#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:32:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179667 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/20/4512068.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_4512068
loop_
_publ_author_name
'Wu, Xue-Ru'
'Yang, Xü'
'Wei, Rong-Jia'
'Li, Jia'
'Zheng, Lan-Sun'
'Tao, Jun'
_publ_section_title
;
 Solvent-Mediated Isomerization of FeIIComplexes from a 3D 65·8
 Framework to a 2D 44Rhombus-Grid Network
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4891
_journal_paper_doi               10.1021/cg5011506
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C34 H24 Fe N6 S2'
_chemical_formula_weight         636.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.140(4)
_cell_angle_beta                 104.351(5)
_cell_angle_gamma                104.366(5)
_cell_formula_units_Z            1
_cell_length_a                   7.7312(4)
_cell_length_b                   9.0974(4)
_cell_length_c                   11.4447(6)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2160
_cell_measurement_theta_min      3.8620
_cell_volume                     734.33(7)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ccd area detector'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4921
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.9341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0398
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                2484
_reflns_number_total             2883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5011506_si_002.cif
_cod_data_source_block           complex_3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4512068
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Fe1 Fe 1.0000 0.5000 0.0000 0.01184(18) Uani 1 2 d S
S1 S 1.48743(9) 0.96499(7) 0.24716(7) 0.0283(2) Uani 1 1 d .
N1 N 1.0662(3) 0.3751(2) 0.14953(18) 0.0150(4) Uani 1 1 d .
N2 N 0.7539(3) 0.5138(2) 0.07391(18) 0.0150(4) Uani 1 1 d .
N3 N 1.1680(3) 0.7110(2) 0.12485(18) 0.0165(4) Uani 1 1 d .
C1 C 0.9059(3) 0.1103(3) 0.4894(2) 0.0171(5) Uani 1 1 d .
H1 H 0.8425 0.1845 0.4826 0.021 Uiso 1 1 calc R
C2 C 0.5307(3) 0.3712(3) 0.4363(2) 0.0144(5) Uani 1 1 d .
H2 H 0.5506 0.2840 0.3938 0.017 Uiso 1 1 calc R
C3 C 1.0218(3) 0.0942(3) 0.4152(2) 0.0146(5) Uani 1 1 d .
C4 C 0.4890(3) 0.3677(3) 0.5474(2) 0.0147(5) Uani 1 1 d .
H4 H 0.4825 0.2788 0.5786 0.018 Uiso 1 1 calc R
C5 C 1.3012(3) 0.8173(3) 0.1765(2) 0.0154(5) Uani 1 1 d .
C6 C 0.5431(3) 0.5032(3) 0.3876(2) 0.0142(5) Uani 1 1 d .
C7 C 0.6457(3) 0.3805(3) 0.0872(2) 0.0160(5) Uani 1 1 d .
H7 H 0.6230 0.2886 0.0291 0.019 Uiso 1 1 calc R
C8 C 1.0424(3) 0.1918(3) 0.3255(2) 0.0148(5) Uani 1 1 d .
C9 C 0.5986(3) 0.5082(3) 0.2726(2) 0.0134(5) Uani 1 1 d .
C10 C 0.8836(3) 0.0179(3) 0.5728(2) 0.0172(5) Uani 1 1 d .
H10 H 0.8055 0.0304 0.6212 0.021 Uiso 1 1 calc R
C11 C 1.0469(3) 0.3476(3) 0.3514(2) 0.0155(5) Uani 1 1 d .
H11 H 1.0404 0.3936 0.4282 0.019 Uiso 1 1 calc R
C12 C 0.6974(3) 0.6484(3) 0.2531(2) 0.0153(5) Uani 1 1 d .
H12 H 0.7143 0.7429 0.3062 0.018 Uiso 1 1 calc R
C13 C 1.0580(3) 0.1328(3) 0.2085(2) 0.0179(5) Uani 1 1 d .
H13 H 1.0619 0.0309 0.1874 0.022 Uiso 1 1 calc R
C14 C 1.0674(4) 0.2260(3) 0.1257(2) 0.0181(5) Uani 1 1 d .
H14 H 1.0750 0.1834 0.0484 0.022 Uiso 1 1 calc R
C15 C 1.0609(3) 0.4342(3) 0.2637(2) 0.0169(5) Uani 1 1 d .
H15 H 1.0669 0.5388 0.2846 0.020 Uiso 1 1 calc R
C16 C 0.7700(3) 0.6451(3) 0.1539(2) 0.0161(5) Uani 1 1 d .
H16 H 0.8338 0.7398 0.1419 0.019 Uiso 1 1 calc R
C17 C 0.5665(3) 0.3732(3) 0.1830(2) 0.0168(5) Uani 1 1 d .
H17 H 0.4919 0.2782 0.1876 0.020 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'
Fe Fe 0.3463 0.8444 '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'
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
N3 Fe1 N3 180.0 . 2_765
N3 Fe1 N1 90.67(7) . 2_765
N3 Fe1 N1 89.33(7) 2_765 2_765
N3 Fe1 N1 89.33(7) . .
N3 Fe1 N1 90.67(7) 2_765 .
N1 Fe1 N1 180.00(7) 2_765 .
N3 Fe1 N2 90.49(7) . .
N3 Fe1 N2 89.51(7) 2_765 .
N1 Fe1 N2 96.74(7) 2_765 .
N1 Fe1 N2 83.26(7) . .
N3 Fe1 N2 89.51(7) . 2_765
N3 Fe1 N2 90.49(7) 2_765 2_765
N1 Fe1 N2 83.26(7) 2_765 2_765
N1 Fe1 N2 96.74(7) . 2_765
N2 Fe1 N2 180.0 . 2_765
C14 N1 C15 116.4(2) . .
C14 N1 Fe1 122.44(15) . .
C15 N1 Fe1 119.28(15) . .
C16 N2 C7 116.10(19) . .
C16 N2 Fe1 118.69(15) . .
C7 N2 Fe1 117.65(15) . .
C5 N3 Fe1 158.71(17) . .
C10 C1 C3 121.3(2) . .
C4 C2 C6 121.1(2) . .
C1 C3 C10 118.4(2) . 2_756
C1 C3 C8 120.7(2) . .
C10 C3 C8 120.8(2) 2_756 .
C2 C4 C6 120.5(2) . 2_666
N3 C5 S1 179.4(2) . .
C2 C6 C4 118.4(2) . 2_666
C2 C6 C9 120.3(2) . .
C4 C6 C9 121.2(2) 2_666 .
N2 C7 C17 123.4(2) . .
C11 C8 C13 116.1(2) . .
C11 C8 C3 121.9(2) . .
C13 C8 C3 121.9(2) . .
C17 C9 C12 116.6(2) . .
C17 C9 C6 122.1(2) . .
C12 C9 C6 121.2(2) . .
C1 C10 C3 120.3(2) . 2_756
C15 C11 C8 120.3(2) . .
C16 C12 C9 119.3(2) . .
C14 C13 C8 119.8(2) . .
N1 C14 C13 123.9(2) . .
N1 C15 C11 123.4(2) . .
N2 C16 C12 124.1(2) . .
C7 C17 C9 120.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N3 2.0940(18) .
Fe1 N3 2.0940(18) 2_765
Fe1 N1 2.226(2) 2_765
Fe1 N1 2.226(2) .
Fe1 N2 2.2878(18) .
Fe1 N2 2.2878(18) 2_765
S1 C5 1.628(2) .
N1 C14 1.343(3) .
N1 C15 1.347(3) .
N2 C16 1.343(3) .
N2 C7 1.346(3) .
N3 C5 1.169(3) .
C1 C10 1.382(3) .
C1 C3 1.396(3) .
C2 C4 1.390(3) .
C2 C6 1.395(3) .
C3 C10 1.399(3) 2_756
C3 C8 1.473(3) .
C4 C6 1.398(3) 2_666
C6 C4 1.398(3) 2_666
C6 C9 1.485(3) .
C7 C17 1.385(3) .
C8 C11 1.391(3) .
C8 C13 1.407(3) .
C9 C17 1.394(3) .
C9 C12 1.397(3) .
C10 C3 1.399(3) 2_756
C11 C15 1.379(3) .
C12 C16 1.385(3) .
C13 C14 1.372(3) .
