#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:45:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179346 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/43/4324305.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_4324305
loop_
_publ_author_name
'Feng-Lei Yang'
'Jun Tao'
'Rong-Bin Huang'
'Lan-Sun Zheng'
_publ_contact_author_address
;
Department of Chemistry
Xiamen University
Xiamen 361005
P. R. China
;
_publ_contact_author_email       taojun@xmu.edu.cn
_publ_contact_author_name        'Prof. Jun Tao'
_publ_contact_author_phone       86-592-2188138
_publ_section_title
;
 Temperature-Dependent in Situ Ligand Cyclization via C=C Coupling and
 Formation of a Spin-Crossover Iron(II) Coordination Polymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              911
_journal_page_last               917
_journal_paper_doi               10.1021/ic101490a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H28 N10 S2 Zn'
_chemical_formula_weight         658.15
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.901(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.799(4)
_cell_length_b                   9.6101(3)
_cell_length_c                   16.1899(13)
_cell_measurement_reflns_used    3859
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0903
_cell_measurement_theta_min      3.1406
_cell_volume                     3085.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7707
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.8296
_exptl_absorpt_correction_T_min  0.6976
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0455P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                2502
_reflns_number_total             3312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101490a_si_001_5.cif
_cod_data_source_block           complex1b
_cod_original_cell_volume        3085.5(6)
_cod_database_code               4324305
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Zn1 Zn -0.5000 1.01963(3) -0.2500 0.02560(11) Uani 1 2 d S
C1 C -0.41543(11) 0.75784(19) -0.22714(16) 0.0319(5) Uani 1 1 d .
H1B H -0.4103 0.7438 -0.1659 0.038 Uiso 1 1 calc R
C2 C -0.38474(11) 0.6659(2) -0.25205(16) 0.0312(5) Uani 1 1 d .
H2A H -0.3596 0.5921 -0.2082 0.037 Uiso 1 1 calc R
C3 C -0.39140(10) 0.68363(19) -0.34368(16) 0.0266(4) Uani 1 1 d .
C4 C -0.42710(11) 0.8004(2) -0.40175(16) 0.0318(5) Uani 1 1 d .
H4A H -0.4308 0.8208 -0.4611 0.038 Uiso 1 1 calc R
C5 C -0.45700(12) 0.8859(2) -0.37213(17) 0.0344(5) Uani 1 1 d .
H5A H -0.4819 0.9614 -0.4140 0.041 Uiso 1 1 calc R
C6 C -0.36097(11) 0.5908(2) -0.37674(16) 0.0294(5) Uani 1 1 d .
C7 C -0.27215(15) 0.4515(2) -0.3975(3) 0.0572(8) Uani 1 1 d .
H7A H -0.2577 0.3890 -0.4278 0.069 Uiso 1 1 calc R
H7B H -0.2323 0.4900 -0.3347 0.069 Uiso 1 1 calc R
C8 C -0.31485(15) 0.5683(2) -0.4729(2) 0.0575(8) Uani 1 1 d .
H8A H -0.2876 0.6241 -0.4851 0.069 Uiso 1 1 calc R
H8B H -0.3519 0.5291 -0.5384 0.069 Uiso 1 1 calc R
C9 C -0.35275(11) 0.45071(19) -0.35927(18) 0.0326(5) Uani 1 1 d .
C10 C -0.38591(11) 0.36513(19) -0.32633(16) 0.0289(5) Uani 1 1 d .
C11 C -0.35184(11) 0.2559(2) -0.25794(18) 0.0385(6) Uani 1 1 d .
H11A H -0.3066 0.2405 -0.2285 0.046 Uiso 1 1 calc R
C12 C -0.38462(11) 0.1705(2) -0.23355(18) 0.0371(5) Uani 1 1 d .
H12A H -0.3602 0.0991 -0.1863 0.045 Uiso 1 1 calc R
C13 C -0.48276(10) 0.29010(19) -0.33929(16) 0.0286(5) Uani 1 1 d .
H13A H -0.5280 0.3023 -0.3678 0.034 Uiso 1 1 calc R
C14 C -0.45345(11) 0.3816(2) -0.36636(16) 0.0299(5) Uani 1 1 d .
H14A H -0.4785 0.4546 -0.4113 0.036 Uiso 1 1 calc R
N1 N -0.45229(9) 0.86640(16) -0.28627(13) 0.0298(4) Uani 1 1 d .
N2 N -0.34089(10) 0.65473(17) -0.43130(15) 0.0407(5) Uani 1 1 d .
H2B H -0.3439 0.7434 -0.4400 0.049 Uiso 1 1 d R
N3 N -0.31137(11) 0.37655(18) -0.37385(19) 0.0534(6) Uani 1 1 d .
H3A H -0.3092 0.2873 -0.3689 0.064 Uiso 1 1 d R
N4 N -0.44962(9) 0.18416(15) -0.27393(13) 0.0287(4) Uani 1 1 d .
S1 S -0.71067(4) 0.98203(7) -0.59728(6) 0.0628(2) Uani 1 1 d .
C15 C -0.63686(12) 1.00020(18) -0.48532(18) 0.0308(5) Uani 1 1 d .
N5 N -0.58484(10) 1.01524(18) -0.40799(14) 0.0371(4) Uani 1 1 d .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N5 Zn1 N5 177.72(9) . 2_454
N5 Zn1 N1 90.32(7) . 2_454
N5 Zn1 N1 88.14(7) 2_454 2_454
N5 Zn1 N1 88.14(7) . .
N5 Zn1 N1 90.32(7) 2_454 .
N1 Zn1 N1 94.96(9) 2_454 .
N5 Zn1 N4 93.40(7) . 1_565
N5 Zn1 N4 88.25(7) 2_454 1_565
N1 Zn1 N4 174.75(6) 2_454 1_565
N1 Zn1 N4 88.88(6) . 1_565
N5 Zn1 N4 88.25(7) . 2_464
N5 Zn1 N4 93.40(7) 2_454 2_464
N1 Zn1 N4 88.88(6) 2_454 2_464
N1 Zn1 N4 174.75(6) . 2_464
N4 Zn1 N4 87.51(8) 1_565 2_464
N1 C1 C2 123.50(18) . .
N1 C1 H1B 118.2 . .
C2 C1 H1B 118.2 . .
C1 C2 C3 119.88(18) . .
C1 C2 H2A 120.1 . .
C3 C2 H2A 120.1 . .
C4 C3 C2 115.93(17) . .
C4 C3 C6 120.31(17) . .
C2 C3 C6 123.70(18) . .
C5 C4 C3 120.41(18) . .
C5 C4 H4A 119.8 . .
C3 C4 H4A 119.8 . .
N1 C5 C4 123.48(19) . .
N1 C5 H5A 118.3 . .
C4 C5 H5A 118.3 . .
C9 C6 N2 120.09(17) . .
C9 C6 C3 124.85(17) . .
N2 C6 C3 115.06(17) . .
N3 C7 C8 109.1(2) . .
N3 C7 H7A 109.9 . .
C8 C7 H7A 109.9 . .
N3 C7 H7B 109.9 . .
C8 C7 H7B 109.9 . .
H7A C7 H7B 108.3 . .
N2 C8 C7 109.9(2) . .
N2 C8 H8A 109.7 . .
C7 C8 H8A 109.7 . .
N2 C8 H8B 109.7 . .
C7 C8 H8B 109.7 . .
H8A C8 H8B 108.2 . .
C6 C9 N3 120.47(17) . .
C6 C9 C10 125.44(17) . .
N3 C9 C10 114.08(17) . .
C11 C10 C14 116.32(18) . .
C11 C10 C9 120.53(19) . .
C14 C10 C9 123.00(19) . .
C12 C11 C10 120.12(19) . .
C12 C11 H11A 119.9 . .
C10 C11 H11A 119.9 . .
N4 C12 C11 123.48(19) . .
N4 C12 H12A 118.3 . .
C11 C12 H12A 118.3 . .
N4 C13 C14 123.37(19) . .
N4 C13 H13A 118.3 . .
C14 C13 H13A 118.3 . .
C13 C14 C10 119.87(19) . .
C13 C14 H14A 120.1 . .
C10 C14 H14A 120.1 . .
C5 N1 C1 116.68(17) . .
C5 N1 Zn1 117.59(13) . .
C1 N1 Zn1 125.63(13) . .
C6 N2 C8 118.27(17) . .
C6 N2 H2B 120.8 . .
C8 N2 H2B 120.9 . .
C9 N3 C7 118.60(17) . .
C9 N3 H3A 120.7 . .
C7 N3 H3A 120.7 . .
C12 N4 C13 116.80(16) . .
C12 N4 Zn1 119.50(13) . 1_545
C13 N4 Zn1 123.04(13) . 1_545
N5 C15 S1 178.4(2) . .
C15 N5 Zn1 165.91(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N5 2.123(2) .
Zn1 N5 2.123(2) 2_454
Zn1 N1 2.1788(16) 2_454
Zn1 N1 2.1788(16) .
Zn1 N4 2.1891(15) 1_565
Zn1 N4 2.1891(15) 2_464
C1 N1 1.338(2) .
C1 C2 1.375(3) .
C1 H1B 0.9300 .
C2 C3 1.401(3) .
C2 H2A 0.9300 .
C3 C4 1.388(3) .
C3 C6 1.462(3) .
C4 C5 1.372(3) .
C4 H4A 0.9300 .
C5 N1 1.337(2) .
C5 H5A 0.9300 .
C6 C9 1.366(3) .
C6 N2 1.390(2) .
C7 N3 1.434(3) .
C7 C8 1.523(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 N2 1.444(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 N3 1.381(2) .
C9 C10 1.471(3) .
C10 C11 1.385(3) .
C10 C14 1.395(3) .
C11 C12 1.370(3) .
C11 H11A 0.9300 .
C12 N4 1.333(3) .
C12 H12A 0.9300 .
C13 N4 1.337(2) .
C13 C14 1.370(3) .
C13 H13A 0.9300 .
C14 H14A 0.9300 .
N2 H2B 0.8600 .
N3 H3A 0.8600 .
N4 Zn1 2.1891(15) 1_545
S1 C15 1.638(3) .
C15 N5 1.146(3) .
