#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:38:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179120 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308219.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_4308219
loop_
_publ_author_name
'Ming-Li Tsai'
'Chung-Hung Hsieh'
'Wen-Feng Liaw'
_publ_section_title
;
Dinitrosyl Iron Complexes (DNICs) Containing S/N/O Ligation:
Transformation of Roussin's Red Ester into the Neutral {Fe(NO)2}10DNICs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5110
_journal_page_last               5117
_journal_paper_doi               10.1021/ic0702567
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C43 H34 Fe N3 O4 P2 S'
_chemical_formula_weight         806.58
_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                 101.753(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2711(5)
_cell_length_b                   21.5461(10)
_cell_length_c                   19.6333(10)
_cell_measurement_reflns_used    4842
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.28
_cell_volume                     3839.6(3)
_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(1)
_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       '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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38077
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.8932
_exptl_absorpt_correction_T_min  0.8596
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0551
_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)+(0.0465P)²+2.0057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                7381
_reflns_number_total             8811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0702567-file003.cif
_cod_data_source_block           ic11480
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4308219
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
Fe Fe 0.63370(4) 0.162962(18) 0.17338(2) 0.02702(11) Uani 1 1 d . . .
S1 S 0.57480(8) 0.11117(4) 0.07116(4) 0.03413(18) Uani 1 1 d . . .
O1 O 0.8610(3) 0.09559(12) 0.26013(13) 0.0538(6) Uani 1 1 d . . .
O2 O 0.4256(3) 0.15602(11) 0.25894(12) 0.0483(6) Uani 1 1 d . . .
O3 O 0.6788(2) 0.24077(9) 0.13338(10) 0.0361(5) Uani 1 1 d . . .
O4 O 0.7545(3) 0.29264(9) 0.05036(11) 0.0425(6) Uani 1 1 d . . .
N1 N 0.7795(3) 0.12703(11) 0.22197(12) 0.0309(5) Uani 1 1 d . . .
N2 N 0.4919(3) 0.16683(12) 0.21546(13) 0.0354(6) Uani 1 1 d . . .
C1 C 0.7486(3) 0.12739(12) 0.05114(14) 0.0260(6) Uani 1 1 d . . .
C2 C 0.8247(4) 0.07926(13) 0.02595(15) 0.0341(7) Uani 1 1 d . . .
H2A H 0.7812 0.0392 0.0197 0.041 Uiso 1 1 calc R . .
C3 C 0.9602(4) 0.08843(14) 0.01011(16) 0.0383(7) Uani 1 1 d . . .
H3A H 1.0093 0.0548 -0.0067 0.046 Uiso 1 1 calc R . .
C4 C 1.0257(3) 0.14600(15) 0.01835(15) 0.0354(7) Uani 1 1 d . . .
H4A H 1.1208 0.1520 0.0084 0.042 Uiso 1 1 calc R . .
C5 C 0.9520(3) 0.19481(13) 0.04125(14) 0.0310(6) Uani 1 1 d . . .
H5A H 0.9959 0.2348 0.0454 0.037 Uiso 1 1 calc R . .
C6 C 0.8147(3) 0.18685(12) 0.05839(13) 0.0252(6) Uani 1 1 d . . .
C7 C 0.7442(3) 0.24441(12) 0.08126(14) 0.0280(6) Uani 1 1 d . . .
P1 P 0.26319(7) 0.41557(3) 0.12091(3) 0.01806(14) Uani 1 1 d . . .
P2 P 0.39178(7) 0.37710(3) 0.26373(3) 0.01759(14) Uani 1 1 d . . .
N3 N 0.3785(2) 0.38507(10) 0.18255(11) 0.0215(4) Uani 1 1 d . . .
C8 C 0.3372(3) 0.48456(11) 0.09019(13) 0.0207(5) Uani 1 1 d . . .
C9 C 0.4881(3) 0.49415(13) 0.10512(14) 0.0274(6) Uani 1 1 d . . .
H9A H 0.5515 0.4646 0.1319 0.033 Uiso 1 1 calc R . .
C10 C 0.5462(4) 0.54679(14) 0.08093(16) 0.0369(7) Uani 1 1 d . . .
H10A H 0.6497 0.5534 0.0909 0.044 Uiso 1 1 calc R . .
C11 C 0.4537(4) 0.59003(14) 0.04208(15) 0.0398(8) Uani 1 1 d . . .
H11A H 0.4939 0.6265 0.0262 0.048 Uiso 1 1 calc R . .
C12 C 0.3050(4) 0.58041(14) 0.02648(16) 0.0392(7) Uani 1 1 d . . .
H12A H 0.2422 0.6101 -0.0005 0.047 Uiso 1 1 calc R . .
C13 C 0.2461(3) 0.52792(13) 0.04978(16) 0.0341(7) Uani 1 1 d . . .
H13A H 0.1427 0.5212 0.0383 0.041 Uiso 1 1 calc R . .
C14 C 0.0903(3) 0.43643(12) 0.14245(13) 0.0213(5) Uani 1 1 d . . .
C15 C 0.0768(3) 0.49354(13) 0.17474(15) 0.0309(6) Uani 1 1 d . . .
H15A H 0.1521 0.5240 0.1782 0.037 Uiso 1 1 calc R . .
C16 C -0.0476(3) 0.50513(15) 0.20162(16) 0.0383(8) Uani 1 1 d . . .
H16A H -0.0578 0.5437 0.2235 0.046 Uiso 1 1 calc R . .
C17 C -0.1571(3) 0.46083(15) 0.19676(15) 0.0364(7) Uani 1 1 d . . .
H17A H -0.2399 0.4684 0.2173 0.044 Uiso 1 1 calc R . .
C18 C -0.1470(3) 0.40592(14) 0.16250(14) 0.0308(6) Uani 1 1 d . . .
H18A H -0.2250 0.3766 0.1573 0.037 Uiso 1 1 calc R . .
C19 C -0.0234(3) 0.39333(12) 0.13550(13) 0.0237(5) Uani 1 1 d . . .
H19A H -0.0162 0.3552 0.1122 0.028 Uiso 1 1 calc R . .
C20 C 0.2305(3) 0.36092(11) 0.05034(13) 0.0210(5) Uani 1 1 d . . .
C21 C 0.1228(3) 0.37283(13) -0.00868(14) 0.0277(6) Uani 1 1 d . . .
H21A H 0.0625 0.4087 -0.0107 0.033 Uiso 1 1 calc R . .
C22 C 0.1035(3) 0.33214(15) -0.06468(15) 0.0364(7) Uani 1 1 d . . .
H22A H 0.0297 0.3400 -0.1050 0.044 Uiso 1 1 calc R . .
C23 C 0.1918(3) 0.28048(14) -0.06152(16) 0.0354(7) Uani 1 1 d . . .
H23A H 0.1784 0.2527 -0.0999 0.042 Uiso 1 1 calc R . .
C24 C 0.2990(3) 0.26857(13) -0.00363(16) 0.0341(7) Uani 1 1 d . . .
H24A H 0.3596 0.2329 -0.0023 0.041 Uiso 1 1 calc R . .
C25 C 0.3189(3) 0.30852(12) 0.05278(14) 0.0259(6) Uani 1 1 d . . .
H25A H 0.3926 0.3001 0.0930 0.031 Uiso 1 1 calc R . .
C26 C 0.2941(3) 0.30980(11) 0.28471(13) 0.0203(5) Uani 1 1 d . . .
C27 C 0.3118(3) 0.29018(12) 0.35373(14) 0.0255(6) Uani 1 1 d . . .
H27A H 0.3774 0.3117 0.3894 0.031 Uiso 1 1 calc R . .
C28 C 0.2340(3) 0.23938(13) 0.37015(15) 0.0306(6) Uani 1 1 d . . .
H28A H 0.2462 0.2260 0.4171 0.037 Uiso 1 1 calc R . .
C29 C 0.1391(3) 0.20825(13) 0.31844(16) 0.0301(6) Uani 1 1 d . . .
H29A H 0.0851 0.1737 0.3299 0.036 Uiso 1 1 calc R . .
C30 C 0.1217(3) 0.22685(12) 0.25007(15) 0.0287(6) Uani 1 1 d . . .
H30A H 0.0562 0.2049 0.2147 0.034 Uiso 1 1 calc R . .
C31 C 0.1994(3) 0.27740(12) 0.23279(14) 0.0245(6) Uani 1 1 d . . .
H31A H 0.1880 0.2899 0.1856 0.029 Uiso 1 1 calc R . .
C32 C 0.5835(3) 0.36553(12) 0.30206(13) 0.0204(5) Uani 1 1 d . . .
C33 C 0.6616(3) 0.32346(13) 0.26976(15) 0.0279(6) Uani 1 1 d . . .
H33A H 0.6147 0.3032 0.2281 0.034 Uiso 1 1 calc R . .
C34 C 0.8078(3) 0.31118(15) 0.29863(17) 0.0374(7) Uani 1 1 d . . .
H34A H 0.8614 0.2825 0.2766 0.045 Uiso 1 1 calc R . .
C35 C 0.8760(3) 0.34031(15) 0.35905(18) 0.0410(8) Uani 1 1 d . . .
H35A H 0.9761 0.3313 0.3788 0.049 Uiso 1 1 calc R . .
C36 C 0.8001(3) 0.38231(15) 0.39094(17) 0.0387(7) Uani 1 1 d . . .
H36A H 0.8478 0.4025 0.4324 0.046 Uiso 1 1 calc R . .
C37 C 0.6528(3) 0.39526(14) 0.36231(14) 0.0300(6) Uani 1 1 d . . .
H37A H 0.6002 0.4244 0.3842 0.036 Uiso 1 1 calc R . .
C38 C 0.3297(3) 0.44294(12) 0.30537(13) 0.0219(5) Uani 1 1 d . . .
C39 C 0.3979(3) 0.49993(12) 0.29957(14) 0.0273(6) Uani 1 1 d . . .
H39A H 0.4778 0.5024 0.2761 0.033 Uiso 1 1 calc R . .
C40 C 0.3491(3) 0.55264(14) 0.32793(16) 0.0363(7) Uani 1 1 d . . .
H40A H 0.3962 0.5913 0.3244 0.044 Uiso 1 1 calc R . .
C41 C 0.2322(3) 0.54912(14) 0.36131(16) 0.0367(7) Uani 1 1 d . . .
H41A H 0.1992 0.5856 0.3807 0.044 Uiso 1 1 calc R . .
C42 C 0.1628(3) 0.49367(14) 0.36684(16) 0.0351(7) Uani 1 1 d . . .
H42A H 0.0820 0.4918 0.3898 0.042 Uiso 1 1 calc R . .
C43 C 0.2109(3) 0.44026(13) 0.33876(14) 0.0284(6) Uani 1 1 d . . .
H43A H 0.1628 0.4018 0.3423 0.034 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 111.20(12) . . ?
N1 Fe O3 114.55(11) . . ?
N2 Fe O3 114.19(11) . . ?
N1 Fe S1 107.32(9) . . ?
N2 Fe S1 112.72(9) . . ?
O3 Fe S1 95.77(6) . . ?
C1 S1 Fe 91.91(9) . . ?
C7 O3 Fe 123.30(17) . . ?
O1 N1 Fe 167.2(2) . . ?
O2 N2 Fe 157.1(2) . . ?
C2 C1 C6 117.9(3) . . ?
C2 C1 S1 118.6(2) . . ?
C6 C1 S1 123.5(2) . . ?
C3 C2 C1 121.7(3) . . ?
C2 C3 C4 120.5(3) . . ?
C3 C4 C5 119.3(3) . . ?
C4 C5 C6 121.6(3) . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C7 116.3(2) . . ?
C1 C6 C7 124.6(2) . . ?
O4 C7 O3 122.9(3) . . ?
O4 C7 C6 118.0(3) . . ?
O3 C7 C6 119.1(2) . . ?
N3 P1 C8 110.87(12) . . ?
N3 P1 C14 114.80(11) . . ?
C8 P1 C14 107.02(12) . . ?
N3 P1 C20 107.37(12) . . ?
C8 P1 C20 107.45(12) . . ?
C14 P1 C20 109.09(12) . . ?
N3 P2 C38 114.06(12) . . ?
N3 P2 C32 107.68(11) . . ?
C38 P2 C32 107.50(12) . . ?
N3 P2 C26 112.21(12) . . ?
C38 P2 C26 108.05(12) . . ?
C32 P2 C26 107.01(11) . . ?
P2 N3 P1 135.73(14) . . ?
C9 C8 C13 119.3(2) . . ?
C9 C8 P1 119.5(2) . . ?
C13 C8 P1 121.2(2) . . ?
C10 C9 C8 119.8(3) . . ?
C9 C10 C11 120.1(3) . . ?
C12 C11 C10 120.3(3) . . ?
C11 C12 C13 120.1(3) . . ?
C12 C13 C8 120.4(3) . . ?
C19 C14 C15 119.7(2) . . ?
C19 C14 P1 120.33(19) . . ?
C15 C14 P1 119.5(2) . . ?
C16 C15 C14 119.2(3) . . ?
C17 C16 C15 120.4(3) . . ?
C18 C17 C16 120.4(3) . . ?
C17 C18 C19 120.0(3) . . ?
C18 C19 C14 120.1(3) . . ?
C25 C20 C21 119.8(2) . . ?
C25 C20 P1 120.0(2) . . ?
C21 C20 P1 120.1(2) . . ?
C22 C21 C20 119.8(3) . . ?
C23 C22 C21 119.7(3) . . ?
C24 C23 C22 120.8(3) . . ?
C23 C24 C25 120.1(3) . . ?
C24 C25 C20 119.7(3) . . ?
C31 C26 C27 119.4(2) . . ?
C31 C26 P2 120.54(19) . . ?
C27 C26 P2 120.01(19) . . ?
C28 C27 C26 120.1(3) . . ?
C29 C28 C27 119.9(3) . . ?
C28 C29 C30 120.5(3) . . ?
C29 C30 C31 120.2(3) . . ?
C30 C31 C26 119.8(3) . . ?
C37 C32 C33 119.9(2) . . ?
C37 C32 P2 122.7(2) . . ?
C33 C32 P2 117.4(2) . . ?
C34 C33 C32 119.7(3) . . ?
C35 C34 C33 120.4(3) . . ?
C36 C35 C34 120.3(3) . . ?
C35 C36 C37 119.9(3) . . ?
C32 C37 C36 119.9(3) . . ?
C43 C38 C39 119.3(2) . . ?
C43 C38 P2 122.8(2) . . ?
C39 C38 P2 117.80(19) . . ?
C40 C39 C38 120.0(3) . . ?
C41 C40 C39 120.0(3) . . ?
C42 C41 C40 120.8(3) . . ?
C41 C42 C43 119.8(3) . . ?
C42 C43 C38 120.1(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 1.677(2) . ?
Fe N2 1.691(2) . ?
Fe O3 1.933(2) . ?
Fe S1 2.2638(9) . ?
S1 C1 1.770(3) . ?
O1 N1 1.166(3) . ?
O2 N2 1.172(3) . ?
O3 C7 1.293(3) . ?
O4 C7 1.217(3) . ?
C1 C2 1.400(4) . ?
C1 C6 1.415(4) . ?
C2 C3 1.368(4) . ?
C3 C4 1.376(4) . ?
C4 C5 1.379(4) . ?
C5 C6 1.392(4) . ?
C6 C7 1.512(4) . ?
P1 N3 1.585(2) . ?
P1 C8 1.792(2) . ?
P1 C14 1.796(2) . ?
P1 C20 1.797(3) . ?
P2 N3 1.583(2) . ?
P2 C38 1.790(3) . ?
P2 C32 1.801(2) . ?
P2 C26 1.801(3) . ?
C8 C9 1.386(4) . ?
C8 C13 1.394(4) . ?
C9 C10 1.381(4) . ?
C10 C11 1.385(5) . ?
C11 C12 1.366(5) . ?
C12 C13 1.374(4) . ?
C14 C19 1.390(4) . ?
C14 C15 1.402(4) . ?
C15 C16 1.385(4) . ?
C16 C17 1.383(4) . ?
C17 C18 1.373(4) . ?
C18 C19 1.384(4) . ?
C20 C25 1.390(4) . ?
C20 C21 1.391(4) . ?
C21 C22 1.389(4) . ?
C22 C23 1.375(4) . ?
C23 C24 1.373(4) . ?
C24 C25 1.385(4) . ?
C26 C31 1.390(4) . ?
C26 C27 1.397(4) . ?
C27 C28 1.385(4) . ?
C28 C29 1.375(4) . ?
C29 C30 1.378(4) . ?
C30 C31 1.386(4) . ?
C32 C37 1.383(4) . ?
C32 C33 1.391(4) . ?
C33 C34 1.384(4) . ?
C34 C35 1.377(5) . ?
C35 C36 1.373(5) . ?
C36 C37 1.395(4) . ?
C38 C43 1.393(3) . ?
C38 C39 1.396(4) . ?
C39 C40 1.381(4) . ?
C40 C41 1.378(4) . ?
C41 C42 1.372(4) . ?
C42 C43 1.388(4) . ?
