#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302130.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_4302130
loop_
_publ_author_name
'C. Matthew Whaley'
'Thomas B. Rauchfuss'
'Scott R. Wilson'
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
Coordination Chemistry of [HFe(CN)2(CO)3]- and Its Derivatives: Toward a
Model for the Iron Subsite of the [NiFe]-Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4462
_journal_page_last               4469
_journal_paper_doi               10.1021/ic900200s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C31 H25 Fe N3 O P2'
_chemical_formula_sum            'C31 H25 Fe N3 O P2'
_chemical_formula_weight         573.33
_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
_audit_update_record
; 
2008-02-22   text and data added, cmw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.145(6)
_cell_length_b                   21.090(8)
_cell_length_c                   8.026(3)
_cell_measurement_reflns_used    4266
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.54
_cell_volume                     2732.8(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga94sfas4
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7844
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9117
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_crystal_id                ga94sfas4
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-3 3 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0444
_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)+(0.0801P)²+0.6366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                2039
_reflns_number_total             2738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900200s_si_002_1.cif
_cod_data_source_block           ga94sfas4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_original_cell_volume        2732.9(17)
_cod_original_sg_symbol_Hall     '-P 2ac 2n '
_cod_original_sg_symbol_H-M      'P n m a '
_cod_database_code               4302130
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 0.15412(3) 0.2500 0.19220(7) 0.02206(18) Uani 1 2 d S . .
C1 C 0.00037(18) 0.28158(13) 0.4514(3) 0.0287(6) Uani 1 1 d . . .
H1 H -0.0347 0.3046 0.5246 0.034 Uiso 1 1 calc R . .
C2 C 0.0985(3) 0.2500 0.0052(5) 0.0281(9) Uani 1 2 d S . .
C3 C 0.22463(18) 0.31450(14) 0.0950(3) 0.0285(6) Uani 1 1 d . . .
C4 C 0.2691(3) 0.2500 0.5046(5) 0.0328(10) Uani 1 2 d S . .
C5 C 0.3230(4) 0.2500 0.6517(6) 0.0519(14) Uani 1 2 d S . .
H5A H 0.3784 0.2387 0.6188 0.078 Uiso 0.50 1 d PR . .
H5B H 0.3028 0.2198 0.7316 0.078 Uiso 0.50 1 d PR . .
H5C H 0.3234 0.2916 0.7008 0.078 Uiso 0.50 1 d PR . .
C6 C -0.00020(18) 0.36246(13) 0.1625(3) 0.0263(6) Uani 1 1 d . . .
C7 C -0.08534(19) 0.36427(15) 0.1881(4) 0.0322(7) Uani 1 1 d . . .
H7 H -0.1084 0.3453 0.2850 0.039 Uiso 1 1 calc R . .
C8 C -0.1368(2) 0.39358(16) 0.0730(4) 0.0394(8) Uani 1 1 d . . .
H8 H -0.1949 0.3947 0.0913 0.047 Uiso 1 1 calc R . .
C9 C -0.1035(2) 0.42121(15) -0.0685(4) 0.0410(8) Uani 1 1 d . . .
H9 H -0.1390 0.4408 -0.1476 0.049 Uiso 1 1 calc R . .
C10 C -0.0188(2) 0.42043(16) -0.0951(4) 0.0410(8) Uani 1 1 d . . .
H10 H 0.0040 0.4400 -0.1914 0.049 Uiso 1 1 calc R . .
C11 C 0.0327(2) 0.39083(15) 0.0202(4) 0.0339(7) Uani 1 1 d . . .
H11 H 0.0908 0.3900 0.0018 0.041 Uiso 1 1 calc R . .
C12 C 0.11145(17) 0.38636(13) 0.4365(3) 0.0252(6) Uani 1 1 d . . .
C13 C 0.14427(18) 0.37234(14) 0.5939(4) 0.0310(7) Uani 1 1 d . . .
H13 H 0.1418 0.3301 0.6347 0.037 Uiso 1 1 calc R . .
C14 C 0.1802(2) 0.41910(16) 0.6906(4) 0.0360(7) Uani 1 1 d . . .
H14 H 0.2028 0.4090 0.7965 0.043 Uiso 1 1 calc R . .
C15 C 0.1830(2) 0.48085(16) 0.6319(4) 0.0387(8) Uani 1 1 d . . .
H15 H 0.2080 0.5130 0.6976 0.046 Uiso 1 1 calc R . .
C16 C 0.1497(2) 0.49583(16) 0.4797(4) 0.0470(9) Uani 1 1 d . . .
H16 H 0.1507 0.5384 0.4411 0.056 Uiso 1 1 calc R . .
C17 C 0.1147(2) 0.44856(15) 0.3821(4) 0.0401(8) Uani 1 1 d . . .
H17 H 0.0925 0.4591 0.2761 0.048 Uiso 1 1 calc R . .
N1 N 0.26684(18) 0.35102(14) 0.0300(3) 0.0454(7) Uani 1 1 d . . .
N2 N 0.2256(2) 0.2500 0.3926(4) 0.0271(7) Uani 1 2 d S . .
O1 O 0.0654(2) 0.2500 -0.1224(4) 0.0427(8) Uani 1 2 d S . .
P1 P 0.06918(5) 0.32266(3) 0.30788(9) 0.0233(2) 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.0100
1.00 0.00 0.00 0.0100
0.00 1.00 0.00 0.0500
0.00 -1.00 0.00 0.0500
0.00 0.00 1.00 0.0700
0.00 0.00 -1.00 0.0900
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
C2 Fe1 C3 87.48(13) . 7_565 ?
C2 Fe1 C3 87.48(13) . . ?
C3 Fe1 C3 89.18(17) 7_565 . ?
C2 Fe1 N2 175.22(17) . . ?
C3 Fe1 N2 89.12(11) 7_565 . ?
C3 Fe1 N2 89.12(11) . . ?
C2 Fe1 P1 92.36(10) . . ?
C3 Fe1 P1 178.18(9) 7_565 . ?
C3 Fe1 P1 92.63(9) . . ?
N2 Fe1 P1 91.14(8) . . ?
C2 Fe1 P1 92.36(10) . 7_565 ?
C3 Fe1 P1 92.63(9) 7_565 7_565 ?
C3 Fe1 P1 178.18(9) . 7_565 ?
N2 Fe1 P1 91.14(8) . 7_565 ?
P1 Fe1 P1 85.56(5) . 7_565 ?
C1 C1 P1 118.43(9) 7_565 . ?
C1 C1 H1 120.8 7_565 . ?
P1 C1 H1 120.8 . . ?
O1 C2 Fe1 176.7(4) . . ?
N1 C3 Fe1 176.5(3) . . ?
N2 C4 C5 178.4(5) . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 119.1(3) . . ?
C7 C6 P1 121.7(2) . . ?
C11 C6 P1 119.2(2) . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 119.5(3) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C6 120.6(3) . . ?
C10 C11 H11 119.7 . . ?
C6 C11 H11 119.7 . . ?
C17 C12 C13 118.0(3) . . ?
C17 C12 P1 122.2(2) . . ?
C13 C12 P1 119.7(2) . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.8(3) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C12 C17 C16 121.2(3) . . ?
C12 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C4 N2 Fe1 177.6(3) . . ?
C1 P1 C6 104.44(14) . . ?
C1 P1 C12 102.75(13) . . ?
C6 P1 C12 104.64(13) . . ?
C1 P1 Fe1 107.94(10) . . ?
C6 P1 Fe1 115.02(9) . . ?
C12 P1 Fe1 120.33(10) . . ?
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 C2 1.748(4) . ?
Fe1 C3 1.938(3) 7_565 ?
Fe1 C3 1.938(3) . ?
Fe1 N2 1.980(4) . ?
Fe1 P1 2.2563(9) . ?
Fe1 P1 2.2564(9) 7_565 ?
C1 C1 1.332(6) 7_565 ?
C1 P1 1.820(3) . ?
C1 H1 0.9500 . ?
C2 O1 1.156(5) . ?
C3 N1 1.153(4) . ?
C4 N2 1.141(5) . ?
C4 C5 1.466(6) . ?
C5 H5A 0.9622 . ?
C5 H5B 0.9619 . ?
C5 H5C 0.9619 . ?
C6 C7 1.390(4) . ?
C6 C11 1.394(4) . ?
C6 P1 1.822(3) . ?
C7 C8 1.388(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C17 1.383(4) . ?
C12 C13 1.401(4) . ?
C12 P1 1.826(3) . ?
C13 C14 1.382(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
