#------------------------------------------------------------------------------
#$Date: 2019-12-12 12:37:28 +0200 (Thu, 12 Dec 2019) $
#$Revision: 245018 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556530.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_1556530
loop_
_publ_author_name
'Iwai, S.'
'Yoshinami, K.'
'Nakashima, S.'
_publ_section_title
;
 Structure and Spin State of Iron(II) Assembled Complexes Using
 9,10-Bis(4-pyridyl)anthracene as Bridging Ligand
;
_journal_name_full               Inorganics
_journal_page_first              61
_journal_paper_doi               10.3390/inorganics5030061
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C50 H32 Fe N6 S2'
_chemical_formula_weight         836.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6020(7)
_cell_length_b                   18.9796(14)
_cell_length_c                   23.8123(18)
_cell_measurement_reflns_used    5061
_cell_measurement_temperature    173.0(2)
_cell_measurement_theta_max      27.2709
_cell_measurement_theta_min      2.3771
_cell_volume                     4339.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'APEX2(Bruker AXS)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'XSHELL V6.3.1(Bruker AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT (Sheldrick 2013)'
_diffrn_ambient_temperature      173.0(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12163
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.622
_refine_diff_density_min         -1.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0974P)²+25.8840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1786
_reflns_number_gt                2125
_reflns_number_total             2537
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            inorganics-2017-5-61.cif
_cod_data_source_block           I
_cod_database_code               1556530
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.5 0.5 0.5 0.0200(2) Uani d T P S 1 . .
S S1 0.0535(2) 0.37237(14) 0.5 0.0856(7) Uani d T P S 1 . .
N N1 0.4246(3) 0.57245(13) 0.56820(10) 0.0296(5) Uani d . . . 1 . .
N N2 0.3041(4) 0.44972(18) 0.5 0.0282(7) Uani d T P S 1 . .
C C1 0.3380(3) 0.66100(17) 0.65683(13) 0.0359(7) Uani d . . . 1 . .
C C2 0.2453(4) 0.6330(2) 0.61897(16) 0.0509(10) Uani d . . . 1 . .
H H2 0.149 0.6439 0.6221 0.061 Uiso calc U . R 1 . .
C C3 0.2906(3) 0.5890(2) 0.57623(15) 0.0436(9) Uani d . . . 1 . .
H H3 0.2232 0.5696 0.5514 0.052 Uiso calc U . R 1 . .
C C4 0.5141(4) 0.6005(2) 0.60431(17) 0.0559(12) Uani d . . . 1 . .
H H4 0.6102 0.5903 0.5994 0.067 Uiso calc U . R 1 . .
C C5 0.4764(4) 0.6438(2) 0.64876(18) 0.0609(13) Uani d . . . 1 . .
H H5 0.5455 0.6616 0.6735 0.073 Uiso calc U . R 1 . .
C C6 0.2925(3) 0.70676(17) 0.70466(13) 0.0354(7) Uani d . . . 1 . .
C C7 0.2197(4) 0.60142(19) 0.75878(17) 0.0494(9) Uani d . . . 1 . .
H H7 0.2487 0.5715 0.729 0.059 Uiso calc U . R 1 . .
C C8 0.1655(4) 0.5725(2) 0.80564(19) 0.0559(10) Uani d . . . 1 . .
H H8 0.1543 0.5228 0.8078 0.067 Uiso calc U . R 1 . .
C C9 0.1249(4) 0.6154(2) 0.85196(17) 0.0509(9) Uani d . . . 1 . .
H H9 0.0893 0.5944 0.8852 0.061 Uiso calc U . R 1 . .
C C10 0.1374(3) 0.68626(19) 0.84838(15) 0.0434(8) Uani d . . . 1 . .
H H10 0.1096 0.7145 0.8794 0.052 Uiso calc U . R 1 . .
C C11 0.1912(3) 0.71974(18) 0.79933(13) 0.0354(7) Uani d . . . 1 . .
C C12 0.2346(3) 0.67608(17) 0.75275(14) 0.0372(7) Uani d . . . 1 . .
C C13 0.1990(5) 0.4193(3) 0.5 0.0441(11) Uani d T P S 1 . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Fe1 N2 9_666 . 180.0
N2 Fe1 N1 9_666 9_666 89.41(9)
N2 Fe1 N1 . 9_666 90.59(9)
N2 Fe1 N1 9_666 10_556 90.59(9)
N2 Fe1 N1 . 10_556 89.41(9)
N1 Fe1 N1 9_666 10_556 87.47(13)
N2 Fe1 N1 9_666 2_665 89.41(9)
N2 Fe1 N1 . 2_665 90.59(9)
N1 Fe1 N1 9_666 2_665 92.53(13)
N1 Fe1 N1 10_556 2_665 180.00(8)
N2 Fe1 N1 9_666 . 90.59(9)
N2 Fe1 N1 . . 89.41(9)
N1 Fe1 N1 9_666 . 180.0
N1 Fe1 N1 10_556 . 92.53(13)
N1 Fe1 N1 2_665 . 87.47(13)
C4 N1 C3 . . 115.8(3)
C4 N1 Fe1 . . 120.4(2)
C3 N1 Fe1 . . 123.79(19)
C13 N2 Fe1 . . 177.1(4)
C2 C1 C5 . . 116.1(3)
C2 C1 C6 . . 122.3(3)
C5 C1 C6 . . 121.6(3)
C1 C2 C3 . . 120.7(3)
C1 C2 H2 . . 119.6
C3 C2 H2 . . 119.6
N1 C3 C2 . . 123.2(3)
N1 C3 H3 . . 118.4
C2 C3 H3 . . 118.4
N1 C4 C5 . . 124.3(3)
N1 C4 H4 . . 117.9
C5 C4 H4 . . 117.9
C4 C5 C1 . . 119.8(3)
C4 C5 H5 . . 120.1
C1 C5 H5 . . 120.1
C12 C6 C11 . 13_566 120.8(3)
C12 C6 C1 . . 119.8(3)
C11 C6 C1 13_566 . 119.4(3)
C8 C7 C12 . . 121.7(3)
C8 C7 H7 . . 119.2
C12 C7 H7 . . 119.2
C7 C8 C9 . . 120.9(4)
C7 C8 H8 . . 119.6
C9 C8 H8 . . 119.6
C10 C9 C8 . . 119.7(4)
C10 C9 H9 . . 120.2
C8 C9 H9 . . 120.2
C9 C10 C11 . . 121.8(3)
C9 C10 H10 . . 119.1
C11 C10 H10 . . 119.1
C6 C11 C10 13_566 . 122.5(3)
C6 C11 C12 13_566 . 119.0(3)
C10 C11 C12 . . 118.5(3)
C6 C12 C7 . . 122.3(3)
C6 C12 C11 . . 120.2(3)
C7 C12 C11 . . 117.5(3)
N2 C13 S1 . . 177.3(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 N2 9_666 2.110(4)
Fe1 N2 . 2.110(4)
Fe1 N1 9_666 2.248(2)
Fe1 N1 10_556 2.248(2)
Fe1 N1 2_665 2.248(2)
Fe1 N1 . 2.248(2)
S1 C13 . 1.657(6)
N1 C4 . 1.327(4)
N1 C3 . 1.338(4)
N2 C13 . 1.162(6)
C1 C2 . 1.374(4)
C1 C5 . 1.382(4)
C1 C6 . 1.497(4)
C2 C3 . 1.387(4)
C2 H2 . 0.95
C3 H3 . 0.95
C4 C5 . 1.388(4)
C4 H4 . 0.95
C5 H5 . 0.95
C6 C12 . 1.400(5)
C6 C11 13_566 1.407(5)
C7 C8 . 1.348(6)
C7 C12 . 1.431(5)
C7 H7 . 0.95
C8 C9 . 1.426(5)
C8 H8 . 0.95
C9 C10 . 1.353(5)
C9 H9 . 0.95
C10 C11 . 1.427(5)
C10 H10 . 0.95
C11 C6 13_566 1.407(5)
C11 C12 . 1.446(4)
