#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310087.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_4310087
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 H20 Co N3 O S2'
_chemical_formula_weight         309.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.676(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2608(13)
_cell_length_b                   12.7516(19)
_cell_length_c                   12.5833(19)
_cell_measurement_reflns_used    6617
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.29
_cell_volume                     1310.3(3)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9943
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    1.612
_exptl_absorpt_correction_T_max  0.8554
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0278P)²+0.5672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                2157
_reflns_number_total             2262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051027ssi20050622_045809_4.cif
_cod_data_source_block           433a
_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               4310087
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Co1 Co 0.22509(2) 0.189531(16) 0.168179(16) 0.01355(8) Uani 1 1 d . A .
S1 S 0.05516(5) 0.06149(3) 0.19684(4) 0.02567(12) Uani 1 1 d . . .
S2 S 0.39293(5) 0.12216(4) 0.30464(3) 0.02472(12) Uani 1 1 d . . .
O1B O 0.404(5) 0.075(3) 0.0549(9) 0.031(5) Uani 0.34(7) 1 d P A -1
O1A O 0.4421(15) 0.111(2) 0.0524(5) 0.032(3) Uani 0.66(7) 1 d P A -2
N1 N 0.02812(16) 0.25584(10) 0.07159(11) 0.0169(3) Uani 1 1 d . . .
N2 N 0.35878(16) 0.32340(10) 0.19039(11) 0.0172(3) Uani 1 1 d . . .
N3 N 0.31425(17) 0.14467(11) 0.05603(11) 0.0207(3) Uani 1 1 d . . .
C1 C -0.1139(2) 0.08690(14) 0.08809(16) 0.0278(4) Uani 1 1 d . . .
H1A H -0.1453 0.0210 0.0487 0.033 Uiso 1 1 calc R . .
H1B H -0.2102 0.1128 0.1185 0.033 Uiso 1 1 calc R . .
C2 C -0.0627(2) 0.16735(14) 0.01202(15) 0.0237(4) Uani 1 1 d . . .
H2A H 0.0079 0.1336 -0.0350 0.028 Uiso 1 1 calc R . .
H2B H -0.1611 0.1950 -0.0342 0.028 Uiso 1 1 calc R . .
C3 C 0.0756(2) 0.32974(13) -0.00977(14) 0.0206(4) Uani 1 1 d . . .
H3A H -0.0251 0.3588 -0.0521 0.025 Uiso 1 1 calc R . .
H3B H 0.1345 0.2901 -0.0598 0.025 Uiso 1 1 calc R . .
C4 C 0.1831(2) 0.41999(13) 0.03728(14) 0.0231(4) Uani 1 1 d . . .
H4A H 0.1273 0.4567 0.0909 0.028 Uiso 1 1 calc R . .
H4B H 0.1943 0.4705 -0.0209 0.028 Uiso 1 1 calc R . .
C5 C 0.3532(2) 0.38802(13) 0.09082(14) 0.0212(4) Uani 1 1 d . . .
H5A H 0.4064 0.3480 0.0382 0.025 Uiso 1 1 calc R . .
H5B H 0.4185 0.4524 0.1090 0.025 Uiso 1 1 calc R . .
C6 C -0.0840(2) 0.30872(13) 0.13631(15) 0.0231(4) Uani 1 1 d . . .
H6A H -0.0322 0.3729 0.1681 0.035 Uiso 1 1 calc R . .
H6B H -0.1073 0.2616 0.1936 0.035 Uiso 1 1 calc R . .
H6C H -0.1864 0.3266 0.0899 0.035 Uiso 1 1 calc R . .
C7 C 0.3070(2) 0.38813(14) 0.27806(14) 0.0232(4) Uani 1 1 d . . .
H7A H 0.3822 0.4475 0.2938 0.035 Uiso 1 1 calc R . .
H7B H 0.3092 0.3451 0.3428 0.035 Uiso 1 1 calc R . .
H7C H 0.1957 0.4144 0.2553 0.035 Uiso 1 1 calc R . .
C8 C 0.5339(2) 0.29288(14) 0.22406(15) 0.0241(4) Uani 1 1 d . . .
H8A H 0.6007 0.3568 0.2413 0.029 Uiso 1 1 calc R . .
H8B H 0.5747 0.2567 0.1638 0.029 Uiso 1 1 calc R . .
C9 C 0.5535(2) 0.22152(16) 0.32106(15) 0.0289(4) Uani 1 1 d . . .
H9A H 0.5469 0.2632 0.3866 0.035 Uiso 1 1 calc R . .
H9B H 0.6622 0.1872 0.3294 0.035 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'
Co Co 0.3494 0.9721 '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 Co1 N2 95.61(6) . . ?
N3 Co1 N1 92.78(6) . . ?
N2 Co1 N1 95.80(5) . . ?
N3 Co1 S2 101.81(5) . . ?
N2 Co1 S2 87.44(4) . . ?
N1 Co1 S2 164.69(4) . . ?
N3 Co1 S1 103.88(5) . . ?
N2 Co1 S1 160.30(4) . . ?
N1 Co1 S1 86.28(4) . . ?
S2 Co1 S1 85.75(2) . . ?
C1 S1 Co1 100.27(6) . . ?
C9 S2 Co1 100.27(6) . . ?
C6 N1 C3 109.95(12) . . ?
C6 N1 C2 108.11(13) . . ?
C3 N1 C2 107.35(13) . . ?
C6 N1 Co1 111.44(10) . . ?
C3 N1 Co1 113.53(10) . . ?
C2 N1 Co1 106.18(10) . . ?
C7 N2 C5 109.81(13) . . ?
C7 N2 C8 107.90(13) . . ?
C5 N2 C8 106.69(13) . . ?
C7 N2 Co1 110.90(10) . . ?
C5 N2 Co1 113.64(10) . . ?
C8 N2 Co1 107.64(10) . . ?
O1A N3 O1B 28.1(13) . . ?
O1A N3 Co1 130.1(3) . . ?
O1B N3 Co1 126.7(10) . . ?
C2 C1 S1 109.87(12) . . ?
N1 C2 C1 111.33(14) . . ?
N1 C3 C4 114.29(14) . . ?
C3 C4 C5 114.63(14) . . ?
N2 C5 C4 115.42(13) . . ?
N2 C8 C9 111.50(14) . . ?
C8 C9 S2 109.84(12) . . ?
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
Co1 N3 1.7818(14) . ?
Co1 N2 2.0294(14) . ?
Co1 N1 2.0598(13) . ?
Co1 S2 2.2115(5) . ?
Co1 S1 2.2180(5) . ?
S1 C1 1.8307(19) . ?
S2 C9 1.823(2) . ?
O1B N3 1.164(10) . ?
O1A N3 1.148(5) . ?
N1 C6 1.484(2) . ?
N1 C3 1.487(2) . ?
N1 C2 1.493(2) . ?
N2 C7 1.491(2) . ?
N2 C5 1.494(2) . ?
N2 C8 1.496(2) . ?
C1 C2 1.506(2) . ?
C3 C4 1.518(2) . ?
C4 C5 1.519(2) . ?
C8 C9 1.511(3) . ?
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 Co1 S1 C1 -76.80(8) . . . . ?
N2 Co1 S1 C1 111.97(13) . . . . ?
N1 Co1 S1 C1 15.15(7) . . . . ?
S2 Co1 S1 C1 -177.93(6) . . . . ?
N3 Co1 S2 C9 83.79(8) . . . . ?
N2 Co1 S2 C9 -11.41(7) . . . . ?
N1 Co1 S2 C9 -114.10(16) . . . . ?
S1 Co1 S2 C9 -172.90(6) . . . . ?
N3 Co1 N1 C6 -178.29(11) . . . . ?
N2 Co1 N1 C6 -82.37(11) . . . . ?
S2 Co1 N1 C6 19.2(2) . . . . ?
S1 Co1 N1 C6 77.97(10) . . . . ?
N3 Co1 N1 C3 -53.49(11) . . . . ?
N2 Co1 N1 C3 42.44(11) . . . . ?
S2 Co1 N1 C3 144.03(13) . . . . ?
S1 Co1 N1 C3 -157.23(10) . . . . ?
N3 Co1 N1 C2 64.22(11) . . . . ?
N2 Co1 N1 C2 160.15(10) . . . . ?
S2 Co1 N1 C2 -98.26(17) . . . . ?
S1 Co1 N1 C2 -39.52(10) . . . . ?
N3 Co1 N2 C7 176.22(11) . . . . ?
N1 Co1 N2 C7 82.84(11) . . . . ?
S2 Co1 N2 C7 -82.16(11) . . . . ?
S1 Co1 N2 C7 -12.3(2) . . . . ?
N3 Co1 N2 C5 51.95(11) . . . . ?
N1 Co1 N2 C5 -41.43(11) . . . . ?
S2 Co1 N2 C5 153.57(10) . . . . ?
S1 Co1 N2 C5 -136.60(11) . . . . ?
N3 Co1 N2 C8 -65.96(11) . . . . ?
N1 Co1 N2 C8 -159.34(10) . . . . ?
S2 Co1 N2 C8 35.66(10) . . . . ?
S1 Co1 N2 C8 105.48(14) . . . . ?
N2 Co1 N3 O1A 73(2) . . . . ?
N1 Co1 N3 O1A 169(2) . . . . ?
S2 Co1 N3 O1A -16(2) . . . . ?
S1 Co1 N3 O1A -104(2) . . . . ?
N2 Co1 N3 O1B 109(3) . . . . ?
N1 Co1 N3 O1B -155(3) . . . . ?
S2 Co1 N3 O1B 20(3) . . . . ?
S1 Co1 N3 O1B -69(3) . . . . ?
Co1 S1 C1 C2 10.32(13) . . . . ?
C6 N1 C2 C1 -62.39(17) . . . . ?
C3 N1 C2 C1 179.04(13) . . . . ?
Co1 N1 C2 C1 57.29(15) . . . . ?
S1 C1 C2 N1 -43.61(17) . . . . ?
C6 N1 C3 C4 67.90(17) . . . . ?
C2 N1 C3 C4 -174.73(13) . . . . ?
Co1 N1 C3 C4 -57.70(16) . . . . ?
N1 C3 C4 C5 66.96(19) . . . . ?
C7 N2 C5 C4 -68.24(17) . . . . ?
C8 N2 C5 C4 175.09(14) . . . . ?
Co1 N2 C5 C4 56.62(16) . . . . ?
C3 C4 C5 N2 -66.48(19) . . . . ?
C7 N2 C8 C9 65.37(18) . . . . ?
C5 N2 C8 C9 -176.69(14) . . . . ?
Co1 N2 C8 C9 -54.37(16) . . . . ?
N2 C8 C9 S2 43.82(17) . . . . ?
Co1 S2 C9 C8 -13.60(13) . . . . ?
