#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316435.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_4316435
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_moiety         'C62 H48 Fe N4 O4 P2 S2'
_chemical_formula_sum            'C62 H48 Fe N4 O4 P2 S2'
_chemical_formula_weight         1094.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.0330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4730(5)
_cell_length_b                   13.4520(3)
_cell_length_c                   19.3090(5)
_cell_measurement_reflns_used    13847
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     5330.8(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12513
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.7552
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0463
_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)+(0.0738P)²+5.9600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                3589
_reflns_number_total             4446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101126v_si_004_2.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4316435
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
C1 C 0.42504(14) 0.14401(19) 0.27783(16) 0.0431(6) Uani 1 1 d . . .
C2 C 0.47242(16) 0.1395(2) 0.35768(17) 0.0525(7) Uani 1 1 d . . .
H2 H 0.5110 0.1753 0.3763 0.063 Uiso 1 1 d R . .
C3 C 0.46137(19) 0.0811(3) 0.4087(2) 0.0655(9) Uani 1 1 d . . .
H3 H 0.4928 0.0783 0.4620 0.079 Uiso 1 1 d R . .
C4 C 0.4049(2) 0.0270(3) 0.3827(2) 0.0714(10) Uani 1 1 d . . .
H4 H 0.3988 -0.0124 0.4182 0.086 Uiso 1 1 d R . .
C5 C 0.35697(19) 0.0306(2) 0.3041(2) 0.0645(9) Uani 1 1 d . . .
H5 H 0.3185 -0.0052 0.2866 0.077 Uiso 1 1 d R . .
C6 C 0.36750(16) 0.0895(2) 0.25167(17) 0.0501(7) Uani 1 1 d . . .
C7 C 0.37771(15) 0.1905(2) 0.14847(16) 0.0463(7) Uani 1 1 d . . .
C8 C 0.25581(14) 0.29700(19) 0.34505(16) 0.0456(7) Uani 1 1 d . . .
C9 C 0.30401(17) 0.2722(2) 0.3258(2) 0.0619(9) Uani 1 1 d . . .
H9 H 0.2997 0.2151 0.2964 0.074 Uiso 1 1 d R . .
C10 C 0.35818(18) 0.3316(3) 0.3501(2) 0.0730(10) Uani 1 1 d . . .
H10 H 0.3900 0.3151 0.3365 0.088 Uiso 1 1 d R . .
C11 C 0.36535(17) 0.4149(3) 0.3940(2) 0.0723(10) Uani 1 1 d . . .
H11 H 0.4019 0.4551 0.4099 0.087 Uiso 1 1 d R . .
C12 C 0.31880(17) 0.4397(2) 0.4151(2) 0.0684(9) Uani 1 1 d . . .
H12 H 0.3243 0.4957 0.4460 0.082 Uiso 1 1 d R . .
C13 C 0.26381(15) 0.3809(2) 0.39009(17) 0.0526(7) Uani 1 1 d . . .
H13 H 0.2321 0.3982 0.4036 0.063 Uiso 1 1 d R . .
C14 C 0.20684(15) 0.0985(2) 0.35111(16) 0.0495(7) Uani 1 1 d . . .
C15 C 0.26587(15) 0.0814(2) 0.41715(18) 0.0575(8) Uani 1 1 d . . .
H15 H 0.2963 0.1324 0.4379 0.069 Uiso 1 1 d R . .
C16 C 0.28027(16) -0.0113(2) 0.45301(19) 0.0643(9) Uani 1 1 d . . .
H16 H 0.3208 -0.0224 0.4971 0.077 Uiso 1 1 d R . .
C17 C 0.23586(19) -0.0860(2) 0.4243(2) 0.0734(10) Uani 1 1 d . . .
H17 H 0.2453 -0.1478 0.4491 0.088 Uiso 1 1 d R . .
C18 C 0.1776(2) -0.0693(3) 0.3591(3) 0.129(2) Uani 1 1 d . . .
H18 H 0.1466 -0.1197 0.3399 0.155 Uiso 1 1 d R . .
C19 C 0.1633(2) 0.0217(3) 0.3208(3) 0.1101(19) Uani 1 1 d . . .
H19 H 0.1242 0.0306 0.2743 0.132 Uiso 1 1 d R . .
C20 C 0.13279(14) 0.2740(2) 0.34575(16) 0.0450(6) Uani 1 1 d . . .
C21 C 0.12943(16) 0.2338(3) 0.40940(18) 0.0617(8) Uani 1 1 d . . .
H21 H 0.1510 0.1747 0.4322 0.074 Uiso 1 1 d R . .
C22 C 0.09400(19) 0.2816(4) 0.4393(2) 0.0787(11) Uani 1 1 d . . .
H22 H 0.0919 0.2545 0.4823 0.094 Uiso 1 1 d R . .
C23 C 0.06199(18) 0.3678(3) 0.4063(2) 0.0761(11) Uani 1 1 d . . .
H23 H 0.0380 0.3991 0.4268 0.091 Uiso 1 1 d R . .
C24 C 0.06484(16) 0.4086(3) 0.3434(2) 0.0674(9) Uani 1 1 d . . .
H24 H 0.0433 0.4681 0.3216 0.081 Uiso 1 1 d R . .
C25 C 0.09944(15) 0.3620(2) 0.31177(19) 0.0567(8) Uani 1 1 d . . .
H25 H 0.1006 0.3894 0.2682 0.068 Uiso 1 1 d R . .
C26 C 0.13974(16) 0.2165(2) 0.20397(16) 0.0525(7) Uani 1 1 d . . .
C27 C 0.07813(18) 0.1746(3) 0.1681(2) 0.0745(10) Uani 1 1 d . . .
H27 H 0.0587 0.1563 0.1984 0.089 Uiso 1 1 d R . .
C28 C 0.0453(2) 0.1602(3) 0.0866(2) 0.0881(13) Uani 1 1 d . . .
H28 H 0.0047 0.1294 0.0623 0.106 Uiso 1 1 d R . .
C29 C 0.0733(3) 0.1915(3) 0.0417(2) 0.0870(13) Uani 1 1 d . . .
H29 H 0.0513 0.1821 -0.0129 0.104 Uiso 1 1 d R . .
C30 C 0.1325(3) 0.2356(3) 0.0768(2) 0.0981(15) Uani 1 1 d . . .
H30 H 0.1503 0.2581 0.0459 0.118 Uiso 1 1 d R . .
C31 C 0.1666(2) 0.2480(3) 0.1582(2) 0.0746(10) Uani 1 1 d . . .
H31 H 0.2077 0.2774 0.1819 0.089 Uiso 1 1 d R . .
Fe1 Fe 0.5000 0.31247(4) 0.2500 0.04412(19) Uani 1 2 d S . .
S1 S 0.31678(4) 0.10962(6) 0.15151(5) 0.0599(2) Uani 1 1 d . . .
P1 P 0.18400(4) 0.22119(5) 0.31048(4) 0.0444(2) Uani 1 1 d . . .
N1 N 0.49526(14) 0.38192(19) 0.17770(15) 0.0610(7) Uani 1 1 d . . .
N2 N 0.42954(11) 0.20125(16) 0.22063(12) 0.0437(5) Uani 1 1 d . . .
O1 O 0.49243(18) 0.4506(2) 0.13624(18) 0.1073(10) Uani 1 1 d . . .
O2 O 0.36781(11) 0.22638(16) 0.08523(11) 0.0620(6) 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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 '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'
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 C1 C6 115.8(2) . . ?
N2 C1 C2 125.0(3) . . ?
C6 C1 C2 119.2(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 121.5(3) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 120.6(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 118.6(3) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C1 C6 C5 121.0(3) . . ?
C1 C6 S1 110.0(2) . . ?
C5 C6 S1 129.1(3) . . ?
O2 C7 N2 129.1(3) . . ?
O2 C7 S1 119.7(2) . . ?
N2 C7 S1 111.2(2) . . ?
C13 C8 C9 119.0(3) . . ?
C13 C8 P1 120.9(2) . . ?
C9 C8 P1 120.1(2) . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C13 119.8(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C8 C13 C12 120.3(3) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 H13 119.8 . . ?
C19 C14 C15 118.5(3) . . ?
C19 C14 P1 120.3(2) . . ?
C15 C14 P1 120.9(2) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 120.6(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.6 . . ?
C18 C17 C16 119.1(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.5 . . ?
C14 C19 C18 120.2(3) . . ?
C14 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 C25 119.4(3) . . ?
C21 C20 P1 121.5(2) . . ?
C25 C20 P1 119.0(2) . . ?
C22 C21 C20 119.7(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.2 . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 120.3(4) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 119.6(3) . . ?
C24 C25 H25 120.1 . . ?
C20 C25 H25 120.3 . . ?
C31 C26 C27 119.8(3) . . ?
C31 C26 P1 122.1(3) . . ?
C27 C26 P1 118.0(3) . . ?
C26 C27 C28 119.5(4) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 120.6(4) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.7 . . ?
C26 C31 C30 119.8(4) . . ?
C26 C31 H31 120.1 . . ?
C30 C31 H31 120.0 . . ?
N1 Fe1 N1 110.45(19) 2_655 . ?
N1 Fe1 N2 110.87(12) 2_655 . ?
N1 Fe1 N2 117.30(11) . . ?
N1 Fe1 N2 117.30(11) 2_655 2_655 ?
N1 Fe1 N2 110.87(12) . 2_655 ?
N2 Fe1 N2 88.80(13) . 2_655 ?
C6 S1 C7 90.24(14) . . ?
C20 P1 C14 108.19(14) . . ?
C20 P1 C26 109.07(14) . . ?
C14 P1 C26 110.58(13) . . ?
C20 P1 C8 108.35(13) . . ?
C14 P1 C8 109.39(13) . . ?
C26 P1 C8 111.19(14) . . ?
O1 N1 Fe1 164.6(3) . . ?
C7 N2 C1 112.6(2) . . ?
C7 N2 Fe1 123.90(18) . . ?
C1 N2 Fe1 122.32(18) . . ?
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
C1 N2 1.392(3) . ?
C1 C6 1.398(4) . ?
C1 C2 1.398(4) . ?
C2 C3 1.379(4) . ?
C2 H2 0.9302 . ?
C3 C4 1.376(5) . ?
C3 H3 0.9303 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9304 . ?
C5 C6 1.399(4) . ?
C5 H5 0.9301 . ?
C6 S1 1.731(3) . ?
C7 O2 1.226(3) . ?
C7 N2 1.341(4) . ?
C7 S1 1.820(3) . ?
C8 C13 1.381(4) . ?
C8 C9 1.392(4) . ?
C8 P1 1.798(3) . ?
C9 C10 1.377(5) . ?
C9 H9 0.9304 . ?
C10 C11 1.366(5) . ?
C10 H10 0.9303 . ?
C11 C12 1.379(5) . ?
C11 H11 0.9301 . ?
C12 C13 1.386(4) . ?
C12 H12 0.9303 . ?
C13 H13 0.9303 . ?
C14 C19 1.368(4) . ?
C14 C15 1.372(4) . ?
C14 P1 1.794(3) . ?
C15 C16 1.386(4) . ?
C15 H15 0.9302 . ?
C16 C17 1.357(5) . ?
C16 H16 0.9303 . ?
C17 C18 1.355(5) . ?
C17 H17 0.9302 . ?
C18 C19 1.384(5) . ?
C18 H18 0.9302 . ?
C19 H19 0.9304 . ?
C20 C21 1.380(4) . ?
C20 C25 1.395(4) . ?
C20 P1 1.791(3) . ?
C21 C22 1.380(5) . ?
C21 H21 0.9303 . ?
C22 C23 1.360(6) . ?
C22 H22 0.9304 . ?
C23 C24 1.364(5) . ?
C23 H23 0.9301 . ?
C24 C25 1.380(4) . ?
C24 H24 0.9301 . ?
C25 H25 0.9304 . ?
C26 C31 1.379(5) . ?
C26 C27 1.384(5) . ?
C26 P1 1.800(3) . ?
C27 C28 1.390(5) . ?
C27 H27 0.9305 . ?
C28 C29 1.383(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.351(6) . ?
C29 H29 0.9305 . ?
C30 C31 1.385(5) . ?
C30 H30 0.9302 . ?
C31 H31 0.9303 . ?
Fe1 N1 1.638(3) 2_655 ?
Fe1 N1 1.638(3) . ?
Fe1 N2 2.094(2) . ?
Fe1 N2 2.094(2) 2_655 ?
N1 O1 1.203(3) . ?
