#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316436.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_4316436
loop_
_publ_author_name
'Jheng-Hong Wang'
'Chien-Hong Chen'
_publ_section_title
;
 New Members of the {Fe(NO)2}10 Dinitrosyliron Complexes Bound with
 [Thiolate, Thiolate] and [Amide, Amide] Ligations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7644
_journal_page_last               7646
_journal_paper_doi               10.1021/ic101126v
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C38 H28 Fe N4 O4 P S2'
_chemical_formula_weight         755.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   15.5535(8)
_cell_length_b                   16.8415(8)
_cell_length_c                   26.5880(12)
_cell_measurement_reflns_used    3590
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.64
_cell_measurement_theta_min      2.42
_cell_volume                     6964.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34619
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.8551
_exptl_absorpt_correction_T_min  0.7821
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0506
_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)+(0.0503P)²+2.1745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                5818
_reflns_number_total             7993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101126v_si_004_3.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4316436
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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
Fe Fe 0.23780(2) 0.11986(2) 0.411750(14) 0.02551(11) Uani 1 1 d . . .
S1 S 0.25724(4) -0.14921(4) 0.42446(3) 0.03081(17) Uani 1 1 d . . .
S2 S 0.28327(6) 0.18568(5) 0.24772(3) 0.0468(2) Uani 1 1 d . . .
N1 N 0.31158(14) 0.15014(13) 0.45400(8) 0.0283(5) Uani 1 1 d . . .
N2 N 0.14346(15) 0.16764(14) 0.41993(9) 0.0358(6) Uani 1 1 d . . .
N3 N 0.22391(13) 0.00229(12) 0.41350(8) 0.0249(5) Uani 1 1 d . . .
N4 N 0.27827(14) 0.13763(12) 0.34148(8) 0.0287(5) Uani 1 1 d . . .
O1 O 0.34648(13) 0.18445(13) 0.48678(7) 0.0418(5) Uani 1 1 d . . .
O2 O 0.08920(14) 0.21098(13) 0.43340(10) 0.0569(7) Uani 1 1 d . . .
O3 O 0.33425(12) -0.02791(11) 0.46886(7) 0.0334(4) Uani 1 1 d . . .
O4 O 0.14853(14) 0.18358(13) 0.30977(8) 0.0476(6) Uani 1 1 d . . .
C1 C 0.27927(16) -0.04531(15) 0.43918(9) 0.0232(5) Uani 1 1 d . . .
C2 C 0.17797(16) -0.12183(15) 0.38156(10) 0.0273(6) Uani 1 1 d . . .
C3 C 0.13213(17) -0.16976(17) 0.34907(11) 0.0353(7) Uani 1 1 d . . .
H3 H 0.1395 -0.2257 0.3496 0.042 Uiso 1 1 calc R . .
C4 C 0.07550(18) -0.13498(18) 0.31594(12) 0.0400(7) Uani 1 1 d . . .
H4 H 0.0454 -0.1670 0.2924 0.048 Uiso 1 1 calc R . .
C5 C 0.06207(17) -0.05338(18) 0.31666(11) 0.0362(7) Uani 1 1 d . . .
H5 H 0.0209 -0.0306 0.2946 0.043 Uiso 1 1 calc R . .
C6 C 0.10778(17) -0.00485(16) 0.34908(11) 0.0312(6) Uani 1 1 d . . .
H6 H 0.0983 0.0509 0.3493 0.037 Uiso 1 1 calc R . .
C7 C 0.16796(15) -0.03894(15) 0.38142(9) 0.0241(5) Uani 1 1 d . . .
C8 C 0.2251(2) 0.16870(17) 0.30564(11) 0.0375(7) Uani 1 1 d . . .
C9 C 0.3778(2) 0.14905(17) 0.27439(11) 0.0369(7) Uani 1 1 d . . .
C10 C 0.4594(2) 0.14267(19) 0.25330(12) 0.0476(8) Uani 1 1 d . . .
H10 H 0.4696 0.1597 0.2198 0.057 Uiso 1 1 calc R . .
C11 C 0.5246(2) 0.1117(2) 0.28145(12) 0.0497(9) Uani 1 1 d . . .
H11 H 0.5807 0.1077 0.2676 0.060 Uiso 1 1 calc R . .
C12 C 0.5094(2) 0.08565(19) 0.33046(12) 0.0461(8) Uani 1 1 d . . .
H12 H 0.5550 0.0627 0.3493 0.055 Uiso 1 1 calc R . .
C13 C 0.42910(18) 0.09284(17) 0.35202(11) 0.0346(6) Uani 1 1 d . . .
H13 H 0.4197 0.0758 0.3856 0.041 Uiso 1 1 calc R . .
C14 C 0.36230(18) 0.12505(15) 0.32427(10) 0.0301(6) Uani 1 1 d . . .
P1 P 0.21012(4) 0.09910(4) 0.61949(2) 0.02353(15) Uani 1 1 d . . .
C15 C 0.32441(16) 0.10020(15) 0.61015(9) 0.0246(5) Uani 1 1 d . . .
C16 C 0.36278(17) 0.05558(16) 0.57274(10) 0.0289(6) Uani 1 1 d . . .
H16 H 0.3293 0.0209 0.5525 0.035 Uiso 1 1 calc R . .
C17 C 0.45078(18) 0.06197(17) 0.56496(11) 0.0345(7) Uani 1 1 d . . .
H17 H 0.4776 0.0309 0.5396 0.041 Uiso 1 1 calc R . .
C18 C 0.49953(18) 0.11291(17) 0.59368(11) 0.0372(7) Uani 1 1 d . . .
H18 H 0.5596 0.1173 0.5877 0.045 Uiso 1 1 calc R . .
C19 C 0.46139(18) 0.15768(18) 0.63119(11) 0.0385(7) Uani 1 1 d . . .
H19 H 0.4951 0.1930 0.6509 0.046 Uiso 1 1 calc R . .
C20 C 0.37399(18) 0.15093(17) 0.63997(11) 0.0337(6) Uani 1 1 d . . .
H20 H 0.3478 0.1807 0.6662 0.040 Uiso 1 1 calc R . .
C21 C 0.16218(17) 0.18434(16) 0.59025(9) 0.0281(6) Uani 1 1 d . . .
C22 C 0.2118(2) 0.24857(17) 0.57478(11) 0.0365(7) Uani 1 1 d . . .
H22 H 0.2724 0.2477 0.5790 0.044 Uiso 1 1 calc R . .
C23 C 0.1720(2) 0.31402(19) 0.55310(11) 0.0475(8) Uani 1 1 d . . .
H23 H 0.2056 0.3580 0.5423 0.057 Uiso 1 1 calc R . .
C24 C 0.0841(2) 0.3152(2) 0.54724(11) 0.0521(9) Uani 1 1 d . . .
H24 H 0.0572 0.3600 0.5323 0.063 Uiso 1 1 calc R . .
C25 C 0.0347(2) 0.2517(2) 0.56294(12) 0.0499(9) Uani 1 1 d . . .
H25 H -0.0260 0.2533 0.5590 0.060 Uiso 1 1 calc R . .
C26 C 0.07297(19) 0.18566(19) 0.58429(10) 0.0381(7) Uani 1 1 d . . .
H26 H 0.0390 0.1418 0.5948 0.046 Uiso 1 1 calc R . .
C27 C 0.19172(16) 0.10053(15) 0.68560(9) 0.0256(6) Uani 1 1 d . . .
C28 C 0.13755(17) 0.15621(16) 0.70761(10) 0.0298(6) Uani 1 1 d . . .
H28 H 0.1108 0.1958 0.6875 0.036 Uiso 1 1 calc R . .
C29 C 0.12272(19) 0.1537(2) 0.75883(11) 0.0406(7) Uani 1 1 d . . .
H29 H 0.0856 0.1916 0.7740 0.049 Uiso 1 1 calc R . .
C30 C 0.1617(2) 0.0963(2) 0.78803(11) 0.0422(8) Uani 1 1 d . . .
H30 H 0.1501 0.0941 0.8231 0.051 Uiso 1 1 calc R . .
C31 C 0.21723(19) 0.04259(19) 0.76685(11) 0.0387(7) Uani 1 1 d . . .
H31 H 0.2449 0.0043 0.7874 0.046 Uiso 1 1 calc R . .
C32 C 0.23302(18) 0.04387(17) 0.71591(10) 0.0335(6) Uani 1 1 d . . .
H32 H 0.2716 0.0067 0.7013 0.040 Uiso 1 1 calc R . .
C33 C 0.16164(16) 0.01260(15) 0.59176(9) 0.0256(6) Uani 1 1 d . . .
C34 C 0.13469(19) -0.05123(17) 0.62108(11) 0.0372(7) Uani 1 1 d . . .
H34 H 0.1424 -0.0503 0.6565 0.045 Uiso 1 1 calc R . .
C35 C 0.0965(2) -0.11617(19) 0.59811(13) 0.0466(8) Uani 1 1 d . . .
H35 H 0.0787 -0.1601 0.6179 0.056 Uiso 1 1 calc R . .
C36 C 0.08406(19) -0.1176(2) 0.54696(13) 0.0465(8) Uani 1 1 d . . .
H36 H 0.0579 -0.1625 0.5316 0.056 Uiso 1 1 calc R . .
C37 C 0.10958(18) -0.0541(2) 0.51778(11) 0.0414(8) Uani 1 1 d . . .
H37 H 0.1005 -0.0551 0.4825 0.050 Uiso 1 1 calc R . .
C38 C 0.14832(17) 0.01102(18) 0.53977(10) 0.0337(6) Uani 1 1 d . . .
H38 H 0.1659 0.0547 0.5196 0.040 Uiso 1 1 calc R . .
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'
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
N1 Fe N2 111.23(11) . . ?
N1 Fe N3 111.04(10) . . ?
N2 Fe N3 112.12(10) . . ?
N1 Fe N4 111.36(10) . . ?
N2 Fe N4 108.88(11) . . ?
N3 Fe N4 101.84(9) . . ?
C2 S1 C1 91.12(12) . . ?
C9 S2 C8 91.11(14) . . ?
O1 N1 Fe 162.8(2) . . ?
O2 N2 Fe 164.3(2) . . ?
C1 N3 C7 114.0(2) . . ?
C1 N3 Fe 121.92(17) . . ?
C7 N3 Fe 123.04(16) . . ?
C8 N4 C14 113.3(2) . . ?
C8 N4 Fe 121.3(2) . . ?
C14 N4 Fe 125.30(18) . . ?
O3 C1 N3 129.6(2) . . ?
O3 C1 S1 120.58(19) . . ?
N3 C1 S1 109.78(18) . . ?
C3 C2 C7 121.5(3) . . ?
C3 C2 S1 128.4(2) . . ?
C7 C2 S1 110.07(19) . . ?
C4 C3 C2 118.8(3) . . ?
C3 C4 C5 120.5(3) . . ?
C6 C5 C4 121.0(3) . . ?
C5 C6 C7 119.1(3) . . ?
C6 C7 N3 126.0(2) . . ?
C6 C7 C2 119.0(2) . . ?
N3 C7 C2 114.9(2) . . ?
O4 C8 N4 127.3(3) . . ?
O4 C8 S2 122.1(2) . . ?
N4 C8 S2 110.6(2) . . ?
C10 C9 C14 120.9(3) . . ?
C10 C9 S2 129.2(2) . . ?
C14 C9 S2 109.9(2) . . ?
C11 C10 C9 119.1(3) . . ?
C10 C11 C12 120.4(3) . . ?
C13 C12 C11 120.9(3) . . ?
C12 C13 C14 119.5(3) . . ?
C13 C14 N4 125.8(2) . . ?
C13 C14 C9 119.1(3) . . ?
N4 C14 C9 115.1(3) . . ?
C27 P1 C21 110.49(12) . . ?
C27 P1 C15 107.19(12) . . ?
C21 P1 C15 110.07(12) . . ?
C27 P1 C33 110.38(12) . . ?
C21 P1 C33 107.22(13) . . ?
C15 P1 C33 111.52(12) . . ?
C16 C15 C20 120.2(2) . . ?
C16 C15 P1 121.4(2) . . ?
C20 C15 P1 118.3(2) . . ?
C15 C16 C17 119.4(3) . . ?
C18 C17 C16 120.6(3) . . ?
C17 C18 C19 120.2(3) . . ?
C18 C19 C20 119.9(3) . . ?
C19 C20 C15 119.8(3) . . ?
C22 C21 C26 120.3(3) . . ?
C22 C21 P1 121.3(2) . . ?
C26 C21 P1 118.3(2) . . ?
C23 C22 C21 119.6(3) . . ?
C24 C23 C22 120.0(3) . . ?
C23 C24 C25 120.5(3) . . ?
C24 C25 C26 120.4(3) . . ?
C25 C26 C21 119.2(3) . . ?
C28 C27 C32 119.6(2) . . ?
C28 C27 P1 121.5(2) . . ?
C32 C27 P1 118.9(2) . . ?
C29 C28 C27 119.7(3) . . ?
C30 C29 C28 120.1(3) . . ?
C31 C30 C29 120.5(3) . . ?
C30 C31 C32 120.4(3) . . ?
C31 C32 C27 119.6(3) . . ?
C34 C33 C38 119.6(3) . . ?
C34 C33 P1 121.5(2) . . ?
C38 C33 P1 118.9(2) . . ?
C35 C34 C33 119.4(3) . . ?
C36 C35 C34 120.7(3) . . ?
C35 C36 C37 120.2(3) . . ?
C36 C37 C38 120.2(3) . . ?
C37 C38 C33 119.9(3) . . ?
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
Fe N1 1.685(2) . ?
Fe N2 1.688(2) . ?
Fe N3 1.992(2) . ?
Fe N4 1.994(2) . ?
S1 C2 1.742(3) . ?
S1 C1 1.826(3) . ?
S2 C9 1.744(3) . ?
S2 C8 1.809(3) . ?
N1 O1 1.178(3) . ?
N2 O2 1.172(3) . ?
N3 C1 1.360(3) . ?
N3 C7 1.402(3) . ?
N4 C8 1.366(4) . ?
N4 C14 1.401(4) . ?
O3 C1 1.200(3) . ?
O4 C8 1.222(4) . ?
C2 C3 1.381(4) . ?
C2 C7 1.405(3) . ?
C3 C4 1.376(4) . ?
C4 C5 1.390(4) . ?
C5 C6 1.384(4) . ?
C6 C7 1.395(4) . ?
C9 C10 1.392(4) . ?
C9 C14 1.407(4) . ?
C10 C11 1.364(5) . ?
C11 C12 1.395(4) . ?
C12 C13 1.379(4) . ?
C13 C14 1.385(4) . ?
P1 C27 1.781(3) . ?
P1 C21 1.795(3) . ?
P1 C15 1.795(3) . ?
P1 C33 1.799(3) . ?
C15 C16 1.382(4) . ?
C15 C20 1.398(4) . ?
C16 C17 1.388(4) . ?
C17 C18 1.376(4) . ?
C18 C19 1.384(4) . ?
C19 C20 1.384(4) . ?
C21 C22 1.391(4) . ?
C21 C26 1.397(4) . ?
C22 C23 1.389(4) . ?
C23 C24 1.376(5) . ?
C24 C25 1.382(5) . ?
C25 C26 1.383(4) . ?
C27 C28 1.390(4) . ?
C27 C32 1.404(4) . ?
C28 C29 1.382(4) . ?
C29 C30 1.380(5) . ?
C30 C31 1.372(4) . ?
C31 C32 1.377(4) . ?
C33 C34 1.393(4) . ?
C33 C38 1.398(4) . ?
C34 C35 1.387(4) . ?
C35 C36 1.374(5) . ?
C36 C37 1.380(5) . ?
C37 C38 1.381(4) . ?
