#------------------------------------------------------------------------------
#$Date: 2016-11-08 22:23:30 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188317 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/41/1544100.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1544100
loop_
_publ_author_name
'Lakhloufi, S.'
'Lemée-Cailleau, M H'
'Chastanet, G.'
'Rosa, P.'
'Daro, N.'
'Guionneau, P.'
_publ_section_title
;
 Structural movies of the gradual spin-crossover in a molecular complex at
 various physical scales.
;
_journal_issue                   40
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              28307
_journal_page_last               28315
_journal_paper_doi               10.1039/c6cp04987g
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C38 H28 N10 S2 Zn'
_chemical_formula_weight         754.19
_chemical_name_systematic
;
     bis(N-(2-Pyridylmethylene)-4-(phenylazo)aniline)-diisothiocyanato-zinc(ii)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.756(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1195(7)
_cell_length_b                   14.4879(11)
_cell_length_c                   17.1458(13)
_cell_measurement_reflns_used    14105
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1
_cell_volume                     3747.7(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.734
_diffrn_measured_fraction_theta_max 0.734
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6247
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.7124
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube-shaped
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         4853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0909P)²+3.9881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                3908
_reflns_number_total             4853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cp04987g4.cif
_cod_data_source_block           znaza250kd
_cod_depositor_comments
'Adding full bibliography for 1544075--1544134.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1544100
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'
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
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
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
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
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
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
