#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:33:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179066 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/28/4302880.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_4302880
loop_
_publ_author_name
'Carsten Milsmann'
'Goutam Kumar Patra'
'Eckhard Bill'
'Thomas Weyhermüller'
'Serena DeBeer George'
'Karl Wieghardt'
_publ_section_title
;
Octahedral Monodithiolene Complexes of Iron: Characterization
of S,S'-Coordinated Dithiolate(1-) π Radical Monoanions: A
Spectroscopic and Density Functional Theoretical Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7430
_journal_page_last               7445
_journal_paper_doi               10.1021/ic900936p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C14 H24 Fe N6 S2, B F4'
_chemical_formula_sum            'C14 H24 B F4 Fe N6 S2'
_chemical_formula_weight         483.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.786(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5350(3)
_cell_length_b                   12.2605(4)
_cell_length_c                   18.9435(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1959.05(11)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'629 images at 1.0 deg. stepwise rotation in omega and phi, 110 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37245
_diffrn_reflns_theta_full        33.16
_diffrn_reflns_theta_max         33.16
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Vers. 2006/1, Bruker AXS (2006)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0320
_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)+(0.0288P)²+1.0754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                6176
_reflns_number_total             7433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900936p_si_002_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302880
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.75231(2) 0.800523(14) 0.118194(9) 0.01225(4) Uani 1 1 d . . .
N1 N 0.83226(12) 0.64198(8) 0.14169(6) 0.01545(19) Uani 1 1 d . . .
H1 H 0.7452 0.6015 0.1505 0.019 Uiso 1 1 calc R . .
N5 N 0.67281(12) 0.75385(9) 0.01599(6) 0.01544(19) Uani 1 1 d . . .
H5 H 0.6685 0.8181 -0.0103 0.019 Uiso 1 1 calc R . .
N8 N 0.51969(12) 0.77190(9) 0.13059(6) 0.01485(19) Uani 1 1 d . . .
H8 H 0.5149 0.6997 0.1452 0.018 Uiso 1 1 calc R . .
N12 N 0.81035(13) 0.81924(8) 0.22637(6) 0.01535(19) Uani 1 1 d . . .
H12 H 0.9012 0.8622 0.2322 0.018 Uiso 1 1 calc R . .
C2 C 0.90833(16) 0.57962(10) 0.08855(7) 0.0190(2) Uani 1 1 d . . .
H2A H 0.9355 0.5056 0.1075 0.023 Uiso 1 1 calc R . .
H2B H 1.0082 0.6164 0.0817 0.023 Uiso 1 1 calc R . .
C3 C 0.80228(16) 0.56987(11) 0.01697(7) 0.0205(2) Uani 1 1 d . . .
H3A H 0.7000 0.5372 0.0244 0.025 Uiso 1 1 calc R . .
H3B H 0.8525 0.5197 -0.0139 0.025 Uiso 1 1 calc R . .
C4 C 0.77037(16) 0.67816(11) -0.02128(7) 0.0195(2) Uani 1 1 d . . .
H4A H 0.8728 0.7137 -0.0253 0.023 Uiso 1 1 calc R . .
H4B H 0.7147 0.6645 -0.0703 0.023 Uiso 1 1 calc R . .
C6 C 0.50537(15) 0.71554(11) 0.00771(7) 0.0187(2) Uani 1 1 d . . .
H6A H 0.5022 0.6366 0.0184 0.022 Uiso 1 1 calc R . .
H6B H 0.4528 0.7274 -0.0420 0.022 Uiso 1 1 calc R . .
C7 C 0.42086(15) 0.77888(11) 0.05870(7) 0.0173(2) Uani 1 1 d . . .
H7A H 0.4078 0.8559 0.0433 0.021 Uiso 1 1 calc R . .
H7B H 0.3146 0.7474 0.0601 0.021 Uiso 1 1 calc R . .
C9 C 0.44489(15) 0.83817(11) 0.18223(7) 0.0171(2) Uani 1 1 d . . .
H9A H 0.3342 0.8136 0.1815 0.020 Uiso 1 1 calc R . .
H9B H 0.4422 0.9156 0.1673 0.020 Uiso 1 1 calc R . .
C10 C 0.53399(15) 0.82862(11) 0.25752(7) 0.0177(2) Uani 1 1 d . . .
H10A H 0.5425 0.7505 0.2709 0.021 Uiso 1 1 calc R . .
H10B H 0.4720 0.8654 0.2907 0.021 Uiso 1 1 calc R . .
C11 C 0.69901(15) 0.87756(10) 0.26689(7) 0.0173(2) Uani 1 1 d . . .
H11A H 0.6910 0.9546 0.2511 0.021 Uiso 1 1 calc R . .
H11B H 0.7436 0.8768 0.3183 0.021 Uiso 1 1 calc R . .
C13 C 0.86242(16) 0.71389(10) 0.26161(7) 0.0184(2) Uani 1 1 d . . .
H13A H 0.7697 0.6734 0.2737 0.022 Uiso 1 1 calc R . .
H13B H 0.9366 0.7275 0.3062 0.022 Uiso 1 1 calc R . .
C14 C 0.94340(15) 0.64855(10) 0.21038(7) 0.0174(2) Uani 1 1 d . . .
H14A H 1.0434 0.6845 0.2029 0.021 Uiso 1 1 calc R . .
H14B H 0.9687 0.5745 0.2296 0.021 Uiso 1 1 calc R . .
S21 S 0.68489(4) 0.97617(2) 0.098836(17) 0.01571(6) Uani 1 1 d . . .
C22 C 0.86275(15) 1.03999(10) 0.09215(6) 0.0144(2) Uani 1 1 d . . .
C23 C 0.99910(14) 0.98118(10) 0.09319(6) 0.0142(2) Uani 1 1 d . . .
S24 S 0.99709(4) 0.84049(2) 0.098222(17) 0.01527(6) Uani 1 1 d . . .
C25 C 0.86252(14) 1.15653(10) 0.08525(6) 0.0153(2) Uani 1 1 d . . .
N26 N 0.86051(13) 1.25004(9) 0.07918(6) 0.0188(2) Uani 1 1 d . . .
C27 C 1.14743(15) 1.03394(10) 0.09087(7) 0.0171(2) Uani 1 1 d . . .
N28 N 1.26810(14) 1.07567(10) 0.09031(7) 0.0237(2) Uani 1 1 d . . .
B30 B 1.42068(18) 0.50690(12) 0.17641(9) 0.0205(3) Uani 1 1 d . . .
F31 F 1.50352(13) 0.49556(10) 0.11841(6) 0.0409(3) Uani 1 1 d . . .
F32 F 1.29127(11) 0.57358(8) 0.15665(6) 0.0387(2) Uani 1 1 d . . .
F33 F 1.37705(11) 0.40591(7) 0.19835(5) 0.0324(2) Uani 1 1 d . . .
F34 F 1.52639(12) 0.55580(8) 0.23065(6) 0.0409(3) 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Fe1 N12 168.40(4) . . ?
N5 Fe1 N8 82.74(4) . . ?
N12 Fe1 N8 89.72(4) . . ?
N5 Fe1 N1 89.52(4) . . ?
N12 Fe1 N1 82.50(4) . . ?
N8 Fe1 N1 96.10(4) . . ?
N5 Fe1 S24 94.89(3) . . ?
N12 Fe1 S24 93.18(3) . . ?
N8 Fe1 S24 175.64(3) . . ?
N1 Fe1 S24 87.51(3) . . ?
N5 Fe1 S21 94.27(3) . . ?
N12 Fe1 S21 94.18(3) . . ?
N8 Fe1 S21 87.40(3) . . ?
N1 Fe1 S21 175.14(3) . . ?
S24 Fe1 S21 89.138(12) . . ?
C2 N1 C14 109.43(10) . . ?
C2 N1 Fe1 119.75(8) . . ?
C14 N1 Fe1 106.25(7) . . ?
C6 N5 C4 110.44(10) . . ?
C6 N5 Fe1 111.36(8) . . ?
C4 N5 Fe1 119.72(8) . . ?
C9 N8 C7 109.23(10) . . ?
C9 N8 Fe1 119.90(8) . . ?
C7 N8 Fe1 107.83(8) . . ?
C13 N12 C11 110.78(10) . . ?
C13 N12 Fe1 111.19(8) . . ?
C11 N12 Fe1 119.54(8) . . ?
N1 C2 C3 112.50(10) . . ?
C2 C3 C4 113.41(11) . . ?
N5 C4 C3 112.97(11) . . ?
N5 C6 C7 108.39(10) . . ?
N8 C7 C6 107.25(10) . . ?
N8 C9 C10 111.88(10) . . ?
C9 C10 C11 113.79(11) . . ?
N12 C11 C10 113.79(10) . . ?
N12 C13 C14 107.90(10) . . ?
N1 C14 C13 107.33(10) . . ?
C22 S21 Fe1 103.89(4) . . ?
C23 C22 C25 121.07(11) . . ?
C23 C22 S21 121.02(9) . . ?
C25 C22 S21 117.92(9) . . ?
C22 C23 C27 121.16(11) . . ?
C22 C23 S24 120.79(9) . . ?
C27 C23 S24 118.04(9) . . ?
C23 S24 Fe1 104.23(4) . . ?
N26 C25 C22 179.14(15) . . ?
N28 C27 C23 178.65(14) . . ?
F33 B30 F32 111.91(12) . . ?
F33 B30 F34 109.80(12) . . ?
F32 B30 F34 110.26(12) . . ?
F33 B30 F31 109.87(12) . . ?
F32 B30 F31 108.97(12) . . ?
F34 B30 F31 105.85(12) . . ?
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 2.0335(11) . ?
Fe1 N12 2.0463(11) . ?
Fe1 N8 2.0646(11) . ?
Fe1 N1 2.0855(10) . ?
Fe1 S24 2.2337(4) . ?
Fe1 S21 2.2447(3) . ?
N1 C2 1.4897(16) . ?
N1 C14 1.4908(17) . ?
N5 C6 1.4897(16) . ?
N5 C4 1.4941(16) . ?
N8 C9 1.4884(16) . ?
N8 C7 1.4908(16) . ?
N12 C13 1.4902(16) . ?
N12 C11 1.4921(16) . ?
C2 C3 1.5158(19) . ?
C3 C4 1.5172(19) . ?
C6 C7 1.5065(18) . ?
C9 C10 1.5149(18) . ?
C10 C11 1.5162(18) . ?
C13 C14 1.5053(18) . ?
S21 C22 1.7296(13) . ?
C22 C23 1.3666(17) . ?
C22 C25 1.4348(17) . ?
C23 C27 1.4283(17) . ?
C23 S24 1.7278(12) . ?
C25 N26 1.1521(17) . ?
C27 N28 1.1515(17) . ?
B30 F33 1.3755(17) . ?
B30 F32 1.3792(17) . ?
B30 F34 1.3950(18) . ?
B30 F31 1.4014(19) . ?
