#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327447.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_4327447
loop_
_publ_author_name
'Irene P. Georgakaki'
'Matthew L. Miller'
'Marcetta Y. Darensbourg'
_publ_section_title
;
 Requirements for Functional Models of the Iron Hydrogenase Active Site:
 D2/H2O Exchange Activity in {(μ-SMe)(μ-pdt)[Fe(CO)2(PMe3)]2+}[BF4-]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2489
_journal_page_last               2494
_journal_paper_doi               10.1021/ic026005+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C14 H27 B F4 Fe2 O4 P2 S3'
_chemical_formula_weight         615.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.79(3)
_cell_length_b                   12.54(2)
_cell_length_c                   12.98(2)
_cell_measurement_temperature    110(2)
_cell_volume                     2407(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.2567
_diffrn_reflns_av_sigmaI/netI    0.3275
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14342
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.647
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_F_000             1256
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.2214
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(3.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0100P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                923
_reflns_number_total             2980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0260052Bsi20030106_092808.cif
_cod_data_source_block           igmb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Orthorhobic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2408(7)
_cod_database_code               4327447
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.24528(9) 0.12605(11) 0.30083(10) 0.0275(3) Uani 1 1 d U . .
S1 S 0.1661(2) 0.2500 0.2058(3) 0.0275(8) Uani 1 2 d S . .
S2 S 0.3609(2) 0.2500 0.2846(3) 0.0301(9) Uani 1 2 d S . .
S3 S 0.2020(2) 0.2500 0.4248(2) 0.0287(9) Uani 1 2 d S . .
P1 P 0.11936(17) 0.0254(2) 0.3140(2) 0.0320(7) Uani 1 1 d . . .
C1 C 0.3036(7) 0.0358(9) 0.3825(8) 0.038(3) Uani 1 1 d U . .
O1 O 0.3424(5) -0.0229(6) 0.4323(5) 0.045(2) Uani 1 1 d U . .
C2 C 0.2770(6) 0.0539(8) 0.1899(8) 0.033(2) Uani 1 1 d . . .
O2 O 0.2981(4) 0.0099(6) 0.1168(5) 0.044(2) Uani 1 1 d . . .
C3 C 0.2061(10) 0.2500 0.0721(8) 0.038(4) Uani 1 2 d S . .
H3A H 0.1720 0.3028 0.0323 0.057 Uiso 0.50 1 calc PR . .
H3B H 0.1970 0.1791 0.0420 0.057 Uiso 0.50 1 calc PR . .
H3C H 0.2705 0.2680 0.0705 0.057 Uiso 0.50 1 calc PR . .
C4 C 0.4235(10) 0.2500 0.4051(12) 0.063(5) Uani 1 2 d SD . 1
H4A H 0.4551 0.3168 0.4081 0.076 Uiso 0.50 1 d PR . 1
H4B H 0.4688 0.1955 0.3986 0.076 Uiso 0.50 1 d PR . 1
C5 C 0.3807(12) 0.227(4) 0.5033(13) 0.041(13) Uani 0.50 1 d PD . 1
H5A H 0.4131 0.2726 0.5500 0.050 Uiso 0.50 1 d PR . 1
H5B H 0.3948 0.1555 0.5233 0.050 Uiso 0.50 1 d PR . 1
C5' C 0.370(3) 0.297(4) 0.490(5) 0.000 Uiso 0.00 1 d PD A 2
C6 C 0.2849(10) 0.2500 0.5287(9) 0.049(5) Uani 1 2 d SD . 1
H6A H 0.2679 0.1948 0.5761 0.059 Uiso 0.50 1 d PR . 1
H6B H 0.2791 0.3165 0.5646 0.059 Uiso 0.50 1 d PR . 1
C7 C 0.0295(7) 0.0848(8) 0.3851(8) 0.053(3) Uani 1 1 d . . .
H7A H -0.0223 0.0361 0.3867 0.079 Uiso 1 1 calc R . .
H7B H 0.0116 0.1518 0.3520 0.079 Uiso 1 1 calc R . .
H7C H 0.0497 0.0993 0.4556 0.079 Uiso 1 1 calc R . .
C8 C 0.0689(8) -0.0057(8) 0.1890(8) 0.054(3) Uani 1 1 d . . .
H8A H 0.0146 -0.0492 0.1992 0.081 Uiso 1 1 calc R . .
H8B H 0.1125 -0.0452 0.1469 0.081 Uiso 1 1 calc R . .
H8C H 0.0525 0.0607 0.1538 0.081 Uiso 1 1 calc R . .
C9 C 0.1356(8) -0.1048(8) 0.3691(9) 0.056(3) Uani 1 1 d . . .
H9A H 0.0775 -0.1424 0.3716 0.084 Uiso 1 1 calc R . .
H9B H 0.1597 -0.0976 0.4391 0.084 Uiso 1 1 calc R . .
H9C H 0.1783 -0.1453 0.3267 0.084 Uiso 1 1 calc R . .
B1 B -0.1100(11) -0.2500 0.2504(13) 0.059(4) Uani 0.71(5) 2 d SPD . 1
F1 F -0.0641(14) -0.2500 0.1566(14) 0.059(4) Uani 0.71(5) 2 d SPD . 1
F2 F -0.0713(12) -0.1745(18) 0.3156(16) 0.059(4) Uani 0.36(3) 1 d PD . 1
F3 F -0.1991(12) -0.2214(18) 0.2313(14) 0.059(4) Uani 0.36(3) 1 d PD . 1
F4 F -0.1055(15) -0.3491(13) 0.2962(16) 0.059(4) Uani 0.36(3) 1 d PD . 1
B1' B -0.113(4) -0.2500 0.255(5) 0.041(9) Uani 0.29(5) 2 d SP . 2
F1' F -0.032(3) -0.2500 0.185(3) 0.041(9) Uani 0.29(5) 2 d SP . 2
F2' F -0.069(3) -0.200(4) 0.345(4) 0.041(9) Uani 0.14(3) 1 d P . 2
F3' F -0.184(3) -0.188(5) 0.238(4) 0.041(9) Uani 0.14(3) 1 d P . 2
F4' F -0.135(3) -0.352(4) 0.260(4) 0.041(9) Uani 0.14(3) 1 d P . 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'
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 '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
C2 Fe1 C1 91.8(5) . .
C2 Fe1 P1 89.7(3) . .
C1 Fe1 P1 89.9(4) . .
C2 Fe1 S1 92.5(3) . .
C1 Fe1 S1 175.7(4) . .
P1 Fe1 S1 89.94(16) . .
C2 Fe1 S2 94.2(3) . .
C1 Fe1 S2 97.1(4) . .
P1 Fe1 S2 171.84(11) . .
S1 Fe1 S2 82.74(15) . .
C2 Fe1 S3 168.6(3) . .
C1 Fe1 S3 98.5(4) . .
P1 Fe1 S3 95.43(14) . .
S1 Fe1 S3 77.27(16) . .
S2 Fe1 S3 79.50(14) . .
C3 S1 Fe1 110.1(3) . 7_565
C3 S1 Fe1 110.1(3) . .
Fe1 S1 Fe1 84.87(18) 7_565 .
C4 S2 Fe1 107.3(4) . .
C4 S2 Fe1 107.3(4) . 7_565
Fe1 S2 Fe1 84.12(19) . 7_565
C6 S3 Fe1 109.1(4) . 7_565
C6 S3 Fe1 109.1(4) . .
Fe1 S3 Fe1 83.85(18) 7_565 .
C7 P1 C9 105.9(5) . .
C7 P1 C8 104.1(6) . .
C9 P1 C8 102.3(5) . .
C7 P1 Fe1 114.9(4) . .
C9 P1 Fe1 115.4(4) . .
C8 P1 Fe1 112.9(4) . .
O1 C1 Fe1 178.0(10) . .
O2 C2 Fe1 178.1(9) . .
C5 C4 C5 23(4) . 7_565
C5 C4 S2 122.2(11) . .
C5 C4 S2 122.2(11) 7_565 .
C5 C5 C4 78.6(18) 7_565 .
C5 C5 C6 78.9(17) 7_565 .
C4 C5 C6 125.0(19) . .
C5 C6 C5 22(3) 7_565 .
C5 C6 S3 118.6(11) 7_565 .
C5 C6 S3 118.6(11) . .
F4 B1 F4 129(2) 7 .
F4 B1 F3 110.8(11) 7 7
F4 B1 F3 83.7(17) . 7
F4 B1 F3 83.7(17) 7 .
F4 B1 F3 110.8(11) . .
F3 B1 F3 29.9(19) 7 .
F4 B1 F2 26.6(19) 7 .
F4 B1 F2 109.4(12) . .
F3 B1 F2 132.4(15) 7 .
F3 B1 F2 108.9(10) . .
F4 B1 F2 109.4(12) 7 7
F4 B1 F2 26.6(19) . 7
F3 B1 F2 108.9(10) 7 7
F3 B1 F2 132.4(15) . 7
F2 B1 F2 86(2) . 7
F4 B1 F1 110.7(10) 7 .
F4 B1 F1 110.7(10) . .
F3 B1 F1 107.8(12) 7 .
F3 B1 F1 107.8(12) . .
F2 B1 F1 109.3(11) . .
F2 B1 F1 109.3(11) 7 .
F4 F2 B1 75.5(14) 7 .
F3 F3 B1 75.0(9) 7 .
F2 F4 B1 77.8(19) 7 .
F4' B1' F4' 151(6) 7 .
F4' B1' F3' 112(6) 7 7
F4' B1' F3' 42(4) . 7
F4' B1' F3' 42(4) 7 .
F4' B1' F3' 112(6) . .
F3' B1' F3' 71(6) 7 .
F4' B1' F2' 70(4) 7 .
F4' B1' F2' 118(5) . .
F3' B1' F2' 137(5) 7 .
F3' B1' F2' 104(3) . .
F4' B1' F2' 118(5) 7 7
F4' B1' F2' 70(4) . 7
F3' B1' F2' 104(3) 7 7
F3' B1' F2' 137(5) . 7
F2' B1' F2' 50(5) . 7
F4' B1' F1' 103(3) 7 .
F4' B1' F1' 103(3) . .
F3' B1' F1' 122(4) 7 .
F3' B1' F1' 122(4) . .
F2' B1' F1' 97(4) . .
F2' B1' F1' 97(4) 7 .
F2' F2' B1' 65(2) 7 .
F2' F2' F4' 114(2) 7 7
B1' F2' F4' 51(3) . 7
F4' F3' B1' 69(4) 7 .
F4' F3' F3' 123(4) 7 7
B1' F3' F3' 54(3) . 7
F3' F4' B1' 69(5) 7 .
F3' F4' F2' 118(5) 7 7
B1' F4' F2' 60(4) . 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C2 1.764(10) .
Fe1 C1 1.774(11) .
Fe1 P1 2.257(4) .
Fe1 S1 2.304(4) .
Fe1 S2 2.321(4) .
Fe1 S3 2.327(4) .
S1 C3 1.833(12) .
S1 Fe1 2.304(4) 7_565
S2 C4 1.818(16) .
S2 Fe1 2.321(4) 7_565
S3 C6 1.822(13) .
S3 Fe1 2.327(4) 7_565
P1 C7 1.782(10) .
P1 C9 1.799(10) .
P1 C8 1.829(10) .
C1 O1 1.136(11) .
C2 O2 1.142(10) .
C4 C5 1.45(2) .
C4 C5 1.45(2) 7_565
C5 C5 0.57(9) 7_565
C5 C6 1.48(2) .
C6 C5 1.48(2) 7_565
B1 F4 1.379(13) 7
B1 F4 1.379(13) .
B1 F3 1.389(16) 7
B1 F3 1.389(16) .
B1 F2 1.392(15) .
B1 F2 1.392(15) 7
B1 F1 1.394(15) .
F2 F4 0.64(4) 7
F3 F3 0.72(4) 7
F4 F2 0.64(4) 7
B1' F4' 1.33(5) 7
B1' F4' 1.33(5) .
B1' F3' 1.33(6) 7
B1' F3' 1.33(6) .
B1' F2' 1.48(7) .
B1' F2' 1.48(7) 7
B1' F1' 1.50(7) .
F2' F2' 1.25(10) 7
F2' F4' 1.61(9) 7
F3' F4' 0.94(8) 7
F3' F3' 1.55(12) 7
F4' F3' 0.94(8) 7
F4' F2' 1.61(9) 7
