# 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_feaza290kd1
_database_code_depnum_ccdc_archive 'CCDC 1492657'
_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                   15.1215(12)
_cell_length_b                   14.5537(12)
_cell_length_c                   17.0259(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.957(4)
_cell_angle_gamma                90.00
_cell_volume                     3742.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    4434
_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    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5549
_exptl_absorpt_correction_T_max  0.8969
_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      290(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            6377
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_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         22.98
_reflns_number_total             3871
_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)+(0.0239P)²+2.0144P] 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         3871
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0806
_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 0.29219(3) 0.28766(4) 0.05535(3) 0.0602(2) Uani 1 1 d . . .
S1 S 0.18856(6) 0.49640(8) -0.14664(6) 0.0759(3) Uani 1 1 d . . .
S2 S 0.43674(7) 0.07271(8) -0.10658(6) 0.0864(4) Uani 1 1 d . . .
N1 N 0.17184(18) 0.2160(2) 0.07805(18) 0.0599(8) Uani 1 1 d . . .
N2 N 0.27368(17) 0.37986(19) 0.16040(15) 0.0492(7) Uani 1 1 d . . .
C1 C 0.1975(2) 0.3852(2) 0.2067(2) 0.0490(9) Uani 1 1 d . . .
C2 C 0.4142(2) 0.1807(2) 0.1913(2) 0.0559(10) Uani 1 1 d . . .
C3 C 0.2135(2) 0.4254(3) -0.0755(2) 0.0584(10) Uani 1 1 d . . .
N3 N 0.32771(19) 0.19050(19) 0.15402(16) 0.0552(8) Uani 1 1 d . . .
C4 C 0.3446(2) 0.4198(2) 0.1851(2) 0.0566(10) Uani 1 1 d . . .
H4 H 0.3459 0.4535 0.2316 0.068 Uiso 1 1 calc R . .
C5 C 0.2611(3) 0.1524(3) 0.1830(2) 0.0600(10) Uani 1 1 d . . .
H5 H 0.2679 0.1172 0.2286 0.072 Uiso 1 1 calc R . .
N4 N 0.41546(18) 0.3610(2) 0.0751(2) 0.0679(9) Uani 1 1 d . . .
N5 N 0.3436(2) 0.2027(3) -0.0272(2) 0.0868(11) Uani 1 1 d . . .
C6 C 0.1737(2) 0.1649(3) 0.1436(2) 0.0566(9) Uani 1 1 d . . .
C7 C 0.0414(2) 0.4030(3) 0.2106(3) 0.0729(12) Uani 1 1 d . . .
H7 H -0.0136 0.4125 0.1849 0.088 Uiso 1 1 calc R . .
C8 C 0.1164(2) 0.3994(2) 0.1686(2) 0.0613(10) Uani 1 1 d . . .
H8 H 0.1123 0.4066 0.1143 0.074 Uiso 1 1 calc R . .
C9 C 0.0482(3) 0.3925(3) 0.2900(4) 0.0798(14) Uani 1 1 d . . .
C10 C 0.0944(3) 0.2253(3) 0.0383(2) 0.0744(12) Uani 1 1 d . . .
H10 H 0.0921 0.2593 -0.0081 0.089 Uiso 1 1 calc R . .
C11 C 0.4826(3) 0.1578(3) 0.1450(2) 0.0724(11) Uani 1 1 d . . .
H11 H 0.4709 0.1459 0.0918 0.087 Uiso 1 1 calc R . .
C12 C 0.3823(2) 0.1485(3) -0.0606(2) 0.0609(10) Uani 1 1 d . . .
C13 C 0.1290(3) 0.3781(3) 0.3289(3) 0.0872(13) Uani 1 1 d . . .
H13 H 0.1331 0.3714 0.3833 0.105 Uiso 1 1 calc R . .
C14 C 0.4317(3) 0.2004(3) 0.2699(2) 0.0705(11) Uani 1 1 d . . .
H14 H 0.3863 0.2169 0.3019 0.085 Uiso 1 1 calc R . .
C15 C 0.4240(2) 0.4124(3) 0.1403(3) 0.0621(10) Uani 1 1 d . . .
C16 C 0.5190(3) 0.1950(3) 0.3004(3) 0.0841(13) Uani 1 1 d . . .
H16 H 0.5321 0.2083 0.3531 0.101 Uiso 1 1 calc R . .
N6 N 0.6916(3) 0.1539(3) 0.3427(3) 0.1020(13) Uani 1 1 d . . .
C17 C 0.9621(3) 0.1179(3) 0.4184(3) 0.0849(13) Uani 1 1 d . . .
H17 H 1.0200 0.1079 0.4376 0.102 Uiso 1 1 calc R . .
N7 N 0.2311(2) 0.3761(3) -0.0244(2) 0.0793(10) Uani 1 1 d . . .
C18 C 0.0993(3) 0.1256(3) 0.1718(2) 0.0762(12) Uani 1 1 d . . .
H18 H 0.1027 0.0916 0.2181 0.091 Uiso 1 1 calc R . .
C19 C 0.5855(3) 0.1701(3) 0.2532(3) 0.0800(13) Uani 1 1 d . . .
N8 N 0.6865(3) 0.1621(3) 0.2755(3) 0.0938(13) Uani 1 1 d . . .
N9 N -0.0822(3) 0.3955(3) 0.3128(2) 0.1000(13) Uani 1 1 d . . .
N10 N -0.0279(3) 0.4021(3) 0.3565(3) 0.1163(17) Uani 1 1 d . . .
C20 C 0.0173(3) 0.1866(3) 0.0629(3) 0.0892(14) Uani 1 1 d . . .
H20 H -0.0356 0.1945 0.0333 0.107 Uiso 1 1 calc R . .
C21 C 0.7916(2) 0.1433(3) 0.3646(4) 0.0849(14) Uani 1 1 d . . .
C22 C 0.5674(3) 0.1525(3) 0.1761(3) 0.0824(13) Uani 1 1 d . . .
H22 H 0.6130 0.1365 0.1441 0.099 Uiso 1 1 calc R . .
C23 C 0.2029(3) 0.3738(3) 0.2868(3) 0.0717(11) Uani 1 1 d . . .
H23 H 0.2577 0.3629 0.3125 0.086 Uiso 1 1 calc R . .
C24 C 0.0189(3) 0.1373(3) 0.1303(3) 0.0889(13) Uani 1 1 d . . .
H24 H -0.0327 0.1119 0.1483 0.107 Uiso 1 1 calc R . .
C25 C 0.8590(3) 0.1611(3) 0.3147(3) 0.0962(14) Uani 1 1 d . . .
H25 H 0.8466 0.1811 0.2635 0.115 Uiso 1 1 calc R . .
C26 C 0.4856(3) 0.3550(3) 0.0317(3) 0.1020(16) Uani 1 1 d . . .
H26 H 0.4814 0.3203 -0.0142 0.122 Uiso 1 1 calc R . .
C27 C 0.8950(3) 0.1024(3) 0.4642(3) 0.1020(16) Uani 1 1 d . . .
H27 H 0.9071 0.0824 0.5155 0.122 Uiso 1 1 calc R . .
C28 C 0.9461(3) 0.1481(3) 0.3440(3) 0.0935(14) Uani 1 1 d . . .
H28 H 0.9930 0.1603 0.3123 0.112 Uiso 1 1 calc R . .
C29 C -0.1612(4) 0.4101(3) 0.3754(4) 0.108(2) Uani 1 1 d . . .
C30 C 0.8100(3) 0.1149(4) 0.4383(3) 0.1072(16) Uani 1 1 d . . .
H30 H 0.7643 0.1037 0.4716 0.129 Uiso 1 1 calc R . .
C31 C 0.5647(4) 0.3987(5) 0.0522(5) 0.131(2) Uani 1 1 d . . .
H31 H 0.6123 0.3941 0.0199 0.158 Uiso 1 1 calc R . .
C32 C 0.5014(3) 0.4556(3) 0.1648(3) 0.0946(14) Uani 1 1 d . . .
H32 H 0.5051 0.4892 0.2113 0.114 Uiso 1 1 calc R . .
C33 C -0.3141(3) 0.4365(4) 0.4506(4) 0.1016(16) Uani 1 1 d . . .
H33 H -0.3667 0.4451 0.4756 0.122 Uiso 1 1 calc R . .
C34 C -0.2405(4) 0.3907(3) 0.3377(3) 0.1060(17) Uani 1 1 d . . .
H34 H -0.2429 0.3688 0.2863 0.127 Uiso 1 1 calc R . .
C35 C -0.3161(3) 0.4035(3) 0.3757(4) 0.1004(15) Uani 1 1 d . . .
H35 H -0.3703 0.3894 0.3503 0.121 Uiso 1 1 calc R . .
C36 C -0.2347(4) 0.4573(4) 0.4894(3) 0.1075(16) Uani 1 1 d . . .
H36 H -0.2330 0.4802 0.5404 0.129 Uiso 1 1 calc R . .
C37 C -0.1570(3) 0.4434(4) 0.4508(4) 0.1083(17) Uani 1 1 d . . .
H37 H -0.1025 0.4567 0.4761 0.130 Uiso 1 1 calc R . .
C38 C 0.5726(3) 0.4482(5) 0.1195(4) 0.133(2) Uani 1 1 d . . .
H38 H 0.6259 0.4766 0.1346 0.159 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 2.055(4) . ?
Fe1 N7 2.055(4) . ?
Fe1 N1 2.150(3) . ?
Fe1 N4 2.159(3) . ?
Fe1 N3 2.240(3) . ?
Fe1 N2 2.265(3) . ?
S1 C3 1.622(5) . ?
S2 C12 1.605(5) . ?
N1 C10 1.329(4) . ?
N1 C6 1.340(4) . ?
N2 C4 1.272(4) . ?
N2 C1 1.431(4) . ?
C1 C23 1.372(5) . ?
C1 C8 1.373(4) . ?
C2 C11 1.374(5) . ?
C2 C14 1.380(5) . ?
C2 N3 1.431(4) . ?
C3 N7 1.149(4) . ?
N3 C5 1.272(4) . ?
C4 C15 1.459(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.463(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.326(4) . ?
N4 C15 1.340(4) . ?
N5 C12 1.149(4) . ?
C6 C18 1.371(5) . ?
C7 C9 1.359(6) . ?
C7 C8 1.373(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.375(6) . ?
C9 N10 1.662(6) . ?
C10 C20 1.380(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.365(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.360(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.396(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.375(5) . ?
C16 C19 1.367(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.148(4) . ?
N6 C21 1.547(5) . ?
C17 C27 1.331(5) . ?
C17 C28 1.351(5) . ?
C17 H17 0.9300 . ?
C18 C24 1.384(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.351(5) . ?
C19 N8 1.559(5) . ?
N9 N10 1.083(4) . ?
N9 C29 1.655(6) . ?
C20 C24 1.352(5) . ?
C20 H20 0.9300 . ?
C21 C30 1.337(6) . ?
C21 C25 1.383(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.398(6) . ?
C25 H25 0.9300 . ?
C26 C31 1.384(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.350(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.361(7) . ?
C29 C37 1.372(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.353(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.360(6) . ?
C32 H32 0.9300 . ?
C33 C35 1.361(6) . ?
C33 C36 1.373(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.355(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.390(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 95.65(14) . . ?
N5 Fe1 N1 100.65(13) . . ?
N7 Fe1 N1 93.81(13) . . ?
N5 Fe1 N4 92.84(14) . . ?
N7 Fe1 N4 98.53(13) . . ?
N1 Fe1 N4 160.73(12) . . ?
N5 Fe1 N3 92.78(13) . . ?
N7 Fe1 N3 166.65(12) . . ?
N1 Fe1 N3 74.42(11) . . ?
N4 Fe1 N3 91.37(11) . . ?
N5 Fe1 N2 164.42(12) . . ?
N7 Fe1 N2 94.63(12) . . ?
N1 Fe1 N2 90.29(10) . . ?
N4 Fe1 N2 74.06(12) . . ?
N3 Fe1 N2 79.42(9) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Fe1 126.2(3) . . ?
C6 N1 Fe1 115.9(2) . . ?
C4 N2 C1 118.8(3) . . ?
C4 N2 Fe1 113.3(2) . . ?
C1 N2 Fe1 127.1(2) . . ?
C23 C1 C8 119.5(3) . . ?
C23 C1 N2 122.2(3) . . ?
C8 C1 N2 118.2(3) . . ?
C11 C2 C14 119.6(3) . . ?
C11 C2 N3 117.8(3) . . ?
C14 C2 N3 122.4(3) . . ?
N7 C3 S1 179.1(4) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.8(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 118.8(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C26 N4 C15 116.9(4) . . ?
C26 N4 Fe1 126.1(3) . . ?
C15 N4 Fe1 116.8(2) . . ?
C12 N5 Fe1 166.2(4) . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 115.6(3) . . ?
C18 C6 C5 121.7(4) . . ?
C9 C7 C8 119.4(4) . . ?
C9 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C1 C8 C7 120.1(4) . . ?
C1 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C7 C9 C13 121.1(3) . . ?
C7 C9 N10 130.4(4) . . ?
C13 C9 N10 108.3(5) . . ?
N1 C10 C20 122.7(4) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
C22 C11 C2 120.7(4) . . ?
C22 C11 H11 119.6 . . ?
C2 C11 H11 119.6 . . ?
N5 C12 S2 179.6(4) . . ?
C23 C13 C9 119.2(4) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C2 C14 C16 118.6(4) . . ?
C2 C14 H14 120.7 . . ?
C16 C14 H14 120.7 . . ?
N4 C15 C32 123.4(4) . . ?
N4 C15 C4 115.3(3) . . ?
C32 C15 C4 121.2(4) . . ?
C19 C16 C14 120.4(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 105.4(4) . . ?
C27 C17 C28 120.0(4) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C3 N7 Fe1 166.0(3) . . ?
C6 C18 C24 119.0(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.2(4) . . ?
C22 C19 N8 111.7(4) . . ?
C16 C19 N8 128.0(5) . . ?
N6 N8 C19 105.5(4) . . ?
N10 N9 C29 95.4(5) . . ?
N9 N10 C9 92.9(5) . . ?
C24 C20 C10 119.7(4) . . ?
C24 C20 H20 120.1 . . ?
C10 C20 H20 120.1 . . ?
C30 C21 C25 120.7(4) . . ?
C30 C21 N6 114.2(5) . . ?
C25 C21 N6 125.1(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 119.7 . . ?
C1 C23 H23 119.7 . . ?
C20 C24 C18 118.4(4) . . ?
C20 C24 H24 120.8 . . ?
C18 C24 H24 120.8 . . ?
C21 C25 C28 117.8(5) . . ?
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 121.9(5) . . ?
C17 C27 H27 119.1 . . ?
C30 C27 H27 119.1 . . ?
C17 C28 C25 119.9(4) . . ?
C17 C28 H28 120.1 . . ?
C25 C28 H28 120.1 . . ?
C34 C29 C37 120.8(4) . . ?
C34 C29 N9 108.6(6) . . ?
C37 C29 N9 130.4(6) . . ?
C21 C30 C27 119.8(5) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.7(5) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C38 C32 C15 118.6(5) . . ?
C38 C32 H32 120.7 . . ?
C15 C32 H32 120.7 . . ?
C35 C33 C36 120.3(4) . . ?
C35 C33 H33 119.8 . . ?
C36 C33 H33 119.8 . . ?
C35 C34 C29 119.4(5) . . ?
C35 C34 H34 120.3 . . ?
C29 C34 H34 120.3 . . ?
C34 C35 C33 121.2(5) . . ?
C34 C35 H35 119.4 . . ?
C33 C35 H35 119.4 . . ?
C33 C36 C37 118.7(5) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C29 C37 C36 119.6(5) . . ?
C29 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C31 C38 C32 119.0(5) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.745
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.745
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.150
_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_feaza275km2
_database_code_depnum_ccdc_archive 'CCDC 1492658'
_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                   15.1192(7)
_cell_length_b                   14.5268(9)
_cell_length_c                   17.0178(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.017(4)
_cell_angle_gamma                90.00
_cell_volume                     3732.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    275(2)
_cell_measurement_reflns_used    4508
_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      275(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            5903
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0474
_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         22.97
_reflns_number_total             4214
_reflns_number_gt                3217
_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)+(0.0165P)²+2.8616P] 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         4214
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0906
_refine_ls_wR_factor_gt          0.0810
_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 0.29174(3) 0.28754(3) 0.05565(3) 0.05546(19) Uani 1 1 d . . .
S1 S 0.18878(6) 0.49699(7) -0.14684(6) 0.0700(3) Uani 1 1 d . . .
S2 S 0.43679(7) 0.07274(8) -0.10643(7) 0.0790(3) Uani 1 1 d . . .
N1 N 0.17163(19) 0.21602(18) 0.07832(18) 0.0556(8) Uani 1 1 d . . .
N2 N 0.27349(17) 0.37995(17) 0.16056(15) 0.0449(7) Uani 1 1 d . . .
C1 C 0.1972(2) 0.3853(2) 0.2068(2) 0.0467(8) Uani 1 1 d . . .
C2 C 0.4140(2) 0.1809(2) 0.1913(2) 0.0523(9) Uani 1 1 d . . .
C3 C 0.2136(2) 0.4259(3) -0.0755(2) 0.0560(10) Uani 1 1 d . . .
N3 N 0.32771(19) 0.19036(18) 0.15433(16) 0.0503(7) Uani 1 1 d . . .
C4 C 0.3446(2) 0.4200(2) 0.1855(2) 0.0545(9) Uani 1 1 d . . .
H4 H 0.3460 0.4538 0.2320 0.065 Uiso 1 1 calc R . .
C5 C 0.2609(3) 0.1521(2) 0.1834(2) 0.0573(10) Uani 1 1 d . . .
H5 H 0.2678 0.1168 0.2289 0.069 Uiso 1 1 calc R . .
N4 N 0.41498(18) 0.3608(2) 0.07500(19) 0.0620(8) Uani 1 1 d . . .
N5 N 0.3426(2) 0.2027(2) -0.0270(2) 0.0813(10) Uani 1 1 d . . .
C6 C 0.1733(2) 0.1647(2) 0.1443(2) 0.0536(9) Uani 1 1 d . . .
C7 C 0.0411(2) 0.4033(2) 0.2115(3) 0.0676(11) Uani 1 1 d . . .
H7 H -0.0142 0.4131 0.1863 0.081 Uiso 1 1 calc R . .
C8 C 0.1160(2) 0.3996(2) 0.1683(2) 0.0572(10) Uani 1 1 d . . .
H8 H 0.1115 0.4067 0.1139 0.069 Uiso 1 1 calc R . .
C9 C 0.0486(3) 0.3926(3) 0.2915(3) 0.0741(13) Uani 1 1 d . . .
C10 C 0.0939(3) 0.2251(3) 0.0382(2) 0.0699(11) Uani 1 1 d . . .
H10 H 0.0918 0.2587 -0.0084 0.084 Uiso 1 1 calc R . .
C11 C 0.4821(3) 0.1573(3) 0.1443(2) 0.0675(11) Uani 1 1 d . . .
H11 H 0.4699 0.1447 0.0912 0.081 Uiso 1 1 calc R . .
C12 C 0.3818(2) 0.1483(3) -0.0603(2) 0.0571(10) Uani 1 1 d . . .
C13 C 0.1292(3) 0.3780(3) 0.3295(3) 0.0806(12) Uani 1 1 d . . .
H13 H 0.1336 0.3710 0.3839 0.097 Uiso 1 1 calc R . .
C14 C 0.4328(3) 0.2006(2) 0.2699(2) 0.0680(11) Uani 1 1 d . . .
H14 H 0.3878 0.2176 0.3021 0.082 Uiso 1 1 calc R . .
C15 C 0.4237(2) 0.4123(2) 0.1403(3) 0.0577(10) Uani 1 1 d . . .
C16 C 0.5202(3) 0.1948(3) 0.3003(3) 0.0761(12) Uani 1 1 d . . .
H16 H 0.5337 0.2076 0.3531 0.091 Uiso 1 1 calc R . .
N6 N 0.6917(3) 0.1539(2) 0.3432(3) 0.0939(12) Uani 1 1 d . . .
C17 C 0.9624(3) 0.1175(3) 0.4180(3) 0.0771(12) Uani 1 1 d . . .
H17 H 1.0204 0.1069 0.4366 0.093 Uiso 1 1 calc R . .
N7 N 0.2304(2) 0.3758(2) -0.0241(2) 0.0751(10) Uani 1 1 d . . .
C18 C 0.0985(3) 0.1254(2) 0.1726(3) 0.0696(11) Uani 1 1 d . . .
H18 H 0.1018 0.0915 0.2191 0.084 Uiso 1 1 calc R . .
C19 C 0.5860(3) 0.1702(3) 0.2524(3) 0.0722(12) Uani 1 1 d . . .
N8 N 0.6860(3) 0.1621(2) 0.2758(2) 0.0842(11) Uani 1 1 d . . .
N9 N -0.0837(3) 0.3957(2) 0.3133(2) 0.0942(13) Uani 1 1 d . . .
N10 N -0.0277(3) 0.4020(3) 0.3561(3) 0.1073(15) Uani 1 1 d . . .
C20 C 0.0165(3) 0.1868(3) 0.0626(3) 0.0827(13) Uani 1 1 d . . .
H20 H -0.0365 0.1946 0.0331 0.099 Uiso 1 1 calc R . .
C21 C 0.7916(2) 0.1431(3) 0.3652(4) 0.0773(13) Uani 1 1 d . . .
C22 C 0.5673(3) 0.1524(3) 0.1752(3) 0.0778(12) Uani 1 1 d . . .
H22 H 0.6127 0.1366 0.1430 0.093 Uiso 1 1 calc R . .
C23 C 0.2031(2) 0.3738(3) 0.2871(2) 0.0668(10) Uani 1 1 d . . .
H23 H 0.2579 0.3631 0.3127 0.080 Uiso 1 1 calc R . .
C24 C 0.0189(3) 0.1372(3) 0.1308(3) 0.0834(13) Uani 1 1 d . . .
H24 H -0.0327 0.1118 0.1489 0.100 Uiso 1 1 calc R . .
C25 C 0.8585(3) 0.1613(3) 0.3155(3) 0.0892(14) Uani 1 1 d . . .
H25 H 0.8458 0.1815 0.2643 0.107 Uiso 1 1 calc R . .
C26 C 0.4847(3) 0.3546(3) 0.0307(3) 0.0943(14) Uani 1 1 d . . .
H26 H 0.4797 0.3200 -0.0154 0.113 Uiso 1 1 calc R . .
C27 C 0.8957(3) 0.1017(3) 0.4649(3) 0.0926(14) Uani 1 1 d . . .
H27 H 0.9082 0.0818 0.5163 0.111 Uiso 1 1 calc R . .
C28 C 0.9462(3) 0.1484(3) 0.3444(3) 0.0863(13) Uani 1 1 d . . .
H28 H 0.9929 0.1612 0.3127 0.104 Uiso 1 1 calc R . .
C29 C -0.1625(4) 0.4093(3) 0.3735(4) 0.1004(19) Uani 1 1 d . . .
C30 C 0.8101(3) 0.1143(3) 0.4390(4) 0.0982(15) Uani 1 1 d . . .
H30 H 0.7645 0.1031 0.4723 0.118 Uiso 1 1 calc R . .
C31 C 0.5640(4) 0.3974(4) 0.0505(5) 0.128(2) Uani 1 1 d . . .
H31 H 0.6113 0.3918 0.0182 0.154 Uiso 1 1 calc R . .
C32 C 0.5017(3) 0.4557(3) 0.1644(3) 0.0890(14) Uani 1 1 d . . .
H32 H 0.5062 0.4892 0.2110 0.107 Uiso 1 1 calc R . .
C33 C -0.3140(3) 0.4367(3) 0.4506(3) 0.0933(14) Uani 1 1 d . . .
H33 H -0.3664 0.4455 0.4758 0.112 Uiso 1 1 calc R . .
C34 C -0.2413(4) 0.3902(3) 0.3379(3) 0.0999(17) Uani 1 1 d . . .
H34 H -0.2444 0.3679 0.2866 0.120 Uiso 1 1 calc R . .
C35 C -0.3166(3) 0.4032(3) 0.3758(3) 0.0933(14) Uani 1 1 d . . .
H35 H -0.3709 0.3890 0.3505 0.112 Uiso 1 1 calc R . .
C36 C -0.2343(4) 0.4577(3) 0.4889(3) 0.1028(15) Uani 1 1 d . . .
H36 H -0.2319 0.4808 0.5399 0.123 Uiso 1 1 calc R . .
C37 C -0.1564(3) 0.4433(3) 0.4488(4) 0.1013(17) Uani 1 1 d . . .
H37 H -0.1013 0.4567 0.4731 0.122 Uiso 1 1 calc R . .
C38 C 0.5727(3) 0.4479(4) 0.1174(5) 0.122(2) Uani 1 1 d . . .
H38 H 0.6261 0.4770 0.1315 0.147 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 2.050(4) . ?
Fe1 N7 2.053(4) . ?
Fe1 N1 2.145(3) . ?
Fe1 N4 2.156(3) . ?
Fe1 N3 2.239(3) . ?
Fe1 N2 2.262(3) . ?
S1 C3 1.622(4) . ?
S2 C12 1.606(4) . ?
N1 C10 1.335(4) . ?
N1 C6 1.347(4) . ?
N2 C4 1.276(4) . ?
N2 C1 1.432(4) . ?
C1 C23 1.374(5) . ?
C1 C8 1.378(4) . ?
C2 C11 1.380(5) . ?
C2 C14 1.383(5) . ?
C2 N3 1.425(4) . ?
C3 N7 1.156(4) . ?
N3 C5 1.276(4) . ?
C4 C15 1.460(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.462(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.332(4) . ?
N4 C15 1.340(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.376(5) . ?
C7 C9 1.368(6) . ?
C7 C8 1.384(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.366(6) . ?
C9 N10 1.640(6) . ?
C10 C20 1.379(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.368(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.363(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.396(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.381(5) . ?
C16 C19 1.367(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.151(4) . ?
N6 C21 1.545(5) . ?
C17 C27 1.338(6) . ?
C17 C28 1.341(6) . ?
C17 H17 0.9300 . ?
C18 C24 1.377(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.354(5) . ?
C19 N8 1.548(5) . ?
N9 N10 1.090(4) . ?
N9 C29 1.623(6) . ?
C20 C24 1.365(6) . ?
C20 H20 0.9300 . ?
C21 C30 1.339(6) . ?
C21 C25 1.376(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.403(6) . ?
C25 H25 0.9300 . ?
C26 C31 1.377(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.358(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.337(7) . ?
C29 C37 1.372(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.355(8) . ?
C31 H31 0.9300 . ?
C32 C38 1.376(7) . ?
C32 H32 0.9300 . ?
C33 C35 1.361(6) . ?
C33 C36 1.374(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.350(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.408(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 95.44(13) . . ?
N5 Fe1 N1 100.58(12) . . ?
N7 Fe1 N1 93.68(13) . . ?
N5 Fe1 N4 92.85(13) . . ?
N7 Fe1 N4 98.59(12) . . ?
N1 Fe1 N4 160.87(12) . . ?
N5 Fe1 N3 92.88(11) . . ?
N7 Fe1 N3 166.71(12) . . ?
N1 Fe1 N3 74.58(11) . . ?
N4 Fe1 N3 91.32(11) . . ?
N5 Fe1 N2 164.59(12) . . ?
N7 Fe1 N2 94.68(11) . . ?
N1 Fe1 N2 90.33(10) . . ?
N4 Fe1 N2 74.14(11) . . ?
N3 Fe1 N2 79.46(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 126.3(3) . . ?
C6 N1 Fe1 116.0(2) . . ?
C4 N2 C1 118.7(3) . . ?
C4 N2 Fe1 113.5(2) . . ?
C1 N2 Fe1 126.9(2) . . ?
C23 C1 C8 120.0(3) . . ?
C23 C1 N2 121.9(3) . . ?
C8 C1 N2 118.0(3) . . ?
C11 C2 C14 119.4(3) . . ?
C11 C2 N3 117.5(3) . . ?
C14 C2 N3 122.9(3) . . ?
N7 C3 S1 179.1(4) . . ?
C5 N3 C2 120.8(3) . . ?
C5 N3 Fe1 113.6(2) . . ?
C2 N3 Fe1 124.9(2) . . ?
N2 C4 C15 119.2(3) . . ?
N2 C4 H4 120.4 . . ?
C15 C4 H4 120.4 . . ?
N3 C5 C6 119.1(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C26 N4 C15 117.5(4) . . ?
C26 N4 Fe1 125.7(3) . . ?
C15 N4 Fe1 116.6(2) . . ?
C12 N5 Fe1 165.8(3) . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 115.2(3) . . ?
C18 C6 C5 122.0(4) . . ?
C9 C7 C8 119.8(4) . . ?
C9 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C1 C8 C7 119.1(4) . . ?
C1 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C13 C9 C7 121.0(3) . . ?
C13 C9 N10 109.7(4) . . ?
C7 C9 N10 129.2(4) . . ?
N1 C10 C20 122.9(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 120.4(4) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
N5 C12 S2 179.7(4) . . ?
C23 C13 C9 119.4(4) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.2(4) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
N4 C15 C32 123.1(4) . . ?
N4 C15 C4 115.7(3) . . ?
C32 C15 C4 121.3(4) . . ?
C19 C16 C14 120.0(4) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 105.8(4) . . ?
C27 C17 C28 120.6(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C3 N7 Fe1 165.3(3) . . ?
C6 C18 C24 118.6(4) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 120.5(4) . . ?
C22 C19 N8 112.8(4) . . ?
C16 C19 N8 126.7(4) . . ?
N6 N8 C19 106.6(4) . . ?
N10 N9 C29 98.0(5) . . ?
N9 N10 C9 95.5(5) . . ?
C24 C20 C10 119.0(4) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.8(4) . . ?
C30 C21 N6 114.3(5) . . ?
C25 C21 N6 124.9(5) . . ?
C19 C22 C11 120.5(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.7(4) . . ?
C13 C23 H23 119.7 . . ?
C1 C23 H23 119.7 . . ?
C20 C24 C18 119.2(4) . . ?
C20 C24 H24 120.4 . . ?
C18 C24 H24 120.4 . . ?
C21 C25 C28 118.1(5) . . ?
C21 C25 H25 121.0 . . ?
C28 C25 H25 121.0 . . ?
N4 C26 C31 122.3(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 119.6(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 120.8(4) . . ?
C34 C29 N9 110.8(6) . . ?
C37 C29 N9 128.1(6) . . ?
C21 C30 C27 119.7(5) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.8(5) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C38 C32 C15 118.1(5) . . ?
C38 C32 H32 121.0 . . ?
C15 C32 H32 121.0 . . ?
C35 C33 C36 120.3(4) . . ?
C35 C33 H33 119.8 . . ?
C36 C33 H33 119.8 . . ?
C29 C34 C35 120.6(5) . . ?
C29 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C33 120.8(5) . . ?
C34 C35 H35 119.6 . . ?
C33 C35 H35 119.6 . . ?
C33 C36 C37 118.2(5) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
C29 C37 C36 119.3(5) . . ?
C29 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C31 C38 C32 119.2(5) . . ?
C31 C38 H38 120.4 . . ?
C32 C38 H38 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.814
_diffrn_reflns_theta_full        22.97
_diffrn_measured_fraction_theta_full 0.815
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.185
_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_feaza140km1
_database_code_depnum_ccdc_archive 'CCDC 1492659'
_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(10)
_cell_length_b                   14.3798(10)
_cell_length_c                   16.6543(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.812(3)
_cell_angle_gamma                90.00
_cell_volume                     3589.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    4620
_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    1.378
_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  0.5429
_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      140(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            5659
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0357
_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         21.30
_reflns_number_total             3382
_reflns_number_gt                2985
_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+1.6277P] 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         3382
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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 0.29146(2) 0.28437(2) 0.06808(2) 0.02352(15) Uani 1 1 d . . .
S1 S 0.19528(4) 0.48715(5) -0.14265(4) 0.0305(2) Uani 1 1 d . . .
S2 S 0.42172(4) 0.07443(5) -0.10805(4) 0.0351(2) Uani 1 1 d . . .
N1 N 0.17768(12) 0.21960(14) 0.08010(12) 0.0223(5) Uani 1 1 d . . .
N2 N 0.27132(12) 0.37418(14) 0.15613(11) 0.0208(5) Uani 1 1 d . . .
C1 C 0.19346(15) 0.38070(17) 0.20306(17) 0.0204(6) Uani 1 1 d . . .
C2 C 0.41742(15) 0.18538(17) 0.18918(17) 0.0228(7) Uani 1 1 d . . .
C3 C 0.22296(15) 0.41652(19) -0.06814(17) 0.0234(7) Uani 1 1 d . . .
N3 N 0.32823(13) 0.19607(14) 0.15486(11) 0.0214(5) Uani 1 1 d . . .
C4 C 0.34047(16) 0.42151(18) 0.17887(15) 0.0251(6) Uani 1 1 d . . .
H4 H 0.3401 0.4616 0.2242 0.030 Uiso 1 1 calc R . .
C5 C 0.26353(16) 0.15202(18) 0.18577(15) 0.0244(6) Uani 1 1 d . . .
H5 H 0.2726 0.1138 0.2320 0.029 Uiso 1 1 calc R . .
N4 N 0.40710(12) 0.35073(15) 0.07100(13) 0.0247(5) Uani 1 1 d . . .
N5 N 0.32829(14) 0.19805(16) -0.01328(13) 0.0305(6) Uani 1 1 d . . .
C6 C 0.17594(15) 0.16387(18) 0.14616(15) 0.0232(6) Uani 1 1 d . . .
C7 C 0.03624(16) 0.40167(18) 0.20873(19) 0.0297(7) Uani 1 1 d . . .
H7 H -0.0205 0.4126 0.1826 0.036 Uiso 1 1 calc R . .
C8 C 0.11128(16) 0.39681(17) 0.16464(15) 0.0251(7) Uani 1 1 d . . .
H8 H 0.1066 0.4045 0.1079 0.030 Uiso 1 1 calc R . .
C9 C 0.04399(17) 0.39048(18) 0.29150(19) 0.0297(7) Uani 1 1 d . . .
C10 C 0.10209(17) 0.22832(18) 0.03510(15) 0.0284(7) Uani 1 1 d . . .
H10 H 0.1025 0.2650 -0.0123 0.034 Uiso 1 1 calc R . .
C11 C 0.48355(16) 0.15768(19) 0.13922(16) 0.0303(7) Uani 1 1 d . . .
H11 H 0.4691 0.1425 0.0846 0.036 Uiso 1 1 calc R . .
C12 C 0.36601(16) 0.14659(19) -0.05320(16) 0.0250(7) Uani 1 1 d . . .
C13 C 0.12614(18) 0.3753(2) 0.32950(17) 0.0363(7) Uani 1 1 d . . .
H13 H 0.1313 0.3691 0.3863 0.044 Uiso 1 1 calc R . .
C14 C 0.43792(16) 0.20748(18) 0.26867(16) 0.0266(7) Uani 1 1 d . . .
H14 H 0.3924 0.2270 0.3025 0.032 Uiso 1 1 calc R . .
C15 C 0.41905(15) 0.41146(18) 0.13279(16) 0.0258(7) Uani 1 1 d . . .
C16 C 0.52583(16) 0.20090(18) 0.29869(16) 0.0283(7) Uani 1 1 d . . .
H16 H 0.5405 0.2159 0.3533 0.034 Uiso 1 1 calc R . .
N6 N 0.69970(13) 0.15415(15) 0.34682(15) 0.0311(6) Uani 1 1 d . . .
C17 C 0.96892(17) 0.11466(19) 0.41876(18) 0.0326(7) Uani 1 1 d . . .
H17 H 1.0293 0.1030 0.4356 0.039 Uiso 1 1 calc R . .
N7 N 0.24330(13) 0.36778(16) -0.01441(14) 0.0284(6) Uani 1 1 d . . .
C18 C 0.09890(16) 0.12178(18) 0.16937(15) 0.0283(7) Uani 1 1 d . . .
H18 H 0.0994 0.0849 0.2167 0.034 Uiso 1 1 calc R . .
C19 C 0.59169(16) 0.17254(18) 0.24912(16) 0.0246(7) Uani 1 1 d . . .
N8 N 0.68471(13) 0.16264(15) 0.27264(15) 0.0298(6) Uani 1 1 d . . .
N9 N -0.10211(16) 0.39275(15) 0.30782(13) 0.0370(6) Uani 1 1 d . . .
N10 N -0.02961(16) 0.39786(16) 0.34568(14) 0.0401(6) Uani 1 1 d . . .
C20 C 0.02330(17) 0.1863(2) 0.05458(17) 0.0341(7) Uani 1 1 d . . .
H20 H -0.0290 0.1938 0.0207 0.041 Uiso 1 1 calc R . .
C21 C 0.79377(16) 0.14385(18) 0.36874(17) 0.0270(7) Uani 1 1 d . . .
C22 C 0.57086(16) 0.15230(18) 0.16972(17) 0.0301(7) Uani 1 1 d . . .
H22 H 0.6167 0.1345 0.1355 0.036 Uiso 1 1 calc R . .
C23 C 0.20054(17) 0.36927(19) 0.28518(18) 0.0308(7) Uani 1 1 d . . .
H23 H 0.2571 0.3571 0.3112 0.037 Uiso 1 1 calc R . .
C24 C 0.02087(17) 0.13379(19) 0.12300(17) 0.0340(7) Uani 1 1 d . . .
H24 H -0.0333 0.1062 0.1383 0.041 Uiso 1 1 calc R . .
C25 C 0.86072(17) 0.16274(19) 0.31667(17) 0.0339(7) Uani 1 1 d . . .
H25 H 0.8465 0.1853 0.2640 0.041 Uiso 1 1 calc R . .
C26 C 0.47409(17) 0.3406(2) 0.02198(17) 0.0358(7) Uani 1 1 d . . .
H26 H 0.4662 0.3001 -0.0229 0.043 Uiso 1 1 calc R . .
C27 C 0.90241(17) 0.09811(19) 0.47018(17) 0.0371(8) Uani 1 1 d . . .
H27 H 0.9167 0.0760 0.5230 0.045 Uiso 1 1 calc R . .
C28 C 0.94864(17) 0.14822(19) 0.34267(18) 0.0350(7) Uani 1 1 d . . .
H28 H 0.9952 0.1615 0.3078 0.042 Uiso 1 1 calc R . .
C29 C -0.17844(18) 0.40581(19) 0.3584(2) 0.0352(8) Uani 1 1 d . . .
C30 C 0.81419(17) 0.11364(19) 0.44519(17) 0.0337(7) Uani 1 1 d . . .
H30 H 0.7680 0.1033 0.4812 0.040 Uiso 1 1 calc R . .
C31 C 0.55418(18) 0.3865(2) 0.0337(2) 0.0454(8) Uani 1 1 d . . .
H31 H 0.6001 0.3777 -0.0028 0.054 Uiso 1 1 calc R . .
C32 C 0.49808(17) 0.4582(2) 0.14882(17) 0.0373(7) Uani 1 1 d . . .
H32 H 0.5049 0.4989 0.1936 0.045 Uiso 1 1 calc R . .
C33 C -0.33058(19) 0.4349(2) 0.4405(2) 0.0444(8) Uani 1 1 d . . .
H33 H -0.3836 0.4444 0.4683 0.053 Uiso 1 1 calc R . .
C34 C -0.25954(19) 0.39087(19) 0.32065(18) 0.0395(8) Uani 1 1 d . . .
H34 H -0.2637 0.3705 0.2663 0.047 Uiso 1 1 calc R . .
C35 C -0.33584(19) 0.4055(2) 0.3618(2) 0.0435(8) Uani 1 1 d . . .
H35 H -0.3926 0.3951 0.3356 0.052 Uiso 1 1 calc R . .
C36 C -0.24850(19) 0.4505(2) 0.47923(19) 0.0458(8) Uani 1 1 d . . .
H36 H -0.2449 0.4711 0.5335 0.055 Uiso 1 1 calc R . .
C37 C -0.17049(18) 0.4359(2) 0.4378(2) 0.0428(8) Uani 1 1 d . . .
H37 H -0.1134 0.4463 0.4635 0.051 Uiso 1 1 calc R . .
C38 C 0.56752(18) 0.4447(2) 0.0981(2) 0.0471(8) Uani 1 1 d . . .
H38 H 0.6232 0.4751 0.1079 0.057 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(3) . ?
Fe1 N5 1.938(2) . ?
Fe1 N1 1.9637(19) . ?
Fe1 N4 1.979(2) . ?
Fe1 N3 1.982(2) . ?
Fe1 N2 1.988(2) . ?
S1 C3 1.641(3) . ?
S2 C12 1.639(3) . ?
N1 C10 1.334(3) . ?
N1 C6 1.363(3) . ?
N2 C4 1.283(3) . ?
N2 C1 1.440(3) . ?
C1 C23 1.376(3) . ?
C1 C8 1.381(3) . ?
C2 C14 1.381(3) . ?
C2 C11 1.384(3) . ?
C2 N3 1.438(3) . ?
C3 N7 1.165(3) . ?
N3 C5 1.288(3) . ?
C4 C15 1.445(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.452(3) . ?
C5 H5 0.9500 . ?
N4 C26 1.334(3) . ?
N4 C15 1.355(3) . ?
N5 C12 1.161(3) . ?
C6 C18 1.377(3) . ?
C7 C8 1.376(3) . ?
C7 C9 1.387(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C13 1.375(4) . ?
C9 N10 1.464(3) . ?
C10 C20 1.381(3) . ?
C10 H10 0.9500 . ?
C11 C22 1.384(3) . ?
C11 H11 0.9500 . ?
C13 C23 1.371(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.391(3) . ?
C14 H14 0.9500 . ?
C15 C32 1.378(3) . ?
C16 C19 1.380(3) . ?
C16 H16 0.9500 . ?
N6 N8 1.251(3) . ?
N6 C21 1.448(3) . ?
C17 C27 1.368(3) . ?
C17 C28 1.376(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.382(3) . ?
C18 H18 0.9500 . ?
C19 C22 1.375(3) . ?
C19 N8 1.438(3) . ?
N9 N10 1.233(3) . ?
N9 C29 1.466(3) . ?
C20 C24 1.369(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.366(3) . ?
C21 C25 1.386(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C28 1.384(3) . ?
C25 H25 0.9500 . ?
C26 C31 1.376(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.386(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.359(4) . ?
C29 C37 1.392(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.367(4) . ?
C31 H31 0.9500 . ?
C32 C38 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C35 1.375(4) . ?
C33 C36 1.381(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.403(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 90.57(9) . . ?
N7 Fe1 N1 94.01(8) . . ?
N5 Fe1 N1 92.68(8) . . ?
N7 Fe1 N4 90.87(8) . . ?
N5 Fe1 N4 92.65(9) . . ?
N1 Fe1 N4 172.74(9) . . ?
N7 Fe1 N3 174.27(8) . . ?
N5 Fe1 N3 91.19(8) . . ?
N1 Fe1 N3 80.46(8) . . ?
N4 Fe1 N3 94.50(8) . . ?
N7 Fe1 N2 93.21(8) . . ?
N5 Fe1 N2 172.14(8) . . ?
N1 Fe1 N2 93.93(8) . . ?
N4 Fe1 N2 80.41(8) . . ?
N3 Fe1 N2 85.72(8) . . ?
C10 N1 C6 117.3(2) . . ?
C10 N1 Fe1 128.15(18) . . ?
C6 N1 Fe1 114.36(15) . . ?
C4 N2 C1 118.1(2) . . ?
C4 N2 Fe1 114.36(16) . . ?
C1 N2 Fe1 126.81(16) . . ?
C23 C1 C8 120.3(2) . . ?
C23 C1 N2 120.4(2) . . ?
C8 C1 N2 119.3(2) . . ?
C14 C2 C11 120.6(2) . . ?
C14 C2 N3 121.0(2) . . ?
C11 C2 N3 118.2(2) . . ?
N7 C3 S1 178.7(2) . . ?
C5 N3 C2 119.6(2) . . ?
C5 N3 Fe1 114.73(16) . . ?
C2 N3 Fe1 125.38(16) . . ?
N2 C4 C15 117.4(2) . . ?
N2 C4 H4 121.3 . . ?
C15 C4 H4 121.3 . . ?
N3 C5 C6 116.4(2) . . ?
N3 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C26 N4 C15 117.4(2) . . ?
C26 N4 Fe1 128.23(19) . . ?
C15 N4 Fe1 114.38(15) . . ?
C12 N5 Fe1 166.6(2) . . ?
N1 C6 C18 122.3(2) . . ?
N1 C6 C5 112.5(2) . . ?
C18 C6 C5 125.1(2) . . ?
C8 C7 C9 119.6(2) . . ?
C8 C7 H7 120.2 . . ?
C9 C7 H7 120.2 . . ?
C7 C8 C1 119.8(2) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
C13 C9 C7 120.3(2) . . ?
C13 C9 N10 114.5(3) . . ?
C7 C9 N10 125.1(2) . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 119.3(2) . . ?
C22 C11 H11 120.4 . . ?
C2 C11 H11 120.4 . . ?
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 119.4(2) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
N4 C15 C32 122.8(2) . . ?
N4 C15 C4 112.7(2) . . ?
C32 C15 C4 124.4(3) . . ?
C19 C16 C14 120.0(2) . . ?
C19 C16 H16 120.0 . . ?
C14 C16 H16 120.0 . . ?
N8 N6 C21 112.6(2) . . ?
C27 C17 C28 120.2(2) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C3 N7 Fe1 172.6(2) . . ?
C6 C18 C24 119.2(3) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C22 C19 C16 120.1(2) . . ?
C22 C19 N8 114.4(2) . . ?
C16 C19 N8 125.5(2) . . ?
N6 N8 C19 113.8(2) . . ?
N10 N9 C29 113.2(2) . . ?
N9 N10 C9 110.7(2) . . ?
C24 C20 C10 119.7(2) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C30 C21 C25 120.6(2) . . ?
C30 C21 N6 116.0(2) . . ?
C25 C21 N6 123.4(2) . . ?
C19 C22 C11 120.5(2) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.1(2) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C20 C24 C18 118.5(2) . . ?
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 122.7(3) . . ?
N4 C26 H26 118.7 . . ?
C31 C26 H26 118.7 . . ?
C17 C27 C30 120.0(3) . . ?
C17 C27 H27 120.0 . . ?
C30 C27 H27 120.0 . . ?
C17 C28 C25 120.4(2) . . ?
C17 C28 H28 119.8 . . ?
C25 C28 H28 119.8 . . ?
C34 C29 C37 121.4(2) . . ?
C34 C29 N9 114.9(3) . . ?
C37 C29 N9 123.5(3) . . ?
C21 C30 C27 119.9(2) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.9(3) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C15 C32 C38 118.6(3) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C35 C33 C36 120.2(3) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.5(3) . . ?
C29 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C33 C35 C34 120.7(3) . . ?
C33 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C33 C36 C37 119.5(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 118.6(3) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.842
_diffrn_reflns_theta_full        21.30
_diffrn_measured_fraction_theta_full 0.842
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.176
_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_znaza100km
_database_code_depnum_ccdc_archive 'CCDC 1492660'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0917(6)
_cell_length_b                   14.1960(9)
_cell_length_c                   17.1443(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.310(3)
_cell_angle_gamma                90.00
_cell_volume                     3662.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14301
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6367
_exptl_absorpt_correction_T_max  0.7072
_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      100(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            6214
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4779
_reflns_number_gt                4423
_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)+(0.0384P)²+7.8755P] 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         4779
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
Zn01 Zn 0.71850(3) 0.28332(3) 0.44598(2) 0.02158(15) Uani 1 1 d . . .
S1 S 0.80779(6) 0.50260(7) 0.64759(4) 0.0262(2) Uani 1 1 d . . .
S2 S 0.56186(7) 0.07299(7) 0.60317(5) 0.0307(3) Uani 1 1 d . . .
N9 N 1.0943(2) 0.3954(2) 0.18438(16) 0.0278(7) Uani 1 1 d . . .
N7 N 0.7808(2) 0.3738(2) 0.52462(16) 0.0290(7) Uani 1 1 d . . .
N2 N 0.73177(19) 0.38139(19) 0.33853(14) 0.0191(6) Uani 1 1 d . . .
C29 C 1.1675(3) 0.4099(3) 0.1353(2) 0.0273(9) Uani 1 1 d . . .
N3 N 0.67656(19) 0.18732(19) 0.34175(14) 0.0199(7) Uani 1 1 d . . .
N1 N 0.83594(19) 0.2126(2) 0.41817(15) 0.0220(7) Uani 1 1 d . . .
C1 C 0.8044(2) 0.3864(2) 0.29040(18) 0.0196(8) Uani 1 1 d . . .
C3 C 0.7915(2) 0.4271(3) 0.57619(18) 0.0223(8) Uani 1 1 d . . .
N4 N 0.5947(2) 0.3585(2) 0.42909(15) 0.0249(7) Uani 1 1 d . . .
C12 C 0.6257(2) 0.1426(3) 0.55777(18) 0.0234(8) Uani 1 1 d . . .
C8 C 0.8889(2) 0.4015(2) 0.32619(18) 0.0230(8) Uani 1 1 d . . .
H8 H 0.8968 0.4092 0.3813 0.028 Uiso 1 1 calc R . .
C10 C 0.9152(3) 0.2214(3) 0.45808(19) 0.0267(9) Uani 1 1 d . . .
H10 H 0.9185 0.2541 0.5066 0.032 Uiso 1 1 calc R . .
N10 N 1.0198(2) 0.4003(2) 0.14863(17) 0.0300(7) Uani 1 1 d . . .
C15 C 0.5813(2) 0.4100(3) 0.36260(19) 0.0244(8) Uani 1 1 d . . .
C4 C 0.6574(2) 0.4189(2) 0.31511(18) 0.0229(8) Uani 1 1 d . . .
H4 H 0.6516 0.4523 0.2670 0.027 Uiso 1 1 calc R . .
C6 C 0.8326(2) 0.1637(2) 0.34991(18) 0.0214(8) Uani 1 1 d . . .
C2 C 0.5887(2) 0.1785(2) 0.30620(18) 0.0209(8) Uani 1 1 d . . .
C11 C 0.5221(2) 0.1548(3) 0.35492(19) 0.0259(8) Uani 1 1 d . . .
H11 H 0.5367 0.1416 0.4087 0.031 Uiso 1 1 calc R . .
C23 C 0.7929(2) 0.3731(3) 0.20981(18) 0.0260(8) Uani 1 1 d . . .
H23 H 0.7354 0.3611 0.1855 0.031 Uiso 1 1 calc R . .
N5 N 0.6715(2) 0.1927(2) 0.52536(16) 0.0327(8) Uani 1 1 d . . .
C13 C 0.8657(3) 0.3775(3) 0.16509(19) 0.0282(9) Uani 1 1 d . . .
H13 H 0.8579 0.3695 0.1100 0.034 Uiso 1 1 calc R . .
C18 C 0.9068(2) 0.1268(3) 0.3199(2) 0.0271(9) Uani 1 1 d . . .
H18 H 0.9022 0.0940 0.2714 0.033 Uiso 1 1 calc R . .
C9 C 0.9494(2) 0.3935(2) 0.20058(19) 0.0245(8) Uani 1 1 d . . .
C17 C 0.0331(3) 0.1155(3) 0.0775(2) 0.0278(9) Uani 1 1 d . . .
H17 H -0.0273 0.1044 0.0605 0.033 Uiso 1 1 calc R . .
C7 C 0.9611(2) 0.4055(3) 0.28163(19) 0.0256(8) Uani 1 1 d . . .
H7 H 1.0188 0.4164 0.3060 0.031 Uiso 1 1 calc R . .
N8 N 0.3200(2) 0.1612(2) 0.22186(16) 0.0282(7) Uani 1 1 d . . .
C38 C 0.4316(3) 0.4422(3) 0.3894(3) 0.0435(11) Uani 1 1 d . . .
H38 H 0.3755 0.4704 0.3757 0.052 Uiso 1 1 calc R . .
C32 C 0.5005(3) 0.4510(3) 0.3409(2) 0.0342(10) Uani 1 1 d . . .
H32 H 0.4921 0.4849 0.2931 0.041 Uiso 1 1 calc R . .
C16 C 0.4793(2) 0.1948(2) 0.19742(19) 0.0255(8) Uani 1 1 d . . .
H16 H 0.4643 0.2089 0.1439 0.031 Uiso 1 1 calc R . .
C5 C 0.7425(2) 0.1515(2) 0.31061(18) 0.0213(8) Uani 1 1 d . . .
H5 H 0.7342 0.1174 0.2629 0.026 Uiso 1 1 calc R . .
C14 C 0.5676(2) 0.1994(2) 0.22748(18) 0.0245(8) Uani 1 1 d . . .
H14 H 0.6130 0.2166 0.1947 0.029 Uiso 1 1 calc R . .
C20 C 0.9925(3) 0.1851(3) 0.4318(2) 0.0304(9) Uani 1 1 d . . .
H20 H 1.0476 0.1924 0.4618 0.036 Uiso 1 1 calc R . .
C22 C 0.4348(3) 0.1508(3) 0.3245(2) 0.0282(9) Uani 1 1 d . . .
H22 H 0.3893 0.1352 0.3576 0.034 Uiso 1 1 calc R . .
C27 C 0.0994(3) 0.0958(3) 0.0282(2) 0.0308(9) Uani 1 1 d . . .
H27 H 0.0842 0.0724 -0.0230 0.037 Uiso 1 1 calc R . .
C24 C 0.9886(3) 0.1380(3) 0.3615(2) 0.0312(9) Uani 1 1 d . . .
H24 H 1.0410 0.1136 0.3417 0.037 Uiso 1 1 calc R . .
C21 C 0.2098(2) 0.1423(3) 0.1284(2) 0.0254(8) Uani 1 1 d . . .
C35 C 1.3254(3) 0.4034(3) 0.1299(2) 0.0332(9) Uani 1 1 d . . .
H35 H 1.3825 0.3890 0.1539 0.040 Uiso 1 1 calc R . .
C28 C 0.0551(3) 0.1512(3) 0.1516(2) 0.0311(9) Uani 1 1 d . . .
H28 H 0.0095 0.1664 0.1848 0.037 Uiso 1 1 calc R . .
C36 C 1.2333(3) 0.4592(3) 0.0188(2) 0.0360(10) Uani 1 1 d . . .
H36 H 1.2275 0.4833 -0.0331 0.043 Uiso 1 1 calc R . .
C26 C 0.5277(3) 0.3506(3) 0.4752(2) 0.0334(9) Uani 1 1 d . . .
H26 H 0.5370 0.3149 0.5220 0.040 Uiso 1 1 calc R . .
C19 C 0.4129(2) 0.1694(2) 0.24557(19) 0.0238(8) Uani 1 1 d . . .
N6 N 0.3034(2) 0.1508(2) 0.14978(16) 0.0267(7) Uani 1 1 d . . .
C31 C 0.4461(3) 0.3914(3) 0.4582(3) 0.0434(11) Uani 1 1 d . . .
H31 H 0.4003 0.3851 0.4930 0.052 Uiso 1 1 calc R . .
C33 C 1.3172(3) 0.4380(3) 0.0543(2) 0.0358(10) Uani 1 1 d . . .
H33 H 1.3686 0.4474 0.0266 0.043 Uiso 1 1 calc R . .
C34 C 1.2505(3) 0.3897(3) 0.1710(2) 0.0320(9) Uani 1 1 d . . .
H34 H 1.2563 0.3666 0.2232 0.038 Uiso 1 1 calc R . .
C30 C 0.1873(3) 0.1103(3) 0.0534(2) 0.0285(9) Uani 1 1 d . . .
H30 H 0.2325 0.0981 0.0191 0.034 Uiso 1 1 calc R . .
C25 C 0.1435(3) 0.1650(3) 0.1774(2) 0.0307(9) Uani 1 1 d . . .
H25 H 0.1586 0.1897 0.2281 0.037 Uiso 1 1 calc R . .
C37 C 1.1585(3) 0.4448(3) 0.0597(2) 0.0332(9) Uani 1 1 d . . .
H37 H 1.1012 0.4589 0.0358 0.040 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
Zn01 N5 2.038(3) . ?
Zn01 N7 2.040(3) . ?
Zn01 N1 2.122(3) . ?
Zn01 N4 2.152(3) . ?
Zn01 N3 2.298(3) . ?
Zn01 N2 2.330(3) . ?
S1 C3 1.632(4) . ?
S2 C12 1.620(4) . ?
N9 N10 1.242(4) . ?
N9 C29 1.453(5) . ?
N7 C3 1.165(5) . ?
N2 C4 1.280(4) . ?
N2 C1 1.423(4) . ?
C29 C34 1.382(5) . ?
C29 C37 1.385(5) . ?
N3 C5 1.271(4) . ?
N3 C2 1.423(4) . ?
N1 C10 1.339(4) . ?
N1 C6 1.358(4) . ?
C1 C8 1.389(5) . ?
C1 C23 1.392(4) . ?
N4 C26 1.334(5) . ?
N4 C15 1.356(5) . ?
C12 N5 1.163(5) . ?
C8 C7 1.379(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.382(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.440(5) . ?
C15 C32 1.377(5) . ?
C15 C4 1.462(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.370(5) . ?
C6 C5 1.482(5) . ?
C2 C14 1.395(4) . ?
C2 C11 1.395(5) . ?
C11 C22 1.382(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.388(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.378(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.388(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.398(5) . ?
C17 C28 1.384(5) . ?
C17 C27 1.385(5) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.251(4) . ?
N8 C19 1.434(5) . ?
C38 C32 1.384(6) . ?
C38 C31 1.385(6) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.392(5) . ?
C16 C14 1.395(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.375(5) . ?
C20 H20 0.9500 . ?
C22 C19 1.393(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.380(5) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.382(5) . ?
C21 C25 1.392(5) . ?
C21 N6 1.438(5) . ?
C35 C33 1.382(5) . ?
C35 C34 1.390(5) . ?
C35 H35 0.9500 . ?
C28 C25 1.388(5) . ?
C28 H28 0.9500 . ?
C36 C37 1.389(6) . ?
C36 C33 1.395(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.374(6) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.03(12) . . ?
N5 Zn01 N1 100.94(12) . . ?
N7 Zn01 N1 95.46(12) . . ?
N5 Zn01 N4 93.49(12) . . ?
N7 Zn01 N4 97.40(12) . . ?
N1 Zn01 N4 159.32(10) . . ?
N5 Zn01 N3 93.19(11) . . ?
N7 Zn01 N3 166.83(12) . . ?
N1 Zn01 N3 74.38(10) . . ?
N4 Zn01 N3 90.22(10) . . ?
N5 Zn01 N2 163.74(11) . . ?
N7 Zn01 N2 94.78(11) . . ?
N1 Zn01 N2 88.98(10) . . ?
N4 Zn01 N2 73.89(11) . . ?
N3 Zn01 N2 76.97(9) . . ?
N10 N9 C29 114.0(3) . . ?
C3 N7 Zn01 160.1(3) . . ?
C4 N2 C1 119.6(3) . . ?
C4 N2 Zn01 111.8(2) . . ?
C1 N2 Zn01 127.2(2) . . ?
C34 C29 C37 120.8(4) . . ?
C34 C29 N9 114.6(3) . . ?
C37 C29 N9 124.5(4) . . ?
C5 N3 C2 121.3(3) . . ?
C5 N3 Zn01 112.7(2) . . ?
C2 N3 Zn01 125.4(2) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Zn01 124.8(2) . . ?
C6 N1 Zn01 117.3(2) . . ?
C8 C1 C23 120.1(3) . . ?
C8 C1 N2 118.2(3) . . ?
C23 C1 N2 121.6(3) . . ?
N7 C3 S1 179.0(4) . . ?
C26 N4 C15 118.2(3) . . ?
C26 N4 Zn01 124.5(3) . . ?
C15 N4 Zn01 117.0(2) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 119.9(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
N9 N10 C9 112.0(3) . . ?
N4 C15 C32 121.9(4) . . ?
N4 C15 C4 116.2(3) . . ?
C32 C15 C4 122.0(3) . . ?
N2 C4 C15 119.8(3) . . ?
N2 C4 H4 120.1 . . ?
C15 C4 H4 120.1 . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 115.1(3) . . ?
C18 C6 C5 122.1(3) . . ?
C14 C2 C11 120.6(3) . . ?
C14 C2 N3 122.2(3) . . ?
C11 C2 N3 117.0(3) . . ?
C22 C11 C2 119.5(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
C13 C23 C1 119.8(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C12 N5 Zn01 162.7(3) . . ?
C9 C13 C23 120.0(3) . . ?
C9 C13 H13 120.0 . . ?
C23 C13 H13 120.0 . . ?
C6 C18 C24 118.9(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C13 C9 C7 120.2(3) . . ?
C13 C9 N10 115.6(3) . . ?
C7 C9 N10 124.2(3) . . ?
C28 C17 C27 120.0(3) . . ?
C28 C17 H17 120.0 . . ?
C27 C17 H17 120.0 . . ?
C8 C7 C9 119.9(3) . . ?
C8 C7 H7 120.0 . . ?
C9 C7 H7 120.0 . . ?
N6 N8 C19 114.1(3) . . ?
C32 C38 C31 118.8(4) . . ?
C32 C38 H38 120.6 . . ?
C31 C38 H38 120.6 . . ?
C15 C32 C38 119.3(4) . . ?
C15 C32 H32 120.4 . . ?
C38 C32 H32 120.4 . . ?
C19 C16 C14 120.3(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N3 C5 C6 118.9(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C16 C14 C2 119.3(3) . . ?
C16 C14 H14 120.4 . . ?
C2 C14 H14 120.4 . . ?
C24 C20 C10 119.1(3) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C11 C22 C19 120.6(3) . . ?
C11 C22 H22 119.7 . . ?
C19 C22 H22 119.7 . . ?
C30 C27 C17 120.0(3) . . ?
C30 C27 H27 120.0 . . ?
C17 C27 H27 120.0 . . ?
C20 C24 C18 119.0(4) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C30 C21 C25 120.0(3) . . ?
C30 C21 N6 115.6(3) . . ?
C25 C21 N6 124.4(3) . . ?
C33 C35 C34 120.4(4) . . ?
C33 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C17 C28 C25 120.1(4) . . ?
C17 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
C37 C36 C33 119.5(4) . . ?
C37 C36 H36 120.2 . . ?
C33 C36 H36 120.2 . . ?
N4 C26 C31 123.1(4) . . ?
N4 C26 H26 118.4 . . ?
C31 C26 H26 118.4 . . ?
C16 C19 C22 119.7(3) . . ?
C16 C19 N8 125.8(3) . . ?
C22 C19 N8 114.5(3) . . ?
N8 N6 C21 112.4(3) . . ?
C26 C31 C38 118.8(4) . . ?
C26 C31 H31 120.6 . . ?
C38 C31 H31 120.6 . . ?
C35 C33 C36 120.0(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.3(3) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C27 C30 C21 120.2(4) . . ?
C27 C30 H30 119.9 . . ?
C21 C30 H30 119.9 . . ?
C28 C25 C21 119.5(3) . . ?
C28 C25 H25 120.2 . . ?
C21 C25 H25 120.2 . . ?
C29 C37 C36 119.9(4) . . ?
C29 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.739
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.739
_refine_diff_density_max         1.874
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_znaza90kd
_database_code_depnum_ccdc_archive 'CCDC 1492661'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0920(6)
_cell_length_b                   14.1832(9)
_cell_length_c                   17.1387(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.321(3)
_cell_angle_gamma                90.00
_cell_volume                     3658.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    14337
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_T_max  0.7069
_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      90(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            6201
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4782
_reflns_number_gt                4457
_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)+(0.0377P)²+8.0199P] 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         4782
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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
Zn01 Zn 0.71859(3) 0.28338(3) 0.445914(19) 0.02026(15) Uani 1 1 d . . .
S1 S 0.80787(6) 0.50285(7) 0.64762(4) 0.0248(2) Uani 1 1 d . . .
S2 S 0.56169(6) 0.07296(7) 0.60314(5) 0.0285(2) Uani 1 1 d . . .
N9 N 1.0943(2) 0.3955(2) 0.18435(16) 0.0262(7) Uani 1 1 d . . .
N7 N 0.7809(2) 0.3740(2) 0.52454(16) 0.0270(7) Uani 1 1 d . . .
N2 N 0.73169(19) 0.38156(19) 0.33852(14) 0.0177(6) Uani 1 1 d . . .
C29 C 1.1674(3) 0.4101(3) 0.1354(2) 0.0260(9) Uani 1 1 d . . .
N3 N 0.67645(19) 0.18724(19) 0.34170(14) 0.0186(6) Uani 1 1 d . . .
N1 N 0.83601(19) 0.2126(2) 0.41798(15) 0.0211(7) Uani 1 1 d . . .
C1 C 0.8043(2) 0.3866(2) 0.29031(18) 0.0186(8) Uani 1 1 d . . .
C3 C 0.7916(2) 0.4271(3) 0.57612(18) 0.0209(8) Uani 1 1 d . . .
N4 N 0.5947(2) 0.3586(2) 0.42903(15) 0.0233(7) Uani 1 1 d . . .
C12 C 0.6257(2) 0.1427(3) 0.55774(17) 0.0217(8) Uani 1 1 d . . .
C8 C 0.8889(2) 0.4018(2) 0.32609(18) 0.0210(8) Uani 1 1 d . . .
H8 H 0.8969 0.4096 0.3812 0.025 Uiso 1 1 calc R . .
C10 C 0.9153(2) 0.2215(2) 0.45796(19) 0.0250(9) Uani 1 1 d . . .
H10 H 0.9185 0.2542 0.5064 0.030 Uiso 1 1 calc R . .
N10 N 1.0196(2) 0.4003(2) 0.14846(17) 0.0276(7) Uani 1 1 d . . .
C15 C 0.5814(2) 0.4100(3) 0.36249(19) 0.0231(8) Uani 1 1 d . . .
C4 C 0.6573(2) 0.4190(2) 0.31504(18) 0.0210(8) Uani 1 1 d . . .
H4 H 0.6515 0.4526 0.2670 0.025 Uiso 1 1 calc R . .
C6 C 0.8325(2) 0.1636(2) 0.34987(18) 0.0199(8) Uani 1 1 d . . .
C2 C 0.5888(2) 0.1783(2) 0.30618(18) 0.0203(8) Uani 1 1 d . . .
C11 C 0.5223(2) 0.1550(3) 0.35483(19) 0.0246(8) Uani 1 1 d . . .
H11 H 0.5369 0.1419 0.4086 0.030 Uiso 1 1 calc R . .
C23 C 0.7929(2) 0.3732(3) 0.20969(18) 0.0242(8) Uani 1 1 d . . .
H23 H 0.7354 0.3612 0.1853 0.029 Uiso 1 1 calc R . .
N5 N 0.6717(2) 0.1925(2) 0.52539(16) 0.0302(8) Uani 1 1 d . . .
C13 C 0.8657(3) 0.3774(3) 0.16508(19) 0.0266(9) Uani 1 1 d . . .
H13 H 0.8578 0.3692 0.1100 0.032 Uiso 1 1 calc R . .
C18 C 0.9067(2) 0.1267(3) 0.31986(19) 0.0257(8) Uani 1 1 d . . .
H18 H 0.9021 0.0939 0.2714 0.031 Uiso 1 1 calc R . .
C9 C 0.9491(2) 0.3935(2) 0.20040(19) 0.0233(8) Uani 1 1 d . . .
C17 C 0.0330(3) 0.1154(2) 0.0775(2) 0.0265(9) Uani 1 1 d . . .
H17 H -0.0275 0.1042 0.0606 0.032 Uiso 1 1 calc R . .
C7 C 0.9611(2) 0.4056(2) 0.28172(19) 0.0238(8) Uani 1 1 d . . .
H7 H 1.0188 0.4165 0.3061 0.029 Uiso 1 1 calc R . .
N8 N 0.3200(2) 0.1613(2) 0.22176(16) 0.0268(7) Uani 1 1 d . . .
C38 C 0.4315(3) 0.4421(3) 0.3894(3) 0.0407(11) Uani 1 1 d . . .
H38 H 0.3753 0.4702 0.3757 0.049 Uiso 1 1 calc R . .
C32 C 0.5004(3) 0.4510(3) 0.3408(2) 0.0328(9) Uani 1 1 d . . .
H32 H 0.4919 0.4849 0.2930 0.039 Uiso 1 1 calc R . .
C16 C 0.4791(2) 0.1948(2) 0.19738(19) 0.0244(8) Uani 1 1 d . . .
H16 H 0.4641 0.2091 0.1438 0.029 Uiso 1 1 calc R . .
C5 C 0.7425(2) 0.1514(2) 0.31053(18) 0.0204(8) Uani 1 1 d . . .
H5 H 0.7343 0.1174 0.2628 0.024 Uiso 1 1 calc R . .
C14 C 0.5675(2) 0.1993(2) 0.22753(18) 0.0229(8) Uani 1 1 d . . .
H14 H 0.6128 0.2166 0.1947 0.027 Uiso 1 1 calc R . .
C20 C 0.9925(3) 0.1851(3) 0.4317(2) 0.0286(9) Uani 1 1 d . . .
H20 H 1.0476 0.1926 0.4618 0.034 Uiso 1 1 calc R . .
C22 C 0.4348(3) 0.1508(3) 0.3244(2) 0.0272(9) Uani 1 1 d . . .
H22 H 0.3894 0.1351 0.3576 0.033 Uiso 1 1 calc R . .
C27 C 0.0993(3) 0.0959(3) 0.0280(2) 0.0293(9) Uani 1 1 d . . .
H27 H 0.0841 0.0726 -0.0232 0.035 Uiso 1 1 calc R . .
C24 C 0.9887(3) 0.1378(3) 0.3614(2) 0.0293(9) Uani 1 1 d . . .
H24 H 1.0412 0.1133 0.3417 0.035 Uiso 1 1 calc R . .
C21 C 0.2097(2) 0.1424(3) 0.1284(2) 0.0244(8) Uani 1 1 d . . .
C35 C 1.3253(3) 0.4034(3) 0.1298(2) 0.0310(9) Uani 1 1 d . . .
H35 H 1.3825 0.3889 0.1538 0.037 Uiso 1 1 calc R . .
C28 C 0.0552(3) 0.1513(3) 0.1516(2) 0.0297(9) Uani 1 1 d . . .
H28 H 0.0097 0.1664 0.1848 0.036 Uiso 1 1 calc R . .
C36 C 1.2333(3) 0.4593(3) 0.0188(2) 0.0331(9) Uani 1 1 d . . .
H36 H 1.2275 0.4836 -0.0330 0.040 Uiso 1 1 calc R . .
C26 C 0.5279(3) 0.3509(3) 0.4753(2) 0.0315(9) Uani 1 1 d . . .
H26 H 0.5374 0.3157 0.5223 0.038 Uiso 1 1 calc R . .
C19 C 0.4128(2) 0.1695(2) 0.24554(19) 0.0220(8) Uani 1 1 d . . .
N6 N 0.3033(2) 0.1509(2) 0.14976(16) 0.0255(7) Uani 1 1 d . . .
C31 C 0.4460(3) 0.3914(3) 0.4584(2) 0.0406(11) Uani 1 1 d . . .
H31 H 0.4003 0.3848 0.4932 0.049 Uiso 1 1 calc R . .
C33 C 1.3171(3) 0.4380(3) 0.0543(2) 0.0334(9) Uani 1 1 d . . .
H33 H 1.3685 0.4474 0.0266 0.040 Uiso 1 1 calc R . .
C34 C 1.2504(3) 0.3896(3) 0.1709(2) 0.0295(9) Uani 1 1 d . . .
H34 H 1.2563 0.3664 0.2231 0.035 Uiso 1 1 calc R . .
C30 C 0.1872(2) 0.1104(3) 0.0532(2) 0.0262(8) Uani 1 1 d . . .
H30 H 0.2325 0.0983 0.0189 0.031 Uiso 1 1 calc R . .
C25 C 0.1433(3) 0.1651(3) 0.1774(2) 0.0287(9) Uani 1 1 d . . .
H25 H 0.1584 0.1899 0.2281 0.034 Uiso 1 1 calc R . .
C37 C 1.1585(3) 0.4450(3) 0.0594(2) 0.0308(9) Uani 1 1 d . . .
H37 H 1.1013 0.4589 0.0354 0.037 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
Zn01 N7 2.040(3) . ?
Zn01 N5 2.040(3) . ?
Zn01 N1 2.123(3) . ?
Zn01 N4 2.154(3) . ?
Zn01 N3 2.298(3) . ?
Zn01 N2 2.328(3) . ?
S1 C3 1.635(3) . ?
S2 C12 1.621(4) . ?
N9 N10 1.244(4) . ?
N9 C29 1.451(5) . ?
N7 C3 1.163(4) . ?
N2 C4 1.280(4) . ?
N2 C1 1.423(4) . ?
C29 C34 1.383(5) . ?
C29 C37 1.389(5) . ?
N3 C5 1.272(4) . ?
N3 C2 1.420(4) . ?
N1 C10 1.339(4) . ?
N1 C6 1.356(4) . ?
C1 C8 1.391(5) . ?
C1 C23 1.392(4) . ?
N4 C26 1.333(5) . ?
N4 C15 1.355(4) . ?
C12 N5 1.161(5) . ?
C8 C7 1.376(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.381(5) . ?
C10 H10 0.9500 . ?
N10 C9 1.441(5) . ?
C15 C32 1.379(5) . ?
C15 C4 1.460(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.372(5) . ?
C6 C5 1.479(5) . ?
C2 C11 1.392(5) . ?
C2 C14 1.394(4) . ?
C11 C22 1.384(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.386(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.375(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.390(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.402(5) . ?
C17 C28 1.385(5) . ?
C17 C27 1.387(5) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.250(4) . ?
N8 C19 1.434(5) . ?
C38 C32 1.387(6) . ?
C38 C31 1.387(6) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.391(5) . ?
C16 C14 1.395(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.376(5) . ?
C20 H20 0.9500 . ?
C22 C19 1.392(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.379(5) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.385(5) . ?
C21 C25 1.392(5) . ?
C21 N6 1.438(5) . ?
C35 C33 1.380(5) . ?
C35 C34 1.390(5) . ?
C35 H35 0.9500 . ?
C28 C25 1.384(5) . ?
C28 H28 0.9500 . ?
C36 C37 1.385(5) . ?
C36 C33 1.394(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.373(6) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N5 97.05(12) . . ?
N7 Zn01 N1 95.50(11) . . ?
N5 Zn01 N1 100.90(12) . . ?
N7 Zn01 N4 97.42(11) . . ?
N5 Zn01 N4 93.52(12) . . ?
N1 Zn01 N4 159.28(10) . . ?
N7 Zn01 N3 166.89(12) . . ?
N5 Zn01 N3 93.12(11) . . ?
N1 Zn01 N3 74.39(10) . . ?
N4 Zn01 N3 90.17(10) . . ?
N7 Zn01 N2 94.77(10) . . ?
N5 Zn01 N2 163.74(11) . . ?
N1 Zn01 N2 89.01(10) . . ?
N4 Zn01 N2 73.86(10) . . ?
N3 Zn01 N2 77.03(9) . . ?
N10 N9 C29 113.9(3) . . ?
C3 N7 Zn01 160.1(3) . . ?
C4 N2 C1 119.5(3) . . ?
C4 N2 Zn01 111.9(2) . . ?
C1 N2 Zn01 127.2(2) . . ?
C34 C29 C37 120.5(3) . . ?
C34 C29 N9 114.7(3) . . ?
C37 C29 N9 124.7(3) . . ?
C5 N3 C2 121.3(3) . . ?
C5 N3 Zn01 112.5(2) . . ?
C2 N3 Zn01 125.5(2) . . ?
C10 N1 C6 117.7(3) . . ?
C10 N1 Zn01 124.7(2) . . ?
C6 N1 Zn01 117.2(2) . . ?
C8 C1 C23 119.9(3) . . ?
C8 C1 N2 118.2(3) . . ?
C23 C1 N2 121.8(3) . . ?
N7 C3 S1 178.9(4) . . ?
C26 N4 C15 118.2(3) . . ?
C26 N4 Zn01 124.6(3) . . ?
C15 N4 Zn01 116.8(2) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 120.1(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
N9 N10 C9 112.0(3) . . ?
N4 C15 C32 121.7(3) . . ?
N4 C15 C4 116.3(3) . . ?
C32 C15 C4 122.0(3) . . ?
N2 C4 C15 119.7(3) . . ?
N2 C4 H4 120.2 . . ?
C15 C4 H4 120.2 . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 115.3(3) . . ?
C18 C6 C5 122.1(3) . . ?
C11 C2 C14 120.4(3) . . ?
C11 C2 N3 117.0(3) . . ?
C14 C2 N3 122.4(3) . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
C13 C23 C1 119.9(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C12 N5 Zn01 162.5(3) . . ?
C9 C13 C23 120.1(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C6 C18 C24 119.0(3) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.2(3) . . ?
C13 C9 N10 115.7(3) . . ?
C7 C9 N10 124.1(3) . . ?
C28 C17 C27 119.8(3) . . ?
C28 C17 H17 120.1 . . ?
C27 C17 H17 120.1 . . ?
C8 C7 C9 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
N6 N8 C19 114.2(3) . . ?
C32 C38 C31 118.8(4) . . ?
C32 C38 H38 120.6 . . ?
C31 C38 H38 120.6 . . ?
C15 C32 C38 119.3(4) . . ?
C15 C32 H32 120.4 . . ?
C38 C32 H32 120.4 . . ?
C19 C16 C14 120.1(3) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N3 C5 C6 118.9(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C2 C14 C16 119.5(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C24 C20 C10 119.1(3) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C11 C22 C19 120.6(3) . . ?
C11 C22 H22 119.7 . . ?
C19 C22 H22 119.7 . . ?
C30 C27 C17 120.0(3) . . ?
C30 C27 H27 120.0 . . ?
C17 C27 H27 120.0 . . ?
C20 C24 C18 118.7(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.0(3) . . ?
C30 C21 N6 115.5(3) . . ?
C25 C21 N6 124.4(3) . . ?
C33 C35 C34 120.4(4) . . ?
C33 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C25 C28 C17 120.4(4) . . ?
C25 C28 H28 119.8 . . ?
C17 C28 H28 119.8 . . ?
C37 C36 C33 119.7(3) . . ?
C37 C36 H36 120.2 . . ?
C33 C36 H36 120.2 . . ?
N4 C26 C31 123.3(4) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C16 C19 C22 119.7(3) . . ?
C16 C19 N8 125.7(3) . . ?
C22 C19 N8 114.6(3) . . ?
N8 N6 C21 112.5(3) . . ?
C26 C31 C38 118.6(4) . . ?
C26 C31 H31 120.7 . . ?
C38 C31 H31 120.7 . . ?
C35 C33 C36 120.0(4) . . ?
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 . . ?
C27 C30 C21 120.2(3) . . ?
C27 C30 H30 119.9 . . ?
C21 C30 H30 119.9 . . ?
C28 C25 C21 119.5(3) . . ?
C28 C25 H25 120.3 . . ?
C21 C25 H25 120.3 . . ?
C36 C37 C29 119.9(4) . . ?
C36 C37 H37 120.0 . . ?
C29 C37 H37 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.741
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.741
_refine_diff_density_max         1.896
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_feaza270kd1
_database_code_depnum_ccdc_archive 'CCDC 1492662'
_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                   15.1117(11)
_cell_length_b                   14.5148(12)
_cell_length_c                   17.0110(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.032(4)
_cell_angle_gamma                90.00
_cell_volume                     3726.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    4451
_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    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5537
_exptl_absorpt_correction_T_max  0.8965
_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      270(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            5885
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0428
_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             3509
_reflns_number_gt                2759
_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)+(0.0255P)²+2.3172P] 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         3509
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 0.29161(3) 0.28753(4) 0.05571(3) 0.0551(2) Uani 1 1 d . . .
S1 S 0.18882(6) 0.49702(8) -0.14668(6) 0.0699(3) Uani 1 1 d . . .
S2 S 0.43672(7) 0.07275(8) -0.10640(6) 0.0786(4) Uani 1 1 d . . .
N1 N 0.17161(19) 0.2159(2) 0.07857(19) 0.0543(8) Uani 1 1 d . . .
N2 N 0.27365(18) 0.37966(19) 0.16045(15) 0.0439(7) Uani 1 1 d . . .
C1 C 0.1976(2) 0.3850(2) 0.2069(2) 0.0445(9) Uani 1 1 d . . .
C2 C 0.4139(2) 0.1809(2) 0.1913(2) 0.0511(10) Uani 1 1 d . . .
C3 C 0.2137(2) 0.4253(3) -0.0756(2) 0.0546(10) Uani 1 1 d . . .
N3 N 0.32769(19) 0.1905(2) 0.15419(16) 0.0493(8) Uani 1 1 d . . .
C4 C 0.3446(2) 0.4199(2) 0.1852(2) 0.0533(10) Uani 1 1 d . . .
H4 H 0.3460 0.4539 0.2316 0.064 Uiso 1 1 calc R . .
C5 C 0.2613(3) 0.1525(3) 0.1832(2) 0.0544(10) Uani 1 1 d . . .
H5 H 0.2684 0.1172 0.2287 0.065 Uiso 1 1 calc R . .
N4 N 0.41523(18) 0.3611(2) 0.0751(2) 0.0613(9) Uani 1 1 d . . .
N5 N 0.3424(2) 0.2026(3) -0.0267(2) 0.0809(11) Uani 1 1 d . . .
C6 C 0.1734(2) 0.1648(3) 0.1444(2) 0.0527(10) Uani 1 1 d . . .
C7 C 0.0410(2) 0.4031(3) 0.2110(3) 0.0653(12) Uani 1 1 d . . .
H7 H -0.0142 0.4123 0.1855 0.078 Uiso 1 1 calc R . .
C8 C 0.1161(2) 0.3996(2) 0.1690(2) 0.0556(10) Uani 1 1 d . . .
H8 H 0.1118 0.4070 0.1147 0.067 Uiso 1 1 calc R . .
C9 C 0.0486(3) 0.3928(3) 0.2907(4) 0.0736(14) Uani 1 1 d . . .
C10 C 0.0941(3) 0.2253(3) 0.0385(2) 0.0690(12) Uani 1 1 d . . .
H10 H 0.0921 0.2593 -0.0079 0.083 Uiso 1 1 calc R . .
C11 C 0.4825(3) 0.1578(3) 0.1445(2) 0.0655(11) Uani 1 1 d . . .
H11 H 0.4704 0.1456 0.0914 0.079 Uiso 1 1 calc R . .
C12 C 0.3813(2) 0.1488(3) -0.0602(2) 0.0565(11) Uani 1 1 d . . .
C13 C 0.1295(3) 0.3778(3) 0.3295(3) 0.0806(13) Uani 1 1 d . . .
H13 H 0.1337 0.3706 0.3839 0.097 Uiso 1 1 calc R . .
C14 C 0.4320(3) 0.2004(3) 0.2700(2) 0.0649(11) Uani 1 1 d . . .
H14 H 0.3868 0.2169 0.3022 0.078 Uiso 1 1 calc R . .
C15 C 0.4237(2) 0.4123(3) 0.1403(3) 0.0551(10) Uani 1 1 d . . .
C16 C 0.5198(3) 0.1950(3) 0.3002(3) 0.0767(13) Uani 1 1 d . . .
H16 H 0.5333 0.2081 0.3530 0.092 Uiso 1 1 calc R . .
N6 N 0.6925(3) 0.1537(3) 0.3432(3) 0.0915(12) Uani 1 1 d . . .
C17 C 0.9627(3) 0.1180(3) 0.4187(3) 0.0763(13) Uani 1 1 d . . .
H17 H 1.0207 0.1082 0.4378 0.092 Uiso 1 1 calc R . .
N7 N 0.2304(2) 0.3758(3) -0.0239(2) 0.0741(11) Uani 1 1 d . . .
C18 C 0.0982(3) 0.1252(3) 0.1723(2) 0.0694(11) Uani 1 1 d . . .
H18 H 0.1013 0.0910 0.2185 0.083 Uiso 1 1 calc R . .
C19 C 0.5862(3) 0.1704(3) 0.2521(3) 0.0712(13) Uani 1 1 d . . .
N8 N 0.6859(3) 0.1623(3) 0.2754(3) 0.0844(12) Uani 1 1 d . . .
N9 N -0.0832(3) 0.3953(2) 0.3132(2) 0.0925(13) Uani 1 1 d . . .
N10 N -0.0268(3) 0.4019(3) 0.3563(3) 0.1081(16) Uani 1 1 d . . .
C20 C 0.0165(3) 0.1868(3) 0.0628(3) 0.0816(13) Uani 1 1 d . . .
H20 H -0.0365 0.1948 0.0331 0.098 Uiso 1 1 calc R . .
C21 C 0.7916(2) 0.1430(3) 0.3655(4) 0.0758(14) Uani 1 1 d . . .
C22 C 0.5675(3) 0.1526(3) 0.1751(3) 0.0750(13) Uani 1 1 d . . .
H22 H 0.6129 0.1368 0.1427 0.090 Uiso 1 1 calc R . .
C23 C 0.2032(2) 0.3738(3) 0.2870(3) 0.0651(11) Uani 1 1 d . . .
H23 H 0.2581 0.3633 0.3126 0.078 Uiso 1 1 calc R . .
C24 C 0.0186(3) 0.1372(3) 0.1302(3) 0.0815(13) Uani 1 1 d . . .
H24 H -0.0331 0.1116 0.1480 0.098 Uiso 1 1 calc R . .
C25 C 0.8583(3) 0.1613(3) 0.3153(3) 0.0861(13) Uani 1 1 d . . .
H25 H 0.8454 0.1814 0.2640 0.103 Uiso 1 1 calc R . .
C26 C 0.4847(3) 0.3554(3) 0.0310(3) 0.0947(15) Uani 1 1 d . . .
H26 H 0.4798 0.3215 -0.0155 0.114 Uiso 1 1 calc R . .
C27 C 0.8957(3) 0.1017(3) 0.4649(3) 0.0908(15) Uani 1 1 d . . .
H27 H 0.9079 0.0813 0.5162 0.109 Uiso 1 1 calc R . .
C28 C 0.9466(3) 0.1486(3) 0.3441(3) 0.0848(14) Uani 1 1 d . . .
H28 H 0.9933 0.1611 0.3123 0.102 Uiso 1 1 calc R . .
C29 C -0.1629(4) 0.4093(4) 0.3738(5) 0.100(2) Uani 1 1 d . . .
C30 C 0.8106(3) 0.1143(3) 0.4389(3) 0.0932(15) Uani 1 1 d . . .
H30 H 0.7651 0.1028 0.4723 0.112 Uiso 1 1 calc R . .
C31 C 0.5643(4) 0.3983(5) 0.0518(5) 0.127(2) Uani 1 1 d . . .
H31 H 0.6120 0.3928 0.0198 0.152 Uiso 1 1 calc R . .
C32 C 0.5017(3) 0.4555(3) 0.1638(3) 0.0867(14) Uani 1 1 d . . .
H32 H 0.5056 0.4894 0.2102 0.104 Uiso 1 1 calc R . .
C33 C -0.3151(3) 0.4366(4) 0.4505(4) 0.0927(15) Uani 1 1 d . . .
H33 H -0.3676 0.4451 0.4757 0.111 Uiso 1 1 calc R . .
C34 C -0.2421(4) 0.3906(3) 0.3372(3) 0.0981(16) Uani 1 1 d . . .
H34 H -0.2451 0.3688 0.2857 0.118 Uiso 1 1 calc R . .
C35 C -0.3171(3) 0.4035(3) 0.3756(4) 0.0935(15) Uani 1 1 d . . .
H35 H -0.3715 0.3894 0.3502 0.112 Uiso 1 1 calc R . .
C36 C -0.2357(4) 0.4575(4) 0.4889(3) 0.0999(16) Uani 1 1 d . . .
H36 H -0.2338 0.4806 0.5400 0.120 Uiso 1 1 calc R . .
C37 C -0.1568(3) 0.4433(4) 0.4497(4) 0.0990(16) Uani 1 1 d . . .
H37 H -0.1019 0.4565 0.4745 0.119 Uiso 1 1 calc R . .
C38 C 0.5724(3) 0.4484(5) 0.1189(5) 0.123(2) Uani 1 1 d . . .
H38 H 0.6256 0.4772 0.1337 0.148 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 2.047(4) . ?
Fe1 N7 2.050(4) . ?
Fe1 N1 2.143(3) . ?
Fe1 N4 2.162(3) . ?
Fe1 N3 2.234(3) . ?
Fe1 N2 2.256(3) . ?
S1 C3 1.625(5) . ?
S2 C12 1.614(5) . ?
N1 C10 1.330(4) . ?
N1 C6 1.342(4) . ?
N2 C4 1.274(4) . ?
N2 C1 1.431(4) . ?
C1 C23 1.369(5) . ?
C1 C8 1.376(4) . ?
C2 C11 1.381(5) . ?
C2 C14 1.381(5) . ?
C2 N3 1.425(4) . ?
C3 N7 1.153(4) . ?
N3 C5 1.268(4) . ?
C4 C15 1.456(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.462(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.325(5) . ?
N4 C15 1.335(4) . ?
N5 C12 1.147(4) . ?
C6 C18 1.379(5) . ?
C7 C9 1.361(6) . ?
C7 C8 1.374(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.375(6) . ?
C9 N10 1.642(6) . ?
C10 C20 1.383(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.363(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.361(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.399(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.376(5) . ?
C16 C19 1.375(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.160(4) . ?
N6 C21 1.533(5) . ?
C17 C27 1.335(5) . ?
C17 C28 1.355(5) . ?
C17 H17 0.9300 . ?
C18 C24 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.350(5) . ?
C19 N8 1.542(5) . ?
N9 N10 1.098(4) . ?
N9 C29 1.640(6) . ?
C20 C24 1.353(5) . ?
C20 H20 0.9300 . ?
C21 C30 1.334(6) . ?
C21 C25 1.382(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.408(6) . ?
C25 H25 0.9300 . ?
C26 C31 1.385(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.350(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.347(7) . ?
C29 C37 1.380(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.352(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.351(6) . ?
C32 H32 0.9300 . ?
C33 C35 1.362(6) . ?
C33 C36 1.369(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.351(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.412(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 95.54(14) . . ?
N5 Fe1 N1 100.60(13) . . ?
N7 Fe1 N1 93.79(13) . . ?
N5 Fe1 N4 92.84(14) . . ?
N7 Fe1 N4 98.54(13) . . ?
N1 Fe1 N4 160.80(13) . . ?
N5 Fe1 N3 92.78(13) . . ?
N7 Fe1 N3 166.78(12) . . ?
N1 Fe1 N3 74.55(12) . . ?
N4 Fe1 N3 91.28(11) . . ?
N5 Fe1 N2 164.45(12) . . ?
N7 Fe1 N2 94.73(12) . . ?
N1 Fe1 N2 90.33(11) . . ?
N4 Fe1 N2 74.09(12) . . ?
N3 Fe1 N2 79.41(9) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Fe1 126.0(3) . . ?
C6 N1 Fe1 116.1(2) . . ?
C4 N2 C1 118.6(3) . . ?
C4 N2 Fe1 113.5(2) . . ?
C1 N2 Fe1 127.0(2) . . ?
C23 C1 C8 119.4(3) . . ?
C23 C1 N2 122.2(3) . . ?
C8 C1 N2 118.3(3) . . ?
C11 C2 C14 119.5(3) . . ?
C11 C2 N3 117.7(4) . . ?
C14 C2 N3 122.6(3) . . ?
N7 C3 S1 178.4(4) . . ?
C5 N3 C2 120.6(3) . . ?
C5 N3 Fe1 113.5(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 119.4(4) . . ?
N2 C4 H4 120.3 . . ?
C15 C4 H4 120.3 . . ?
N3 C5 C6 119.4(4) . . ?
N3 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C26 N4 C15 117.5(4) . . ?
C26 N4 Fe1 125.9(3) . . ?
C15 N4 Fe1 116.4(2) . . ?
C12 N5 Fe1 166.2(4) . . ?
N1 C6 C18 122.5(3) . . ?
N1 C6 C5 114.9(3) . . ?
C18 C6 C5 122.6(4) . . ?
C9 C7 C8 119.0(4) . . ?
C9 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C7 C8 C1 120.4(4) . . ?
C7 C8 H8 119.8 . . ?
C1 C8 H8 119.8 . . ?
C7 C9 C13 121.4(3) . . ?
C7 C9 N10 130.0(4) . . ?
C13 C9 N10 108.5(5) . . ?
N1 C10 C20 123.0(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 121.0(4) . . ?
C22 C11 H11 119.5 . . ?
C2 C11 H11 119.5 . . ?
N5 C12 S2 179.3(4) . . ?
C23 C13 C9 118.9(4) . . ?
C23 C13 H13 120.6 . . ?
C9 C13 H13 120.6 . . ?
C2 C14 C16 118.6(4) . . ?
C2 C14 H14 120.7 . . ?
C16 C14 H14 120.7 . . ?
N4 C15 C32 122.5(4) . . ?
N4 C15 C4 115.7(3) . . ?
C32 C15 C4 121.8(4) . . ?
C19 C16 C14 120.2(4) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 106.7(4) . . ?
C27 C17 C28 120.4(4) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 165.1(3) . . ?
C24 C18 C6 118.8(4) . . ?
C24 C18 H18 120.6 . . ?
C6 C18 H18 120.6 . . ?
C22 C19 C16 120.4(4) . . ?
C22 C19 N8 112.7(4) . . ?
C16 C19 N8 126.9(5) . . ?
N6 N8 C19 107.2(4) . . ?
N10 N9 C29 97.9(5) . . ?
N9 N10 C9 94.6(5) . . ?
C24 C20 C10 119.1(4) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 120.7(4) . . ?
C30 C21 N6 115.0(5) . . ?
C25 C21 N6 124.3(5) . . ?
C19 C22 C11 120.2(4) . . ?
C19 C22 H22 119.9 . . ?
C11 C22 H22 119.9 . . ?
C13 C23 C1 120.9(4) . . ?
C13 C23 H23 119.5 . . ?
C1 C23 H23 119.5 . . ?
C20 C24 C18 119.2(4) . . ?
C20 C24 H24 120.4 . . ?
C18 C24 H24 120.4 . . ?
C21 C25 C28 117.9(4) . . ?
C21 C25 H25 121.0 . . ?
C28 C25 H25 121.0 . . ?
N4 C26 C31 122.0(5) . . ?
N4 C26 H26 119.0 . . ?
C31 C26 H26 119.0 . . ?
C17 C27 C30 121.4(5) . . ?
C17 C27 H27 119.3 . . ?
C30 C27 H27 119.3 . . ?
C17 C28 C25 119.3(4) . . ?
C17 C28 H28 120.4 . . ?
C25 C28 H28 120.4 . . ?
C34 C29 C37 121.2(4) . . ?
C34 C29 N9 110.4(6) . . ?
C37 C29 N9 128.2(6) . . ?
C21 C30 C27 120.2(4) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C38 C31 C26 119.8(5) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C38 C32 C15 119.5(5) . . ?
C38 C32 H32 120.3 . . ?
C15 C32 H32 120.3 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.8(5) . . ?
C29 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C33 121.5(5) . . ?
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(5) . . ?
C29 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C32 C38 C31 118.6(5) . . ?
C32 C38 H38 120.7 . . ?
C31 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         0.305
_refine_diff_density_min         -0.178
_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_znaza130kd
_database_code_depnum_ccdc_archive 'CCDC 1492663'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0934(6)
_cell_length_b                   14.2495(9)
_cell_length_c                   17.1470(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.234(3)
_cell_angle_gamma                90.00
_cell_volume                     3677.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    14421
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_T_max  0.7081
_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            6234
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4801
_reflns_number_gt                4389
_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)+(0.0467P)²+6.3872P] 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         4801
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.1128
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
Zn01 Zn 0.71751(3) 0.28355(3) 0.44622(2) 0.02688(16) Uani 1 1 d . . .
S1 S 0.80761(6) 0.50170(7) 0.64750(5) 0.0325(2) Uani 1 1 d . . .
S2 S 0.56230(7) 0.07284(7) 0.60354(5) 0.0385(3) Uani 1 1 d . . .
N9 N 1.0940(2) 0.3954(2) 0.18464(17) 0.0352(8) Uani 1 1 d . . .
N7 N 0.7797(2) 0.3739(2) 0.52455(17) 0.0356(8) Uani 1 1 d . . .
N2 N 0.73175(19) 0.38118(19) 0.33854(15) 0.0234(7) Uani 1 1 d . . .
C29 C 1.1680(3) 0.4098(3) 0.1352(2) 0.0353(9) Uani 1 1 d . . .
N3 N 0.6757(2) 0.1874(2) 0.34215(15) 0.0243(7) Uani 1 1 d . . .
N1 N 0.8348(2) 0.2126(2) 0.41866(15) 0.0268(7) Uani 1 1 d . . .
C1 C 0.8044(2) 0.3864(2) 0.29058(18) 0.0240(8) Uani 1 1 d . . .
C3 C 0.7908(2) 0.4268(3) 0.57596(19) 0.0275(8) Uani 1 1 d . . .
N4 N 0.5940(2) 0.3587(2) 0.42869(16) 0.0311(7) Uani 1 1 d . . .
C12 C 0.6252(2) 0.1432(3) 0.55793(18) 0.0286(8) Uani 1 1 d . . .
C8 C 0.8889(2) 0.4010(2) 0.32660(19) 0.0276(8) Uani 1 1 d . . .
H8 H 0.8967 0.4081 0.3818 0.033 Uiso 1 1 calc R . .
C10 C 0.9140(3) 0.2217(3) 0.4585(2) 0.0330(9) Uani 1 1 d . . .
H10 H 0.9172 0.2548 0.5067 0.040 Uiso 1 1 calc R . .
N10 N 1.0201(2) 0.4005(2) 0.14877(18) 0.0388(8) Uani 1 1 d . . .
C15 C 0.5812(3) 0.4103(3) 0.3624(2) 0.0300(9) Uani 1 1 d . . .
C4 C 0.6573(2) 0.4189(2) 0.31536(19) 0.0277(8) Uani 1 1 d . . .
H4 H 0.6518 0.4526 0.2674 0.033 Uiso 1 1 calc R . .
C6 C 0.8317(2) 0.1639(2) 0.35066(18) 0.0259(8) Uani 1 1 d . . .
C2 C 0.5881(2) 0.1788(2) 0.30612(19) 0.0261(8) Uani 1 1 d . . .
C11 C 0.5215(3) 0.1551(3) 0.3547(2) 0.0334(9) Uani 1 1 d . . .
H11 H 0.5361 0.1416 0.4084 0.040 Uiso 1 1 calc R . .
C23 C 0.7934(3) 0.3735(3) 0.21006(19) 0.0324(9) Uani 1 1 d . . .
H23 H 0.7360 0.3615 0.1855 0.039 Uiso 1 1 calc R . .
N5 N 0.6704(2) 0.1933(2) 0.52544(17) 0.0400(8) Uani 1 1 d . . .
C13 C 0.8663(3) 0.3780(3) 0.1658(2) 0.0362(9) Uani 1 1 d . . .
H13 H 0.8587 0.3706 0.1106 0.043 Uiso 1 1 calc R . .
C18 C 0.9057(3) 0.1269(3) 0.3207(2) 0.0343(9) Uani 1 1 d . . .
H18 H 0.9011 0.0941 0.2724 0.041 Uiso 1 1 calc R . .
C9 C 0.9495(3) 0.3933(3) 0.2012(2) 0.0304(9) Uani 1 1 d . . .
C17 C 0.0334(3) 0.1154(3) 0.0775(2) 0.0346(9) Uani 1 1 d . . .
H17 H -0.0269 0.1044 0.0600 0.042 Uiso 1 1 calc R . .
C7 C 0.9612(3) 0.4051(3) 0.2823(2) 0.0316(9) Uani 1 1 d . . .
H7 H 1.0189 0.4159 0.3067 0.038 Uiso 1 1 calc R . .
N8 N 0.3190(2) 0.1612(2) 0.22180(17) 0.0359(8) Uani 1 1 d . . .
C38 C 0.4316(3) 0.4424(3) 0.3890(3) 0.0564(13) Uani 1 1 d . . .
H38 H 0.3756 0.4707 0.3754 0.068 Uiso 1 1 calc R . .
C32 C 0.5008(3) 0.4513(3) 0.3404(3) 0.0431(10) Uani 1 1 d . . .
H32 H 0.4927 0.4853 0.2928 0.052 Uiso 1 1 calc R . .
C16 C 0.4792(3) 0.1950(3) 0.1976(2) 0.0336(9) Uani 1 1 d . . .
H16 H 0.4646 0.2092 0.1440 0.040 Uiso 1 1 calc R . .
C5 C 0.7420(2) 0.1515(2) 0.31118(18) 0.0265(8) Uani 1 1 d . . .
H5 H 0.7340 0.1174 0.2636 0.032 Uiso 1 1 calc R . .
C14 C 0.5671(3) 0.1996(3) 0.22783(19) 0.0301(8) Uani 1 1 d . . .
H14 H 0.6125 0.2170 0.1951 0.036 Uiso 1 1 calc R . .
C20 C 0.9910(3) 0.1852(3) 0.4324(2) 0.0383(10) Uani 1 1 d . . .
H20 H 1.0459 0.1925 0.4626 0.046 Uiso 1 1 calc R . .
C22 C 0.4336(3) 0.1512(3) 0.3244(2) 0.0352(9) Uani 1 1 d . . .
H22 H 0.3880 0.1360 0.3576 0.042 Uiso 1 1 calc R . .
C27 C 0.0996(3) 0.0961(3) 0.0290(2) 0.0389(10) Uani 1 1 d . . .
H27 H 0.0848 0.0727 -0.0222 0.047 Uiso 1 1 calc R . .
C24 C 0.9877(3) 0.1381(3) 0.3624(2) 0.0385(10) Uani 1 1 d . . .
H24 H 1.0402 0.1138 0.3428 0.046 Uiso 1 1 calc R . .
C21 C 0.2092(2) 0.1421(3) 0.1292(2) 0.0322(9) Uani 1 1 d . . .
C35 C 1.3248(3) 0.4034(3) 0.1295(2) 0.0418(10) Uani 1 1 d . . .
H35 H 1.3820 0.3890 0.1533 0.050 Uiso 1 1 calc R . .
C28 C 0.0544(3) 0.1508(3) 0.1514(2) 0.0388(10) Uani 1 1 d . . .
H28 H 0.0085 0.1658 0.1843 0.047 Uiso 1 1 calc R . .
C36 C 1.2333(3) 0.4589(3) 0.0187(2) 0.0444(11) Uani 1 1 d . . .
H36 H 1.2275 0.4830 -0.0331 0.053 Uiso 1 1 calc R . .
C26 C 0.5269(3) 0.3511(3) 0.4745(2) 0.0427(10) Uani 1 1 d . . .
H26 H 0.5360 0.3157 0.5213 0.051 Uiso 1 1 calc R . .
C19 C 0.4122(2) 0.1695(3) 0.2455(2) 0.0313(9) Uani 1 1 d . . .
N6 N 0.3032(2) 0.1507(2) 0.15047(17) 0.0344(8) Uani 1 1 d . . .
C31 C 0.4456(3) 0.3915(3) 0.4577(3) 0.0543(12) Uani 1 1 d . . .
H31 H 0.3997 0.3849 0.4923 0.065 Uiso 1 1 calc R . .
C33 C 1.3169(3) 0.4379(3) 0.0542(2) 0.0455(11) Uani 1 1 d . . .
H33 H 1.3685 0.4473 0.0266 0.055 Uiso 1 1 calc R . .
C34 C 1.2505(3) 0.3895(3) 0.1708(2) 0.0396(10) Uani 1 1 d . . .
H34 H 1.2564 0.3663 0.2229 0.047 Uiso 1 1 calc R . .
C30 C 0.1875(3) 0.1104(3) 0.0543(2) 0.0359(9) Uani 1 1 d . . .
H30 H 0.2330 0.0985 0.0201 0.043 Uiso 1 1 calc R . .
C25 C 0.1429(3) 0.1646(3) 0.1776(2) 0.0385(10) Uani 1 1 d . . .
H25 H 0.1577 0.1893 0.2284 0.046 Uiso 1 1 calc R . .
C37 C 1.1584(3) 0.4443(3) 0.0597(2) 0.0418(10) Uani 1 1 d . . .
H37 H 1.1010 0.4580 0.0359 0.050 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
Zn01 N5 2.036(3) . ?
Zn01 N7 2.039(3) . ?
Zn01 N1 2.123(3) . ?
Zn01 N4 2.151(3) . ?
Zn01 N3 2.301(3) . ?
Zn01 N2 2.334(3) . ?
S1 C3 1.632(4) . ?
S2 C12 1.620(4) . ?
N9 N10 1.235(4) . ?
N9 C29 1.466(5) . ?
N7 C3 1.162(5) . ?
N2 C4 1.282(4) . ?
N2 C1 1.420(4) . ?
C29 C34 1.377(6) . ?
C29 C37 1.382(6) . ?
N3 C5 1.275(5) . ?
N3 C2 1.422(4) . ?
N1 C10 1.338(4) . ?
N1 C6 1.354(4) . ?
C1 C23 1.391(4) . ?
C1 C8 1.391(5) . ?
N4 C26 1.331(5) . ?
N4 C15 1.356(5) . ?
C12 N5 1.159(5) . ?
C8 C7 1.377(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.379(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.448(5) . ?
C15 C32 1.375(6) . ?
C15 C4 1.456(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.369(5) . ?
C6 C5 1.478(5) . ?
C2 C14 1.389(5) . ?
C2 C11 1.394(5) . ?
C11 C22 1.389(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.384(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.371(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.392(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.398(5) . ?
C17 C27 1.374(6) . ?
C17 C28 1.379(5) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.238(4) . ?
N8 C19 1.440(5) . ?
C38 C31 1.385(7) . ?
C38 C32 1.389(6) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C14 1.389(5) . ?
C16 C19 1.398(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.373(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.391(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.380(5) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.378(5) . ?
C21 C25 1.384(6) . ?
C21 N6 1.444(5) . ?
C35 C33 1.377(6) . ?
C35 C34 1.384(6) . ?
C35 H35 0.9500 . ?
C28 C25 1.391(6) . ?
C28 H28 0.9500 . ?
C36 C37 1.391(6) . ?
C36 C33 1.393(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.367(6) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.21(13) . . ?
N5 Zn01 N1 100.71(13) . . ?
N7 Zn01 N1 95.54(12) . . ?
N5 Zn01 N4 93.78(13) . . ?
N7 Zn01 N4 97.45(12) . . ?
N1 Zn01 N4 159.14(10) . . ?
N5 Zn01 N3 92.99(11) . . ?
N7 Zn01 N3 166.82(12) . . ?
N1 Zn01 N3 74.29(10) . . ?
N4 Zn01 N3 90.16(11) . . ?
N5 Zn01 N2 163.95(12) . . ?
N7 Zn01 N2 94.59(11) . . ?
N1 Zn01 N2 88.91(10) . . ?
N4 Zn01 N2 73.87(11) . . ?
N3 Zn01 N2 77.15(9) . . ?
N10 N9 C29 113.7(3) . . ?
C3 N7 Zn01 160.5(3) . . ?
C4 N2 C1 119.7(3) . . ?
C4 N2 Zn01 111.4(2) . . ?
C1 N2 Zn01 127.5(2) . . ?
C34 C29 C37 121.2(4) . . ?
C34 C29 N9 114.6(3) . . ?
C37 C29 N9 124.1(4) . . ?
C5 N3 C2 121.2(3) . . ?
C5 N3 Zn01 112.5(2) . . ?
C2 N3 Zn01 125.5(2) . . ?
C10 N1 C6 117.6(3) . . ?
C10 N1 Zn01 124.6(2) . . ?
C6 N1 Zn01 117.3(2) . . ?
C23 C1 C8 119.9(3) . . ?
C23 C1 N2 121.9(3) . . ?
C8 C1 N2 118.2(3) . . ?
N7 C3 S1 179.2(4) . . ?
C26 N4 C15 118.1(3) . . ?
C26 N4 Zn01 124.5(3) . . ?
C15 N4 Zn01 117.1(2) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 122.7(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
N9 N10 C9 111.4(3) . . ?
N4 C15 C32 121.9(4) . . ?
N4 C15 C4 116.2(3) . . ?
C32 C15 C4 121.9(4) . . ?
N2 C4 C15 120.1(3) . . ?
N2 C4 H4 119.9 . . ?
C15 C4 H4 119.9 . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 115.4(3) . . ?
C18 C6 C5 121.8(3) . . ?
C14 C2 C11 120.4(3) . . ?
C14 C2 N3 122.7(3) . . ?
C11 C2 N3 116.7(3) . . ?
C22 C11 C2 119.8(3) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
C13 C23 C1 119.8(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C12 N5 Zn01 163.2(3) . . ?
C9 C13 C23 120.2(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C6 C18 C24 118.9(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C13 C9 C7 120.2(3) . . ?
C13 C9 N10 115.4(3) . . ?
C7 C9 N10 124.3(3) . . ?
C27 C17 C28 120.1(4) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C8 C7 C9 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
N6 N8 C19 113.7(3) . . ?
C31 C38 C32 118.9(4) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?
C15 C32 C38 119.0(4) . . ?
C15 C32 H32 120.5 . . ?
C38 C32 H32 120.5 . . ?
C14 C16 C19 120.3(3) . . ?
C14 C16 H16 119.8 . . ?
C19 C16 H16 119.8 . . ?
N3 C5 C6 118.8(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C2 C14 C16 119.6(3) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C24 C20 C10 119.3(3) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C11 C22 C19 120.2(4) . . ?
C11 C22 H22 119.9 . . ?
C19 C22 H22 119.9 . . ?
C17 C27 C30 120.3(4) . . ?
C17 C27 H27 119.8 . . ?
C30 C27 H27 119.8 . . ?
C20 C24 C18 118.6(4) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C30 C21 C25 120.2(3) . . ?
C30 C21 N6 115.1(3) . . ?
C25 C21 N6 124.7(3) . . ?
C33 C35 C34 120.9(4) . . ?
C33 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C17 C28 C25 119.9(4) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C37 C36 C33 119.4(4) . . ?
C37 C36 H36 120.3 . . ?
C33 C36 H36 120.3 . . ?
N4 C26 C31 123.5(4) . . ?
N4 C26 H26 118.2 . . ?
C31 C26 H26 118.2 . . ?
C22 C19 C16 119.6(3) . . ?
C22 C19 N8 114.3(3) . . ?
C16 C19 N8 126.1(3) . . ?
N8 N6 C21 112.0(3) . . ?
C26 C31 C38 118.5(4) . . ?
C26 C31 H31 120.7 . . ?
C38 C31 H31 120.7 . . ?
C35 C33 C36 120.0(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 118.9(4) . . ?
C29 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C21 C30 C27 119.9(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C21 C25 C28 119.5(3) . . ?
C21 C25 H25 120.2 . . ?
C28 C25 H25 120.2 . . ?
C29 C37 C36 119.6(4) . . ?
C29 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.739
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.739
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_feaza260km1
_database_code_depnum_ccdc_archive 'CCDC 1492664'
_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                   15.1103(11)
_cell_length_b                   14.4939(12)
_cell_length_c                   17.0017(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.063(4)
_cell_angle_gamma                90.00
_cell_volume                     3718.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(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    1.330
_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  0.5531
_exptl_absorpt_correction_T_max  0.8963
_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      260(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            5872
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0424
_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         21.26
_reflns_number_total             3506
_reflns_number_gt                2763
_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)+(0.0301P)²+2.0259P] 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         3506
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0796
_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 0.29133(3) 0.28749(4) 0.05595(3) 0.0530(2) Uani 1 1 d . . .
S1 S 0.18909(6) 0.49731(8) -0.14676(6) 0.0670(3) Uani 1 1 d . . .
S2 S 0.43674(7) 0.07274(8) -0.10634(6) 0.0755(4) Uani 1 1 d . . .
N1 N 0.17148(18) 0.2157(2) 0.07864(18) 0.0510(8) Uani 1 1 d . . .
N2 N 0.27343(17) 0.37983(19) 0.16049(15) 0.0421(7) Uani 1 1 d . . .
C1 C 0.1971(2) 0.3852(2) 0.2070(2) 0.0428(9) Uani 1 1 d . . .
C2 C 0.4139(2) 0.1810(2) 0.1913(2) 0.0496(10) Uani 1 1 d . . .
C3 C 0.2135(2) 0.4256(3) -0.0753(2) 0.0533(10) Uani 1 1 d . . .
N3 N 0.32764(19) 0.19069(19) 0.15422(16) 0.0478(8) Uani 1 1 d . . .
C4 C 0.3443(2) 0.4199(2) 0.1851(2) 0.0502(9) Uani 1 1 d . . .
H4 H 0.3458 0.4537 0.2317 0.060 Uiso 1 1 calc R . .
C5 C 0.2612(3) 0.1524(2) 0.1835(2) 0.0520(10) Uani 1 1 d . . .
H5 H 0.2684 0.1172 0.2291 0.062 Uiso 1 1 calc R . .
N4 N 0.41460(18) 0.3606(2) 0.0748(2) 0.0583(9) Uani 1 1 d . . .
N5 N 0.3417(2) 0.2024(3) -0.0268(2) 0.0774(11) Uani 1 1 d . . .
C6 C 0.1733(2) 0.1644(3) 0.1444(2) 0.0493(9) Uani 1 1 d . . .
C7 C 0.0410(2) 0.4032(3) 0.2110(3) 0.0636(11) Uani 1 1 d . . .
H7 H -0.0143 0.4127 0.1855 0.076 Uiso 1 1 calc R . .
C8 C 0.1158(2) 0.3996(2) 0.1690(2) 0.0530(10) Uani 1 1 d . . .
H8 H 0.1116 0.4069 0.1146 0.064 Uiso 1 1 calc R . .
C9 C 0.0487(3) 0.3925(3) 0.2912(4) 0.0725(13) Uani 1 1 d . . .
C10 C 0.0938(3) 0.2254(3) 0.0387(2) 0.0669(11) Uani 1 1 d . . .
H10 H 0.0916 0.2598 -0.0075 0.080 Uiso 1 1 calc R . .
C11 C 0.4823(2) 0.1579(3) 0.1442(2) 0.0645(11) Uani 1 1 d . . .
H11 H 0.4703 0.1460 0.0909 0.077 Uiso 1 1 calc R . .
C12 C 0.3812(2) 0.1483(3) -0.0603(2) 0.0540(10) Uani 1 1 d . . .
C13 C 0.1293(3) 0.3778(3) 0.3297(3) 0.0775(13) Uani 1 1 d . . .
H13 H 0.1337 0.3707 0.3842 0.093 Uiso 1 1 calc R . .
C14 C 0.4322(3) 0.2003(3) 0.2698(2) 0.0615(11) Uani 1 1 d . . .
H14 H 0.3869 0.2168 0.3021 0.074 Uiso 1 1 calc R . .
C15 C 0.4236(2) 0.4127(3) 0.1401(3) 0.0543(10) Uani 1 1 d . . .
C16 C 0.5199(3) 0.1948(3) 0.3002(2) 0.0725(12) Uani 1 1 d . . .
H16 H 0.5331 0.2076 0.3532 0.087 Uiso 1 1 calc R . .
N6 N 0.6930(3) 0.1536(2) 0.3433(3) 0.0876(12) Uani 1 1 d . . .
C17 C 0.9631(3) 0.1176(3) 0.4184(3) 0.0731(12) Uani 1 1 d . . .
H17 H 1.0213 0.1076 0.4371 0.088 Uiso 1 1 calc R . .
N7 N 0.2302(2) 0.3757(3) -0.0238(2) 0.0717(10) Uani 1 1 d . . .
C18 C 0.0982(3) 0.1250(3) 0.1726(2) 0.0654(11) Uani 1 1 d . . .
H18 H 0.1015 0.0909 0.2191 0.078 Uiso 1 1 calc R . .
C19 C 0.5863(3) 0.1705(3) 0.2526(3) 0.0672(12) Uani 1 1 d . . .
N8 N 0.6852(2) 0.1627(2) 0.2752(2) 0.0800(11) Uani 1 1 d . . .
N9 N -0.0843(3) 0.3951(2) 0.3133(2) 0.0889(12) Uani 1 1 d . . .
N10 N -0.0261(3) 0.4018(3) 0.3557(3) 0.1045(16) Uani 1 1 d . . .
C20 C 0.0163(3) 0.1867(3) 0.0630(3) 0.0804(13) Uani 1 1 d . . .
H20 H -0.0366 0.1946 0.0333 0.097 Uiso 1 1 calc R . .
C21 C 0.7914(2) 0.1430(3) 0.3660(3) 0.0724(13) Uani 1 1 d . . .
C22 C 0.5676(3) 0.1526(3) 0.1754(3) 0.0701(12) Uani 1 1 d . . .
H22 H 0.6131 0.1366 0.1432 0.084 Uiso 1 1 calc R . .
C23 C 0.2029(2) 0.3737(3) 0.2871(3) 0.0628(11) Uani 1 1 d . . .
H23 H 0.2579 0.3629 0.3127 0.075 Uiso 1 1 calc R . .
C24 C 0.0182(3) 0.1368(3) 0.1309(3) 0.0789(13) Uani 1 1 d . . .
H24 H -0.0335 0.1113 0.1488 0.095 Uiso 1 1 calc R . .
C25 C 0.8586(3) 0.1616(3) 0.3154(3) 0.0829(13) Uani 1 1 d . . .
H25 H 0.8455 0.1821 0.2643 0.099 Uiso 1 1 calc R . .
C26 C 0.4845(3) 0.3547(3) 0.0310(3) 0.0887(14) Uani 1 1 d . . .
H26 H 0.4798 0.3201 -0.0151 0.106 Uiso 1 1 calc R . .
C27 C 0.8963(3) 0.1013(3) 0.4651(3) 0.0859(14) Uani 1 1 d . . .
H27 H 0.9088 0.0808 0.5164 0.103 Uiso 1 1 calc R . .
C28 C 0.9464(3) 0.1489(3) 0.3437(3) 0.0811(13) Uani 1 1 d . . .
H28 H 0.9928 0.1616 0.3116 0.097 Uiso 1 1 calc R . .
C29 C -0.1640(4) 0.4091(3) 0.3729(4) 0.0976(19) Uani 1 1 d . . .
C30 C 0.8109(3) 0.1141(3) 0.4391(3) 0.0885(14) Uani 1 1 d . . .
H30 H 0.7656 0.1025 0.4727 0.106 Uiso 1 1 calc R . .
C31 C 0.5638(4) 0.3982(5) 0.0512(5) 0.123(2) Uani 1 1 d . . .
H31 H 0.6111 0.3931 0.0186 0.147 Uiso 1 1 calc R . .
C32 C 0.5017(3) 0.4557(3) 0.1635(3) 0.0845(13) Uani 1 1 d . . .
H32 H 0.5058 0.4898 0.2099 0.101 Uiso 1 1 calc R . .
C33 C -0.3150(3) 0.4370(4) 0.4506(4) 0.0897(15) Uani 1 1 d . . .
H33 H -0.3673 0.4457 0.4761 0.108 Uiso 1 1 calc R . .
C34 C -0.2432(4) 0.3903(3) 0.3366(3) 0.0960(16) Uani 1 1 d . . .
H34 H -0.2466 0.3684 0.2851 0.115 Uiso 1 1 calc R . .
C35 C -0.3176(3) 0.4034(3) 0.3756(4) 0.0897(15) Uani 1 1 d . . .
H35 H -0.3721 0.3892 0.3506 0.108 Uiso 1 1 calc R . .
C36 C -0.2350(4) 0.4578(3) 0.4884(3) 0.0955(15) Uani 1 1 d . . .
H36 H -0.2325 0.4814 0.5393 0.115 Uiso 1 1 calc R . .
C37 C -0.1567(3) 0.4429(4) 0.4490(4) 0.0963(16) Uani 1 1 d . . .
H37 H -0.1016 0.4555 0.4734 0.116 Uiso 1 1 calc R . .
C38 C 0.5728(3) 0.4481(4) 0.1182(5) 0.1153(19) Uani 1 1 d . . .
H38 H 0.6263 0.4765 0.1330 0.138 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 2.048(4) . ?
Fe1 N5 2.048(4) . ?
Fe1 N1 2.141(3) . ?
Fe1 N4 2.152(3) . ?
Fe1 N3 2.228(3) . ?
Fe1 N2 2.253(3) . ?
S1 C3 1.627(5) . ?
S2 C12 1.609(5) . ?
N1 C10 1.331(4) . ?
N1 C6 1.342(4) . ?
N2 C4 1.270(4) . ?
N2 C1 1.435(4) . ?
C1 C23 1.370(5) . ?
C1 C8 1.373(4) . ?
C2 C14 1.377(5) . ?
C2 C11 1.382(5) . ?
C2 N3 1.424(4) . ?
C3 N7 1.152(4) . ?
N3 C5 1.271(4) . ?
C4 C15 1.459(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.463(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.327(4) . ?
N4 C15 1.343(4) . ?
N5 C12 1.154(4) . ?
C6 C18 1.379(5) . ?
C7 C9 1.370(6) . ?
C7 C8 1.371(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.370(6) . ?
C9 N10 1.622(6) . ?
C10 C20 1.382(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.370(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.360(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.399(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.376(5) . ?
C16 C19 1.370(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.165(4) . ?
N6 C21 1.524(5) . ?
C17 C27 1.339(5) . ?
C17 C28 1.359(5) . ?
C17 H17 0.9300 . ?
C18 C24 1.380(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.353(5) . ?
C19 N8 1.527(5) . ?
N9 N10 1.110(4) . ?
N9 C29 1.628(6) . ?
C20 C24 1.361(5) . ?
C20 H20 0.9300 . ?
C21 C30 1.331(6) . ?
C21 C25 1.391(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.399(5) . ?
C25 H25 0.9300 . ?
C26 C31 1.382(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.354(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.344(7) . ?
C29 C37 1.382(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.351(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.359(6) . ?
C32 H32 0.9300 . ?
C33 C35 1.364(6) . ?
C33 C36 1.372(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.349(6) . ?
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
N7 Fe1 N5 95.31(14) . . ?
N7 Fe1 N1 93.83(13) . . ?
N5 Fe1 N1 100.36(13) . . ?
N7 Fe1 N4 98.46(12) . . ?
N5 Fe1 N4 92.78(14) . . ?
N1 Fe1 N4 161.09(12) . . ?
N7 Fe1 N3 166.96(12) . . ?
N5 Fe1 N3 92.86(12) . . ?
N1 Fe1 N3 74.68(11) . . ?
N4 Fe1 N3 91.26(11) . . ?
N7 Fe1 N2 94.74(12) . . ?
N5 Fe1 N2 164.69(12) . . ?
N1 Fe1 N2 90.46(10) . . ?
N4 Fe1 N2 74.31(12) . . ?
N3 Fe1 N2 79.49(9) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Fe1 126.0(3) . . ?
C6 N1 Fe1 116.1(2) . . ?
C4 N2 C1 118.8(3) . . ?
C4 N2 Fe1 113.4(2) . . ?
C1 N2 Fe1 127.0(2) . . ?
C23 C1 C8 119.6(3) . . ?
C23 C1 N2 122.1(3) . . ?
C8 C1 N2 118.2(3) . . ?
C14 C2 C11 119.6(3) . . ?
C14 C2 N3 122.7(3) . . ?
C11 C2 N3 117.5(3) . . ?
N7 C3 S1 178.9(4) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.6(2) . . ?
C2 N3 Fe1 125.3(2) . . ?
N2 C4 C15 119.7(3) . . ?
N2 C4 H4 120.1 . . ?
C15 C4 H4 120.1 . . ?
N3 C5 C6 119.2(3) . . ?
N3 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C26 N4 C15 116.9(4) . . ?
C26 N4 Fe1 126.4(3) . . ?
C15 N4 Fe1 116.6(2) . . ?
C12 N5 Fe1 165.8(3) . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 114.9(3) . . ?
C18 C6 C5 122.5(4) . . ?
C9 C7 C8 119.1(3) . . ?
C9 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C7 C8 C1 120.2(4) . . ?
C7 C8 H8 119.9 . . ?
C1 C8 H8 119.9 . . ?
C13 C9 C7 121.3(3) . . ?
C13 C9 N10 108.9(5) . . ?
C7 C9 N10 129.7(4) . . ?
N1 C10 C20 122.8(4) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 120.4(4) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
N5 C12 S2 179.5(4) . . ?
C23 C13 C9 118.9(4) . . ?
C23 C13 H13 120.5 . . ?
C9 C13 H13 120.5 . . ?
C2 C14 C16 118.9(4) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
N4 C15 C32 122.8(4) . . ?
N4 C15 C4 115.2(3) . . ?
C32 C15 C4 122.0(4) . . ?
C19 C16 C14 120.4(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 108.0(4) . . ?
C27 C17 C28 120.3(4) . . ?
C27 C17 H17 119.8 . . ?
C28 C17 H17 119.8 . . ?
C3 N7 Fe1 165.3(3) . . ?
C6 C18 C24 118.9(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C22 C19 C16 120.1(4) . . ?
C22 C19 N8 112.4(4) . . ?
C16 C19 N8 127.5(4) . . ?
N6 N8 C19 107.8(4) . . ?
N10 N9 C29 99.9(5) . . ?
N9 N10 C9 96.3(5) . . ?
C24 C20 C10 119.4(4) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 120.4(4) . . ?
C30 C21 N6 115.6(4) . . ?
C25 C21 N6 124.0(5) . . ?
C19 C22 C11 120.5(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.9(4) . . ?
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 118.2(4) . . ?
C21 C25 H25 120.9 . . ?
C28 C25 H25 120.9 . . ?
N4 C26 C31 122.5(5) . . ?
N4 C26 H26 118.7 . . ?
C31 C26 H26 118.7 . . ?
C17 C27 C30 121.2(5) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C17 C28 C25 119.4(4) . . ?
C17 C28 H28 120.3 . . ?
C25 C28 H28 120.3 . . ?
C34 C29 C37 121.7(4) . . ?
C34 C29 N9 111.1(6) . . ?
C37 C29 N9 127.0(6) . . ?
C21 C30 C27 120.5(4) . . ?
C21 C30 H30 119.7 . . ?
C27 C30 H30 119.7 . . ?
C38 C31 C26 120.0(5) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C38 C32 C15 119.4(5) . . ?
C38 C32 H32 120.3 . . ?
C15 C32 H32 120.3 . . ?
C35 C33 C36 119.7(4) . . ?
C35 C33 H33 120.2 . . ?
C36 C33 H33 120.2 . . ?
C29 C34 C35 119.3(5) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C33 121.9(5) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C33 C36 C37 119.1(5) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C29 C37 C36 118.3(5) . . ?
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 0.847
_diffrn_reflns_theta_full        21.26
_diffrn_measured_fraction_theta_full 0.847
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.187
_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_feaza285kd2
_database_code_depnum_ccdc_archive 'CCDC 1492665'
_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                   15.1196(7)
_cell_length_b                   14.5444(10)
_cell_length_c                   17.0230(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.966(4)
_cell_angle_gamma                90.00
_cell_volume                     3738.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    285(2)
_cell_measurement_reflns_used    4232
_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    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5546
_exptl_absorpt_correction_T_max  0.8968
_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      285(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            5476
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -15
_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             3810
_reflns_number_gt                2988
_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+2.1896P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3810
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.29203(3) 0.28764(3) 0.05543(3) 0.0574(2) Uani 1 1 d . . .
S1 S 0.18863(6) 0.49674(7) -0.14671(6) 0.0727(3) Uani 1 1 d . . .
S2 S 0.43670(7) 0.07273(7) -0.10647(7) 0.0823(3) Uani 1 1 d . . .
N1 N 0.17206(19) 0.21595(18) 0.07828(18) 0.0573(8) Uani 1 1 d . . .
N2 N 0.27330(17) 0.37974(17) 0.16039(15) 0.0461(7) Uani 1 1 d . . .
C1 C 0.1976(2) 0.3852(2) 0.2067(2) 0.0467(8) Uani 1 1 d . . .
C2 C 0.4140(2) 0.1807(2) 0.1914(2) 0.0542(9) Uani 1 1 d . . .
C3 C 0.2137(2) 0.4255(3) -0.0754(2) 0.0580(10) Uani 1 1 d . . .
N3 N 0.3276(2) 0.19038(18) 0.15401(16) 0.0519(7) Uani 1 1 d . . .
C4 C 0.3443(2) 0.4198(2) 0.1853(2) 0.0562(9) Uani 1 1 d . . .
H4 H 0.3456 0.4535 0.2317 0.067 Uiso 1 1 calc R . .
C5 C 0.2611(3) 0.1522(2) 0.1832(2) 0.0573(9) Uani 1 1 d . . .
H5 H 0.2681 0.1170 0.2287 0.069 Uiso 1 1 calc R . .
N4 N 0.41533(18) 0.3609(2) 0.07488(19) 0.0641(8) Uani 1 1 d . . .
N5 N 0.3432(2) 0.2027(2) -0.0272(2) 0.0829(10) Uani 1 1 d . . .
C6 C 0.1735(2) 0.1646(2) 0.1440(2) 0.0550(9) Uani 1 1 d . . .
C7 C 0.0410(2) 0.4033(2) 0.2114(3) 0.0709(11) Uani 1 1 d . . .
H7 H -0.0143 0.4130 0.1863 0.085 Uiso 1 1 calc R . .
C8 C 0.1160(2) 0.3994(2) 0.1685(2) 0.0594(10) Uani 1 1 d . . .
H8 H 0.1116 0.4064 0.1141 0.071 Uiso 1 1 calc R . .
C9 C 0.0490(3) 0.3926(2) 0.2912(3) 0.0758(13) Uani 1 1 d . . .
C10 C 0.0947(3) 0.2253(3) 0.0379(2) 0.0730(11) Uani 1 1 d . . .
H10 H 0.0928 0.2590 -0.0085 0.088 Uiso 1 1 calc R . .
C11 C 0.4819(3) 0.1573(2) 0.1442(2) 0.0700(11) Uani 1 1 d . . .
H11 H 0.4698 0.1450 0.0911 0.084 Uiso 1 1 calc R . .
C12 C 0.3821(2) 0.1485(3) -0.0604(2) 0.0590(10) Uani 1 1 d . . .
C13 C 0.1294(3) 0.3780(3) 0.3292(3) 0.0830(12) Uani 1 1 d . . .
H13 H 0.1338 0.3709 0.3836 0.100 Uiso 1 1 calc R . .
C14 C 0.4325(3) 0.2006(2) 0.2699(2) 0.0704(11) Uani 1 1 d . . .
H14 H 0.3874 0.2178 0.3020 0.085 Uiso 1 1 calc R . .
C15 C 0.4239(2) 0.4124(2) 0.1402(3) 0.0605(10) Uani 1 1 d . . .
C16 C 0.5198(3) 0.1946(3) 0.3003(3) 0.0790(12) Uani 1 1 d . . .
H16 H 0.5332 0.2072 0.3532 0.095 Uiso 1 1 calc R . .
N6 N 0.6912(3) 0.1543(2) 0.3426(3) 0.0983(13) Uani 1 1 d . . .
C17 C 0.9621(3) 0.1179(3) 0.4178(3) 0.0821(13) Uani 1 1 d . . .
H17 H 1.0202 0.1076 0.4364 0.098 Uiso 1 1 calc R . .
N7 N 0.2310(2) 0.3759(2) -0.0238(2) 0.0778(10) Uani 1 1 d . . .
C18 C 0.0986(3) 0.1253(2) 0.1721(2) 0.0735(11) Uani 1 1 d . . .
H18 H 0.1018 0.0912 0.2183 0.088 Uiso 1 1 calc R . .
C19 C 0.5856(3) 0.1702(3) 0.2524(3) 0.0760(12) Uani 1 1 d . . .
N8 N 0.6866(3) 0.1619(2) 0.2758(2) 0.0888(12) Uani 1 1 d . . .
N9 N -0.0832(3) 0.3955(2) 0.3130(2) 0.0967(13) Uani 1 1 d . . .
N10 N -0.0280(3) 0.4024(2) 0.3562(3) 0.1126(16) Uani 1 1 d . . .
C20 C 0.0171(3) 0.1870(3) 0.0622(3) 0.0903(14) Uani 1 1 d . . .
H20 H -0.0356 0.1950 0.0324 0.108 Uiso 1 1 calc R . .
C21 C 0.7917(2) 0.1430(3) 0.3650(4) 0.0813(14) Uani 1 1 d . . .
C22 C 0.5670(3) 0.1523(3) 0.1752(3) 0.0801(12) Uani 1 1 d . . .
H22 H 0.6125 0.1365 0.1431 0.096 Uiso 1 1 calc R . .
C23 C 0.2029(2) 0.3739(3) 0.2869(2) 0.0689(10) Uani 1 1 d . . .
H23 H 0.2577 0.3634 0.3126 0.083 Uiso 1 1 calc R . .
C24 C 0.0186(3) 0.1375(3) 0.1301(3) 0.0861(13) Uani 1 1 d . . .
H24 H -0.0333 0.1124 0.1481 0.103 Uiso 1 1 calc R . .
C25 C 0.8581(3) 0.1609(3) 0.3154(3) 0.0918(14) Uani 1 1 d . . .
H25 H 0.8453 0.1806 0.2641 0.110 Uiso 1 1 calc R . .
C26 C 0.4851(3) 0.3547(3) 0.0316(3) 0.0982(14) Uani 1 1 d . . .
H26 H 0.4805 0.3197 -0.0141 0.118 Uiso 1 1 calc R . .
C27 C 0.8962(3) 0.1021(3) 0.4644(3) 0.0978(14) Uani 1 1 d . . .
H27 H 0.9090 0.0820 0.5156 0.117 Uiso 1 1 calc R . .
C28 C 0.9458(3) 0.1487(3) 0.3440(4) 0.0919(14) Uani 1 1 d . . .
H28 H 0.9924 0.1618 0.3122 0.110 Uiso 1 1 calc R . .
C29 C -0.1627(4) 0.4090(3) 0.3736(4) 0.104(2) Uani 1 1 d . . .
C30 C 0.8108(3) 0.1146(3) 0.4391(4) 0.1037(16) Uani 1 1 d . . .
H30 H 0.7654 0.1037 0.4728 0.124 Uiso 1 1 calc R . .
C31 C 0.5643(4) 0.3979(5) 0.0511(5) 0.133(2) Uani 1 1 d . . .
H31 H 0.6116 0.3928 0.0185 0.160 Uiso 1 1 calc R . .
C32 C 0.5019(3) 0.4556(3) 0.1650(3) 0.0933(14) Uani 1 1 d . . .
H32 H 0.5063 0.4888 0.2117 0.112 Uiso 1 1 calc R . .
C33 C -0.3141(3) 0.4368(3) 0.4508(4) 0.0988(15) Uani 1 1 d . . .
H33 H -0.3666 0.4458 0.4758 0.119 Uiso 1 1 calc R . .
C34 C -0.2416(4) 0.3904(3) 0.3381(3) 0.1014(16) Uani 1 1 d . . .
H34 H -0.2448 0.3684 0.2868 0.122 Uiso 1 1 calc R . .
C35 C -0.3164(3) 0.4032(3) 0.3760(4) 0.0987(15) Uani 1 1 d . . .
H35 H -0.3707 0.3888 0.3508 0.118 Uiso 1 1 calc R . .
C36 C -0.2344(4) 0.4575(3) 0.4892(3) 0.1060(15) Uani 1 1 d . . .
H36 H -0.2321 0.4804 0.5403 0.127 Uiso 1 1 calc R . .
C37 C -0.1564(3) 0.4430(3) 0.4491(4) 0.1064(17) Uani 1 1 d . . .
H37 H -0.1014 0.4562 0.4734 0.128 Uiso 1 1 calc R . .
C38 C 0.5727(3) 0.4477(4) 0.1181(5) 0.128(2) Uani 1 1 d . . .
H38 H 0.6261 0.4764 0.1323 0.154 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 2.047(4) . ?
Fe1 N5 2.053(4) . ?
Fe1 N1 2.145(3) . ?
Fe1 N4 2.158(3) . ?
Fe1 N3 2.239(3) . ?
Fe1 N2 2.262(3) . ?
S1 C3 1.626(5) . ?
S2 C12 1.605(4) . ?
N1 C10 1.333(4) . ?
N1 C6 1.344(4) . ?
N2 C4 1.275(4) . ?
N2 C1 1.425(4) . ?
C1 C23 1.373(4) . ?
C1 C8 1.380(4) . ?
C2 C11 1.379(5) . ?
C2 C14 1.381(5) . ?
C2 N3 1.430(4) . ?
C3 N7 1.156(4) . ?
N3 C5 1.271(4) . ?
C4 C15 1.464(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.463(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.320(5) . ?
N4 C15 1.341(4) . ?
N5 C12 1.150(4) . ?
C6 C18 1.376(5) . ?
C7 C9 1.367(5) . ?
C7 C8 1.382(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.364(5) . ?
C9 N10 1.653(6) . ?
C10 C20 1.381(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.368(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.356(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.397(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.384(5) . ?
C16 C19 1.365(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.141(4) . ?
N6 C21 1.557(5) . ?
C17 C27 1.325(6) . ?
C17 C28 1.345(6) . ?
C17 H17 0.9300 . ?
C18 C24 1.385(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.355(5) . ?
C19 N8 1.564(5) . ?
N9 N10 1.089(4) . ?
N9 C29 1.635(6) . ?
C20 C24 1.361(6) . ?
C20 H20 0.9300 . ?
C21 C30 1.344(6) . ?
C21 C25 1.369(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.400(6) . ?
C25 H25 0.9300 . ?
C26 C31 1.378(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.353(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.336(7) . ?
C29 C37 1.377(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.351(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.372(7) . ?
C32 H32 0.9300 . ?
C33 C35 1.362(6) . ?
C33 C36 1.374(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.344(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.408(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
N7 Fe1 N5 95.71(13) . . ?
N7 Fe1 N1 93.88(13) . . ?
N5 Fe1 N1 100.59(12) . . ?
N7 Fe1 N4 98.50(12) . . ?
N5 Fe1 N4 92.80(13) . . ?
N1 Fe1 N4 160.75(12) . . ?
N7 Fe1 N3 166.59(12) . . ?
N5 Fe1 N3 92.77(11) . . ?
N1 Fe1 N3 74.32(12) . . ?
N4 Fe1 N3 91.42(11) . . ?
N7 Fe1 N2 94.50(11) . . ?
N5 Fe1 N2 164.60(11) . . ?
N1 Fe1 N2 90.17(10) . . ?
N4 Fe1 N2 74.27(11) . . ?
N3 Fe1 N2 79.47(9) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Fe1 125.8(3) . . ?
C6 N1 Fe1 116.3(2) . . ?
C4 N2 C1 118.6(3) . . ?
C4 N2 Fe1 113.3(2) . . ?
C1 N2 Fe1 127.3(2) . . ?
C23 C1 C8 119.5(3) . . ?
C23 C1 N2 122.4(3) . . ?
C8 C1 N2 118.1(3) . . ?
C11 C2 C14 119.7(3) . . ?
C11 C2 N3 117.1(3) . . ?
C14 C2 N3 123.0(3) . . ?
N7 C3 S1 178.8(4) . . ?
C5 N3 C2 120.3(3) . . ?
C5 N3 Fe1 113.8(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 119.6(3) . . ?
N2 C4 H4 120.2 . . ?
C15 C4 H4 120.2 . . ?
N3 C5 C6 119.0(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C26 N4 C15 117.0(4) . . ?
C26 N4 Fe1 126.1(3) . . ?
C15 N4 Fe1 116.7(2) . . ?
C12 N5 Fe1 166.0(3) . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.2(4) . . ?
C9 C7 C8 119.2(3) . . ?
C9 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C1 C8 C7 119.6(4) . . ?
C1 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C13 C9 C7 121.3(3) . . ?
C13 C9 N10 109.7(4) . . ?
C7 C9 N10 128.8(4) . . ?
N1 C10 C20 122.8(4) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
C22 C11 C2 120.2(4) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
N5 C12 S2 179.7(4) . . ?
C23 C13 C9 119.3(4) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.1(4) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
N4 C15 C32 123.4(4) . . ?
N4 C15 C4 115.4(3) . . ?
C32 C15 C4 121.2(4) . . ?
C19 C16 C14 119.9(4) . . ?
C19 C16 H16 120.1 . . ?
C14 C16 H16 120.1 . . ?
N8 N6 C21 105.2(4) . . ?
C27 C17 C28 120.6(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C3 N7 Fe1 165.6(3) . . ?
C6 C18 C24 118.8(4) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.6(4) . . ?
C22 C19 N8 112.5(4) . . ?
C16 C19 N8 126.9(5) . . ?
N6 N8 C19 105.5(4) . . ?
N10 N9 C29 97.2(5) . . ?
N9 N10 C9 94.7(5) . . ?
C24 C20 C10 119.4(4) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C30 C21 C25 120.6(4) . . ?
C30 C21 N6 114.9(5) . . ?
C25 C21 N6 124.5(5) . . ?
C19 C22 C11 120.5(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 121.0(4) . . ?
C13 C23 H23 119.5 . . ?
C1 C23 H23 119.5 . . ?
C20 C24 C18 118.7(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C21 C25 C28 118.2(5) . . ?
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 121.4(5) . . ?
C17 C27 H27 119.3 . . ?
C30 C27 H27 119.3 . . ?
C17 C28 C25 119.5(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 120.8(4) . . ?
C34 C29 N9 111.1(6) . . ?
C37 C29 N9 127.9(6) . . ?
C21 C30 C27 119.7(5) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C38 C31 C26 119.3(5) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C38 C32 C15 117.6(5) . . ?
C38 C32 H32 121.2 . . ?
C15 C32 H32 121.2 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 120.6(5) . . ?
C29 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C33 121.2(5) . . ?
C34 C35 H35 119.4 . . ?
C33 C35 H35 119.4 . . ?
C33 C36 C37 118.2(5) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
C29 C37 C36 119.2(5) . . ?
C29 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C31 C38 C32 119.6(5) . . ?
C31 C38 H38 120.2 . . ?
C32 C38 H38 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        21.26
_diffrn_measured_fraction_theta_full 0.916
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.032
####################################################################### 
# 
# 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_znaza110kd
_database_code_depnum_ccdc_archive 'CCDC 1492666'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0918(6)
_cell_length_b                   14.2146(9)
_cell_length_c                   17.1441(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.286(3)
_cell_angle_gamma                90.00
_cell_volume                     3667.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    14315
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_T_max  0.7075
_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            6199
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4780
_reflns_number_gt                4413
_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)+(0.0332P)²+8.0341P] 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         4780
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1069
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
Zn01 Zn 0.71828(3) 0.28337(3) 0.44606(2) 0.02333(15) Uani 1 1 d . . .
S1 S 0.80774(6) 0.50230(7) 0.64752(4) 0.0282(2) Uani 1 1 d . . .
S2 S 0.56201(7) 0.07304(7) 0.60327(5) 0.0332(3) Uani 1 1 d . . .
N9 N 1.0947(2) 0.3954(2) 0.18439(17) 0.0302(7) Uani 1 1 d . . .
N7 N 0.7806(2) 0.3739(2) 0.52446(16) 0.0312(7) Uani 1 1 d . . .
N2 N 0.73169(19) 0.38139(19) 0.33843(14) 0.0207(6) Uani 1 1 d . . .
C29 C 1.1677(3) 0.4098(3) 0.1352(2) 0.0298(9) Uani 1 1 d . . .
N3 N 0.67616(19) 0.18741(19) 0.34192(15) 0.0215(7) Uani 1 1 d . . .
N1 N 0.83571(19) 0.21261(19) 0.41830(15) 0.0237(7) Uani 1 1 d . . .
C1 C 0.8044(2) 0.3864(2) 0.29049(18) 0.0210(8) Uani 1 1 d . . .
C3 C 0.7913(2) 0.4270(3) 0.57608(18) 0.0233(8) Uani 1 1 d . . .
N4 N 0.59469(19) 0.3585(2) 0.42897(16) 0.0263(7) Uani 1 1 d . . .
C12 C 0.6258(2) 0.1429(3) 0.55790(18) 0.0250(8) Uani 1 1 d . . .
C8 C 0.8891(2) 0.4015(2) 0.32624(18) 0.0245(8) Uani 1 1 d . . .
H8 H 0.8971 0.4091 0.3814 0.029 Uiso 1 1 calc R . .
C10 C 0.9148(3) 0.2216(2) 0.45828(19) 0.0286(9) Uani 1 1 d . . .
H10 H 0.9181 0.2542 0.5068 0.034 Uiso 1 1 calc R . .
N10 N 1.0200(2) 0.4003(2) 0.14862(17) 0.0325(8) Uani 1 1 d . . .
C15 C 0.5814(2) 0.4099(3) 0.36271(19) 0.0263(8) Uani 1 1 d . . .
C4 C 0.6574(2) 0.4188(2) 0.31523(18) 0.0243(8) Uani 1 1 d . . .
H4 H 0.6516 0.4524 0.2672 0.029 Uiso 1 1 calc R . .
C6 C 0.8322(2) 0.1638(2) 0.35018(18) 0.0230(8) Uani 1 1 d . . .
C2 C 0.5885(2) 0.1784(2) 0.30626(18) 0.0226(8) Uani 1 1 d . . .
C11 C 0.5221(2) 0.1550(3) 0.35496(19) 0.0291(9) Uani 1 1 d . . .
H11 H 0.5367 0.1419 0.4087 0.035 Uiso 1 1 calc R . .
C23 C 0.7931(2) 0.3733(3) 0.20976(18) 0.0278(8) Uani 1 1 d . . .
H23 H 0.7356 0.3614 0.1853 0.033 Uiso 1 1 calc R . .
N5 N 0.6712(2) 0.1927(2) 0.52552(16) 0.0348(8) Uani 1 1 d . . .
C13 C 0.8659(3) 0.3777(3) 0.1654(2) 0.0308(9) Uani 1 1 d . . .
H13 H 0.8582 0.3697 0.1103 0.037 Uiso 1 1 calc R . .
C18 C 0.9064(2) 0.1267(3) 0.3202(2) 0.0291(9) Uani 1 1 d . . .
H18 H 0.9018 0.0939 0.2718 0.035 Uiso 1 1 calc R . .
C9 C 0.9493(2) 0.3935(2) 0.20062(19) 0.0262(8) Uani 1 1 d . . .
C17 C 0.0335(3) 0.1155(3) 0.0774(2) 0.0301(9) Uani 1 1 d . . .
H17 H -0.0269 0.1045 0.0602 0.036 Uiso 1 1 calc R . .
C7 C 0.9610(2) 0.4055(2) 0.28170(19) 0.0272(8) Uani 1 1 d . . .
H7 H 1.0187 0.4165 0.3060 0.033 Uiso 1 1 calc R . .
N8 N 0.3198(2) 0.1612(2) 0.22183(16) 0.0305(7) Uani 1 1 d . . .
C38 C 0.4314(3) 0.4420(3) 0.3893(3) 0.0474(11) Uani 1 1 d . . .
H38 H 0.3752 0.4700 0.3757 0.057 Uiso 1 1 calc R . .
C32 C 0.5005(3) 0.4511(3) 0.3407(2) 0.0373(10) Uani 1 1 d . . .
H32 H 0.4922 0.4851 0.2930 0.045 Uiso 1 1 calc R . .
C16 C 0.4793(2) 0.1947(3) 0.19756(19) 0.0281(9) Uani 1 1 d . . .
H16 H 0.4644 0.2088 0.1440 0.034 Uiso 1 1 calc R . .
C5 C 0.7423(2) 0.1515(2) 0.31074(18) 0.0234(8) Uani 1 1 d . . .
H5 H 0.7340 0.1175 0.2631 0.028 Uiso 1 1 calc R . .
C14 C 0.5673(2) 0.1994(2) 0.22770(18) 0.0262(8) Uani 1 1 d . . .
H14 H 0.6126 0.2167 0.1949 0.031 Uiso 1 1 calc R . .
C20 C 0.9923(3) 0.1850(3) 0.4317(2) 0.0326(9) Uani 1 1 d . . .
H20 H 1.0474 0.1926 0.4617 0.039 Uiso 1 1 calc R . .
C22 C 0.4343(3) 0.1509(3) 0.3245(2) 0.0307(9) Uani 1 1 d . . .
H22 H 0.3888 0.1353 0.3576 0.037 Uiso 1 1 calc R . .
C27 C 0.0995(3) 0.0961(3) 0.0284(2) 0.0340(9) Uani 1 1 d . . .
H27 H 0.0845 0.0729 -0.0228 0.041 Uiso 1 1 calc R . .
C24 C 0.9885(3) 0.1379(3) 0.3618(2) 0.0334(9) Uani 1 1 d . . .
H24 H 1.0409 0.1134 0.3420 0.040 Uiso 1 1 calc R . .
C21 C 0.2097(2) 0.1422(3) 0.1287(2) 0.0274(8) Uani 1 1 d . . .
C35 C 1.3252(3) 0.4034(3) 0.1298(2) 0.0357(9) Uani 1 1 d . . .
H35 H 1.3825 0.3892 0.1538 0.043 Uiso 1 1 calc R . .
C28 C 0.0552(3) 0.1508(3) 0.1514(2) 0.0331(9) Uani 1 1 d . . .
H28 H 0.0095 0.1655 0.1846 0.040 Uiso 1 1 calc R . .
C36 C 1.2331(3) 0.4591(3) 0.0190(2) 0.0386(10) Uani 1 1 d . . .
H36 H 1.2272 0.4835 -0.0328 0.046 Uiso 1 1 calc R . .
C26 C 0.5276(3) 0.3507(3) 0.4750(2) 0.0361(10) Uani 1 1 d . . .
H26 H 0.5368 0.3152 0.5218 0.043 Uiso 1 1 calc R . .
C19 C 0.4127(2) 0.1695(2) 0.2457(2) 0.0262(8) Uani 1 1 d . . .
N6 N 0.3033(2) 0.1509(2) 0.15013(16) 0.0291(7) Uani 1 1 d . . .
C31 C 0.4462(3) 0.3913(3) 0.4582(3) 0.0471(11) Uani 1 1 d . . .
H31 H 0.4005 0.3848 0.4931 0.056 Uiso 1 1 calc R . .
C33 C 1.3168(3) 0.4378(3) 0.0543(2) 0.0386(10) Uani 1 1 d . . .
H33 H 1.3682 0.4470 0.0265 0.046 Uiso 1 1 calc R . .
C34 C 1.2506(3) 0.3895(3) 0.1708(2) 0.0337(9) Uani 1 1 d . . .
H34 H 1.2564 0.3663 0.2228 0.040 Uiso 1 1 calc R . .
C30 C 0.1874(3) 0.1103(3) 0.0537(2) 0.0308(9) Uani 1 1 d . . .
H30 H 0.2327 0.0981 0.0195 0.037 Uiso 1 1 calc R . .
C25 C 0.1434(3) 0.1648(3) 0.1774(2) 0.0329(9) Uani 1 1 d . . .
H25 H 0.1583 0.1897 0.2281 0.040 Uiso 1 1 calc R . .
C37 C 1.1584(3) 0.4446(3) 0.0597(2) 0.0354(9) Uani 1 1 d . . .
H37 H 1.1011 0.4586 0.0359 0.042 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
Zn01 N7 2.039(3) . ?
Zn01 N5 2.041(3) . ?
Zn01 N1 2.123(3) . ?
Zn01 N4 2.151(3) . ?
Zn01 N3 2.298(3) . ?
Zn01 N2 2.333(3) . ?
S1 C3 1.631(3) . ?
S2 C12 1.622(4) . ?
N9 N10 1.245(4) . ?
N9 C29 1.451(5) . ?
N7 C3 1.166(4) . ?
N2 C4 1.277(4) . ?
N2 C1 1.421(4) . ?
C29 C34 1.380(5) . ?
C29 C37 1.383(5) . ?
N3 C5 1.273(4) . ?
N3 C2 1.421(4) . ?
N1 C10 1.338(4) . ?
N1 C6 1.356(4) . ?
C1 C8 1.393(5) . ?
C1 C23 1.394(4) . ?
N4 C26 1.334(5) . ?
N4 C15 1.353(5) . ?
C12 N5 1.157(5) . ?
C8 C7 1.374(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.387(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.443(5) . ?
C15 C32 1.380(5) . ?
C15 C4 1.461(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.372(5) . ?
C6 C5 1.481(5) . ?
C2 C11 1.393(5) . ?
C2 C14 1.393(4) . ?
C11 C22 1.387(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.384(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.374(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.391(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.399(5) . ?
C17 C27 1.377(5) . ?
C17 C28 1.381(5) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.245(4) . ?
N8 C19 1.436(5) . ?
C38 C31 1.387(6) . ?
C38 C32 1.388(6) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C14 1.390(5) . ?
C16 C19 1.393(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.371(5) . ?
C20 H20 0.9500 . ?
C22 C19 1.392(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.378(5) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.381(5) . ?
C21 C25 1.388(5) . ?
C21 N6 1.438(5) . ?
C35 C33 1.380(5) . ?
C35 C34 1.386(5) . ?
C35 H35 0.9500 . ?
C28 C25 1.387(5) . ?
C28 H28 0.9500 . ?
C36 C37 1.384(5) . ?
C36 C33 1.394(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.368(6) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N5 97.16(12) . . ?
N7 Zn01 N1 95.46(11) . . ?
N5 Zn01 N1 100.87(12) . . ?
N7 Zn01 N4 97.41(12) . . ?
N5 Zn01 N4 93.62(12) . . ?
N1 Zn01 N4 159.24(10) . . ?
N7 Zn01 N3 166.83(12) . . ?
N5 Zn01 N3 93.10(11) . . ?
N1 Zn01 N3 74.43(10) . . ?
N4 Zn01 N3 90.13(10) . . ?
N7 Zn01 N2 94.68(11) . . ?
N5 Zn01 N2 163.76(11) . . ?
N1 Zn01 N2 88.99(10) . . ?
N4 Zn01 N2 73.81(11) . . ?
N3 Zn01 N2 77.02(9) . . ?
N10 N9 C29 113.9(3) . . ?
C3 N7 Zn01 160.1(3) . . ?
C4 N2 C1 119.8(3) . . ?
C4 N2 Zn01 111.7(2) . . ?
C1 N2 Zn01 127.1(2) . . ?
C34 C29 C37 120.9(4) . . ?
C34 C29 N9 114.6(3) . . ?
C37 C29 N9 124.5(4) . . ?
C5 N3 C2 121.1(3) . . ?
C5 N3 Zn01 112.6(2) . . ?
C2 N3 Zn01 125.6(2) . . ?
C10 N1 C6 117.8(3) . . ?
C10 N1 Zn01 124.6(2) . . ?
C6 N1 Zn01 117.1(2) . . ?
C8 C1 C23 119.8(3) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.7(3) . . ?
N7 C3 S1 178.9(4) . . ?
C26 N4 C15 118.0(3) . . ?
C26 N4 Zn01 124.5(3) . . ?
C15 N4 Zn01 117.1(2) . . ?
N5 C12 S2 179.9(4) . . ?
C7 C8 C1 119.9(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 122.6(3) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
N9 N10 C9 112.1(3) . . ?
N4 C15 C32 122.1(4) . . ?
N4 C15 C4 116.2(3) . . ?
C32 C15 C4 121.7(3) . . ?
N2 C4 C15 119.9(3) . . ?
N2 C4 H4 120.1 . . ?
C15 C4 H4 120.1 . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 115.4(3) . . ?
C18 C6 C5 122.0(3) . . ?
C11 C2 C14 120.4(3) . . ?
C11 C2 N3 116.9(3) . . ?
C14 C2 N3 122.4(3) . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
C13 C23 C1 119.8(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C12 N5 Zn01 162.9(3) . . ?
C9 C13 C23 120.3(3) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C6 C18 C24 119.0(3) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.0(3) . . ?
C13 C9 N10 115.7(3) . . ?
C7 C9 N10 124.2(3) . . ?
C27 C17 C28 120.0(3) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C8 C7 C9 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C9 C7 H7 120.0 . . ?
N6 N8 C19 114.3(3) . . ?
C31 C38 C32 118.6(4) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?
C15 C32 C38 119.0(4) . . ?
C15 C32 H32 120.5 . . ?
C38 C32 H32 120.5 . . ?
C14 C16 C19 120.2(3) . . ?
C14 C16 H16 119.9 . . ?
C19 C16 H16 119.9 . . ?
N3 C5 C6 118.8(3) . . ?
N3 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C16 C14 C2 119.6(3) . . ?
C16 C14 H14 120.2 . . ?
C2 C14 H14 120.2 . . ?
C24 C20 C10 119.2(3) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C11 C22 C19 120.3(3) . . ?
C11 C22 H22 119.8 . . ?
C19 C22 H22 119.8 . . ?
C17 C27 C30 120.1(3) . . ?
C17 C27 H27 119.9 . . ?
C30 C27 H27 119.9 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.0(3) . . ?
C30 C21 N6 115.6(3) . . ?
C25 C21 N6 124.4(3) . . ?
C33 C35 C34 120.3(4) . . ?
C33 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C17 C28 C25 120.3(4) . . ?
C17 C28 H28 119.9 . . ?
C25 C28 H28 119.9 . . ?
C37 C36 C33 119.6(4) . . ?
C37 C36 H36 120.2 . . ?
C33 C36 H36 120.2 . . ?
N4 C26 C31 123.3(4) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C22 C19 C16 119.8(3) . . ?
C22 C19 N8 114.5(3) . . ?
C16 C19 N8 125.8(3) . . ?
N8 N6 C21 112.6(3) . . ?
C26 C31 C38 118.9(4) . . ?
C26 C31 H31 120.6 . . ?
C38 C31 H31 120.6 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 119.4(4) . . ?
C29 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C27 C30 C21 120.2(4) . . ?
C27 C30 H30 119.9 . . ?
C21 C30 H30 119.9 . . ?
C28 C25 C21 119.4(3) . . ?
C28 C25 H25 120.3 . . ?
C21 C25 H25 120.3 . . ?
C29 C37 C36 119.7(4) . . ?
C29 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?

_diffrn_measured_fraction_theta_max 0.738
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.738
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_znaza160km
_database_code_depnum_ccdc_archive 'CCDC 1492667'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0970(6)
_cell_length_b                   14.3013(9)
_cell_length_c                   17.1496(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.136(4)
_cell_angle_gamma                90.00
_cell_volume                     3693.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    14690
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_T_max  0.7091
_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            6250
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4824
_reflns_number_gt                4274
_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)+(0.0562P)²+5.6740P] 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         4824
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1185
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
Zn01 Zn 0.71599(3) 0.28395(3) 0.44646(2) 0.03252(17) Uani 1 1 d . . .
S1 S 0.80761(7) 0.50068(7) 0.64745(5) 0.0390(3) Uani 1 1 d . . .
S2 S 0.56264(7) 0.07243(8) 0.60391(6) 0.0462(3) Uani 1 1 d . . .
N9 N 1.0931(2) 0.3955(2) 0.18501(19) 0.0448(9) Uani 1 1 d . . .
N7 N 0.7781(2) 0.3739(2) 0.52467(18) 0.0428(8) Uani 1 1 d . . .
N2 N 0.73155(19) 0.38114(19) 0.33843(15) 0.0275(7) Uani 1 1 d . . .
C29 C 1.1685(3) 0.4099(3) 0.1349(2) 0.0447(11) Uani 1 1 d . . .
N3 N 0.6746(2) 0.1877(2) 0.34238(15) 0.0294(7) Uani 1 1 d . . .
N1 N 0.8331(2) 0.2128(2) 0.41956(16) 0.0327(7) Uani 1 1 d . . .
C1 C 0.8047(2) 0.3865(2) 0.29101(18) 0.0274(8) Uani 1 1 d . . .
C3 C 0.7898(2) 0.4266(3) 0.57600(19) 0.0327(9) Uani 1 1 d . . .
N4 N 0.5929(2) 0.3591(2) 0.42786(17) 0.0372(8) Uani 1 1 d . . .
C12 C 0.6241(2) 0.1437(3) 0.55826(18) 0.0331(9) Uani 1 1 d . . .
C8 C 0.8888(2) 0.4004(3) 0.3273(2) 0.0331(9) Uani 1 1 d . . .
H8 H 0.8964 0.4070 0.3825 0.040 Uiso 1 1 calc R . .
C10 C 0.9125(3) 0.2217(3) 0.4592(2) 0.0395(10) Uani 1 1 d . . .
H10 H 0.9158 0.2548 0.5073 0.047 Uiso 1 1 calc R . .
N10 N 1.0209(3) 0.4010(2) 0.1487(2) 0.0498(9) Uani 1 1 d . . .
C15 C 0.5811(3) 0.4106(3) 0.3616(2) 0.0360(9) Uani 1 1 d . . .
C4 C 0.6577(3) 0.4192(2) 0.31504(19) 0.0326(9) Uani 1 1 d . . .
H4 H 0.6528 0.4532 0.2673 0.039 Uiso 1 1 calc R . .
C6 C 0.8305(2) 0.1639(2) 0.35154(19) 0.0316(9) Uani 1 1 d . . .
C2 C 0.5873(2) 0.1791(2) 0.3061(2) 0.0320(9) Uani 1 1 d . . .
C11 C 0.5204(3) 0.1554(3) 0.3544(2) 0.0404(10) Uani 1 1 d . . .
H11 H 0.5347 0.1421 0.4082 0.048 Uiso 1 1 calc R . .
C23 C 0.7946(3) 0.3743(3) 0.2103(2) 0.0400(10) Uani 1 1 d . . .
H23 H 0.7374 0.3629 0.1854 0.048 Uiso 1 1 calc R . .
N5 N 0.6682(3) 0.1943(3) 0.52569(18) 0.0498(9) Uani 1 1 d . . .
C13 C 0.8672(3) 0.3788(3) 0.1666(2) 0.0454(10) Uani 1 1 d . . .
H13 H 0.8598 0.3715 0.1115 0.054 Uiso 1 1 calc R . .
C18 C 0.9045(3) 0.1269(3) 0.3221(2) 0.0407(10) Uani 1 1 d . . .
H18 H 0.9002 0.0939 0.2739 0.049 Uiso 1 1 calc R . .
C9 C 0.9498(3) 0.3935(3) 0.2021(2) 0.0375(9) Uani 1 1 d . . .
C17 C 0.0336(3) 0.1151(3) 0.0773(2) 0.0419(10) Uani 1 1 d . . .
H17 H -0.0265 0.1040 0.0593 0.050 Uiso 1 1 calc R . .
C7 C 0.9611(3) 0.4046(3) 0.2831(2) 0.0388(9) Uani 1 1 d . . .
H7 H 1.0187 0.4149 0.3077 0.047 Uiso 1 1 calc R . .
N8 N 0.3175(2) 0.1613(2) 0.22187(19) 0.0451(9) Uani 1 1 d . . .
C38 C 0.4314(3) 0.4433(4) 0.3877(4) 0.0713(15) Uani 1 1 d . . .
H38 H 0.3756 0.4719 0.3739 0.086 Uiso 1 1 calc R . .
C32 C 0.5008(3) 0.4519(3) 0.3398(3) 0.0525(11) Uani 1 1 d . . .
H32 H 0.4931 0.4861 0.2923 0.063 Uiso 1 1 calc R . .
C16 C 0.4786(3) 0.1950(3) 0.1977(2) 0.0425(10) Uani 1 1 d . . .
H16 H 0.4641 0.2092 0.1441 0.051 Uiso 1 1 calc R . .
C5 C 0.7406(2) 0.1516(2) 0.31210(19) 0.0315(9) Uani 1 1 d . . .
H5 H 0.7327 0.1172 0.2647 0.038 Uiso 1 1 calc R . .
C14 C 0.5667(3) 0.1998(3) 0.2280(2) 0.0371(9) Uani 1 1 d . . .
H14 H 0.6122 0.2171 0.1953 0.044 Uiso 1 1 calc R . .
C20 C 0.9894(3) 0.1852(3) 0.4334(2) 0.0463(11) Uani 1 1 d . . .
H20 H 1.0442 0.1926 0.4636 0.056 Uiso 1 1 calc R . .
C22 C 0.4328(3) 0.1513(3) 0.3236(2) 0.0445(10) Uani 1 1 d . . .
H22 H 0.3871 0.1357 0.3566 0.053 Uiso 1 1 calc R . .
C27 C 0.1004(3) 0.0963(3) 0.0297(2) 0.0469(11) Uani 1 1 d . . .
H27 H 0.0863 0.0732 -0.0216 0.056 Uiso 1 1 calc R . .
C24 C 0.9863(3) 0.1382(3) 0.3636(2) 0.0463(10) Uani 1 1 d . . .
H24 H 1.0389 0.1139 0.3440 0.056 Uiso 1 1 calc R . .
C21 C 0.2083(3) 0.1419(3) 0.1300(2) 0.0396(10) Uani 1 1 d . . .
C35 C 1.3242(3) 0.4038(3) 0.1293(3) 0.0494(11) Uani 1 1 d . . .
H35 H 1.3812 0.3898 0.1534 0.059 Uiso 1 1 calc R . .
C28 C 0.0534(3) 0.1500(3) 0.1514(2) 0.0468(11) Uani 1 1 d . . .
H28 H 0.0071 0.1645 0.1841 0.056 Uiso 1 1 calc R . .
C36 C 1.2336(3) 0.4587(3) 0.0183(3) 0.0561(12) Uani 1 1 d . . .
H36 H 1.2280 0.4827 -0.0335 0.067 Uiso 1 1 calc R . .
C26 C 0.5257(3) 0.3519(3) 0.4733(3) 0.0528(12) Uani 1 1 d . . .
H26 H 0.5344 0.3168 0.5203 0.063 Uiso 1 1 calc R . .
C19 C 0.4118(3) 0.1697(3) 0.2453(2) 0.0386(9) Uani 1 1 d . . .
N6 N 0.3032(2) 0.1510(2) 0.15127(19) 0.0446(9) Uani 1 1 d . . .
C31 C 0.4449(4) 0.3922(4) 0.4561(3) 0.0673(14) Uani 1 1 d . . .
H31 H 0.3986 0.3853 0.4904 0.081 Uiso 1 1 calc R . .
C33 C 1.3165(3) 0.4380(3) 0.0538(3) 0.0554(12) Uani 1 1 d . . .
H33 H 1.3682 0.4473 0.0263 0.066 Uiso 1 1 calc R . .
C34 C 1.2497(3) 0.3896(3) 0.1701(3) 0.0496(11) Uani 1 1 d . . .
H34 H 1.2552 0.3661 0.2220 0.060 Uiso 1 1 calc R . .
C30 C 0.1875(3) 0.1105(3) 0.0555(2) 0.0463(10) Uani 1 1 d . . .
H30 H 0.2334 0.0985 0.0217 0.056 Uiso 1 1 calc R . .
C25 C 0.1418(3) 0.1639(3) 0.1780(2) 0.0481(11) Uani 1 1 d . . .
H25 H 0.1563 0.1883 0.2288 0.058 Uiso 1 1 calc R . .
C37 C 1.1584(3) 0.4441(3) 0.0593(3) 0.0537(12) Uani 1 1 d . . .
H37 H 1.1009 0.4574 0.0357 0.064 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
Zn01 N7 2.037(3) . ?
Zn01 N5 2.038(3) . ?
Zn01 N1 2.119(3) . ?
Zn01 N4 2.150(3) . ?
Zn01 N3 2.304(3) . ?
Zn01 N2 2.342(3) . ?
S1 C3 1.627(4) . ?
S2 C12 1.618(4) . ?
N9 N10 1.219(5) . ?
N9 C29 1.490(5) . ?
N7 C3 1.163(5) . ?
N2 C4 1.279(4) . ?
N2 C1 1.420(4) . ?
C29 C34 1.358(6) . ?
C29 C37 1.383(6) . ?
N3 C5 1.267(5) . ?
N3 C2 1.421(4) . ?
N1 C10 1.341(5) . ?
N1 C6 1.359(4) . ?
C1 C8 1.388(5) . ?
C1 C23 1.393(5) . ?
N4 C26 1.328(5) . ?
N4 C15 1.355(5) . ?
C12 N5 1.154(5) . ?
C8 C7 1.374(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.376(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.464(5) . ?
C15 C32 1.375(6) . ?
C15 C4 1.458(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.366(6) . ?
C6 C5 1.481(5) . ?
C2 C14 1.384(5) . ?
C2 C11 1.394(5) . ?
C11 C22 1.390(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.372(6) . ?
C23 H23 0.9500 . ?
C13 C9 1.364(6) . ?
C13 H13 0.9500 . ?
C18 C24 1.389(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.398(5) . ?
C17 C27 1.370(6) . ?
C17 C28 1.378(6) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.223(4) . ?
N8 C19 1.456(5) . ?
C38 C32 1.382(7) . ?
C38 C31 1.385(8) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.391(6) . ?
C16 C14 1.394(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.371(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.383(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.372(6) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.369(6) . ?
C21 C25 1.379(6) . ?
C21 N6 1.458(5) . ?
C35 C33 1.380(6) . ?
C35 C34 1.381(6) . ?
C35 H35 0.9500 . ?
C28 C25 1.394(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.385(7) . ?
C36 C37 1.395(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.362(7) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N5 97.27(13) . . ?
N7 Zn01 N1 95.43(12) . . ?
N5 Zn01 N1 100.65(14) . . ?
N7 Zn01 N4 97.69(13) . . ?
N5 Zn01 N4 93.98(14) . . ?
N1 Zn01 N4 158.93(11) . . ?
N7 Zn01 N3 166.71(12) . . ?
N5 Zn01 N3 92.95(12) . . ?
N1 Zn01 N3 74.26(11) . . ?
N4 Zn01 N3 90.03(11) . . ?
N7 Zn01 N2 94.50(11) . . ?
N5 Zn01 N2 164.07(12) . . ?
N1 Zn01 N2 88.84(11) . . ?
N4 Zn01 N2 73.78(11) . . ?
N3 Zn01 N2 77.21(9) . . ?
N10 N9 C29 112.9(3) . . ?
C3 N7 Zn01 161.0(3) . . ?
C4 N2 C1 119.6(3) . . ?
C4 N2 Zn01 111.5(2) . . ?
C1 N2 Zn01 127.7(2) . . ?
C34 C29 C37 121.8(4) . . ?
C34 C29 N9 114.7(4) . . ?
C37 C29 N9 123.5(4) . . ?
C5 N3 C2 121.1(3) . . ?
C5 N3 Zn01 112.5(2) . . ?
C2 N3 Zn01 125.6(2) . . ?
C10 N1 C6 117.0(3) . . ?
C10 N1 Zn01 125.0(3) . . ?
C6 N1 Zn01 117.5(2) . . ?
C8 C1 C23 119.6(3) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.9(3) . . ?
N7 C3 S1 179.2(4) . . ?
C26 N4 C15 118.3(4) . . ?
C26 N4 Zn01 124.3(3) . . ?
C15 N4 Zn01 117.2(3) . . ?
N5 C12 S2 179.7(4) . . ?
C7 C8 C1 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
N1 C10 C20 123.1(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
N9 N10 C9 110.2(3) . . ?
N4 C15 C32 121.4(4) . . ?
N4 C15 C4 116.3(3) . . ?
C32 C15 C4 122.2(4) . . ?
N2 C4 C15 120.0(3) . . ?
N2 C4 H4 120.0 . . ?
C15 C4 H4 120.0 . . ?
N1 C6 C18 122.9(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.1(3) . . ?
C14 C2 C11 120.4(3) . . ?
C14 C2 N3 122.8(3) . . ?
C11 C2 N3 116.6(3) . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
C13 C23 C1 120.1(3) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C12 N5 Zn01 164.1(3) . . ?
C9 C13 C23 120.3(3) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C6 C18 C24 119.1(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.2(3) . . ?
C13 C9 N10 114.9(3) . . ?
C7 C9 N10 124.8(4) . . ?
C27 C17 C28 120.1(4) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C8 C7 C9 119.9(3) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
N6 N8 C19 112.5(3) . . ?
C32 C38 C31 118.6(5) . . ?
C32 C38 H38 120.7 . . ?
C31 C38 H38 120.7 . . ?
C15 C32 C38 119.4(5) . . ?
C15 C32 H32 120.3 . . ?
C38 C32 H32 120.3 . . ?
C19 C16 C14 120.4(3) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N3 C5 C6 119.1(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C2 C14 C16 119.5(4) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
C24 C20 C10 119.3(4) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C19 C22 C11 120.4(4) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C17 C27 C30 120.6(4) . . ?
C17 C27 H27 119.7 . . ?
C30 C27 H27 119.7 . . ?
C20 C24 C18 118.6(4) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C30 C21 C25 120.3(4) . . ?
C30 C21 N6 114.7(4) . . ?
C25 C21 N6 125.0(4) . . ?
C33 C35 C34 120.7(4) . . ?
C33 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C17 C28 C25 119.5(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C33 C36 C37 119.2(4) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
N4 C26 C31 123.4(5) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C22 C19 C16 119.7(3) . . ?
C22 C19 N8 113.8(4) . . ?
C16 C19 N8 126.5(3) . . ?
N8 N6 C21 111.0(3) . . ?
C26 C31 C38 118.7(5) . . ?
C26 C31 H31 120.6 . . ?
C38 C31 H31 120.6 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 119.0(4) . . ?
C29 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C21 C30 C27 119.9(4) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C21 C25 C28 119.6(4) . . ?
C21 C25 H25 120.2 . . ?
C28 C25 H25 120.2 . . ?
C29 C37 C36 119.2(4) . . ?
C29 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.741
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.741
_refine_diff_density_max         1.401
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_znaza140km
_database_code_depnum_ccdc_archive 'CCDC 1492668'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0940(6)
_cell_length_b                   14.2636(9)
_cell_length_c                   17.1499(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.206(3)
_cell_angle_gamma                90.00
_cell_volume                     3682.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    14429
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6381
_exptl_absorpt_correction_T_max  0.7084
_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      140(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            6207
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4805
_reflns_number_gt                4326
_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)+(0.0386P)²+6.9838P] 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         4805
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.1083
_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
Zn01 Zn 0.71706(3) 0.28363(3) 0.44629(2) 0.02872(15) Uani 1 1 d . . .
S1 S 0.80759(6) 0.50135(7) 0.64744(5) 0.0345(2) Uani 1 1 d . . .
S2 S 0.56240(7) 0.07271(8) 0.60362(5) 0.0412(3) Uani 1 1 d . . .
N9 N 1.0939(2) 0.3955(2) 0.18480(18) 0.0385(8) Uani 1 1 d . . .
N7 N 0.7793(2) 0.3738(2) 0.52455(17) 0.0386(8) Uani 1 1 d . . .
N2 N 0.73146(19) 0.38116(19) 0.33856(15) 0.0249(7) Uani 1 1 d . . .
C29 C 1.1681(3) 0.4098(3) 0.1352(2) 0.0381(10) Uani 1 1 d . . .
N3 N 0.6752(2) 0.18757(19) 0.34220(15) 0.0260(7) Uani 1 1 d . . .
N1 N 0.8343(2) 0.2128(2) 0.41871(15) 0.0292(7) Uani 1 1 d . . .
C1 C 0.8045(2) 0.3865(2) 0.29078(18) 0.0249(8) Uani 1 1 d . . .
C3 C 0.7906(2) 0.4265(3) 0.57595(19) 0.0292(8) Uani 1 1 d . . .
N4 N 0.5938(2) 0.3588(2) 0.42836(16) 0.0334(7) Uani 1 1 d . . .
C12 C 0.6249(2) 0.1433(3) 0.55789(18) 0.0297(8) Uani 1 1 d . . .
C8 C 0.8887(2) 0.4008(2) 0.32675(19) 0.0291(8) Uani 1 1 d . . .
H8 H 0.8964 0.4078 0.3819 0.035 Uiso 1 1 calc R . .
C10 C 0.9135(3) 0.2215(3) 0.4588(2) 0.0356(9) Uani 1 1 d . . .
H10 H 0.9166 0.2541 0.5072 0.043 Uiso 1 1 calc R . .
N10 N 1.0203(2) 0.4008(2) 0.14877(19) 0.0420(8) Uani 1 1 d . . .
C15 C 0.5812(3) 0.4102(3) 0.3622(2) 0.0321(9) Uani 1 1 d . . .
C4 C 0.6576(2) 0.4191(2) 0.31512(19) 0.0289(8) Uani 1 1 d . . .
H4 H 0.6523 0.4529 0.2673 0.035 Uiso 1 1 calc R . .
C6 C 0.8314(2) 0.1639(2) 0.35092(18) 0.0277(8) Uani 1 1 d . . .
C2 C 0.5880(2) 0.1787(2) 0.30619(19) 0.0286(8) Uani 1 1 d . . .
C11 C 0.5210(3) 0.1552(3) 0.3546(2) 0.0358(9) Uani 1 1 d . . .
H11 H 0.5352 0.1421 0.4084 0.043 Uiso 1 1 calc R . .
C23 C 0.7938(3) 0.3737(3) 0.21014(19) 0.0344(9) Uani 1 1 d . . .
H23 H 0.7365 0.3620 0.1855 0.041 Uiso 1 1 calc R . .
N5 N 0.6696(2) 0.1936(2) 0.52548(17) 0.0436(9) Uani 1 1 d . . .
C13 C 0.8666(3) 0.3783(3) 0.1661(2) 0.0384(10) Uani 1 1 d . . .
H13 H 0.8592 0.3708 0.1110 0.046 Uiso 1 1 calc R . .
C18 C 0.9055(3) 0.1269(3) 0.3210(2) 0.0348(9) Uani 1 1 d . . .
H18 H 0.9011 0.0943 0.2726 0.042 Uiso 1 1 calc R . .
C9 C 0.9495(3) 0.3934(3) 0.2015(2) 0.0329(9) Uani 1 1 d . . .
C17 C 0.0333(3) 0.1153(3) 0.0773(2) 0.0362(9) Uani 1 1 d . . .
H17 H -0.0270 0.1044 0.0597 0.043 Uiso 1 1 calc R . .
C7 C 0.9610(3) 0.4050(3) 0.2826(2) 0.0336(9) Uani 1 1 d . . .
H7 H 1.0186 0.4157 0.3070 0.040 Uiso 1 1 calc R . .
N8 N 0.3186(2) 0.1611(2) 0.22173(18) 0.0391(8) Uani 1 1 d . . .
C38 C 0.4315(3) 0.4426(4) 0.3885(3) 0.0612(13) Uani 1 1 d . . .
H38 H 0.3755 0.4709 0.3748 0.073 Uiso 1 1 calc R . .
C32 C 0.5007(3) 0.4515(3) 0.3403(3) 0.0463(11) Uani 1 1 d . . .
H32 H 0.4927 0.4857 0.2927 0.056 Uiso 1 1 calc R . .
C16 C 0.4791(3) 0.1949(3) 0.1976(2) 0.0360(9) Uani 1 1 d . . .
H16 H 0.4645 0.2089 0.1441 0.043 Uiso 1 1 calc R . .
C5 C 0.7414(2) 0.1516(2) 0.31148(19) 0.0283(8) Uani 1 1 d . . .
H5 H 0.7333 0.1174 0.2640 0.034 Uiso 1 1 calc R . .
C14 C 0.5668(3) 0.1997(3) 0.2278(2) 0.0323(9) Uani 1 1 d . . .
H14 H 0.6122 0.2173 0.1951 0.039 Uiso 1 1 calc R . .
C20 C 0.9907(3) 0.1851(3) 0.4326(2) 0.0411(10) Uani 1 1 d . . .
H20 H 1.0456 0.1926 0.4627 0.049 Uiso 1 1 calc R . .
C22 C 0.4335(3) 0.1510(3) 0.3238(2) 0.0387(10) Uani 1 1 d . . .
H22 H 0.3878 0.1354 0.3568 0.046 Uiso 1 1 calc R . .
C27 C 0.0998(3) 0.0961(3) 0.0292(2) 0.0410(10) Uani 1 1 d . . .
H27 H 0.0853 0.0729 -0.0221 0.049 Uiso 1 1 calc R . .
C24 C 0.9873(3) 0.1381(3) 0.3628(2) 0.0412(10) Uani 1 1 d . . .
H24 H 1.0399 0.1136 0.3434 0.049 Uiso 1 1 calc R . .
C21 C 0.2089(3) 0.1422(3) 0.1294(2) 0.0348(9) Uani 1 1 d . . .
C35 C 1.3243(3) 0.4036(3) 0.1294(2) 0.0451(10) Uani 1 1 d . . .
H35 H 1.3815 0.3894 0.1535 0.054 Uiso 1 1 calc R . .
C28 C 0.0543(3) 0.1505(3) 0.1514(2) 0.0412(10) Uani 1 1 d . . .
H28 H 0.0084 0.1652 0.1844 0.049 Uiso 1 1 calc R . .
C36 C 1.2333(3) 0.4589(3) 0.0188(3) 0.0485(11) Uani 1 1 d . . .
H36 H 1.2275 0.4833 -0.0329 0.058 Uiso 1 1 calc R . .
C26 C 0.5265(3) 0.3512(3) 0.4742(2) 0.0459(11) Uani 1 1 d . . .
H26 H 0.5354 0.3159 0.5211 0.055 Uiso 1 1 calc R . .
C19 C 0.4123(2) 0.1695(3) 0.2456(2) 0.0327(9) Uani 1 1 d . . .
N6 N 0.3034(2) 0.1510(2) 0.15066(17) 0.0380(8) Uani 1 1 d . . .
C31 C 0.4453(3) 0.3917(4) 0.4570(3) 0.0586(13) Uani 1 1 d . . .
H31 H 0.3992 0.3850 0.4915 0.070 Uiso 1 1 calc R . .
C33 C 1.3167(3) 0.4378(3) 0.0540(3) 0.0482(11) Uani 1 1 d . . .
H33 H 1.3683 0.4469 0.0263 0.058 Uiso 1 1 calc R . .
C34 C 1.2501(3) 0.3895(3) 0.1706(2) 0.0429(10) Uani 1 1 d . . .
H34 H 1.2558 0.3660 0.2226 0.051 Uiso 1 1 calc R . .
C30 C 0.1875(3) 0.1103(3) 0.0547(2) 0.0400(10) Uani 1 1 d . . .
H30 H 0.2331 0.0980 0.0207 0.048 Uiso 1 1 calc R . .
C25 C 0.1424(3) 0.1644(3) 0.1777(2) 0.0418(10) Uani 1 1 d . . .
H25 H 0.1570 0.1889 0.2285 0.050 Uiso 1 1 calc R . .
C37 C 1.1584(3) 0.4443(3) 0.0597(2) 0.0452(11) Uani 1 1 d . . .
H37 H 1.1010 0.4577 0.0359 0.054 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
Zn01 N5 2.037(3) . ?
Zn01 N7 2.037(3) . ?
Zn01 N1 2.121(3) . ?
Zn01 N4 2.150(3) . ?
Zn01 N3 2.302(3) . ?
Zn01 N2 2.336(3) . ?
S1 C3 1.632(4) . ?
S2 C12 1.621(4) . ?
N9 N10 1.232(4) . ?
N9 C29 1.471(5) . ?
N7 C3 1.162(5) . ?
N2 C4 1.278(4) . ?
N2 C1 1.423(4) . ?
C29 C34 1.368(6) . ?
C29 C37 1.383(6) . ?
N3 C5 1.271(5) . ?
N3 C2 1.418(4) . ?
N1 C10 1.340(4) . ?
N1 C6 1.354(4) . ?
C1 C8 1.386(5) . ?
C1 C23 1.392(4) . ?
N4 C26 1.334(5) . ?
N4 C15 1.353(5) . ?
C12 N5 1.155(5) . ?
C8 C7 1.375(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.380(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.454(5) . ?
C15 C32 1.378(6) . ?
C15 C4 1.461(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.369(5) . ?
C6 C5 1.484(5) . ?
C2 C14 1.391(5) . ?
C2 C11 1.396(5) . ?
C11 C22 1.387(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.380(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.366(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.391(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.398(5) . ?
C17 C27 1.373(6) . ?
C17 C28 1.382(5) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.232(4) . ?
N8 C19 1.448(5) . ?
C38 C31 1.385(7) . ?
C38 C32 1.385(7) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C14 1.388(5) . ?
C16 C19 1.395(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.369(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.382(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.378(5) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.376(5) . ?
C21 C25 1.384(6) . ?
C21 N6 1.452(5) . ?
C35 C33 1.380(6) . ?
C35 C34 1.383(6) . ?
C35 H35 0.9500 . ?
C28 C25 1.386(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.388(6) . ?
C36 C37 1.389(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.367(7) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.25(13) . . ?
N5 Zn01 N1 100.87(13) . . ?
N7 Zn01 N1 95.49(12) . . ?
N5 Zn01 N4 93.81(13) . . ?
N7 Zn01 N4 97.58(12) . . ?
N1 Zn01 N4 158.92(10) . . ?
N5 Zn01 N3 92.98(11) . . ?
N7 Zn01 N3 166.80(12) . . ?
N1 Zn01 N3 74.31(10) . . ?
N4 Zn01 N3 90.02(11) . . ?
N5 Zn01 N2 163.85(12) . . ?
N7 Zn01 N2 94.59(11) . . ?
N1 Zn01 N2 88.84(10) . . ?
N4 Zn01 N2 73.71(11) . . ?
N3 Zn01 N2 77.13(9) . . ?
N10 N9 C29 113.5(3) . . ?
C3 N7 Zn01 160.6(3) . . ?
C4 N2 C1 119.4(3) . . ?
C4 N2 Zn01 111.8(2) . . ?
C1 N2 Zn01 127.5(2) . . ?
C34 C29 C37 121.4(4) . . ?
C34 C29 N9 114.6(3) . . ?
C37 C29 N9 123.9(4) . . ?
C5 N3 C2 121.1(3) . . ?
C5 N3 Zn01 112.5(2) . . ?
C2 N3 Zn01 125.7(2) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Zn01 124.7(2) . . ?
C6 N1 Zn01 117.6(2) . . ?
C8 C1 C23 119.8(3) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.8(3) . . ?
N7 C3 S1 179.2(4) . . ?
C26 N4 C15 118.2(3) . . ?
C26 N4 Zn01 124.3(3) . . ?
C15 N4 Zn01 117.2(2) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 122.8(3) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
N9 N10 C9 111.1(3) . . ?
N4 C15 C32 121.8(4) . . ?
N4 C15 C4 116.3(3) . . ?
C32 C15 C4 121.9(4) . . ?
N2 C4 C15 119.7(3) . . ?
N2 C4 H4 120.1 . . ?
C15 C4 H4 120.1 . . ?
N1 C6 C18 123.0(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.0(3) . . ?
C14 C2 C11 120.1(3) . . ?
C14 C2 N3 122.8(3) . . ?
C11 C2 N3 116.9(3) . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
C13 C23 C1 119.9(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C12 N5 Zn01 163.5(3) . . ?
C9 C13 C23 120.3(3) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C6 C18 C24 118.7(3) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C13 C9 C7 120.2(3) . . ?
C13 C9 N10 115.2(3) . . ?
C7 C9 N10 124.5(3) . . ?
C27 C17 C28 119.8(4) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C8 C7 C9 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
N6 N8 C19 113.3(3) . . ?
C31 C38 C32 118.8(4) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?
C15 C32 C38 119.1(4) . . ?
C15 C32 H32 120.4 . . ?
C38 C32 H32 120.4 . . ?
C14 C16 C19 120.3(3) . . ?
C14 C16 H16 119.8 . . ?
C19 C16 H16 119.8 . . ?
N3 C5 C6 119.0(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C16 C14 C2 119.7(3) . . ?
C16 C14 H14 120.2 . . ?
C2 C14 H14 120.2 . . ?
C24 C20 C10 119.4(3) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C19 C22 C11 120.6(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C17 C27 C30 120.5(4) . . ?
C17 C27 H27 119.7 . . ?
C30 C27 H27 119.7 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.2(3) . . ?
C30 C21 N6 114.9(4) . . ?
C25 C21 N6 124.9(3) . . ?
C33 C35 C34 121.0(4) . . ?
C33 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C17 C28 C25 120.1(4) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C33 C36 C37 119.6(4) . . ?
C33 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
N4 C26 C31 123.3(4) . . ?
N4 C26 H26 118.4 . . ?
C31 C26 H26 118.4 . . ?
C22 C19 C16 119.7(3) . . ?
C22 C19 N8 114.2(3) . . ?
C16 C19 N8 126.1(3) . . ?
N8 N6 C21 111.5(3) . . ?
C26 C31 C38 118.8(4) . . ?
C26 C31 H31 120.6 . . ?
C38 C31 H31 120.6 . . ?
C35 C33 C36 119.7(4) . . ?
C35 C33 H33 120.2 . . ?
C36 C33 H33 120.2 . . ?
C29 C34 C35 118.9(4) . . ?
C29 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C21 C30 C27 119.9(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C21 C25 C28 119.5(4) . . ?
C21 C25 H25 120.2 . . ?
C28 C25 H25 120.2 . . ?
C29 C37 C36 119.4(4) . . ?
C29 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?

_diffrn_measured_fraction_theta_max 0.739
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.739
_refine_diff_density_max         1.563
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_znaza150kd
_database_code_depnum_ccdc_archive 'CCDC 1492669'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0958(6)
_cell_length_b                   14.2842(9)
_cell_length_c                   17.1476(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.159(3)
_cell_angle_gamma                90.00
_cell_volume                     3687.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14582
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6385
_exptl_absorpt_correction_T_max  0.7088
_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            6255
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.04
_reflns_number_total             4823
_reflns_number_gt                4326
_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)+(0.0543P)²+5.6594P] 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         4823
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1212
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
Zn01 Zn 0.71646(3) 0.28382(3) 0.44640(2) 0.03042(16) Uani 1 1 d . . .
S1 S 0.80765(6) 0.50112(7) 0.64747(5) 0.0367(3) Uani 1 1 d . . .
S2 S 0.56248(7) 0.07252(8) 0.60382(5) 0.0437(3) Uani 1 1 d . . .
N9 N 1.0933(2) 0.3952(2) 0.18509(18) 0.0409(8) Uani 1 1 d . . .
N7 N 0.7785(2) 0.3741(2) 0.52453(17) 0.0408(8) Uani 1 1 d . . .
N2 N 0.73149(19) 0.38114(19) 0.33845(15) 0.0261(7) Uani 1 1 d . . .
C29 C 1.1683(3) 0.4097(3) 0.1351(2) 0.0410(10) Uani 1 1 d . . .
N3 N 0.6749(2) 0.1877(2) 0.34234(15) 0.0276(7) Uani 1 1 d . . .
N1 N 0.8337(2) 0.2129(2) 0.41925(16) 0.0304(7) Uani 1 1 d . . .
C1 C 0.8045(2) 0.3866(2) 0.29079(18) 0.0264(8) Uani 1 1 d . . .
C3 C 0.7901(2) 0.4265(3) 0.57603(19) 0.0305(9) Uani 1 1 d . . .
N4 N 0.5933(2) 0.3590(2) 0.42817(17) 0.0350(7) Uani 1 1 d . . .
C12 C 0.6246(2) 0.1435(3) 0.55823(18) 0.0319(9) Uani 1 1 d . . .
C8 C 0.8887(2) 0.4007(2) 0.32688(19) 0.0305(8) Uani 1 1 d . . .
H8 H 0.8963 0.4074 0.3821 0.037 Uiso 1 1 calc R . .
C10 C 0.9131(3) 0.2217(3) 0.4590(2) 0.0371(10) Uani 1 1 d . . .
H10 H 0.9164 0.2547 0.5072 0.045 Uiso 1 1 calc R . .
N10 N 1.0207(2) 0.4008(2) 0.1486(2) 0.0464(9) Uani 1 1 d . . .
C15 C 0.5811(3) 0.4104(3) 0.3620(2) 0.0334(9) Uani 1 1 d . . .
C4 C 0.6578(2) 0.4192(2) 0.31519(19) 0.0309(9) Uani 1 1 d . . .
H4 H 0.6528 0.4532 0.2675 0.037 Uiso 1 1 calc R . .
C6 C 0.8311(2) 0.1641(2) 0.35125(19) 0.0296(8) Uani 1 1 d . . .
C2 C 0.5877(2) 0.1791(2) 0.30626(19) 0.0296(8) Uani 1 1 d . . .
C11 C 0.5208(3) 0.1553(3) 0.3545(2) 0.0374(9) Uani 1 1 d . . .
H11 H 0.5350 0.1418 0.4082 0.045 Uiso 1 1 calc R . .
C23 C 0.7943(3) 0.3737(3) 0.21002(19) 0.0369(9) Uani 1 1 d . . .
H23 H 0.7371 0.3617 0.1852 0.044 Uiso 1 1 calc R . .
N5 N 0.6686(2) 0.1941(3) 0.52569(18) 0.0458(9) Uani 1 1 d . . .
C13 C 0.8671(3) 0.3784(3) 0.1664(2) 0.0411(10) Uani 1 1 d . . .
H13 H 0.8598 0.3710 0.1113 0.049 Uiso 1 1 calc R . .
C18 C 0.9048(3) 0.1269(3) 0.3217(2) 0.0376(9) Uani 1 1 d . . .
H18 H 0.9002 0.0939 0.2735 0.045 Uiso 1 1 calc R . .
C9 C 0.9497(3) 0.3934(3) 0.2017(2) 0.0347(9) Uani 1 1 d . . .
C17 C 0.0334(3) 0.1153(3) 0.0776(2) 0.0398(10) Uani 1 1 d . . .
H17 H -0.0268 0.1040 0.0601 0.048 Uiso 1 1 calc R . .
C7 C 0.9611(3) 0.4048(3) 0.2828(2) 0.0366(9) Uani 1 1 d . . .
H7 H 1.0187 0.4154 0.3073 0.044 Uiso 1 1 calc R . .
N8 N 0.3179(2) 0.1612(2) 0.22193(18) 0.0414(8) Uani 1 1 d . . .
C38 C 0.4319(3) 0.4430(4) 0.3880(3) 0.0664(14) Uani 1 1 d . . .
H38 H 0.3761 0.4714 0.3743 0.080 Uiso 1 1 calc R . .
C32 C 0.5009(3) 0.4518(3) 0.3398(3) 0.0482(11) Uani 1 1 d . . .
H32 H 0.4932 0.4859 0.2922 0.058 Uiso 1 1 calc R . .
C16 C 0.4787(3) 0.1950(3) 0.1976(2) 0.0389(10) Uani 1 1 d . . .
H16 H 0.4641 0.2092 0.1441 0.047 Uiso 1 1 calc R . .
C5 C 0.7410(2) 0.1518(2) 0.31186(18) 0.0293(8) Uani 1 1 d . . .
H5 H 0.7329 0.1175 0.2644 0.035 Uiso 1 1 calc R . .
C14 C 0.5667(3) 0.1998(3) 0.2278(2) 0.0350(9) Uani 1 1 d . . .
H14 H 0.6121 0.2171 0.1951 0.042 Uiso 1 1 calc R . .
C20 C 0.9898(3) 0.1854(3) 0.4333(2) 0.0437(11) Uani 1 1 d . . .
H20 H 1.0446 0.1929 0.4636 0.052 Uiso 1 1 calc R . .
C22 C 0.4333(3) 0.1513(3) 0.3238(2) 0.0413(10) Uani 1 1 d . . .
H22 H 0.3875 0.1360 0.3569 0.050 Uiso 1 1 calc R . .
C27 C 0.0999(3) 0.0964(3) 0.0296(2) 0.0437(10) Uani 1 1 d . . .
H27 H 0.0853 0.0734 -0.0217 0.052 Uiso 1 1 calc R . .
C24 C 0.9869(3) 0.1379(3) 0.3631(2) 0.0446(10) Uani 1 1 d . . .
H24 H 1.0395 0.1133 0.3436 0.053 Uiso 1 1 calc R . .
C21 C 0.2087(3) 0.1418(3) 0.1296(2) 0.0374(9) Uani 1 1 d . . .
C35 C 1.3241(3) 0.4036(3) 0.1292(3) 0.0477(11) Uani 1 1 d . . .
H35 H 1.3813 0.3895 0.1531 0.057 Uiso 1 1 calc R . .
C28 C 0.0541(3) 0.1506(3) 0.1513(2) 0.0435(10) Uani 1 1 d . . .
H28 H 0.0080 0.1657 0.1841 0.052 Uiso 1 1 calc R . .
C36 C 1.2334(3) 0.4586(3) 0.0185(3) 0.0518(11) Uani 1 1 d . . .
H36 H 1.2278 0.4825 -0.0333 0.062 Uiso 1 1 calc R . .
C26 C 0.5257(3) 0.3516(3) 0.4737(3) 0.0492(11) Uani 1 1 d . . .
H26 H 0.5343 0.3161 0.5205 0.059 Uiso 1 1 calc R . .
C19 C 0.4121(3) 0.1695(3) 0.2454(2) 0.0358(9) Uani 1 1 d . . .
N6 N 0.3034(2) 0.1511(2) 0.15084(18) 0.0402(8) Uani 1 1 d . . .
C31 C 0.4452(3) 0.3920(4) 0.4568(3) 0.0618(13) Uani 1 1 d . . .
H31 H 0.3991 0.3856 0.4913 0.074 Uiso 1 1 calc R . .
C33 C 1.3165(3) 0.4379(3) 0.0539(3) 0.0510(11) Uani 1 1 d . . .
H33 H 1.3681 0.4473 0.0264 0.061 Uiso 1 1 calc R . .
C34 C 1.2501(3) 0.3896(3) 0.1703(3) 0.0461(10) Uani 1 1 d . . .
H34 H 1.2559 0.3663 0.2224 0.055 Uiso 1 1 calc R . .
C30 C 0.1876(3) 0.1104(3) 0.0549(2) 0.0426(10) Uani 1 1 d . . .
H30 H 0.2332 0.0984 0.0209 0.051 Uiso 1 1 calc R . .
C25 C 0.1419(3) 0.1642(3) 0.1777(2) 0.0443(10) Uani 1 1 d . . .
H25 H 0.1563 0.1887 0.2285 0.053 Uiso 1 1 calc R . .
C37 C 1.1582(3) 0.4440(3) 0.0594(3) 0.0493(11) Uani 1 1 d . . .
H37 H 1.1008 0.4575 0.0357 0.059 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
Zn01 N7 2.038(3) . ?
Zn01 N5 2.039(3) . ?
Zn01 N1 2.120(3) . ?
Zn01 N4 2.151(3) . ?
Zn01 N3 2.302(3) . ?
Zn01 N2 2.339(3) . ?
S1 C3 1.631(4) . ?
S2 C12 1.621(4) . ?
N9 N10 1.225(4) . ?
N9 C29 1.484(5) . ?
N7 C3 1.160(5) . ?
N2 C4 1.276(4) . ?
N2 C1 1.421(4) . ?
C29 C34 1.365(6) . ?
C29 C37 1.385(6) . ?
N3 C5 1.268(5) . ?
N3 C2 1.418(4) . ?
N1 C10 1.342(4) . ?
N1 C6 1.356(4) . ?
C1 C8 1.387(5) . ?
C1 C23 1.395(5) . ?
N4 C26 1.333(5) . ?
N4 C15 1.352(5) . ?
C12 N5 1.152(5) . ?
C8 C7 1.375(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.370(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.458(5) . ?
C15 C32 1.375(6) . ?
C15 C4 1.462(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.364(5) . ?
C6 C5 1.484(5) . ?
C2 C14 1.391(5) . ?
C2 C11 1.394(5) . ?
C11 C22 1.387(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.375(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.363(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.392(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.398(5) . ?
C17 C27 1.371(6) . ?
C17 C28 1.375(6) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.231(4) . ?
N8 C19 1.455(5) . ?
C38 C32 1.382(7) . ?
C38 C31 1.388(7) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.390(6) . ?
C16 C14 1.392(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.379(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.384(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.378(6) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.372(5) . ?
C21 C25 1.386(6) . ?
C21 N6 1.454(5) . ?
C35 C33 1.377(6) . ?
C35 C34 1.380(6) . ?
C35 H35 0.9500 . ?
C28 C25 1.383(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.385(6) . ?
C36 C37 1.393(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.357(7) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N5 97.33(13) . . ?
N7 Zn01 N1 95.51(12) . . ?
N5 Zn01 N1 100.82(13) . . ?
N7 Zn01 N4 97.50(12) . . ?
N5 Zn01 N4 93.81(13) . . ?
N1 Zn01 N4 158.99(11) . . ?
N7 Zn01 N3 166.75(12) . . ?
N5 Zn01 N3 92.99(12) . . ?
N1 Zn01 N3 74.32(11) . . ?
N4 Zn01 N3 90.05(11) . . ?
N7 Zn01 N2 94.46(11) . . ?
N5 Zn01 N2 163.92(12) . . ?
N1 Zn01 N2 88.85(10) . . ?
N4 Zn01 N2 73.77(11) . . ?
N3 Zn01 N2 77.15(9) . . ?
N10 N9 C29 112.8(3) . . ?
C3 N7 Zn01 160.9(3) . . ?
C4 N2 C1 119.5(3) . . ?
C4 N2 Zn01 111.6(2) . . ?
C1 N2 Zn01 127.7(2) . . ?
C34 C29 C37 121.6(4) . . ?
C34 C29 N9 114.7(4) . . ?
C37 C29 N9 123.7(4) . . ?
C5 N3 C2 121.2(3) . . ?
C5 N3 Zn01 112.5(2) . . ?
C2 N3 Zn01 125.6(2) . . ?
C10 N1 C6 117.0(3) . . ?
C10 N1 Zn01 125.0(2) . . ?
C6 N1 Zn01 117.5(2) . . ?
C8 C1 C23 119.6(3) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 122.0(3) . . ?
N7 C3 S1 179.0(4) . . ?
C26 N4 C15 118.1(4) . . ?
C26 N4 Zn01 124.4(3) . . ?
C15 N4 Zn01 117.2(3) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 123.1(3) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
N9 N10 C9 110.3(3) . . ?
N4 C15 C32 121.9(4) . . ?
N4 C15 C4 116.3(3) . . ?
C32 C15 C4 121.8(4) . . ?
N2 C4 C15 120.0(3) . . ?
N2 C4 H4 120.0 . . ?
C15 C4 H4 120.0 . . ?
N1 C6 C18 123.0(3) . . ?
N1 C6 C5 114.9(3) . . ?
C18 C6 C5 122.1(3) . . ?
C14 C2 C11 120.1(3) . . ?
C14 C2 N3 122.9(3) . . ?
C11 C2 N3 116.9(3) . . ?
C22 C11 C2 119.8(3) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
C13 C23 C1 119.9(3) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C12 N5 Zn01 164.1(3) . . ?
C9 C13 C23 120.5(3) . . ?
C9 C13 H13 119.7 . . ?
C23 C13 H13 119.7 . . ?
C6 C18 C24 119.2(4) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C13 C9 C7 120.1(3) . . ?
C13 C9 N10 115.1(3) . . ?
C7 C9 N10 124.7(3) . . ?
C27 C17 C28 119.8(4) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C8 C7 C9 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
N6 N8 C19 112.6(3) . . ?
C32 C38 C31 119.2(4) . . ?
C32 C38 H38 120.4 . . ?
C31 C38 H38 120.4 . . ?
C15 C32 C38 118.8(4) . . ?
C15 C32 H32 120.6 . . ?
C38 C32 H32 120.6 . . ?
C19 C16 C14 120.3(3) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N3 C5 C6 119.1(3) . . ?
N3 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C2 C14 C16 119.6(4) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C10 C20 C24 119.5(4) . . ?
C10 C20 H20 120.2 . . ?
C24 C20 H20 120.2 . . ?
C19 C22 C11 120.4(4) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C17 C27 C30 120.7(4) . . ?
C17 C27 H27 119.7 . . ?
C30 C27 H27 119.7 . . ?
C20 C24 C18 118.1(4) . . ?
C20 C24 H24 121.0 . . ?
C18 C24 H24 121.0 . . ?
C30 C21 C25 120.0(4) . . ?
C30 C21 N6 114.9(4) . . ?
C25 C21 N6 125.1(3) . . ?
C33 C35 C34 121.0(4) . . ?
C33 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C17 C28 C25 120.1(4) . . ?
C17 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C33 C36 C37 119.5(4) . . ?
C33 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
N4 C26 C31 123.6(5) . . ?
N4 C26 H26 118.2 . . ?
C31 C26 H26 118.2 . . ?
C22 C19 C16 119.7(3) . . ?
C22 C19 N8 113.9(4) . . ?
C16 C19 N8 126.3(3) . . ?
N8 N6 C21 111.1(3) . . ?
C26 C31 C38 118.4(5) . . ?
C26 C31 H31 120.8 . . ?
C38 C31 H31 120.8 . . ?
C35 C33 C36 119.9(4) . . ?
C35 C33 H33 120.1 . . ?
C36 C33 H33 120.1 . . ?
C29 C34 C35 118.9(4) . . ?
C29 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C21 C30 C27 119.7(4) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C28 C25 C21 119.7(4) . . ?
C28 C25 H25 120.2 . . ?
C21 C25 H25 120.2 . . ?
C29 C37 C36 119.1(4) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.740
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.740
_refine_diff_density_max         1.457
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_znaza190kd
_database_code_depnum_ccdc_archive 'CCDC 1492670'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1034(6)
_cell_length_b                   14.3594(10)
_cell_length_c                   17.1456(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.006(4)
_cell_angle_gamma                90.00
_cell_volume                     3709.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    14527
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6400
_exptl_absorpt_correction_T_max  0.7101
_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            6307
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4856
_reflns_number_gt                4213
_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)+(0.0573P)²+5.4488P] 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         4856
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1292
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
Zn01 Zn 0.71433(3) 0.28440(3) 0.44675(2) 0.03838(18) Uani 1 1 d . . .
S1 S 0.80762(7) 0.49970(8) 0.64745(5) 0.0458(3) Uani 1 1 d . . .
S2 S 0.56295(8) 0.07205(9) 0.60439(6) 0.0547(3) Uani 1 1 d . . .
N9 N 1.0914(3) 0.3953(2) 0.1856(2) 0.0562(10) Uani 1 1 d . . .
N7 N 0.7763(2) 0.3743(3) 0.52482(19) 0.0508(9) Uani 1 1 d . . .
N2 N 0.7311(2) 0.3809(2) 0.33831(16) 0.0322(7) Uani 1 1 d . . .
C29 C 1.1690(4) 0.4095(3) 0.1343(3) 0.0583(13) Uani 1 1 d . . .
N3 N 0.6730(2) 0.1882(2) 0.34282(16) 0.0349(7) Uani 1 1 d . . .
N1 N 0.8314(2) 0.2134(2) 0.42028(17) 0.0379(8) Uani 1 1 d . . .
C1 C 0.8047(3) 0.3866(2) 0.2914(2) 0.0333(9) Uani 1 1 d . . .
C3 C 0.7887(2) 0.4261(3) 0.5761(2) 0.0377(9) Uani 1 1 d . . .
N4 N 0.5919(2) 0.3595(2) 0.42716(19) 0.0444(8) Uani 1 1 d . . .
C12 C 0.6228(3) 0.1444(3) 0.5585(2) 0.0394(9) Uani 1 1 d . . .
C8 C 0.8882(3) 0.3997(3) 0.3279(2) 0.0386(9) Uani 1 1 d . . .
H8 H 0.8953 0.4056 0.3832 0.046 Uiso 1 1 calc R . .
C10 C 0.9107(3) 0.2216(3) 0.4601(2) 0.0454(11) Uani 1 1 d . . .
H10 H 0.9138 0.2543 0.5084 0.055 Uiso 1 1 calc R . .
N10 N 1.0221(3) 0.4016(3) 0.1481(2) 0.0645(11) Uani 1 1 d . . .
C15 C 0.5806(3) 0.4109(3) 0.3611(2) 0.0426(10) Uani 1 1 d . . .
C4 C 0.6576(3) 0.4193(3) 0.3151(2) 0.0384(9) Uani 1 1 d . . .
H4 H 0.6532 0.4536 0.2676 0.046 Uiso 1 1 calc R . .
C6 C 0.8290(3) 0.1642(3) 0.3526(2) 0.0365(9) Uani 1 1 d . . .
C2 C 0.5864(3) 0.1796(3) 0.3064(2) 0.0377(9) Uani 1 1 d . . .
C11 C 0.5192(3) 0.1559(3) 0.3538(2) 0.0475(11) Uani 1 1 d . . .
H11 H 0.5328 0.1426 0.4075 0.057 Uiso 1 1 calc R . .
C23 C 0.7952(3) 0.3746(3) 0.2107(2) 0.0458(10) Uani 1 1 d . . .
H23 H 0.7382 0.3630 0.1856 0.055 Uiso 1 1 calc R . .
N5 N 0.6655(3) 0.1956(3) 0.5260(2) 0.0584(10) Uani 1 1 d . . .
C13 C 0.8682(3) 0.3793(3) 0.1675(2) 0.0544(12) Uani 1 1 d . . .
H13 H 0.8613 0.3727 0.1123 0.065 Uiso 1 1 calc R . .
C18 C 0.9031(3) 0.1271(3) 0.3235(2) 0.0477(11) Uani 1 1 d . . .
H18 H 0.8991 0.0939 0.2754 0.057 Uiso 1 1 calc R . .
C9 C 0.9501(3) 0.3935(3) 0.2033(2) 0.0465(11) Uani 1 1 d . . .
C17 C 0.0333(3) 0.1150(3) 0.0773(3) 0.0490(11) Uani 1 1 d . . .
H17 H -0.0265 0.1040 0.0587 0.059 Uiso 1 1 calc R . .
C7 C 0.9613(3) 0.4040(3) 0.2842(2) 0.0464(10) Uani 1 1 d . . .
H7 H 1.0187 0.4141 0.3090 0.056 Uiso 1 1 calc R . .
N8 N 0.3158(3) 0.1612(3) 0.2215(2) 0.0567(10) Uani 1 1 d . . .
C38 C 0.4312(4) 0.4441(4) 0.3864(4) 0.0841(18) Uani 1 1 d . . .
H38 H 0.3757 0.4727 0.3724 0.101 Uiso 1 1 calc R . .
C32 C 0.5011(3) 0.4528(3) 0.3387(3) 0.0616(13) Uani 1 1 d . . .
H32 H 0.4941 0.4871 0.2913 0.074 Uiso 1 1 calc R . .
C16 C 0.4782(3) 0.1951(3) 0.1978(2) 0.0518(12) Uani 1 1 d . . .
H16 H 0.4640 0.2091 0.1442 0.062 Uiso 1 1 calc R . .
C5 C 0.7393(3) 0.1523(3) 0.3131(2) 0.0370(9) Uani 1 1 d . . .
H5 H 0.7316 0.1178 0.2659 0.044 Uiso 1 1 calc R . .
C14 C 0.5665(3) 0.2002(3) 0.2282(2) 0.0447(10) Uani 1 1 d . . .
H14 H 0.6122 0.2176 0.1957 0.054 Uiso 1 1 calc R . .
C20 C 0.9872(3) 0.1855(3) 0.4348(3) 0.0543(12) Uani 1 1 d . . .
H20 H 1.0418 0.1927 0.4652 0.065 Uiso 1 1 calc R . .
C22 C 0.4320(3) 0.1516(3) 0.3226(3) 0.0523(11) Uani 1 1 d . . .
H22 H 0.3861 0.1360 0.3555 0.063 Uiso 1 1 calc R . .
C27 C 0.1008(3) 0.0967(3) 0.0307(3) 0.0565(12) Uani 1 1 d . . .
H27 H 0.0874 0.0742 -0.0208 0.068 Uiso 1 1 calc R . .
C24 C 0.9843(3) 0.1385(3) 0.3651(3) 0.0567(12) Uani 1 1 d . . .
H24 H 1.0370 0.1143 0.3457 0.068 Uiso 1 1 calc R . .
C21 C 0.2075(3) 0.1419(3) 0.1313(3) 0.0498(11) Uani 1 1 d . . .
C35 C 1.3228(3) 0.4038(3) 0.1285(3) 0.0624(13) Uani 1 1 d . . .
H35 H 1.3799 0.3898 0.1525 0.075 Uiso 1 1 calc R . .
C28 C 0.0524(3) 0.1497(3) 0.1517(3) 0.0563(12) Uani 1 1 d . . .
H28 H 0.0059 0.1640 0.1842 0.068 Uiso 1 1 calc R . .
C36 C 1.2339(4) 0.4586(4) 0.0173(3) 0.0687(14) Uani 1 1 d . . .
H36 H 1.2287 0.4825 -0.0345 0.082 Uiso 1 1 calc R . .
C26 C 0.5238(4) 0.3527(4) 0.4719(3) 0.0643(13) Uani 1 1 d . . .
H26 H 0.5317 0.3175 0.5188 0.077 Uiso 1 1 calc R . .
C19 C 0.4115(3) 0.1698(3) 0.2448(3) 0.0464(11) Uani 1 1 d . . .
N6 N 0.3035(3) 0.1516(3) 0.1519(2) 0.0552(10) Uani 1 1 d . . .
C31 C 0.4434(4) 0.3933(4) 0.4544(4) 0.0800(17) Uani 1 1 d . . .
H31 H 0.3967 0.3868 0.4884 0.096 Uiso 1 1 calc R . .
C33 C 1.3160(4) 0.4380(4) 0.0530(3) 0.0658(14) Uani 1 1 d . . .
H33 H 1.3679 0.4472 0.0257 0.079 Uiso 1 1 calc R . .
C34 C 1.2494(4) 0.3897(3) 0.1697(3) 0.0630(13) Uani 1 1 d . . .
H34 H 1.2550 0.3665 0.2217 0.076 Uiso 1 1 calc R . .
C30 C 0.1875(3) 0.1103(3) 0.0569(3) 0.0552(12) Uani 1 1 d . . .
H30 H 0.2337 0.0978 0.0235 0.066 Uiso 1 1 calc R . .
C25 C 0.1407(3) 0.1633(3) 0.1784(3) 0.0570(12) Uani 1 1 d . . .
H25 H 0.1546 0.1875 0.2293 0.068 Uiso 1 1 calc R . .
C37 C 1.1579(3) 0.4439(3) 0.0583(3) 0.0663(14) Uani 1 1 d . . .
H37 H 1.1004 0.4571 0.0349 0.080 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
Zn01 N5 2.039(4) . ?
Zn01 N7 2.040(3) . ?
Zn01 N1 2.118(3) . ?
Zn01 N4 2.146(3) . ?
Zn01 N3 2.306(3) . ?
Zn01 N2 2.347(3) . ?
S1 C3 1.626(4) . ?
S2 C12 1.617(4) . ?
N9 N10 1.193(5) . ?
N9 C29 1.528(6) . ?
N7 C3 1.157(5) . ?
N2 C4 1.278(5) . ?
N2 C1 1.419(5) . ?
C29 C34 1.349(7) . ?
C29 C37 1.393(7) . ?
N3 C5 1.264(5) . ?
N3 C2 1.416(5) . ?
N1 C10 1.342(5) . ?
N1 C6 1.357(5) . ?
C1 C8 1.381(5) . ?
C1 C23 1.392(5) . ?
N4 C26 1.330(6) . ?
N4 C15 1.353(5) . ?
C12 N5 1.148(5) . ?
C8 C7 1.377(6) . ?
C8 H8 0.9500 . ?
C10 C20 1.364(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.494(6) . ?
C15 C32 1.374(6) . ?
C15 C4 1.456(6) . ?
C4 H4 0.9500 . ?
C6 C18 1.365(6) . ?
C6 C5 1.481(5) . ?
C2 C14 1.385(5) . ?
C2 C11 1.386(6) . ?
C11 C22 1.386(6) . ?
C11 H11 0.9500 . ?
C23 C13 1.372(6) . ?
C23 H23 0.9500 . ?
C13 C9 1.358(6) . ?
C13 H13 0.9500 . ?
C18 C24 1.385(6) . ?
C18 H18 0.9500 . ?
C9 C7 1.394(6) . ?
C17 C27 1.364(6) . ?
C17 C28 1.380(6) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.203(5) . ?
N8 C19 1.478(6) . ?
C38 C31 1.377(8) . ?
C38 C32 1.385(8) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.383(6) . ?
C16 C14 1.400(6) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.370(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.374(6) . ?
C22 H22 0.9500 . ?
C27 C30 1.369(6) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.367(6) . ?
C21 C25 1.370(6) . ?
C21 N6 1.476(6) . ?
C35 C34 1.371(7) . ?
C35 C33 1.382(7) . ?
C35 H35 0.9500 . ?
C28 C25 1.394(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.376(7) . ?
C36 C37 1.404(7) . ?
C36 H36 0.9500 . ?
C26 C31 1.362(8) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.45(14) . . ?
N5 Zn01 N1 100.83(15) . . ?
N7 Zn01 N1 95.36(13) . . ?
N5 Zn01 N4 94.07(15) . . ?
N7 Zn01 N4 97.79(14) . . ?
N1 Zn01 N4 158.65(12) . . ?
N5 Zn01 N3 92.82(13) . . ?
N7 Zn01 N3 166.73(13) . . ?
N1 Zn01 N3 74.38(11) . . ?
N4 Zn01 N3 89.81(12) . . ?
N5 Zn01 N2 164.06(13) . . ?
N7 Zn01 N2 94.35(12) . . ?
N1 Zn01 N2 88.65(11) . . ?
N4 Zn01 N2 73.67(12) . . ?
N3 Zn01 N2 77.30(10) . . ?
N10 N9 C29 111.0(4) . . ?
C3 N7 Zn01 161.5(3) . . ?
C4 N2 C1 119.8(3) . . ?
C4 N2 Zn01 111.2(2) . . ?
C1 N2 Zn01 127.9(2) . . ?
C34 C29 C37 122.8(5) . . ?
C34 C29 N9 114.6(4) . . ?
C37 C29 N9 122.6(5) . . ?
C5 N3 C2 121.4(3) . . ?
C5 N3 Zn01 112.1(2) . . ?
C2 N3 Zn01 125.8(2) . . ?
C10 N1 C6 116.8(3) . . ?
C10 N1 Zn01 125.3(3) . . ?
C6 N1 Zn01 117.4(2) . . ?
C8 C1 C23 119.7(4) . . ?
C8 C1 N2 118.6(3) . . ?
C23 C1 N2 121.7(3) . . ?
N7 C3 S1 179.0(4) . . ?
C26 N4 C15 117.8(4) . . ?
C26 N4 Zn01 124.4(3) . . ?
C15 N4 Zn01 117.5(3) . . ?
N5 C12 S2 179.8(5) . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 123.4(4) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
N9 N10 C9 107.6(4) . . ?
N4 C15 C32 122.0(4) . . ?
N4 C15 C4 116.1(3) . . ?
C32 C15 C4 121.9(4) . . ?
N2 C4 C15 120.3(3) . . ?
N2 C4 H4 119.8 . . ?
C15 C4 H4 119.8 . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.3(3) . . ?
C14 C2 C11 120.1(4) . . ?
C14 C2 N3 122.6(4) . . ?
C11 C2 N3 117.1(3) . . ?
C2 C11 C22 120.0(4) . . ?
C2 C11 H11 120.0 . . ?
C22 C11 H11 120.0 . . ?
C13 C23 C1 120.0(4) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C12 N5 Zn01 165.0(3) . . ?
C9 C13 C23 120.3(4) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C6 C18 C24 118.9(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.6(4) . . ?
C13 C9 N10 113.9(4) . . ?
C7 C9 N10 125.4(4) . . ?
C27 C17 C28 119.6(4) . . ?
C27 C17 H17 120.2 . . ?
C28 C17 H17 120.2 . . ?
C8 C7 C9 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
C9 C7 H7 120.3 . . ?
N6 N8 C19 110.9(4) . . ?
C31 C38 C32 119.1(5) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?
C15 C32 C38 118.8(5) . . ?
C15 C32 H32 120.6 . . ?
C38 C32 H32 120.6 . . ?
C19 C16 C14 120.8(4) . . ?
C19 C16 H16 119.6 . . ?
C14 C16 H16 119.6 . . ?
N3 C5 C6 119.6(3) . . ?
N3 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C2 C14 C16 119.0(4) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
C10 C20 C24 119.2(4) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C19 C22 C11 120.6(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C17 C27 C30 121.2(4) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.1(4) . . ?
C30 C21 N6 113.8(4) . . ?
C25 C21 N6 126.1(4) . . ?
C34 C35 C33 121.7(5) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C17 C28 C25 119.2(4) . . ?
C17 C28 H28 120.4 . . ?
C25 C28 H28 120.4 . . ?
C33 C36 C37 119.2(5) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
N4 C26 C31 123.7(5) . . ?
N4 C26 H26 118.1 . . ?
C31 C26 H26 118.1 . . ?
C22 C19 C16 119.4(4) . . ?
C22 C19 N8 113.4(4) . . ?
C16 C19 N8 127.1(4) . . ?
N8 N6 C21 109.2(4) . . ?
C26 C31 C38 118.5(5) . . ?
C26 C31 H31 120.7 . . ?
C38 C31 H31 120.7 . . ?
C36 C33 C35 119.9(5) . . ?
C36 C33 H33 120.0 . . ?
C35 C33 H33 120.0 . . ?
C29 C34 C35 118.2(5) . . ?
C29 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
C21 C30 C27 119.8(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C21 C25 C28 120.1(4) . . ?
C21 C25 H25 120.0 . . ?
C28 C25 H25 120.0 . . ?
C29 C37 C36 118.2(5) . . ?
C29 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?

_diffrn_measured_fraction_theta_max 0.742
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.742
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_znaza170kd
_database_code_depnum_ccdc_archive 'CCDC 1492671'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0995(6)
_cell_length_b                   14.3215(10)
_cell_length_c                   17.1475(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.087(4)
_cell_angle_gamma                90.00
_cell_volume                     3698.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    14499
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_T_max  0.7094
_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            6270
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4832
_reflns_number_gt                4246
_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)+(0.0547P)²+5.9718P] 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         4832
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1249
_refine_ls_wR_factor_gt          0.1197
_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
Zn01 Zn 0.71541(3) 0.28409(3) 0.44658(2) 0.03453(17) Uani 1 1 d . . .
S1 S 0.80762(7) 0.50038(8) 0.64747(5) 0.0413(3) Uani 1 1 d . . .
S2 S 0.56274(8) 0.07226(8) 0.60413(6) 0.0491(3) Uani 1 1 d . . .
N9 N 1.0922(3) 0.3953(2) 0.1854(2) 0.0486(9) Uani 1 1 d . . .
N7 N 0.7774(2) 0.3742(2) 0.52473(18) 0.0450(9) Uani 1 1 d . . .
N2 N 0.7313(2) 0.3810(2) 0.33838(16) 0.0294(7) Uani 1 1 d . . .
C29 C 1.1685(3) 0.4099(3) 0.1348(3) 0.0481(11) Uani 1 1 d . . .
N3 N 0.6739(2) 0.1880(2) 0.34251(16) 0.0313(7) Uani 1 1 d . . .
N1 N 0.8326(2) 0.2130(2) 0.41962(16) 0.0343(7) Uani 1 1 d . . .
C1 C 0.8048(2) 0.3865(2) 0.29112(19) 0.0303(8) Uani 1 1 d . . .
C3 C 0.7894(2) 0.4263(3) 0.5761(2) 0.0342(9) Uani 1 1 d . . .
N4 N 0.5925(2) 0.3592(2) 0.42777(18) 0.0400(8) Uani 1 1 d . . .
C12 C 0.6236(3) 0.1438(3) 0.55825(19) 0.0351(9) Uani 1 1 d . . .
C8 C 0.8884(3) 0.4002(3) 0.3275(2) 0.0346(9) Uani 1 1 d . . .
H8 H 0.8957 0.4067 0.3827 0.042 Uiso 1 1 calc R . .
C10 C 0.9119(3) 0.2219(3) 0.4595(2) 0.0417(10) Uani 1 1 d . . .
H10 H 0.9151 0.2550 0.5076 0.050 Uiso 1 1 calc R . .
N10 N 1.0212(3) 0.4014(3) 0.1483(2) 0.0557(10) Uani 1 1 d . . .
C15 C 0.5808(3) 0.4106(3) 0.3615(2) 0.0389(9) Uani 1 1 d . . .
C4 C 0.6574(3) 0.4190(3) 0.3151(2) 0.0352(9) Uani 1 1 d . . .
H4 H 0.6526 0.4529 0.2674 0.042 Uiso 1 1 calc R . .
C6 C 0.8298(3) 0.1641(3) 0.35181(19) 0.0326(9) Uani 1 1 d . . .
C2 C 0.5871(3) 0.1792(3) 0.3064(2) 0.0334(9) Uani 1 1 d . . .
C11 C 0.5200(3) 0.1557(3) 0.3541(2) 0.0423(10) Uani 1 1 d . . .
H11 H 0.5340 0.1425 0.4079 0.051 Uiso 1 1 calc R . .
C23 C 0.7948(3) 0.3743(3) 0.2103(2) 0.0415(10) Uani 1 1 d . . .
H23 H 0.7377 0.3628 0.1853 0.050 Uiso 1 1 calc R . .
N5 N 0.6672(3) 0.1949(3) 0.52586(19) 0.0527(10) Uani 1 1 d . . .
C13 C 0.8674(3) 0.3789(3) 0.1669(2) 0.0486(11) Uani 1 1 d . . .
H13 H 0.8603 0.3719 0.1117 0.058 Uiso 1 1 calc R . .
C18 C 0.9038(3) 0.1269(3) 0.3226(2) 0.0427(10) Uani 1 1 d . . .
H18 H 0.8995 0.0936 0.2746 0.051 Uiso 1 1 calc R . .
C9 C 0.9499(3) 0.3936(3) 0.2023(2) 0.0407(10) Uani 1 1 d . . .
C17 C 0.0332(3) 0.1151(3) 0.0774(2) 0.0443(10) Uani 1 1 d . . .
H17 H -0.0268 0.1040 0.0592 0.053 Uiso 1 1 calc R . .
C7 C 0.9612(3) 0.4043(3) 0.2834(2) 0.0415(10) Uani 1 1 d . . .
H7 H 1.0188 0.4145 0.3080 0.050 Uiso 1 1 calc R . .
N8 N 0.3169(2) 0.1612(2) 0.2218(2) 0.0489(9) Uani 1 1 d . . .
C38 C 0.4314(3) 0.4435(4) 0.3874(4) 0.0751(16) Uani 1 1 d . . .
H38 H 0.3758 0.4721 0.3735 0.090 Uiso 1 1 calc R . .
C32 C 0.5009(3) 0.4520(3) 0.3394(3) 0.0553(12) Uani 1 1 d . . .
H32 H 0.4934 0.4861 0.2919 0.066 Uiso 1 1 calc R . .
C16 C 0.4786(3) 0.1949(3) 0.1977(2) 0.0452(11) Uani 1 1 d . . .
H16 H 0.4642 0.2090 0.1442 0.054 Uiso 1 1 calc R . .
C5 C 0.7402(3) 0.1520(3) 0.31244(19) 0.0331(9) Uani 1 1 d . . .
H5 H 0.7324 0.1176 0.2651 0.040 Uiso 1 1 calc R . .
C14 C 0.5666(3) 0.1999(3) 0.2280(2) 0.0394(10) Uani 1 1 d . . .
H14 H 0.6122 0.2173 0.1954 0.047 Uiso 1 1 calc R . .
C20 C 0.9883(3) 0.1854(3) 0.4341(3) 0.0500(12) Uani 1 1 d . . .
H20 H 1.0430 0.1924 0.4646 0.060 Uiso 1 1 calc R . .
C22 C 0.4324(3) 0.1513(3) 0.3233(2) 0.0471(11) Uani 1 1 d . . .
H22 H 0.3866 0.1357 0.3562 0.056 Uiso 1 1 calc R . .
C27 C 0.1003(3) 0.0965(3) 0.0301(3) 0.0497(11) Uani 1 1 d . . .
H27 H 0.0863 0.0735 -0.0212 0.060 Uiso 1 1 calc R . .
C24 C 0.9855(3) 0.1384(3) 0.3642(3) 0.0504(11) Uani 1 1 d . . .
H24 H 1.0382 0.1144 0.3446 0.060 Uiso 1 1 calc R . .
C21 C 0.2079(3) 0.1417(3) 0.1306(3) 0.0436(10) Uani 1 1 d . . .
C35 C 1.3234(3) 0.4036(3) 0.1289(3) 0.0547(12) Uani 1 1 d . . .
H35 H 1.3804 0.3893 0.1528 0.066 Uiso 1 1 calc R . .
C28 C 0.0529(3) 0.1500(3) 0.1517(3) 0.0502(11) Uani 1 1 d . . .
H28 H 0.0066 0.1646 0.1844 0.060 Uiso 1 1 calc R . .
C36 C 1.2338(3) 0.4586(3) 0.0179(3) 0.0600(13) Uani 1 1 d . . .
H36 H 1.2284 0.4825 -0.0339 0.072 Uiso 1 1 calc R . .
C26 C 0.5249(3) 0.3521(3) 0.4730(3) 0.0574(12) Uani 1 1 d . . .
H26 H 0.5332 0.3167 0.5198 0.069 Uiso 1 1 calc R . .
C19 C 0.4118(3) 0.1696(3) 0.2451(2) 0.0411(10) Uani 1 1 d . . .
N6 N 0.3033(2) 0.1513(2) 0.15157(19) 0.0474(9) Uani 1 1 d . . .
C31 C 0.4444(4) 0.3926(4) 0.4557(4) 0.0722(15) Uani 1 1 d . . .
H31 H 0.3980 0.3860 0.4900 0.087 Uiso 1 1 calc R . .
C33 C 1.3162(3) 0.4380(3) 0.0535(3) 0.0584(13) Uani 1 1 d . . .
H33 H 1.3680 0.4475 0.0262 0.070 Uiso 1 1 calc R . .
C34 C 1.2496(3) 0.3897(3) 0.1698(3) 0.0541(12) Uani 1 1 d . . .
H34 H 1.2552 0.3664 0.2218 0.065 Uiso 1 1 calc R . .
C30 C 0.1875(3) 0.1106(3) 0.0559(3) 0.0484(11) Uani 1 1 d . . .
H30 H 0.2335 0.0988 0.0221 0.058 Uiso 1 1 calc R . .
C25 C 0.1414(3) 0.1637(3) 0.1782(3) 0.0515(12) Uani 1 1 d . . .
H25 H 0.1558 0.1881 0.2291 0.062 Uiso 1 1 calc R . .
C37 C 1.1583(3) 0.4440(3) 0.0589(3) 0.0569(12) Uani 1 1 d . . .
H37 H 1.1008 0.4572 0.0352 0.068 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
Zn01 N5 2.037(4) . ?
Zn01 N7 2.039(3) . ?
Zn01 N1 2.120(3) . ?
Zn01 N4 2.149(3) . ?
Zn01 N3 2.304(3) . ?
Zn01 N2 2.343(3) . ?
S1 C3 1.627(4) . ?
S2 C12 1.617(4) . ?
N9 N10 1.211(5) . ?
N9 C29 1.505(6) . ?
N7 C3 1.160(5) . ?
N2 C4 1.279(5) . ?
N2 C1 1.422(5) . ?
C29 C34 1.356(7) . ?
C29 C37 1.389(7) . ?
N3 C5 1.268(5) . ?
N3 C2 1.415(5) . ?
N1 C10 1.343(5) . ?
N1 C6 1.356(5) . ?
C1 C8 1.381(5) . ?
C1 C23 1.395(5) . ?
N4 C26 1.330(5) . ?
N4 C15 1.355(5) . ?
C12 N5 1.154(5) . ?
C8 C7 1.380(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.366(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.473(5) . ?
C15 C32 1.374(6) . ?
C15 C4 1.454(6) . ?
C4 H4 0.9500 . ?
C6 C18 1.364(6) . ?
C6 C5 1.478(5) . ?
C2 C11 1.388(5) . ?
C2 C14 1.391(5) . ?
C11 C22 1.390(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.370(6) . ?
C23 H23 0.9500 . ?
C13 C9 1.362(6) . ?
C13 H13 0.9500 . ?
C18 C24 1.390(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.397(5) . ?
C17 C27 1.367(6) . ?
C17 C28 1.381(6) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.215(4) . ?
N8 C19 1.465(5) . ?
C38 C32 1.383(7) . ?
C38 C31 1.383(8) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.388(6) . ?
C16 C14 1.393(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.372(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.380(6) . ?
C22 H22 0.9500 . ?
C27 C30 1.374(6) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.371(6) . ?
C21 C25 1.375(6) . ?
C21 N6 1.466(5) . ?
C35 C34 1.374(6) . ?
C35 C33 1.379(6) . ?
C35 H35 0.9500 . ?
C28 C25 1.395(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.378(7) . ?
C36 C37 1.397(7) . ?
C36 H36 0.9500 . ?
C26 C31 1.360(7) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.30(14) . . ?
N5 Zn01 N1 100.82(14) . . ?
N7 Zn01 N1 95.51(12) . . ?
N5 Zn01 N4 93.94(14) . . ?
N7 Zn01 N4 97.63(13) . . ?
N1 Zn01 N4 158.80(11) . . ?
N5 Zn01 N3 93.00(12) . . ?
N7 Zn01 N3 166.75(13) . . ?
N1 Zn01 N3 74.30(11) . . ?
N4 Zn01 N3 89.93(11) . . ?
N5 Zn01 N2 164.05(13) . . ?
N7 Zn01 N2 94.44(12) . . ?
N1 Zn01 N2 88.71(11) . . ?
N4 Zn01 N2 73.78(12) . . ?
N3 Zn01 N2 77.18(10) . . ?
N10 N9 C29 111.9(4) . . ?
C3 N7 Zn01 161.2(3) . . ?
C4 N2 C1 119.8(3) . . ?
C4 N2 Zn01 111.2(2) . . ?
C1 N2 Zn01 127.7(2) . . ?
C34 C29 C37 121.7(4) . . ?
C34 C29 N9 114.8(4) . . ?
C37 C29 N9 123.4(4) . . ?
C5 N3 C2 121.3(3) . . ?
C5 N3 Zn01 112.3(2) . . ?
C2 N3 Zn01 125.7(2) . . ?
C10 N1 C6 117.2(3) . . ?
C10 N1 Zn01 124.9(3) . . ?
C6 N1 Zn01 117.4(2) . . ?
C8 C1 C23 119.8(3) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.7(3) . . ?
N7 C3 S1 179.1(4) . . ?
C26 N4 C15 118.1(4) . . ?
C26 N4 Zn01 124.4(3) . . ?
C15 N4 Zn01 117.2(3) . . ?
N5 C12 S2 179.7(4) . . ?
C7 C8 C1 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
N1 C10 C20 123.0(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
N9 N10 C9 108.9(4) . . ?
N4 C15 C32 121.7(4) . . ?
N4 C15 C4 116.3(3) . . ?
C32 C15 C4 122.1(4) . . ?
N2 C4 C15 120.3(3) . . ?
N2 C4 H4 119.9 . . ?
C15 C4 H4 119.9 . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.2(3) . . ?
C11 C2 C14 120.1(3) . . ?
C11 C2 N3 117.1(3) . . ?
C14 C2 N3 122.6(3) . . ?
C2 C11 C22 120.1(4) . . ?
C2 C11 H11 120.0 . . ?
C22 C11 H11 120.0 . . ?
C13 C23 C1 120.0(4) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C12 N5 Zn01 164.3(3) . . ?
C9 C13 C23 120.4(4) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C6 C18 C24 119.1(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.3(4) . . ?
C13 C9 N10 114.6(3) . . ?
C7 C9 N10 125.0(4) . . ?
C27 C17 C28 119.8(4) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C8 C7 C9 119.6(4) . . ?
C8 C7 H7 120.2 . . ?
C9 C7 H7 120.2 . . ?
N6 N8 C19 111.9(4) . . ?
C32 C38 C31 118.9(5) . . ?
C32 C38 H38 120.5 . . ?
C31 C38 H38 120.5 . . ?
C15 C32 C38 119.1(5) . . ?
C15 C32 H32 120.4 . . ?
C38 C32 H32 120.4 . . ?
C19 C16 C14 120.6(4) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N3 C5 C6 119.3(3) . . ?
N3 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C2 C14 C16 119.3(4) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
C10 C20 C24 119.4(4) . . ?
C10 C20 H20 120.3 . . ?
C24 C20 H20 120.3 . . ?
C19 C22 C11 120.2(4) . . ?
C19 C22 H22 119.9 . . ?
C11 C22 H22 119.9 . . ?
C17 C27 C30 121.0(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C20 C24 C18 118.5(4) . . ?
C20 C24 H24 120.8 . . ?
C18 C24 H24 120.8 . . ?
C30 C21 C25 120.3(4) . . ?
C30 C21 N6 114.2(4) . . ?
C25 C21 N6 125.4(4) . . ?
C34 C35 C33 121.2(5) . . ?
C34 C35 H35 119.4 . . ?
C33 C35 H35 119.4 . . ?
C17 C28 C25 119.4(4) . . ?
C17 C28 H28 120.3 . . ?
C25 C28 H28 120.3 . . ?
C33 C36 C37 119.3(5) . . ?
C33 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
N4 C26 C31 123.5(5) . . ?
N4 C26 H26 118.2 . . ?
C31 C26 H26 118.2 . . ?
C22 C19 C16 119.7(4) . . ?
C22 C19 N8 113.5(4) . . ?
C16 C19 N8 126.8(4) . . ?
N8 N6 C21 110.4(4) . . ?
C26 C31 C38 118.6(5) . . ?
C26 C31 H31 120.7 . . ?
C38 C31 H31 120.7 . . ?
C36 C33 C35 120.0(4) . . ?
C36 C33 H33 120.0 . . ?
C35 C33 H33 120.0 . . ?
C29 C34 C35 118.9(4) . . ?
C29 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C21 C30 C27 119.6(4) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C21 C25 C28 119.8(4) . . ?
C21 C25 H25 120.1 . . ?
C28 C25 H25 120.1 . . ?
C29 C37 C36 118.9(4) . . ?
C29 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.741
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.741
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.055
####################################################################### 
# 
# 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_feaza295km2
_database_code_depnum_ccdc_archive 'CCDC 1492672'
_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                   15.1239(7)
_cell_length_b                   14.5665(10)
_cell_length_c                   17.0273(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.929(4)
_cell_angle_gamma                90.00
_cell_volume                     3746.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4505
_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    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5552
_exptl_absorpt_correction_T_max  0.8970
_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      295(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            5918
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0487
_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             4228
_reflns_number_gt                3159
_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)+(0.0198P)²+2.3367P] 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         4228
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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 0.29234(3) 0.28767(3) 0.05530(3) 0.0594(2) Uani 1 1 d . . .
S1 S 0.18854(6) 0.49631(7) -0.14673(6) 0.0753(3) Uani 1 1 d . . .
S2 S 0.43682(7) 0.07275(8) -0.10661(7) 0.0855(4) Uani 1 1 d . . .
N1 N 0.17234(19) 0.21574(18) 0.07823(18) 0.0593(8) Uani 1 1 d . . .
N2 N 0.27371(18) 0.37965(17) 0.16055(15) 0.0490(7) Uani 1 1 d . . .
C1 C 0.1974(2) 0.3850(2) 0.2069(2) 0.0498(9) Uani 1 1 d . . .
C2 C 0.4140(2) 0.1808(2) 0.1912(2) 0.0568(9) Uani 1 1 d . . .
C3 C 0.2138(2) 0.4257(3) -0.0755(2) 0.0590(10) Uani 1 1 d . . .
N3 N 0.3279(2) 0.19048(18) 0.15396(16) 0.0545(7) Uani 1 1 d . . .
C4 C 0.3445(2) 0.4199(2) 0.1853(2) 0.0583(9) Uani 1 1 d . . .
H4 H 0.3457 0.4539 0.2315 0.070 Uiso 1 1 calc R . .
C5 C 0.2612(3) 0.1524(2) 0.1829(2) 0.0609(10) Uani 1 1 d . . .
H5 H 0.2681 0.1171 0.2283 0.073 Uiso 1 1 calc R . .
N4 N 0.41576(18) 0.3610(2) 0.0751(2) 0.0664(8) Uani 1 1 d . . .
N5 N 0.3440(2) 0.2029(2) -0.0274(2) 0.0873(11) Uani 1 1 d . . .
C6 C 0.1736(2) 0.1648(2) 0.1440(2) 0.0579(9) Uani 1 1 d . . .
C7 C 0.0410(2) 0.4031(2) 0.2112(3) 0.0742(12) Uani 1 1 d . . .
H7 H -0.0143 0.4129 0.1860 0.089 Uiso 1 1 calc R . .
C8 C 0.1164(2) 0.3992(2) 0.1681(2) 0.0610(10) Uani 1 1 d . . .
H8 H 0.1122 0.4061 0.1138 0.073 Uiso 1 1 calc R . .
C9 C 0.0488(3) 0.3925(3) 0.2910(3) 0.0794(13) Uani 1 1 d . . .
C10 C 0.0948(3) 0.2253(3) 0.0383(2) 0.0759(11) Uani 1 1 d . . .
H10 H 0.0929 0.2594 -0.0080 0.091 Uiso 1 1 calc R . .
C11 C 0.4823(3) 0.1574(3) 0.1450(2) 0.0726(11) Uani 1 1 d . . .
H11 H 0.4704 0.1449 0.0919 0.087 Uiso 1 1 calc R . .
C12 C 0.3826(2) 0.1484(3) -0.0605(2) 0.0610(10) Uani 1 1 d . . .
C13 C 0.1289(3) 0.3782(3) 0.3292(3) 0.0845(12) Uani 1 1 d . . .
H13 H 0.1330 0.3713 0.3835 0.101 Uiso 1 1 calc R . .
C14 C 0.4323(3) 0.2003(2) 0.2695(3) 0.0740(11) Uani 1 1 d . . .
H14 H 0.3871 0.2171 0.3017 0.089 Uiso 1 1 calc R . .
C15 C 0.4239(2) 0.4122(2) 0.1403(3) 0.0622(10) Uani 1 1 d . . .
C16 C 0.5197(3) 0.1945(3) 0.3000(3) 0.0841(13) Uani 1 1 d . . .
H16 H 0.5329 0.2074 0.3527 0.101 Uiso 1 1 calc R . .
N6 N 0.6907(3) 0.1540(2) 0.3424(3) 0.1027(13) Uani 1 1 d . . .
C17 C 0.9616(3) 0.1181(3) 0.4180(4) 0.0848(13) Uani 1 1 d . . .
H17 H 1.0196 0.1084 0.4371 0.102 Uiso 1 1 calc R . .
N7 N 0.2311(2) 0.3762(2) -0.0242(2) 0.0806(10) Uani 1 1 d . . .
C18 C 0.0988(3) 0.1254(3) 0.1721(3) 0.0757(11) Uani 1 1 d . . .
H18 H 0.1020 0.0914 0.2184 0.091 Uiso 1 1 calc R . .
C19 C 0.5856(3) 0.1700(3) 0.2524(4) 0.0798(13) Uani 1 1 d . . .
N8 N 0.6868(3) 0.1620(2) 0.2757(3) 0.0915(12) Uani 1 1 d . . .
N9 N -0.0823(3) 0.3956(2) 0.3132(3) 0.0994(13) Uani 1 1 d . . .
N10 N -0.0282(3) 0.4026(3) 0.3568(3) 0.1169(17) Uani 1 1 d . . .
C20 C 0.0171(3) 0.1870(3) 0.0624(3) 0.0926(14) Uani 1 1 d . . .
H20 H -0.0357 0.1950 0.0328 0.111 Uiso 1 1 calc R . .
C21 C 0.7920(2) 0.1433(3) 0.3643(4) 0.0857(14) Uani 1 1 d . . .
C22 C 0.5673(3) 0.1521(3) 0.1756(3) 0.0847(13) Uani 1 1 d . . .
H22 H 0.6127 0.1362 0.1434 0.102 Uiso 1 1 calc R . .
C23 C 0.2028(2) 0.3741(3) 0.2871(2) 0.0717(11) Uani 1 1 d . . .
H23 H 0.2576 0.3637 0.3130 0.086 Uiso 1 1 calc R . .
C24 C 0.0193(3) 0.1373(3) 0.1303(3) 0.0899(13) Uani 1 1 d . . .
H24 H -0.0324 0.1117 0.1482 0.108 Uiso 1 1 calc R . .
C25 C 0.8589(3) 0.1608(3) 0.3149(3) 0.0954(14) Uani 1 1 d . . .
H25 H 0.8466 0.1803 0.2635 0.114 Uiso 1 1 calc R . .
C26 C 0.4855(3) 0.3550(3) 0.0316(3) 0.1028(15) Uani 1 1 d . . .
H26 H 0.4809 0.3203 -0.0142 0.123 Uiso 1 1 calc R . .
C27 C 0.8950(3) 0.1019(3) 0.4643(3) 0.1044(15) Uani 1 1 d . . .
H27 H 0.9072 0.0814 0.5155 0.125 Uiso 1 1 calc R . .
C28 C 0.9462(3) 0.1484(3) 0.3442(4) 0.0961(14) Uani 1 1 d . . .
H28 H 0.9932 0.1610 0.3127 0.115 Uiso 1 1 calc R . .
C29 C -0.1614(4) 0.4097(3) 0.3751(5) 0.108(2) Uani 1 1 d . . .
C30 C 0.8097(3) 0.1149(3) 0.4381(4) 0.1061(16) Uani 1 1 d . . .
H30 H 0.7638 0.1041 0.4712 0.127 Uiso 1 1 calc R . .
C31 C 0.5647(4) 0.3979(5) 0.0513(5) 0.139(2) Uani 1 1 d . . .
H31 H 0.6121 0.3925 0.0188 0.167 Uiso 1 1 calc R . .
C32 C 0.5019(3) 0.4557(3) 0.1646(3) 0.0954(14) Uani 1 1 d . . .
H32 H 0.5061 0.4892 0.2111 0.115 Uiso 1 1 calc R . .
C33 C -0.3139(3) 0.4366(3) 0.4506(4) 0.1022(15) Uani 1 1 d . . .
H33 H -0.3665 0.4451 0.4756 0.123 Uiso 1 1 calc R . .
C34 C -0.2405(4) 0.3904(3) 0.3382(3) 0.1062(17) Uani 1 1 d . . .
H34 H -0.2429 0.3681 0.2870 0.127 Uiso 1 1 calc R . .
C35 C -0.3160(3) 0.4033(3) 0.3757(4) 0.1019(15) Uani 1 1 d . . .
H35 H -0.3701 0.3894 0.3501 0.122 Uiso 1 1 calc R . .
C36 C -0.2344(4) 0.4577(3) 0.4896(3) 0.1093(16) Uani 1 1 d . . .
H36 H -0.2325 0.4809 0.5406 0.131 Uiso 1 1 calc R . .
C37 C -0.1567(3) 0.4431(3) 0.4502(4) 0.1096(18) Uani 1 1 d . . .
H37 H -0.1019 0.4562 0.4750 0.132 Uiso 1 1 calc R . .
C38 C 0.5729(3) 0.4477(4) 0.1178(5) 0.133(2) Uani 1 1 d . . .
H38 H 0.6263 0.4764 0.1321 0.160 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 2.056(4) . ?
Fe1 N5 2.058(4) . ?
Fe1 N1 2.149(3) . ?
Fe1 N4 2.162(3) . ?
Fe1 N3 2.241(3) . ?
Fe1 N2 2.267(3) . ?
S1 C3 1.622(4) . ?
S2 C12 1.603(4) . ?
N1 C10 1.332(4) . ?
N1 C6 1.343(4) . ?
N2 C4 1.273(4) . ?
N2 C1 1.433(4) . ?
C1 C23 1.374(5) . ?
C1 C8 1.378(4) . ?
C2 C11 1.373(5) . ?
C2 C14 1.377(5) . ?
C2 N3 1.427(4) . ?
C3 N7 1.151(4) . ?
N3 C5 1.272(4) . ?
C4 C15 1.461(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.463(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.322(5) . ?
N4 C15 1.337(4) . ?
N5 C12 1.148(4) . ?
C6 C18 1.375(5) . ?
C7 C9 1.367(6) . ?
C7 C8 1.389(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.361(6) . ?
C9 N10 1.662(6) . ?
C10 C20 1.383(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.364(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.359(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.398(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.384(5) . ?
C16 C19 1.364(6) . ?
C16 H16 0.9300 . ?
N6 N8 1.140(4) . ?
N6 C21 1.566(5) . ?
C17 C27 1.331(6) . ?
C17 C28 1.342(6) . ?
C17 H17 0.9300 . ?
C18 C24 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.348(6) . ?
C19 N8 1.566(5) . ?
N9 N10 1.082(4) . ?
N9 C29 1.647(6) . ?
C20 C24 1.363(6) . ?
C20 H20 0.9300 . ?
C21 C30 1.337(6) . ?
C21 C25 1.372(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.399(6) . ?
C25 H25 0.9300 . ?
C26 C31 1.377(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.358(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.352(7) . ?
C29 C37 1.367(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.346(8) . ?
C31 H31 0.9300 . ?
C32 C38 1.375(7) . ?
C32 H32 0.9300 . ?
C33 C35 1.364(6) . ?
C33 C36 1.378(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.349(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.399(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
N7 Fe1 N5 95.73(14) . . ?
N7 Fe1 N1 93.97(13) . . ?
N5 Fe1 N1 100.69(12) . . ?
N7 Fe1 N4 98.59(12) . . ?
N5 Fe1 N4 92.78(13) . . ?
N1 Fe1 N4 160.57(12) . . ?
N7 Fe1 N3 166.57(12) . . ?
N5 Fe1 N3 92.82(12) . . ?
N1 Fe1 N3 74.22(12) . . ?
N4 Fe1 N3 91.32(11) . . ?
N7 Fe1 N2 94.58(12) . . ?
N5 Fe1 N2 164.39(12) . . ?
N1 Fe1 N2 90.24(10) . . ?
N4 Fe1 N2 74.08(11) . . ?
N3 Fe1 N2 79.37(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 125.8(3) . . ?
C6 N1 Fe1 116.4(2) . . ?
C4 N2 C1 118.7(3) . . ?
C4 N2 Fe1 113.4(2) . . ?
C1 N2 Fe1 127.1(2) . . ?
C23 C1 C8 120.0(3) . . ?
C23 C1 N2 122.2(3) . . ?
C8 C1 N2 117.8(3) . . ?
C11 C2 C14 119.2(4) . . ?
C11 C2 N3 117.7(4) . . ?
C14 C2 N3 122.9(3) . . ?
N7 C3 S1 179.1(4) . . ?
C5 N3 C2 120.5(3) . . ?
C5 N3 Fe1 113.7(2) . . ?
C2 N3 Fe1 125.1(2) . . ?
N2 C4 C15 119.4(3) . . ?
N2 C4 H4 120.3 . . ?
C15 C4 H4 120.3 . . ?
N3 C5 C6 119.2(3) . . ?
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 165.9(3) . . ?
N1 C6 C18 123.0(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.2(4) . . ?
C9 C7 C8 119.3(4) . . ?
C9 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C1 C8 C7 119.2(4) . . ?
C1 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C13 C9 C7 121.4(4) . . ?
C13 C9 N10 109.2(4) . . ?
C7 C9 N10 129.2(4) . . ?
N1 C10 C20 123.0(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 121.1(4) . . ?
C22 C11 H11 119.5 . . ?
C2 C11 H11 119.5 . . ?
N5 C12 S2 179.7(4) . . ?
C23 C13 C9 119.4(4) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C2 C14 C16 119.0(4) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
N4 C15 C32 123.0(4) . . ?
N4 C15 C4 115.8(3) . . ?
C32 C15 C4 121.3(4) . . ?
C19 C16 C14 120.1(4) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N8 N6 C21 104.2(5) . . ?
C27 C17 C28 120.8(5) . . ?
C27 C17 H17 119.6 . . ?
C28 C17 H17 119.6 . . ?
C3 N7 Fe1 165.7(3) . . ?
C6 C18 C24 118.6(4) . . ?
C6 C18 H18 120.7 . . ?
C24 C18 H18 120.7 . . ?
C22 C19 C16 120.4(4) . . ?
C22 C19 N8 112.4(4) . . ?
C16 C19 N8 127.1(5) . . ?
N6 N8 C19 105.0(4) . . ?
N10 N9 C29 95.6(5) . . ?
N9 N10 C9 93.4(5) . . ?
C24 C20 C10 118.9(4) . . ?
C24 C20 H20 120.6 . . ?
C10 C20 H20 120.6 . . ?
C30 C21 C25 121.0(4) . . ?
C30 C21 N6 113.6(5) . . ?
C25 C21 N6 125.4(5) . . ?
C19 C22 C11 120.2(4) . . ?
C19 C22 H22 119.9 . . ?
C11 C22 H22 119.9 . . ?
C13 C23 C1 120.7(4) . . ?
C13 C23 H23 119.7 . . ?
C1 C23 H23 119.7 . . ?
C20 C24 C18 119.2(4) . . ?
C20 C24 H24 120.4 . . ?
C18 C24 H24 120.4 . . ?
C21 C25 C28 118.0(5) . . ?
C21 C25 H25 121.0 . . ?
C28 C25 H25 121.0 . . ?
N4 C26 C31 122.9(5) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 121.0(5) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C17 C28 C25 119.5(5) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 120.8(5) . . ?
C34 C29 N9 109.3(6) . . ?
C37 C29 N9 129.7(6) . . ?
C21 C30 C27 119.6(5) . . ?
C21 C30 H30 120.2 . . ?
C27 C30 H30 120.2 . . ?
C38 C31 C26 119.4(5) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C38 C32 C15 117.9(5) . . ?
C38 C32 H32 121.1 . . ?
C15 C32 H32 121.1 . . ?
C35 C33 C36 120.5(4) . . ?
C35 C33 H33 119.7 . . ?
C36 C33 H33 119.7 . . ?
C35 C34 C29 120.1(6) . . ?
C35 C34 H34 119.9 . . ?
C29 C34 H34 119.9 . . ?
C34 C35 C33 120.8(5) . . ?
C34 C35 H35 119.6 . . ?
C33 C35 H35 119.6 . . ?
C33 C36 C37 117.9(5) . . ?
C33 C36 H36 121.0 . . ?
C37 C36 H36 121.0 . . ?
C29 C37 C36 119.8(5) . . ?
C29 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C31 C38 C32 119.5(5) . . ?
C31 C38 H38 120.3 . . ?
C32 C38 H38 120.3 . . ?

_diffrn_measured_fraction_theta_max 0.812
_diffrn_reflns_theta_full        22.98
_diffrn_measured_fraction_theta_full 0.812
_refine_diff_density_max         0.231
_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_feaza265kd2
_database_code_depnum_ccdc_archive 'CCDC 1492673'
_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                   15.1158(7)
_cell_length_b                   14.5070(9)
_cell_length_c                   17.0102(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.051(4)
_cell_angle_gamma                90.00
_cell_volume                     3724.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    265(2)
_cell_measurement_reflns_used    4304
_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    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5536
_exptl_absorpt_correction_T_max  0.8964
_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      265(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            5453
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0438
_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             3791
_reflns_number_gt                2995
_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)+(0.0273P)²+1.9708P] 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         3791
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0874
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.29145(3) 0.28752(3) 0.05584(3) 0.0536(2) Uani 1 1 d . . .
S1 S 0.18895(6) 0.49732(7) -0.14686(6) 0.0678(3) Uani 1 1 d . . .
S2 S 0.43670(6) 0.07281(7) -0.10635(6) 0.0766(3) Uani 1 1 d . . .
N1 N 0.17163(18) 0.21589(17) 0.07841(18) 0.0534(7) Uani 1 1 d . . .
N2 N 0.27322(17) 0.37996(16) 0.16052(15) 0.0429(6) Uani 1 1 d . . .
C1 C 0.1971(2) 0.3852(2) 0.2065(2) 0.0448(8) Uani 1 1 d . . .
C2 C 0.4143(2) 0.1809(2) 0.1911(2) 0.0513(9) Uani 1 1 d . . .
C3 C 0.2135(2) 0.4259(3) -0.0754(2) 0.0546(9) Uani 1 1 d . . .
N3 N 0.32747(19) 0.19045(17) 0.15436(16) 0.0496(7) Uani 1 1 d . . .
C4 C 0.3444(2) 0.4199(2) 0.1852(2) 0.0523(9) Uani 1 1 d . . .
H4 H 0.3459 0.4537 0.2317 0.063 Uiso 1 1 calc R . .
C5 C 0.2607(2) 0.1522(2) 0.1837(2) 0.0534(9) Uani 1 1 d . . .
H5 H 0.2677 0.1169 0.2292 0.064 Uiso 1 1 calc R . .
N4 N 0.41447(17) 0.3608(2) 0.07477(19) 0.0600(8) Uani 1 1 d . . .
N5 N 0.3422(2) 0.2025(2) -0.02669(19) 0.0779(10) Uani 1 1 d . . .
C6 C 0.1733(2) 0.1647(2) 0.1446(2) 0.0502(9) Uani 1 1 d . . .
C7 C 0.0409(2) 0.4032(2) 0.2120(3) 0.0662(11) Uani 1 1 d . . .
H7 H -0.0146 0.4129 0.1871 0.079 Uiso 1 1 calc R . .
C8 C 0.1157(2) 0.3995(2) 0.1685(2) 0.0550(9) Uani 1 1 d . . .
H8 H 0.1108 0.4067 0.1141 0.066 Uiso 1 1 calc R . .
C9 C 0.0496(3) 0.3924(2) 0.2922(3) 0.0722(12) Uani 1 1 d . . .
C10 C 0.0939(3) 0.2252(2) 0.0386(2) 0.0678(10) Uani 1 1 d . . .
H10 H 0.0918 0.2593 -0.0078 0.081 Uiso 1 1 calc R . .
C11 C 0.4820(2) 0.1574(2) 0.1438(2) 0.0656(10) Uani 1 1 d . . .
H11 H 0.4698 0.1452 0.0907 0.079 Uiso 1 1 calc R . .
C12 C 0.3817(2) 0.1483(3) -0.0603(2) 0.0548(9) Uani 1 1 d . . .
C13 C 0.1299(3) 0.3774(3) 0.3299(2) 0.0773(11) Uani 1 1 d . . .
H13 H 0.1346 0.3697 0.3842 0.093 Uiso 1 1 calc R . .
C14 C 0.4330(3) 0.2007(2) 0.2696(2) 0.0643(10) Uani 1 1 d . . .
H14 H 0.3878 0.2177 0.3018 0.077 Uiso 1 1 calc R . .
C15 C 0.4237(2) 0.4123(2) 0.1401(2) 0.0556(9) Uani 1 1 d . . .
C16 C 0.5202(3) 0.1948(2) 0.3002(2) 0.0729(11) Uani 1 1 d . . .
H16 H 0.5336 0.2072 0.3532 0.088 Uiso 1 1 calc R . .
N6 N 0.6922(2) 0.1539(2) 0.3434(3) 0.0881(11) Uani 1 1 d . . .
C17 C 0.9628(3) 0.1178(3) 0.4177(3) 0.0738(11) Uani 1 1 d . . .
H17 H 1.0210 0.1074 0.4359 0.089 Uiso 1 1 calc R . .
N7 N 0.2302(2) 0.3758(2) -0.0240(2) 0.0730(9) Uani 1 1 d . . .
C18 C 0.0985(3) 0.1254(2) 0.1728(2) 0.0672(10) Uani 1 1 d . . .
H18 H 0.1017 0.0916 0.2194 0.081 Uiso 1 1 calc R . .
C19 C 0.5858(2) 0.1708(2) 0.2520(3) 0.0691(11) Uani 1 1 d . . .
N8 N 0.6857(2) 0.1623(2) 0.2754(2) 0.0821(11) Uani 1 1 d . . .
N9 N -0.0841(3) 0.3955(2) 0.3136(2) 0.0910(12) Uani 1 1 d . . .
N10 N -0.0270(3) 0.4021(2) 0.3561(3) 0.1058(15) Uani 1 1 d . . .
C20 C 0.0163(3) 0.1867(3) 0.0627(3) 0.0823(13) Uani 1 1 d . . .
H20 H -0.0366 0.1945 0.0330 0.099 Uiso 1 1 calc R . .
C21 C 0.7916(2) 0.1430(3) 0.3655(3) 0.0742(13) Uani 1 1 d . . .
C22 C 0.5672(3) 0.1521(2) 0.1748(3) 0.0733(11) Uani 1 1 d . . .
H22 H 0.6125 0.1355 0.1427 0.088 Uiso 1 1 calc R . .
C23 C 0.2031(2) 0.3737(2) 0.2871(2) 0.0638(10) Uani 1 1 d . . .
H23 H 0.2582 0.3632 0.3125 0.077 Uiso 1 1 calc R . .
C24 C 0.0186(3) 0.1370(3) 0.1310(3) 0.0792(12) Uani 1 1 d . . .
H24 H -0.0329 0.1113 0.1490 0.095 Uiso 1 1 calc R . .
C25 C 0.8579(3) 0.1615(3) 0.3157(3) 0.0843(13) Uani 1 1 d . . .
H25 H 0.8447 0.1817 0.2646 0.101 Uiso 1 1 calc R . .
C26 C 0.4842(3) 0.3546(3) 0.0307(3) 0.0918(14) Uani 1 1 d . . .
H26 H 0.4792 0.3198 -0.0152 0.110 Uiso 1 1 calc R . .
C27 C 0.8966(3) 0.1014(3) 0.4651(3) 0.0893(13) Uani 1 1 d . . .
H27 H 0.9095 0.0808 0.5162 0.107 Uiso 1 1 calc R . .
C28 C 0.9460(3) 0.1492(3) 0.3438(3) 0.0837(12) Uani 1 1 d . . .
H28 H 0.9923 0.1626 0.3118 0.100 Uiso 1 1 calc R . .
C29 C -0.1637(4) 0.4090(3) 0.3726(4) 0.0986(18) Uani 1 1 d . . .
C30 C 0.8106(3) 0.1144(3) 0.4393(3) 0.0945(14) Uani 1 1 d . . .
H30 H 0.7652 0.1034 0.4729 0.113 Uiso 1 1 calc R . .
C31 C 0.5634(3) 0.3975(4) 0.0500(5) 0.124(2) Uani 1 1 d . . .
H31 H 0.6105 0.3920 0.0173 0.149 Uiso 1 1 calc R . .
C32 C 0.5019(3) 0.4558(3) 0.1640(3) 0.0862(13) Uani 1 1 d . . .
H32 H 0.5064 0.4896 0.2105 0.103 Uiso 1 1 calc R . .
C33 C -0.3145(3) 0.4369(3) 0.4505(3) 0.0920(14) Uani 1 1 d . . .
H33 H -0.3668 0.4458 0.4760 0.110 Uiso 1 1 calc R . .
C34 C -0.2428(4) 0.3901(3) 0.3374(3) 0.0960(15) Uani 1 1 d . . .
H34 H -0.2461 0.3678 0.2861 0.115 Uiso 1 1 calc R . .
C35 C -0.3174(3) 0.4030(3) 0.3751(3) 0.0908(14) Uani 1 1 d . . .
H35 H -0.3718 0.3887 0.3499 0.109 Uiso 1 1 calc R . .
C36 C -0.2345(3) 0.4577(3) 0.4886(3) 0.0999(14) Uani 1 1 d . . .
H36 H -0.2320 0.4810 0.5396 0.120 Uiso 1 1 calc R . .
C37 C -0.1566(3) 0.4429(3) 0.4488(4) 0.0992(16) Uani 1 1 d . . .
H37 H -0.1014 0.4557 0.4732 0.119 Uiso 1 1 calc R . .
C38 C 0.5725(3) 0.4477(4) 0.1172(5) 0.1187(19) Uani 1 1 d . . .
H38 H 0.6260 0.4764 0.1313 0.142 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(3) . ?
Fe1 N1 2.140(3) . ?
Fe1 N4 2.151(3) . ?
Fe1 N3 2.234(3) . ?
Fe1 N2 2.258(3) . ?
S1 C3 1.625(4) . ?
S2 C12 1.605(4) . ?
N1 C10 1.332(4) . ?
N1 C6 1.348(4) . ?
N2 C4 1.274(4) . ?
N2 C1 1.427(4) . ?
C1 C8 1.376(4) . ?
C1 C23 1.379(4) . ?
C2 C11 1.378(5) . ?
C2 C14 1.380(5) . ?
C2 N3 1.429(4) . ?
C3 N7 1.155(4) . ?
N3 C5 1.276(4) . ?
C4 C15 1.461(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.459(4) . ?
C5 H5 0.9300 . ?
N4 C26 1.328(4) . ?
N4 C15 1.341(4) . ?
N5 C12 1.155(4) . ?
C6 C18 1.376(4) . ?
C7 C9 1.373(5) . ?
C7 C8 1.384(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.360(5) . ?
C9 N10 1.636(6) . ?
C10 C20 1.380(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.366(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.358(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.394(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.381(5) . ?
C16 C19 1.365(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.162(4) . ?
N6 C21 1.536(5) . ?
C17 C27 1.339(5) . ?
C17 C28 1.348(5) . ?
C17 H17 0.9300 . ?
C18 C24 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.357(5) . ?
C19 N8 1.545(5) . ?
N9 N10 1.101(4) . ?
N9 C29 1.620(6) . ?
C20 C24 1.368(5) . ?
C20 H20 0.9300 . ?
C21 C30 1.338(6) . ?
C21 C25 1.373(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.402(5) . ?
C25 H25 0.9300 . ?
C26 C31 1.373(6) . ?
C26 H26 0.9300 . ?
C27 C30 1.363(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.338(7) . ?
C29 C37 1.385(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.356(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.370(6) . ?
C32 H32 0.9300 . ?
C33 C35 1.372(6) . ?
C33 C36 1.375(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.340(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 95.44(13) . . ?
N5 Fe1 N1 100.47(11) . . ?
N7 Fe1 N1 93.76(12) . . ?
N5 Fe1 N4 92.76(12) . . ?
N7 Fe1 N4 98.42(12) . . ?
N1 Fe1 N4 161.08(12) . . ?
N5 Fe1 N3 92.81(11) . . ?
N7 Fe1 N3 166.80(12) . . ?
N1 Fe1 N3 74.58(11) . . ?
N4 Fe1 N3 91.44(11) . . ?
N5 Fe1 N2 164.61(11) . . ?
N7 Fe1 N2 94.68(11) . . ?
N1 Fe1 N2 90.40(10) . . ?
N4 Fe1 N2 74.29(11) . . ?
N3 Fe1 N2 79.51(9) . . ?
C10 N1 C6 117.3(3) . . ?
C10 N1 Fe1 126.3(3) . . ?
C6 N1 Fe1 116.0(2) . . ?
C4 N2 C1 119.1(3) . . ?
C4 N2 Fe1 113.2(2) . . ?
C1 N2 Fe1 126.9(2) . . ?
C8 C1 C23 119.6(3) . . ?
C8 C1 N2 118.6(3) . . ?
C23 C1 N2 121.8(3) . . ?
C11 C2 C14 119.7(3) . . ?
C11 C2 N3 117.5(3) . . ?
C14 C2 N3 122.6(3) . . ?
N7 C3 S1 179.1(3) . . ?
C5 N3 C2 120.9(3) . . ?
C5 N3 Fe1 113.7(2) . . ?
C2 N3 Fe1 124.8(2) . . ?
N2 C4 C15 119.7(3) . . ?
N2 C4 H4 120.2 . . ?
C15 C4 H4 120.2 . . ?
N3 C5 C6 118.9(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C26 N4 C15 117.0(3) . . ?
C26 N4 Fe1 126.0(3) . . ?
C15 N4 Fe1 116.8(2) . . ?
C12 N5 Fe1 166.0(3) . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 115.2(3) . . ?
C18 C6 C5 122.1(3) . . ?
C9 C7 C8 119.3(3) . . ?
C9 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C1 C8 C7 119.4(3) . . ?
C1 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C13 C9 C7 121.5(3) . . ?
C13 C9 N10 110.2(4) . . ?
C7 C9 N10 128.1(4) . . ?
N1 C10 C20 123.2(4) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
C22 C11 C2 120.2(4) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
N5 C12 S2 179.6(4) . . ?
C23 C13 C9 119.1(4) . . ?
C23 C13 H13 120.5 . . ?
C9 C13 H13 120.5 . . ?
C2 C14 C16 119.3(4) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
N4 C15 C32 123.2(3) . . ?
N4 C15 C4 115.2(3) . . ?
C32 C15 C4 121.6(4) . . ?
C19 C16 C14 119.6(4) . . ?
C19 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
N8 N6 C21 106.5(4) . . ?
C27 C17 C28 120.7(4) . . ?
C27 C17 H17 119.6 . . ?
C28 C17 H17 119.6 . . ?
C3 N7 Fe1 165.3(3) . . ?
C6 C18 C24 118.9(4) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.8(4) . . ?
C22 C19 N8 112.6(4) . . ?
C16 C19 N8 126.6(4) . . ?
N6 N8 C19 107.2(4) . . ?
N10 N9 C29 99.4(5) . . ?
N9 N10 C9 96.5(5) . . ?
C24 C20 C10 118.9(4) . . ?
C24 C20 H20 120.6 . . ?
C10 C20 H20 120.6 . . ?
C30 C21 C25 120.8(4) . . ?
C30 C21 N6 114.8(4) . . ?
C25 C21 N6 124.4(5) . . ?
C19 C22 C11 120.3(4) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C13 C23 C1 121.1(3) . . ?
C13 C23 H23 119.5 . . ?
C1 C23 H23 119.5 . . ?
C20 C24 C18 119.0(4) . . ?
C20 C24 H24 120.5 . . ?
C18 C24 H24 120.5 . . ?
C21 C25 C28 118.5(4) . . ?
C21 C25 H25 120.8 . . ?
C28 C25 H25 120.8 . . ?
N4 C26 C31 122.9(5) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C17 C27 C30 120.8(5) . . ?
C17 C27 H27 119.6 . . ?
C30 C27 H27 119.6 . . ?
C17 C28 C25 119.3(4) . . ?
C17 C28 H28 120.4 . . ?
C25 C28 H28 120.4 . . ?
C34 C29 C37 121.0(4) . . ?
C34 C29 N9 111.9(6) . . ?
C37 C29 N9 126.9(6) . . ?
C21 C30 C27 119.9(4) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C38 C31 C26 119.5(5) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C38 C32 C15 118.1(5) . . ?
C38 C32 H32 121.0 . . ?
C15 C32 H32 121.0 . . ?
C35 C33 C36 120.2(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 120.8(5) . . ?
C29 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C33 120.8(5) . . ?
C34 C35 H35 119.6 . . ?
C33 C35 H35 119.6 . . ?
C33 C36 C37 118.6(5) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
C29 C37 C36 118.6(5) . . ?
C29 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C31 C38 C32 119.3(5) . . ?
C31 C38 H38 120.4 . . ?
C32 C38 H38 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        21.26
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.185
_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_znaza220km
_database_code_depnum_ccdc_archive 'CCDC 1492674'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1104(7)
_cell_length_b                   14.4217(10)
_cell_length_c                   17.1457(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.883(4)
_cell_angle_gamma                90.00
_cell_volume                     3727.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    14740
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_T_max  0.7112
_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            6360
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4875
_reflns_number_gt                4094
_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)+(0.0472P)²+5.8393P] 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         4875
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1240
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Zn01 Zn 0.71267(3) 0.28483(3) 0.44706(2) 0.04267(18) Uani 1 1 d . . .
S1 S 0.80772(7) 0.49862(8) 0.64742(6) 0.0510(3) Uani 1 1 d . . .
S2 S 0.56325(8) 0.07175(9) 0.60478(7) 0.0616(3) Uani 1 1 d . . .
N9 N 1.0897(3) 0.3954(3) 0.1862(2) 0.0664(11) Uani 1 1 d . . .
N7 N 0.7741(2) 0.3745(3) 0.5247(2) 0.0567(10) Uani 1 1 d . . .
N2 N 0.7308(2) 0.3806(2) 0.33825(16) 0.0342(7) Uani 1 1 d . . .
C29 C 1.1686(4) 0.4094(3) 0.1333(3) 0.0709(16) Uani 1 1 d . . .
N3 N 0.6721(2) 0.1888(2) 0.34308(17) 0.0381(8) Uani 1 1 d . . .
N1 N 0.8298(2) 0.2135(2) 0.42109(17) 0.0413(8) Uani 1 1 d . . .
C1 C 0.8048(3) 0.3860(2) 0.2915(2) 0.0357(9) Uani 1 1 d . . .
C3 C 0.7876(2) 0.4254(3) 0.5762(2) 0.0411(10) Uani 1 1 d . . .
N4 N 0.5908(2) 0.3599(2) 0.42670(19) 0.0484(9) Uani 1 1 d . . .
C12 C 0.6218(3) 0.1451(3) 0.5586(2) 0.0442(10) Uani 1 1 d . . .
C8 C 0.8879(3) 0.3994(3) 0.3289(2) 0.0435(10) Uani 1 1 d . . .
H8 H 0.8943 0.4056 0.3835 0.052 Uiso 1 1 calc R . .
C10 C 0.9087(3) 0.2224(3) 0.4610(2) 0.0517(11) Uani 1 1 d . . .
H10 H 0.9116 0.2556 0.5083 0.062 Uiso 1 1 calc R . .
N10 N 1.0244(3) 0.4019(3) 0.1471(3) 0.0788(14) Uani 1 1 d . . .
C15 C 0.5805(3) 0.4113(3) 0.3605(2) 0.0473(10) Uani 1 1 d . . .
C4 C 0.6579(3) 0.4194(3) 0.3148(2) 0.0416(10) Uani 1 1 d . . .
H4 H 0.6542 0.4533 0.2679 0.050 Uiso 1 1 calc R . .
C6 C 0.8275(3) 0.1643(3) 0.3533(2) 0.0401(10) Uani 1 1 d . . .
C2 C 0.5855(3) 0.1799(3) 0.3063(2) 0.0402(9) Uani 1 1 d . . .
C11 C 0.5176(3) 0.1563(3) 0.3528(2) 0.0529(11) Uani 1 1 d . . .
H11 H 0.5304 0.1434 0.4061 0.063 Uiso 1 1 calc R . .
C23 C 0.7962(3) 0.3751(3) 0.2112(2) 0.0502(11) Uani 1 1 d . . .
H23 H 0.7399 0.3646 0.1860 0.060 Uiso 1 1 calc R . .
N5 N 0.6637(3) 0.1969(3) 0.5261(2) 0.0643(11) Uani 1 1 d . . .
C13 C 0.8691(3) 0.3797(3) 0.1682(3) 0.0623(13) Uani 1 1 d . . .
H13 H 0.8627 0.3733 0.1136 0.075 Uiso 1 1 calc R . .
C18 C 0.9019(3) 0.1269(3) 0.3247(3) 0.0533(11) Uani 1 1 d . . .
H18 H 0.8982 0.0938 0.2774 0.064 Uiso 1 1 calc R . .
C9 C 0.9506(3) 0.3934(3) 0.2046(3) 0.0543(12) Uani 1 1 d . . .
C17 C 0.0340(3) 0.1148(3) 0.0772(3) 0.0555(12) Uani 1 1 d . . .
H17 H -0.0249 0.1038 0.0581 0.067 Uiso 1 1 calc R . .
C7 C 0.9614(3) 0.4035(3) 0.2853(3) 0.0520(11) Uani 1 1 d . . .
H7 H 1.0182 0.4130 0.3099 0.062 Uiso 1 1 calc R . .
N8 N 0.3137(3) 0.1612(3) 0.2217(2) 0.0665(11) Uani 1 1 d . . .
C38 C 0.4310(4) 0.4445(5) 0.3843(5) 0.095(2) Uani 1 1 d . . .
H38 H 0.3761 0.4726 0.3699 0.114 Uiso 1 1 calc R . .
C32 C 0.5014(3) 0.4534(4) 0.3374(3) 0.0690(14) Uani 1 1 d . . .
H32 H 0.4953 0.4876 0.2906 0.083 Uiso 1 1 calc R . .
C16 C 0.4784(3) 0.1950(3) 0.1974(3) 0.0597(13) Uani 1 1 d . . .
H16 H 0.4647 0.2086 0.1444 0.072 Uiso 1 1 calc R . .
C5 C 0.7381(3) 0.1528(3) 0.3138(2) 0.0416(10) Uani 1 1 d . . .
H5 H 0.7307 0.1189 0.2670 0.050 Uiso 1 1 calc R . .
C14 C 0.5659(3) 0.2007(3) 0.2284(2) 0.0508(11) Uani 1 1 d . . .
H14 H 0.6112 0.2186 0.1966 0.061 Uiso 1 1 calc R . .
C20 C 0.9853(3) 0.1856(3) 0.4362(3) 0.0638(13) Uani 1 1 d . . .
H20 H 1.0391 0.1925 0.4664 0.077 Uiso 1 1 calc R . .
C22 C 0.4314(3) 0.1516(3) 0.3214(3) 0.0615(13) Uani 1 1 d . . .
H22 H 0.3857 0.1357 0.3535 0.074 Uiso 1 1 calc R . .
C27 C 0.1014(3) 0.0972(3) 0.0315(3) 0.0626(13) Uani 1 1 d . . .
H27 H 0.0888 0.0751 -0.0196 0.075 Uiso 1 1 calc R . .
C24 C 0.9827(3) 0.1386(3) 0.3665(3) 0.0625(13) Uani 1 1 d . . .
H24 H 1.0350 0.1146 0.3476 0.075 Uiso 1 1 calc R . .
C21 C 0.2065(3) 0.1419(3) 0.1325(3) 0.0578(12) Uani 1 1 d . . .
C35 C 1.3214(4) 0.4039(4) 0.1275(3) 0.0716(15) Uani 1 1 d . . .
H35 H 1.3777 0.3897 0.1511 0.086 Uiso 1 1 calc R . .
C28 C 0.0514(3) 0.1488(3) 0.1515(3) 0.0634(13) Uani 1 1 d . . .
H28 H 0.0047 0.1625 0.1832 0.076 Uiso 1 1 calc R . .
C36 C 1.2342(4) 0.4590(4) 0.0164(4) 0.0796(16) Uani 1 1 d . . .
H36 H 1.2298 0.4832 -0.0346 0.095 Uiso 1 1 calc R . .
C26 C 0.5219(4) 0.3532(4) 0.4704(3) 0.0723(15) Uani 1 1 d . . .
H26 H 0.5286 0.3181 0.5167 0.087 Uiso 1 1 calc R . .
C19 C 0.4119(3) 0.1697(3) 0.2441(3) 0.0552(12) Uani 1 1 d . . .
N6 N 0.3044(3) 0.1521(3) 0.1531(2) 0.0669(11) Uani 1 1 d . . .
C31 C 0.4422(4) 0.3943(5) 0.4520(5) 0.0922(19) Uani 1 1 d . . .
H31 H 0.3956 0.3883 0.4853 0.111 Uiso 1 1 calc R . .
C33 C 1.3152(4) 0.4379(4) 0.0526(3) 0.0735(15) Uani 1 1 d . . .
H33 H 1.3669 0.4469 0.0260 0.088 Uiso 1 1 calc R . .
C34 C 1.2486(4) 0.3900(3) 0.1687(3) 0.0721(14) Uani 1 1 d . . .
H34 H 1.2541 0.3675 0.2202 0.087 Uiso 1 1 calc R . .
C30 C 0.1874(3) 0.1107(3) 0.0583(3) 0.0637(13) Uani 1 1 d . . .
H30 H 0.2335 0.0986 0.0256 0.076 Uiso 1 1 calc R . .
C25 C 0.1394(4) 0.1626(3) 0.1792(3) 0.0667(14) Uani 1 1 d . . .
H25 H 0.1524 0.1860 0.2299 0.080 Uiso 1 1 calc R . .
C37 C 1.1572(4) 0.4436(4) 0.0574(4) 0.0791(17) Uani 1 1 d . . .
H37 H 1.1003 0.4560 0.0341 0.095 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
Zn01 N5 2.031(4) . ?
Zn01 N7 2.035(3) . ?
Zn01 N1 2.121(3) . ?
Zn01 N4 2.144(4) . ?
Zn01 N3 2.308(3) . ?
Zn01 N2 2.352(3) . ?
S1 C3 1.627(4) . ?
S2 C12 1.619(5) . ?
N9 N10 1.159(5) . ?
N9 C29 1.558(6) . ?
N7 C3 1.155(5) . ?
N2 C4 1.275(5) . ?
N2 C1 1.421(5) . ?
C29 C34 1.346(8) . ?
C29 C37 1.392(8) . ?
N3 C5 1.259(5) . ?
N3 C2 1.420(5) . ?
N1 C10 1.340(5) . ?
N1 C6 1.360(5) . ?
C1 C8 1.384(5) . ?
C1 C23 1.384(5) . ?
N4 C26 1.327(6) . ?
N4 C15 1.356(5) . ?
C12 N5 1.149(5) . ?
C8 C7 1.382(6) . ?
C8 H8 0.9400 . ?
C10 C20 1.367(7) . ?
C10 H10 0.9400 . ?
N10 C9 1.542(6) . ?
C15 C32 1.375(6) . ?
C15 C4 1.457(6) . ?
C4 H4 0.9400 . ?
C6 C18 1.367(6) . ?
C6 C5 1.479(5) . ?
C2 C14 1.380(5) . ?
C2 C11 1.383(6) . ?
C11 C22 1.377(6) . ?
C11 H11 0.9400 . ?
C23 C13 1.367(6) . ?
C23 H23 0.9400 . ?
C13 C9 1.357(6) . ?
C13 H13 0.9400 . ?
C18 C24 1.384(6) . ?
C18 H18 0.9400 . ?
C9 C7 1.389(6) . ?
C17 C27 1.351(6) . ?
C17 C28 1.374(6) . ?
C17 H17 0.9400 . ?
C7 H7 0.9400 . ?
N8 N6 1.182(5) . ?
N8 C19 1.512(6) . ?
C38 C31 1.369(9) . ?
C38 C32 1.384(8) . ?
C38 H38 0.9400 . ?
C32 H32 0.9400 . ?
C16 C19 1.376(7) . ?
C16 C14 1.394(6) . ?
C16 H16 0.9400 . ?
C5 H5 0.9400 . ?
C14 H14 0.9400 . ?
C20 C24 1.371(7) . ?
C20 H20 0.9400 . ?
C22 C19 1.363(6) . ?
C22 H22 0.9400 . ?
C27 C30 1.362(6) . ?
C27 H27 0.9400 . ?
C24 H24 0.9400 . ?
C21 C30 1.361(7) . ?
C21 C25 1.368(7) . ?
C21 N6 1.506(6) . ?
C35 C34 1.361(7) . ?
C35 C33 1.372(7) . ?
C35 H35 0.9400 . ?
C28 C25 1.395(7) . ?
C28 H28 0.9400 . ?
C36 C33 1.368(7) . ?
C36 C37 1.418(8) . ?
C36 H36 0.9400 . ?
C26 C31 1.360(8) . ?
C26 H26 0.9400 . ?
C31 H31 0.9400 . ?
C33 H33 0.9400 . ?
C34 H34 0.9400 . ?
C30 H30 0.9400 . ?
C25 H25 0.9400 . ?
C37 H37 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 Zn01 N7 97.53(15) . . ?
N5 Zn01 N1 100.62(15) . . ?
N7 Zn01 N1 95.47(13) . . ?
N5 Zn01 N4 94.35(15) . . ?
N7 Zn01 N4 97.72(14) . . ?
N1 Zn01 N4 158.54(12) . . ?
N5 Zn01 N3 92.90(13) . . ?
N7 Zn01 N3 166.60(14) . . ?
N1 Zn01 N3 74.26(12) . . ?
N4 Zn01 N3 89.82(12) . . ?
N5 Zn01 N2 164.31(13) . . ?
N7 Zn01 N2 94.20(13) . . ?
N1 Zn01 N2 88.54(11) . . ?
N4 Zn01 N2 73.70(12) . . ?
N3 Zn01 N2 77.24(10) . . ?
N10 N9 C29 108.0(5) . . ?
C3 N7 Zn01 162.4(3) . . ?
C4 N2 C1 119.6(3) . . ?
C4 N2 Zn01 111.3(2) . . ?
C1 N2 Zn01 128.1(2) . . ?
C34 C29 C37 123.0(5) . . ?
C34 C29 N9 114.2(5) . . ?
C37 C29 N9 122.6(6) . . ?
C5 N3 C2 121.2(3) . . ?
C5 N3 Zn01 112.2(2) . . ?
C2 N3 Zn01 125.9(3) . . ?
C10 N1 C6 117.2(4) . . ?
C10 N1 Zn01 124.9(3) . . ?
C6 N1 Zn01 117.3(2) . . ?
C8 C1 C23 119.9(4) . . ?
C8 C1 N2 118.1(3) . . ?
C23 C1 N2 122.0(3) . . ?
N7 C3 S1 178.7(4) . . ?
C26 N4 C15 117.6(4) . . ?
C26 N4 Zn01 124.7(3) . . ?
C15 N4 Zn01 117.4(3) . . ?
N5 C12 S2 179.6(4) . . ?
C7 C8 C1 119.5(4) . . ?
C7 C8 H8 120.2 . . ?
C1 C8 H8 120.2 . . ?
N1 C10 C20 123.1(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
N9 N10 C9 104.4(5) . . ?
N4 C15 C32 122.1(4) . . ?
N4 C15 C4 116.3(4) . . ?
C32 C15 C4 121.6(4) . . ?
N2 C4 C15 120.2(4) . . ?
N2 C4 H4 119.9 . . ?
C15 C4 H4 119.9 . . ?
N1 C6 C18 122.5(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.6(4) . . ?
C14 C2 C11 119.5(4) . . ?
C14 C2 N3 122.7(4) . . ?
C11 C2 N3 117.5(3) . . ?
C22 C11 C2 120.3(4) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
C13 C23 C1 120.3(4) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C12 N5 Zn01 165.5(3) . . ?
C9 C13 C23 119.9(4) . . ?
C9 C13 H13 120.0 . . ?
C23 C13 H13 120.0 . . ?
C6 C18 C24 119.0(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 121.0(4) . . ?
C13 C9 N10 113.0(4) . . ?
C7 C9 N10 125.9(4) . . ?
C27 C17 C28 120.0(4) . . ?
C27 C17 H17 120.0 . . ?
C28 C17 H17 120.0 . . ?
C8 C7 C9 119.3(4) . . ?
C8 C7 H7 120.3 . . ?
C9 C7 H7 120.3 . . ?
N6 N8 C19 108.1(4) . . ?
C31 C38 C32 119.1(5) . . ?
C31 C38 H38 120.4 . . ?
C32 C38 H38 120.4 . . ?
C15 C32 C38 118.6(5) . . ?
C15 C32 H32 120.7 . . ?
C38 C32 H32 120.7 . . ?
C19 C16 C14 120.3(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N3 C5 C6 119.7(3) . . ?
N3 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C2 C14 C16 119.4(4) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
C10 C20 C24 119.3(4) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C19 C22 C11 120.5(5) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C17 C27 C30 121.2(5) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C20 C24 C18 118.9(5) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.1(4) . . ?
C30 C21 N6 113.2(5) . . ?
C25 C21 N6 126.7(4) . . ?
C34 C35 C33 122.1(5) . . ?
C34 C35 H35 118.9 . . ?
C33 C35 H35 118.9 . . ?
C17 C28 C25 119.0(5) . . ?
C17 C28 H28 120.5 . . ?
C25 C28 H28 120.5 . . ?
C33 C36 C37 118.7(5) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
N4 C26 C31 123.6(6) . . ?
N4 C26 H26 118.2 . . ?
C31 C26 H26 118.2 . . ?
C22 C19 C16 119.9(4) . . ?
C22 C19 N8 112.1(4) . . ?
C16 C19 N8 128.0(4) . . ?
N8 N6 C21 107.0(4) . . ?
C26 C31 C38 119.0(6) . . ?
C26 C31 H31 120.5 . . ?
C38 C31 H31 120.5 . . ?
C36 C33 C35 120.4(5) . . ?
C36 C33 H33 119.8 . . ?
C35 C33 H33 119.8 . . ?
C29 C34 C35 118.0(5) . . ?
C29 C34 H34 121.0 . . ?
C35 C34 H34 121.0 . . ?
C21 C30 C27 119.9(5) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C21 C25 C28 119.8(4) . . ?
C21 C25 H25 120.1 . . ?
C28 C25 H25 120.1 . . ?
C29 C37 C36 117.7(5) . . ?
C29 C37 H37 121.1 . . ?
C36 C37 H37 121.1 . . ?

_diffrn_measured_fraction_theta_max 0.741
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.741
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.051
####################################################################### 
# 
# 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_feaza290kd2
_database_code_depnum_ccdc_archive 'CCDC 1492675'
_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                   15.1213(7)
_cell_length_b                   14.5553(10)
_cell_length_c                   17.0282(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.945(4)
_cell_angle_gamma                90.00
_cell_volume                     3742.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    4285
_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    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5550
_exptl_absorpt_correction_T_max  0.8969
_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      290(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            5484
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -15
_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         21.27
_reflns_number_total             3816
_reflns_number_gt                2977
_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)+(0.0271P)²+1.9331P] 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         3816
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0888
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.29221(3) 0.28763(3) 0.05533(3) 0.0585(2) Uani 1 1 d . . .
S1 S 0.18853(6) 0.49648(7) -0.14667(6) 0.0741(3) Uani 1 1 d . . .
S2 S 0.43674(7) 0.07273(7) -0.10654(7) 0.0839(4) Uani 1 1 d . . .
N1 N 0.17227(19) 0.21596(18) 0.07807(18) 0.0581(7) Uani 1 1 d . . .
N2 N 0.27371(17) 0.37970(17) 0.16051(15) 0.0473(7) Uani 1 1 d . . .
C1 C 0.1977(2) 0.3848(2) 0.2065(2) 0.0483(8) Uani 1 1 d . . .
C2 C 0.4139(2) 0.1805(2) 0.1913(2) 0.0564(9) Uani 1 1 d . . .
C3 C 0.2138(2) 0.4255(3) -0.0752(2) 0.0582(10) Uani 1 1 d . . .
N3 N 0.3279(2) 0.19049(17) 0.15387(16) 0.0536(7) Uani 1 1 d . . .
C4 C 0.3445(2) 0.4198(2) 0.1853(2) 0.0582(9) Uani 1 1 d . . .
H4 H 0.3457 0.4537 0.2317 0.070 Uiso 1 1 calc R . .
C5 C 0.2614(3) 0.1525(2) 0.1830(2) 0.0599(9) Uani 1 1 d . . .
H5 H 0.2684 0.1173 0.2285 0.072 Uiso 1 1 calc R . .
N4 N 0.41547(17) 0.3611(2) 0.07506(19) 0.0648(8) Uani 1 1 d . . .
N5 N 0.3433(2) 0.2028(2) -0.02725(19) 0.0842(10) Uani 1 1 d . . .
C6 C 0.1735(2) 0.1648(2) 0.1440(2) 0.0551(9) Uani 1 1 d . . .
C7 C 0.0408(2) 0.4031(2) 0.2115(3) 0.0721(11) Uani 1 1 d . . .
H7 H -0.0145 0.4128 0.1863 0.086 Uiso 1 1 calc R . .
C8 C 0.1163(2) 0.3993(2) 0.1688(2) 0.0602(10) Uani 1 1 d . . .
H8 H 0.1120 0.4067 0.1144 0.072 Uiso 1 1 calc R . .
C9 C 0.0490(3) 0.3925(2) 0.2910(3) 0.0784(13) Uani 1 1 d . . .
C10 C 0.0948(3) 0.2253(2) 0.0380(2) 0.0745(11) Uani 1 1 d . . .
H10 H 0.0929 0.2589 -0.0085 0.089 Uiso 1 1 calc R . .
C11 C 0.4818(3) 0.1575(2) 0.1444(2) 0.0722(11) Uani 1 1 d . . .
H11 H 0.4699 0.1455 0.0913 0.087 Uiso 1 1 calc R . .
C12 C 0.3824(2) 0.1484(3) -0.0603(2) 0.0597(10) Uani 1 1 d . . .
C13 C 0.1291(3) 0.3779(3) 0.3289(2) 0.0837(12) Uani 1 1 d . . .
H13 H 0.1333 0.3707 0.3832 0.100 Uiso 1 1 calc R . .
C14 C 0.4322(3) 0.2003(2) 0.2698(2) 0.0713(11) Uani 1 1 d . . .
H14 H 0.3871 0.2173 0.3020 0.086 Uiso 1 1 calc R . .
C15 C 0.4239(2) 0.4120(2) 0.1402(2) 0.0601(10) Uani 1 1 d . . .
C16 C 0.5198(3) 0.1944(3) 0.3001(3) 0.0818(12) Uani 1 1 d . . .
H16 H 0.5330 0.2071 0.3529 0.098 Uiso 1 1 calc R . .
N6 N 0.6906(3) 0.1542(2) 0.3426(3) 0.1017(13) Uani 1 1 d . . .
C17 C 0.9617(3) 0.1178(3) 0.4185(3) 0.0839(12) Uani 1 1 d . . .
H17 H 1.0197 0.1077 0.4376 0.101 Uiso 1 1 calc R . .
N7 N 0.2310(2) 0.3758(2) -0.0239(2) 0.0796(10) Uani 1 1 d . . .
C18 C 0.0986(3) 0.1255(2) 0.1718(2) 0.0741(11) Uani 1 1 d . . .
H18 H 0.1017 0.0914 0.2181 0.089 Uiso 1 1 calc R . .
C19 C 0.5859(3) 0.1702(3) 0.2526(3) 0.0769(12) Uani 1 1 d . . .
N8 N 0.6873(3) 0.1617(2) 0.2758(2) 0.0904(11) Uani 1 1 d . . .
N9 N -0.0831(3) 0.3954(2) 0.3131(2) 0.0989(13) Uani 1 1 d . . .
N10 N -0.0280(3) 0.4022(2) 0.3562(3) 0.1143(16) Uani 1 1 d . . .
C20 C 0.0168(3) 0.1871(3) 0.0625(3) 0.0893(13) Uani 1 1 d . . .
H20 H -0.0361 0.1955 0.0331 0.107 Uiso 1 1 calc R . .
C21 C 0.7921(2) 0.1430(3) 0.3647(4) 0.0824(14) Uani 1 1 d . . .
C22 C 0.5672(3) 0.1521(3) 0.1756(3) 0.0816(12) Uani 1 1 d . . .
H22 H 0.6126 0.1358 0.1435 0.098 Uiso 1 1 calc R . .
C23 C 0.2029(2) 0.3740(3) 0.2869(2) 0.0695(10) Uani 1 1 d . . .
H23 H 0.2577 0.3638 0.3128 0.083 Uiso 1 1 calc R . .
C24 C 0.0189(3) 0.1375(3) 0.1301(3) 0.0881(13) Uani 1 1 d . . .
H24 H -0.0327 0.1118 0.1479 0.106 Uiso 1 1 calc R . .
C25 C 0.8585(3) 0.1610(3) 0.3149(3) 0.0946(14) Uani 1 1 d . . .
H25 H 0.8460 0.1808 0.2636 0.114 Uiso 1 1 calc R . .
C26 C 0.4854(3) 0.3549(3) 0.0316(3) 0.0998(14) Uani 1 1 d . . .
H26 H 0.4810 0.3199 -0.0141 0.120 Uiso 1 1 calc R . .
C27 C 0.8956(3) 0.1021(3) 0.4647(3) 0.1007(15) Uani 1 1 d . . .
H27 H 0.9080 0.0821 0.5159 0.121 Uiso 1 1 calc R . .
C28 C 0.9463(3) 0.1481(3) 0.3444(4) 0.0931(14) Uani 1 1 d . . .
H28 H 0.9934 0.1605 0.3130 0.112 Uiso 1 1 calc R . .
C29 C -0.1628(4) 0.4090(3) 0.3736(4) 0.106(2) Uani 1 1 d . . .
C30 C 0.8103(3) 0.1147(3) 0.4389(4) 0.1062(16) Uani 1 1 d . . .
H30 H 0.7646 0.1038 0.4723 0.127 Uiso 1 1 calc R . .
C31 C 0.5645(4) 0.3982(5) 0.0514(5) 0.136(2) Uani 1 1 d . . .
H31 H 0.6116 0.3935 0.0187 0.163 Uiso 1 1 calc R . .
C32 C 0.5019(3) 0.4555(3) 0.1646(3) 0.0942(14) Uani 1 1 d . . .
H32 H 0.5058 0.4893 0.2110 0.113 Uiso 1 1 calc R . .
C33 C -0.3138(3) 0.4367(3) 0.4509(3) 0.0991(15) Uani 1 1 d . . .
H33 H -0.3663 0.4457 0.4761 0.119 Uiso 1 1 calc R . .
C34 C -0.2416(4) 0.3903(3) 0.3379(3) 0.1028(16) Uani 1 1 d . . .
H34 H -0.2448 0.3683 0.2865 0.123 Uiso 1 1 calc R . .
C35 C -0.3163(3) 0.4033(3) 0.3762(3) 0.0987(15) Uani 1 1 d . . .
H35 H -0.3706 0.3891 0.3511 0.118 Uiso 1 1 calc R . .
C36 C -0.2341(4) 0.4573(3) 0.4891(3) 0.1090(15) Uani 1 1 d . . .
H36 H -0.2316 0.4802 0.5401 0.131 Uiso 1 1 calc R . .
C37 C -0.1563(3) 0.4429(3) 0.4490(4) 0.1079(17) Uani 1 1 d . . .
H37 H -0.1013 0.4562 0.4731 0.129 Uiso 1 1 calc R . .
C38 C 0.5732(3) 0.4476(4) 0.1185(5) 0.132(2) Uani 1 1 d . . .
H38 H 0.6267 0.4758 0.1331 0.158 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 2.049(3) . ?
Fe1 N5 2.052(4) . ?
Fe1 N1 2.145(3) . ?
Fe1 N4 2.160(3) . ?
Fe1 N3 2.239(3) . ?
Fe1 N2 2.266(3) . ?
S1 C3 1.626(4) . ?
S2 C12 1.605(4) . ?
N1 C10 1.332(4) . ?
N1 C6 1.346(4) . ?
N2 C4 1.272(4) . ?
N2 C1 1.426(4) . ?
C1 C8 1.374(4) . ?
C1 C23 1.377(4) . ?
C2 C11 1.374(5) . ?
C2 C14 1.382(5) . ?
C2 N3 1.426(4) . ?
C3 N7 1.154(4) . ?
N3 C5 1.271(4) . ?
C4 C15 1.462(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.467(5) . ?
C5 H5 0.9300 . ?
N4 C26 1.325(4) . ?
N4 C15 1.335(4) . ?
N5 C12 1.152(4) . ?
C6 C18 1.374(5) . ?
C7 C9 1.364(5) . ?
C7 C8 1.386(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.359(5) . ?
C9 N10 1.654(6) . ?
C10 C20 1.387(5) . ?
C10 H10 0.9300 . ?
C11 C22 1.373(5) . ?
C11 H11 0.9300 . ?
C13 C23 1.357(5) . ?
C13 H13 0.9300 . ?
C14 C16 1.398(5) . ?
C14 H14 0.9300 . ?
C15 C32 1.384(5) . ?
C16 C19 1.365(5) . ?
C16 H16 0.9300 . ?
N6 N8 1.140(4) . ?
N6 C21 1.570(5) . ?
C17 C27 1.323(6) . ?
C17 C28 1.346(6) . ?
C17 H17 0.9300 . ?
C18 C24 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C22 1.353(5) . ?
C19 N8 1.568(5) . ?
N9 N10 1.086(4) . ?
N9 C29 1.637(6) . ?
C20 C24 1.357(6) . ?
C20 H20 0.9300 . ?
C21 C30 1.345(6) . ?
C21 C25 1.372(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C28 1.409(5) . ?
C25 H25 0.9300 . ?
C26 C31 1.379(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.353(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C34 1.338(7) . ?
C29 C37 1.374(7) . ?
C30 H30 0.9300 . ?
C31 C38 1.350(7) . ?
C31 H31 0.9300 . ?
C32 C38 1.372(7) . ?
C32 H32 0.9300 . ?
C33 C35 1.360(6) . ?
C33 C36 1.374(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.346(6) . ?
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
N7 Fe1 N5 95.65(13) . . ?
N7 Fe1 N1 93.79(12) . . ?
N5 Fe1 N1 100.50(12) . . ?
N7 Fe1 N4 98.59(12) . . ?
N5 Fe1 N4 93.01(13) . . ?
N1 Fe1 N4 160.67(12) . . ?
N7 Fe1 N3 166.59(12) . . ?
N5 Fe1 N3 92.80(11) . . ?
N1 Fe1 N3 74.40(12) . . ?
N4 Fe1 N3 91.33(11) . . ?
N7 Fe1 N2 94.62(11) . . ?
N5 Fe1 N2 164.55(12) . . ?
N1 Fe1 N2 90.29(10) . . ?
N4 Fe1 N2 74.03(11) . . ?
N3 Fe1 N2 79.39(9) . . ?
C10 N1 C6 117.2(3) . . ?
C10 N1 Fe1 126.0(3) . . ?
C6 N1 Fe1 116.4(2) . . ?
C4 N2 C1 118.8(3) . . ?
C4 N2 Fe1 113.5(2) . . ?
C1 N2 Fe1 126.9(2) . . ?
C8 C1 C23 119.2(3) . . ?
C8 C1 N2 118.6(3) . . ?
C23 C1 N2 122.2(3) . . ?
C11 C2 C14 119.7(3) . . ?
C11 C2 N3 117.2(3) . . ?
C14 C2 N3 122.9(3) . . ?
N7 C3 S1 179.2(4) . . ?
C5 N3 C2 120.2(3) . . ?
C5 N3 Fe1 113.7(2) . . ?
C2 N3 Fe1 125.3(2) . . ?
N2 C4 C15 119.3(3) . . ?
N2 C4 H4 120.4 . . ?
C15 C4 H4 120.4 . . ?
N3 C5 C6 119.1(3) . . ?
N3 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C26 N4 C15 117.3(4) . . ?
C26 N4 Fe1 125.9(3) . . ?
C15 N4 Fe1 116.6(2) . . ?
C12 N5 Fe1 165.7(3) . . ?
N1 C6 C18 122.8(3) . . ?
N1 C6 C5 114.7(3) . . ?
C18 C6 C5 122.4(4) . . ?
C9 C7 C8 118.8(3) . . ?
C9 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C1 C8 C7 120.1(4) . . ?
C1 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C13 C9 C7 121.5(3) . . ?
C13 C9 N10 109.6(4) . . ?
C7 C9 N10 128.7(4) . . ?
N1 C10 C20 123.0(4) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
C22 C11 C2 120.3(4) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
N5 C12 S2 179.8(4) . . ?
C23 C13 C9 119.6(4) . . ?
C23 C13 H13 120.2 . . ?
C9 C13 H13 120.2 . . ?
C2 C14 C16 118.9(4) . . ?
C2 C14 H14 120.6 . . ?
C16 C14 H14 120.6 . . ?
N4 C15 C32 123.1(4) . . ?
N4 C15 C4 115.7(3) . . ?
C32 C15 C4 121.1(4) . . ?
C19 C16 C14 120.4(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N8 N6 C21 104.0(4) . . ?
C27 C17 C28 120.9(4) . . ?
C27 C17 H17 119.5 . . ?
C28 C17 H17 119.5 . . ?
C3 N7 Fe1 165.6(3) . . ?
C6 C18 C24 118.9(4) . . ?
C6 C18 H18 120.6 . . ?
C24 C18 H18 120.6 . . ?
C22 C19 C16 120.1(4) . . ?
C22 C19 N8 112.5(4) . . ?
C16 C19 N8 127.4(4) . . ?
N6 N8 C19 104.6(4) . . ?
N10 N9 C29 97.4(5) . . ?
N9 N10 C9 94.7(5) . . ?
C24 C20 C10 119.0(4) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C30 C21 C25 121.2(4) . . ?
C30 C21 N6 114.1(5) . . ?
C25 C21 N6 124.7(5) . . ?
C19 C22 C11 120.7(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C13 C23 C1 120.8(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 117.5(5) . . ?
C21 C25 H25 121.3 . . ?
C28 C25 H25 121.3 . . ?
N4 C26 C31 122.6(5) . . ?
N4 C26 H26 118.7 . . ?
C31 C26 H26 118.7 . . ?
C17 C27 C30 121.4(5) . . ?
C17 C27 H27 119.3 . . ?
C30 C27 H27 119.3 . . ?
C17 C28 C25 119.5(4) . . ?
C17 C28 H28 120.2 . . ?
C25 C28 H28 120.2 . . ?
C34 C29 C37 121.1(4) . . ?
C34 C29 N9 110.9(6) . . ?
C37 C29 N9 127.7(6) . . ?
C21 C30 C27 119.4(5) . . ?
C21 C30 H30 120.3 . . ?
C27 C30 H30 120.3 . . ?
C38 C31 C26 119.8(5) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C38 C32 C15 118.2(5) . . ?
C38 C32 H32 120.9 . . ?
C15 C32 H32 120.9 . . ?
C35 C33 C36 120.1(4) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 120.1(5) . . ?
C29 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C33 121.3(5) . . ?
C34 C35 H35 119.3 . . ?
C33 C35 H35 119.3 . . ?
C33 C36 C37 118.3(5) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
C29 C37 C36 119.1(5) . . ?
C29 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C31 C38 C32 118.9(5) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?

_diffrn_measured_fraction_theta_max 0.915
_diffrn_reflns_theta_full        21.27
_diffrn_measured_fraction_theta_full 0.915
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.032
####################################################################### 
# 
# 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_znaza260km
_database_code_depnum_ccdc_archive 'CCDC 1492676'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1221(7)
_cell_length_b                   14.5091(11)
_cell_length_c                   17.1448(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.707(4)
_cell_angle_gamma                90.00
_cell_volume                     3753.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    14220
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6431
_exptl_absorpt_correction_T_max  0.7128
_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      260(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            6395
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4922
_reflns_number_gt                3973
_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)+(0.0589P)²+3.6844P] 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         4922
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1352
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Zn01 Zn 0.71069(3) 0.28521(3) 0.44743(2) 0.0534(2) Uani 1 1 d . . .
S1 S 0.80776(7) 0.49697(9) 0.64726(6) 0.0633(3) Uani 1 1 d . . .
S2 S 0.56375(9) 0.07178(10) 0.60526(7) 0.0758(4) Uani 1 1 d . . .
N9 N 1.0865(4) 0.3956(3) 0.1867(3) 0.0858(13) Uani 1 1 d . . .
N7 N 0.7719(2) 0.3747(3) 0.5250(2) 0.0697(10) Uani 1 1 d . . .
N2 N 0.7304(2) 0.3806(2) 0.33839(17) 0.0434(7) Uani 1 1 d . . .
C29 C 1.1678(5) 0.4099(4) 0.1317(4) 0.093(2) Uani 1 1 d . . .
N3 N 0.6700(2) 0.1893(2) 0.34372(17) 0.0471(8) Uani 1 1 d . . .
N1 N 0.8281(2) 0.2138(2) 0.42192(18) 0.0520(8) Uani 1 1 d . . .
C1 C 0.8055(2) 0.3861(2) 0.2922(2) 0.0435(9) Uani 1 1 d . . .
C3 C 0.7861(2) 0.4251(3) 0.5760(2) 0.0521(10) Uani 1 1 d . . .
N4 N 0.5895(2) 0.3600(2) 0.4257(2) 0.0593(9) Uani 1 1 d . . .
C12 C 0.6207(3) 0.1460(3) 0.5592(2) 0.0534(10) Uani 1 1 d . . .
C8 C 0.8873(3) 0.3987(3) 0.3300(2) 0.0534(10) Uani 1 1 d . . .
H8 H 0.8931 0.4044 0.3841 0.064 Uiso 1 1 calc R . .
C10 C 0.9059(3) 0.2227(3) 0.4622(3) 0.0652(12) Uani 1 1 d . . .
H10 H 0.9083 0.2554 0.5090 0.078 Uiso 1 1 calc R . .
N10 N 1.0259(4) 0.4025(3) 0.1456(3) 0.1017(17) Uani 1 1 d . . .
C15 C 0.5801(3) 0.4112(3) 0.3599(3) 0.0568(11) Uani 1 1 d . . .
C4 C 0.6579(3) 0.4191(3) 0.3147(2) 0.0521(10) Uani 1 1 d . . .
H4 H 0.6547 0.4523 0.2682 0.063 Uiso 1 1 calc R . .
C6 C 0.8257(3) 0.1648(3) 0.3549(2) 0.0490(10) Uani 1 1 d . . .
C2 C 0.5847(3) 0.1801(3) 0.3060(2) 0.0498(10) Uani 1 1 d . . .
C11 C 0.5167(3) 0.1566(3) 0.3521(3) 0.0654(12) Uani 1 1 d . . .
H11 H 0.5288 0.1443 0.4050 0.078 Uiso 1 1 calc R . .
C23 C 0.7974(3) 0.3757(3) 0.2120(2) 0.0632(12) Uani 1 1 d . . .
H23 H 0.7419 0.3654 0.1869 0.076 Uiso 1 1 calc R . .
N5 N 0.6610(3) 0.1984(3) 0.5264(2) 0.0774(12) Uani 1 1 d . . .
C13 C 0.8704(4) 0.3802(4) 0.1695(3) 0.0777(14) Uani 1 1 d . . .
H13 H 0.8647 0.3744 0.1154 0.093 Uiso 1 1 calc R . .
C18 C 0.8999(3) 0.1269(3) 0.3267(3) 0.0664(12) Uani 1 1 d . . .
H18 H 0.8963 0.0938 0.2801 0.080 Uiso 1 1 calc R . .
C9 C 0.9518(4) 0.3933(3) 0.2065(3) 0.0689(14) Uani 1 1 d . . .
C17 C 0.0343(3) 0.1150(3) 0.0776(3) 0.0683(13) Uani 1 1 d . . .
H17 H -0.0235 0.1044 0.0579 0.082 Uiso 1 1 calc R . .
C7 C 0.9611(3) 0.4027(3) 0.2866(3) 0.0654(12) Uani 1 1 d . . .
H7 H 1.0170 0.4116 0.3114 0.078 Uiso 1 1 calc R . .
N8 N 0.3108(3) 0.1607(3) 0.2213(3) 0.0858(13) Uani 1 1 d . . .
C38 C 0.4307(4) 0.4460(5) 0.3828(5) 0.111(2) Uani 1 1 d . . .
H38 H 0.3770 0.4744 0.3685 0.133 Uiso 1 1 calc R . .
C32 C 0.5015(4) 0.4539(4) 0.3367(4) 0.0848(15) Uani 1 1 d . . .
H32 H 0.4963 0.4875 0.2905 0.102 Uiso 1 1 calc R . .
C16 C 0.4796(4) 0.1950(3) 0.1972(3) 0.0752(15) Uani 1 1 d . . .
H16 H 0.4669 0.2084 0.1447 0.090 Uiso 1 1 calc R . .
C5 C 0.7364(3) 0.1534(3) 0.3154(2) 0.0525(10) Uani 1 1 d . . .
H5 H 0.7294 0.1194 0.2694 0.063 Uiso 1 1 calc R . .
C14 C 0.5662(3) 0.2007(3) 0.2285(2) 0.0619(12) Uani 1 1 d . . .
H14 H 0.6114 0.2183 0.1973 0.074 Uiso 1 1 calc R . .
C20 C 0.9827(3) 0.1857(4) 0.4376(3) 0.0771(14) Uani 1 1 d . . .
H20 H 1.0358 0.1926 0.4676 0.093 Uiso 1 1 calc R . .
C22 C 0.4311(3) 0.1513(3) 0.3200(3) 0.0769(14) Uani 1 1 d . . .
H22 H 0.3857 0.1350 0.3513 0.092 Uiso 1 1 calc R . .
C27 C 0.1027(4) 0.0974(4) 0.0329(3) 0.0808(15) Uani 1 1 d . . .
H27 H 0.0912 0.0755 -0.0177 0.097 Uiso 1 1 calc R . .
C24 C 0.9806(3) 0.1385(4) 0.3684(3) 0.0773(14) Uani 1 1 d . . .
H24 H 1.0323 0.1148 0.3498 0.093 Uiso 1 1 calc R . .
C21 C 0.2056(3) 0.1420(3) 0.1338(4) 0.0735(14) Uani 1 1 d . . .
C35 C 1.3198(4) 0.4040(4) 0.1270(4) 0.0902(17) Uani 1 1 d . . .
H35 H 1.3751 0.3900 0.1510 0.108 Uiso 1 1 calc R . .
C28 C 0.0498(3) 0.1482(4) 0.1514(3) 0.0794(14) Uani 1 1 d . . .
H28 H 0.0031 0.1619 0.1822 0.095 Uiso 1 1 calc R . .
C36 C 1.2338(4) 0.4590(4) 0.0151(4) 0.0976(18) Uani 1 1 d . . .
H36 H 1.2297 0.4827 -0.0354 0.117 Uiso 1 1 calc R . .
C26 C 0.5197(4) 0.3539(4) 0.4690(3) 0.0882(16) Uani 1 1 d . . .
H26 H 0.5251 0.3193 0.5147 0.106 Uiso 1 1 calc R . .
C19 C 0.4122(3) 0.1698(3) 0.2428(3) 0.0695(14) Uani 1 1 d . . .
N6 N 0.3061(3) 0.1527(3) 0.1545(3) 0.0891(13) Uani 1 1 d . . .
C31 C 0.4408(4) 0.3960(5) 0.4495(5) 0.112(2) Uani 1 1 d . . .
H31 H 0.3941 0.3904 0.4819 0.135 Uiso 1 1 calc R . .
C33 C 1.3156(4) 0.4380(4) 0.0520(4) 0.0914(17) Uani 1 1 d . . .
H33 H 1.3672 0.4469 0.0263 0.110 Uiso 1 1 calc R . .
C34 C 1.2471(5) 0.3901(4) 0.1672(4) 0.0935(17) Uani 1 1 d . . .
H34 H 1.2519 0.3676 0.2181 0.112 Uiso 1 1 calc R . .
C30 C 0.1876(3) 0.1112(4) 0.0605(3) 0.0812(15) Uani 1 1 d . . .
H30 H 0.2337 0.0993 0.0286 0.097 Uiso 1 1 calc R . .
C25 C 0.1385(4) 0.1614(4) 0.1801(3) 0.0848(16) Uani 1 1 d . . .
H25 H 0.1509 0.1833 0.2306 0.102 Uiso 1 1 calc R . .
C37 C 1.1574(4) 0.4438(4) 0.0553(5) 0.098(2) Uani 1 1 d . . .
H37 H 1.1014 0.4559 0.0318 0.118 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
Zn01 N5 2.029(4) . ?
Zn01 N7 2.037(4) . ?
Zn01 N1 2.125(3) . ?
Zn01 N4 2.142(4) . ?
Zn01 N3 2.310(3) . ?
Zn01 N2 2.360(3) . ?
S1 C3 1.624(4) . ?
S2 C12 1.616(5) . ?
N9 N10 1.125(5) . ?
N9 C29 1.611(7) . ?
N7 C3 1.150(5) . ?
N2 C4 1.272(5) . ?
N2 C1 1.428(5) . ?
C29 C34 1.341(9) . ?
C29 C37 1.399(9) . ?
N3 C5 1.257(5) . ?
N3 C2 1.412(5) . ?
N1 C10 1.333(5) . ?
N1 C6 1.350(5) . ?
C1 C8 1.372(5) . ?
C1 C23 1.381(5) . ?
N4 C26 1.333(6) . ?
N4 C15 1.350(5) . ?
C12 N5 1.145(5) . ?
C8 C7 1.381(6) . ?
C8 H8 0.9300 . ?
C10 C20 1.371(7) . ?
C10 H10 0.9300 . ?
N10 C9 1.586(7) . ?
C15 C32 1.376(6) . ?
C15 C4 1.455(6) . ?
C4 H4 0.9300 . ?
C6 C18 1.366(6) . ?
C6 C5 1.480(5) . ?
C2 C14 1.373(5) . ?
C2 C11 1.380(6) . ?
C11 C22 1.375(6) . ?
C11 H11 0.9300 . ?
C23 C13 1.364(6) . ?
C23 H23 0.9300 . ?
C13 C9 1.360(7) . ?
C13 H13 0.9300 . ?
C18 C24 1.384(6) . ?
C18 H18 0.9300 . ?
C9 C7 1.379(6) . ?
C17 C27 1.350(7) . ?
C17 C28 1.360(7) . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
N8 N6 1.149(5) . ?
N8 C19 1.559(6) . ?
C38 C31 1.355(9) . ?
C38 C32 1.376(8) . ?
C38 H38 0.9300 . ?
C32 H32 0.9300 . ?
C16 C19 1.373(7) . ?
C16 C14 1.385(6) . ?
C16 H16 0.9300 . ?
C5 H5 0.9300 . ?
C14 H14 0.9300 . ?
C20 C24 1.368(7) . ?
C20 H20 0.9300 . ?
C22 C19 1.363(7) . ?
C22 H22 0.9300 . ?
C27 C30 1.355(7) . ?
C27 H27 0.9300 . ?
C24 H24 0.9300 . ?
C21 C30 1.345(7) . ?
C21 C25 1.358(8) . ?
C21 N6 1.546(7) . ?
C35 C34 1.350(8) . ?
C35 C33 1.374(8) . ?
C35 H35 0.9300 . ?
C28 C25 1.411(7) . ?
C28 H28 0.9300 . ?
C36 C33 1.387(8) . ?
C36 C37 1.400(8) . ?
C36 H36 0.9300 . ?
C26 C31 1.362(8) . ?
C26 H26 0.9300 . ?
C31 H31 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C25 H25 0.9300 . ?
C37 H37 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Zn01 N7 97.60(16) . . ?
N5 Zn01 N1 100.67(16) . . ?
N7 Zn01 N1 95.46(14) . . ?
N5 Zn01 N4 94.64(16) . . ?
N7 Zn01 N4 97.93(14) . . ?
N1 Zn01 N4 158.11(13) . . ?
N5 Zn01 N3 92.77(14) . . ?
N7 Zn01 N3 166.76(14) . . ?
N1 Zn01 N3 74.46(12) . . ?
N4 Zn01 N3 89.36(13) . . ?
N5 Zn01 N2 164.51(14) . . ?
N7 Zn01 N2 93.90(13) . . ?
N1 Zn01 N2 88.47(12) . . ?
N4 Zn01 N2 73.45(12) . . ?
N3 Zn01 N2 77.54(10) . . ?
N10 N9 C29 104.1(6) . . ?
C3 N7 Zn01 163.0(4) . . ?
C4 N2 C1 119.8(3) . . ?
C4 N2 Zn01 111.1(3) . . ?
C1 N2 Zn01 128.1(2) . . ?
C34 C29 C37 122.9(5) . . ?
C34 C29 N9 113.6(6) . . ?
C37 C29 N9 123.4(7) . . ?
C5 N3 C2 120.9(3) . . ?
C5 N3 Zn01 111.6(2) . . ?
C2 N3 Zn01 126.9(3) . . ?
C10 N1 C6 117.8(4) . . ?
C10 N1 Zn01 124.6(3) . . ?
C6 N1 Zn01 117.1(2) . . ?
C8 C1 C23 120.3(4) . . ?
C8 C1 N2 118.1(3) . . ?
C23 C1 N2 121.5(3) . . ?
N7 C3 S1 178.9(4) . . ?
C26 N4 C15 117.3(4) . . ?
C26 N4 Zn01 124.7(4) . . ?
C15 N4 Zn01 117.8(3) . . ?
N5 C12 S2 179.8(5) . . ?
C1 C8 C7 119.1(4) . . ?
C1 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
N1 C10 C20 122.6(4) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
N9 N10 C9 99.3(5) . . ?
N4 C15 C32 122.1(4) . . ?
N4 C15 C4 116.3(4) . . ?
C32 C15 C4 121.6(5) . . ?
N2 C4 C15 120.3(4) . . ?
N2 C4 H4 119.8 . . ?
C15 C4 H4 119.8 . . ?
N1 C6 C18 122.4(4) . . ?
N1 C6 C5 114.9(4) . . ?
C18 C6 C5 122.6(4) . . ?
C14 C2 C11 119.8(4) . . ?
C14 C2 N3 123.1(4) . . ?
C11 C2 N3 116.9(3) . . ?
C22 C11 C2 120.0(4) . . ?
C22 C11 H11 120.0 . . ?
C2 C11 H11 120.0 . . ?
C13 C23 C1 120.2(4) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C12 N5 Zn01 166.5(4) . . ?
C9 C13 C23 119.8(4) . . ?
C9 C13 H13 120.1 . . ?
C23 C13 H13 120.1 . . ?
C6 C18 C24 119.0(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.6(4) . . ?
C13 C9 N10 111.1(4) . . ?
C7 C9 N10 128.1(5) . . ?
C27 C17 C28 120.2(4) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C9 C7 C8 119.9(4) . . ?
C9 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
N6 N8 C19 103.9(5) . . ?
C31 C38 C32 118.7(6) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?
C38 C32 C15 119.1(6) . . ?
C38 C32 H32 120.4 . . ?
C15 C32 H32 120.4 . . ?
C19 C16 C14 121.0(4) . . ?
C19 C16 H16 119.5 . . ?
C14 C16 H16 119.5 . . ?
N3 C5 C6 120.3(3) . . ?
N3 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C2 C14 C16 119.3(4) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
C24 C20 C10 119.4(4) . . ?
C24 C20 H20 120.3 . . ?
C10 C20 H20 120.3 . . ?
C19 C22 C11 120.8(5) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C17 C27 C30 121.1(5) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C20 C24 C18 118.6(5) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C30 C21 C25 120.1(4) . . ?
C30 C21 N6 112.6(5) . . ?
C25 C21 N6 127.3(5) . . ?
C34 C35 C33 122.8(6) . . ?
C34 C35 H35 118.6 . . ?
C33 C35 H35 118.6 . . ?
C17 C28 C25 118.3(5) . . ?
C17 C28 H28 120.8 . . ?
C25 C28 H28 120.8 . . ?
C33 C36 C37 118.7(6) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
N4 C26 C31 123.1(6) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C22 C19 C16 119.2(4) . . ?
C22 C19 N8 110.7(5) . . ?
C16 C19 N8 130.1(4) . . ?
N8 N6 C21 103.6(5) . . ?
C38 C31 C26 119.8(6) . . ?
C38 C31 H31 120.1 . . ?
C26 C31 H31 120.1 . . ?
C35 C33 C36 119.5(5) . . ?
C35 C33 H33 120.3 . . ?
C36 C33 H33 120.3 . . ?
C29 C34 C35 118.1(6) . . ?
C29 C34 H34 121.0 . . ?
C35 C34 H34 121.0 . . ?
C21 C30 C27 120.4(5) . . ?
C21 C30 H30 119.8 . . ?
C27 C30 H30 119.8 . . ?
C21 C25 C28 119.9(5) . . ?
C21 C25 H25 120.1 . . ?
C28 C25 H25 120.1 . . ?
C29 C37 C36 118.0(6) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?

_diffrn_measured_fraction_theta_max 0.744
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.744
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.047
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_znaza180km
_database_code_depnum_ccdc_archive 'CCDC 1492677'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1005(6)
_cell_length_b                   14.3391(10)
_cell_length_c                   17.1470(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.050(4)
_cell_angle_gamma                90.00
_cell_volume                     3703.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    14666
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_T_max  0.7097
_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            6250
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4818
_reflns_number_gt                4200
_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)+(0.0523P)²+5.7779P] 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         4818
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1167
_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
Zn01 Zn 0.71489(3) 0.28423(3) 0.44667(2) 0.03650(17) Uani 1 1 d . . .
S1 S 0.80760(7) 0.50008(8) 0.64743(5) 0.0437(3) Uani 1 1 d . . .
S2 S 0.56278(8) 0.07217(8) 0.60424(6) 0.0519(3) Uani 1 1 d . . .
N9 N 1.0920(3) 0.3954(2) 0.1856(2) 0.0520(9) Uani 1 1 d . . .
N7 N 0.7768(2) 0.3742(2) 0.52460(18) 0.0482(9) Uani 1 1 d . . .
N2 N 0.7310(2) 0.3811(2) 0.33847(15) 0.0307(7) Uani 1 1 d . . .
C29 C 1.1684(3) 0.4097(3) 0.1346(3) 0.0534(12) Uani 1 1 d . . .
N3 N 0.6735(2) 0.1880(2) 0.34274(16) 0.0330(7) Uani 1 1 d . . .
N1 N 0.8321(2) 0.2132(2) 0.41993(17) 0.0371(8) Uani 1 1 d . . .
C1 C 0.8047(2) 0.3865(2) 0.29136(19) 0.0312(8) Uani 1 1 d . . .
C3 C 0.7889(2) 0.4262(3) 0.5762(2) 0.0367(9) Uani 1 1 d . . .
N4 N 0.5923(2) 0.3593(2) 0.42746(18) 0.0417(8) Uani 1 1 d . . .
C12 C 0.6235(3) 0.1442(3) 0.55839(19) 0.0374(9) Uani 1 1 d . . .
C8 C 0.8886(2) 0.4000(3) 0.3277(2) 0.0369(9) Uani 1 1 d . . .
H8 H 0.8958 0.4062 0.3830 0.044 Uiso 1 1 calc R . .
C10 C 0.9112(3) 0.2218(3) 0.4598(2) 0.0441(10) Uani 1 1 d . . .
H10 H 0.9144 0.2547 0.5080 0.053 Uiso 1 1 calc R . .
N10 N 1.0214(3) 0.4015(3) 0.1484(2) 0.0596(10) Uani 1 1 d . . .
C15 C 0.5808(3) 0.4107(3) 0.3611(2) 0.0406(9) Uani 1 1 d . . .
C4 C 0.6578(3) 0.4193(3) 0.3150(2) 0.0366(9) Uani 1 1 d . . .
H4 H 0.6534 0.4535 0.2675 0.044 Uiso 1 1 calc R . .
C6 C 0.8296(3) 0.1641(3) 0.35228(19) 0.0349(9) Uani 1 1 d . . .
C2 C 0.5868(3) 0.1794(2) 0.3062(2) 0.0352(9) Uani 1 1 d . . .
C11 C 0.5196(3) 0.1558(3) 0.3539(2) 0.0448(10) Uani 1 1 d . . .
H11 H 0.5334 0.1426 0.4077 0.054 Uiso 1 1 calc R . .
C23 C 0.7950(3) 0.3745(3) 0.2106(2) 0.0449(10) Uani 1 1 d . . .
H23 H 0.7379 0.3630 0.1855 0.054 Uiso 1 1 calc R . .
N5 N 0.6666(3) 0.1953(3) 0.52588(19) 0.0556(10) Uani 1 1 d . . .
C13 C 0.8677(3) 0.3791(3) 0.1674(2) 0.0510(11) Uani 1 1 d . . .
H13 H 0.8608 0.3723 0.1121 0.061 Uiso 1 1 calc R . .
C18 C 0.9035(3) 0.1269(3) 0.3231(2) 0.0444(10) Uani 1 1 d . . .
H18 H 0.8992 0.0938 0.2750 0.053 Uiso 1 1 calc R . .
C9 C 0.9496(3) 0.3934(3) 0.2031(2) 0.0434(10) Uani 1 1 d . . .
C17 C 0.0336(3) 0.1149(3) 0.0772(2) 0.0464(10) Uani 1 1 d . . .
H17 H -0.0264 0.1039 0.0588 0.056 Uiso 1 1 calc R . .
C7 C 0.9612(3) 0.4044(3) 0.2839(2) 0.0439(10) Uani 1 1 d . . .
H7 H 1.0187 0.4149 0.3085 0.053 Uiso 1 1 calc R . .
N8 N 0.3161(2) 0.1612(2) 0.2218(2) 0.0523(9) Uani 1 1 d . . .
C38 C 0.4316(3) 0.4437(4) 0.3868(4) 0.0798(17) Uani 1 1 d . . .
H38 H 0.3759 0.4722 0.3730 0.096 Uiso 1 1 calc R . .
C32 C 0.5011(3) 0.4525(3) 0.3389(3) 0.0585(12) Uani 1 1 d . . .
H32 H 0.4938 0.4869 0.2915 0.070 Uiso 1 1 calc R . .
C16 C 0.4787(3) 0.1952(3) 0.1976(2) 0.0482(11) Uani 1 1 d . . .
H16 H 0.4646 0.2093 0.1440 0.058 Uiso 1 1 calc R . .
C5 C 0.7398(3) 0.1520(2) 0.3126(2) 0.0349(9) Uani 1 1 d . . .
H5 H 0.7321 0.1177 0.2653 0.042 Uiso 1 1 calc R . .
C14 C 0.5662(3) 0.2001(3) 0.2282(2) 0.0416(10) Uani 1 1 d . . .
H14 H 0.6118 0.2177 0.1957 0.050 Uiso 1 1 calc R . .
C20 C 0.9880(3) 0.1853(3) 0.4340(3) 0.0521(12) Uani 1 1 d . . .
H20 H 1.0427 0.1927 0.4642 0.063 Uiso 1 1 calc R . .
C22 C 0.4326(3) 0.1515(3) 0.3229(2) 0.0501(11) Uani 1 1 d . . .
H22 H 0.3868 0.1357 0.3558 0.060 Uiso 1 1 calc R . .
C27 C 0.1007(3) 0.0965(3) 0.0303(3) 0.0527(11) Uani 1 1 d . . .
H27 H 0.0871 0.0738 -0.0212 0.063 Uiso 1 1 calc R . .
C24 C 0.9850(3) 0.1382(3) 0.3646(3) 0.0534(11) Uani 1 1 d . . .
H24 H 1.0376 0.1137 0.3452 0.064 Uiso 1 1 calc R . .
C21 C 0.2078(3) 0.1419(3) 0.1308(3) 0.0460(10) Uani 1 1 d . . .
C35 C 1.3229(3) 0.4037(3) 0.1287(3) 0.0584(12) Uani 1 1 d . . .
H35 H 1.3800 0.3895 0.1527 0.070 Uiso 1 1 calc R . .
C28 C 0.0531(3) 0.1496(3) 0.1514(3) 0.0538(11) Uani 1 1 d . . .
H28 H 0.0065 0.1639 0.1839 0.065 Uiso 1 1 calc R . .
C36 C 1.2338(3) 0.4587(3) 0.0178(3) 0.0642(13) Uani 1 1 d . . .
H36 H 1.2286 0.4826 -0.0340 0.077 Uiso 1 1 calc R . .
C26 C 0.5243(3) 0.3522(3) 0.4725(3) 0.0605(13) Uani 1 1 d . . .
H26 H 0.5324 0.3167 0.5192 0.073 Uiso 1 1 calc R . .
C19 C 0.4118(3) 0.1699(3) 0.2450(2) 0.0444(10) Uani 1 1 d . . .
N6 N 0.3036(2) 0.1515(2) 0.1519(2) 0.0516(9) Uani 1 1 d . . .
C31 C 0.4445(4) 0.3927(4) 0.4552(4) 0.0759(16) Uani 1 1 d . . .
H31 H 0.3980 0.3863 0.4894 0.091 Uiso 1 1 calc R . .
C33 C 1.3162(3) 0.4382(3) 0.0534(3) 0.0626(13) Uani 1 1 d . . .
H33 H 1.3682 0.4478 0.0262 0.075 Uiso 1 1 calc R . .
C34 C 1.2497(3) 0.3895(3) 0.1697(3) 0.0569(12) Uani 1 1 d . . .
H34 H 1.2555 0.3661 0.2216 0.068 Uiso 1 1 calc R . .
C30 C 0.1873(3) 0.1103(3) 0.0565(3) 0.0524(11) Uani 1 1 d . . .
H30 H 0.2334 0.0979 0.0230 0.063 Uiso 1 1 calc R . .
C25 C 0.1408(3) 0.1634(3) 0.1784(3) 0.0544(12) Uani 1 1 d . . .
H25 H 0.1547 0.1876 0.2294 0.065 Uiso 1 1 calc R . .
C37 C 1.1577(3) 0.4440(3) 0.0587(3) 0.0619(13) Uani 1 1 d . . .
H37 H 1.1002 0.4571 0.0351 0.074 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
Zn01 N5 2.036(4) . ?
Zn01 N7 2.037(3) . ?
Zn01 N1 2.120(3) . ?
Zn01 N4 2.147(3) . ?
Zn01 N3 2.305(3) . ?
Zn01 N2 2.344(3) . ?
S1 C3 1.627(4) . ?
S2 C12 1.620(4) . ?
N9 N10 1.206(5) . ?
N9 C29 1.510(6) . ?
N7 C3 1.161(5) . ?
N2 C4 1.274(5) . ?
N2 C1 1.423(5) . ?
C29 C34 1.360(7) . ?
C29 C37 1.389(7) . ?
N3 C5 1.268(5) . ?
N3 C2 1.416(4) . ?
N1 C10 1.340(5) . ?
N1 C6 1.355(5) . ?
C1 C8 1.385(5) . ?
C1 C23 1.393(5) . ?
N4 C26 1.331(5) . ?
N4 C15 1.357(5) . ?
C12 N5 1.151(5) . ?
C8 C7 1.375(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.373(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.487(5) . ?
C15 C32 1.375(6) . ?
C15 C4 1.456(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.364(6) . ?
C6 C5 1.483(5) . ?
C2 C14 1.384(5) . ?
C2 C11 1.390(5) . ?
C11 C22 1.383(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.370(6) . ?
C23 H23 0.9500 . ?
C13 C9 1.355(6) . ?
C13 H13 0.9500 . ?
C18 C24 1.387(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.394(5) . ?
C17 C27 1.363(6) . ?
C17 C28 1.378(6) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.208(4) . ?
N8 C19 1.476(5) . ?
C38 C32 1.383(7) . ?
C38 C31 1.384(8) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C14 1.389(5) . ?
C16 C19 1.391(6) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.367(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.376(6) . ?
C22 H22 0.9500 . ?
C27 C30 1.368(6) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.366(6) . ?
C21 C25 1.379(6) . ?
C21 N6 1.472(5) . ?
C35 C34 1.366(6) . ?
C35 C33 1.379(7) . ?
C35 H35 0.9500 . ?
C28 C25 1.386(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.379(7) . ?
C36 C37 1.405(7) . ?
C36 H36 0.9500 . ?
C26 C31 1.353(7) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.39(14) . . ?
N5 Zn01 N1 100.79(14) . . ?
N7 Zn01 N1 95.42(13) . . ?
N5 Zn01 N4 94.06(14) . . ?
N7 Zn01 N4 97.71(13) . . ?
N1 Zn01 N4 158.72(11) . . ?
N5 Zn01 N3 92.88(12) . . ?
N7 Zn01 N3 166.74(13) . . ?
N1 Zn01 N3 74.34(11) . . ?
N4 Zn01 N3 89.88(11) . . ?
N5 Zn01 N2 164.07(12) . . ?
N7 Zn01 N2 94.33(12) . . ?
N1 Zn01 N2 88.76(11) . . ?
N4 Zn01 N2 73.64(11) . . ?
N3 Zn01 N2 77.32(9) . . ?
N10 N9 C29 111.5(4) . . ?
C3 N7 Zn01 161.1(3) . . ?
C4 N2 C1 119.6(3) . . ?
C4 N2 Zn01 111.6(2) . . ?
C1 N2 Zn01 127.7(2) . . ?
C34 C29 C37 122.1(4) . . ?
C34 C29 N9 114.7(4) . . ?
C37 C29 N9 123.2(4) . . ?
C5 N3 C2 121.1(3) . . ?
C5 N3 Zn01 112.3(2) . . ?
C2 N3 Zn01 125.9(2) . . ?
C10 N1 C6 117.0(3) . . ?
C10 N1 Zn01 125.0(3) . . ?
C6 N1 Zn01 117.5(2) . . ?
C8 C1 C23 119.6(3) . . ?
C8 C1 N2 118.6(3) . . ?
C23 C1 N2 121.7(3) . . ?
N7 C3 S1 178.7(4) . . ?
C26 N4 C15 118.1(4) . . ?
C26 N4 Zn01 124.4(3) . . ?
C15 N4 Zn01 117.3(3) . . ?
N5 C12 S2 179.9(4) . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 122.9(4) . . ?
N1 C10 H10 118.6 . . ?
C20 C10 H10 118.6 . . ?
N9 N10 C9 108.6(4) . . ?
N4 C15 C32 121.8(4) . . ?
N4 C15 C4 116.2(3) . . ?
C32 C15 C4 122.0(4) . . ?
N2 C4 C15 120.1(3) . . ?
N2 C4 H4 120.0 . . ?
C15 C4 H4 120.0 . . ?
N1 C6 C18 122.9(3) . . ?
N1 C6 C5 115.0(3) . . ?
C18 C6 C5 122.1(3) . . ?
C14 C2 C11 119.8(3) . . ?
C14 C2 N3 123.1(3) . . ?
C11 C2 N3 116.8(3) . . ?
C22 C11 C2 119.9(4) . . ?
C22 C11 H11 120.1 . . ?
C2 C11 H11 120.1 . . ?
C13 C23 C1 120.0(4) . . ?
C13 C23 H23 120.0 . . ?
C1 C23 H23 120.0 . . ?
C12 N5 Zn01 164.7(3) . . ?
C9 C13 C23 120.2(4) . . ?
C9 C13 H13 119.9 . . ?
C23 C13 H13 119.9 . . ?
C6 C18 C24 119.1(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.9(4) . . ?
C13 C9 N10 114.2(3) . . ?
C7 C9 N10 124.8(4) . . ?
C27 C17 C28 119.7(4) . . ?
C27 C17 H17 120.2 . . ?
C28 C17 H17 120.2 . . ?
C8 C7 C9 119.3(4) . . ?
C8 C7 H7 120.4 . . ?
C9 C7 H7 120.4 . . ?
N6 N8 C19 111.1(4) . . ?
C32 C38 C31 119.0(5) . . ?
C32 C38 H38 120.5 . . ?
C31 C38 H38 120.5 . . ?
C15 C32 C38 118.8(5) . . ?
C15 C32 H32 120.6 . . ?
C38 C32 H32 120.6 . . ?
C14 C16 C19 120.2(4) . . ?
C14 C16 H16 119.9 . . ?
C19 C16 H16 119.9 . . ?
N3 C5 C6 119.3(3) . . ?
N3 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C2 C14 C16 119.8(4) . . ?
C2 C14 H14 120.1 . . ?
C16 C14 H14 120.1 . . ?
C24 C20 C10 119.5(4) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C19 C22 C11 120.7(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C17 C27 C30 120.8(4) . . ?
C17 C27 H27 119.6 . . ?
C30 C27 H27 119.6 . . ?
C20 C24 C18 118.5(4) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C30 C21 C25 119.9(4) . . ?
C30 C21 N6 114.4(4) . . ?
C25 C21 N6 125.7(4) . . ?
C34 C35 C33 121.8(5) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C17 C28 C25 119.8(4) . . ?
C17 C28 H28 120.1 . . ?
C25 C28 H28 120.1 . . ?
C33 C36 C37 119.5(5) . . ?
C33 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
N4 C26 C31 123.5(5) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C22 C19 C16 119.5(4) . . ?
C22 C19 N8 113.5(4) . . ?
C16 C19 N8 127.0(4) . . ?
N8 N6 C21 109.7(4) . . ?
C26 C31 C38 118.8(5) . . ?
C26 C31 H31 120.6 . . ?
C38 C31 H31 120.6 . . ?
C36 C33 C35 119.7(5) . . ?
C36 C33 H33 120.2 . . ?
C35 C33 H33 120.2 . . ?
C29 C34 C35 118.6(5) . . ?
C29 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
C21 C30 C27 120.2(4) . . ?
C21 C30 H30 119.9 . . ?
C27 C30 H30 119.9 . . ?
C21 C25 C28 119.6(4) . . ?
C21 C25 H25 120.2 . . ?
C28 C25 H25 120.2 . . ?
C29 C37 C36 118.4(5) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.737
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.737
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.053
####################################################################### 
# 
# 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_znaza240km
_database_code_depnum_ccdc_archive 'CCDC 1492678'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1170(7)
_cell_length_b                   14.4666(10)
_cell_length_c                   17.1452(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.793(4)
_cell_angle_gamma                90.00
_cell_volume                     3741.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    16193
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_T_max  0.7120
_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            7719
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         27.87
_reflns_number_total             5987
_reflns_number_gt                4502
_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)+(0.0605P)²+3.8859P] 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         5987
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1274
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
Zn01 Zn 0.71163(3) 0.28506(3) 0.44724(2) 0.04934(17) Uani 1 1 d . . .
S1 S 0.80773(7) 0.49783(8) 0.64735(5) 0.0584(3) Uani 1 1 d . . .
S2 S 0.56356(8) 0.07166(9) 0.60505(7) 0.0701(3) Uani 1 1 d . . .
N9 N 1.0882(3) 0.3956(2) 0.1862(2) 0.0776(11) Uani 1 1 d . . .
N7 N 0.7730(2) 0.3745(3) 0.52489(19) 0.0648(9) Uani 1 1 d . . .
N2 N 0.73060(19) 0.38053(19) 0.33828(15) 0.0408(7) Uani 1 1 d . . .
C29 C 1.1685(4) 0.4093(3) 0.1326(4) 0.0824(16) Uani 1 1 d . . .
N3 N 0.6711(2) 0.1891(2) 0.34347(16) 0.0433(7) Uani 1 1 d . . .
N1 N 0.8292(2) 0.2136(2) 0.42153(16) 0.0482(7) Uani 1 1 d . . .
C1 C 0.8051(2) 0.3863(2) 0.29218(19) 0.0412(8) Uani 1 1 d . . .
C3 C 0.7868(2) 0.4254(3) 0.5761(2) 0.0474(9) Uani 1 1 d . . .
N4 N 0.5901(2) 0.3601(2) 0.42618(19) 0.0553(8) Uani 1 1 d . . .
C12 C 0.6210(2) 0.1458(3) 0.55910(19) 0.0496(9) Uani 1 1 d . . .
C8 C 0.8877(3) 0.3991(3) 0.3293(2) 0.0505(9) Uani 1 1 d . . .
H8 H 0.8940 0.4050 0.3840 0.061 Uiso 1 1 calc R . .
C10 C 0.9073(3) 0.2225(3) 0.4618(2) 0.0590(11) Uani 1 1 d . . .
H10 H 0.9099 0.2552 0.5093 0.071 Uiso 1 1 calc R . .
N10 N 1.0252(3) 0.4022(3) 0.1458(3) 0.0925(15) Uani 1 1 d . . .
C15 C 0.5802(3) 0.4113(3) 0.3602(2) 0.0527(10) Uani 1 1 d . . .
C4 C 0.6578(3) 0.4193(3) 0.3150(2) 0.0484(9) Uani 1 1 d . . .
H4 H 0.6543 0.4535 0.2683 0.058 Uiso 1 1 calc R . .
C6 C 0.8265(2) 0.1647(2) 0.35423(19) 0.0457(9) Uani 1 1 d . . .
C2 C 0.5852(2) 0.1800(2) 0.3062(2) 0.0466(9) Uani 1 1 d . . .
C11 C 0.5175(3) 0.1565(3) 0.3525(2) 0.0610(11) Uani 1 1 d . . .
H11 H 0.5301 0.1437 0.4058 0.073 Uiso 1 1 calc R . .
C23 C 0.7966(3) 0.3754(3) 0.2113(2) 0.0585(10) Uani 1 1 d . . .
H23 H 0.7405 0.3649 0.1860 0.070 Uiso 1 1 calc R . .
N5 N 0.6623(3) 0.1976(3) 0.5265(2) 0.0730(11) Uani 1 1 d . . .
C13 C 0.8700(3) 0.3799(3) 0.1686(3) 0.0718(13) Uani 1 1 d . . .
H13 H 0.8641 0.3735 0.1140 0.086 Uiso 1 1 calc R . .
C18 C 0.9008(3) 0.1273(3) 0.3257(2) 0.0609(11) Uani 1 1 d . . .
H18 H 0.8971 0.0944 0.2783 0.073 Uiso 1 1 calc R . .
C9 C 0.9511(3) 0.3935(3) 0.2056(3) 0.0640(12) Uani 1 1 d . . .
C17 C 0.0345(3) 0.1152(3) 0.0774(3) 0.0641(12) Uani 1 1 d . . .
H17 H -0.0242 0.1048 0.0578 0.077 Uiso 1 1 calc R . .
C7 C 0.9609(3) 0.4031(3) 0.2860(3) 0.0616(11) Uani 1 1 d . . .
H7 H 1.0175 0.4122 0.3110 0.074 Uiso 1 1 calc R . .
N8 N 0.3123(3) 0.1609(3) 0.2213(2) 0.0760(11) Uani 1 1 d . . .
C38 C 0.4307(4) 0.4456(5) 0.3837(5) 0.105(2) Uani 1 1 d . . .
H38 H 0.3762 0.4742 0.3694 0.127 Uiso 1 1 calc R . .
C32 C 0.5014(3) 0.4535(3) 0.3374(3) 0.0789(14) Uani 1 1 d . . .
H32 H 0.4957 0.4875 0.2906 0.095 Uiso 1 1 calc R . .
C16 C 0.4791(3) 0.1949(3) 0.1971(3) 0.0690(13) Uani 1 1 d . . .
H16 H 0.4659 0.2078 0.1439 0.083 Uiso 1 1 calc R . .
C5 C 0.7373(3) 0.1530(2) 0.3146(2) 0.0480(9) Uani 1 1 d . . .
H5 H 0.7301 0.1187 0.2681 0.058 Uiso 1 1 calc R . .
C14 C 0.5661(3) 0.2010(3) 0.2285(2) 0.0579(10) Uani 1 1 d . . .
H14 H 0.6115 0.2194 0.1969 0.069 Uiso 1 1 calc R . .
C20 C 0.9835(3) 0.1859(3) 0.4367(3) 0.0720(13) Uani 1 1 d . . .
H20 H 1.0373 0.1932 0.4667 0.086 Uiso 1 1 calc R . .
C22 C 0.4311(3) 0.1516(3) 0.3209(3) 0.0706(12) Uani 1 1 d . . .
H22 H 0.3853 0.1354 0.3528 0.085 Uiso 1 1 calc R . .
C27 C 0.1017(3) 0.0972(3) 0.0323(3) 0.0728(13) Uani 1 1 d . . .
H27 H 0.0895 0.0746 -0.0187 0.087 Uiso 1 1 calc R . .
C24 C 0.9813(3) 0.1386(3) 0.3675(3) 0.0711(12) Uani 1 1 d . . .
H24 H 1.0335 0.1142 0.3488 0.085 Uiso 1 1 calc R . .
C21 C 0.2061(3) 0.1421(3) 0.1332(3) 0.0658(12) Uani 1 1 d . . .
C35 C 1.3200(3) 0.4042(3) 0.1270(3) 0.0819(15) Uani 1 1 d . . .
H35 H 1.3761 0.3902 0.1509 0.098 Uiso 1 1 calc R . .
C28 C 0.0506(3) 0.1485(3) 0.1516(3) 0.0724(12) Uani 1 1 d . . .
H28 H 0.0036 0.1619 0.1831 0.087 Uiso 1 1 calc R . .
C36 C 1.2340(4) 0.4590(4) 0.0154(3) 0.0891(16) Uani 1 1 d . . .
H36 H 1.2296 0.4828 -0.0357 0.107 Uiso 1 1 calc R . .
C26 C 0.5210(4) 0.3536(4) 0.4699(3) 0.0812(14) Uani 1 1 d . . .
H26 H 0.5272 0.3188 0.5162 0.097 Uiso 1 1 calc R . .
C19 C 0.4117(3) 0.1700(3) 0.2437(3) 0.0644(12) Uani 1 1 d . . .
N6 N 0.3046(3) 0.1522(3) 0.1537(2) 0.0779(11) Uani 1 1 d . . .
C31 C 0.4420(4) 0.3950(5) 0.4508(5) 0.104(2) Uani 1 1 d . . .
H31 H 0.3951 0.3889 0.4838 0.125 Uiso 1 1 calc R . .
C33 C 1.3150(4) 0.4381(4) 0.0519(3) 0.0832(15) Uani 1 1 d . . .
H33 H 1.3670 0.4471 0.0257 0.100 Uiso 1 1 calc R . .
C34 C 1.2479(4) 0.3901(3) 0.1680(4) 0.0839(15) Uani 1 1 d . . .
H34 H 1.2534 0.3677 0.2196 0.101 Uiso 1 1 calc R . .
C30 C 0.1877(3) 0.1113(3) 0.0593(3) 0.0752(13) Uani 1 1 d . . .
H30 H 0.2340 0.0996 0.0266 0.090 Uiso 1 1 calc R . .
C25 C 0.1385(4) 0.1621(3) 0.1796(3) 0.0771(14) Uani 1 1 d . . .
H25 H 0.1512 0.1850 0.2304 0.092 Uiso 1 1 calc R . .
C37 C 1.1572(3) 0.4437(4) 0.0567(4) 0.0897(17) Uani 1 1 d . . .
H37 H 1.1004 0.4563 0.0335 0.108 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
Zn01 N5 2.034(4) . ?
Zn01 N7 2.036(3) . ?
Zn01 N1 2.127(3) . ?
Zn01 N4 2.144(3) . ?
Zn01 N3 2.308(3) . ?
Zn01 N2 2.356(3) . ?
S1 C3 1.624(4) . ?
S2 C12 1.617(4) . ?
N9 N10 1.143(5) . ?
N9 C29 1.582(6) . ?
N7 C3 1.154(5) . ?
N2 C4 1.276(4) . ?
N2 C1 1.421(4) . ?
C29 C34 1.338(8) . ?
C29 C37 1.394(8) . ?
N3 C5 1.259(5) . ?
N3 C2 1.415(4) . ?
N1 C10 1.334(5) . ?
N1 C6 1.352(4) . ?
C1 C8 1.376(5) . ?
C1 C23 1.392(5) . ?
N4 C26 1.328(5) . ?
N4 C15 1.352(5) . ?
C12 N5 1.144(5) . ?
C8 C7 1.374(5) . ?
C8 H8 0.9400 . ?
C10 C20 1.363(6) . ?
C10 H10 0.9400 . ?
N10 C9 1.572(6) . ?
C15 C32 1.373(6) . ?
C15 C4 1.452(5) . ?
C4 H4 0.9400 . ?
C6 C18 1.366(6) . ?
C6 C5 1.479(5) . ?
C2 C11 1.379(5) . ?
C2 C14 1.379(5) . ?
C11 C22 1.383(5) . ?
C11 H11 0.9400 . ?
C23 C13 1.370(6) . ?
C23 H23 0.9400 . ?
C13 C9 1.357(6) . ?
C13 H13 0.9400 . ?
C18 C24 1.380(6) . ?
C18 H18 0.9400 . ?
C9 C7 1.385(6) . ?
C17 C27 1.344(6) . ?
C17 C28 1.367(6) . ?
C17 H17 0.9400 . ?
C7 H7 0.9400 . ?
N8 N6 1.163(5) . ?
N8 C19 1.531(6) . ?
C38 C31 1.366(9) . ?
C38 C32 1.377(8) . ?
C38 H38 0.9400 . ?
C32 H32 0.9400 . ?
C16 C19 1.383(7) . ?
C16 C14 1.390(6) . ?
C16 H16 0.9400 . ?
C5 H5 0.9400 . ?
C14 H14 0.9400 . ?
C20 C24 1.368(6) . ?
C20 H20 0.9400 . ?
C22 C19 1.362(6) . ?
C22 H22 0.9400 . ?
C27 C30 1.365(6) . ?
C27 H27 0.9400 . ?
C24 H24 0.9400 . ?
C21 C30 1.355(7) . ?
C21 C25 1.366(7) . ?
C21 N6 1.514(6) . ?
C35 C34 1.351(7) . ?
C35 C33 1.375(7) . ?
C35 H35 0.9400 . ?
C28 C25 1.397(6) . ?
C28 H28 0.9400 . ?
C36 C33 1.371(7) . ?
C36 C37 1.416(7) . ?
C36 H36 0.9400 . ?
C26 C31 1.357(8) . ?
C26 H26 0.9400 . ?
C31 H31 0.9400 . ?
C33 H33 0.9400 . ?
C34 H34 0.9400 . ?
C30 H30 0.9400 . ?
C25 H25 0.9400 . ?
C37 H37 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 Zn01 N7 97.48(14) . . ?
N5 Zn01 N1 100.63(14) . . ?
N7 Zn01 N1 95.37(13) . . ?
N5 Zn01 N4 94.58(15) . . ?
N7 Zn01 N4 97.85(13) . . ?
N1 Zn01 N4 158.36(11) . . ?
N5 Zn01 N3 92.88(13) . . ?
N7 Zn01 N3 166.66(13) . . ?
N1 Zn01 N3 74.38(11) . . ?
N4 Zn01 N3 89.65(11) . . ?
N5 Zn01 N2 164.49(13) . . ?
N7 Zn01 N2 94.11(12) . . ?
N1 Zn01 N2 88.47(11) . . ?
N4 Zn01 N2 73.59(11) . . ?
N3 Zn01 N2 77.38(9) . . ?
N10 N9 C29 106.2(5) . . ?
C3 N7 Zn01 162.6(3) . . ?
C4 N2 C1 120.0(3) . . ?
C4 N2 Zn01 111.0(2) . . ?
C1 N2 Zn01 128.2(2) . . ?
C34 C29 C37 123.2(5) . . ?
C34 C29 N9 114.2(5) . . ?
C37 C29 N9 122.4(6) . . ?
C5 N3 C2 121.0(3) . . ?
C5 N3 Zn01 112.0(2) . . ?
C2 N3 Zn01 126.4(2) . . ?
C10 N1 C6 117.8(3) . . ?
C10 N1 Zn01 124.7(3) . . ?
C6 N1 Zn01 117.0(2) . . ?
C8 C1 C23 119.8(3) . . ?
C8 C1 N2 118.6(3) . . ?
C23 C1 N2 121.5(3) . . ?
N7 C3 S1 178.9(4) . . ?
C26 N4 C15 117.6(4) . . ?
C26 N4 Zn01 124.5(3) . . ?
C15 N4 Zn01 117.7(3) . . ?
N5 C12 S2 179.4(4) . . ?
C7 C8 C1 119.6(3) . . ?
C7 C8 H8 120.2 . . ?
C1 C8 H8 120.2 . . ?
N1 C10 C20 122.5(4) . . ?
N1 C10 H10 118.8 . . ?
C20 C10 H10 118.8 . . ?
N9 N10 C9 101.5(5) . . ?
N4 C15 C32 121.9(4) . . ?
N4 C15 C4 116.2(3) . . ?
C32 C15 C4 121.9(4) . . ?
N2 C4 C15 120.6(3) . . ?
N2 C4 H4 119.7 . . ?
C15 C4 H4 119.7 . . ?
N1 C6 C18 122.3(3) . . ?
N1 C6 C5 115.2(3) . . ?
C18 C6 C5 122.4(3) . . ?
C11 C2 C14 119.7(3) . . ?
C11 C2 N3 117.2(3) . . ?
C14 C2 N3 122.9(3) . . ?
C2 C11 C22 120.3(4) . . ?
C2 C11 H11 119.8 . . ?
C22 C11 H11 119.8 . . ?
C13 C23 C1 120.1(4) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C12 N5 Zn01 165.8(3) . . ?
C9 C13 C23 119.7(4) . . ?
C9 C13 H13 120.1 . . ?
C23 C13 H13 120.1 . . ?
C6 C18 C24 119.0(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.9(4) . . ?
C13 C9 N10 111.6(4) . . ?
C7 C9 N10 127.4(4) . . ?
C27 C17 C28 120.6(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C8 C7 C9 119.8(4) . . ?
C8 C7 H7 120.1 . . ?
C9 C7 H7 120.1 . . ?
N6 N8 C19 106.9(4) . . ?
C31 C38 C32 118.1(5) . . ?
C31 C38 H38 120.9 . . ?
C32 C38 H38 120.9 . . ?
C15 C32 C38 119.4(5) . . ?
C15 C32 H32 120.3 . . ?
C38 C32 H32 120.3 . . ?
C19 C16 C14 120.5(4) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N3 C5 C6 119.8(3) . . ?
N3 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C2 C14 C16 119.4(4) . . ?
C2 C14 H14 120.3 . . ?
C16 C14 H14 120.3 . . ?
C10 C20 C24 119.7(4) . . ?
C10 C20 H20 120.1 . . ?
C24 C20 H20 120.1 . . ?
C19 C22 C11 120.5(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C17 C27 C30 121.0(4) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C20 C24 C18 118.7(4) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C30 C21 C25 119.9(4) . . ?
C30 C21 N6 112.8(5) . . ?
C25 C21 N6 127.3(4) . . ?
C34 C35 C33 123.1(5) . . ?
C34 C35 H35 118.5 . . ?
C33 C35 H35 118.5 . . ?
C17 C28 C25 118.4(5) . . ?
C17 C28 H28 120.8 . . ?
C25 C28 H28 120.8 . . ?
C33 C36 C37 118.3(5) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
N4 C26 C31 123.0(5) . . ?
N4 C26 H26 118.5 . . ?
C31 C26 H26 118.5 . . ?
C22 C19 C16 119.5(4) . . ?
C22 C19 N8 111.8(4) . . ?
C16 C19 N8 128.7(4) . . ?
N8 N6 C21 105.9(4) . . ?
C26 C31 C38 119.9(5) . . ?
C26 C31 H31 120.0 . . ?
C38 C31 H31 120.0 . . ?
C36 C33 C35 119.9(5) . . ?
C36 C33 H33 120.1 . . ?
C35 C33 H33 120.1 . . ?
C29 C34 C35 117.6(6) . . ?
C29 C34 H34 121.2 . . ?
C35 C34 H34 121.2 . . ?
C21 C30 C27 119.9(5) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C21 C25 C28 120.1(4) . . ?
C21 C25 H25 119.9 . . ?
C28 C25 H25 119.9 . . ?
C29 C37 C36 118.0(5) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?

_diffrn_measured_fraction_theta_max 0.671
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.671
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_znaza280km
_database_code_depnum_ccdc_archive 'CCDC 1492679'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1281(7)
_cell_length_b                   14.5550(11)
_cell_length_c                   17.1464(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.621(4)
_cell_angle_gamma                90.00
_cell_volume                     3767.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    280(2)
_cell_measurement_reflns_used    14228
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_T_max  0.7136
_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            6403
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4932
_reflns_number_gt                3891
_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)+(0.0471P)²+3.6436P] 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         4932
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1231
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Zn01 Zn 0.70984(3) 0.28536(3) 0.44762(2) 0.05788(19) Uani 1 1 d . . .
S1 S 0.80784(7) 0.49608(8) 0.64717(6) 0.0687(3) Uani 1 1 d . . .
S2 S 0.56403(8) 0.07171(9) 0.60551(7) 0.0820(4) Uani 1 1 d . . .
N9 N 1.0861(3) 0.3957(3) 0.1870(2) 0.0912(13) Uani 1 1 d . . .
N7 N 0.7711(2) 0.3749(3) 0.5246(2) 0.0760(10) Uani 1 1 d . . .
N2 N 0.7303(2) 0.3804(2) 0.33847(16) 0.0475(7) Uani 1 1 d . . .
C29 C 1.1672(5) 0.4095(4) 0.1311(4) 0.101(2) Uani 1 1 d . . .
N3 N 0.6699(2) 0.1893(2) 0.34397(17) 0.0505(8) Uani 1 1 d . . .
N1 N 0.8272(2) 0.2138(2) 0.42256(17) 0.0559(8) Uani 1 1 d . . .
C1 C 0.8054(2) 0.3858(2) 0.2925(2) 0.0482(9) Uani 1 1 d . . .
C3 C 0.7856(2) 0.4243(3) 0.5757(2) 0.0558(10) Uani 1 1 d . . .
N4 N 0.5888(2) 0.3602(2) 0.4253(2) 0.0638(9) Uani 1 1 d . . .
C12 C 0.6200(3) 0.1465(3) 0.5595(2) 0.0570(10) Uani 1 1 d . . .
C8 C 0.8874(3) 0.3984(3) 0.3305(2) 0.0586(10) Uani 1 1 d . . .
H8 H 0.8928 0.4042 0.3846 0.070 Uiso 1 1 calc R . .
C10 C 0.9055(3) 0.2227(3) 0.4623(3) 0.0691(12) Uani 1 1 d . . .
H10 H 0.9079 0.2554 0.5090 0.083 Uiso 1 1 calc R . .
N10 N 1.0277(4) 0.4028(3) 0.1451(3) 0.1126(18) Uani 1 1 d . . .
C15 C 0.5801(3) 0.4113(3) 0.3599(2) 0.0610(10) Uani 1 1 d . . .
C4 C 0.6583(3) 0.4191(3) 0.3148(2) 0.0552(10) Uani 1 1 d . . .
H4 H 0.6554 0.4526 0.2686 0.066 Uiso 1 1 calc R . .
C6 C 0.8248(3) 0.1652(3) 0.3552(2) 0.0536(10) Uani 1 1 d . . .
C2 C 0.5843(3) 0.1804(3) 0.3063(2) 0.0535(10) Uani 1 1 d . . .
C11 C 0.5159(3) 0.1567(3) 0.3519(3) 0.0715(12) Uani 1 1 d . . .
H11 H 0.5275 0.1443 0.4047 0.086 Uiso 1 1 calc R . .
C23 C 0.7979(3) 0.3759(3) 0.2121(2) 0.0680(12) Uani 1 1 d . . .
H23 H 0.7425 0.3663 0.1867 0.082 Uiso 1 1 calc R . .
N5 N 0.6599(3) 0.1990(3) 0.5266(2) 0.0844(12) Uani 1 1 d . . .
C13 C 0.8709(4) 0.3800(3) 0.1701(3) 0.0851(14) Uani 1 1 d . . .
H13 H 0.8654 0.3737 0.1160 0.102 Uiso 1 1 calc R . .
C18 C 0.8990(3) 0.1270(3) 0.3273(3) 0.0713(12) Uani 1 1 d . . .
H18 H 0.8955 0.0938 0.2809 0.086 Uiso 1 1 calc R . .
C9 C 0.9523(3) 0.3935(3) 0.2073(3) 0.0746(14) Uani 1 1 d . . .
C17 C 0.0352(3) 0.1153(3) 0.0776(3) 0.0767(13) Uani 1 1 d . . .
H17 H -0.0225 0.1050 0.0576 0.092 Uiso 1 1 calc R . .
C7 C 0.9614(3) 0.4023(3) 0.2875(3) 0.0716(12) Uani 1 1 d . . .
H7 H 1.0172 0.4109 0.3125 0.086 Uiso 1 1 calc R . .
N8 N 0.3101(3) 0.1604(3) 0.2208(3) 0.0929(13) Uani 1 1 d . . .
C38 C 0.4311(4) 0.4462(5) 0.3825(5) 0.120(2) Uani 1 1 d . . .
H38 H 0.3776 0.4750 0.3682 0.144 Uiso 1 1 calc R . .
C32 C 0.5019(3) 0.4542(4) 0.3359(3) 0.0901(15) Uani 1 1 d . . .
H32 H 0.4969 0.4876 0.2896 0.108 Uiso 1 1 calc R . .
C16 C 0.4794(3) 0.1948(3) 0.1971(3) 0.0796(14) Uani 1 1 d . . .
H16 H 0.4669 0.2078 0.1444 0.096 Uiso 1 1 calc R . .
C5 C 0.7362(3) 0.1534(3) 0.3156(2) 0.0557(10) Uani 1 1 d . . .
H5 H 0.7294 0.1194 0.2696 0.067 Uiso 1 1 calc R . .
C14 C 0.5658(3) 0.2009(3) 0.2286(2) 0.0676(11) Uani 1 1 d . . .
H14 H 0.6110 0.2187 0.1975 0.081 Uiso 1 1 calc R . .
C20 C 0.9818(3) 0.1863(3) 0.4381(3) 0.0820(14) Uani 1 1 d . . .
H20 H 1.0348 0.1939 0.4680 0.098 Uiso 1 1 calc R . .
C22 C 0.4309(3) 0.1515(3) 0.3197(3) 0.0805(14) Uani 1 1 d . . .
H22 H 0.3853 0.1352 0.3508 0.097 Uiso 1 1 calc R . .
C27 C 0.1033(4) 0.0977(4) 0.0331(3) 0.0890(15) Uani 1 1 d . . .
H27 H 0.0920 0.0759 -0.0175 0.107 Uiso 1 1 calc R . .
C24 C 0.9799(3) 0.1385(3) 0.3695(3) 0.0825(14) Uani 1 1 d . . .
H24 H 1.0316 0.1142 0.3513 0.099 Uiso 1 1 calc R . .
C21 C 0.2050(3) 0.1421(3) 0.1346(4) 0.0802(15) Uani 1 1 d . . .
C35 C 1.3192(4) 0.4042(4) 0.1261(4) 0.0967(17) Uani 1 1 d . . .
H35 H 1.3744 0.3901 0.1501 0.116 Uiso 1 1 calc R . .
C28 C 0.0499(3) 0.1479(4) 0.1513(3) 0.0869(14) Uani 1 1 d . . .
H28 H 0.0028 0.1611 0.1818 0.104 Uiso 1 1 calc R . .
C36 C 1.2341(4) 0.4592(4) 0.0144(4) 0.1048(18) Uani 1 1 d . . .
H36 H 1.2303 0.4832 -0.0360 0.126 Uiso 1 1 calc R . .
C26 C 0.5190(4) 0.3541(4) 0.4684(3) 0.0947(16) Uani 1 1 d . . .
H26 H 0.5240 0.3195 0.5141 0.114 Uiso 1 1 calc R . .
C19 C 0.4125(3) 0.1698(3) 0.2426(3) 0.0764(14) Uani 1 1 d . . .
N6 N 0.3072(3) 0.1530(3) 0.1553(3) 0.0993(14) Uani 1 1 d . . .
C31 C 0.4401(4) 0.3965(5) 0.4486(5) 0.121(2) Uani 1 1 d . . .
H31 H 0.3931 0.3910 0.4807 0.145 Uiso 1 1 calc R . .
C33 C 1.3147(4) 0.4383(4) 0.0515(4) 0.0980(17) Uani 1 1 d . . .
H33 H 1.3664 0.4474 0.0258 0.118 Uiso 1 1 calc R . .
C34 C 1.2461(5) 0.3904(4) 0.1663(4) 0.1010(18) Uani 1 1 d . . .
H34 H 1.2508 0.3681 0.2172 0.121 Uiso 1 1 calc R . .
C30 C 0.1882(3) 0.1115(4) 0.0610(4) 0.0923(16) Uani 1 1 d . . .
H30 H 0.2347 0.0999 0.0294 0.111 Uiso 1 1 calc R . .
C25 C 0.1371(4) 0.1611(4) 0.1807(3) 0.0914(16) Uani 1 1 d . . .
H25 H 0.1488 0.1828 0.2313 0.110 Uiso 1 1 calc R . .
C37 C 1.1569(4) 0.4432(4) 0.0551(5) 0.106(2) Uani 1 1 d . . .
H37 H 1.1009 0.4548 0.0317 0.127 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
Zn01 N5 2.028(4) . ?
Zn01 N7 2.036(3) . ?
Zn01 N1 2.125(3) . ?
Zn01 N4 2.145(3) . ?
Zn01 N3 2.311(3) . ?
Zn01 N2 2.364(3) . ?
S1 C3 1.628(4) . ?
S2 C12 1.616(5) . ?
N9 N10 1.109(5) . ?
N9 C29 1.617(7) . ?
N7 C3 1.144(5) . ?
N2 C4 1.271(4) . ?
N2 C1 1.426(4) . ?
C29 C34 1.332(8) . ?
C29 C37 1.391(9) . ?
N3 C5 1.256(5) . ?
N3 C2 1.417(4) . ?
N1 C10 1.335(5) . ?
N1 C6 1.354(5) . ?
C1 C8 1.376(5) . ?
C1 C23 1.383(5) . ?
N4 C26 1.330(6) . ?
N4 C15 1.345(5) . ?
C12 N5 1.143(5) . ?
C8 C7 1.380(6) . ?
C8 H8 0.9300 . ?
C10 C20 1.359(7) . ?
C10 H10 0.9300 . ?
N10 C9 1.616(7) . ?
C15 C32 1.377(6) . ?
C15 C4 1.458(6) . ?
C4 H4 0.9300 . ?
C6 C18 1.365(6) . ?
C6 C5 1.474(5) . ?
C2 C14 1.375(5) . ?
C2 C11 1.381(6) . ?
C11 C22 1.369(6) . ?
C11 H11 0.9300 . ?
C23 C13 1.357(6) . ?
C23 H23 0.9300 . ?
C13 C9 1.365(7) . ?
C13 H13 0.9300 . ?
C18 C24 1.392(6) . ?
C18 H18 0.9300 . ?
C9 C7 1.380(6) . ?
C17 C27 1.345(7) . ?
C17 C28 1.356(7) . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
N8 N6 1.127(5) . ?
N8 C19 1.575(6) . ?
C38 C31 1.345(9) . ?
C38 C32 1.380(8) . ?
C38 H38 0.9300 . ?
C32 H32 0.9300 . ?
C16 C19 1.367(7) . ?
C16 C14 1.386(6) . ?
C16 H16 0.9300 . ?
C5 H5 0.9300 . ?
C14 H14 0.9300 . ?
C20 C24 1.366(7) . ?
C20 H20 0.9300 . ?
C22 C19 1.360(7) . ?
C22 H22 0.9300 . ?
C27 C30 1.357(6) . ?
C27 H27 0.9300 . ?
C24 H24 0.9300 . ?
C21 C30 1.347(7) . ?
C21 C25 1.364(7) . ?
C21 N6 1.572(6) . ?
C35 C34 1.354(7) . ?
C35 C33 1.371(7) . ?
C35 H35 0.9300 . ?
C28 C25 1.395(7) . ?
C28 H28 0.9300 . ?
C36 C33 1.373(8) . ?
C36 C37 1.417(8) . ?
C36 H36 0.9300 . ?
C26 C31 1.366(8) . ?
C26 H26 0.9300 . ?
C31 H31 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C25 H25 0.9300 . ?
C37 H37 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Zn01 N7 97.87(15) . . ?
N5 Zn01 N1 100.51(15) . . ?
N7 Zn01 N1 95.33(13) . . ?
N5 Zn01 N4 94.84(16) . . ?
N7 Zn01 N4 98.01(14) . . ?
N1 Zn01 N4 158.06(12) . . ?
N5 Zn01 N3 92.78(13) . . ?
N7 Zn01 N3 166.37(13) . . ?
N1 Zn01 N3 74.28(11) . . ?
N4 Zn01 N3 89.50(12) . . ?
N5 Zn01 N2 164.69(13) . . ?
N7 Zn01 N2 93.56(13) . . ?
N1 Zn01 N2 88.49(11) . . ?
N4 Zn01 N2 73.40(12) . . ?
N3 Zn01 N2 77.64(10) . . ?
N10 N9 C29 102.0(6) . . ?
C3 N7 Zn01 163.0(3) . . ?
C4 N2 C1 119.8(3) . . ?
C4 N2 Zn01 111.0(2) . . ?
C1 N2 Zn01 128.3(2) . . ?
C34 C29 C37 122.8(5) . . ?
C34 C29 N9 113.3(6) . . ?
C37 C29 N9 123.7(7) . . ?
C5 N3 C2 120.9(3) . . ?
C5 N3 Zn01 112.0(2) . . ?
C2 N3 Zn01 126.4(3) . . ?
C10 N1 C6 117.4(4) . . ?
C10 N1 Zn01 125.1(3) . . ?
C6 N1 Zn01 116.9(2) . . ?
C8 C1 C23 120.0(4) . . ?
C8 C1 N2 118.1(3) . . ?
C23 C1 N2 121.8(3) . . ?
N7 C3 S1 178.6(4) . . ?
C26 N4 C15 117.5(4) . . ?
C26 N4 Zn01 124.4(4) . . ?
C15 N4 Zn01 117.9(3) . . ?
N5 C12 S2 179.5(5) . . ?
C1 C8 C7 119.3(4) . . ?
C1 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
N1 C10 C20 123.4(4) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
N9 N10 C9 97.6(5) . . ?
N4 C15 C32 122.4(4) . . ?
N4 C15 C4 116.4(4) . . ?
C32 C15 C4 121.2(4) . . ?
N2 C4 C15 120.3(4) . . ?
N2 C4 H4 119.8 . . ?
C15 C4 H4 119.8 . . ?
N1 C6 C18 122.3(3) . . ?
N1 C6 C5 115.4(3) . . ?
C18 C6 C5 122.3(4) . . ?
C14 C2 C11 119.3(4) . . ?
C14 C2 N3 123.1(4) . . ?
C11 C2 N3 117.5(3) . . ?
C22 C11 C2 120.3(4) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
C13 C23 C1 120.4(4) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C12 N5 Zn01 166.7(4) . . ?
C23 C13 C9 119.9(4) . . ?
C23 C13 H13 120.1 . . ?
C9 C13 H13 120.1 . . ?
C6 C18 C24 118.9(4) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.7(4) . . ?
C13 C9 N10 110.9(4) . . ?
C7 C9 N10 128.3(5) . . ?
C27 C17 C28 120.6(4) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C9 C7 C8 119.6(4) . . ?
C9 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
N6 N8 C19 102.8(5) . . ?
C31 C38 C32 119.4(6) . . ?
C31 C38 H38 120.3 . . ?
C32 C38 H38 120.3 . . ?
C15 C32 C38 118.2(6) . . ?
C15 C32 H32 120.9 . . ?
C38 C32 H32 120.9 . . ?
C19 C16 C14 120.6(4) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N3 C5 C6 119.9(3) . . ?
N3 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C2 C14 C16 119.5(4) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C10 C20 C24 119.3(4) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C19 C22 C11 120.7(5) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C17 C27 C30 120.9(5) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C20 C24 C18 118.7(5) . . ?
C20 C24 H24 120.7 . . ?
C18 C24 H24 120.7 . . ?
C30 C21 C25 120.3(4) . . ?
C30 C21 N6 111.6(5) . . ?
C25 C21 N6 128.0(5) . . ?
C34 C35 C33 122.3(6) . . ?
C34 C35 H35 118.9 . . ?
C33 C35 H35 118.9 . . ?
C17 C28 C25 118.8(5) . . ?
C17 C28 H28 120.6 . . ?
C25 C28 H28 120.6 . . ?
C33 C36 C37 118.1(6) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
N4 C26 C31 122.8(6) . . ?
N4 C26 H26 118.6 . . ?
C31 C26 H26 118.6 . . ?
C22 C19 C16 119.6(4) . . ?
C22 C19 N8 110.6(5) . . ?
C16 C19 N8 129.8(5) . . ?
N8 N6 C21 102.1(5) . . ?
C38 C31 C26 119.5(6) . . ?
C38 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C35 C33 C36 120.2(5) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 118.4(6) . . ?
C29 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
C21 C30 C27 119.9(5) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C21 C25 C28 119.5(5) . . ?
C21 C25 H25 120.2 . . ?
C28 C25 H25 120.2 . . ?
C29 C37 C36 118.2(6) . . ?
C29 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?

_diffrn_measured_fraction_theta_max 0.743
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.743
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.042
####################################################################### 
# 
# 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_znaza270kd
_database_code_depnum_ccdc_archive 'CCDC 1492680'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1251(8)
_cell_length_b                   14.5335(12)
_cell_length_c                   17.1467(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.657(5)
_cell_angle_gamma                90.00
_cell_volume                     3761.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    13917
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_T_max  0.7132
_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      270(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            6447
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4954
_reflns_number_gt                3678
_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)+(0.0607P)²+3.4090P] 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         4954
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1238
_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
Zn01 Zn 0.71027(3) 0.28530(4) 0.44753(3) 0.0548(2) Uani 1 1 d . . .
S1 S 0.80781(8) 0.49663(9) 0.64709(7) 0.0654(4) Uani 1 1 d . . .
S2 S 0.56393(9) 0.07177(10) 0.60536(8) 0.0782(4) Uani 1 1 d . . .
N9 N 1.0863(4) 0.3957(3) 0.1870(3) 0.0883(14) Uani 1 1 d . . .
N7 N 0.7712(3) 0.3747(3) 0.5246(2) 0.0721(12) Uani 1 1 d . . .
N2 N 0.7302(2) 0.3805(2) 0.33836(18) 0.0444(8) Uani 1 1 d . . .
C29 C 1.1670(5) 0.4097(4) 0.1306(5) 0.096(2) Uani 1 1 d . . .
N3 N 0.6700(2) 0.1893(2) 0.34401(19) 0.0481(9) Uani 1 1 d . . .
N1 N 0.8277(2) 0.2138(2) 0.4223(2) 0.0527(9) Uani 1 1 d . . .
C1 C 0.8057(3) 0.3857(3) 0.2924(2) 0.0444(10) Uani 1 1 d . . .
C3 C 0.7857(3) 0.4249(3) 0.5758(3) 0.0532(11) Uani 1 1 d . . .
N4 N 0.5892(2) 0.3602(3) 0.4260(2) 0.0600(10) Uani 1 1 d . . .
C12 C 0.6204(3) 0.1461(3) 0.5596(2) 0.0533(11) Uani 1 1 d . . .
C8 C 0.8872(3) 0.3985(3) 0.3303(3) 0.0550(11) Uani 1 1 d . . .
H8 H 0.8926 0.4046 0.3844 0.066 Uiso 1 1 calc R . .
C10 C 0.9053(3) 0.2231(3) 0.4625(3) 0.0661(13) Uani 1 1 d . . .
H10 H 0.9078 0.2559 0.5092 0.079 Uiso 1 1 calc R . .
N10 N 1.0267(4) 0.4025(3) 0.1454(3) 0.1055(19) Uani 1 1 d . . .
C15 C 0.5803(3) 0.4106(3) 0.3603(3) 0.0583(12) Uani 1 1 d . . .
C4 C 0.6581(3) 0.4190(3) 0.3146(2) 0.0523(11) Uani 1 1 d . . .
H4 H 0.6549 0.4524 0.2683 0.063 Uiso 1 1 calc R . .
C6 C 0.8251(3) 0.1651(3) 0.3551(2) 0.0504(11) Uani 1 1 d . . .
C2 C 0.5848(3) 0.1803(3) 0.3061(3) 0.0508(11) Uani 1 1 d . . .
C11 C 0.5162(3) 0.1571(4) 0.3522(3) 0.0690(14) Uani 1 1 d . . .
H11 H 0.5279 0.1454 0.4052 0.083 Uiso 1 1 calc R . .
C23 C 0.7975(3) 0.3757(3) 0.2123(3) 0.0639(13) Uani 1 1 d . . .
H23 H 0.7420 0.3660 0.1872 0.077 Uiso 1 1 calc R . .
N5 N 0.6600(3) 0.1987(3) 0.5266(2) 0.0808(13) Uani 1 1 d . . .
C13 C 0.8704(4) 0.3801(4) 0.1695(3) 0.0802(16) Uani 1 1 d . . .
H13 H 0.8647 0.3742 0.1154 0.096 Uiso 1 1 calc R . .
C18 C 0.8998(3) 0.1266(3) 0.3273(3) 0.0685(13) Uani 1 1 d . . .
H18 H 0.8962 0.0929 0.2812 0.082 Uiso 1 1 calc R . .
C9 C 0.9521(4) 0.3932(3) 0.2072(3) 0.0716(15) Uani 1 1 d . . .
C17 C 0.0345(3) 0.1154(3) 0.0780(3) 0.0715(14) Uani 1 1 d . . .
H17 H -0.0233 0.1053 0.0581 0.086 Uiso 1 1 calc R . .
C7 C 0.9613(3) 0.4022(3) 0.2874(3) 0.0674(14) Uani 1 1 d . . .
H7 H 1.0171 0.4107 0.3124 0.081 Uiso 1 1 calc R . .
N8 N 0.3105(3) 0.1604(3) 0.2211(3) 0.0886(14) Uani 1 1 d . . .
C38 C 0.4309(4) 0.4464(6) 0.3823(6) 0.115(2) Uani 1 1 d . . .
H38 H 0.3773 0.4747 0.3675 0.138 Uiso 1 1 calc R . .
C32 C 0.5019(4) 0.4538(4) 0.3366(4) 0.0858(17) Uani 1 1 d . . .
H32 H 0.4973 0.4875 0.2903 0.103 Uiso 1 1 calc R . .
C16 C 0.4797(4) 0.1950(4) 0.1972(3) 0.0753(15) Uani 1 1 d . . .
H16 H 0.4671 0.2085 0.1447 0.090 Uiso 1 1 calc R . .
C5 C 0.7365(3) 0.1530(3) 0.3156(2) 0.0533(11) Uani 1 1 d . . .
H5 H 0.7296 0.1187 0.2698 0.064 Uiso 1 1 calc R . .
C14 C 0.5664(3) 0.2009(3) 0.2284(3) 0.0639(13) Uani 1 1 d . . .
H14 H 0.6115 0.2186 0.1972 0.077 Uiso 1 1 calc R . .
C20 C 0.9819(4) 0.1858(4) 0.4375(4) 0.0791(16) Uani 1 1 d . . .
H20 H 1.0349 0.1928 0.4674 0.095 Uiso 1 1 calc R . .
C22 C 0.4311(3) 0.1513(4) 0.3197(4) 0.0773(15) Uani 1 1 d . . .
H22 H 0.3855 0.1347 0.3508 0.093 Uiso 1 1 calc R . .
C27 C 0.1028(4) 0.0976(4) 0.0330(3) 0.0830(16) Uani 1 1 d . . .
H27 H 0.0912 0.0758 -0.0176 0.100 Uiso 1 1 calc R . .
C24 C 0.9803(3) 0.1384(4) 0.3689(3) 0.0779(15) Uani 1 1 d . . .
H24 H 1.0321 0.1146 0.3504 0.093 Uiso 1 1 calc R . .
C21 C 0.2053(3) 0.1418(4) 0.1342(4) 0.0770(16) Uani 1 1 d . . .
C35 C 1.3200(4) 0.4039(4) 0.1262(4) 0.0944(19) Uani 1 1 d . . .
H35 H 1.3752 0.3896 0.1501 0.113 Uiso 1 1 calc R . .
C28 C 0.0496(4) 0.1478(4) 0.1518(4) 0.0814(16) Uani 1 1 d . . .
H28 H 0.0028 0.1608 0.1827 0.098 Uiso 1 1 calc R . .
C36 C 1.2338(5) 0.4591(4) 0.0146(4) 0.0993(19) Uani 1 1 d . . .
H36 H 1.2300 0.4831 -0.0357 0.119 Uiso 1 1 calc R . .
C26 C 0.5196(4) 0.3538(4) 0.4693(4) 0.0904(18) Uani 1 1 d . . .
H26 H 0.5246 0.3189 0.5148 0.108 Uiso 1 1 calc R . .
C19 C 0.4126(3) 0.1697(4) 0.2422(4) 0.0734(15) Uani 1 1 d . . .
N6 N 0.3071(4) 0.1535(3) 0.1554(3) 0.0943(15) Uani 1 1 d . . .
C31 C 0.4405(5) 0.3971(6) 0.4492(6) 0.116(2) Uani 1 1 d . . .
H31 H 0.3937 0.3925 0.4816 0.139 Uiso 1 1 calc R . .
C33 C 1.3151(4) 0.4380(4) 0.0514(4) 0.0954(19) Uani 1 1 d . . .
H33 H 1.3666 0.4469 0.0255 0.114 Uiso 1 1 calc R . .
C34 C 1.2466(5) 0.3906(4) 0.1664(4) 0.098(2) Uani 1 1 d . . .
H34 H 1.2512 0.3687 0.2174 0.118 Uiso 1 1 calc R . .
C30 C 0.1879(4) 0.1113(4) 0.0606(4) 0.0864(17) Uani 1 1 d . . .
H30 H 0.2341 0.0995 0.0287 0.104 Uiso 1 1 calc R . .
C25 C 0.1380(4) 0.1612(4) 0.1804(4) 0.0867(17) Uani 1 1 d . . .
H25 H 0.1503 0.1832 0.2309 0.104 Uiso 1 1 calc R . .
C37 C 1.1573(4) 0.4437(4) 0.0544(5) 0.100(2) Uani 1 1 d . . .
H37 H 1.1015 0.4558 0.0308 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
Zn01 N7 2.032(4) . ?
Zn01 N5 2.033(4) . ?
Zn01 N1 2.126(4) . ?
Zn01 N4 2.142(4) . ?
Zn01 N3 2.309(3) . ?
Zn01 N2 2.362(3) . ?
S1 C3 1.625(5) . ?
S2 C12 1.612(5) . ?
N9 N10 1.118(6) . ?
N9 C29 1.617(8) . ?
N7 C3 1.151(5) . ?
N2 C4 1.269(5) . ?
N2 C1 1.431(5) . ?
C29 C34 1.344(9) . ?
C29 C37 1.396(9) . ?
N3 C5 1.260(5) . ?
N3 C2 1.412(5) . ?
N1 C10 1.330(5) . ?
N1 C6 1.351(5) . ?
C1 C8 1.369(5) . ?
C1 C23 1.379(6) . ?
N4 C26 1.329(6) . ?
N4 C15 1.343(6) . ?
C12 N5 1.142(6) . ?
C8 C7 1.380(6) . ?
C8 H8 0.9300 . ?
C10 C20 1.372(7) . ?
C10 H10 0.9300 . ?
N10 C9 1.602(7) . ?
C15 C32 1.380(7) . ?
C15 C4 1.460(6) . ?
C4 H4 0.9300 . ?
C6 C18 1.372(6) . ?
C6 C5 1.474(6) . ?
C2 C14 1.376(6) . ?
C2 C11 1.384(6) . ?
C11 C22 1.373(6) . ?
C11 H11 0.9300 . ?
C23 C13 1.363(7) . ?
C23 H23 0.9300 . ?
C13 C9 1.372(7) . ?
C13 H13 0.9300 . ?
C18 C24 1.382(6) . ?
C18 H18 0.9300 . ?
C9 C7 1.379(7) . ?
C17 C27 1.352(7) . ?
C17 C28 1.357(7) . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
N8 N6 1.129(5) . ?
N8 C19 1.569(7) . ?
C38 C31 1.353(10) . ?
C38 C32 1.373(9) . ?
C38 H38 0.9300 . ?
C32 H32 0.9300 . ?
C16 C19 1.364(8) . ?
C16 C14 1.387(6) . ?
C16 H16 0.9300 . ?
C5 H5 0.9300 . ?
C14 H14 0.9300 . ?
C20 C24 1.362(7) . ?
C20 H20 0.9300 . ?
C22 C19 1.366(7) . ?
C22 H22 0.9300 . ?
C27 C30 1.357(7) . ?
C27 H27 0.9300 . ?
C24 H24 0.9300 . ?
C21 C30 1.347(8) . ?
C21 C25 1.359(8) . ?
C21 N6 1.569(7) . ?
C35 C34 1.357(8) . ?
C35 C33 1.373(8) . ?
C35 H35 0.9300 . ?
C28 C25 1.408(7) . ?
C28 H28 0.9300 . ?
C36 C33 1.380(8) . ?
C36 C37 1.398(8) . ?
C36 H36 0.9300 . ?
C26 C31 1.376(9) . ?
C26 H26 0.9300 . ?
C31 H31 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C25 H25 0.9300 . ?
C37 H37 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Zn01 N5 97.79(17) . . ?
N7 Zn01 N1 95.45(15) . . ?
N5 Zn01 N1 100.73(16) . . ?
N7 Zn01 N4 97.75(15) . . ?
N5 Zn01 N4 94.44(17) . . ?
N1 Zn01 N4 158.33(14) . . ?
N7 Zn01 N3 166.64(15) . . ?
N5 Zn01 N3 92.70(15) . . ?
N1 Zn01 N3 74.39(13) . . ?
N4 Zn01 N3 89.62(14) . . ?
N7 Zn01 N2 93.74(14) . . ?
N5 Zn01 N2 164.41(15) . . ?
N1 Zn01 N2 88.53(12) . . ?
N4 Zn01 N2 73.55(13) . . ?
N3 Zn01 N2 77.61(11) . . ?
N10 N9 C29 102.5(6) . . ?
C3 N7 Zn01 163.2(4) . . ?
C4 N2 C1 120.0(3) . . ?
C4 N2 Zn01 111.2(3) . . ?
C1 N2 Zn01 127.9(2) . . ?
C34 C29 C37 122.5(6) . . ?
C34 C29 N9 112.9(7) . . ?
C37 C29 N9 124.5(7) . . ?
C5 N3 C2 120.7(4) . . ?
C5 N3 Zn01 111.8(3) . . ?
C2 N3 Zn01 126.7(3) . . ?
C10 N1 C6 118.2(4) . . ?
C10 N1 Zn01 124.5(3) . . ?
C6 N1 Zn01 116.8(3) . . ?
C8 C1 C23 120.5(4) . . ?
C8 C1 N2 118.2(4) . . ?
C23 C1 N2 121.3(4) . . ?
N7 C3 S1 178.9(5) . . ?
C26 N4 C15 117.8(5) . . ?
C26 N4 Zn01 124.5(4) . . ?
C15 N4 Zn01 117.4(3) . . ?
N5 C12 S2 179.4(4) . . ?
C1 C8 C7 119.3(4) . . ?
C1 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
N1 C10 C20 122.2(5) . . ?
N1 C10 H10 118.9 . . ?
C20 C10 H10 118.9 . . ?
N9 N10 C9 98.2(6) . . ?
N4 C15 C32 122.3(5) . . ?
N4 C15 C4 117.0(4) . . ?
C32 C15 C4 120.7(5) . . ?
N2 C4 C15 119.8(4) . . ?
N2 C4 H4 120.1 . . ?
C15 C4 H4 120.1 . . ?
N1 C6 C18 122.0(4) . . ?
N1 C6 C5 115.5(4) . . ?
C18 C6 C5 122.5(4) . . ?
C14 C2 C11 119.5(4) . . ?
C14 C2 N3 123.2(4) . . ?
C11 C2 N3 117.0(4) . . ?
C22 C11 C2 120.0(5) . . ?
C22 C11 H11 120.0 . . ?
C2 C11 H11 120.0 . . ?
C13 C23 C1 120.5(4) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C12 N5 Zn01 167.0(4) . . ?
C23 C13 C9 119.2(5) . . ?
C23 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?
C6 C18 C24 119.2(5) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C13 C9 C7 120.9(4) . . ?
C13 C9 N10 110.5(5) . . ?
C7 C9 N10 128.4(5) . . ?
C27 C17 C28 120.6(5) . . ?
C27 C17 H17 119.7 . . ?
C28 C17 H17 119.7 . . ?
C9 C7 C8 119.6(4) . . ?
C9 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
N6 N8 C19 102.6(5) . . ?
C31 C38 C32 118.7(6) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?
C38 C32 C15 119.0(6) . . ?
C38 C32 H32 120.5 . . ?
C15 C32 H32 120.5 . . ?
C19 C16 C14 121.2(5) . . ?
C19 C16 H16 119.4 . . ?
C14 C16 H16 119.4 . . ?
N3 C5 C6 119.8(4) . . ?
N3 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C2 C14 C16 119.2(5) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
C24 C20 C10 120.1(5) . . ?
C24 C20 H20 119.9 . . ?
C10 C20 H20 119.9 . . ?
C19 C22 C11 120.7(5) . . ?
C19 C22 H22 119.6 . . ?
C11 C22 H22 119.6 . . ?
C17 C27 C30 121.0(5) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C20 C24 C18 118.3(5) . . ?
C20 C24 H24 120.9 . . ?
C18 C24 H24 120.9 . . ?
C30 C21 C25 120.4(5) . . ?
C30 C21 N6 112.6(6) . . ?
C25 C21 N6 127.1(6) . . ?
C34 C35 C33 122.0(6) . . ?
C34 C35 H35 119.0 . . ?
C33 C35 H35 119.0 . . ?
C17 C28 C25 118.2(5) . . ?
C17 C28 H28 120.9 . . ?
C25 C28 H28 120.9 . . ?
C33 C36 C37 118.9(7) . . ?
C33 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
N4 C26 C31 122.3(6) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C16 C19 C22 119.3(4) . . ?
C16 C19 N8 130.5(5) . . ?
C22 C19 N8 110.1(5) . . ?
N8 N6 C21 102.9(5) . . ?
C38 C31 C26 119.9(6) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C35 C33 C36 120.0(6) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 118.5(7) . . ?
C29 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
C21 C30 C27 119.9(5) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C21 C25 C28 119.9(5) . . ?
C21 C25 H25 120.1 . . ?
C28 C25 H25 120.1 . . ?
C29 C37 C36 118.2(6) . . ?
C29 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?

_diffrn_measured_fraction_theta_max 0.747
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.747
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.048
####################################################################### 
# 
# 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_znaza120km
_database_code_depnum_ccdc_archive 'CCDC 1492681'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.0920(6)
_cell_length_b                   14.2288(9)
_cell_length_c                   17.1508(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.277(3)
_cell_angle_gamma                90.00
_cell_volume                     3672.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    14345
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6374
_exptl_absorpt_correction_T_max  0.7078
_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      120(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            6194
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.04
_reflns_number_total             4793
_reflns_number_gt                4404
_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)+(0.0410P)²+6.4675P] 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         4793
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1105
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
Zn01 Zn 0.71800(3) 0.28340(3) 0.44611(2) 0.02489(15) Uani 1 1 d . . .
S1 S 0.80767(6) 0.50194(7) 0.64748(4) 0.0301(2) Uani 1 1 d . . .
S2 S 0.56221(7) 0.07290(7) 0.60333(5) 0.0357(3) Uani 1 1 d . . .
N9 N 1.0945(2) 0.3953(2) 0.18456(17) 0.0321(7) Uani 1 1 d . . .
N7 N 0.7801(2) 0.3737(2) 0.52461(16) 0.0336(7) Uani 1 1 d . . .
N2 N 0.73171(19) 0.38134(19) 0.33844(14) 0.0220(6) Uani 1 1 d . . .
C29 C 1.1676(3) 0.4100(3) 0.1353(2) 0.0323(9) Uani 1 1 d . . .
N3 N 0.67612(19) 0.18742(19) 0.34195(14) 0.0225(6) Uani 1 1 d . . .
N1 N 0.83539(19) 0.21254(19) 0.41841(15) 0.0249(7) Uani 1 1 d . . .
C1 C 0.8042(2) 0.3864(2) 0.29050(17) 0.0222(7) Uani 1 1 d . . .
C3 C 0.7911(2) 0.4266(3) 0.57614(18) 0.0247(8) Uani 1 1 d . . .
N4 N 0.59424(19) 0.3585(2) 0.42884(16) 0.0284(7) Uani 1 1 d . . .
C12 C 0.6257(2) 0.1431(3) 0.55790(18) 0.0271(8) Uani 1 1 d . . .
C8 C 0.8890(2) 0.4014(2) 0.32631(18) 0.0256(8) Uani 1 1 d . . .
H8 H 0.8970 0.4089 0.3814 0.031 Uiso 1 1 calc R . .
C10 C 0.9145(2) 0.2214(2) 0.45810(19) 0.0303(9) Uani 1 1 d . . .
H10 H 0.9177 0.2541 0.5065 0.036 Uiso 1 1 calc R . .
N10 N 1.0201(2) 0.4005(2) 0.14884(17) 0.0347(8) Uani 1 1 d . . .
C15 C 0.5811(2) 0.4100(3) 0.36254(19) 0.0282(8) Uani 1 1 d . . .
C4 C 0.6576(2) 0.4189(2) 0.31522(18) 0.0258(8) Uani 1 1 d . . .
H4 H 0.6521 0.4526 0.2673 0.031 Uiso 1 1 calc R . .
C6 C 0.8320(2) 0.1637(2) 0.35032(18) 0.0243(8) Uani 1 1 d . . .
C2 C 0.5884(2) 0.1786(2) 0.30621(18) 0.0244(8) Uani 1 1 d . . .
C11 C 0.5217(2) 0.1550(3) 0.35475(19) 0.0304(9) Uani 1 1 d . . .
H11 H 0.5362 0.1417 0.4085 0.036 Uiso 1 1 calc R . .
C23 C 0.7931(2) 0.3733(3) 0.20994(18) 0.0304(9) Uani 1 1 d . . .
H23 H 0.7357 0.3613 0.1854 0.036 Uiso 1 1 calc R . .
N5 N 0.6711(2) 0.1931(2) 0.52545(16) 0.0372(8) Uani 1 1 d . . .
C13 C 0.8662(3) 0.3777(3) 0.1655(2) 0.0335(9) Uani 1 1 d . . .
H13 H 0.8585 0.3698 0.1104 0.040 Uiso 1 1 calc R . .
C18 C 0.9062(2) 0.1267(3) 0.3204(2) 0.0313(9) Uani 1 1 d . . .
H18 H 0.9017 0.0939 0.2720 0.038 Uiso 1 1 calc R . .
C9 C 0.9496(2) 0.3935(2) 0.20080(19) 0.0281(8) Uani 1 1 d . . .
C17 C 0.0334(2) 0.1153(2) 0.0775(2) 0.0315(9) Uani 1 1 d . . .
H17 H -0.0270 0.1041 0.0604 0.038 Uiso 1 1 calc R . .
C7 C 0.9611(2) 0.4053(2) 0.2820(2) 0.0296(8) Uani 1 1 d . . .
H7 H 1.0187 0.4160 0.3064 0.036 Uiso 1 1 calc R . .
N8 N 0.3197(2) 0.1612(2) 0.22166(16) 0.0327(7) Uani 1 1 d . . .
C38 C 0.4315(3) 0.4424(3) 0.3892(3) 0.0517(12) Uani 1 1 d . . .
H38 H 0.3754 0.4707 0.3757 0.062 Uiso 1 1 calc R . .
C32 C 0.5004(3) 0.4511(3) 0.3407(2) 0.0393(10) Uani 1 1 d . . .
H32 H 0.4921 0.4850 0.2930 0.047 Uiso 1 1 calc R . .
C16 C 0.4791(2) 0.1949(3) 0.19760(19) 0.0307(9) Uani 1 1 d . . .
H16 H 0.4643 0.2092 0.1441 0.037 Uiso 1 1 calc R . .
C5 C 0.7419(2) 0.1514(2) 0.31114(18) 0.0247(8) Uani 1 1 d . . .
H5 H 0.7336 0.1172 0.2636 0.030 Uiso 1 1 calc R . .
C14 C 0.5670(2) 0.1994(2) 0.22770(19) 0.0283(8) Uani 1 1 d . . .
H14 H 0.6123 0.2167 0.1949 0.034 Uiso 1 1 calc R . .
C20 C 0.9919(3) 0.1852(3) 0.4319(2) 0.0354(9) Uani 1 1 d . . .
H20 H 1.0469 0.1930 0.4619 0.043 Uiso 1 1 calc R . .
C22 C 0.4344(3) 0.1510(3) 0.3242(2) 0.0329(9) Uani 1 1 d . . .
H22 H 0.3888 0.1356 0.3573 0.040 Uiso 1 1 calc R . .
C27 C 0.0996(3) 0.0961(3) 0.0287(2) 0.0355(9) Uani 1 1 d . . .
H27 H 0.0846 0.0728 -0.0225 0.043 Uiso 1 1 calc R . .
C24 C 0.9881(3) 0.1378(3) 0.3620(2) 0.0354(9) Uani 1 1 d . . .
H24 H 1.0405 0.1131 0.3425 0.042 Uiso 1 1 calc R . .
C21 C 0.2094(2) 0.1421(3) 0.1288(2) 0.0297(8) Uani 1 1 d . . .
C35 C 1.3250(3) 0.4034(3) 0.1297(2) 0.0389(10) Uani 1 1 d . . .
H35 H 1.3822 0.3890 0.1536 0.047 Uiso 1 1 calc R . .
C28 C 0.0552(3) 0.1509(3) 0.1514(2) 0.0358(9) Uani 1 1 d . . .
H28 H 0.0095 0.1658 0.1846 0.043 Uiso 1 1 calc R . .
C36 C 1.2333(3) 0.4589(3) 0.0190(2) 0.0416(10) Uani 1 1 d . . .
H36 H 1.2275 0.4830 -0.0328 0.050 Uiso 1 1 calc R . .
C26 C 0.5271(3) 0.3508(3) 0.4748(2) 0.0397(10) Uani 1 1 d . . .
H26 H 0.5362 0.3153 0.5216 0.048 Uiso 1 1 calc R . .
C19 C 0.4126(2) 0.1695(2) 0.24553(19) 0.0274(8) Uani 1 1 d . . .
N6 N 0.3034(2) 0.1508(2) 0.15012(16) 0.0314(7) Uani 1 1 d . . .
C31 C 0.4461(3) 0.3914(3) 0.4580(3) 0.0496(11) Uani 1 1 d . . .
H31 H 0.4003 0.3848 0.4928 0.060 Uiso 1 1 calc R . .
C33 C 1.3169(3) 0.4379(3) 0.0543(2) 0.0417(10) Uani 1 1 d . . .
H33 H 1.3684 0.4472 0.0265 0.050 Uiso 1 1 calc R . .
C34 C 1.2507(3) 0.3896(3) 0.1710(2) 0.0362(9) Uani 1 1 d . . .
H34 H 1.2566 0.3665 0.2231 0.043 Uiso 1 1 calc R . .
C30 C 0.1874(3) 0.1104(3) 0.0539(2) 0.0337(9) Uani 1 1 d . . .
H30 H 0.2327 0.0984 0.0196 0.040 Uiso 1 1 calc R . .
C25 C 0.1428(3) 0.1647(3) 0.1774(2) 0.0352(9) Uani 1 1 d . . .
H25 H 0.1576 0.1896 0.2281 0.042 Uiso 1 1 calc R . .
C37 C 1.1583(3) 0.4446(3) 0.0597(2) 0.0383(10) Uani 1 1 d . . .
H37 H 1.1009 0.4584 0.0359 0.046 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
Zn01 N5 2.037(3) . ?
Zn01 N7 2.038(3) . ?
Zn01 N1 2.123(3) . ?
Zn01 N4 2.153(3) . ?
Zn01 N3 2.299(3) . ?
Zn01 N2 2.335(3) . ?
S1 C3 1.632(3) . ?
S2 C12 1.623(4) . ?
N9 N10 1.240(4) . ?
N9 C29 1.454(5) . ?
N7 C3 1.163(4) . ?
N2 C4 1.276(4) . ?
N2 C1 1.419(4) . ?
C29 C37 1.383(5) . ?
C29 C34 1.385(5) . ?
N3 C5 1.267(4) . ?
N3 C2 1.423(4) . ?
N1 C10 1.336(4) . ?
N1 C6 1.357(4) . ?
C1 C23 1.392(4) . ?
C1 C8 1.394(5) . ?
N4 C26 1.334(5) . ?
N4 C15 1.354(5) . ?
C12 N5 1.158(5) . ?
C8 C7 1.374(5) . ?
C8 H8 0.9500 . ?
C10 C20 1.381(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.442(5) . ?
C15 C32 1.378(5) . ?
C15 C4 1.465(5) . ?
C4 H4 0.9500 . ?
C6 C18 1.370(5) . ?
C6 C5 1.481(4) . ?
C2 C14 1.393(4) . ?
C2 C11 1.394(5) . ?
C11 C22 1.383(5) . ?
C11 H11 0.9500 . ?
C23 C13 1.388(5) . ?
C23 H23 0.9500 . ?
C13 C9 1.373(5) . ?
C13 H13 0.9500 . ?
C18 C24 1.389(5) . ?
C18 H18 0.9500 . ?
C9 C7 1.400(5) . ?
C17 C27 1.377(5) . ?
C17 C28 1.382(5) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.242(4) . ?
N8 C19 1.435(5) . ?
C38 C32 1.385(6) . ?
C38 C31 1.389(6) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C14 1.389(5) . ?
C16 C19 1.392(5) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.373(5) . ?
C20 H20 0.9500 . ?
C22 C19 1.389(5) . ?
C22 H22 0.9500 . ?
C27 C30 1.377(5) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.380(5) . ?
C21 C25 1.390(5) . ?
C21 N6 1.443(5) . ?
C35 C33 1.381(6) . ?
C35 C34 1.384(5) . ?
C35 H35 0.9500 . ?
C28 C25 1.377(5) . ?
C28 H28 0.9500 . ?
C36 C37 1.390(6) . ?
C36 C33 1.391(6) . ?
C36 H36 0.9500 . ?
C26 C31 1.364(6) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.00(12) . . ?
N5 Zn01 N1 100.77(12) . . ?
N7 Zn01 N1 95.56(11) . . ?
N5 Zn01 N4 93.69(12) . . ?
N7 Zn01 N4 97.42(12) . . ?
N1 Zn01 N4 159.20(10) . . ?
N5 Zn01 N3 93.16(11) . . ?
N7 Zn01 N3 166.87(11) . . ?
N1 Zn01 N3 74.32(10) . . ?
N4 Zn01 N3 90.16(10) . . ?
N5 Zn01 N2 163.90(11) . . ?
N7 Zn01 N2 94.75(11) . . ?
N1 Zn01 N2 88.96(10) . . ?
N4 Zn01 N2 73.86(11) . . ?
N3 Zn01 N2 77.03(9) . . ?
N10 N9 C29 113.7(3) . . ?
C3 N7 Zn01 160.4(3) . . ?
C4 N2 C1 119.6(3) . . ?
C4 N2 Zn01 111.7(2) . . ?
C1 N2 Zn01 127.3(2) . . ?
C37 C29 C34 120.9(4) . . ?
C37 C29 N9 124.6(4) . . ?
C34 C29 N9 114.5(3) . . ?
C5 N3 C2 121.2(3) . . ?
C5 N3 Zn01 112.7(2) . . ?
C2 N3 Zn01 125.5(2) . . ?
C10 N1 C6 117.5(3) . . ?
C10 N1 Zn01 124.8(2) . . ?
C6 N1 Zn01 117.2(2) . . ?
C23 C1 C8 119.8(3) . . ?
C23 C1 N2 121.8(3) . . ?
C8 C1 N2 118.3(3) . . ?
N7 C3 S1 178.9(4) . . ?
C26 N4 C15 118.1(3) . . ?
C26 N4 Zn01 124.5(3) . . ?
C15 N4 Zn01 117.0(2) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 123.0(3) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
N9 N10 C9 111.9(3) . . ?
N4 C15 C32 121.9(4) . . ?
N4 C15 C4 116.1(3) . . ?
C32 C15 C4 122.0(3) . . ?
N2 C4 C15 119.9(3) . . ?
N2 C4 H4 120.0 . . ?
C15 C4 H4 120.0 . . ?
N1 C6 C18 122.6(3) . . ?
N1 C6 C5 115.1(3) . . ?
C18 C6 C5 122.2(3) . . ?
C14 C2 C11 120.2(3) . . ?
C14 C2 N3 122.6(3) . . ?
C11 C2 N3 117.0(3) . . ?
C22 C11 C2 119.6(3) . . ?
C22 C11 H11 120.2 . . ?
C2 C11 H11 120.2 . . ?
C13 C23 C1 119.8(3) . . ?
C13 C23 H23 120.1 . . ?
C1 C23 H23 120.1 . . ?
C12 N5 Zn01 162.9(3) . . ?
C9 C13 C23 120.3(3) . . ?
C9 C13 H13 119.8 . . ?
C23 C13 H13 119.8 . . ?
C6 C18 C24 119.0(3) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C13 C9 C7 120.0(3) . . ?
C13 C9 N10 115.7(3) . . ?
C7 C9 N10 124.3(3) . . ?
C27 C17 C28 119.8(3) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C8 C7 C9 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C9 C7 H7 120.0 . . ?
N6 N8 C19 114.1(3) . . ?
C32 C38 C31 118.6(4) . . ?
C32 C38 H38 120.7 . . ?
C31 C38 H38 120.7 . . ?
C15 C32 C38 119.2(4) . . ?
C15 C32 H32 120.4 . . ?
C38 C32 H32 120.4 . . ?
C14 C16 C19 120.2(3) . . ?
C14 C16 H16 119.9 . . ?
C19 C16 H16 119.9 . . ?
N3 C5 C6 119.0(3) . . ?
N3 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C16 C14 C2 119.7(3) . . ?
C16 C14 H14 120.1 . . ?
C2 C14 H14 120.1 . . ?
C24 C20 C10 119.1(3) . . ?
C24 C20 H20 120.5 . . ?
C10 C20 H20 120.5 . . ?
C11 C22 C19 120.7(3) . . ?
C11 C22 H22 119.7 . . ?
C19 C22 H22 119.7 . . ?
C17 C27 C30 120.3(3) . . ?
C17 C27 H27 119.8 . . ?
C30 C27 H27 119.8 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 119.9(3) . . ?
C30 C21 N6 115.4(3) . . ?
C25 C21 N6 124.7(3) . . ?
C33 C35 C34 120.8(4) . . ?
C33 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C25 C28 C17 120.4(4) . . ?
C25 C28 H28 119.8 . . ?
C17 C28 H28 119.8 . . ?
C37 C36 C33 119.8(4) . . ?
C37 C36 H36 120.1 . . ?
C33 C36 H36 120.1 . . ?
N4 C26 C31 123.3(4) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C22 C19 C16 119.6(3) . . ?
C22 C19 N8 114.6(3) . . ?
C16 C19 N8 125.8(3) . . ?
N8 N6 C21 112.3(3) . . ?
C26 C31 C38 118.9(4) . . ?
C26 C31 H31 120.5 . . ?
C38 C31 H31 120.5 . . ?
C35 C33 C36 119.9(4) . . ?
C35 C33 H33 120.1 . . ?
C36 C33 H33 120.1 . . ?
C35 C34 C29 119.1(4) . . ?
C35 C34 H34 120.5 . . ?
C29 C34 H34 120.5 . . ?
C27 C30 C21 120.0(4) . . ?
C27 C30 H30 120.0 . . ?
C21 C30 H30 120.0 . . ?
C28 C25 C21 119.5(3) . . ?
C28 C25 H25 120.2 . . ?
C21 C25 H25 120.2 . . ?
C29 C37 C36 119.6(4) . . ?
C29 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.738
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.737
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_znaza250kd
_database_code_depnum_ccdc_archive 'CCDC 1492682'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1195(7)
_cell_length_b                   14.4879(11)
_cell_length_c                   17.1458(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.756(4)
_cell_angle_gamma                90.00
_cell_volume                     3747.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    14105
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_T_max  0.7124
_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            6247
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4853
_reflns_number_gt                3908
_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)+(0.0909P)²+3.9881P] 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         4853
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1690
_refine_ls_wR_factor_gt          0.1567
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
Zn01 Zn 0.71114(3) 0.28512(4) 0.44739(3) 0.0507(2) Uani 1 1 d . . .
S1 S 0.80773(8) 0.49745(10) 0.64727(7) 0.0604(4) Uani 1 1 d . . .
S2 S 0.56367(10) 0.07170(11) 0.60512(8) 0.0720(4) Uani 1 1 d . . .
N9 N 1.0874(4) 0.3956(3) 0.1866(3) 0.0807(14) Uani 1 1 d . . .
N7 N 0.7723(3) 0.3745(3) 0.5247(3) 0.0679(12) Uani 1 1 d . . .
N2 N 0.7303(2) 0.3808(2) 0.33804(19) 0.0421(8) Uani 1 1 d . . .
C29 C 1.1688(6) 0.4094(4) 0.1324(5) 0.088(2) Uani 1 1 d . . .
N3 N 0.6707(3) 0.1893(2) 0.3436(2) 0.0444(9) Uani 1 1 d . . .
N1 N 0.8286(2) 0.2137(2) 0.4219(2) 0.0494(9) Uani 1 1 d . . .
C1 C 0.8055(3) 0.3861(3) 0.2922(2) 0.0425(10) Uani 1 1 d . . .
C3 C 0.7864(3) 0.4251(3) 0.5762(3) 0.0494(11) Uani 1 1 d . . .
N4 N 0.5897(3) 0.3600(3) 0.4262(2) 0.0564(10) Uani 1 1 d . . .
C12 C 0.6207(3) 0.1458(3) 0.5596(2) 0.0506(11) Uani 1 1 d . . .
C8 C 0.8876(3) 0.3987(3) 0.3295(3) 0.0514(11) Uani 1 1 d . . .
H8 H 0.8936 0.4045 0.3842 0.062 Uiso 1 1 calc R . .
C10 C 0.9069(4) 0.2225(3) 0.4616(3) 0.0633(14) Uani 1 1 d . . .
H10 H 0.9097 0.2556 0.5088 0.076 Uiso 1 1 calc R . .
N10 N 1.0253(4) 0.4023(4) 0.1457(4) 0.0958(19) Uani 1 1 d . . .
C15 C 0.5798(3) 0.4115(3) 0.3605(3) 0.0566(12) Uani 1 1 d . . .
C4 C 0.6577(3) 0.4195(3) 0.3148(3) 0.0500(11) Uani 1 1 d . . .
H4 H 0.6542 0.4535 0.2680 0.060 Uiso 1 1 calc R . .
C6 C 0.8261(3) 0.1645(3) 0.3546(2) 0.0479(11) Uani 1 1 d . . .
C2 C 0.5850(3) 0.1801(3) 0.3061(3) 0.0477(11) Uani 1 1 d . . .
C11 C 0.5166(3) 0.1564(4) 0.3527(3) 0.0625(13) Uani 1 1 d . . .
H11 H 0.5289 0.1440 0.4061 0.075 Uiso 1 1 calc R . .
C23 C 0.7972(3) 0.3755(4) 0.2119(3) 0.0599(13) Uani 1 1 d . . .
H23 H 0.7410 0.3650 0.1867 0.072 Uiso 1 1 calc R . .
N5 N 0.6612(3) 0.1983(3) 0.5266(3) 0.0752(13) Uani 1 1 d . . .
C13 C 0.8699(4) 0.3801(4) 0.1689(3) 0.0731(15) Uani 1 1 d . . .
H13 H 0.8639 0.3742 0.1142 0.088 Uiso 1 1 calc R . .
C18 C 0.9004(4) 0.1272(4) 0.3262(3) 0.0630(13) Uani 1 1 d . . .
H18 H 0.8968 0.0943 0.2789 0.076 Uiso 1 1 calc R . .
C9 C 0.9518(4) 0.3933(3) 0.2062(3) 0.0663(15) Uani 1 1 d . . .
C17 C 0.0340(4) 0.1150(4) 0.0769(3) 0.0663(15) Uani 1 1 d . . .
H17 H -0.0244 0.1046 0.0568 0.080 Uiso 1 1 calc R . .
C7 C 0.9613(3) 0.4027(3) 0.2865(3) 0.0635(14) Uani 1 1 d . . .
H7 H 1.0177 0.4117 0.3117 0.076 Uiso 1 1 calc R . .
N8 N 0.3121(4) 0.1607(3) 0.2215(3) 0.0800(14) Uani 1 1 d . . .
C38 C 0.4309(5) 0.4465(6) 0.3827(6) 0.112(3) Uani 1 1 d . . .
H38 H 0.3768 0.4759 0.3684 0.134 Uiso 1 1 calc R . .
C32 C 0.5014(4) 0.4540(4) 0.3370(4) 0.0796(17) Uani 1 1 d . . .
H32 H 0.4962 0.4878 0.2902 0.096 Uiso 1 1 calc R . .
C16 C 0.4789(4) 0.1947(4) 0.1974(3) 0.0713(16) Uani 1 1 d . . .
H16 H 0.4657 0.2078 0.1442 0.086 Uiso 1 1 calc R . .
C5 C 0.7368(3) 0.1531(3) 0.3149(3) 0.0493(11) Uani 1 1 d . . .
H5 H 0.7295 0.1190 0.2683 0.059 Uiso 1 1 calc R . .
C14 C 0.5663(4) 0.2010(3) 0.2282(3) 0.0596(13) Uani 1 1 d . . .
H14 H 0.6117 0.2191 0.1965 0.072 Uiso 1 1 calc R . .
C20 C 0.9833(4) 0.1857(4) 0.4368(4) 0.0734(16) Uani 1 1 d . . .
H20 H 1.0370 0.1928 0.4670 0.088 Uiso 1 1 calc R . .
C22 C 0.4312(4) 0.1511(4) 0.3207(4) 0.0726(15) Uani 1 1 d . . .
H22 H 0.3854 0.1344 0.3525 0.087 Uiso 1 1 calc R . .
C27 C 0.1022(4) 0.0972(4) 0.0325(4) 0.0775(16) Uani 1 1 d . . .
H27 H 0.0905 0.0743 -0.0184 0.093 Uiso 1 1 calc R . .
C24 C 0.9808(4) 0.1385(4) 0.3678(4) 0.0742(16) Uani 1 1 d . . .
H24 H 1.0330 0.1141 0.3490 0.089 Uiso 1 1 calc R . .
C21 C 0.2062(3) 0.1415(4) 0.1334(4) 0.0683(15) Uani 1 1 d . . .
C35 C 1.3206(4) 0.4039(4) 0.1274(4) 0.0854(19) Uani 1 1 d . . .
H35 H 1.3767 0.3896 0.1511 0.103 Uiso 1 1 calc R . .
C28 C 0.0495(4) 0.1481(4) 0.1512(4) 0.0753(16) Uani 1 1 d . . .
H28 H 0.0024 0.1615 0.1825 0.090 Uiso 1 1 calc R . .
C36 C 1.2339(5) 0.4592(5) 0.0155(4) 0.0914(19) Uani 1 1 d . . .
H36 H 1.2301 0.4834 -0.0355 0.110 Uiso 1 1 calc R . .
C26 C 0.5202(4) 0.3540(4) 0.4690(4) 0.0831(18) Uani 1 1 d . . .
H26 H 0.5259 0.3192 0.5153 0.100 Uiso 1 1 calc R . .
C19 C 0.4118(3) 0.1699(4) 0.2429(4) 0.0654(15) Uani 1 1 d . . .
N6 N 0.3051(4) 0.1523(3) 0.1541(3) 0.0820(14) Uani 1 1 d . . .
C31 C 0.4408(5) 0.3955(6) 0.4495(6) 0.108(3) Uani 1 1 d . . .
H31 H 0.3933 0.3890 0.4819 0.129 Uiso 1 1 calc R . .
C33 C 1.3151(5) 0.4382(4) 0.0525(4) 0.0842(18) Uani 1 1 d . . .
H33 H 1.3671 0.4473 0.0264 0.101 Uiso 1 1 calc R . .
C34 C 1.2477(5) 0.3901(4) 0.1682(5) 0.090(2) Uani 1 1 d . . .
H34 H 1.2527 0.3679 0.2198 0.107 Uiso 1 1 calc R . .
C30 C 0.1875(4) 0.1116(4) 0.0595(4) 0.0776(16) Uani 1 1 d . . .
H30 H 0.2337 0.1007 0.0266 0.093 Uiso 1 1 calc R . .
C25 C 0.1391(5) 0.1619(4) 0.1797(4) 0.0830(18) Uani 1 1 d . . .
H25 H 0.1519 0.1850 0.2305 0.100 Uiso 1 1 calc R . .
C37 C 1.1573(4) 0.4438(5) 0.0554(5) 0.096(2) Uani 1 1 d . . .
H37 H 1.1006 0.4560 0.0319 0.115 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
Zn01 N7 2.032(4) . ?
Zn01 N5 2.032(5) . ?
Zn01 N1 2.125(4) . ?
Zn01 N4 2.143(4) . ?
Zn01 N3 2.308(3) . ?
Zn01 N2 2.364(3) . ?
S1 C3 1.624(5) . ?
S2 C12 1.611(5) . ?
N9 N10 1.139(6) . ?
N9 C29 1.603(8) . ?
N7 C3 1.156(6) . ?
N2 C4 1.273(5) . ?
N2 C1 1.428(6) . ?
C29 C34 1.336(10) . ?
C29 C37 1.411(10) . ?
N3 C5 1.257(6) . ?
N3 C2 1.414(5) . ?
N1 C10 1.333(6) . ?
N1 C6 1.355(6) . ?
C1 C8 1.371(6) . ?
C1 C23 1.382(6) . ?
N4 C26 1.323(7) . ?
N4 C15 1.352(6) . ?
C12 N5 1.148(6) . ?
C8 C7 1.376(7) . ?
C8 H8 0.9400 . ?
C10 C20 1.364(8) . ?
C10 H10 0.9400 . ?
N10 C9 1.575(8) . ?
C15 C32 1.372(8) . ?
C15 C4 1.461(7) . ?
C4 H4 0.9400 . ?
C6 C18 1.365(7) . ?
C6 C5 1.481(6) . ?
C2 C14 1.380(6) . ?
C2 C11 1.391(7) . ?
C11 C22 1.371(7) . ?
C11 H11 0.9400 . ?
C23 C13 1.365(7) . ?
C23 H23 0.9400 . ?
C13 C9 1.369(8) . ?
C13 H13 0.9400 . ?
C18 C24 1.378(7) . ?
C18 H18 0.9400 . ?
C9 C7 1.382(8) . ?
C17 C27 1.346(8) . ?
C17 C28 1.367(8) . ?
C17 H17 0.9400 . ?
C7 H7 0.9400 . ?
N8 N6 1.160(6) . ?
N8 C19 1.533(7) . ?
C38 C31 1.363(11) . ?
C38 C32 1.369(10) . ?
C38 H38 0.9400 . ?
C32 H32 0.9400 . ?
C16 C19 1.367(8) . ?
C16 C14 1.394(7) . ?
C16 H16 0.9400 . ?
C5 H5 0.9400 . ?
C14 H14 0.9400 . ?
C20 C24 1.365(8) . ?
C20 H20 0.9400 . ?
C22 C19 1.374(8) . ?
C22 H22 0.9400 . ?
C27 C30 1.357(8) . ?
C27 H27 0.9400 . ?
C24 H24 0.9400 . ?
C21 C30 1.352(8) . ?
C21 C25 1.361(9) . ?
C21 N6 1.521(7) . ?
C35 C34 1.358(9) . ?
C35 C33 1.373(9) . ?
C35 H35 0.9400 . ?
C28 C25 1.424(8) . ?
C28 H28 0.9400 . ?
C36 C33 1.378(9) . ?
C36 C37 1.402(9) . ?
C36 H36 0.9400 . ?
C26 C31 1.366(10) . ?
C26 H26 0.9400 . ?
C31 H31 0.9400 . ?
C33 H33 0.9400 . ?
C34 H34 0.9400 . ?
C30 H30 0.9400 . ?
C25 H25 0.9400 . ?
C37 H37 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 Zn01 N5 97.58(18) . . ?
N7 Zn01 N1 95.38(16) . . ?
N5 Zn01 N1 100.84(18) . . ?
N7 Zn01 N4 97.82(17) . . ?
N5 Zn01 N4 94.31(18) . . ?
N1 Zn01 N4 158.39(14) . . ?
N7 Zn01 N3 166.60(16) . . ?
N5 Zn01 N3 92.94(16) . . ?
N1 Zn01 N3 74.41(13) . . ?
N4 Zn01 N3 89.61(14) . . ?
N7 Zn01 N2 93.99(15) . . ?
N5 Zn01 N2 164.29(16) . . ?
N1 Zn01 N2 88.56(13) . . ?
N4 Zn01 N2 73.55(14) . . ?
N3 Zn01 N2 77.37(12) . . ?
N10 N9 C29 105.4(6) . . ?
C3 N7 Zn01 162.8(4) . . ?
C4 N2 C1 120.4(4) . . ?
C4 N2 Zn01 111.1(3) . . ?
C1 N2 Zn01 127.7(3) . . ?
C34 C29 C37 123.8(6) . . ?
C34 C29 N9 113.8(7) . . ?
C37 C29 N9 122.3(7) . . ?
C5 N3 C2 120.7(4) . . ?
C5 N3 Zn01 112.1(3) . . ?
C2 N3 Zn01 126.6(3) . . ?
C10 N1 C6 117.3(4) . . ?
C10 N1 Zn01 125.1(3) . . ?
C6 N1 Zn01 117.0(3) . . ?
C8 C1 C23 120.1(4) . . ?
C8 C1 N2 118.7(4) . . ?
C23 C1 N2 121.2(4) . . ?
N7 C3 S1 178.6(5) . . ?
C26 N4 C15 116.8(5) . . ?
C26 N4 Zn01 125.1(4) . . ?
C15 N4 Zn01 117.9(3) . . ?
N5 C12 S2 179.5(5) . . ?
C1 C8 C7 119.6(4) . . ?
C1 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
N1 C10 C20 123.1(5) . . ?
N1 C10 H10 118.5 . . ?
C20 C10 H10 118.5 . . ?
N9 N10 C9 100.2(6) . . ?
N4 C15 C32 122.6(5) . . ?
N4 C15 C4 116.2(4) . . ?
C32 C15 C4 121.2(5) . . ?
N2 C4 C15 120.4(4) . . ?
N2 C4 H4 119.8 . . ?
C15 C4 H4 119.8 . . ?
N1 C6 C18 122.3(4) . . ?
N1 C6 C5 115.1(4) . . ?
C18 C6 C5 122.6(4) . . ?
C14 C2 C11 119.8(4) . . ?
C14 C2 N3 122.9(4) . . ?
C11 C2 N3 117.1(4) . . ?
C22 C11 C2 120.0(5) . . ?
C22 C11 H11 120.0 . . ?
C2 C11 H11 120.0 . . ?
C13 C23 C1 120.5(5) . . ?
C13 C23 H23 119.7 . . ?
C1 C23 H23 119.7 . . ?
C12 N5 Zn01 166.5(4) . . ?
C23 C13 C9 119.3(5) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C6 C18 C24 119.2(5) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C13 C9 C7 120.7(5) . . ?
C13 C9 N10 111.1(5) . . ?
C7 C9 N10 128.1(5) . . ?
C27 C17 C28 120.2(5) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C8 C7 C9 119.7(5) . . ?
C8 C7 H7 120.2 . . ?
C9 C7 H7 120.2 . . ?
N6 N8 C19 105.9(5) . . ?
C31 C38 C32 118.5(7) . . ?
C31 C38 H38 120.7 . . ?
C32 C38 H38 120.7 . . ?
C38 C32 C15 119.2(7) . . ?
C38 C32 H32 120.4 . . ?
C15 C32 H32 120.4 . . ?
C19 C16 C14 121.4(5) . . ?
C19 C16 H16 119.3 . . ?
C14 C16 H16 119.3 . . ?
N3 C5 C6 119.9(4) . . ?
N3 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C2 C14 C16 118.8(5) . . ?
C2 C14 H14 120.6 . . ?
C16 C14 H14 120.6 . . ?
C10 C20 C24 119.3(5) . . ?
C10 C20 H20 120.3 . . ?
C24 C20 H20 120.3 . . ?
C11 C22 C19 120.8(5) . . ?
C11 C22 H22 119.6 . . ?
C19 C22 H22 119.6 . . ?
C17 C27 C30 121.6(6) . . ?
C17 C27 H27 119.2 . . ?
C30 C27 H27 119.2 . . ?
C20 C24 C18 118.7(5) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 119.9(5) . . ?
C30 C21 N6 113.1(6) . . ?
C25 C21 N6 126.9(6) . . ?
C34 C35 C33 122.3(7) . . ?
C34 C35 H35 118.9 . . ?
C33 C35 H35 118.9 . . ?
C17 C28 C25 118.1(6) . . ?
C17 C28 H28 121.0 . . ?
C25 C28 H28 121.0 . . ?
C33 C36 C37 118.6(7) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
N4 C26 C31 123.6(7) . . ?
N4 C26 H26 118.2 . . ?
C31 C26 H26 118.2 . . ?
C16 C19 C22 119.1(4) . . ?
C16 C19 N8 129.8(5) . . ?
C22 C19 N8 111.1(5) . . ?
N8 N6 C21 105.5(5) . . ?
C38 C31 C26 119.4(7) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C35 C33 C36 120.5(6) . . ?
C35 C33 H33 119.7 . . ?
C36 C33 H33 119.7 . . ?
C29 C34 C35 117.5(7) . . ?
C29 C34 H34 121.2 . . ?
C35 C34 H34 121.2 . . ?
C21 C30 C27 120.3(6) . . ?
C21 C30 H30 119.8 . . ?
C27 C30 H30 119.8 . . ?
C21 C25 C28 119.8(6) . . ?
C21 C25 H25 120.1 . . ?
C28 C25 H25 120.1 . . ?
C36 C37 C29 117.2(6) . . ?
C36 C37 H37 121.4 . . ?
C29 C37 H37 121.4 . . ?

_diffrn_measured_fraction_theta_max 0.734
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.734
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_znaza290kd
_database_code_depnum_ccdc_archive 'CCDC 1492683'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1300(8)
_cell_length_b                   14.5806(13)
_cell_length_c                   17.1485(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.558(5)
_cell_angle_gamma                90.00
_cell_volume                     3775.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    13976
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_T_max  0.7141
_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      290(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            6496
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4961
_reflns_number_gt                3519
_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)+(0.0518P)²+3.4507P] 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         4961
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
Zn01 Zn 0.70942(3) 0.28541(4) 0.44773(3) 0.0567(2) Uani 1 1 d . . .
S1 S 0.80772(8) 0.49570(10) 0.64697(7) 0.0682(4) Uani 1 1 d . . .
S2 S 0.56421(9) 0.07188(11) 0.60561(8) 0.0825(4) Uani 1 1 d . . .
N9 N 1.0854(4) 0.3959(3) 0.1872(3) 0.0955(16) Uani 1 1 d . . .
N7 N 0.7703(3) 0.3746(3) 0.5245(2) 0.0759(12) Uani 1 1 d . . .
N2 N 0.7304(2) 0.3803(2) 0.33831(19) 0.0459(8) Uani 1 1 d . . .
C29 C 1.1658(6) 0.4101(4) 0.1289(6) 0.103(2) Uani 1 1 d . . .
N3 N 0.6699(2) 0.1897(2) 0.34407(19) 0.0492(9) Uani 1 1 d . . .
N1 N 0.8267(2) 0.2139(2) 0.4227(2) 0.0542(9) Uani 1 1 d . . .
C1 C 0.8058(3) 0.3855(3) 0.2924(2) 0.0463(10) Uani 1 1 d . . .
C3 C 0.7853(3) 0.4243(3) 0.5756(3) 0.0542(12) Uani 1 1 d . . .
N4 N 0.5885(2) 0.3603(3) 0.4251(2) 0.0616(10) Uani 1 1 d . . .
C12 C 0.6197(3) 0.1466(4) 0.5596(2) 0.0547(12) Uani 1 1 d . . .
C8 C 0.8874(3) 0.3984(3) 0.3306(3) 0.0584(12) Uani 1 1 d . . .
H8 H 0.8925 0.4046 0.3847 0.070 Uiso 1 1 calc R . .
C10 C 0.9048(4) 0.2231(3) 0.4626(3) 0.0686(14) Uani 1 1 d . . .
H10 H 0.9071 0.2560 0.5091 0.082 Uiso 1 1 calc R . .
N10 N 1.0278(4) 0.4026(4) 0.1448(4) 0.112(2) Uani 1 1 d . . .
C15 C 0.5800(3) 0.4107(3) 0.3597(3) 0.0599(12) Uani 1 1 d . . .
C4 C 0.6584(3) 0.4189(3) 0.3149(3) 0.0535(11) Uani 1 1 d . . .
H4 H 0.6557 0.4527 0.2688 0.064 Uiso 1 1 calc R . .
C6 C 0.8243(3) 0.1652(3) 0.3557(3) 0.0525(11) Uani 1 1 d . . .
C2 C 0.5842(3) 0.1803(3) 0.3062(3) 0.0523(11) Uani 1 1 d . . .
C11 C 0.5155(3) 0.1571(3) 0.3514(3) 0.0692(14) Uani 1 1 d . . .
H11 H 0.5268 0.1451 0.4043 0.083 Uiso 1 1 calc R . .
C23 C 0.7986(3) 0.3759(3) 0.2125(3) 0.0647(13) Uani 1 1 d . . .
H23 H 0.7432 0.3664 0.1872 0.078 Uiso 1 1 calc R . .
N5 N 0.6591(3) 0.1993(3) 0.5268(2) 0.0838(14) Uani 1 1 d . . .
C13 C 0.8711(4) 0.3802(4) 0.1704(3) 0.0844(16) Uani 1 1 d . . .
H13 H 0.8656 0.3745 0.1163 0.101 Uiso 1 1 calc R . .
C18 C 0.8985(4) 0.1272(3) 0.3279(3) 0.0716(14) Uani 1 1 d . . .
H18 H 0.8952 0.0940 0.2815 0.086 Uiso 1 1 calc R . .
C9 C 0.9531(4) 0.3932(3) 0.2082(3) 0.0749(16) Uani 1 1 d . . .
C17 C 0.0352(4) 0.1156(4) 0.0779(4) 0.0750(15) Uani 1 1 d . . .
H17 H -0.0225 0.1057 0.0576 0.090 Uiso 1 1 calc R . .
C7 C 0.9618(3) 0.4023(3) 0.2878(3) 0.0696(14) Uani 1 1 d . . .
H7 H 1.0174 0.4109 0.3129 0.083 Uiso 1 1 calc R . .
N8 N 0.3090(4) 0.1602(3) 0.2209(3) 0.0940(16) Uani 1 1 d . . .
C38 C 0.4309(4) 0.4461(6) 0.3820(6) 0.120(3) Uani 1 1 d . . .
H38 H 0.3775 0.4750 0.3679 0.144 Uiso 1 1 calc R . .
C32 C 0.5016(4) 0.4541(4) 0.3357(4) 0.0890(17) Uani 1 1 d . . .
H32 H 0.4968 0.4877 0.2895 0.107 Uiso 1 1 calc R . .
C16 C 0.4794(4) 0.1950(4) 0.1972(3) 0.0809(16) Uani 1 1 d . . .
H16 H 0.4670 0.2084 0.1446 0.097 Uiso 1 1 calc R . .
C5 C 0.7361(3) 0.1536(3) 0.3162(3) 0.0533(11) Uani 1 1 d . . .
H5 H 0.7293 0.1193 0.2705 0.064 Uiso 1 1 calc R . .
C14 C 0.5660(3) 0.2008(3) 0.2291(3) 0.0667(13) Uani 1 1 d . . .
H14 H 0.6113 0.2185 0.1981 0.080 Uiso 1 1 calc R . .
C20 C 0.9813(4) 0.1864(4) 0.4385(4) 0.0809(16) Uani 1 1 d . . .
H20 H 1.0342 0.1939 0.4684 0.097 Uiso 1 1 calc R . .
C22 C 0.4308(3) 0.1516(4) 0.3187(4) 0.0804(16) Uani 1 1 d . . .
H22 H 0.3851 0.1352 0.3497 0.097 Uiso 1 1 calc R . .
C27 C 0.1038(4) 0.0979(4) 0.0336(4) 0.0908(17) Uani 1 1 d . . .
H27 H 0.0928 0.0758 -0.0169 0.109 Uiso 1 1 calc R . .
C24 C 0.9793(3) 0.1388(4) 0.3701(4) 0.0839(16) Uani 1 1 d . . .
H24 H 1.0310 0.1145 0.3519 0.101 Uiso 1 1 calc R . .
C21 C 0.2048(3) 0.1415(4) 0.1350(4) 0.0799(17) Uani 1 1 d . . .
C35 C 1.3190(4) 0.4044(4) 0.1252(5) 0.099(2) Uani 1 1 d . . .
H35 H 1.3740 0.3901 0.1492 0.119 Uiso 1 1 calc R . .
C28 C 0.0493(4) 0.1475(4) 0.1511(4) 0.0864(17) Uani 1 1 d . . .
H28 H 0.0021 0.1606 0.1816 0.104 Uiso 1 1 calc R . .
C36 C 1.2342(5) 0.4595(5) 0.0138(4) 0.108(2) Uani 1 1 d . . .
H36 H 1.2308 0.4838 -0.0364 0.129 Uiso 1 1 calc R . .
C26 C 0.5191(4) 0.3535(4) 0.4677(4) 0.0927(18) Uani 1 1 d . . .
H26 H 0.5238 0.3183 0.5130 0.111 Uiso 1 1 calc R . .
C19 C 0.4126(3) 0.1696(4) 0.2424(4) 0.0750(16) Uani 1 1 d . . .
N6 N 0.3080(4) 0.1535(3) 0.1562(3) 0.1032(17) Uani 1 1 d . . .
C31 C 0.4400(5) 0.3966(6) 0.4476(6) 0.122(3) Uani 1 1 d . . .
H31 H 0.3929 0.3912 0.4796 0.146 Uiso 1 1 calc R . .
C33 C 1.3146(4) 0.4385(5) 0.0508(4) 0.098(2) Uani 1 1 d . . .
H33 H 1.3664 0.4475 0.0253 0.118 Uiso 1 1 calc R . .
C34 C 1.2450(6) 0.3905(4) 0.1653(4) 0.101(2) Uani 1 1 d . . .
H34 H 1.2491 0.3683 0.2162 0.121 Uiso 1 1 calc R . .
C30 C 0.1882(4) 0.1116(4) 0.0615(4) 0.0926(18) Uani 1 1 d . . .
H30 H 0.2348 0.1003 0.0299 0.111 Uiso 1 1 calc R . .
C25 C 0.1370(4) 0.1605(4) 0.1804(4) 0.0915(18) Uani 1 1 d . . .
H25 H 0.1487 0.1822 0.2310 0.110 Uiso 1 1 calc R . .
C37 C 1.1568(4) 0.4434(5) 0.0535(5) 0.106(2) Uani 1 1 d . . .
H37 H 1.1011 0.4550 0.0295 0.127 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
Zn01 N7 2.030(4) . ?
Zn01 N5 2.031(5) . ?
Zn01 N1 2.125(4) . ?
Zn01 N4 2.145(4) . ?
Zn01 N3 2.309(3) . ?
Zn01 N2 2.368(3) . ?
S1 C3 1.627(5) . ?
S2 C12 1.611(6) . ?
N9 N10 1.105(6) . ?
N9 C29 1.635(8) . ?
N7 C3 1.148(5) . ?
N2 C4 1.268(5) . ?
N2 C1 1.429(5) . ?
C29 C34 1.346(10) . ?
C29 C37 1.380(10) . ?
N3 C5 1.252(5) . ?
N3 C2 1.420(5) . ?
N1 C10 1.334(5) . ?
N1 C6 1.351(5) . ?
C1 C8 1.374(6) . ?
C1 C23 1.374(6) . ?
N4 C26 1.319(6) . ?
N4 C15 1.341(6) . ?
C12 N5 1.141(6) . ?
C8 C7 1.382(6) . ?
C8 H8 0.9300 . ?
C10 C20 1.362(7) . ?
C10 H10 0.9300 . ?
N10 C9 1.622(8) . ?
C15 C32 1.384(7) . ?
C15 C4 1.458(6) . ?
C4 H4 0.9300 . ?
C6 C18 1.364(6) . ?
C6 C5 1.468(6) . ?
C2 C14 1.367(6) . ?
C2 C11 1.375(6) . ?
C11 C22 1.369(6) . ?
C11 H11 0.9300 . ?
C23 C13 1.352(7) . ?
C23 H23 0.9300 . ?
C13 C9 1.378(7) . ?
C13 H13 0.9300 . ?
C18 C24 1.391(7) . ?
C18 H18 0.9300 . ?
C9 C7 1.370(7) . ?
C17 C28 1.343(7) . ?
C17 C27 1.350(7) . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
N8 N6 1.113(6) . ?
N8 C19 1.594(7) . ?
C38 C31 1.337(10) . ?
C38 C32 1.376(9) . ?
C38 H38 0.9300 . ?
C32 H32 0.9300 . ?
C16 C19 1.362(8) . ?
C16 C14 1.391(7) . ?
C16 H16 0.9300 . ?
C5 H5 0.9300 . ?
C14 H14 0.9300 . ?
C20 C24 1.363(7) . ?
C20 H20 0.9300 . ?
C22 C19 1.346(8) . ?
C22 H22 0.9300 . ?
C27 C30 1.350(7) . ?
C27 H27 0.9300 . ?
C24 H24 0.9300 . ?
C21 C30 1.342(8) . ?
C21 C25 1.355(8) . ?
C21 N6 1.591(7) . ?
C35 C34 1.365(8) . ?
C35 C33 1.367(8) . ?
C35 H35 0.9300 . ?
C28 C25 1.403(7) . ?
C28 H28 0.9300 . ?
C36 C33 1.372(8) . ?
C36 C37 1.410(9) . ?
C36 H36 0.9300 . ?
C26 C31 1.377(9) . ?
C26 H26 0.9300 . ?
C31 H31 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C25 H25 0.9300 . ?
C37 H37 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Zn01 N5 97.86(18) . . ?
N7 Zn01 N1 95.41(15) . . ?
N5 Zn01 N1 100.59(17) . . ?
N7 Zn01 N4 97.96(16) . . ?
N5 Zn01 N4 94.84(18) . . ?
N1 Zn01 N4 157.98(14) . . ?
N7 Zn01 N3 166.32(15) . . ?
N5 Zn01 N3 92.90(15) . . ?
N1 Zn01 N3 74.22(13) . . ?
N4 Zn01 N3 89.50(14) . . ?
N7 Zn01 N2 93.56(15) . . ?
N5 Zn01 N2 164.68(15) . . ?
N1 Zn01 N2 88.41(13) . . ?
N4 Zn01 N2 73.39(14) . . ?
N3 Zn01 N2 77.53(11) . . ?
N10 N9 C29 99.9(7) . . ?
C3 N7 Zn01 163.6(4) . . ?
C4 N2 C1 120.1(4) . . ?
C4 N2 Zn01 110.9(3) . . ?
C1 N2 Zn01 128.2(3) . . ?
C34 C29 C37 122.8(6) . . ?
C34 C29 N9 111.3(8) . . ?
C37 C29 N9 125.7(8) . . ?
C5 N3 C2 121.0(4) . . ?
C5 N3 Zn01 111.9(3) . . ?
C2 N3 Zn01 126.5(3) . . ?
C10 N1 C6 117.7(4) . . ?
C10 N1 Zn01 124.9(3) . . ?
C6 N1 Zn01 116.8(3) . . ?
C8 C1 C23 120.2(4) . . ?
C8 C1 N2 118.0(4) . . ?
C23 C1 N2 121.7(4) . . ?
N7 C3 S1 179.0(5) . . ?
C26 N4 C15 117.8(5) . . ?
C26 N4 Zn01 124.1(4) . . ?
C15 N4 Zn01 117.8(3) . . ?
N5 C12 S2 179.7(5) . . ?
C1 C8 C7 119.3(4) . . ?
C1 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
N1 C10 C20 123.2(5) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
N9 N10 C9 96.0(6) . . ?
N4 C15 C32 122.3(5) . . ?
N4 C15 C4 116.6(4) . . ?
C32 C15 C4 121.1(5) . . ?
N2 C4 C15 120.4(4) . . ?
N2 C4 H4 119.8 . . ?
C15 C4 H4 119.8 . . ?
N1 C6 C18 122.1(4) . . ?
N1 C6 C5 115.4(4) . . ?
C18 C6 C5 122.5(4) . . ?
C14 C2 C11 119.0(4) . . ?
C14 C2 N3 123.0(4) . . ?
C11 C2 N3 117.8(4) . . ?
C22 C11 C2 120.3(5) . . ?
C22 C11 H11 119.8 . . ?
C2 C11 H11 119.8 . . ?
C13 C23 C1 120.7(4) . . ?
C13 C23 H23 119.6 . . ?
C1 C23 H23 119.6 . . ?
C12 N5 Zn01 166.9(4) . . ?
C23 C13 C9 119.4(5) . . ?
C23 C13 H13 120.3 . . ?
C9 C13 H13 120.3 . . ?
C6 C18 C24 118.9(5) . . ?
C6 C18 H18 120.5 . . ?
C24 C18 H18 120.5 . . ?
C7 C9 C13 120.7(4) . . ?
C7 C9 N10 129.2(5) . . ?
C13 C9 N10 109.9(5) . . ?
C28 C17 C27 120.6(5) . . ?
C28 C17 H17 119.7 . . ?
C27 C17 H17 119.7 . . ?
C9 C7 C8 119.6(4) . . ?
C9 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
N6 N8 C19 101.0(6) . . ?
C31 C38 C32 119.2(6) . . ?
C31 C38 H38 120.4 . . ?
C32 C38 H38 120.4 . . ?
C38 C32 C15 118.2(6) . . ?
C38 C32 H32 120.9 . . ?
C15 C32 H32 120.9 . . ?
C19 C16 C14 120.4(5) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N3 C5 C6 120.1(4) . . ?
N3 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C2 C14 C16 119.7(5) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C10 C20 C24 119.1(5) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C19 C22 C11 121.1(5) . . ?
C19 C22 H22 119.5 . . ?
C11 C22 H22 119.5 . . ?
C17 C27 C30 121.1(6) . . ?
C17 C27 H27 119.5 . . ?
C30 C27 H27 119.5 . . ?
C20 C24 C18 118.8(5) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.2(5) . . ?
C30 C21 N6 112.0(6) . . ?
C25 C21 N6 127.8(6) . . ?
C34 C35 C33 122.0(7) . . ?
C34 C35 H35 119.0 . . ?
C33 C35 H35 119.0 . . ?
C17 C28 C25 118.3(5) . . ?
C17 C28 H28 120.9 . . ?
C25 C28 H28 120.9 . . ?
C33 C36 C37 118.6(7) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
N4 C26 C31 122.4(6) . . ?
N4 C26 H26 118.8 . . ?
C31 C26 H26 118.8 . . ?
C22 C19 C16 119.5(4) . . ?
C22 C19 N8 110.3(5) . . ?
C16 C19 N8 130.2(5) . . ?
N8 N6 C21 100.9(6) . . ?
C38 C31 C26 120.0(6) . . ?
C38 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C35 C33 C36 120.2(6) . . ?
C35 C33 H33 119.9 . . ?
C36 C33 H33 119.9 . . ?
C29 C34 C35 118.0(7) . . ?
C29 C34 H34 121.0 . . ?
C35 C34 H34 121.0 . . ?
C21 C30 C27 119.9(6) . . ?
C21 C30 H30 120.1 . . ?
C27 C30 H30 120.1 . . ?
C21 C25 C28 120.0(6) . . ?
C21 C25 H25 120.0 . . ?
C28 C25 H25 120.0 . . ?
C29 C37 C36 118.3(6) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.746
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.746
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_znaza230kd
_database_code_depnum_ccdc_archive 'CCDC 1492684'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1135(7)
_cell_length_b                   14.4437(10)
_cell_length_c                   17.1447(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.836(4)
_cell_angle_gamma                90.00
_cell_volume                     3734.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    14578
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_T_max  0.7116
_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            6364
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4904
_reflns_number_gt                4098
_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)+(0.0578P)²+4.8508P] 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         4904
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1330
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Zn01 Zn 0.71213(3) 0.28493(3) 0.44715(2) 0.04693(19) Uani 1 1 d . . .
S1 S 0.80768(7) 0.49821(8) 0.64735(6) 0.0557(3) Uani 1 1 d . . .
S2 S 0.56340(8) 0.07167(9) 0.60494(7) 0.0665(4) Uani 1 1 d . . .
N9 N 1.0887(3) 0.3953(3) 0.1865(2) 0.0737(12) Uani 1 1 d . . .
N7 N 0.7736(2) 0.3746(3) 0.5247(2) 0.0621(10) Uani 1 1 d . . .
N2 N 0.7308(2) 0.3808(2) 0.33828(17) 0.0387(7) Uani 1 1 d . . .
C29 C 1.1692(5) 0.4092(4) 0.1333(4) 0.0786(17) Uani 1 1 d . . .
N3 N 0.6712(2) 0.1889(2) 0.34343(17) 0.0416(8) Uani 1 1 d . . .
N1 N 0.8294(2) 0.2135(2) 0.42129(18) 0.0453(8) Uani 1 1 d . . .
C1 C 0.8049(3) 0.3861(2) 0.2919(2) 0.0384(9) Uani 1 1 d . . .
C3 C 0.7870(2) 0.4255(3) 0.5761(2) 0.0461(10) Uani 1 1 d . . .
N4 N 0.5904(2) 0.3599(2) 0.4263(2) 0.0526(9) Uani 1 1 d . . .
C12 C 0.6212(3) 0.1452(3) 0.5589(2) 0.0476(10) Uani 1 1 d . . .
C8 C 0.8878(3) 0.3989(3) 0.3290(2) 0.0476(10) Uani 1 1 d . . .
H8 H 0.8941 0.4047 0.3837 0.057 Uiso 1 1 calc R . .
C10 C 0.9080(3) 0.2225(3) 0.4615(3) 0.0566(12) Uani 1 1 d . . .
H10 H 0.9107 0.2554 0.5089 0.068 Uiso 1 1 calc R . .
N10 N 1.0245(3) 0.4021(3) 0.1465(3) 0.0868(15) Uani 1 1 d . . .
C15 C 0.5802(3) 0.4113(3) 0.3604(3) 0.0507(10) Uani 1 1 d . . .
C4 C 0.6578(3) 0.4195(3) 0.3148(2) 0.0463(10) Uani 1 1 d . . .
H4 H 0.6542 0.4534 0.2679 0.056 Uiso 1 1 calc R . .
C6 C 0.8270(3) 0.1644(3) 0.3538(2) 0.0439(10) Uani 1 1 d . . .
C2 C 0.5853(3) 0.1799(3) 0.3063(2) 0.0443(10) Uani 1 1 d . . .
C11 C 0.5175(3) 0.1563(3) 0.3529(3) 0.0567(11) Uani 1 1 d . . .
H11 H 0.5303 0.1436 0.4062 0.068 Uiso 1 1 calc R . .
C23 C 0.7966(3) 0.3754(3) 0.2115(2) 0.0565(11) Uani 1 1 d . . .
H23 H 0.7404 0.3649 0.1861 0.068 Uiso 1 1 calc R . .
N5 N 0.6625(3) 0.1973(3) 0.5265(2) 0.0695(11) Uani 1 1 d . . .
C13 C 0.8697(3) 0.3800(4) 0.1686(3) 0.0679(13) Uani 1 1 d . . .
H13 H 0.8636 0.3738 0.1139 0.082 Uiso 1 1 calc R . .
C18 C 0.9017(3) 0.1273(3) 0.3254(3) 0.0582(12) Uani 1 1 d . . .
H18 H 0.8981 0.0944 0.2779 0.070 Uiso 1 1 calc R . .
C9 C 0.9510(3) 0.3936(3) 0.2053(3) 0.0592(12) Uani 1 1 d . . .
C17 C 0.0343(3) 0.1151(3) 0.0771(3) 0.0600(12) Uani 1 1 d . . .
H17 H -0.0244 0.1043 0.0575 0.072 Uiso 1 1 calc R . .
C7 C 0.9611(3) 0.4031(3) 0.2858(3) 0.0583(12) Uani 1 1 d . . .
H7 H 1.0177 0.4123 0.3107 0.070 Uiso 1 1 calc R . .
N8 N 0.3130(3) 0.1609(3) 0.2212(2) 0.0734(12) Uani 1 1 d . . .
C38 C 0.4304(4) 0.4453(5) 0.3840(5) 0.100(2) Uani 1 1 d . . .
H38 H 0.3758 0.4737 0.3696 0.120 Uiso 1 1 calc R . .
C32 C 0.5011(4) 0.4534(4) 0.3376(3) 0.0750(15) Uani 1 1 d . . .
H32 H 0.4953 0.4873 0.2907 0.090 Uiso 1 1 calc R . .
C16 C 0.4786(3) 0.1951(3) 0.1974(3) 0.0646(13) Uani 1 1 d . . .
H16 H 0.4651 0.2088 0.1444 0.077 Uiso 1 1 calc R . .
C5 C 0.7376(3) 0.1529(3) 0.3141(2) 0.0453(10) Uani 1 1 d . . .
H5 H 0.7302 0.1189 0.2674 0.054 Uiso 1 1 calc R . .
C14 C 0.5663(3) 0.2005(3) 0.2283(2) 0.0552(11) Uani 1 1 d . . .
H14 H 0.6118 0.2180 0.1965 0.066 Uiso 1 1 calc R . .
C20 C 0.9847(3) 0.1855(3) 0.4362(3) 0.0686(14) Uani 1 1 d . . .
H20 H 1.0386 0.1924 0.4664 0.082 Uiso 1 1 calc R . .
C22 C 0.4313(3) 0.1513(3) 0.3214(3) 0.0666(13) Uani 1 1 d . . .
H22 H 0.3856 0.1351 0.3533 0.080 Uiso 1 1 calc R . .
C27 C 0.1018(3) 0.0973(4) 0.0320(3) 0.0688(13) Uani 1 1 d . . .
H27 H 0.0896 0.0749 -0.0190 0.083 Uiso 1 1 calc R . .
C24 C 0.9822(3) 0.1385(3) 0.3670(3) 0.0671(13) Uani 1 1 d . . .
H24 H 1.0344 0.1143 0.3481 0.080 Uiso 1 1 calc R . .
C21 C 0.2063(3) 0.1420(3) 0.1327(3) 0.0628(13) Uani 1 1 d . . .
C35 C 1.3212(4) 0.4039(4) 0.1274(3) 0.0780(15) Uani 1 1 d . . .
H35 H 1.3774 0.3898 0.1513 0.094 Uiso 1 1 calc R . .
C28 C 0.0507(3) 0.1490(4) 0.1518(3) 0.0693(13) Uani 1 1 d . . .
H28 H 0.0039 0.1626 0.1834 0.083 Uiso 1 1 calc R . .
C36 C 1.2339(4) 0.4592(4) 0.0157(4) 0.0859(16) Uani 1 1 d . . .
H36 H 1.2292 0.4833 -0.0353 0.103 Uiso 1 1 calc R . .
C26 C 0.5215(4) 0.3538(4) 0.4700(3) 0.0773(15) Uani 1 1 d . . .
H26 H 0.5279 0.3190 0.5163 0.093 Uiso 1 1 calc R . .
C19 C 0.4119(3) 0.1698(3) 0.2438(3) 0.0599(12) Uani 1 1 d . . .
N6 N 0.3046(3) 0.1521(3) 0.1533(2) 0.0734(12) Uani 1 1 d . . .
C31 C 0.4417(4) 0.3953(5) 0.4511(5) 0.099(2) Uani 1 1 d . . .
H31 H 0.3950 0.3893 0.4843 0.119 Uiso 1 1 calc R . .
C33 C 1.3156(4) 0.4379(4) 0.0524(3) 0.0796(16) Uani 1 1 d . . .
H33 H 1.3675 0.4467 0.0259 0.096 Uiso 1 1 calc R . .
C34 C 1.2488(4) 0.3900(4) 0.1683(4) 0.0804(16) Uani 1 1 d . . .
H34 H 1.2543 0.3675 0.2199 0.096 Uiso 1 1 calc R . .
C30 C 0.1876(3) 0.1112(4) 0.0589(3) 0.0698(14) Uani 1 1 d . . .
H30 H 0.2338 0.0995 0.0262 0.084 Uiso 1 1 calc R . .
C25 C 0.1391(4) 0.1625(4) 0.1794(3) 0.0732(14) Uani 1 1 d . . .
H25 H 0.1522 0.1858 0.2300 0.088 Uiso 1 1 calc R . .
C37 C 1.1576(4) 0.4436(4) 0.0570(4) 0.0849(18) Uani 1 1 d . . .
H37 H 1.1007 0.4560 0.0339 0.102 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
Zn01 N7 2.036(3) . ?
Zn01 N5 2.038(4) . ?
Zn01 N1 2.124(3) . ?
Zn01 N4 2.144(4) . ?
Zn01 N3 2.307(3) . ?
Zn01 N2 2.356(3) . ?
S1 C3 1.625(4) . ?
S2 C12 1.615(5) . ?
N9 N10 1.154(5) . ?
N9 C29 1.581(7) . ?
N7 C3 1.156(5) . ?
N2 C4 1.277(5) . ?
N2 C1 1.419(5) . ?
C29 C34 1.337(8) . ?
C29 C37 1.399(8) . ?
N3 C5 1.264(5) . ?
N3 C2 1.414(5) . ?
N1 C10 1.338(5) . ?
N1 C6 1.355(5) . ?
C1 C8 1.378(5) . ?
C1 C23 1.385(5) . ?
N4 C26 1.325(6) . ?
N4 C15 1.352(5) . ?
C12 N5 1.144(5) . ?
C8 C7 1.375(6) . ?
C8 H8 0.9400 . ?
C10 C20 1.373(7) . ?
C10 H10 0.9400 . ?
N10 C9 1.553(7) . ?
C15 C32 1.374(6) . ?
C15 C4 1.457(6) . ?
C4 H4 0.9400 . ?
C6 C18 1.369(6) . ?
C6 C5 1.481(5) . ?
C2 C14 1.380(5) . ?
C2 C11 1.383(6) . ?
C11 C22 1.378(6) . ?
C11 H11 0.9400 . ?
C23 C13 1.368(6) . ?
C23 H23 0.9400 . ?
C13 C9 1.357(7) . ?
C13 H13 0.9400 . ?
C18 C24 1.379(6) . ?
C18 H18 0.9400 . ?
C9 C7 1.385(6) . ?
C17 C27 1.346(7) . ?
C17 C28 1.379(7) . ?
C17 H17 0.9400 . ?
C7 H7 0.9400 . ?
N8 N6 1.169(5) . ?
N8 C19 1.524(6) . ?
C38 C31 1.360(9) . ?
C38 C32 1.379(8) . ?
C38 H38 0.9400 . ?
C32 H32 0.9400 . ?
C16 C19 1.374(7) . ?
C16 C14 1.396(6) . ?
C16 H16 0.9400 . ?
C5 H5 0.9400 . ?
C14 H14 0.9400 . ?
C20 C24 1.365(7) . ?
C20 H20 0.9400 . ?
C22 C19 1.369(7) . ?
C22 H22 0.9400 . ?
C27 C30 1.360(6) . ?
C27 H27 0.9400 . ?
C24 H24 0.9400 . ?
C21 C30 1.353(7) . ?
C21 C25 1.367(7) . ?
C21 N6 1.511(6) . ?
C35 C34 1.353(7) . ?
C35 C33 1.375(7) . ?
C35 H35 0.9400 . ?
C28 C25 1.400(7) . ?
C28 H28 0.9400 . ?
C36 C33 1.383(8) . ?
C36 C37 1.410(8) . ?
C36 H36 0.9400 . ?
C26 C31 1.366(8) . ?
C26 H26 0.9400 . ?
C31 H31 0.9400 . ?
C33 H33 0.9400 . ?
C34 H34 0.9400 . ?
C30 H30 0.9400 . ?
C25 H25 0.9400 . ?
C37 H37 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 Zn01 N5 97.57(15) . . ?
N7 Zn01 N1 95.43(14) . . ?
N5 Zn01 N1 100.81(15) . . ?
N7 Zn01 N4 97.84(14) . . ?
N5 Zn01 N4 94.28(16) . . ?
N1 Zn01 N4 158.40(12) . . ?
N7 Zn01 N3 166.71(14) . . ?
N5 Zn01 N3 92.84(13) . . ?
N1 Zn01 N3 74.43(12) . . ?
N4 Zn01 N3 89.56(12) . . ?
N7 Zn01 N2 93.99(13) . . ?
N5 Zn01 N2 164.34(14) . . ?
N1 Zn01 N2 88.53(11) . . ?
N4 Zn01 N2 73.63(12) . . ?
N3 Zn01 N2 77.45(10) . . ?
N10 N9 C29 107.2(5) . . ?
C3 N7 Zn01 162.3(4) . . ?
C4 N2 C1 119.8(3) . . ?
C4 N2 Zn01 111.1(3) . . ?
C1 N2 Zn01 128.1(2) . . ?
C34 C29 C37 123.1(5) . . ?
C34 C29 N9 114.7(5) . . ?
C37 C29 N9 122.1(6) . . ?
C5 N3 C2 120.8(3) . . ?
C5 N3 Zn01 112.0(2) . . ?
C2 N3 Zn01 126.4(3) . . ?
C10 N1 C6 117.6(4) . . ?
C10 N1 Zn01 124.7(3) . . ?
C6 N1 Zn01 117.2(2) . . ?
C8 C1 C23 119.6(4) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.9(3) . . ?
N7 C3 S1 178.7(4) . . ?
C26 N4 C15 117.4(4) . . ?
C26 N4 Zn01 124.7(4) . . ?
C15 N4 Zn01 117.7(3) . . ?
N5 C12 S2 179.7(4) . . ?
C7 C8 C1 119.9(4) . . ?
C7 C8 H8 120.1 . . ?
C1 C8 H8 120.1 . . ?
N1 C10 C20 122.6(4) . . ?
N1 C10 H10 118.7 . . ?
C20 C10 H10 118.7 . . ?
N9 N10 C9 102.6(5) . . ?
N4 C15 C32 121.9(4) . . ?
N4 C15 C4 116.3(4) . . ?
C32 C15 C4 121.8(4) . . ?
N2 C4 C15 120.3(4) . . ?
N2 C4 H4 119.9 . . ?
C15 C4 H4 119.9 . . ?
N1 C6 C18 122.2(4) . . ?
N1 C6 C5 115.1(4) . . ?
C18 C6 C5 122.7(4) . . ?
C14 C2 C11 119.9(4) . . ?
C14 C2 N3 122.8(4) . . ?
C11 C2 N3 117.1(3) . . ?
C22 C11 C2 120.2(4) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
C13 C23 C1 120.4(4) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C12 N5 Zn01 165.8(3) . . ?
C9 C13 C23 119.8(4) . . ?
C9 C13 H13 120.1 . . ?
C23 C13 H13 120.1 . . ?
C6 C18 C24 119.3(4) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C13 C9 C7 120.8(4) . . ?
C13 C9 N10 112.0(4) . . ?
C7 C9 N10 127.1(4) . . ?
C27 C17 C28 120.3(4) . . ?
C27 C17 H17 119.9 . . ?
C28 C17 H17 119.9 . . ?
C8 C7 C9 119.5(4) . . ?
C8 C7 H7 120.2 . . ?
C9 C7 H7 120.2 . . ?
N6 N8 C19 107.6(4) . . ?
C31 C38 C32 118.4(6) . . ?
C31 C38 H38 120.8 . . ?
C32 C38 H38 120.8 . . ?
C15 C32 C38 119.4(6) . . ?
C15 C32 H32 120.3 . . ?
C38 C32 H32 120.3 . . ?
C19 C16 C14 120.6(4) . . ?
C19 C16 H16 119.7 . . ?
C14 C16 H16 119.7 . . ?
N3 C5 C6 119.6(3) . . ?
N3 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C2 C14 C16 119.1(4) . . ?
C2 C14 H14 120.5 . . ?
C16 C14 H14 120.5 . . ?
C24 C20 C10 119.5(4) . . ?
C24 C20 H20 120.2 . . ?
C10 C20 H20 120.2 . . ?
C19 C22 C11 120.4(5) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C17 C27 C30 121.3(5) . . ?
C17 C27 H27 119.3 . . ?
C30 C27 H27 119.3 . . ?
C20 C24 C18 118.8(5) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 120.1(4) . . ?
C30 C21 N6 113.0(5) . . ?
C25 C21 N6 126.8(5) . . ?
C34 C35 C33 122.5(6) . . ?
C34 C35 H35 118.8 . . ?
C33 C35 H35 118.8 . . ?
C17 C28 C25 118.2(5) . . ?
C17 C28 H28 120.9 . . ?
C25 C28 H28 120.9 . . ?
C33 C36 C37 118.1(6) . . ?
C33 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
N4 C26 C31 123.5(6) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C22 C19 C16 119.8(4) . . ?
C22 C19 N8 111.9(5) . . ?
C16 C19 N8 128.3(4) . . ?
N8 N6 C21 106.5(5) . . ?
C38 C31 C26 119.5(6) . . ?
C38 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C35 C33 C36 120.1(5) . . ?
C35 C33 H33 120.0 . . ?
C36 C33 H33 120.0 . . ?
C29 C34 C35 118.1(6) . . ?
C29 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
C21 C30 C27 120.0(5) . . ?
C21 C30 H30 120.0 . . ?
C27 C30 H30 120.0 . . ?
C21 C25 C28 120.1(5) . . ?
C21 C25 H25 120.0 . . ?
C28 C25 H25 120.0 . . ?
C29 C37 C36 118.1(5) . . ?
C29 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?

_diffrn_measured_fraction_theta_max 0.745
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.745
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.049
####################################################################### 
# 
# 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_znaza210kd
_database_code_depnum_ccdc_archive 'CCDC 1492685'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1082(7)
_cell_length_b                   14.4006(10)
_cell_length_c                   17.1451(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.924(4)
_cell_angle_gamma                90.00
_cell_volume                     3721.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    14509
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_T_max  0.7108
_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            6349
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4893
_reflns_number_gt                4170
_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)+(0.0590P)²+5.2244P] 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         4893
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.1269
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
Zn01 Zn 0.71322(3) 0.28468(3) 0.44696(2) 0.04253(19) Uani 1 1 d . . .
S1 S 0.80761(7) 0.49896(8) 0.64741(6) 0.0504(3) Uani 1 1 d . . .
S2 S 0.56319(8) 0.07179(9) 0.60469(7) 0.0606(3) Uani 1 1 d . . .
N9 N 1.0900(3) 0.3955(3) 0.1860(2) 0.0655(11) Uani 1 1 d . . .
N7 N 0.7750(2) 0.3744(3) 0.5246(2) 0.0563(10) Uani 1 1 d . . .
N2 N 0.7310(2) 0.3809(2) 0.33829(16) 0.0351(7) Uani 1 1 d . . .
C29 C 1.1689(4) 0.4095(3) 0.1337(3) 0.0685(15) Uani 1 1 d . . .
N3 N 0.6723(2) 0.1885(2) 0.34313(17) 0.0382(8) Uani 1 1 d . . .
N1 N 0.8303(2) 0.2134(2) 0.42082(18) 0.0420(8) Uani 1 1 d . . .
C1 C 0.8049(3) 0.3864(2) 0.2918(2) 0.0355(9) Uani 1 1 d . . .
C3 C 0.7880(2) 0.4260(3) 0.5761(2) 0.0415(10) Uani 1 1 d . . .
N4 N 0.5911(2) 0.3598(2) 0.42679(19) 0.0475(9) Uani 1 1 d . . .
C12 C 0.6220(3) 0.1448(3) 0.5588(2) 0.0442(10) Uani 1 1 d . . .
C8 C 0.8879(3) 0.3994(3) 0.3285(2) 0.0431(10) Uani 1 1 d . . .
H8 H 0.8946 0.4053 0.3832 0.052 Uiso 1 1 calc R . .
C10 C 0.9094(3) 0.2222(3) 0.4607(2) 0.0510(11) Uani 1 1 d . . .
H10 H 0.9123 0.2551 0.5081 0.061 Uiso 1 1 calc R . .
N10 N 1.0232(3) 0.4017(3) 0.1471(3) 0.0756(13) Uani 1 1 d . . .
C15 C 0.5803(3) 0.4110(3) 0.3606(2) 0.0469(10) Uani 1 1 d . . .
C4 C 0.6578(3) 0.4194(3) 0.3147(2) 0.0429(10) Uani 1 1 d . . .
H4 H 0.6538 0.4533 0.2678 0.051 Uiso 1 1 calc R . .
C6 C 0.8279(3) 0.1642(3) 0.3531(2) 0.0407(10) Uani 1 1 d . . .
C2 C 0.5859(3) 0.1799(3) 0.3063(2) 0.0401(9) Uani 1 1 d . . .
C11 C 0.5183(3) 0.1562(3) 0.3533(2) 0.0518(11) Uani 1 1 d . . .
H11 H 0.5314 0.1434 0.4065 0.062 Uiso 1 1 calc R . .
C23 C 0.7961(3) 0.3750(3) 0.2113(2) 0.0506(11) Uani 1 1 d . . .
H23 H 0.7398 0.3641 0.1862 0.061 Uiso 1 1 calc R . .
N5 N 0.6643(3) 0.1964(3) 0.5262(2) 0.0636(11) Uani 1 1 d . . .
C13 C 0.8690(3) 0.3796(3) 0.1681(3) 0.0614(13) Uani 1 1 d . . .
H13 H 0.8624 0.3730 0.1135 0.074 Uiso 1 1 calc R . .
C18 C 0.9024(3) 0.1272(3) 0.3245(3) 0.0538(11) Uani 1 1 d . . .
H18 H 0.8986 0.0943 0.2770 0.065 Uiso 1 1 calc R . .
C9 C 0.9503(3) 0.3936(3) 0.2040(3) 0.0527(12) Uani 1 1 d . . .
C17 C 0.0336(3) 0.1149(3) 0.0773(3) 0.0540(12) Uani 1 1 d . . .
H17 H -0.0254 0.1038 0.0584 0.065 Uiso 1 1 calc R . .
C7 C 0.9611(3) 0.4035(3) 0.2848(3) 0.0526(11) Uani 1 1 d . . .
H7 H 1.0180 0.4129 0.3095 0.063 Uiso 1 1 calc R . .
N8 N 0.3144(3) 0.1611(3) 0.2215(2) 0.0648(11) Uani 1 1 d . . .
C38 C 0.4309(4) 0.4447(5) 0.3850(5) 0.0915(19) Uani 1 1 d . . .
H38 H 0.3761 0.4730 0.3707 0.110 Uiso 1 1 calc R . .
C32 C 0.5012(3) 0.4531(4) 0.3383(3) 0.0683(14) Uani 1 1 d . . .
H32 H 0.4949 0.4874 0.2916 0.082 Uiso 1 1 calc R . .
C16 C 0.4784(3) 0.1953(3) 0.1975(3) 0.0586(13) Uani 1 1 d . . .
H16 H 0.4646 0.2093 0.1445 0.070 Uiso 1 1 calc R . .
C5 C 0.7384(3) 0.1527(3) 0.3134(2) 0.0412(10) Uani 1 1 d . . .
H5 H 0.7310 0.1190 0.2665 0.049 Uiso 1 1 calc R . .
C14 C 0.5663(3) 0.2005(3) 0.2283(2) 0.0502(11) Uani 1 1 d . . .
H14 H 0.6117 0.2180 0.1964 0.060 Uiso 1 1 calc R . .
C20 C 0.9860(3) 0.1854(3) 0.4355(3) 0.0613(13) Uani 1 1 d . . .
H20 H 1.0399 0.1924 0.4657 0.074 Uiso 1 1 calc R . .
C22 C 0.4316(3) 0.1515(3) 0.3220(3) 0.0599(12) Uani 1 1 d . . .
H22 H 0.3859 0.1359 0.3542 0.072 Uiso 1 1 calc R . .
C27 C 0.1012(3) 0.0970(3) 0.0315(3) 0.0616(13) Uani 1 1 d . . .
H27 H 0.0883 0.0747 -0.0195 0.074 Uiso 1 1 calc R . .
C24 C 0.9832(3) 0.1385(3) 0.3661(3) 0.0612(13) Uani 1 1 d . . .
H24 H 1.0354 0.1145 0.3470 0.073 Uiso 1 1 calc R . .
C21 C 0.2066(3) 0.1421(3) 0.1321(3) 0.0566(12) Uani 1 1 d . . .
C35 C 1.3220(4) 0.4038(4) 0.1280(3) 0.0685(14) Uani 1 1 d . . .
H35 H 1.3783 0.3898 0.1520 0.082 Uiso 1 1 calc R . .
C28 C 0.0517(3) 0.1494(3) 0.1515(3) 0.0622(13) Uani 1 1 d . . .
H28 H 0.0053 0.1637 0.1833 0.075 Uiso 1 1 calc R . .
C36 C 1.2341(4) 0.4589(4) 0.0165(3) 0.0758(15) Uani 1 1 d . . .
H36 H 1.2292 0.4829 -0.0346 0.091 Uiso 1 1 calc R . .
C26 C 0.5226(4) 0.3531(4) 0.4712(3) 0.0714(15) Uani 1 1 d . . .
H26 H 0.5297 0.3183 0.5175 0.086 Uiso 1 1 calc R . .
C19 C 0.4118(3) 0.1696(3) 0.2443(3) 0.0534(12) Uani 1 1 d . . .
N6 N 0.3039(3) 0.1517(3) 0.1529(2) 0.0643(11) Uani 1 1 d . . .
C31 C 0.4425(4) 0.3943(5) 0.4527(5) 0.0900(19) Uani 1 1 d . . .
H31 H 0.3959 0.3882 0.4860 0.108 Uiso 1 1 calc R . .
C33 C 1.3158(4) 0.4380(4) 0.0527(3) 0.0731(15) Uani 1 1 d . . .
H33 H 1.3675 0.4469 0.0260 0.088 Uiso 1 1 calc R . .
C34 C 1.2488(4) 0.3897(4) 0.1688(3) 0.0709(14) Uani 1 1 d . . .
H34 H 1.2542 0.3666 0.2202 0.085 Uiso 1 1 calc R . .
C30 C 0.1873(3) 0.1107(3) 0.0578(3) 0.0630(13) Uani 1 1 d . . .
H30 H 0.2333 0.0985 0.0249 0.076 Uiso 1 1 calc R . .
C25 C 0.1397(4) 0.1628(3) 0.1789(3) 0.0657(14) Uani 1 1 d . . .
H25 H 0.1531 0.1861 0.2296 0.079 Uiso 1 1 calc R . .
C37 C 1.1579(4) 0.4436(4) 0.0578(4) 0.0758(16) Uani 1 1 d . . .
H37 H 1.1009 0.4562 0.0346 0.091 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
Zn01 N7 2.036(3) . ?
Zn01 N5 2.036(4) . ?
Zn01 N1 2.120(3) . ?
Zn01 N4 2.146(4) . ?
Zn01 N3 2.307(3) . ?
Zn01 N2 2.352(3) . ?
S1 C3 1.623(4) . ?
S2 C12 1.616(5) . ?
N9 N10 1.174(5) . ?
N9 C29 1.552(7) . ?
N7 C3 1.161(5) . ?
N2 C4 1.278(5) . ?
N2 C1 1.418(5) . ?
C29 C34 1.342(8) . ?
C29 C37 1.390(8) . ?
N3 C5 1.263(5) . ?
N3 C2 1.416(5) . ?
N1 C10 1.340(5) . ?
N1 C6 1.358(5) . ?
C1 C8 1.378(5) . ?
C1 C23 1.387(5) . ?
N4 C26 1.329(6) . ?
N4 C15 1.353(5) . ?
C12 N5 1.149(5) . ?
C8 C7 1.380(6) . ?
C8 H8 0.9400 . ?
C10 C20 1.369(7) . ?
C10 H10 0.9400 . ?
N10 C9 1.524(6) . ?
C15 C32 1.372(6) . ?
C15 C4 1.459(6) . ?
C4 H4 0.9400 . ?
C6 C18 1.367(6) . ?
C6 C5 1.480(5) . ?
C2 C14 1.381(5) . ?
C2 C11 1.386(6) . ?
C11 C22 1.383(6) . ?
C11 H11 0.9400 . ?
C23 C13 1.370(6) . ?
C23 H23 0.9400 . ?
C13 C9 1.350(6) . ?
C13 H13 0.9400 . ?
C18 C24 1.382(6) . ?
C18 H18 0.9400 . ?
C9 C7 1.392(6) . ?
C17 C27 1.355(7) . ?
C17 C28 1.376(7) . ?
C17 H17 0.9400 . ?
C7 H7 0.9400 . ?
N8 N6 1.184(5) . ?
N8 C19 1.501(6) . ?
C38 C31 1.370(9) . ?
C38 C32 1.377(8) . ?
C38 H38 0.9400 . ?
C32 H32 0.9400 . ?
C16 C19 1.381(7) . ?
C16 C14 1.398(6) . ?
C16 H16 0.9400 . ?
C5 H5 0.9400 . ?
C14 H14 0.9400 . ?
C20 C24 1.366(7) . ?
C20 H20 0.9400 . ?
C22 C19 1.370(6) . ?
C22 H22 0.9400 . ?
C27 C30 1.362(6) . ?
C27 H27 0.9400 . ?
C24 H24 0.9400 . ?
C21 C25 1.365(7) . ?
C21 C30 1.365(7) . ?
C21 N6 1.496(6) . ?
C35 C34 1.363(7) . ?
C35 C33 1.380(7) . ?
C35 H35 0.9400 . ?
C28 C25 1.394(7) . ?
C28 H28 0.9400 . ?
C36 C33 1.377(8) . ?
C36 C37 1.410(7) . ?
C36 H36 0.9400 . ?
C26 C31 1.366(8) . ?
C26 H26 0.9400 . ?
C31 H31 0.9400 . ?
C33 H33 0.9400 . ?
C34 H34 0.9400 . ?
C30 H30 0.9400 . ?
C25 H25 0.9400 . ?
C37 H37 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 Zn01 N5 97.52(15) . . ?
N7 Zn01 N1 95.36(14) . . ?
N5 Zn01 N1 100.65(15) . . ?
N7 Zn01 N4 97.84(14) . . ?
N5 Zn01 N4 94.31(15) . . ?
N1 Zn01 N4 158.55(12) . . ?
N7 Zn01 N3 166.63(14) . . ?
N5 Zn01 N3 92.82(13) . . ?
N1 Zn01 N3 74.32(12) . . ?
N4 Zn01 N3 89.78(12) . . ?
N7 Zn01 N2 94.16(13) . . ?
N5 Zn01 N2 164.31(14) . . ?
N1 Zn01 N2 88.60(11) . . ?
N4 Zn01 N2 73.68(12) . . ?
N3 Zn01 N2 77.39(10) . . ?
N10 N9 C29 109.1(5) . . ?
C3 N7 Zn01 161.8(4) . . ?
C4 N2 C1 119.7(3) . . ?
C4 N2 Zn01 111.3(3) . . ?
C1 N2 Zn01 128.0(2) . . ?
C34 C29 C37 122.7(5) . . ?
C34 C29 N9 114.7(5) . . ?
C37 C29 N9 122.6(5) . . ?
C5 N3 C2 121.0(3) . . ?
C5 N3 Zn01 112.3(2) . . ?
C2 N3 Zn01 126.0(3) . . ?
C10 N1 C6 117.1(4) . . ?
C10 N1 Zn01 125.0(3) . . ?
C6 N1 Zn01 117.3(3) . . ?
C8 C1 C23 119.6(4) . . ?
C8 C1 N2 118.5(3) . . ?
C23 C1 N2 121.9(3) . . ?
N7 C3 S1 179.0(4) . . ?
C26 N4 C15 117.8(4) . . ?
C26 N4 Zn01 124.4(4) . . ?
C15 N4 Zn01 117.5(3) . . ?
N5 C12 S2 179.6(5) . . ?
C1 C8 C7 119.7(4) . . ?
C1 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
N1 C10 C20 123.1(4) . . ?
N1 C10 H10 118.4 . . ?
C20 C10 H10 118.4 . . ?
N9 N10 C9 105.2(4) . . ?
N4 C15 C32 121.8(4) . . ?
N4 C15 C4 116.3(4) . . ?
C32 C15 C4 121.9(4) . . ?
N2 C4 C15 120.1(4) . . ?
N2 C4 H4 119.9 . . ?
C15 C4 H4 119.9 . . ?
N1 C6 C18 122.4(4) . . ?
N1 C6 C5 115.0(4) . . ?
C18 C6 C5 122.6(4) . . ?
C14 C2 C11 119.9(4) . . ?
C14 C2 N3 122.9(4) . . ?
C11 C2 N3 117.1(3) . . ?
C22 C11 C2 120.2(4) . . ?
C22 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
C13 C23 C1 120.5(4) . . ?
C13 C23 H23 119.8 . . ?
C1 C23 H23 119.8 . . ?
C12 N5 Zn01 165.3(3) . . ?
C9 C13 C23 120.0(4) . . ?
C9 C13 H13 120.0 . . ?
C23 C13 H13 120.0 . . ?
C6 C18 C24 119.3(4) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C13 C9 C7 120.7(4) . . ?
C13 C9 N10 113.3(4) . . ?
C7 C9 N10 126.0(4) . . ?
C27 C17 C28 119.6(4) . . ?
C27 C17 H17 120.2 . . ?
C28 C17 H17 120.2 . . ?
C8 C7 C9 119.5(4) . . ?
C8 C7 H7 120.3 . . ?
C9 C7 H7 120.3 . . ?
N6 N8 C19 109.3(4) . . ?
C31 C38 C32 118.7(5) . . ?
C31 C38 H38 120.6 . . ?
C32 C38 H38 120.6 . . ?
C15 C32 C38 119.4(6) . . ?
C15 C32 H32 120.3 . . ?
C38 C32 H32 120.3 . . ?
C19 C16 C14 120.4(4) . . ?
C19 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
N3 C5 C6 119.4(3) . . ?
N3 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C2 C14 C16 119.3(4) . . ?
C2 C14 H14 120.4 . . ?
C16 C14 H14 120.4 . . ?
C24 C20 C10 119.3(4) . . ?
C24 C20 H20 120.4 . . ?
C10 C20 H20 120.4 . . ?
C19 C22 C11 120.4(4) . . ?
C19 C22 H22 119.8 . . ?
C11 C22 H22 119.8 . . ?
C17 C27 C30 121.5(5) . . ?
C17 C27 H27 119.3 . . ?
C30 C27 H27 119.3 . . ?
C20 C24 C18 118.8(5) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C25 C21 C30 120.2(4) . . ?
C25 C21 N6 126.5(4) . . ?
C30 C21 N6 113.3(5) . . ?
C34 C35 C33 121.9(5) . . ?
C34 C35 H35 119.1 . . ?
C33 C35 H35 119.1 . . ?
C17 C28 C25 119.1(5) . . ?
C17 C28 H28 120.5 . . ?
C25 C28 H28 120.5 . . ?
C33 C36 C37 118.5(5) . . ?
C33 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
N4 C26 C31 123.3(6) . . ?
N4 C26 H26 118.4 . . ?
C31 C26 H26 118.4 . . ?
C22 C19 C16 119.8(4) . . ?
C22 C19 N8 112.5(4) . . ?
C16 C19 N8 127.7(4) . . ?
N8 N6 C21 108.1(4) . . ?
C26 C31 C38 119.0(6) . . ?
C26 C31 H31 120.5 . . ?
C38 C31 H31 120.5 . . ?
C36 C33 C35 120.1(5) . . ?
C36 C33 H33 120.0 . . ?
C35 C33 H33 120.0 . . ?
C29 C34 C35 118.4(5) . . ?
C29 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
C27 C30 C21 119.6(5) . . ?
C27 C30 H30 120.2 . . ?
C21 C30 H30 120.2 . . ?
C21 C25 C28 119.9(5) . . ?
C21 C25 H25 120.0 . . ?
C28 C25 H25 120.0 . . ?
C29 C37 C36 118.4(5) . . ?
C29 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?

_diffrn_measured_fraction_theta_max 0.744
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.744
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.053
####################################################################### 
# 
# 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_znaza200km
_database_code_depnum_ccdc_archive 'CCDC 1492686'
_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-zinc(ii)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19

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'
Zn Zn 0.2839 1.4301 '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                   15.1058(7)
_cell_length_b                   14.3790(10)
_cell_length_c                   17.1457(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.973(4)
_cell_angle_gamma                90.00
_cell_volume                     3715.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    14595
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1

_exptl_crystal_description       cube-shaped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6404
_exptl_absorpt_correction_T_max  0.7104
_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            6282
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4853
_reflns_number_gt                4155
_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)+(0.0541P)²+5.1049P] 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         4853
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1265
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Zn01 Zn 0.71376(3) 0.28452(3) 0.44684(2) 0.04066(18) Uani 1 1 d . . .
S1 S 0.80763(7) 0.49932(8) 0.64745(5) 0.0484(3) Uani 1 1 d . . .
S2 S 0.56305(8) 0.07193(9) 0.60455(6) 0.0578(3) Uani 1 1 d . . .
N9 N 1.0909(3) 0.3955(2) 0.1858(2) 0.0606(10) Uani 1 1 d . . .
N7 N 0.7756(2) 0.3742(3) 0.52475(19) 0.0536(9) Uani 1 1 d . . .
N2 N 0.7310(2) 0.3809(2) 0.33842(16) 0.0335(7) Uani 1 1 d . . .
C29 C 1.1691(4) 0.4096(3) 0.1341(3) 0.0625(13) Uani 1 1 d . . .
N3 N 0.6726(2) 0.1885(2) 0.34296(16) 0.0364(7) Uani 1 1 d . . .
N1 N 0.8309(2) 0.2133(2) 0.42048(17) 0.0402(8) Uani 1 1 d . . .
C1 C 0.8049(3) 0.3864(2) 0.29150(19) 0.0354(9) Uani 1 1 d . . .
C3 C 0.7884(2) 0.4259(3) 0.5763(2) 0.0397(9) Uani 1 1 d . . .
N4 N 0.5915(2) 0.3597(2) 0.42687(19) 0.0468(8) Uani 1 1 d . . .
C12 C 0.6225(3) 0.1445(3) 0.5586(2) 0.0417(9) Uani 1 1 d . . .
C8 C 0.8883(3) 0.3996(3) 0.3282(2) 0.0415(9) Uani 1 1 d . . .
H8 H 0.8951 0.4058 0.3835 0.050 Uiso 1 1 calc R . .
C10 C 0.9103(3) 0.2219(3) 0.4603(2) 0.0495(11) Uani 1 1 d . . .
H10 H 0.9133 0.2548 0.5084 0.059 Uiso 1 1 calc R . .
N10 N 1.0227(3) 0.4018(3) 0.1479(2) 0.0700(12) Uani 1 1 d . . .
C15 C 0.5807(3) 0.4108(3) 0.3609(2) 0.0452(10) Uani 1 1 d . . .
C4 C 0.6578(3) 0.4194(3) 0.3149(2) 0.0405(9) Uani 1 1 d . . .
H4 H 0.6536 0.4535 0.2673 0.049 Uiso 1 1 calc R . .
C6 C 0.8286(3) 0.1642(3) 0.3528(2) 0.0388(9) Uani 1 1 d . . .
C2 C 0.5860(3) 0.1799(3) 0.3062(2) 0.0388(9) Uani 1 1 d . . .
C11 C 0.5189(3) 0.1560(3) 0.3536(2) 0.0506(11) Uani 1 1 d . . .
H11 H 0.5325 0.1427 0.4074 0.061 Uiso 1 1 calc R . .
C23 C 0.7957(3) 0.3748(3) 0.2108(2) 0.0476(10) Uani 1 1 d . . .
H23 H 0.7387 0.3636 0.1856 0.057 Uiso 1 1 calc R . .
N5 N 0.6650(3) 0.1961(3) 0.5261(2) 0.0624(11) Uani 1 1 d . . .
C13 C 0.8685(3) 0.3795(3) 0.1676(2) 0.0577(12) Uani 1 1 d . . .
H13 H 0.8618 0.3729 0.1124 0.069 Uiso 1 1 calc R . .
C18 C 0.9027(3) 0.1272(3) 0.3240(2) 0.0501(11) Uani 1 1 d . . .
H18 H 0.8987 0.0941 0.2759 0.060 Uiso 1 1 calc R . .
C9 C 0.9501(3) 0.3935(3) 0.2037(2) 0.0502(11) Uani 1 1 d . . .
C17 C 0.0335(3) 0.1150(3) 0.0773(3) 0.0522(11) Uani 1 1 d . . .
H17 H -0.0262 0.1042 0.0584 0.063 Uiso 1 1 calc R . .
C7 C 0.9614(3) 0.4038(3) 0.2847(3) 0.0499(11) Uani 1 1 d . . .
H7 H 1.0188 0.4137 0.3095 0.060 Uiso 1 1 calc R . .
N8 N 0.3149(3) 0.1611(3) 0.2218(2) 0.0608(10) Uani 1 1 d . . .
C38 C 0.4312(4) 0.4441(4) 0.3856(4) 0.0890(19) Uani 1 1 d . . .
H38 H 0.3757 0.4725 0.3713 0.107 Uiso 1 1 calc R . .
C32 C 0.5013(3) 0.4528(3) 0.3383(3) 0.0648(13) Uani 1 1 d . . .
H32 H 0.4946 0.4872 0.2910 0.078 Uiso 1 1 calc R . .
C16 C 0.4785(3) 0.1951(3) 0.1974(2) 0.0541(12) Uani 1 1 d . . .
H16 H 0.4645 0.2087 0.1437 0.065 Uiso 1 1 calc R . .
C5 C 0.7391(3) 0.1524(3) 0.3132(2) 0.0401(9) Uani 1 1 d . . .
H5 H 0.7315 0.1181 0.2658 0.048 Uiso 1 1 calc R . .
C14 C 0.5662(3) 0.2004(3) 0.2283(2) 0.0472(10) Uani 1 1 d . . .
H14 H 0.6119 0.2181 0.1960 0.057 Uiso 1 1 calc R . .
C20 C 0.9867(3) 0.1856(3) 0.4351(3) 0.0591(12) Uani 1 1 d . . .
H20 H 1.0413 0.1929 0.4655 0.071 Uiso 1 1 calc R . .
C22 C 0.4317(3) 0.1516(3) 0.3223(3) 0.0564(12) Uani 1 1 d . . .
H22 H 0.3857 0.1358 0.3549 0.068 Uiso 1 1 calc R . .
C27 C 0.1010(3) 0.0967(3) 0.0311(3) 0.0590(12) Uani 1 1 d . . .
H27 H 0.0878 0.0738 -0.0204 0.071 Uiso 1 1 calc R . .
C24 C 0.9836(3) 0.1384(3) 0.3655(3) 0.0598(12) Uani 1 1 d . . .
H24 H 1.0362 0.1138 0.3462 0.072 Uiso 1 1 calc R . .
C21 C 0.2073(3) 0.1419(3) 0.1316(3) 0.0543(12) Uani 1 1 d . . .
C35 C 1.3225(3) 0.4038(3) 0.1281(3) 0.0657(13) Uani 1 1 d . . .
H35 H 1.3795 0.3896 0.1521 0.079 Uiso 1 1 calc R . .
C28 C 0.0519(3) 0.1493(3) 0.1515(3) 0.0591(12) Uani 1 1 d . . .
H28 H 0.0052 0.1635 0.1839 0.071 Uiso 1 1 calc R . .
C36 C 1.2339(4) 0.4585(4) 0.0170(3) 0.0717(14) Uani 1 1 d . . .
H36 H 1.2288 0.4822 -0.0348 0.086 Uiso 1 1 calc R . .
C26 C 0.5233(4) 0.3527(4) 0.4716(3) 0.0677(14) Uani 1 1 d . . .
H26 H 0.5309 0.3174 0.5184 0.081 Uiso 1 1 calc R . .
C19 C 0.4116(3) 0.1699(3) 0.2447(3) 0.0514(11) Uani 1 1 d . . .
N6 N 0.3038(3) 0.1519(3) 0.1526(2) 0.0609(10) Uani 1 1 d . . .
C31 C 0.4430(4) 0.3936(4) 0.4537(4) 0.0858(18) Uani 1 1 d . . .
H31 H 0.3962 0.3874 0.4876 0.103 Uiso 1 1 calc R . .
C33 C 1.3158(4) 0.4381(4) 0.0529(3) 0.0696(14) Uani 1 1 d . . .
H33 H 1.3678 0.4477 0.0258 0.084 Uiso 1 1 calc R . .
C34 C 1.2488(4) 0.3896(3) 0.1693(3) 0.0678(14) Uani 1 1 d . . .
H34 H 1.2541 0.3662 0.2213 0.081 Uiso 1 1 calc R . .
C30 C 0.1874(3) 0.1105(3) 0.0572(3) 0.0589(12) Uani 1 1 d . . .
H30 H 0.2337 0.0984 0.0238 0.071 Uiso 1 1 calc R . .
C25 C 0.1403(3) 0.1630(3) 0.1786(3) 0.0624(13) Uani 1 1 d . . .
H25 H 0.1540 0.1870 0.2297 0.075 Uiso 1 1 calc R . .
C37 C 1.1576(3) 0.4436(3) 0.0583(3) 0.0711(15) Uani 1 1 d . . .
H37 H 1.1000 0.4565 0.0350 0.085 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
Zn01 N5 2.036(4) . ?
Zn01 N7 2.036(3) . ?
Zn01 N1 2.120(3) . ?
Zn01 N4 2.147(3) . ?
Zn01 N3 2.305(3) . ?
Zn01 N2 2.347(3) . ?
S1 C3 1.624(4) . ?
S2 C12 1.617(5) . ?
N9 N10 1.183(5) . ?
N9 C29 1.539(6) . ?
N7 C3 1.161(5) . ?
N2 C4 1.276(5) . ?
N2 C1 1.423(5) . ?
C29 C34 1.339(7) . ?
C29 C37 1.388(7) . ?
N3 C5 1.269(5) . ?
N3 C2 1.417(5) . ?
N1 C10 1.344(5) . ?
N1 C6 1.357(5) . ?
C1 C8 1.382(5) . ?
C1 C23 1.391(5) . ?
N4 C26 1.331(6) . ?
N4 C15 1.350(5) . ?
C12 N5 1.150(5) . ?
C8 C7 1.377(6) . ?
C8 H8 0.9500 . ?
C10 C20 1.364(6) . ?
C10 H10 0.9500 . ?
N10 C9 1.509(6) . ?
C15 C32 1.375(6) . ?
C15 C4 1.456(6) . ?
C4 H4 0.9500 . ?
C6 C18 1.362(6) . ?
C6 C5 1.480(5) . ?
C2 C14 1.380(5) . ?
C2 C11 1.385(6) . ?
C11 C22 1.390(6) . ?
C11 H11 0.9500 . ?
C23 C13 1.369(6) . ?
C23 H23 0.9500 . ?
C13 C9 1.356(6) . ?
C13 H13 0.9500 . ?
C18 C24 1.381(6) . ?
C18 H18 0.9500 . ?
C9 C7 1.395(6) . ?
C17 C27 1.361(6) . ?
C17 C28 1.375(6) . ?
C17 H17 0.9500 . ?
C7 H7 0.9500 . ?
N8 N6 1.195(5) . ?
N8 C19 1.491(6) . ?
C38 C31 1.376(9) . ?
C38 C32 1.383(8) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C16 C19 1.386(6) . ?
C16 C14 1.395(6) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C14 H14 0.9500 . ?
C20 C24 1.371(6) . ?
C20 H20 0.9500 . ?
C22 C19 1.370(6) . ?
C22 H22 0.9500 . ?
C27 C30 1.365(6) . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C21 C30 1.367(6) . ?
C21 C25 1.370(7) . ?
C21 N6 1.484(6) . ?
C35 C34 1.375(7) . ?
C35 C33 1.378(7) . ?
C35 H35 0.9500 . ?
C28 C25 1.397(6) . ?
C28 H28 0.9500 . ?
C36 C33 1.375(7) . ?
C36 C37 1.410(7) . ?
C36 H36 0.9500 . ?
C26 C31 1.363(8) . ?
C26 H26 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C30 H30 0.9500 . ?
C25 H25 0.9500 . ?
C37 H37 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 Zn01 N7 97.37(14) . . ?
N5 Zn01 N1 100.76(15) . . ?
N7 Zn01 N1 95.41(13) . . ?
N5 Zn01 N4 94.25(15) . . ?
N7 Zn01 N4 97.80(14) . . ?
N1 Zn01 N4 158.53(12) . . ?
N5 Zn01 N3 92.91(13) . . ?
N7 Zn01 N3 166.73(13) . . ?
N1 Zn01 N3 74.36(11) . . ?
N4 Zn01 N3 89.74(12) . . ?
N5 Zn01 N2 164.23(13) . . ?
N7 Zn01 N2 94.28(12) . . ?
N1 Zn01 N2 88.64(11) . . ?
N4 Zn01 N2 73.60(12) . . ?
N3 Zn01 N2 77.33(10) . . ?
N10 N9 C29 110.3(4) . . ?
C3 N7 Zn01 161.8(3) . . ?
C4 N2 C1 119.6(3) . . ?
C4 N2 Zn01 111.4(2) . . ?
C1 N2 Zn01 128.0(2) . . ?
C34 C29 C37 123.3(5) . . ?
C34 C29 N9 114.4(4) . . ?
C37 C29 N9 122.3(5) . . ?
C5 N3 C2 121.2(3) . . ?
C5 N3 Zn01 112.1(2) . . ?
C2 N3 Zn01 126.0(2) . . ?
C10 N1 C6 116.8(3) . . ?
C10 N1 Zn01 125.2(3) . . ?
C6 N1 Zn01 117.5(2) . . ?
C8 C1 C23 119.7(4) . . ?
C8 C1 N2 118.4(3) . . ?
C23 C1 N2 121.8(3) . . ?
N7 C3 S1 178.9(4) . . ?
C26 N4 C15 118.1(4) . . ?
C26 N4 Zn01 124.2(3) . . ?
C15 N4 Zn01 117.4(3) . . ?
N5 C12 S2 179.8(4) . . ?
C7 C8 C1 119.9(3) . . ?
C7 C8 H8 120.0 . . ?
C1 C8 H8 120.0 . . ?
N1 C10 C20 123.3(4) . . ?
N1 C10 H10 118.3 . . ?
C20 C10 H10 118.3 . . ?
N9 N10 C9 106.8(4) . . ?
N4 C15 C32 121.8(4) . . ?
N4 C15 C4 116.4(3) . . ?
C32 C15 C4 121.7(4) . . ?
N2 C4 C15 120.0(3) . . ?
N2 C4 H4 120.0 . . ?
C15 C4 H4 120.0 . . ?
N1 C6 C18 122.7(3) . . ?
N1 C6 C5 114.8(3) . . ?
C18 C6 C5 122.4(3) . . ?
C14 C2 C11 120.1(4) . . ?
C14 C2 N3 122.9(4) . . ?
C11 C2 N3 116.8(3) . . ?
C2 C11 C22 119.8(4) . . ?
C2 C11 H11 120.1 . . ?
C22 C11 H11 120.1 . . ?
C13 C23 C1 120.2(4) . . ?
C13 C23 H23 119.9 . . ?
C1 C23 H23 119.9 . . ?
C12 N5 Zn01 165.1(3) . . ?
C9 C13 C23 120.0(4) . . ?
C9 C13 H13 120.0 . . ?
C23 C13 H13 120.0 . . ?
C6 C18 C24 119.2(4) . . ?
C6 C18 H18 120.4 . . ?
C24 C18 H18 120.4 . . ?
C13 C9 C7 120.9(4) . . ?
C13 C9 N10 113.6(4) . . ?
C7 C9 N10 125.4(4) . . ?
C27 C17 C28 119.8(4) . . ?
C27 C17 H17 120.1 . . ?
C28 C17 H17 120.1 . . ?
C8 C7 C9 119.2(4) . . ?
C8 C7 H7 120.4 . . ?
C9 C7 H7 120.4 . . ?
N6 N8 C19 109.8(4) . . ?
C31 C38 C32 119.1(5) . . ?
C31 C38 H38 120.5 . . ?
C32 C38 H38 120.5 . . ?
C15 C32 C38 119.0(5) . . ?
C15 C32 H32 120.5 . . ?
C38 C32 H32 120.5 . . ?
C19 C16 C14 120.2(4) . . ?
C19 C16 H16 119.9 . . ?
C14 C16 H16 119.9 . . ?
N3 C5 C6 119.5(3) . . ?
N3 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C2 C14 C16 119.5(4) . . ?
C2 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C10 C20 C24 119.1(4) . . ?
C10 C20 H20 120.4 . . ?
C24 C20 H20 120.4 . . ?
C19 C22 C11 120.5(4) . . ?
C19 C22 H22 119.7 . . ?
C11 C22 H22 119.7 . . ?
C17 C27 C30 121.3(4) . . ?
C17 C27 H27 119.4 . . ?
C30 C27 H27 119.4 . . ?
C20 C24 C18 118.8(4) . . ?
C20 C24 H24 120.6 . . ?
C18 C24 H24 120.6 . . ?
C30 C21 C25 119.9(4) . . ?
C30 C21 N6 113.9(4) . . ?
C25 C21 N6 126.1(4) . . ?
C34 C35 C33 121.6(5) . . ?
C34 C35 H35 119.2 . . ?
C33 C35 H35 119.2 . . ?
C17 C28 C25 119.1(4) . . ?
C17 C28 H28 120.4 . . ?
C25 C28 H28 120.4 . . ?
C33 C36 C37 119.0(5) . . ?
C33 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
N4 C26 C31 123.4(5) . . ?
N4 C26 H26 118.3 . . ?
C31 C26 H26 118.3 . . ?
C22 C19 C16 119.8(4) . . ?
C22 C19 N8 112.7(4) . . ?
C16 C19 N8 127.5(4) . . ?
N8 N6 C21 108.6(4) . . ?
C26 C31 C38 118.7(5) . . ?
C26 C31 H31 120.7 . . ?
C38 C31 H31 120.7 . . ?
C36 C33 C35 120.1(5) . . ?
C36 C33 H33 120.0 . . ?
C35 C33 H33 120.0 . . ?
C29 C34 C35 118.1(5) . . ?
C29 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
C27 C30 C21 119.9(4) . . ?
C27 C30 H30 120.1 . . ?
C21 C30 H30 120.1 . . ?
C21 C25 C28 120.0(4) . . ?
C21 C25 H25 120.0 . . ?
C28 C25 H25 120.0 . . ?
C29 C37 C36 118.0(5) . . ?
C29 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?

_diffrn_measured_fraction_theta_max 0.740
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.740
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.050
