#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318272.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_4318272
loop_
_publ_author_name
'Jason A. Halfen'
'Heather L. Moore'
'Derek C. Fox'
_publ_section_title
;
 Synthetic Models of the Reduced Active Site of Superoxide Reductase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3935
_journal_page_last               3943
_journal_paper_doi               10.1021/ic025517l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C24 H35 B F4 Fe N4 S'
_chemical_formula_weight         554.28
_chemical_name_common            '[(L8py2)Fe(SC6H11)]BF4 (7)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 112.18(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.532(3)
_cell_length_b                   12.157(1)
_cell_length_c                   14.028(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.17
_cell_measurement_theta_min      9.43
_cell_volume                     2768.6(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_method       'omega 2-theta 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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2651
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.09
_diffrn_standards_interval_count 2
_diffrn_standards_interval_time  '5400 seconds'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9160
_exptl_absorpt_correction_type   'psi-scan corrections'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0745P)²+3.4287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                1782
_reflns_number_total             2560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025517l_s1_7.cif
_cod_data_source_block           compd7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2768.6(8)
_cod_database_code               4318272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.44506(5) 0.0000 0.22466(6) 0.0671(3) Uani 1 2 d S . .
S1 S 0.37869(13) 0.0000 0.05182(14) 0.1177(9) Uani 1 2 d S . .
N1 N 0.5505(2) -0.1171(4) 0.2667(3) 0.0850(11) Uani 1 1 d . . .
N2 N 0.4025(2) -0.1431(3) 0.2854(3) 0.0713(9) Uani 1 1 d . . .
C1 C 0.5996(3) -0.1038(6) 0.2000(4) 0.115(2) Uani 1 1 d . . .
H1A H 0.6366 -0.1661 0.2114 0.139 Uiso 1 1 calc R . .
H1B H 0.5622 -0.1055 0.1285 0.139 Uiso 1 1 calc R . .
C2 C 0.6492(5) 0.0000 0.2189(6) 0.125(4) Uani 1 2 d S . .
H2A H 0.6806 0.0000 0.1748 0.150 Uiso 1 2 calc SR . .
H2B H 0.6883 0.0000 0.2896 0.150 Uiso 1 2 calc SR . .
C3 C 0.6033(3) -0.1074(5) 0.3785(3) 0.0980(17) Uani 1 1 d . . .
H3A H 0.6608 -0.1124 0.3871 0.118 Uiso 1 1 calc R . .
H3B H 0.5915 -0.1683 0.4155 0.118 Uiso 1 1 calc R . .
C4 C 0.5894(4) 0.0000 0.4247(5) 0.092(2) Uani 1 2 d S . .
H4A H 0.5331 0.0000 0.4212 0.111 Uiso 1 2 calc SR . .
H4B H 0.6250 0.0000 0.4970 0.111 Uiso 1 2 calc SR . .
C5 C 0.5107(4) -0.2250(5) 0.2445(4) 0.1058(18) Uani 1 1 d . . .
H5A H 0.5517 -0.2821 0.2726 0.127 Uiso 1 1 calc R . .
H5B H 0.4852 -0.2354 0.1706 0.127 Uiso 1 1 calc R . .
C6 C 0.4463(3) -0.2340(4) 0.2909(4) 0.0896(14) Uani 1 1 d . . .
C7 C 0.4321(5) -0.3281(5) 0.3331(6) 0.132(2) Uani 1 1 d . . .
H7A H 0.4643 -0.3899 0.3365 0.158 Uiso 1 1 calc R . .
C8 C 0.3706(5) -0.3330(5) 0.3708(6) 0.134(2) Uani 1 1 d . . .
H8A H 0.3616 -0.3968 0.4016 0.161 Uiso 1 1 calc R . .
C9 C 0.3235(4) -0.2429(4) 0.3622(4) 0.1037(17) Uani 1 1 d . . .
H9A H 0.2800 -0.2443 0.3848 0.124 Uiso 1 1 calc R . .
C10 C 0.3407(3) -0.1496(4) 0.3197(4) 0.0811(13) Uani 1 1 d . . .
H10A H 0.3081 -0.0878 0.3143 0.097 Uiso 1 1 calc R . .
C11 C 0.2703(5) 0.0000 0.0404(9) 0.144(4) Uani 1 2 d S . .
H11A H 0.2758 0.0000 0.1126 0.173 Uiso 1 2 calc SR . .
C12 C 0.2312(6) 0.0992(10) 0.0049(11) 0.250(5) Uani 1 1 d U . .
H12A H 0.2306 0.1131 -0.0634 0.301 Uiso 1 1 calc R . .
H12B H 0.2622 0.1578 0.0497 0.301 Uiso 1 1 calc R . .
C13 C 0.1390(7) 0.1009(12) 0.0005(13) 0.292(7) Uani 1 1 d U . .
H13A H 0.1388 0.1200 0.0675 0.351 Uiso 1 1 calc R . .
H13B H 0.1071 0.1557 -0.0487 0.351 Uiso 1 1 calc R . .
C14 C 0.1048(13) 0.0000 -0.028(2) 0.294(10) Uani 1 2 d SU . .
H14A H 0.0846 0.0000 -0.1026 0.353 Uiso 1 2 calc SR . .
H14B H 0.0562 0.0000 -0.0107 0.353 Uiso 1 2 calc SR . .
B1 B 0.6615(4) -0.5000 0.3971(6) 0.091(3) Uani 1 2 d SD . .
F1 F 0.6967(7) -0.5920(9) 0.4400(10) 0.171(5) Uani 0.50 1 d PDU A 1
F2 F 0.6552(17) -0.5000 0.3023(10) 0.220(10) Uani 0.50 2 d SPDU A 1
F3 F 0.5900(7) -0.5000 0.4027(18) 0.182(9) Uani 0.50 2 d SPDU A 1
F1' F 0.6815(11) -0.4210(14) 0.3507(14) 0.289(11) Uani 0.50 1 d PDU A 2
F2' F 0.5838(5) -0.5000 0.376(2) 0.203(11) Uani 0.50 2 d SPDU A 2
F3' F 0.7082(9) -0.5000 0.4932(9) 0.225(9) Uani 0.50 2 d SPDU A 2
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
N2 Fe1 N2 105.26(18) . 6 ?
N2 Fe1 N1 140.84(14) . 6 ?
N2 Fe1 N1 76.12(15) 6 6 ?
N2 Fe1 N1 76.12(15) . . ?
N2 Fe1 N1 140.84(14) 6 . ?
N1 Fe1 N1 79.4(2) 6 . ?
N2 Fe1 S1 107.75(10) . . ?
N2 Fe1 S1 107.75(10) 6 . ?
N1 Fe1 S1 108.88(11) 6 . ?
N1 Fe1 S1 108.88(11) . . ?
C11 S1 Fe1 100.9(4) . . ?
C5 N1 C3 110.5(4) . . ?
C5 N1 C1 107.7(4) . . ?
C3 N1 C1 111.8(4) . . ?
C5 N1 Fe1 103.6(3) . . ?
C3 N1 Fe1 110.5(3) . . ?
C1 N1 Fe1 112.4(3) . . ?
C6 N2 C10 117.1(4) . . ?
C6 N2 Fe1 114.1(3) . . ?
C10 N2 Fe1 128.8(3) . . ?
C2 C1 N1 114.4(5) . . ?
C1 C2 C1 114.7(7) . 6 ?
N1 C3 C4 112.3(4) . . ?
C3 C4 C3 118.7(6) 6 . ?
N1 C5 C6 110.4(4) . . ?
N2 C6 C7 122.0(5) . . ?
N2 C6 C5 115.2(5) . . ?
C7 C6 C5 122.8(5) . . ?
C6 C7 C8 120.4(6) . . ?
C9 C8 C7 118.4(6) . . ?
C8 C9 C10 118.9(6) . . ?
N2 C10 C9 123.1(5) . . ?
C12 C11 C12 121.3(12) 6 . ?
C12 C11 S1 112.6(7) 6 . ?
C12 C11 S1 112.6(7) . . ?
C11 C12 C13 112.5(11) . . ?
C14 C13 C12 109.2(15) . . ?
C13 C14 C13 129(2) . 6 ?
F1' B1 F1' 97(2) 6_545 . ?
F1' B1 F2' 110.7(10) 6_545 . ?
F1' B1 F2' 110.7(10) . . ?
F1' B1 F3 119.4(12) 6_545 . ?
F1' B1 F3 119.4(12) . . ?
F2' B1 F3 16(2) . . ?
F1' B1 F3' 110.2(10) 6_545 . ?
F1' B1 F3' 110.2(10) . . ?
F2' B1 F3' 116.2(13) . . ?
F3 B1 F3' 100.6(15) . . ?
F1' B1 F2 53.9(10) 6_545 . ?
F1' B1 F2 53.9(10) . . ?
F2' B1 F2 95.3(19) . . ?
F3 B1 F2 110.9(14) . . ?
F3' B1 F2 148.5(15) . . ?
F1' B1 F1 134.6(11) 6_545 6_545 ?
F1' B1 F1 54.6(9) . 6_545 ?
F2' B1 F1 112.5(8) . 6_545 ?
F3 B1 F1 105.8(7) . 6_545 ?
F3' B1 F1 61.0(7) . 6_545 ?
F2 B1 F1 108.4(8) . 6_545 ?
F1' B1 F1 54.6(9) 6_545 . ?
F1' B1 F1 134.6(11) . . ?
F2' B1 F1 112.5(8) . . ?
F3 B1 F1 105.8(7) . . ?
F3' B1 F1 61.0(7) . . ?
F2 B1 F1 108.4(8) . . ?
F1 B1 F1 117.4(15) 6_545 . ?
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 N2 2.189(4) . ?
Fe1 N2 2.189(4) 6 ?
Fe1 N1 2.228(4) 6 ?
Fe1 N1 2.228(4) . ?
Fe1 S1 2.259(2) . ?
S1 C11 1.847(10) . ?
N1 C5 1.463(7) . ?
N1 C3 1.496(5) . ?
N1 C1 1.500(6) . ?
N2 C6 1.332(6) . ?
N2 C10 1.344(5) . ?
C1 C2 1.499(7) . ?
C2 C1 1.499(7) 6 ?
C3 C4 1.517(6) . ?
C4 C3 1.517(6) 6 ?
C5 C6 1.504(7) . ?
C6 C7 1.354(8) . ?
C7 C8 1.370(9) . ?
C8 C9 1.350(8) . ?
C9 C10 1.367(6) . ?
C11 C12 1.383(10) 6 ?
C11 C12 1.383(10) . ?
C12 C13 1.594(15) . ?
C13 C14 1.358(16) . ?
C14 C13 1.358(16) 6 ?
B1 F1' 1.280(7) 6_545 ?
B1 F1' 1.280(7) . ?
B1 F2' 1.281(7) . ?
B1 F3 1.285(8) . ?
B1 F3' 1.287(8) . ?
B1 F2 1.292(8) . ?
B1 F1 1.309(6) 6_545 ?
B1 F1 1.309(6) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Fe1 S1 C11 56.56(10) . . . . ?
N2 Fe1 S1 C11 -56.56(10) 6 . . . ?
N1 Fe1 S1 C11 -137.54(13) 6 . . . ?
N1 Fe1 S1 C11 137.54(13) . . . . ?
N2 Fe1 N1 C5 34.4(3) . . . . ?
N2 Fe1 N1 C5 131.6(3) 6 . . . ?
N1 Fe1 N1 C5 -176.5(3) 6 . . . ?
S1 Fe1 N1 C5 -70.0(3) . . . . ?
N2 Fe1 N1 C3 -84.0(3) . . . . ?
N2 Fe1 N1 C3 13.2(5) 6 . . . ?
N1 Fe1 N1 C3 65.1(4) 6 . . . ?
S1 Fe1 N1 C3 171.6(3) . . . . ?
N2 Fe1 N1 C1 150.3(4) . . . . ?
N2 Fe1 N1 C1 -112.4(4) 6 . . . ?
N1 Fe1 N1 C1 -60.5(4) 6 . . . ?
S1 Fe1 N1 C1 46.0(4) . . . . ?
N2 Fe1 N2 C6 -155.9(3) 6 . . . ?
N1 Fe1 N2 C6 -69.3(4) 6 . . . ?
N1 Fe1 N2 C6 -16.4(3) . . . . ?
S1 Fe1 N2 C6 89.3(3) . . . . ?
N2 Fe1 N2 C10 22.1(5) 6 . . . ?
N1 Fe1 N2 C10 108.7(4) 6 . . . ?
N1 Fe1 N2 C10 161.6(4) . . . . ?
S1 Fe1 N2 C10 -92.7(4) . . . . ?
C5 N1 C1 C2 -175.9(5) . . . . ?
C3 N1 C1 C2 -54.4(7) . . . . ?
Fe1 N1 C1 C2 70.6(5) . . . . ?
N1 C1 C2 C1 -60.8(8) . . . 6 ?
C5 N1 C3 C4 -132.8(5) . . . . ?
C1 N1 C3 C4 107.3(5) . . . . ?
Fe1 N1 C3 C4 -18.7(5) . . . . ?
N1 C3 C4 C3 -58.3(8) . . . 6 ?
C3 N1 C5 C6 69.9(5) . . . . ?
C1 N1 C5 C6 -167.7(4) . . . . ?
Fe1 N1 C5 C6 -48.5(5) . . . . ?
C10 N2 C6 C7 -2.7(8) . . . . ?
Fe1 N2 C6 C7 175.5(5) . . . . ?
C10 N2 C6 C5 175.7(4) . . . . ?
Fe1 N2 C6 C5 -6.1(5) . . . . ?
N1 C5 C6 N2 38.7(6) . . . . ?
N1 C5 C6 C7 -142.9(6) . . . . ?
N2 C6 C7 C8 0.8(10) . . . . ?
C5 C6 C7 C8 -177.5(7) . . . . ?
C6 C7 C8 C9 1.8(11) . . . . ?
C7 C8 C9 C10 -2.3(10) . . . . ?
C6 N2 C10 C9 2.3(7) . . . . ?
Fe1 N2 C10 C9 -175.6(4) . . . . ?
C8 C9 C10 N2 0.3(9) . . . . ?
Fe1 S1 C11 C12 -109.2(10) . . . 6 ?
Fe1 S1 C11 C12 109.2(10) . . . . ?
C12 C11 C12 C13 45(2) 6 . . . ?
S1 C11 C12 C13 -177.2(9) . . . . ?
C11 C12 C13 C14 -36(2) . . . . ?
C12 C13 C14 C13 40(5) . . . 6 ?
