#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310085.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_4310085
loop_
_publ_author_name
'Chao-Yi Chiang'
'Jonghyuk Lee'
'Christopher Dalrymple'
'Michael C. Sarahan'
'Joseph H. Reibenspies'
'Marcetta Y. Darensbourg'
_publ_section_title
;
Synthesis and Molecular Structures of Mononitrosyl (N2S2)M(NO) Complexes (M
= Fe, Co)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9007
_journal_page_last               9016
_journal_paper_doi               10.1021/ic051027s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C9 H18 Fe N3 O S2'
_chemical_formula_weight         304.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.523(2)
_cell_angle_beta                 97.570(2)
_cell_angle_gamma                114.273(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3544(9)
_cell_length_b                   8.0686(10)
_cell_length_c                   11.6108(14)
_cell_measurement_reflns_used    3095
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.81
_cell_volume                     613.92(13)
_computing_cell_refinement       'Bruker SMART'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'CCD 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  0.0097
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3095
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0550P)²+0.8231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                1962
_reflns_number_total             2067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051027ssi20050622_045809_2.cif
_cod_data_source_block           mdjc
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4310085
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
O1A O 0.193(4) 0.4857(19) 0.4239(11) 0.039(4) Uani 0.65(12) 1 d P A -1
O1B O 0.124(16) 0.464(9) 0.419(4) 0.064(10) Uani 0.35(12) 1 d P A -2
Fe1 Fe 0.11229(5) 0.17603(4) 0.25967(3) 0.01759(14) Uani 1 1 d . A .
S1 S -0.02905(10) 0.29064(9) 0.12802(6) 0.02600(18) Uani 1 1 d . . .
S2 S -0.17619(10) -0.07391(9) 0.25896(6) 0.02542(18) Uani 1 1 d . . .
N1 N 0.3692(3) 0.2922(3) 0.1975(2) 0.0248(5) Uani 1 1 d . . .
N2 N 0.2586(3) 0.0245(3) 0.31388(19) 0.0202(4) Uani 1 1 d . . .
N3 N 0.1638(4) 0.3385(3) 0.3797(2) 0.0276(5) Uani 1 1 d . . .
C1 C 0.2000(4) 0.4369(4) 0.0756(2) 0.0273(6) Uani 1 1 d . . .
H1A H 0.2041 0.3753 -0.0014 0.033 Uiso 1 1 calc R . .
H1B H 0.1963 0.5556 0.0644 0.033 Uiso 1 1 calc R . .
C2 C 0.3872(4) 0.4721(4) 0.1632(3) 0.0303(6) Uani 1 1 d . . .
H2A H 0.5094 0.5281 0.1278 0.036 Uiso 1 1 calc R . .
H2B H 0.4007 0.5587 0.2337 0.036 Uiso 1 1 calc R . .
C3 C 0.3692(4) 0.1682(4) 0.0952(3) 0.0306(6) Uani 1 1 d . . .
H3A H 0.4779 0.2388 0.0534 0.037 Uiso 1 1 calc R . .
H3B H 0.2377 0.1224 0.0400 0.037 Uiso 1 1 calc R . .
C4 C 0.4018(5) 0.0070(4) 0.1302(3) 0.0318(6) Uani 1 1 d . . .
H4A H 0.5448 0.0516 0.1702 0.038 Uiso 1 1 calc R . .
H4B H 0.3801 -0.0798 0.0579 0.038 Uiso 1 1 calc R . .
C5 C 0.2650(4) -0.0965(4) 0.2105(2) 0.0260(6) Uani 1 1 d . . .
H5A H 0.1256 -0.1670 0.1643 0.031 Uiso 1 1 calc R . .
H5B H 0.3123 -0.1862 0.2394 0.031 Uiso 1 1 calc R . .
C6 C 0.5376(4) 0.3243(4) 0.2975(3) 0.0322(6) Uani 1 1 d . . .
H6A H 0.5729 0.4419 0.3497 0.039 Uiso 1 1 calc R . .
H6B H 0.6597 0.3333 0.2663 0.039 Uiso 1 1 calc R . .
C7 C 0.4688(4) 0.1606(4) 0.3698(3) 0.0278(6) Uani 1 1 d . . .
H7A H 0.5624 0.1007 0.3702 0.033 Uiso 1 1 calc R . .
H7B H 0.4721 0.2079 0.4523 0.033 Uiso 1 1 calc R . .
C8 C 0.1496(4) -0.0916(3) 0.3972(2) 0.0229(5) Uani 1 1 d . . .
H8A H 0.1578 -0.0115 0.4697 0.027 Uiso 1 1 calc R . .
H8B H 0.2153 -0.1721 0.4195 0.027 Uiso 1 1 calc R . .
C9 C -0.0703(4) -0.2087(4) 0.3412(3) 0.0265(6) Uani 1 1 d . . .
H9A H -0.1495 -0.2552 0.4031 0.032 Uiso 1 1 calc R . .
H9B H -0.0813 -0.3163 0.2869 0.032 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'
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
N3 Fe1 N1 99.65(11) . . ?
N3 Fe1 N2 104.29(10) . . ?
N1 Fe1 N2 79.03(9) . . ?
N3 Fe1 S1 98.52(8) . . ?
N1 Fe1 S1 87.77(7) . . ?
N2 Fe1 S1 155.21(7) . . ?
N3 Fe1 S2 110.48(8) . . ?
N1 Fe1 S2 148.93(7) . . ?
N2 Fe1 S2 86.19(6) . . ?
S1 Fe1 S2 94.91(3) . . ?
C1 S1 Fe1 98.72(9) . . ?
C9 S2 Fe1 99.49(9) . . ?
C3 N1 C2 110.5(2) . . ?
C3 N1 C6 111.0(2) . . ?
C2 N1 C6 110.4(2) . . ?
C3 N1 Fe1 110.38(17) . . ?
C2 N1 Fe1 108.82(17) . . ?
C6 N1 Fe1 105.62(17) . . ?
C8 N2 C7 112.7(2) . . ?
C8 N2 C5 109.43(19) . . ?
C7 N2 C5 109.7(2) . . ?
C8 N2 Fe1 109.44(15) . . ?
C7 N2 Fe1 105.58(15) . . ?
C5 N2 Fe1 109.92(16) . . ?
O1A N3 Fe1 152.4(6) . . ?
O1B N3 Fe1 144(3) . . ?
C2 C1 S1 110.25(19) . . ?
N1 C2 C1 108.7(2) . . ?
N1 C3 C4 112.5(2) . . ?
C3 C4 C5 114.6(2) . . ?
N2 C5 C4 113.9(2) . . ?
N1 C6 C7 109.8(2) . . ?
N2 C7 C6 108.7(2) . . ?
N2 C8 C9 110.5(2) . . ?
C8 C9 S2 110.69(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
O1A N3 1.167(18) . ?
O1B N3 1.23(3) . ?
Fe1 N3 1.705(2) . ?
Fe1 N1 2.001(2) . ?
Fe1 N2 2.025(2) . ?
Fe1 S1 2.2172(7) . ?
Fe1 S2 2.2456(7) . ?
S1 C1 1.837(3) . ?
S2 C9 1.844(3) . ?
N1 C3 1.477(4) . ?
N1 C2 1.500(4) . ?
N1 C6 1.499(4) . ?
N2 C8 1.488(3) . ?
N2 C7 1.490(3) . ?
N2 C5 1.491(3) . ?
C1 C2 1.504(4) . ?
C3 C4 1.498(4) . ?
C4 C5 1.512(4) . ?
C6 C7 1.575(4) . ?
C8 C9 1.510(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Fe1 S1 C1 90.85(13) . . . . ?
N1 Fe1 S1 C1 -8.58(12) . . . . ?
N2 Fe1 S1 C1 -66.00(18) . . . . ?
S2 Fe1 S1 C1 -157.56(10) . . . . ?
N3 Fe1 S2 C9 -90.67(13) . . . . ?
N1 Fe1 S2 C9 74.48(16) . . . . ?
N2 Fe1 S2 C9 13.17(11) . . . . ?
S1 Fe1 S2 C9 168.32(10) . . . . ?
N3 Fe1 N1 C3 175.73(18) . . . . ?
N2 Fe1 N1 C3 72.90(18) . . . . ?
S1 Fe1 N1 C3 -86.01(17) . . . . ?
S2 Fe1 N1 C3 9.8(3) . . . . ?
N3 Fe1 N1 C2 -62.84(19) . . . . ?
N2 Fe1 N1 C2 -165.67(19) . . . . ?
S1 Fe1 N1 C2 35.43(17) . . . . ?
S2 Fe1 N1 C2 131.26(16) . . . . ?
N3 Fe1 N1 C6 55.68(19) . . . . ?
N2 Fe1 N1 C6 -47.15(17) . . . . ?
S1 Fe1 N1 C6 153.95(17) . . . . ?
S2 Fe1 N1 C6 -110.22(18) . . . . ?
N3 Fe1 N2 C8 72.29(18) . . . . ?
N1 Fe1 N2 C8 169.58(17) . . . . ?
S1 Fe1 N2 C8 -131.36(16) . . . . ?
S2 Fe1 N2 C8 -37.89(15) . . . . ?
N3 Fe1 N2 C7 -49.23(19) . . . . ?
N1 Fe1 N2 C7 48.06(17) . . . . ?
S1 Fe1 N2 C7 107.12(19) . . . . ?
S2 Fe1 N2 C7 -159.41(16) . . . . ?
N3 Fe1 N2 C5 -167.51(17) . . . . ?
N1 Fe1 N2 C5 -70.22(17) . . . . ?
S1 Fe1 N2 C5 -11.2(3) . . . . ?
S2 Fe1 N2 C5 82.31(16) . . . . ?
N1 Fe1 N3 O1A 67(3) . . . . ?
N2 Fe1 N3 O1A 148(3) . . . . ?
S1 Fe1 N3 O1A -23(3) . . . . ?
S2 Fe1 N3 O1A -121(3) . . . . ?
N1 Fe1 N3 O1B 106(7) . . . . ?
N2 Fe1 N3 O1B -173(7) . . . . ?
S1 Fe1 N3 O1B 16(7) . . . . ?
S2 Fe1 N3 O1B -82(7) . . . . ?
Fe1 S1 C1 C2 -18.6(2) . . . . ?
C3 N1 C2 C1 65.1(3) . . . . ?
C6 N1 C2 C1 -171.7(2) . . . . ?
Fe1 N1 C2 C1 -56.2(3) . . . . ?
S1 C1 C2 N1 47.8(3) . . . . ?
C2 N1 C3 C4 166.3(2) . . . . ?
C6 N1 C3 C4 43.5(3) . . . . ?
Fe1 N1 C3 C4 -73.3(2) . . . . ?
N1 C3 C4 C5 50.1(3) . . . . ?
C8 N2 C5 C4 -170.4(2) . . . . ?
C7 N2 C5 C4 -46.3(3) . . . . ?
Fe1 N2 C5 C4 69.4(2) . . . . ?
C3 C4 C5 N2 -49.2(3) . . . . ?
C3 N1 C6 C7 -83.0(3) . . . . ?
C2 N1 C6 C7 154.2(2) . . . . ?
Fe1 N1 C6 C7 36.7(2) . . . . ?
C8 N2 C7 C6 -157.0(2) . . . . ?
C5 N2 C7 C6 80.8(2) . . . . ?
Fe1 N2 C7 C6 -37.6(2) . . . . ?
N1 C6 C7 N2 0.9(3) . . . . ?
C7 N2 C8 C9 172.4(2) . . . . ?
C5 N2 C8 C9 -65.2(3) . . . . ?
Fe1 N2 C8 C9 55.3(2) . . . . ?
N2 C8 C9 S2 -42.0(3) . . . . ?
Fe1 S2 C9 C8 11.6(2) . . . . ?
