.9400 . ?
C15 C32 1.372(5) . ?
C16 C19 1.379(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.177(4) . ?
N6 C21 1.518(5) . ?
C17 C27 1.340(5) . ?
C17 C28 1.358(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.378(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.353(5) . ?
C19 N8 1.519(5) . ?
N9 N10 1.112(4) . ?
N9 C29 1.621(6) . ?
C20 C24 1.361(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.339(5) . ?
C21 C25 1.389(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.398(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.377(7) . ?
C26 H26 0.9400 . ?
C27 C30 1.357(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.341(7) . ?
C29 C37 1.393(7) . ?
C30 H30 0.9400 . ?
C31 C38 1.356(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.366(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.370(6) . ?
C33 C36 1.371(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.350(6) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.405(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 95.15(14) . . ?
N5 Fe1 N1 100.35(13) . . ?
N7 Fe1 N1 93.87(12) . . ?
N5 Fe1 N4 92.83(14) . . ?
N7 Fe1 N4 98.28(12) . . ?
N1 Fe1 N4 161.19(12) . . ?
N5 Fe1 N3 92.83(12) . . ?
N7 Fe1 N3 167.08(12) . . ?
N1 Fe1 N3 74.67(11) . . ?
N4 Fe1 N3 91.45(11) . . ?
N5 Fe1 N2 164.79(12) . . ?
N7 Fe1 N2 94.80(12) . . ?
N1 Fe1 N2 90.43(10) . . ?
N4 Fe1 N2 74.35(12) . . ?
N3 Fe1 N2 79.60(9) . . ?
C10 N1 C6 117.7(3) . . ?
C10 N1 Fe1 126.0(3) . . ?
C6 N1 Fe1 116.0(2) . . ?
C4 N2 C1 118.7(3) . . ?
C4 N2 Fe1 113.4(2) . . ?
C1 N2 Fe1 127.1(2) . . ?
C8 C1 C23 119.5(3) . . ?
C8 C1 N2 118.3(3) . . ?
C23 C1 N2 122.2(3) . . ?
C14 C2 C11 119.6(3) . . ?
C14 C2 N3 122.5(3) . . ?
C11 C2 N3 117.7(3) . . ?
N7 C3 S1 179.2(4) . . ?
C5 N3 C2 120.6(3) . . ?
C5 N3 Fe1 113.7(2) . . ?
C2 N3 Fe1 125.0(2) . . ?
N2 C4 C15 119.7(3) . . ?
N2 C4 H4 120.2 . . ?
C15 C4 H4 120.2 . . ?
N3 C5 C6 119.2(3) . . ?
N3 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C26 N4 C15 117.1(4) . . ?
C26 N4 Fe1 126.0(3) . . ?
C15 N4 Fe1 116.7(2) . . ?
C12 N5 Fe1 165.7(3) . . ?
N1 C6 C18 122.2(3) . . ?
N1 C6 C5 114.9(3) . . ?
C18 C6 C5 122.8(4) . . ?
C9 C7 C8 119.0(3) . . ?
C9 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C7 C8 C1 120.3(4) . . ?
C7 C8 H8 119.9 . . ?
C1 C8 H8 119.9 . . ?
C7 C9 C13 121.9(3) . . ?
C7 C9 N10 129.4(4) . . ?
C13 C9 N10 108.5(4) . . ?
N1 C10 C20 122.9(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 120.8(4) . . ?
C22 C11 H11 119.6 . . ?
C2 C11 H11 119.6 . . ?
N5 C12 S2 179.6(4) . . ?
C23 C13 C9 118.5(4) . . ?
C23 C13 H13 120.8 . . ?
C9 C13 H13 120.8 . . ?
C2 C14 C16 118.6(4) . . ?
C2 C14 H14 120.7 . . ?
C16 C14 H14 120.7 . . ?
N4 C15 C32 122.9(4) . . ?
N4 C15 C4 115.0(3) . . ?
C32 C15 C4 122.1(4) . . ?
C19 C16 C14 120.3(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 107.9(4) . . ?
C27 C17 C28 120.4(4) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 165.4(3) . . ?
C6 C18 C24 119.1(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.2(4) . . ?
C22 C19 N8 113.2(4) . . ?
C16 C19 N8 126.6(4) . . ?
N6 N8 C19 108.8(4) . . ?
N10 N9 C29 100.8(5) . . ?
N9 N10 C9 97.0(4) . . ?
C24 C20 C10 119.0(4) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.7(4) . . ?
C30 C21 N6 114.9(4) . . ?
C25 C21 N6 124.3(4) . . ?
C19 C22 C11 120.4(4) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.9(4) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 119.1(4) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C21 C25 C28 117.8(4) . . ?
C21 C25 H25 121.1 . . ?
C28 C25 H25 121.1 . . ?
N4 C26 C31 122.3(5) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 121.0(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C17 C28 C25 119.8(4) . . ?
C17 C28 H28 120.1 . . ?
C25 C28 H28 120.1 . . ?
C34 C29 C37 122.0(4) . . ?
C34 C29 N9 111.2(6) . . ?
C37 C29 N9 126.6(6) . . ?
C21 C30 C27 120.2(4) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C38 C31 C26 120.1(5) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C38 C32 C15 119.2(5) . . ?
C38 C32 H32 120.4 . . ?
C15 C32 H32 120.4 . . ?
C35 C33 C36 120.4(4) . . ?
C35 C33 H33 119.8 . . ?
C36 C33 H33 119.8 . . ?
C29 C34 C35 119.3(5) . . ?
C29 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C33 121.4(5) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.7(5) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C29 C37 C36 118.1(5) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
C31 C38 C32 118.4(5) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.847
_diffrn_reflns_theta_full        21.24
_diffrn_measured_fraction_theta_full 0.847
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.033
####################################################################### 
# 
# 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_feaza215km2
_database_code_depnum_ccdc_archive 'CCDC 1492650'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
    bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0902(6)
_cell_length_b                   14.4342(9)
_cell_length_c                   16.9112(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.056(3)
_cell_angle_gamma                90.00
_cell_volume                     3678.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    215(2)
_cell_measurement_reflns_used    4392
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5499
_exptl_absorpt_correction_T_max  0.8952
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
                    its'aim being to analyse the evolution of partial collection of data, 
                    always carried out over the same part of reciprocal space, 
                    and over a large scale of temperature.
                    This  explain the poor completness of data as well as the low theta(max) value, 
                    the low number of unique reflexions collected.
                    In ordre to obtain significant intensities with an exposure time relatively short, 
                    a crystal of neutron size was used. As the aim is to compare the diffraction data 
                    always obtained from the same part of the crystal at different temperature, 
                    problems of intensity scale are not considered to be of prior importance.
                    The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                    over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                    these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                    or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                    but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      215(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5827
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         22.97
_reflns_number_total             4163
_reflns_number_gt                3303
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0213P)²+2.6479P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4163
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0797
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29099(3) 0.28678(3) 0.05857(3) 0.04634(17) Uani 1 1 d . . .
S1 S 0.19083(6) 0.49636(7) -0.14625(6) 0.0592(3) Uani 1 1 d . . .
S2 S 0.43405(6) 0.07327(7) -0.10701(6) 0.0640(3) Uani 1 1 d . . .
N1 N 0.17297(17) 0.21649(16) 0.07921(16) 0.0442(7) Uani 1 1 d . . .
N2 N 0.27277(15) 0.37889(16) 0.15930(14) 0.0356(6) Uani 1 1 d . . .
C1 C 0.19657(19) 0.38448(19) 0.20591(19) 0.0369(8) Uani 1 1 d . . .
C2 C 0.4152(2) 0.18211(19) 0.1907(2) 0.0411(8) Uani 1 1 d . . .
C3 C 0.2157(2) 0.4246(3) -0.0742(2) 0.0507(9) Uani 1 1 d . . .
N3 N 0.32782(17) 0.19187(16) 0.15447(15) 0.0395(6) Uani 1 1 d . . .
C4 C 0.3436(2) 0.4209(2) 0.1841(2) 0.0424(8) Uani 1 1 d . . .
H4 H 0.3448 0.4565 0.2308 0.051 Uiso 1 1 calc R . .
C5 C 0.2618(2) 0.1520(2) 0.18465(19) 0.0437(8) Uani 1 1 d . . .
H5 H 0.2697 0.1157 0.2306 0.052 Uiso 1 1 calc R . .
N4 N 0.41236(16) 0.35854(18) 0.07331(16) 0.0479(7) Uani 1 1 d . . .
N5 N 0.3383(2) 0.2014(2) -0.02392(19) 0.0671(9) Uani 1 1 d . . .
C6 C 0.1740(2) 0.1644(2) 0.1457(2) 0.0423(8) Uani 1 1 d . . .
C7 C 0.0397(2) 0.4035(2) 0.2115(2) 0.0544(10) Uani 1 1 d . . .
H7 H -0.0164 0.4138 0.1861 0.065 Uiso 1 1 calc R . .
C8 C 0.1147(2) 0.3993(2) 0.1678(2) 0.0450(8) Uani 1 1 d . . .
H8 H 0.1098 0.4066 0.1125 0.054 Uiso 1 1 calc R . .
C9 C 0.0480(2) 0.3922(2) 0.2923(3) 0.0595(11) Uani 1 1 d . . .
C10 C 0.0953(3) 0.2257(2) 0.0380(2) 0.0569(10) Uani 1 1 d . . .
H10 H 0.0937 0.2603 -0.0091 0.068 Uiso 1 1 calc R . .
C11 C 0.4825(2) 0.1575(2) 0.1420(2) 0.0523(9) Uani 1 1 d . . .
H11 H 0.4693 0.1441 0.0883 0.063 Uiso 1 1 calc R . .
C12 C 0.3780(2) 0.1480(2) -0.0590(2) 0.0488(9) Uani 1 1 d . . .
C13 C 0.1291(3) 0.3772(3) 0.3302(2) 0.0651(10) Uani 1 1 d . . .
H13 H 0.1339 0.3700 0.3855 0.078 Uiso 1 1 calc R . .
C14 C 0.4349(2) 0.2026(2) 0.2695(2) 0.0507(9) Uani 1 1 d . . .
H14 H 0.3897 0.2203 0.3025 0.061 Uiso 1 1 calc R . .
C15 C 0.42235(19) 0.4122(2) 0.1381(2) 0.0456(8) Uani 1 1 d . . .
C16 C 0.5224(2) 0.1967(2) 0.2994(2) 0.0552(9) Uani 1 1 d . . .
H16 H 0.5364 0.2101 0.3530 0.066 Uiso 1 1 calc R . .
N6 N 0.6957(2) 0.15334(19) 0.3450(2) 0.0636(8) Uani 1 1 d . . .
C17 C 0.9652(2) 0.1172(2) 0.4181(3) 0.0583(10) Uani 1 1 d . . .
H17 H 1.0243 0.1069 0.4362 0.070 Uiso 1 1 calc R . .
N7 N 0.2322(2) 0.3742(2) -0.0220(2) 0.0646(9) Uani 1 1 d . . .
C18 C 0.0988(2) 0.1243(2) 0.1732(2) 0.0540(9) Uani 1 1 d . . .
H18 H 0.1016 0.0894 0.2202 0.065 Uiso 1 1 calc R . .
C19 C 0.5881(2) 0.1716(2) 0.2511(2) 0.0508(9) Uani 1 1 d . . .
N8 N 0.6845(2) 0.16280(19) 0.2745(2) 0.0596(8) Uani 1 1 d . . .
N9 N -0.0885(3) 0.3951(2) 0.3129(2) 0.0780(10) Uani 1 1 d . . .
N10 N -0.0270(3) 0.4012(2) 0.3541(3) 0.0878(12) Uani 1 1 d . . .
C20 C 0.0174(3) 0.1866(3) 0.0616(3) 0.0687(11) Uani 1 1 d . . .
H20 H -0.0359 0.1945 0.0310 0.082 Uiso 1 1 calc R . .
C21 C 0.7921(2) 0.1433(2) 0.3670(3) 0.0534(10) Uani 1 1 d . . .
C22 C 0.5685(2) 0.1529(2) 0.1727(2) 0.0583(10) Uani 1 1 d . . .
H22 H 0.6142 0.1368 0.1397 0.070 Uiso 1 1 calc R . .
C23 C 0.2027(2) 0.3728(2) 0.2871(2) 0.0538(9) Uani 1 1 d . . .
H23 H 0.2584 0.3616 0.3130 0.065 Uiso 1 1 calc R . .
C24 C 0.0189(2) 0.1364(2) 0.1302(3) 0.0667(11) Uani 1 1 d . . .
H24 H -0.0336 0.1105 0.1480 0.080 Uiso 1 1 calc R . .
C25 C 0.8590(2) 0.1624(2) 0.3164(2) 0.0649(10) Uani 1 1 d . . .
H25 H 0.8454 0.1840 0.2647 0.078 Uiso 1 1 calc R . .
C26 C 0.4810(2) 0.3515(3) 0.0276(3) 0.0735(12) Uani 1 1 d . . .
H26 H 0.4749 0.3152 -0.0185 0.088 Uiso 1 1 calc R . .
C27 C 0.8983(2) 0.1000(3) 0.4667(3) 0.0684(11) Uani 1 1 d . . .
H27 H 0.9117 0.0785 0.5184 0.082 Uiso 1 1 calc R . .
C28 C 0.9470(2) 0.1491(2) 0.3437(3) 0.0647(11) Uani 1 1 d . . .
H28 H 0.9935 0.1622 0.3106 0.078 Uiso 1 1 calc R . .
C29 C -0.1665(3) 0.4081(3) 0.3698(4) 0.0805(15) Uani 1 1 d . . .
C30 C 0.8118(2) 0.1137(3) 0.4416(3) 0.0679(11) Uani 1 1 d . . .
H30 H 0.7661 0.1025 0.4761 0.081 Uiso 1 1 calc R . .
C31 C 0.5606(3) 0.3949(4) 0.0450(4) 0.0994(17) Uani 1 1 d . . .
H31 H 0.6076 0.3883 0.0110 0.119 Uiso 1 1 calc R . .
C32 C 0.5009(2) 0.4570(3) 0.1603(3) 0.0714(12) Uani 1 1 d . . .
H32 H 0.5062 0.4925 0.2069 0.086 Uiso 1 1 calc R . .
C33 C -0.3178(3) 0.4368(3) 0.4489(3) 0.0738(12) Uani 1 1 d . . .
H33 H -0.3708 0.4459 0.4746 0.089 Uiso 1 1 calc R . .
C34 C -0.2459(3) 0.3900(3) 0.3341(3) 0.0825(14) Uani 1 1 d . . .
H34 H -0.2496 0.3678 0.2817 0.099 Uiso 1 1 calc R . .
C35 C -0.3207(3) 0.4034(3) 0.3730(3) 0.0759(12) Uani 1 1 d . . .
H35 H -0.3759 0.3894 0.3475 0.091 Uiso 1 1 calc R . .
C36 C -0.2375(3) 0.4570(3) 0.4876(3) 0.0840(13) Uani 1 1 d . . .
H36 H -0.2347 0.4803 0.5396 0.101 Uiso 1 1 calc R . .
C37 C -0.1592(3) 0.4418(3) 0.4468(3) 0.0829(14) Uani 1 1 d . . .
H37 H -0.1031 0.4544 0.4714 0.099 Uiso 1 1 calc R . .
C38 C 0.5713(3) 0.4478(3) 0.1117(4) 0.0973(16) Uani 1 1 d . . .
H38 H 0.6256 0.4774 0.1245 0.117 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.020(3) . ?
Fe1 N7 2.026(4) . ?
Fe1 N1 2.095(3) . ?
Fe1 N4 2.107(3) . ?
Fe1 N3 2.173(2) . ?
Fe1 N2 2.190(2) . ?
S1 C3 1.628(4) . ?
S2 C12 1.616(4) . ?
N1 C10 1.337(4) . ?
N1 C6 1.352(4) . ?
N2 C4 1.280(3) . ?
N2 C1 1.431(3) . ?
C1 C8 1.380(4) . ?
C1 C23 1.382(4) . ?
C2 C14 1.381(4) . ?
C2 C11 1.387(4) . ?
C2 N3 1.432(4) . ?
C3 N7 1.160(4) . ?
N3 C5 1.280(4) . ?
C4 C15 1.461(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.459(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.329(4) . ?
N4 C15 1.343(4) . ?
N5 C12 1.159(4) . ?
C6 C18 1.376(4) . ?
C7 C9 1.375(5) . ?
C7 C8 1.385(4) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.368(5) . ?
C9 N10 1.585(5) . ?
C10 C20 1.382(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.374(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.362(4) . ?
C13 H13 0.9400 . ?
C14 C16 1.392(4) . ?
C14 H14 0.9400 . ?
C15 C32 1.384(4) . ?
C16 C19 1.367(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.203(4) . ?
N6 C21 1.489(4) . ?
C17 C28 1.353(5) . ?
C17 C27 1.359(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.385(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.369(5) . ?
C19 N8 1.491(4) . ?
N9 N10 1.135(4) . ?
N9 C29 1.572(5) . ?
C20 C24 1.366(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.350(5) . ?
C21 C25 1.385(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.396(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.372(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.365(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.338(6) . ?
C29 C37 1.388(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.365(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.384(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.368(6) . ?
C33 C36 1.379(5) . ?
C33 H33 0.9400 . ?
C34 C35 1.351(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.417(5) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 94.23(12) . . ?
N5 Fe1 N1 98.86(11) . . ?
N7 Fe1 N1 93.90(11) . . ?
N5 Fe1 N4 92.58(12) . . ?
N7 Fe1 N4 96.89(11) . . ?
N1 Fe1 N4 163.64(11) . . ?
N5 Fe1 N3 92.57(11) . . ?
N7 Fe1 N3 168.51(11) . . ?
N1 Fe1 N3 75.88(10) . . ?
N4 Fe1 N3 92.04(10) . . ?
N5 Fe1 N2 166.25(11) . . ?
N7 Fe1 N2 94.39(10) . . ?
N1 Fe1 N2 91.22(9) . . ?
N4 Fe1 N2 75.75(10) . . ?
N3 Fe1 N2 80.78(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 126.4(2) . . ?
C6 N1 Fe1 115.9(2) . . ?
C4 N2 C1 118.3(3) . . ?
C4 N2 Fe1 114.0(2) . . ?
C1 N2 Fe1 126.93(19) . . ?
C8 C1 C23 119.6(3) . . ?
C8 C1 N2 118.5(3) . . ?
C23 C1 N2 121.8(3) . . ?
C14 C2 C11 120.1(3) . . ?
C14 C2 N3 122.5(3) . . ?
C11 C2 N3 117.2(3) . . ?
N7 C3 S1 178.8(3) . . ?
C5 N3 C2 120.3(3) . . ?
C5 N3 Fe1 114.1(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 118.2(3) . . ?
N2 C4 H4 120.9 . . ?
C15 C4 H4 120.9 . . ?
N3 C5 C6 118.2(3) . . ?
N3 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C26 N4 C15 117.4(3) . . ?
C26 N4 Fe1 126.4(3) . . ?
C15 N4 Fe1 116.04(19) . . ?
C12 N5 Fe1 166.1(3) . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 114.4(3) . . ?
C18 C6 C5 122.8(3) . . ?
C9 C7 C8 119.4(3) . . ?
C9 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C1 C8 C7 119.6(3) . . ?
C1 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C13 C9 C7 121.0(3) . . ?
C13 C9 N10 110.8(4) . . ?
C7 C9 N10 128.0(4) . . ?
N1 C10 C20 123.0(3) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
N5 C12 S2 179.3(3) . . ?
C23 C13 C9 119.5(4) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.2(3) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
N4 C15 C32 123.2(3) . . ?
N4 C15 C4 115.2(3) . . ?
C32 C15 C4 121.6(3) . . ?
C19 C16 C14 120.3(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 110.0(3) . . ?
C28 C17 C27 120.3(3) . . ?
C28 C17 H17 119.9 . . ?
C27 C17 H17 119.9 . . ?
C3 N7 Fe1 166.0(3) . . ?
C6 C18 C24 118.7(3) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C16 C19 C22 120.2(3) . . ?
C16 C19 N8 126.3(3) . . ?
C22 C19 N8 113.5(3) . . ?
N6 N8 C19 110.9(3) . . ?
N10 N9 C29 103.3(4) . . ?
N9 N10 C9 100.3(4) . . ?
C24 C20 C10 119.1(3) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.6(3) . . ?
C30 C21 N6 115.3(3) . . ?
C25 C21 N6 124.1(4) . . ?
C19 C22 C11 120.6(3) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.8(3) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 119.2(3) . . ?
C20 C24 H24 120.4 . . ?
C18 C24 H24 120.4 . . ?
C21 C25 C28 118.7(4) . . ?
C21 C25 H25 120.6 . . ?
C28 C25 H25 120.6 . . ?
N4 C26 C31 122.8(4) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 120.9(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C17 C28 C25 119.8(4) . . ?
C17 C28 H28 120.1 . . ?
C25 C28 H28 120.1 . . ?
C34 C29 C37 121.2(4) . . ?
C34 C29 N9 112.4(5) . . ?
C37 C29 N9 126.2(5) . . ?
C21 C30 C27 119.7(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.7(4) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C38 C32 C15 117.8(4) . . ?
C38 C32 H32 121.1 . . ?
C15 C32 H32 121.1 . . ?
C35 C33 C36 120.2(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 120.1(5) . . ?
C29 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C33 121.5(4) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.1(5) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
C29 C37 C36 118.9(4) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C31 C38 C32 119.0(4) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.816
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.816
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_feaza255km2
_database_code_depnum_ccdc_archive 'CCDC 1492651'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1127(7)
_cell_length_b                   14.4897(9)
_cell_length_c                   16.9969(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.083(4)
_cell_angle_gamma                90.00
_cell_volume                     3716.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    255(2)
_cell_measurement_reflns_used    4443
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5529
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
                    its'aim being to analyse the evolution of partial collection of data, 
                    always carried out over the same part of reciprocal space, 
                    and over a large scale of temperature.
                    This  explain the poor completness of data as well as the low theta(max) value, 
                    the low number of unique reflexions collected.
                    In ordre to obtain significant intensities with an exposure time relatively short, 
                    a crystal of neutron size was used. As the aim is to compare the diffraction data 
                    always obtained from the same part of the crystal at different temperature, 
                    problems of intensity scale are not considered to be of prior importance.
                    The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
                    over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
                    these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
                    or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
                    but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      255(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5886
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         22.98
_reflns_number_total             4201
_reflns_number_gt                3244
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0189P)²+2.6154P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4201
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0895
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29118(3) 0.28744(3) 0.05613(3) 0.05205(18) Uani 1 1 d . . .
S1 S 0.18921(6) 0.49747(7) -0.14684(6) 0.0657(3) Uani 1 1 d . . .
S2 S 0.43656(6) 0.07273(7) -0.10639(6) 0.0737(3) Uani 1 1 d . . .
N1 N 0.17166(18) 0.21593(17) 0.07865(17) 0.0519(7) Uani 1 1 d . . .
N2 N 0.27305(16) 0.37989(16) 0.16029(15) 0.0410(6) Uani 1 1 d . . .
C1 C 0.1971(2) 0.3852(2) 0.2066(2) 0.0429(8) Uani 1 1 d . . .
C2 C 0.4141(2) 0.1809(2) 0.1909(2) 0.0484(9) Uani 1 1 d . . .
C3 C 0.2136(2) 0.4260(3) -0.0756(2) 0.0543(9) Uani 1 1 d . . .
N3 N 0.32765(18) 0.19056(17) 0.15429(16) 0.0475(7) Uani 1 1 d . . .
C4 C 0.3443(2) 0.4202(2) 0.1852(2) 0.0509(9) Uani 1 1 d . . .
H4 H 0.3458 0.4542 0.2316 0.061 Uiso 1 1 calc R . .
C5 C 0.2613(2) 0.1522(2) 0.1840(2) 0.0523(9) Uani 1 1 d . . .
H5 H 0.2686 0.1170 0.2296 0.063 Uiso 1 1 calc R . .
N4 N 0.41410(17) 0.3607(2) 0.07452(18) 0.0578(8) Uani 1 1 d . . .
N5 N 0.3414(2) 0.2024(2) -0.02657(19) 0.0761(10) Uani 1 1 d . . .
C6 C 0.1731(2) 0.1645(2) 0.1449(2) 0.0506(9) Uani 1 1 d . . .
C7 C 0.0409(2) 0.4035(2) 0.2119(3) 0.0638(11) Uani 1 1 d . . .
H7 H -0.0145 0.4136 0.1868 0.077 Uiso 1 1 calc R . .
C8 C 0.1157(2) 0.3995(2) 0.1686(2) 0.0521(9) Uani 1 1 d . . .
H8 H 0.1110 0.4065 0.1142 0.062 Uiso 1 1 calc R . .
C9 C 0.0489(3) 0.3923(2) 0.2922(3) 0.0697(12) Uani 1 1 d . . .
C10 C 0.0940(3) 0.2253(2) 0.0383(2) 0.0655(10) Uani 1 1 d . . .
H10 H 0.0919 0.2592 -0.0082 0.079 Uiso 1 1 calc R . .
C11 C 0.4821(2) 0.1573(2) 0.1439(2) 0.0623(10) Uani 1 1 d . . .
H11 H 0.4698 0.1445 0.0908 0.075 Uiso 1 1 calc R . .
C12 C 0.3809(2) 0.1482(3) -0.0601(2) 0.0546(9) Uani 1 1 d . . .
C13 C 0.1295(3) 0.3776(3) 0.3298(2) 0.0747(11) Uani 1 1 d . . .
H13 H 0.1341 0.3704 0.3843 0.090 Uiso 1 1 calc R . .
C14 C 0.4329(2) 0.2007(2) 0.2696(2) 0.0620(10) Uani 1 1 d . . .
H14 H 0.3879 0.2174 0.3020 0.074 Uiso 1 1 calc R . .
C15 C 0.4236(2) 0.4123(2) 0.1401(2) 0.0543(9) Uani 1 1 d . . .
C16 C 0.5205(3) 0.1954(2) 0.2999(2) 0.0690(11) Uani 1 1 d . . .
H16 H 0.5339 0.2087 0.3527 0.083 Uiso 1 1 calc R . .
N6 N 0.6927(2) 0.1536(2) 0.3438(2) 0.0831(11) Uani 1 1 d . . .
C17 C 0.9632(3) 0.1177(3) 0.4180(3) 0.0708(11) Uani 1 1 d . . .
H17 H 1.0214 0.1074 0.4364 0.085 Uiso 1 1 calc R . .
N7 N 0.2299(2) 0.3757(2) -0.0237(2) 0.0705(9) Uani 1 1 d . . .
C18 C 0.0983(2) 0.1250(2) 0.1730(2) 0.0650(10) Uani 1 1 d . . .
H18 H 0.1015 0.0908 0.2194 0.078 Uiso 1 1 calc R . .
C19 C 0.5863(2) 0.1706(2) 0.2523(3) 0.0654(11) Uani 1 1 d . . .
N8 N 0.6854(2) 0.1622(2) 0.2757(2) 0.0766(10) Uani 1 1 d . . .
N9 N -0.0849(3) 0.3955(2) 0.3136(2) 0.0879(12) Uani 1 1 d . . .
N10 N -0.0270(3) 0.4020(2) 0.3558(3) 0.1022(15) Uani 1 1 d . . .
C20 C 0.0165(3) 0.1868(3) 0.0626(3) 0.0783(12) Uani 1 1 d . . .
H20 H -0.0363 0.1945 0.0327 0.094 Uiso 1 1 calc R . .
C21 C 0.7918(2) 0.1432(3) 0.3655(3) 0.0697(12) Uani 1 1 d . . .
C22 C 0.5675(3) 0.1525(3) 0.1747(3) 0.0715(11) Uani 1 1 d . . .
H22 H 0.6130 0.1369 0.1423 0.086 Uiso 1 1 calc R . .
C23 C 0.2032(2) 0.3735(2) 0.2873(2) 0.0621(10) Uani 1 1 d . . .
H23 H 0.2582 0.3627 0.3129 0.074 Uiso 1 1 calc R . .
C24 C 0.0181(3) 0.1373(3) 0.1309(3) 0.0771(12) Uani 1 1 d . . .
H24 H -0.0337 0.1122 0.1489 0.092 Uiso 1 1 calc R . .
C25 C 0.8584(3) 0.1620(3) 0.3156(3) 0.0808(12) Uani 1 1 d . . .
H25 H 0.8453 0.1827 0.2645 0.097 Uiso 1 1 calc R . .
C26 C 0.4839(3) 0.3544(3) 0.0305(3) 0.0887(13) Uani 1 1 d . . .
H26 H 0.4788 0.3192 -0.0153 0.106 Uiso 1 1 calc R . .
C27 C 0.8967(3) 0.1012(3) 0.4653(3) 0.0851(13) Uani 1 1 d . . .
H27 H 0.9096 0.0807 0.5165 0.102 Uiso 1 1 calc R . .
C28 C 0.9462(3) 0.1491(3) 0.3439(3) 0.0789(12) Uani 1 1 d . . .
H28 H 0.9926 0.1621 0.3119 0.095 Uiso 1 1 calc R . .
C29 C -0.1630(4) 0.4092(3) 0.3728(4) 0.0950(18) Uani 1 1 d . . .
C30 C 0.8107(3) 0.1140(3) 0.4397(3) 0.0874(13) Uani 1 1 d . . .
H30 H 0.7653 0.1027 0.4732 0.105 Uiso 1 1 calc R . .
C31 C 0.5632(3) 0.3974(4) 0.0496(4) 0.120(2) Uani 1 1 d . . .
H31 H 0.6101 0.3923 0.0166 0.144 Uiso 1 1 calc R . .
C32 C 0.5017(3) 0.4557(3) 0.1636(3) 0.0823(13) Uani 1 1 d . . .
H32 H 0.5063 0.4898 0.2100 0.099 Uiso 1 1 calc R . .
C33 C -0.3146(3) 0.4370(3) 0.4502(3) 0.0868(13) Uani 1 1 d . . .
H33 H -0.3670 0.4462 0.4754 0.104 Uiso 1 1 calc R . .
C34 C -0.2423(4) 0.3903(3) 0.3370(3) 0.0936(15) Uani 1 1 d . . .
H34 H -0.2455 0.3684 0.2855 0.112 Uiso 1 1 calc R . .
C35 C -0.3175(3) 0.4030(3) 0.3752(3) 0.0880(14) Uani 1 1 d . . .
H35 H -0.3719 0.3884 0.3501 0.106 Uiso 1 1 calc R . .
C36 C -0.2348(3) 0.4578(3) 0.4888(3) 0.0968(14) Uani 1 1 d . . .
H36 H -0.2323 0.4809 0.5399 0.116 Uiso 1 1 calc R . .
C37 C -0.1569(3) 0.4429(3) 0.4488(4) 0.0960(16) Uani 1 1 d . . .
H37 H -0.1018 0.4558 0.4734 0.115 Uiso 1 1 calc R . .
C38 C 0.5725(3) 0.4475(4) 0.1169(5) 0.1157(19) Uani 1 1 d . . .
H38 H 0.6261 0.4759 0.1312 0.139 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.046(4) . ?
Fe1 N7 2.050(3) . ?
Fe1 N1 2.135(3) . ?
Fe1 N4 2.148(3) . ?
Fe1 N3 2.227(3) . ?
Fe1 N2 2.249(3) . ?
S1 C3 1.620(4) . ?
S2 C12 1.611(4) . ?
N1 C10 1.334(4) . ?
N1 C6 1.349(4) . ?
N2 C4 1.277(4) . ?
N2 C1 1.429(4) . ?
C1 C8 1.374(4) . ?
C1 C23 1.380(4) . ?
C2 C11 1.379(5) . ?
C2 C14 1.384(5) . ?
C2 N3 1.423(4) . ?
C3 N7 1.160(4) . ?
N3 C5 1.274(4) . ?
C4 C15 1.461(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.467(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.328(4) . ?
N4 C15 1.343(4) . ?
N5 C12 1.154(4) . ?
C6 C18 1.376(5) . ?
C7 C9 1.373(5) . ?
C7 C8 1.383(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.361(5) . ?
C9 N10 1.625(6) . ?
C10 C20 1.381(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.368(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.362(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.395(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.378(5) . ?
C16 C19 1.364(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.164(4) . ?
N6 C21 1.530(5) . ?
C17 C27 1.341(5) . ?
C17 C28 1.350(5) . ?
C17 H17 0.9300 . ?
C18 C24 1.385(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.360(5) . ?
C19 N8 1.534(5) . ?
N9 N10 1.105(4) . ?
N9 C29 1.605(6) . ?
C20 C24 1.364(5) . ?
C20 H20 0.9300 . ?
C21 C30 1.346(6) . ?
C21 C25 1.376(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.400(5) . ?
C25 H25 0.9300 . ?
C26 C31 1.375(6) . ?
C26 H26 0.9300 . ?
C27 C30 1.362(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.342(7) . ?
C29 C37 1.379(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.355(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.371(6) . ?
C32 H32 0.9300 . ?
C33 C35 1.364(6) . ?
C33 C36 1.375(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.352(5) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.406(6) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 H38 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
N5 Fe1 N7 95.29(13) . . ?
N5 Fe1 N1 100.34(12) . . ?
N7 Fe1 N1 93.72(12) . . ?
N5 Fe1 N4 92.74(12) . . ?
N7 Fe1 N4 98.31(12) . . ?
N1 Fe1 N4 161.33(11) . . ?
N5 Fe1 N3 92.80(11) . . ?
N7 Fe1 N3 166.99(12) . . ?
N1 Fe1 N3 74.77(11) . . ?
N4 Fe1 N3 91.45(11) . . ?
N5 Fe1 N2 164.85(11) . . ?
N7 Fe1 N2 94.58(11) . . ?
N1 Fe1 N2 90.45(10) . . ?
N4 Fe1 N2 74.46(11) . . ?
N3 Fe1 N2 79.71(9) . . ?
C10 N1 C6 117.4(3) . . ?
C10 N1 Fe1 126.0(3) . . ?
C6 N1 Fe1 116.2(2) . . ?
C4 N2 C1 118.7(3) . . ?
C4 N2 Fe1 113.4(2) . . ?
C1 N2 Fe1 127.0(2) . . ?
C8 C1 C23 119.7(3) . . ?
C8 C1 N2 118.3(3) . . ?
C23 C1 N2 121.9(3) . . ?
C11 C2 C14 119.4(3) . . ?
C11 C2 N3 117.8(3) . . ?
C14 C2 N3 122.6(3) . . ?
N7 C3 S1 178.7(3) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.8(2) . . ?
C2 N3 Fe1 125.0(2) . . ?
N2 C4 C15 119.4(3) . . ?
N2 C4 H4 120.3 . . ?
C15 C4 H4 120.3 . . ?
N3 C5 C6 118.9(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C26 N4 C15 116.9(3) . . ?
C26 N4 Fe1 126.2(3) . . ?
C15 N4 Fe1 116.7(2) . . ?
C12 N5 Fe1 165.7(3) . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.4(3) . . ?
C9 C7 C8 119.5(3) . . ?
C9 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C1 C8 C7 119.5(3) . . ?
C1 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C13 C9 C7 121.0(3) . . ?
C13 C9 N10 110.3(4) . . ?
C7 C9 N10 128.6(4) . . ?
N1 C10 C20 122.8(4) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 120.6(4) . . ?
C22 C11 H11 119.7 . . ?
C2 C11 H11 119.7 . . ?
N5 C12 S2 179.6(4) . . ?
C9 C13 C23 119.6(4) . . ?
C9 C13 H13 120.2 . . ?
C23 C13 H13 120.2 . . ?
C2 C14 C16 119.2(3) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
N4 C15 C32 123.1(3) . . ?
N4 C15 C4 115.2(3) . . ?
C32 C15 C4 121.7(4) . . ?
C19 C16 C14 120.2(4) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 106.8(4) . . ?
C27 C17 C28 120.5(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C3 N7 Fe1 164.8(3) . . ?
C6 C18 C24 118.7(4) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 120.4(3) . . ?
C22 C19 N8 112.7(4) . . ?
C16 C19 N8 126.9(4) . . ?
N6 N8 C19 107.8(4) . . ?
N10 N9 C29 99.5(5) . . ?
N9 N10 C9 97.1(5) . . ?
C24 C20 C10 119.4(4) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 120.9(4) . . ?
C30 C21 N6 114.3(4) . . ?
C25 C21 N6 124.7(4) . . ?
C19 C22 C11 120.3(4) . . ?
C19 C22 H22 119.9 . . ?
C11 C22 H22 119.9 . . ?
C13 C23 C1 120.6(3) . . ?
C13 C23 H23 119.7 . . ?
C1 C23 H23 119.7 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.2(4) . . ?
C21 C25 H25 120.9 . . ?
C28 C25 H25 120.9 . . ?
N4 C26 C31 123.0(5) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 121.2(5) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C17 C28 C25 119.6(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 120.6(4) . . ?
C34 C29 N9 111.1(5) . . ?
C37 C29 N9 128.1(5) . . ?
C21 C30 C27 119.5(4) . . ?
C21 C30 H30 120.3 . . ?
C27 C30 H30 120.3 . . ?
C38 C31 C26 119.4(4) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C38 C32 C15 118.4(5) . . ?
C38 C32 H32 120.8 . . ?
C15 C32 H32 120.8 . . ?
C35 C33 C36 120.6(4) . . ?
C35 C33 H33 119.7 . . ?
C36 C33 H33 119.7 . . ?
C29 C34 C35 120.5(5) . . ?
C29 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C33 120.7(5) . . ?
C34 C35 H35 119.6 . . ?
C33 C35 H35 119.6 . . ?
C33 C36 C37 118.1(5) . . ?
C33 C36 H36 121.0 . . ?
C37 C36 H36 121.0 . . ?
C29 C37 C36 119.4(5) . . ?
C29 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
C31 C38 C32 119.1(5) . . ?
C31 C38 H38 120.4 . . ?
C32 C38 H38 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.814
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.814
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.036
####################################################################### 
# 
# 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_feaza190kd1
_database_code_depnum_ccdc_archive 'CCDC 1492652'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0573(10)
_cell_length_b                   14.4200(10)
_cell_length_c                   16.7947(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.889(4)
_cell_angle_gamma                90.00
_cell_volume                     3641.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    4516
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5471
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
   its'aim being to analyse the evolution of partial collection of data, 
   always carried out over the same part of reciprocal space, 
   and over a large scale of temperature.
   This  explain the poor completness of data as well as the low theta(max) value, 
   the low number of unique reflexions collected.
   In ordre to obtain significant intensities with an exposure time relatively short, 
   a crystal of neutron size was used. As the aim is to compare the diffraction data 
   always obtained from the same part of the crystal at different temperature, 
   problems of intensity scale are not considered to be of prior importance.
   The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
   over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
   these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
   or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
   but modelling this two conformations is over the scope 
  of this study of partial data collections.

;

_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5754
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         21.25
_reflns_number_total             3434
_reflns_number_gt                2862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0295P)²+2.1057P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3434
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0748
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29184(3) 0.28576(3) 0.06255(3) 0.04108(19) Uani 1 1 d . . .
S1 S 0.19306(5) 0.49215(7) -0.14437(5) 0.0533(3) Uani 1 1 d . . .
S2 S 0.42909(6) 0.07397(7) -0.10800(5) 0.0569(3) Uani 1 1 d . . .
N1 N 0.17550(16) 0.21796(17) 0.07965(16) 0.0372(7) Uani 1 1 d . . .
N2 N 0.27265(15) 0.37695(17) 0.15770(13) 0.0310(6) Uani 1 1 d . . .
C1 C 0.19545(18) 0.3829(2) 0.2045(2) 0.0316(8) Uani 1 1 d . . .
C2 C 0.4166(2) 0.1836(2) 0.1896(2) 0.0358(8) Uani 1 1 d . . .
C3 C 0.2191(2) 0.4206(3) -0.0708(2) 0.0442(9) Uani 1 1 d . . .
N3 N 0.32844(16) 0.19371(17) 0.15434(14) 0.0333(7) Uani 1 1 d . . .
C4 C 0.3426(2) 0.4215(2) 0.18183(19) 0.0373(8) Uani 1 1 d . . .
H4 H 0.3431 0.4593 0.2282 0.045 Uiso 1 1 calc R . .
C5 C 0.2631(2) 0.1519(2) 0.18494(18) 0.0358(8) Uani 1 1 d . . .
H5 H 0.2716 0.1144 0.2312 0.043 Uiso 1 1 calc R . .
N4 N 0.41059(15) 0.35533(19) 0.07245(17) 0.0403(7) Uani 1 1 d . . .
N5 N 0.3346(2) 0.2001(2) -0.01940(19) 0.0584(9) Uani 1 1 d . . .
C6 C 0.1756(2) 0.1643(2) 0.14565(19) 0.0351(8) Uani 1 1 d . . .
C7 C 0.0385(2) 0.4027(2) 0.2093(3) 0.0454(9) Uani 1 1 d . . .
H7 H -0.0181 0.4129 0.1832 0.054 Uiso 1 1 calc R . .
C8 C 0.1139(2) 0.3984(2) 0.16620(19) 0.0390(9) Uani 1 1 d . . .
H8 H 0.1095 0.4061 0.1100 0.047 Uiso 1 1 calc R . .
C9 C 0.0466(2) 0.3918(2) 0.2905(3) 0.0504(10) Uani 1 1 d . . .
C10 C 0.0991(2) 0.2270(2) 0.0368(2) 0.0488(9) Uani 1 1 d . . .
H10 H 0.0985 0.2627 -0.0108 0.059 Uiso 1 1 calc R . .
C11 C 0.4838(2) 0.1578(2) 0.1407(2) 0.0447(9) Uani 1 1 d . . .
H11 H 0.4703 0.1436 0.0862 0.054 Uiso 1 1 calc R . .
C12 C 0.3730(2) 0.1478(3) -0.0567(2) 0.0443(9) Uani 1 1 d . . .
C13 C 0.1279(2) 0.3765(3) 0.3294(2) 0.0565(10) Uani 1 1 d . . .
H13 H 0.1324 0.3695 0.3857 0.068 Uiso 1 1 calc R . .
C14 C 0.4367(2) 0.2045(2) 0.2688(2) 0.0408(9) Uani 1 1 d . . .
H14 H 0.3910 0.2227 0.3026 0.049 Uiso 1 1 calc R . .
C15 C 0.42101(19) 0.4122(2) 0.1357(2) 0.0395(9) Uani 1 1 d . . .
C16 C 0.5243(2) 0.1986(2) 0.2987(2) 0.0462(9) Uani 1 1 d . . .
H16 H 0.5385 0.2129 0.3530 0.055 Uiso 1 1 calc R . .
N6 N 0.69796(18) 0.15372(19) 0.3458(2) 0.0518(8) Uani 1 1 d . . .
C17 C 0.9668(2) 0.1163(2) 0.4188(2) 0.0498(10) Uani 1 1 d . . .
H17 H 1.0268 0.1052 0.4365 0.060 Uiso 1 1 calc R . .
N7 N 0.2378(2) 0.3712(2) -0.0182(2) 0.0571(9) Uani 1 1 d . . .
C18 C 0.0997(2) 0.1235(2) 0.1712(2) 0.0465(9) Uani 1 1 d . . .
H18 H 0.1016 0.0876 0.2186 0.056 Uiso 1 1 calc R . .
C19 C 0.5903(2) 0.1721(2) 0.2501(2) 0.0414(9) Uani 1 1 d . . .
N8 N 0.68470(18) 0.16345(19) 0.2734(2) 0.0484(8) Uani 1 1 d . . .
N9 N -0.0927(3) 0.3944(2) 0.31068(19) 0.0667(9) Uani 1 1 d . . .
N10 N -0.0280(2) 0.4002(2) 0.3509(2) 0.0756(11) Uani 1 1 d . . .
C20 C 0.0209(2) 0.1867(3) 0.0588(2) 0.0584(11) Uani 1 1 d . . .
H20 H -0.0322 0.1947 0.0266 0.070 Uiso 1 1 calc R . .
C21 C 0.7930(2) 0.1437(2) 0.3676(2) 0.0456(9) Uani 1 1 d . . .
C22 C 0.5703(2) 0.1527(2) 0.1713(2) 0.0470(9) Uani 1 1 d . . .
H22 H 0.6164 0.1357 0.1376 0.056 Uiso 1 1 calc R . .
C23 C 0.2019(2) 0.3716(2) 0.2861(2) 0.0459(9) Uani 1 1 d . . .
H23 H 0.2583 0.3603 0.3123 0.055 Uiso 1 1 calc R . .
C24 C 0.0204(2) 0.1353(3) 0.1270(2) 0.0570(10) Uani 1 1 d . . .
H24 H -0.0331 0.1083 0.1437 0.068 Uiso 1 1 calc R . .
C25 C 0.8600(2) 0.1629(3) 0.3160(2) 0.0554(10) Uani 1 1 d . . .
H25 H 0.8461 0.1848 0.2635 0.067 Uiso 1 1 calc R . .
C26 C 0.4783(2) 0.3471(3) 0.0253(2) 0.0619(11) Uani 1 1 d . . .
H26 H 0.4714 0.3087 -0.0205 0.074 Uiso 1 1 calc R . .
C27 C 0.9000(2) 0.0994(3) 0.4684(2) 0.0583(11) Uani 1 1 d . . .
H27 H 0.9135 0.0776 0.5210 0.070 Uiso 1 1 calc R . .
C28 C 0.9478(2) 0.1493(3) 0.3429(3) 0.0559(10) Uani 1 1 d . . .
H28 H 0.9948 0.1628 0.3090 0.067 Uiso 1 1 calc R . .
C29 C -0.1718(3) 0.4068(3) 0.3659(3) 0.0675(13) Uani 1 1 d . . .
C30 C 0.8130(2) 0.1139(3) 0.4429(2) 0.0542(10) Uani 1 1 d . . .
H30 H 0.7667 0.1030 0.4781 0.065 Uiso 1 1 calc R . .
C31 C 0.5575(3) 0.3916(3) 0.0399(3) 0.0806(14) Uani 1 1 d . . .
H31 H 0.6042 0.3840 0.0045 0.097 Uiso 1 1 calc R . .
C32 C 0.4996(2) 0.4580(3) 0.1550(2) 0.0609(11) Uani 1 1 d . . .
H32 H 0.5055 0.4962 0.2010 0.073 Uiso 1 1 calc R . .
C33 C -0.3231(3) 0.4364(3) 0.4463(3) 0.0666(12) Uani 1 1 d . . .
H33 H -0.3766 0.4461 0.4728 0.080 Uiso 1 1 calc R . .
C34 C -0.2513(3) 0.3901(3) 0.3289(3) 0.0723(13) Uani 1 1 d . . .
H34 H -0.2553 0.3689 0.2753 0.087 Uiso 1 1 calc R . .
C35 C -0.3263(3) 0.4042(3) 0.3696(3) 0.0681(12) Uani 1 1 d . . .
H35 H -0.3825 0.3912 0.3438 0.082 Uiso 1 1 calc R . .
C36 C -0.2424(3) 0.4547(3) 0.4852(3) 0.0724(12) Uani 1 1 d . . .
H36 H -0.2395 0.4773 0.5384 0.087 Uiso 1 1 calc R . .
C37 C -0.1637(3) 0.4392(3) 0.4442(3) 0.0714(13) Uani 1 1 d . . .
H37 H -0.1068 0.4507 0.4694 0.086 Uiso 1 1 calc R . .
C38 C 0.5695(2) 0.4469(3) 0.1056(3) 0.0804(14) Uani 1 1 d . . .
H38 H 0.6248 0.4771 0.1171 0.097 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.977(4) . ?
Fe1 N5 1.981(4) . ?
Fe1 N1 2.039(3) . ?
Fe1 N4 2.050(3) . ?
Fe1 N3 2.087(2) . ?
Fe1 N2 2.101(2) . ?
S1 C3 1.642(5) . ?
S2 C12 1.631(4) . ?
N1 C10 1.332(4) . ?
N1 C6 1.352(4) . ?
N2 C4 1.282(4) . ?
N2 C1 1.438(4) . ?
C1 C8 1.376(4) . ?
C1 C23 1.379(4) . ?
C2 C14 1.382(4) . ?
C2 C11 1.387(4) . ?
C2 N3 1.433(4) . ?
C3 N7 1.158(4) . ?
N3 C5 1.283(4) . ?
C4 C15 1.450(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.455(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.328(4) . ?
N4 C15 1.345(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.373(4) . ?
C7 C9 1.373(5) . ?
C7 C8 1.378(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.376(5) . ?
C9 N10 1.556(5) . ?
C10 C20 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C22 1.378(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.362(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.390(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.380(4) . ?
C16 C19 1.372(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.231(3) . ?
N6 C21 1.466(4) . ?
C17 C27 1.361(5) . ?
C17 C28 1.376(5) . ?
C17 H17 0.9500 . ?
C18 C24 1.385(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.371(4) . ?
C19 N8 1.460(4) . ?
N9 N10 1.160(4) . ?
N9 C29 1.556(5) . ?
C20 C24 1.364(5) . ?
C20 H20 0.9500 . ?
C21 C30 1.355(4) . ?
C21 C25 1.391(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.389(5) . ?
C25 H25 0.9500 . ?
C26 C31 1.365(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.373(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.343(6) . ?
C29 C37 1.396(6) . ?
C30 H30 0.9500 . ?
C31 C38 1.366(6) . ?
C31 H31 0.9500 . ?
C32 C38 1.382(5) . ?
C32 H32 0.9500 . ?
C33 C35 1.368(5) . ?
C33 C36 1.374(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.363(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.418(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 92.79(12) . . ?
N7 Fe1 N1 93.93(11) . . ?
N5 Fe1 N1 96.33(11) . . ?
N7 Fe1 N4 94.47(11) . . ?
N5 Fe1 N4 92.81(12) . . ?
N1 Fe1 N4 167.26(11) . . ?
N7 Fe1 N3 170.85(11) . . ?
N5 Fe1 N3 91.93(11) . . ?
N1 Fe1 N3 77.75(10) . . ?
N4 Fe1 N3 93.13(10) . . ?
N7 Fe1 N2 93.69(11) . . ?
N5 Fe1 N2 168.79(11) . . ?
N1 Fe1 N2 92.35(10) . . ?
N4 Fe1 N2 77.57(11) . . ?
N3 Fe1 N2 82.97(9) . . ?
C10 N1 C6 117.7(3) . . ?
C10 N1 Fe1 127.0(2) . . ?
C6 N1 Fe1 115.12(19) . . ?
C4 N2 C1 118.1(3) . . ?
C4 N2 Fe1 114.3(2) . . ?
C1 N2 Fe1 126.8(2) . . ?
C8 C1 C23 120.0(3) . . ?
C8 C1 N2 118.8(3) . . ?
C23 C1 N2 121.2(3) . . ?
C14 C2 C11 119.8(3) . . ?
C14 C2 N3 122.0(3) . . ?
C11 C2 N3 118.1(3) . . ?
N7 C3 S1 179.0(4) . . ?
C5 N3 C2 119.9(3) . . ?
C5 N3 Fe1 114.6(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 117.6(3) . . ?
N2 C4 H4 121.2 . . ?
C15 C4 H4 121.2 . . ?
N3 C5 C6 117.1(3) . . ?
N3 C5 H5 121.4 . . ?
C6 C5 H5 121.4 . . ?
C26 N4 C15 117.6(3) . . ?
C26 N4 Fe1 127.0(3) . . ?
C15 N4 Fe1 115.40(19) . . ?
C12 N5 Fe1 166.8(3) . . ?
N1 C6 C18 122.3(3) . . ?
N1 C6 C5 113.9(3) . . ?
C18 C6 C5 123.7(3) . . ?
C9 C7 C8 118.8(3) . . ?
C9 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C1 C8 C7 120.1(3) . . ?
C1 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C7 C9 C13 121.5(3) . . ?
C7 C9 N10 127.5(3) . . ?
C13 C9 N10 110.9(4) . . ?
N1 C10 C20 122.6(3) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
C22 C11 C2 119.9(3) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
N5 C12 S2 178.8(3) . . ?
C23 C13 C9 119.2(3) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C2 C14 C16 119.4(3) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
N4 C15 C32 122.8(3) . . ?
N4 C15 C4 114.4(3) . . ?
C32 C15 C4 122.8(4) . . ?
C19 C16 C14 120.4(3) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 111.4(3) . . ?
C27 C17 C28 120.2(3) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 169.1(3) . . ?
C6 C18 C24 119.2(3) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C22 C19 C16 120.0(3) . . ?
C22 C19 N8 113.9(3) . . ?
C16 C19 N8 126.1(3) . . ?
N6 N8 C19 112.4(3) . . ?
N10 N9 C29 106.8(4) . . ?
N9 N10 C9 103.1(4) . . ?
C24 C20 C10 119.6(3) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C30 C21 C25 120.7(3) . . ?
C30 C21 N6 115.6(3) . . ?
C25 C21 N6 123.7(3) . . ?
C19 C22 C11 120.4(3) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.4(3) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C20 C24 C18 118.4(3) . . ?
C20 C24 H24 120.8 . . ?
C18 C24 H24 120.8 . . ?
C28 C25 C21 118.5(3) . . ?
C28 C25 H25 120.7 . . ?
C21 C25 H25 120.7 . . ?
N4 C26 C31 122.8(4) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 120.3(4) . . ?
C17 C27 H27 119.9 . . ?
C30 C27 H27 119.9 . . ?
C17 C28 C25 120.0(3) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C34 C29 C37 122.0(3) . . ?
C34 C29 N9 113.3(4) . . ?
C37 C29 N9 124.5(4) . . ?
C21 C30 C27 120.2(3) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C26 C31 C38 119.9(4) . . ?
C26 C31 H31 120.0 . . ?
C38 C31 H31 120.0 . . ?
C15 C32 C38 118.3(4) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 118.9(4) . . ?
C29 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C34 C35 C33 122.1(4) . . ?
C34 C35 H35 119.0 . . ?
C33 C35 H35 119.0 . . ?
C33 C36 C37 118.7(4) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
C29 C37 C36 118.3(4) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 118.6(4) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.847
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.847
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.035
####################################################################### 
# 
# 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_feaza230kd1
_database_code_depnum_ccdc_archive 'CCDC 1492653'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0961(11)
_cell_length_b                   14.4493(11)
_cell_length_c                   16.9550(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.099(4)
_cell_angle_gamma                90.00
_cell_volume                     3693.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    4318
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5511
_exptl_absorpt_correction_T_max  0.8956
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
  its'aim being to analyse the evolution of partial collection of data, 
  always carried out over the same part of reciprocal space, 
  and over a large scale of temperature.
  This  explain the poor completness of data as well as the low theta(max) value, 
  the low number of unique reflexions collected.
  In ordre to obtain significant intensities with an exposure time relatively short, 
  a crystal of neutron size was used. As the aim is to compare the diffraction data 
  always obtained from the same part of the crystal at different temperature, 
  problems of intensity scale are not considered to be of prior importance.
  The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
  over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
  these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
  or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
  but modelling this two conformations is over the scope 
 of this study of partial data collections.
;

_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5827
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         21.31
_reflns_number_total             3484
_reflns_number_gt                2809
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0307P)²+2.2369P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3484
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29088(3) 0.28710(4) 0.05718(3) 0.0485(2) Uani 1 1 d . . .
S1 S 0.18994(6) 0.49732(8) -0.14658(6) 0.0616(3) Uani 1 1 d . . .
S2 S 0.43550(6) 0.07291(8) -0.10649(6) 0.0678(3) Uani 1 1 d . . .
N1 N 0.17172(17) 0.21618(19) 0.07891(17) 0.0469(7) Uani 1 1 d . . .
N2 N 0.27282(16) 0.37937(18) 0.15983(14) 0.0381(7) Uani 1 1 d . . .
C1 C 0.19704(19) 0.3846(2) 0.2070(2) 0.0378(8) Uani 1 1 d . . .
C2 C 0.4144(2) 0.1815(2) 0.1908(2) 0.0447(9) Uani 1 1 d . . .
C3 C 0.2138(2) 0.4254(3) -0.0750(2) 0.0504(10) Uani 1 1 d . . .
N3 N 0.32750(17) 0.19124(18) 0.15441(15) 0.0420(7) Uani 1 1 d . . .
C4 C 0.3440(2) 0.4202(2) 0.1843(2) 0.0451(9) Uani 1 1 d . . .
H4 H 0.3455 0.4549 0.2312 0.054 Uiso 1 1 calc R . .
C5 C 0.2616(2) 0.1522(2) 0.1842(2) 0.0459(9) Uani 1 1 d . . .
H5 H 0.2692 0.1162 0.2302 0.055 Uiso 1 1 calc R . .
N4 N 0.41359(17) 0.3598(2) 0.07389(19) 0.0523(8) Uani 1 1 d . . .
N5 N 0.3397(2) 0.2017(3) -0.0255(2) 0.0712(10) Uani 1 1 d . . .
C6 C 0.1734(2) 0.1646(2) 0.1452(2) 0.0447(9) Uani 1 1 d . . .
C7 C 0.0406(2) 0.4031(2) 0.2114(3) 0.0559(10) Uani 1 1 d . . .
H7 H -0.0153 0.4130 0.1857 0.067 Uiso 1 1 calc R . .
C8 C 0.1156(2) 0.3994(2) 0.1689(2) 0.0484(9) Uani 1 1 d . . .
H8 H 0.1112 0.4071 0.1138 0.058 Uiso 1 1 calc R . .
C9 C 0.0486(3) 0.3922(3) 0.2917(3) 0.0631(12) Uani 1 1 d . . .
C10 C 0.0939(3) 0.2258(3) 0.0385(2) 0.0603(11) Uani 1 1 d . . .
H10 H 0.0918 0.2607 -0.0083 0.072 Uiso 1 1 calc R . .
C11 C 0.4825(2) 0.1579(3) 0.1432(2) 0.0561(10) Uani 1 1 d . . .
H11 H 0.4698 0.1451 0.0894 0.067 Uiso 1 1 calc R . .
C12 C 0.3796(2) 0.1480(3) -0.0597(2) 0.0499(10) Uani 1 1 d . . .
C13 C 0.1296(3) 0.3773(3) 0.3302(2) 0.0690(12) Uani 1 1 d . . .
H13 H 0.1342 0.3702 0.3854 0.083 Uiso 1 1 calc R . .
C14 C 0.4334(2) 0.2015(2) 0.2696(2) 0.0537(10) Uani 1 1 d . . .
H14 H 0.3879 0.2187 0.3024 0.064 Uiso 1 1 calc R . .
C15 C 0.4228(2) 0.4125(3) 0.1392(2) 0.0484(9) Uani 1 1 d . . .
C16 C 0.5215(3) 0.1959(3) 0.2997(2) 0.0620(11) Uani 1 1 d . . .
H16 H 0.5354 0.2091 0.3532 0.074 Uiso 1 1 calc R . .
N6 N 0.6947(2) 0.1534(2) 0.3445(2) 0.0722(10) Uani 1 1 d . . .
C17 C 0.9644(2) 0.1170(3) 0.4183(3) 0.0639(11) Uani 1 1 d . . .
H17 H 1.0233 0.1062 0.4367 0.077 Uiso 1 1 calc R . .
N7 N 0.2306(2) 0.3751(2) -0.0230(2) 0.0659(10) Uani 1 1 d . . .
C18 C 0.0983(2) 0.1247(3) 0.1729(2) 0.0588(10) Uani 1 1 d . . .
H18 H 0.1015 0.0899 0.2198 0.071 Uiso 1 1 calc R . .
C19 C 0.5876(2) 0.1711(3) 0.2513(3) 0.0573(11) Uani 1 1 d . . .
N8 N 0.6845(2) 0.1629(2) 0.2747(2) 0.0676(10) Uani 1 1 d . . .
N9 N -0.0863(3) 0.3950(2) 0.3134(2) 0.0806(11) Uani 1 1 d . . .
N10 N -0.0259(3) 0.4015(3) 0.3548(3) 0.0945(14) Uani 1 1 d . . .
C20 C 0.0165(3) 0.1866(3) 0.0626(3) 0.0720(12) Uani 1 1 d . . .
H20 H -0.0369 0.1943 0.0322 0.086 Uiso 1 1 calc R . .
C21 C 0.7918(2) 0.1429(3) 0.3668(3) 0.0617(11) Uani 1 1 d . . .
C22 C 0.5684(2) 0.1529(3) 0.1737(3) 0.0622(11) Uani 1 1 d . . .
H22 H 0.6142 0.1369 0.1408 0.075 Uiso 1 1 calc R . .
C23 C 0.2031(2) 0.3729(3) 0.2876(2) 0.0554(10) Uani 1 1 d . . .
H23 H 0.2588 0.3619 0.3134 0.067 Uiso 1 1 calc R . .
C24 C 0.0181(3) 0.1368(3) 0.1307(3) 0.0706(12) Uani 1 1 d . . .
H24 H -0.0343 0.1110 0.1487 0.085 Uiso 1 1 calc R . .
C25 C 0.8587(3) 0.1621(3) 0.3160(2) 0.0704(12) Uani 1 1 d . . .
H25 H 0.8450 0.1833 0.2643 0.085 Uiso 1 1 calc R . .
C26 C 0.4827(3) 0.3534(3) 0.0291(3) 0.0802(13) Uani 1 1 d . . .
H26 H 0.4771 0.3177 -0.0173 0.096 Uiso 1 1 calc R . .
C27 C 0.8974(3) 0.1006(3) 0.4659(3) 0.0761(12) Uani 1 1 d . . .
H27 H 0.9106 0.0797 0.5177 0.091 Uiso 1 1 calc R . .
C28 C 0.9467(3) 0.1493(3) 0.3435(3) 0.0708(12) Uani 1 1 d . . .
H28 H 0.9934 0.1628 0.3108 0.085 Uiso 1 1 calc R . .
C29 C -0.1654(4) 0.4088(3) 0.3717(4) 0.0856(16) Uani 1 1 d . . .
C30 C 0.8114(3) 0.1136(3) 0.4407(3) 0.0744(12) Uani 1 1 d . . .
H30 H 0.7658 0.1021 0.4751 0.089 Uiso 1 1 calc R . .
C31 C 0.5622(3) 0.3969(4) 0.0476(4) 0.1063(18) Uani 1 1 d . . .
H31 H 0.6095 0.3914 0.0140 0.128 Uiso 1 1 calc R . .
C32 C 0.5013(3) 0.4561(3) 0.1616(3) 0.0738(12) Uani 1 1 d . . .
H32 H 0.5062 0.4910 0.2085 0.089 Uiso 1 1 calc R . .
C33 C -0.3165(3) 0.4371(3) 0.4500(3) 0.0803(13) Uani 1 1 d . . .
H33 H -0.3694 0.4462 0.4758 0.096 Uiso 1 1 calc R . .
C34 C -0.2448(3) 0.3898(3) 0.3350(3) 0.0847(14) Uani 1 1 d . . .
H34 H -0.2484 0.3674 0.2829 0.102 Uiso 1 1 calc R . .
C35 C -0.3192(3) 0.4036(3) 0.3747(3) 0.0799(13) Uani 1 1 d . . .
H35 H -0.3746 0.3897 0.3494 0.096 Uiso 1 1 calc R . .
C36 C -0.2362(3) 0.4574(3) 0.4880(3) 0.0858(14) Uani 1 1 d . . .
H36 H -0.2336 0.4809 0.5398 0.103 Uiso 1 1 calc R . .
C37 C -0.1578(3) 0.4425(3) 0.4483(4) 0.0873(15) Uani 1 1 d . . .
H37 H -0.1019 0.4552 0.4731 0.105 Uiso 1 1 calc R . .
C38 C 0.5720(3) 0.4481(4) 0.1150(4) 0.1045(17) Uani 1 1 d . . .
H38 H 0.6262 0.4772 0.1291 0.125 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.035(4) . ?
Fe1 N7 2.040(4) . ?
Fe1 N1 2.120(3) . ?
Fe1 N4 2.135(3) . ?
Fe1 N3 2.201(3) . ?
Fe1 N2 2.221(3) . ?
S1 C3 1.624(5) . ?
S2 C12 1.609(5) . ?
N1 C10 1.335(4) . ?
N1 C6 1.347(4) . ?
N2 C4 1.275(4) . ?
N2 C1 1.432(4) . ?
C1 C8 1.374(4) . ?
C1 C23 1.375(4) . ?
C2 C14 1.382(4) . ?
C2 C11 1.383(4) . ?
C2 N3 1.426(4) . ?
C3 N7 1.159(4) . ?
N3 C5 1.272(4) . ?
C4 C15 1.453(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.465(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.327(4) . ?
N4 C15 1.344(4) . ?
N5 C12 1.157(4) . ?
C6 C18 1.377(5) . ?
C7 C9 1.370(5) . ?
C7 C8 1.375(5) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.373(5) . ?
C9 N10 1.598(5) . ?
C10 C20 1.380(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.372(4) . ?
C11 H11 0.9400 . ?
C13 C23 1.358(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.402(5) . ?
C14 H14 0.9400 . ?
C15 C32 1.377(5) . ?
C16 C19 1.373(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.194(4) . ?
N6 C21 1.500(5) . ?
C17 C27 1.348(5) . ?
C17 C28 1.363(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.384(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.357(5) . ?
C19 N8 1.500(4) . ?
N9 N10 1.123(4) . ?
N9 C29 1.604(5) . ?
C20 C24 1.359(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.341(5) . ?
C21 C25 1.391(5) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.397(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.377(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.357(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.348(7) . ?
C29 C37 1.386(6) . ?
C30 H30 0.9400 . ?
C31 C38 1.361(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.368(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.365(6) . ?
C33 C36 1.373(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.355(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.409(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 94.85(13) . . ?
N5 Fe1 N1 99.72(12) . . ?
N7 Fe1 N1 93.73(12) . . ?
N5 Fe1 N4 92.63(13) . . ?
N7 Fe1 N4 97.71(12) . . ?
N1 Fe1 N4 162.38(12) . . ?
N5 Fe1 N3 92.78(12) . . ?
N7 Fe1 N3 167.60(11) . . ?
N1 Fe1 N3 75.33(11) . . ?
N4 Fe1 N3 91.68(11) . . ?
N5 Fe1 N2 165.47(11) . . ?
N7 Fe1 N2 94.51(11) . . ?
N1 Fe1 N2 90.72(10) . . ?
N4 Fe1 N2 75.10(11) . . ?
N3 Fe1 N2 80.05(9) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Fe1 126.3(3) . . ?
C6 N1 Fe1 115.7(2) . . ?
C4 N2 C1 118.6(3) . . ?
C4 N2 Fe1 113.3(2) . . ?
C1 N2 Fe1 127.2(2) . . ?
C8 C1 C23 119.7(3) . . ?
C8 C1 N2 117.9(3) . . ?
C23 C1 N2 122.4(3) . . ?
C14 C2 C11 119.6(3) . . ?
C14 C2 N3 122.3(3) . . ?
C11 C2 N3 117.9(3) . . ?
N7 C3 S1 179.0(4) . . ?
C5 N3 C2 120.4(3) . . ?
C5 N3 Fe1 114.0(2) . . ?
C2 N3 Fe1 125.0(2) . . ?
N2 C4 C15 119.6(3) . . ?
N2 C4 H4 120.2 . . ?
C15 C4 H4 120.2 . . ?
N3 C5 C6 118.5(3) . . ?
N3 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C26 N4 C15 117.5(3) . . ?
C26 N4 Fe1 126.4(3) . . ?
C15 N4 Fe1 116.0(2) . . ?
C12 N5 Fe1 165.8(3) . . ?
N1 C6 C18 122.5(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.6(4) . . ?
C9 C7 C8 119.0(3) . . ?
C9 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C1 C8 C7 120.1(3) . . ?
C1 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C7 C9 C13 121.3(3) . . ?
C7 C9 N10 128.9(4) . . ?
C13 C9 N10 109.7(4) . . ?
N1 C10 C20 122.7(4) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 120.7(3) . . ?
C22 C11 H11 119.7 . . ?
C2 C11 H11 119.7 . . ?
N5 C12 S2 179.4(4) . . ?
C23 C13 C9 119.2(4) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C2 C14 C16 118.9(3) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
N4 C15 C32 122.4(3) . . ?
N4 C15 C4 115.2(3) . . ?
C32 C15 C4 122.4(4) . . ?
C19 C16 C14 120.2(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 109.5(4) . . ?
C27 C17 C28 120.1(4) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 165.6(3) . . ?
C6 C18 C24 118.9(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.4(3) . . ?
C22 C19 N8 113.2(4) . . ?
C16 C19 N8 126.4(4) . . ?
N6 N8 C19 110.0(4) . . ?
N10 N9 C29 102.2(5) . . ?
N9 N10 C9 98.7(4) . . ?
C24 C20 C10 119.5(4) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C30 C21 C25 120.7(3) . . ?
C30 C21 N6 115.5(4) . . ?
C25 C21 N6 123.8(4) . . ?
C19 C22 C11 120.2(4) . . ?
C19 C22 H22 119.9 . . ?
C11 C22 H22 119.9 . . ?
C13 C23 C1 120.7(3) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 118.7(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.4(4) . . ?
C21 C25 H25 120.8 . . ?
C28 C25 H25 120.8 . . ?
N4 C26 C31 122.7(5) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 121.6(4) . . ?
C17 C27 H27 119.2 . . ?
C30 C27 H27 119.2 . . ?
C17 C28 C25 119.4(4) . . ?
C17 C28 H28 120.3 . . ?
C25 C28 H28 120.3 . . ?
C34 C29 C37 122.1(4) . . ?
C34 C29 N9 111.3(5) . . ?
C37 C29 N9 126.4(5) . . ?
C21 C30 C27 119.8(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.5(4) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C38 C32 C15 119.2(4) . . ?
C38 C32 H32 120.4 . . ?
C15 C32 H32 120.4 . . ?
C35 C33 C36 119.8(4) . . ?
C35 C33 H33 120.1 . . ?
C36 C33 H33 120.1 . . ?
C29 C34 C35 118.7(5) . . ?
C29 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C34 C35 C33 122.2(5) . . ?
C34 C35 H35 118.9 . . ?
C33 C35 H35 118.9 . . ?
C33 C36 C37 119.1(5) . . ?
C33 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C29 C37 C36 118.1(4) . . ?
C29 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?
C31 C38 C32 118.6(4) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.842
_diffrn_reflns_theta_full        21.31
_diffrn_measured_fraction_theta_full 0.842
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza245kd2
_database_code_depnum_ccdc_archive 'CCDC 1492654'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
     bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1081(7)
_cell_length_b                   14.4721(9)
_cell_length_c                   16.9844(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.095(4)
_cell_angle_gamma                90.00
_cell_volume                     3708.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    245(2)
_cell_measurement_reflns_used    4333
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      21.261

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5523
_exptl_absorpt_correction_T_max  0.8960
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
         its'aim being to analyse the evolution of partial collection of data, 
         always carried out over the same part of reciprocal space, 
         and over a large scale of temperature.
         This  explain the poor completness of data as well as the low theta(max) value, 
         the low number of unique reflexions collected.
         In ordre to obtain significant intensities with an exposure time relatively short, 
         a crystal of neutron size was used. As the aim is to compare the diffraction data 
         always obtained from the same part of the crystal at different temperature, 
         problems of intensity scale are not considered to be of prior importance.
         The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
         over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
         these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
         or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
         but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      245(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5431
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         21.26
_reflns_number_total             3776
_reflns_number_gt                3035
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0220P)²+2.3742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3776
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29099(3) 0.28735(3) 0.05649(3) 0.05016(19) Uani 1 1 d . . .
S1 S 0.18945(6) 0.49759(7) -0.14683(6) 0.0637(3) Uani 1 1 d . . .
S2 S 0.43625(6) 0.07289(7) -0.10639(6) 0.0711(3) Uani 1 1 d . . .
N1 N 0.17153(18) 0.21602(17) 0.07890(17) 0.0492(7) Uani 1 1 d . . .
N2 N 0.27312(16) 0.37952(16) 0.16028(15) 0.0397(6) Uani 1 1 d . . .
C1 C 0.1973(2) 0.38489(19) 0.2068(2) 0.0407(8) Uani 1 1 d . . .
C2 C 0.4141(2) 0.1810(2) 0.1911(2) 0.0470(9) Uani 1 1 d . . .
C3 C 0.2140(2) 0.4261(3) -0.0754(2) 0.0532(9) Uani 1 1 d . . .
N3 N 0.32745(18) 0.19086(17) 0.15449(15) 0.0445(7) Uani 1 1 d . . .
C4 C 0.3442(2) 0.4201(2) 0.1850(2) 0.0486(9) Uani 1 1 d . . .
H4 H 0.3457 0.4547 0.2319 0.058 Uiso 1 1 calc R . .
C5 C 0.2612(2) 0.1520(2) 0.1839(2) 0.0494(9) Uani 1 1 d . . .
H5 H 0.2687 0.1159 0.2297 0.059 Uiso 1 1 calc R . .
N4 N 0.41397(17) 0.36021(19) 0.07425(18) 0.0554(8) Uani 1 1 d . . .
N5 N 0.3410(2) 0.2021(2) -0.02630(19) 0.0733(9) Uani 1 1 d . . .
C6 C 0.1732(2) 0.1645(2) 0.1450(2) 0.0470(9) Uani 1 1 d . . .
C7 C 0.0407(2) 0.4036(2) 0.2123(3) 0.0616(10) Uani 1 1 d . . .
H7 H -0.0154 0.4139 0.1872 0.074 Uiso 1 1 calc R . .
C8 C 0.1155(2) 0.3995(2) 0.1686(2) 0.0513(9) Uani 1 1 d . . .
H8 H 0.1106 0.4067 0.1136 0.062 Uiso 1 1 calc R . .
C9 C 0.0494(3) 0.3924(2) 0.2925(3) 0.0670(12) Uani 1 1 d . . .
C10 C 0.0937(3) 0.2253(2) 0.0384(2) 0.0624(10) Uani 1 1 d . . .
H10 H 0.0917 0.2596 -0.0087 0.075 Uiso 1 1 calc R . .
C11 C 0.4819(2) 0.1576(2) 0.1434(2) 0.0596(10) Uani 1 1 d . . .
H11 H 0.4693 0.1452 0.0896 0.072 Uiso 1 1 calc R . .
C12 C 0.3805(2) 0.1480(3) -0.0598(2) 0.0520(9) Uani 1 1 d . . .
C13 C 0.1299(3) 0.3774(3) 0.3303(2) 0.0705(11) Uani 1 1 d . . .
H13 H 0.1348 0.3701 0.3853 0.085 Uiso 1 1 calc R . .
C14 C 0.4333(2) 0.2008(2) 0.2696(2) 0.0592(10) Uani 1 1 d . . .
H14 H 0.3879 0.2179 0.3024 0.071 Uiso 1 1 calc R . .
C15 C 0.4233(2) 0.4124(2) 0.1396(2) 0.0516(9) Uani 1 1 d . . .
C16 C 0.5210(3) 0.1952(2) 0.3000(2) 0.0666(11) Uani 1 1 d . . .
H16 H 0.5348 0.2083 0.3534 0.080 Uiso 1 1 calc R . .
N6 N 0.6933(2) 0.1536(2) 0.3439(3) 0.0797(10) Uani 1 1 d . . .
C17 C 0.9634(3) 0.1177(3) 0.4179(3) 0.0685(11) Uani 1 1 d . . .
H17 H 1.0223 0.1074 0.4362 0.082 Uiso 1 1 calc R . .
N7 N 0.2299(2) 0.3755(2) -0.0236(2) 0.0691(9) Uani 1 1 d . . .
C18 C 0.0981(2) 0.1249(2) 0.1731(2) 0.0620(10) Uani 1 1 d . . .
H18 H 0.1011 0.0905 0.2201 0.074 Uiso 1 1 calc R . .
C19 C 0.5866(2) 0.1706(2) 0.2515(3) 0.0611(11) Uani 1 1 d . . .
N8 N 0.6850(2) 0.1626(2) 0.2750(2) 0.0732(10) Uani 1 1 d . . .
N9 N -0.0851(3) 0.3953(2) 0.3138(2) 0.0849(11) Uani 1 1 d . . .
N10 N -0.0262(3) 0.4017(2) 0.3555(3) 0.0995(14) Uani 1 1 d . . .
C20 C 0.0159(3) 0.1869(3) 0.0626(3) 0.0771(12) Uani 1 1 d . . .
H20 H -0.0376 0.1950 0.0327 0.093 Uiso 1 1 calc R . .
C21 C 0.7917(2) 0.1428(2) 0.3662(3) 0.0655(11) Uani 1 1 d . . .
C22 C 0.5674(3) 0.1523(2) 0.1744(3) 0.0673(11) Uani 1 1 d . . .
H22 H 0.6132 0.1358 0.1417 0.081 Uiso 1 1 calc R . .
C23 C 0.2032(2) 0.3732(2) 0.2875(2) 0.0585(10) Uani 1 1 d . . .
H23 H 0.2589 0.3622 0.3133 0.070 Uiso 1 1 calc R . .
C24 C 0.0183(3) 0.1369(3) 0.1308(3) 0.0745(12) Uani 1 1 d . . .
H24 H -0.0340 0.1109 0.1488 0.089 Uiso 1 1 calc R . .
C25 C 0.8580(3) 0.1620(3) 0.3159(3) 0.0765(12) Uani 1 1 d . . .
H25 H 0.8443 0.1833 0.2644 0.092 Uiso 1 1 calc R . .
C26 C 0.4832(3) 0.3540(3) 0.0299(3) 0.0839(13) Uani 1 1 d . . .
H26 H 0.4778 0.3185 -0.0165 0.101 Uiso 1 1 calc R . .
C27 C 0.8970(3) 0.1010(3) 0.4657(3) 0.0811(12) Uani 1 1 d . . .
H27 H 0.9103 0.0801 0.5174 0.097 Uiso 1 1 calc R . .
C28 C 0.9459(3) 0.1491(3) 0.3435(3) 0.0765(12) Uani 1 1 d . . .
H28 H 0.9926 0.1620 0.3107 0.092 Uiso 1 1 calc R . .
C29 C -0.1648(4) 0.4088(3) 0.3714(4) 0.0909(17) Uani 1 1 d . . .
C30 C 0.8109(3) 0.1139(3) 0.4403(3) 0.0844(13) Uani 1 1 d . . .
H30 H 0.7652 0.1027 0.4745 0.101 Uiso 1 1 calc R . .
C31 C 0.5624(3) 0.3970(4) 0.0486(4) 0.1140(19) Uani 1 1 d . . .
H31 H 0.6097 0.3914 0.0151 0.137 Uiso 1 1 calc R . .
C32 C 0.5013(3) 0.4563(3) 0.1629(3) 0.0813(13) Uani 1 1 d . . .
H32 H 0.5059 0.4912 0.2097 0.098 Uiso 1 1 calc R . .
C33 C -0.3155(3) 0.4370(3) 0.4504(3) 0.0843(13) Uani 1 1 d . . .
H33 H -0.3684 0.4463 0.4761 0.101 Uiso 1 1 calc R . .
C34 C -0.2437(4) 0.3898(3) 0.3363(3) 0.0905(15) Uani 1 1 d . . .
H34 H -0.2475 0.3673 0.2843 0.109 Uiso 1 1 calc R . .
C35 C -0.3181(3) 0.4030(3) 0.3752(3) 0.0854(13) Uani 1 1 d . . .
H35 H -0.3733 0.3885 0.3500 0.102 Uiso 1 1 calc R . .
C36 C -0.2351(3) 0.4575(3) 0.4884(3) 0.0916(14) Uani 1 1 d . . .
H36 H -0.2321 0.4809 0.5401 0.110 Uiso 1 1 calc R . .
C37 C -0.1571(3) 0.4425(3) 0.4478(4) 0.0934(16) Uani 1 1 d . . .
H37 H -0.1011 0.4553 0.4722 0.112 Uiso 1 1 calc R . .
C38 C 0.5722(3) 0.4479(4) 0.1161(4) 0.1116(18) Uani 1 1 d . . .
H38 H 0.6265 0.4767 0.1303 0.134 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.046(4) . ?
Fe1 N7 2.048(4) . ?
Fe1 N1 2.131(3) . ?
Fe1 N4 2.143(3) . ?
Fe1 N3 2.219(3) . ?
Fe1 N2 2.238(3) . ?
S1 C3 1.622(5) . ?
S2 C12 1.609(4) . ?
N1 C10 1.337(4) . ?
N1 C6 1.348(4) . ?
N2 C4 1.275(4) . ?
N2 C1 1.428(4) . ?
C1 C23 1.380(4) . ?
C1 C8 1.380(4) . ?
C2 C14 1.379(5) . ?
C2 C11 1.382(5) . ?
C2 N3 1.426(4) . ?
C3 N7 1.160(4) . ?
N3 C5 1.273(4) . ?
C4 C15 1.461(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.463(4) . ?
C5 H5 0.9400 . ?
N4 C26 1.325(4) . ?
N4 C15 1.344(4) . ?
N5 C12 1.152(4) . ?
C6 C18 1.379(4) . ?
C7 C9 1.371(5) . ?
C7 C8 1.387(5) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 C13 1.362(5) . ?
C9 N10 1.612(5) . ?
C10 C20 1.383(5) . ?
C10 H10 0.9400 . ?
C11 C22 1.370(5) . ?
C11 H11 0.9400 . ?
C13 C23 1.358(5) . ?
C13 H13 0.9400 . ?
C14 C16 1.397(5) . ?
C14 H14 0.9400 . ?
C15 C32 1.379(5) . ?
C16 C19 1.369(5) . ?
C16 H16 0.9400 . ?
N6 N8 1.178(4) . ?
N6 C21 1.522(5) . ?
C17 C27 1.346(5) . ?
C17 C28 1.355(5) . ?
C17 H17 0.9400 . ?
C18 C24 1.381(5) . ?
C18 H18 0.9400 . ?
C19 C22 1.353(5) . ?
C19 N8 1.523(5) . ?
N9 N10 1.111(4) . ?
N9 C29 1.604(6) . ?
C20 C24 1.363(5) . ?
C20 H20 0.9400 . ?
C21 C30 1.342(5) . ?
C21 C25 1.379(6) . ?
C22 H22 0.9400 . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
C25 C28 1.398(5) . ?
C25 H25 0.9400 . ?
C26 C31 1.371(6) . ?
C26 H26 0.9400 . ?
C27 C30 1.360(5) . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 C34 1.333(7) . ?
C29 C37 1.385(7) . ?
C30 H30 0.9400 . ?
C31 C38 1.364(7) . ?
C31 H31 0.9400 . ?
C32 C38 1.374(6) . ?
C32 H32 0.9400 . ?
C33 C35 1.368(6) . ?
C33 C36 1.377(6) . ?
C33 H33 0.9400 . ?
C34 C35 1.348(5) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C36 C37 1.414(6) . ?
C36 H36 0.9400 . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?

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
N5 Fe1 N7 95.10(13) . . ?
N5 Fe1 N1 100.28(11) . . ?
N7 Fe1 N1 93.72(12) . . ?
N5 Fe1 N4 92.51(12) . . ?
N7 Fe1 N4 98.23(12) . . ?
N1 Fe1 N4 161.65(12) . . ?
N5 Fe1 N3 92.86(11) . . ?
N7 Fe1 N3 167.15(12) . . ?
N1 Fe1 N3 74.90(11) . . ?
N4 Fe1 N3 91.48(11) . . ?
N5 Fe1 N2 164.86(11) . . ?
N7 Fe1 N2 94.77(11) . . ?
N1 Fe1 N2 90.50(10) . . ?
N4 Fe1 N2 74.72(10) . . ?
N3 Fe1 N2 79.62(9) . . ?
C10 N1 C6 117.4(3) . . ?
C10 N1 Fe1 126.1(3) . . ?
C6 N1 Fe1 116.0(2) . . ?
C4 N2 C1 118.6(3) . . ?
C4 N2 Fe1 113.5(2) . . ?
C1 N2 Fe1 127.0(2) . . ?
C23 C1 C8 119.6(3) . . ?
C23 C1 N2 122.1(3) . . ?
C8 C1 N2 118.3(3) . . ?
C14 C2 C11 119.6(3) . . ?
C14 C2 N3 122.8(3) . . ?
C11 C2 N3 117.5(3) . . ?
N7 C3 S1 178.6(3) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.8(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 119.3(3) . . ?
N2 C4 H4 120.4 . . ?
C15 C4 H4 120.4 . . ?
N3 C5 C6 118.9(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C26 N4 C15 117.2(3) . . ?
C26 N4 Fe1 126.3(3) . . ?
C15 N4 Fe1 116.3(2) . . ?
C12 N5 Fe1 165.7(3) . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.5(3) . . ?
C9 C7 C8 119.3(3) . . ?
C9 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C1 C8 C7 119.4(3) . . ?
C1 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C13 C9 C7 121.4(3) . . ?
C13 C9 N10 110.4(4) . . ?
C7 C9 N10 128.0(4) . . ?
N1 C10 C20 123.0(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 120.1(4) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
N5 C12 S2 179.6(4) . . ?
C23 C13 C9 119.3(4) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C2 C14 C16 119.4(3) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
N4 C15 C32 123.1(3) . . ?
N4 C15 C4 115.3(3) . . ?
C32 C15 C4 121.6(4) . . ?
C19 C16 C14 119.7(4) . . ?
C19 C16 H16 120.1 . . ?
C14 C16 H16 120.1 . . ?
N8 N6 C21 108.0(4) . . ?
C27 C17 C28 120.6(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C3 N7 Fe1 164.8(3) . . ?
C6 C18 C24 118.7(4) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 120.6(3) . . ?
C22 C19 N8 113.2(4) . . ?
C16 C19 N8 126.2(4) . . ?
N6 N8 C19 108.6(4) . . ?
N10 N9 C29 101.6(5) . . ?
N9 N10 C9 98.2(5) . . ?
C24 C20 C10 118.8(4) . . ?
C24 C20 H20 120.6 . . ?
C10 C20 H20 120.6 . . ?
C30 C21 C25 121.1(4) . . ?
C30 C21 N6 115.1(4) . . ?
C25 C21 N6 123.8(4) . . ?
C19 C22 C11 120.6(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 121.0(3) . . ?
C13 C23 H23 119.5 . . ?
C1 C23 H23 119.5 . . ?
C20 C24 C18 119.4(4) . . ?
C20 C24 H24 120.3 . . ?
C18 C24 H24 120.3 . . ?
C21 C25 C28 118.3(4) . . ?
C21 C25 H25 120.8 . . ?
C28 C25 H25 120.8 . . ?
N4 C26 C31 122.9(5) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C17 C27 C30 121.0(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C17 C28 C25 119.4(4) . . ?
C17 C28 H28 120.3 . . ?
C25 C28 H28 120.3 . . ?
C34 C29 C37 121.3(4) . . ?
C34 C29 N9 112.6(5) . . ?
C37 C29 N9 126.0(5) . . ?
C21 C30 C27 119.6(4) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C38 C31 C26 119.6(4) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C38 C32 C15 118.3(5) . . ?
C38 C32 H32 120.9 . . ?
C15 C32 H32 120.9 . . ?
C35 C33 C36 119.7(4) . . ?
C35 C33 H33 120.1 . . ?
C36 C33 H33 120.1 . . ?
C29 C34 C35 120.1(5) . . ?
C29 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C33 121.7(5) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C33 C36 C37 118.4(5) . . ?
C33 C36 H36 120.8 . . ?
C37 C36 H36 120.8 . . ?
C29 C37 C36 118.8(5) . . ?
C29 C37 H37 120.6 . . ?
C36 C37 H37 120.6 . . ?
C31 C38 C32 118.8(5) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        21.26
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_feaza200km1
_database_code_depnum_ccdc_archive 'CCDC 1492655'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
   bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.0713(10)
_cell_length_b                   14.4223(11)
_cell_length_c                   16.8453(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.962(4)
_cell_angle_gamma                90.00
_cell_volume                     3656.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4318
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5482
_exptl_absorpt_correction_T_max  0.8946
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
 This experiment does not claim to be full or nearly data collection, 
         its'aim being to analyse the evolution of partial collection of data, 
         always carried out over the same part of reciprocal space, 
         and over a large scale of temperature.
         This  explain the poor completness of data as well as the low theta(max) value, 
         the low number of unique reflexions collected.
         In ordre to obtain significant intensities with an exposure time relatively short, 
         a crystal of neutron size was used. As the aim is to compare the diffraction data 
         always obtained from the same part of the crystal at different temperature, 
         problems of intensity scale are not considered to be of prior importance.
         The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
         over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
         these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
         or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
         but modelling this two conformations is over the scope 
  of this study of partial data collections.
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5753
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         21.23
_reflns_number_total             3432
_reflns_number_gt                2822
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0288P)²+2.0111P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3432
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29152(3) 0.28622(3) 0.06063(3) 0.0440(2) Uani 1 1 d . . .
S1 S 0.19205(5) 0.49432(7) -0.14521(5) 0.0567(3) Uani 1 1 d . . .
S2 S 0.43155(6) 0.07367(7) -0.10759(5) 0.0603(3) Uani 1 1 d . . .
N1 N 0.17416(16) 0.21717(18) 0.07947(16) 0.0406(7) Uani 1 1 d . . .
N2 N 0.27269(15) 0.37789(17) 0.15846(13) 0.0337(6) Uani 1 1 d . . .
C1 C 0.19600(18) 0.3836(2) 0.2057(2) 0.0338(8) Uani 1 1 d . . .
C2 C 0.4159(2) 0.1829(2) 0.1899(2) 0.0383(8) Uani 1 1 d . . .
C3 C 0.2173(2) 0.4223(3) -0.0723(2) 0.0474(10) Uani 1 1 d . . .
N3 N 0.32807(16) 0.19288(17) 0.15434(14) 0.0364(7) Uani 1 1 d . . .
C4 C 0.3430(2) 0.4211(2) 0.18286(18) 0.0391(8) Uani 1 1 d . . .
H4 H 0.3440 0.4577 0.2298 0.047 Uiso 1 1 calc R . .
C5 C 0.2626(2) 0.1522(2) 0.18468(18) 0.0394(8) Uani 1 1 d . . .
H5 H 0.2709 0.1154 0.2312 0.047 Uiso 1 1 calc R . .
N4 N 0.41145(16) 0.3569(2) 0.07286(17) 0.0442(7) Uani 1 1 d . . .
N5 N 0.3366(2) 0.2008(2) -0.02182(19) 0.0636(9) Uani 1 1 d . . .
C6 C 0.1749(2) 0.1640(2) 0.14562(19) 0.0382(8) Uani 1 1 d . . .
C7 C 0.0391(2) 0.4029(2) 0.2099(3) 0.0481(10) Uani 1 1 d . . .
H7 H -0.0175 0.4132 0.1838 0.058 Uiso 1 1 calc R . .
C8 C 0.1144(2) 0.3988(2) 0.16709(19) 0.0411(9) Uani 1 1 d . . .
H8 H 0.1102 0.4063 0.1110 0.049 Uiso 1 1 calc R . .
C9 C 0.0473(2) 0.3921(2) 0.2907(3) 0.0560(11) Uani 1 1 d . . .
C10 C 0.0975(2) 0.2262(2) 0.0376(2) 0.0526(10) Uani 1 1 d . . .
H10 H 0.0964 0.2617 -0.0100 0.063 Uiso 1 1 calc R . .
C11 C 0.4835(2) 0.1581(2) 0.1414(2) 0.0484(9) Uani 1 1 d . . .
H11 H 0.4703 0.1446 0.0869 0.058 Uiso 1 1 calc R . .
C12 C 0.3755(2) 0.1477(3) -0.0578(2) 0.0466(9) Uani 1 1 d . . .
C13 C 0.1284(2) 0.3771(3) 0.3296(2) 0.0594(10) Uani 1 1 d . . .
H13 H 0.1327 0.3703 0.3858 0.071 Uiso 1 1 calc R . .
C14 C 0.4355(2) 0.2036(2) 0.2691(2) 0.0444(9) Uani 1 1 d . . .
H14 H 0.3896 0.2214 0.3026 0.053 Uiso 1 1 calc R . .
C15 C 0.42144(19) 0.4126(2) 0.1367(2) 0.0419(9) Uani 1 1 d . . .
C16 C 0.5232(2) 0.1981(2) 0.2991(2) 0.0494(9) Uani 1 1 d . . .
H16 H 0.5372 0.2125 0.3533 0.059 Uiso 1 1 calc R . .
N6 N 0.69701(18) 0.1536(2) 0.3453(2) 0.0577(8) Uani 1 1 d . . .
C17 C 0.9664(2) 0.1167(2) 0.4182(3) 0.0539(10) Uani 1 1 d . . .
H17 H 1.0263 0.1060 0.4361 0.065 Uiso 1 1 calc R . .
N7 N 0.2355(2) 0.3727(2) -0.0200(2) 0.0625(9) Uani 1 1 d . . .
C18 C 0.0991(2) 0.1240(2) 0.1720(2) 0.0508(9) Uani 1 1 d . . .
H18 H 0.1013 0.0887 0.2197 0.061 Uiso 1 1 calc R . .
C19 C 0.5897(2) 0.1719(2) 0.2508(2) 0.0458(9) Uani 1 1 d . . .
N8 N 0.68466(19) 0.1632(2) 0.2735(2) 0.0552(8) Uani 1 1 d . . .
N9 N -0.0904(3) 0.3946(2) 0.31181(19) 0.0721(10) Uani 1 1 d . . .
N10 N -0.0273(2) 0.4008(2) 0.3526(2) 0.0813(12) Uani 1 1 d . . .
C20 C 0.0193(3) 0.1865(3) 0.0600(2) 0.0641(11) Uani 1 1 d . . .
H20 H -0.0341 0.1944 0.0283 0.077 Uiso 1 1 calc R . .
C21 C 0.7924(2) 0.1434(2) 0.3674(2) 0.0494(10) Uani 1 1 d . . .
C22 C 0.5695(2) 0.1530(2) 0.1723(2) 0.0521(10) Uani 1 1 d . . .
H22 H 0.6156 0.1362 0.1387 0.062 Uiso 1 1 calc R . .
C23 C 0.2024(2) 0.3722(2) 0.2870(2) 0.0483(9) Uani 1 1 d . . .
H23 H 0.2586 0.3608 0.3133 0.058 Uiso 1 1 calc R . .
C24 C 0.0198(2) 0.1357(3) 0.1285(2) 0.0609(11) Uani 1 1 d . . .
H24 H -0.0335 0.1090 0.1458 0.073 Uiso 1 1 calc R . .
C25 C 0.8598(2) 0.1631(3) 0.3161(2) 0.0589(10) Uani 1 1 d . . .
H25 H 0.8459 0.1854 0.2638 0.071 Uiso 1 1 calc R . .
C26 C 0.4799(3) 0.3494(3) 0.0262(2) 0.0682(11) Uani 1 1 d . . .
H26 H 0.4733 0.3119 -0.0202 0.082 Uiso 1 1 calc R . .
C27 C 0.8995(2) 0.0998(3) 0.4674(2) 0.0623(11) Uani 1 1 d . . .
H27 H 0.9132 0.0780 0.5199 0.075 Uiso 1 1 calc R . .
C28 C 0.9476(2) 0.1493(3) 0.3429(3) 0.0600(11) Uani 1 1 d . . .
H28 H 0.9944 0.1625 0.3090 0.072 Uiso 1 1 calc R . .
C29 C -0.1697(3) 0.4076(3) 0.3680(3) 0.0744(14) Uani 1 1 d . . .
C30 C 0.8125(2) 0.1137(3) 0.4422(2) 0.0599(10) Uani 1 1 d . . .
H30 H 0.7664 0.1025 0.4773 0.072 Uiso 1 1 calc R . .
C31 C 0.5590(3) 0.3933(4) 0.0423(3) 0.0887(15) Uani 1 1 d . . .
H31 H 0.6060 0.3861 0.0073 0.106 Uiso 1 1 calc R . .
C32 C 0.5000(2) 0.4575(3) 0.1573(2) 0.0657(11) Uani 1 1 d . . .
H32 H 0.5056 0.4946 0.2039 0.079 Uiso 1 1 calc R . .
C33 C -0.3206(3) 0.4367(3) 0.4479(3) 0.0704(12) Uani 1 1 d . . .
H33 H -0.3740 0.4460 0.4743 0.084 Uiso 1 1 calc R . .
C34 C -0.2490(3) 0.3899(3) 0.3314(3) 0.0775(13) Uani 1 1 d . . .
H34 H -0.2529 0.3679 0.2782 0.093 Uiso 1 1 calc R . .
C35 C -0.3232(3) 0.4040(3) 0.3715(3) 0.0716(12) Uani 1 1 d . . .
H35 H -0.3793 0.3907 0.3457 0.086 Uiso 1 1 calc R . .
C36 C -0.2399(3) 0.4558(3) 0.4861(3) 0.0771(12) Uani 1 1 d . . .
H36 H -0.2370 0.4790 0.5390 0.093 Uiso 1 1 calc R . .
C37 C -0.1614(3) 0.4406(3) 0.4459(3) 0.0765(13) Uani 1 1 d . . .
H37 H -0.1047 0.4524 0.4711 0.092 Uiso 1 1 calc R . .
C38 C 0.5706(3) 0.4474(4) 0.1085(4) 0.0886(14) Uani 1 1 d . . .
H38 H 0.6257 0.4775 0.1208 0.106 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N7 1.999(4) . ?
Fe1 N5 2.001(4) . ?
Fe1 N1 2.068(3) . ?
Fe1 N4 2.076(3) . ?
Fe1 N3 2.125(2) . ?
Fe1 N2 2.143(2) . ?
S1 C3 1.639(5) . ?
S2 C12 1.622(4) . ?
N1 C10 1.330(4) . ?
N1 C6 1.352(4) . ?
N2 C4 1.279(3) . ?
N2 C1 1.439(4) . ?
C1 C23 1.377(4) . ?
C1 C8 1.379(4) . ?
C2 C14 1.383(4) . ?
C2 C11 1.385(4) . ?
C2 N3 1.432(4) . ?
C3 N7 1.156(4) . ?
N3 C5 1.277(4) . ?
C4 C15 1.453(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.456(4) . ?
C5 H5 0.9500 . ?
N4 C26 1.333(4) . ?
N4 C15 1.344(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.373(4) . ?
C7 C9 1.370(5) . ?
C7 C8 1.377(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.374(5) . ?
C9 N10 1.577(5) . ?
C10 C20 1.379(5) . ?
C10 H10 0.9500 . ?
C11 C22 1.373(4) . ?
C11 H11 0.9500 . ?
C13 C23 1.360(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.393(4) . ?
C14 H14 0.9500 . ?
C15 C32 1.378(4) . ?
C16 C19 1.376(4) . ?
C16 H16 0.9500 . ?
N6 N8 1.221(3) . ?
N6 C21 1.474(4) . ?
C17 C27 1.361(5) . ?
C17 C28 1.368(5) . ?
C17 H17 0.9500 . ?
C18 C24 1.381(4) . ?
C18 H18 0.9500 . ?
C19 C22 1.369(4) . ?
C19 N8 1.468(4) . ?
N9 N10 1.148(4) . ?
N9 C29 1.574(5) . ?
C20 C24 1.366(5) . ?
C20 H20 0.9500 . ?
C21 C30 1.350(5) . ?
C21 C25 1.396(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.390(5) . ?
C25 H25 0.9500 . ?
C26 C31 1.364(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.372(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.340(6) . ?
C29 C37 1.396(6) . ?
C30 H30 0.9500 . ?
C31 C38 1.366(6) . ?
C31 H31 0.9500 . ?
C32 C38 1.386(5) . ?
C32 H32 0.9500 . ?
C33 C35 1.369(5) . ?
C33 C36 1.373(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.352(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.411(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 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
N7 Fe1 N5 93.39(13) . . ?
N7 Fe1 N1 94.02(11) . . ?
N5 Fe1 N1 97.67(11) . . ?
N7 Fe1 N4 95.51(11) . . ?
N5 Fe1 N4 92.66(12) . . ?
N1 Fe1 N4 165.49(11) . . ?
N7 Fe1 N3 169.76(11) . . ?
N5 Fe1 N3 92.37(11) . . ?
N1 Fe1 N3 76.82(10) . . ?
N4 Fe1 N3 92.67(10) . . ?
N7 Fe1 N2 93.98(11) . . ?
N5 Fe1 N2 167.58(11) . . ?
N1 Fe1 N2 91.76(9) . . ?
N4 Fe1 N2 76.69(11) . . ?
N3 Fe1 N2 81.91(9) . . ?
C10 N1 C6 117.6(3) . . ?
C10 N1 Fe1 126.7(2) . . ?
C6 N1 Fe1 115.4(2) . . ?
C4 N2 C1 118.1(3) . . ?
C4 N2 Fe1 114.0(2) . . ?
C1 N2 Fe1 127.1(2) . . ?
C23 C1 C8 120.2(3) . . ?
C23 C1 N2 121.7(3) . . ?
C8 C1 N2 118.0(3) . . ?
C14 C2 C11 119.9(3) . . ?
C14 C2 N3 121.9(3) . . ?
C11 C2 N3 118.1(3) . . ?
N7 C3 S1 178.8(4) . . ?
C5 N3 C2 120.2(3) . . ?
C5 N3 Fe1 114.4(2) . . ?
C2 N3 Fe1 125.0(2) . . ?
N2 C4 C15 118.1(3) . . ?
N2 C4 H4 121.0 . . ?
C15 C4 H4 121.0 . . ?
N3 C5 C6 117.9(3) . . ?
N3 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C26 N4 C15 117.6(3) . . ?
C26 N4 Fe1 126.7(3) . . ?
C15 N4 Fe1 115.69(19) . . ?
C12 N5 Fe1 166.4(3) . . ?
N1 C6 C18 122.3(3) . . ?
N1 C6 C5 114.0(3) . . ?
C18 C6 C5 123.7(3) . . ?
C9 C7 C8 118.8(3) . . ?
C9 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C7 C8 C1 119.9(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
C7 C9 C13 121.6(3) . . ?
C7 C9 N10 128.1(4) . . ?
C13 C9 N10 110.1(4) . . ?
N1 C10 C20 123.0(3) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 119.9(3) . . ?
C22 C11 H11 120.0 . . ?
C2 C11 H11 120.0 . . ?
N5 C12 S2 179.1(3) . . ?
C23 C13 C9 119.4(3) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.2(3) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
N4 C15 C32 122.8(3) . . ?
N4 C15 C4 114.7(3) . . ?
C32 C15 C4 122.5(4) . . ?
C19 C16 C14 120.6(3) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N8 N6 C21 111.0(3) . . ?
C27 C17 C28 120.1(3) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 168.1(3) . . ?
C6 C18 C24 119.2(3) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C22 C19 C16 119.5(3) . . ?
C22 C19 N8 113.6(3) . . ?
C16 C19 N8 126.8(3) . . ?
N6 N8 C19 111.4(3) . . ?
N10 N9 C29 105.2(4) . . ?
N9 N10 C9 101.2(4) . . ?
C24 C20 C10 119.2(3) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C30 C21 C25 120.5(3) . . ?
C30 C21 N6 115.9(3) . . ?
C25 C21 N6 123.6(3) . . ?
C19 C22 C11 120.9(3) . . ?
C19 C22 H22 119.5 . . ?
C11 C22 H22 119.5 . . ?
C13 C23 C1 120.1(3) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C20 C24 C18 118.7(3) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C28 C25 C21 118.7(3) . . ?
C28 C25 H25 120.7 . . ?
C21 C25 H25 120.7 . . ?
N4 C26 C31 122.6(4) . . ?
N4 C26 H26 118.7 . . ?
C31 C26 H26 118.7 . . ?
C17 C27 C30 120.7(4) . . ?
C17 C27 H27 119.6 . . ?
C30 C27 H27 119.6 . . ?
C17 C28 C25 119.9(3) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C34 C29 C37 122.2(3) . . ?
C34 C29 N9 112.8(5) . . ?
C37 C29 N9 124.9(5) . . ?
C21 C30 C27 120.0(3) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C26 C31 C38 120.1(4) . . ?
C26 C31 H31 119.9 . . ?
C38 C31 H31 119.9 . . ?
C15 C32 C38 118.5(4) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C35 C33 C36 119.5(4) . . ?
C35 C33 H33 120.3 . . ?
C36 C33 H33 120.3 . . ?
C29 C34 C35 118.9(4) . . ?
C29 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C34 C35 C33 122.4(4) . . ?
C34 C35 H35 118.8 . . ?
C33 C35 H35 118.8 . . ?
C33 C36 C37 119.2(4) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C29 C37 C36 117.9(4) . . ?
C29 C37 H37 121.1 . . ?
C36 C37 H37 121.1 . . ?
C31 C38 C32 118.3(4) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.846
_diffrn_reflns_theta_full        21.23
_diffrn_measured_fraction_theta_full 0.846
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.035
####################################################################### 
# 
# 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_feaza280km1
_database_code_depnum_ccdc_archive 'CCDC 1492656'
_audit_update_record             
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
    bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-iron(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Fe N10 S2'
_chemical_formula_weight         744.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1186(12)
_cell_length_b                   14.5293(12)
_cell_length_c                   17.0171(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.012(4)
_cell_angle_gamma                90.00
_cell_volume                     3732.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    280(2)
_cell_measurement_reflns_used    4420
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      22.986

_exptl_crystal_description       spearhead
_exptl_crystal_colour            black
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5542
_exptl_absorpt_correction_T_max  0.8966
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
This experiment does not claim to be full or nearly data collection, 
           its'aim being to analyse the evolution of partial collection of data, 
           always carried out over the same part of reciprocal space, 
           and over a large scale of temperature.
           This  explain the poor completness of data as well as the low theta(max) value, 
           the low number of unique reflexions collected.
           In ordre to obtain significant intensities with an exposure time relatively short, 
           a crystal of neutron size was used. As the aim is to compare the diffraction data 
           always obtained from the same part of the crystal at different temperature, 
           problems of intensity scale are not considered to be of prior importance.
           The authors are aware that the (phenylazo)aniline are disordered (conformationnal disorder 
           over two sites), this explain problems faced with the Hirshfeld Rigid-Bond Test for atoms of
           these ligands, as well as the one of small average C-C bond distance in their phenyl groups, 
           or the one of High Ueq as Compared to Neighbors for atoms of these ligands,
           but modelling this two conformations is over the scope 
   of this study of partial data collections.
;

_diffrn_ambient_temperature      280(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5876
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         21.25
_reflns_number_total             3507
_reflns_number_gt                2745
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0219P)²+2.2637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3507
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29184(3) 0.28761(4) 0.05551(3) 0.0569(2) Uani 1 1 d . . .
S1 S 0.18870(6) 0.49677(8) -0.14675(6) 0.0722(4) Uani 1 1 d . . .
S2 S 0.43685(7) 0.07277(8) -0.10637(6) 0.0817(4) Uani 1 1 d . . .
N1 N 0.17175(18) 0.2159(2) 0.07825(18) 0.0554(8) Uani 1 1 d . . .
N2 N 0.27359(18) 0.37987(19) 0.16054(15) 0.0457(7) Uani 1 1 d . . .
C1 C 0.1972(2) 0.3852(2) 0.2066(2) 0.0459(9) Uani 1 1 d . . .
C2 C 0.4142(2) 0.1809(2) 0.1914(2) 0.0530(10) Uani 1 1 d . . .
C3 C 0.2136(2) 0.4256(3) -0.0757(2) 0.0563(11) Uani 1 1 d . . .
N3 N 0.3278(2) 0.1907(2) 0.15409(16) 0.0525(8) Uani 1 1 d . . .
C4 C 0.3448(2) 0.4198(2) 0.1849(2) 0.0547(10) Uani 1 1 d . . .
H4 H 0.3462 0.4539 0.2313 0.066 Uiso 1 1 calc R . .
C5 C 0.2613(3) 0.1526(3) 0.1831(2) 0.0574(10) Uani 1 1 d . . .
H5 H 0.2683 0.1174 0.2287 0.069 Uiso 1 1 calc R . .
N4 N 0.41529(19) 0.3611(2) 0.0750(2) 0.0643(9) Uani 1 1 d . . .
N5 N 0.3428(2) 0.2029(3) -0.0271(2) 0.0846(12) Uani 1 1 d . . .
C6 C 0.1734(2) 0.1647(3) 0.1440(2) 0.0539(10) Uani 1 1 d . . .
C7 C 0.0413(2) 0.4032(3) 0.2106(3) 0.0689(12) Uani 1 1 d . . .
H7 H -0.0139 0.4129 0.1853 0.083 Uiso 1 1 calc R . .
C8 C 0.1160(2) 0.3992(2) 0.1685(2) 0.0588(10) Uani 1 1 d . . .
H8 H 0.1117 0.4061 0.1141 0.071 Uiso 1 1 calc R . .
C9 C 0.0491(3) 0.3925(3) 0.2907(4) 0.0769(14) Uani 1 1 d . . .
C10 C 0.0941(3) 0.2253(3) 0.0386(2) 0.0724(12) Uani 1 1 d . . .
H10 H 0.0920 0.2593 -0.0077 0.087 Uiso 1 1 calc R . .
C11 C 0.4825(3) 0.1578(3) 0.1448(2) 0.0691(12) Uani 1 1 d . . .
H11 H 0.4706 0.1455 0.0916 0.083 Uiso 1 1 calc R . .
C12 C 0.3820(2) 0.1485(3) -0.0601(2) 0.0588(11) Uani 1 1 d . . .
C13 C 0.1297(3) 0.3782(3) 0.3293(3) 0.0817(13) Uani 1 1 d . . .
H13 H 0.1340 0.3716 0.3837 0.098 Uiso 1 1 calc R . .
C14 C 0.4318(3) 0.2003(3) 0.2699(2) 0.0680(12) Uani 1 1 d . . .
H14 H 0.3865 0.2167 0.3020 0.082 Uiso 1 1 calc R . .
C15 C 0.4239(2) 0.4122(3) 0.1404(3) 0.0592(11) Uani 1 1 d . . .
C16 C 0.5191(3) 0.1950(3) 0.3000(3) 0.0795(13) Uani 1 1 d . . .
H16 H 0.5323 0.2082 0.3528 0.095 Uiso 1 1 calc R . .
N6 N 0.6922(3) 0.1539(3) 0.3428(3) 0.0970(13) Uani 1 1 d . . .
C17 C 0.9620(3) 0.1180(3) 0.4183(3) 0.0784(13) Uani 1 1 d . . .
H17 H 1.0200 0.1079 0.4373 0.094 Uiso 1 1 calc R . .
N7 N 0.2309(2) 0.3760(3) -0.0242(2) 0.0757(11) Uani 1 1 d . . .
C18 C 0.0988(3) 0.1255(3) 0.1722(2) 0.0722(12) Uani 1 1 d . . .
H18 H 0.1020 0.0915 0.2186 0.087 Uiso 1 1 calc R . .
C19 C 0.5858(3) 0.1705(3) 0.2527(3) 0.0743(13) Uani 1 1 d . . .
N8 N 0.6861(3) 0.1622(3) 0.2753(3) 0.0888(13) Uani 1 1 d . . .
N9 N -0.0828(3) 0.3957(3) 0.3129(2) 0.0957(13) Uani 1 1 d . . .
N10 N -0.0275(3) 0.4022(3) 0.3564(3) 0.1150(17) Uani 1 1 d . . .
C20 C 0.0165(3) 0.1871(3) 0.0625(3) 0.0874(14) Uani 1 1 d . . .
H20 H -0.0365 0.1953 0.0330 0.105 Uiso 1 1 calc R . .
C21 C 0.7914(3) 0.1428(3) 0.3648(4) 0.0800(14) Uani 1 1 d . . .
C22 C 0.5675(3) 0.1527(3) 0.1757(3) 0.0773(13) Uani 1 1 d . . .
H22 H 0.6130 0.1368 0.1435 0.093 Uiso 1 1 calc R . .
C23 C 0.2032(3) 0.3738(3) 0.2867(3) 0.0671(11) Uani 1 1 d . . .
H23 H 0.2581 0.3629 0.3122 0.081 Uiso 1 1 calc R . .
C24 C 0.0190(3) 0.1374(3) 0.1303(3) 0.0853(13) Uani 1 1 d . . .
H24 H -0.0326 0.1117 0.1482 0.102 Uiso 1 1 calc R . .
C25 C 0.8589(3) 0.1613(3) 0.3152(3) 0.0900(14) Uani 1 1 d . . .
H25 H 0.8463 0.1816 0.2640 0.108 Uiso 1 1 calc R . .
C26 C 0.4848(3) 0.3551(3) 0.0313(3) 0.0957(15) Uani 1 1 d . . .
H26 H 0.4799 0.3207 -0.0149 0.115 Uiso 1 1 calc R . .
C27 C 0.8955(3) 0.1023(3) 0.4645(3) 0.0950(15) Uani 1 1 d . . .
H27 H 0.9077 0.0823 0.5159 0.114 Uiso 1 1 calc R . .
C28 C 0.9462(3) 0.1488(3) 0.3437(3) 0.0883(14) Uani 1 1 d . . .
H28 H 0.9929 0.1613 0.3119 0.106 Uiso 1 1 calc R . .
C29 C -0.1630(4) 0.4091(4) 0.3740(5) 0.103(2) Uani 1 1 d . . .
C30 C 0.8107(3) 0.1147(4) 0.4383(3) 0.0997(16) Uani 1 1 d . . .
H30 H 0.7652 0.1036 0.4717 0.120 Uiso 1 1 calc R . .
C31 C 0.5642(4) 0.3979(5) 0.0516(5) 0.130(2) Uani 1 1 d . . .
H31 H 0.6117 0.3925 0.0192 0.156 Uiso 1 1 calc R . .
C32 C 0.5014(3) 0.4554(3) 0.1643(3) 0.0901(14) Uani 1 1 d . . .
H32 H 0.5052 0.4893 0.2107 0.108 Uiso 1 1 calc R . .
C33 C -0.3140(3) 0.4370(4) 0.4510(4) 0.0973(16) Uani 1 1 d . . .
H33 H -0.3665 0.4459 0.4762 0.117 Uiso 1 1 calc R . .
C34 C -0.2416(4) 0.3907(3) 0.3374(3) 0.1026(17) Uani 1 1 d . . .
H34 H -0.2446 0.3694 0.2858 0.123 Uiso 1 1 calc R . .
C35 C -0.3166(3) 0.4033(3) 0.3760(4) 0.0967(15) Uani 1 1 d . . .
H35 H -0.3710 0.3887 0.3511 0.116 Uiso 1 1 calc R . .
C36 C -0.2347(4) 0.4577(4) 0.4890(3) 0.1036(16) Uani 1 1 d . . .
H36 H -0.2326 0.4809 0.5400 0.124 Uiso 1 1 calc R . .
C37 C -0.1566(3) 0.4434(4) 0.4499(4) 0.1040(17) Uani 1 1 d . . .
H37 H -0.1016 0.4567 0.4744 0.125 Uiso 1 1 calc R . .
C38 C 0.5728(3) 0.4479(5) 0.1188(5) 0.126(2) Uani 1 1 d . . .
H38 H 0.6262 0.4764 0.1336 0.152 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.049(4) . ?
Fe1 N7 2.051(4) . ?
Fe1 N1 2.146(3) . ?
Fe1 N4 2.161(3) . ?
Fe1 N3 2.235(3) . ?
Fe1 N2 2.263(3) . ?
S1 C3 1.620(5) . ?
S2 C12 1.608(5) . ?
N1 C10 1.331(4) . ?
N1 C6 1.343(4) . ?
N2 C4 1.273(4) . ?
N2 C1 1.432(4) . ?
C1 C23 1.371(5) . ?
C1 C8 1.374(4) . ?
C2 C14 1.377(5) . ?
C2 C11 1.378(5) . ?
C2 N3 1.429(4) . ?
C3 N7 1.154(4) . ?
N3 C5 1.271(4) . ?
C4 C15 1.453(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.464(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.322(5) . ?
N4 C15 1.338(4) . ?
N5 C12 1.152(4) . ?
C6 C18 1.373(5) . ?
C7 C9 1.370(6) . ?
C7 C8 1.370(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.369(6) . ?
C9 N10 1.658(6) . ?
C10 C20 1.378(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.364(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.360(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.393(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.372(5) . ?
C16 C19 1.370(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.153(4) . ?
N6 C21 1.535(5) . ?
C17 C27 1.329(5) . ?
C17 C28 1.355(6) . ?
C17 H17 0.9300 . ?
C18 C24 1.380(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.351(5) . ?
C19 N8 1.549(5) . ?
N9 N10 1.092(4) . ?
N9 C29 1.650(6) . ?
C20 C24 1.360(6) . ?
C20 H20 0.9300 . ?
C21 C30 1.333(6) . ?
C21 C25 1.384(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.393(6) . ?
C25 H25 0.9300 . ?
C26 C31 1.380(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.348(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.339(7) . ?
C29 C37 1.383(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.355(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.366(6) . ?
C32 H32 0.9300 . ?
C33 C35 1.365(6) . ?
C33 C36 1.366(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.352(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.402(6) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 H38 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
N5 Fe1 N7 95.41(14) . . ?
N5 Fe1 N1 100.61(13) . . ?
N7 Fe1 N1 93.89(13) . . ?
N5 Fe1 N4 92.85(14) . . ?
N7 Fe1 N4 98.44(13) . . ?
N1 Fe1 N4 160.80(13) . . ?
N5 Fe1 N3 92.94(13) . . ?
N7 Fe1 N3 166.84(12) . . ?
N1 Fe1 N3 74.55(12) . . ?
N4 Fe1 N3 91.27(12) . . ?
N5 Fe1 N2 164.53(12) . . ?
N7 Fe1 N2 94.72(12) . . ?
N1 Fe1 N2 90.33(11) . . ?
N4 Fe1 N2 74.10(12) . . ?
N3 Fe1 N2 79.36(9) . . ?
C10 N1 C6 117.2(3) . . ?
C10 N1 Fe1 126.3(3) . . ?
C6 N1 Fe1 116.1(2) . . ?
C4 N2 C1 119.3(3) . . ?
C4 N2 Fe1 113.1(2) . . ?
C1 N2 Fe1 126.9(2) . . ?
C23 C1 C8 119.9(3) . . ?
C23 C1 N2 121.6(3) . . ?
C8 C1 N2 118.4(3) . . ?
C14 C2 C11 119.7(3) . . ?
C14 C2 N3 122.5(3) . . ?
C11 C2 N3 117.6(4) . . ?
N7 C3 S1 178.9(4) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.6(2) . . ?
C2 N3 Fe1 125.2(2) . . ?
N2 C4 C15 120.0(4) . . ?
N2 C4 H4 120.0 . . ?
C15 C4 H4 120.0 . . ?
N3 C5 C6 119.2(4) . . ?
N3 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C26 N4 C15 117.4(4) . . ?
C26 N4 Fe1 125.9(3) . . ?
C15 N4 Fe1 116.6(2) . . ?
C12 N5 Fe1 165.5(4) . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.2(4) . . ?
C9 C7 C8 119.1(4) . . ?
C9 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C7 C8 C1 119.9(4) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
C13 C9 C7 121.5(3) . . ?
C13 C9 N10 108.9(5) . . ?
C7 C9 N10 129.4(4) . . ?
N1 C10 C20 123.5(4) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
C22 C11 C2 120.7(4) . . ?
C22 C11 H11 119.6 . . ?
C2 C11 H11 119.6 . . ?
N5 C12 S2 179.8(5) . . ?
C23 C13 C9 118.9(4) . . ?
C23 C13 H13 120.6 . . ?
C9 C13 H13 120.6 . . ?
C2 C14 C16 118.5(4) . . ?
C2 C14 H14 120.7 . . ?
C16 C14 H14 120.7 . . ?
N4 C15 C32 122.9(4) . . ?
N4 C15 C4 115.4(3) . . ?
C32 C15 C4 121.6(5) . . ?
C19 C16 C14 120.7(4) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N8 N6 C21 106.3(4) . . ?
C27 C17 C28 120.6(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C3 N7 Fe1 165.7(3) . . ?
C6 C18 C24 118.7(4) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 120.1(4) . . ?
C22 C19 N8 112.0(4) . . ?
C16 C19 N8 127.9(5) . . ?
N6 N8 C19 106.4(4) . . ?
N10 N9 C29 97.1(5) . . ?
N9 N10 C9 94.1(5) . . ?
C24 C20 C10 118.6(4) . . ?
C24 C20 H20 120.7 . . ?
C10 C20 H20 120.7 . . ?
C30 C21 C25 120.0(4) . . ?
C30 C21 N6 115.1(5) . . ?
C25 C21 N6 125.0(5) . . ?
C19 C22 C11 120.3(4) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 120.7(4) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C20 C24 C18 119.3(4) . . ?
C20 C24 H24 120.3 . . ?
C18 C24 H24 120.3 . . ?
C21 C25 C28 118.5(4) . . ?
C21 C25 H25 120.7 . . ?
C28 C25 H25 120.7 . . ?
N4 C26 C31 122.4(5) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C17 C27 C30 121.2(5) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C17 C28 C25 119.2(4) . . ?
C17 C28 H28 120.4 . . ?
C25 C28 H28 120.4 . . ?
C34 C29 C37 121.6(4) . . ?
C34 C29 N9 110.3(6) . . ?
C37 C29 N9 127.8(6) . . ?
C21 C30 C27 120.6(5) . . ?
C21 C30 H30 119.7 . . ?
C27 C30 H30 119.7 . . ?
C38 C31 C26 119.8(5) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C38 C32 C15 119.0(5) . . ?
C38 C32 H32 120.5 . . ?
C15 C32 H32 120.5 . . ?
C35 C33 C36 120.2(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.5(6) . . ?
C29 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C33 121.3(5) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.9(5) . . ?
C33 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C29 C37 C36 118.5(5) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
C31 C38 C32 118.5(5) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.845
_diffrn_reflns_theta_full        21.25
_diffrn_measured_fraction_theta_full 0.845
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.032
