#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008184.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_7008184
loop_
_publ_author_name
'Fourmigué, Marc'
'Avarvari, Narcis'
_publ_section_title
;
 A series of neutral radical CpNi(dithiolene). complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1365
_journal_page_last               1371
_journal_paper_doi               10.1039/b418756n
_journal_year                    2005
_chemical_formula_moiety         'C8 H5 Ni1 O1 S4'
_chemical_formula_sum            'C8 H5 Ni O S4'
_chemical_formula_weight         304.07
_chemical_name_common            CpNi(dmid)
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_date             2003-02-25T18:17:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0485(7)
_cell_length_b                   7.2993(7)
_cell_length_c                   17.7872(19)
_cell_measurement_reflns_used    4442
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      2.25
_cell_volume                     1044.97(18)
_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-97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       'oscillation, phi incr. 1.3 deg.'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5997
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    2.613
_exptl_absorpt_correction_T_max  0.6005
_exptl_absorpt_correction_T_min  0.5384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0398P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                823
_reflns_number_total             1075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418756n.txt
_cod_data_source_block           mf308
_cod_database_code               7008184
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Ni1 Ni 0.17565(6) 0.25 0.60354(2) 0.03973(16) Uani 1 d S . .
S2 S 0.44164(11) 0.25 0.59577(4) 0.0408(2) Uani 1 d S . .
S4 S 0.66480(11) 0.25 0.45936(5) 0.0474(3) Uani 1 d S . .
S1 S 0.13595(11) 0.25 0.48470(5) 0.0478(3) Uani 1 d S . .
S3 S 0.37782(13) 0.25 0.35616(5) 0.0468(3) Uani 1 d S . .
O1 O 0.6889(4) 0.25 0.31141(16) 0.0657(9) Uani 1 d S . .
C1 C 0.3365(4) 0.25 0.45268(17) 0.0349(8) Uani 1 d S . .
C2 C 0.4681(4) 0.25 0.49994(17) 0.0326(8) Uani 1 d S . .
C3 C 0.5973(5) 0.25 0.3647(2) 0.0443(9) Uani 1 d S . .
C4 C 0.1426(8) 0.1637(18) 0.7170(4) 0.055(3) Uani 0.5 d PG . .
H4 H 0.2244 0.113 0.7475 0.066 Uiso 0.5 calc PR . .
C5 C 0.0307(8) 0.0670(9) 0.6727(5) 0.039(2) Uani 0.5 d PG . .
H5 H 0.0243 -0.0598 0.6684 0.047 Uiso 0.5 calc PR . .
C6 C -0.0702(5) 0.1929(7) 0.6360(3) 0.065(5) Uani 0.5 d PG . .
H6 H -0.1559 0.1653 0.6028 0.078 Uiso 0.5 calc PR . .
C7 C -0.0205(11) 0.3674(12) 0.6576(6) 0.076(4) Uani 0.5 d PG . .
H7 H -0.0672 0.4771 0.6414 0.091 Uiso 0.5 calc PR . .
C8 C 0.1110(9) 0.349(2) 0.7076(4) 0.076(5) Uani 0.5 d PG . .
H8 H 0.1678 0.4448 0.7308 0.092 Uiso 0.5 calc PR . .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
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
C7 Ni1 C7 49.7(3) 8_565 . ?
C7 Ni1 C8 61.8(3) 8_565 . ?
C7 Ni1 C8 39.67(14) . . ?
C7 Ni1 C8 39.67(14) 8_565 8_565 ?
C7 Ni1 C8 61.8(5) . 8_565 ?
C8 Ni1 C8 41.3(7) . 8_565 ?
C7 Ni1 C6 19.6(2) 8_565 . ?
C7 Ni1 C6 39.16(13) . . ?
C8 Ni1 C6 65.42(18) . . ?
C8 Ni1 C6 56.24(19) 8_565 . ?
C7 Ni1 C6 39.16(15) 8_565 8_565 ?
C7 Ni1 C6 19.6(3) . 8_565 ?
C8 Ni1 C6 56.2(2) . 8_565 ?
C8 Ni1 C6 65.4(3) 8_565 8_565 ?
C6 Ni1 C6 22.9(3) . 8_565 ?
C7 Ni1 S1 110.54(11) 8_565 . ?
C7 Ni1 S1 110.5(3) . . ?
C8 Ni1 S1 148.5(3) . . ?
C8 Ni1 S1 148.52(16) 8_565 . ?
C6 Ni1 S1 97.53(13) . . ?
C6 Ni1 S1 97.5(2) 8_565 . ?
C7 Ni1 S2 143.48(15) 8_565 . ?
C7 Ni1 S2 143.5(2) . . ?
C8 Ni1 S2 108.11(19) . . ?
C8 Ni1 S2 108.11(18) 8_565 . ?
C6 Ni1 S2 163.06(12) . . ?
C6 Ni1 S2 163.1(2) 8_565 . ?
S1 Ni1 S2 94.90(4) . . ?
C7 Ni1 C4 65.2(2) 8_565 8_565 ?
C7 Ni1 C4 48.1(4) . 8_565 ?
C8 Ni1 C4 8.5(5) . 8_565 ?
C8 Ni1 C4 38.71(14) 8_565 8_565 ?
C6 Ni1 C4 71.39(16) . 8_565 ?
C6 Ni1 C4 64.1(3) 8_565 8_565 ?
S1 Ni1 C4 156.6(3) . 8_565 ?
S2 Ni1 C4 100.70(17) . 8_565 ?
C7 Ni1 C4 48.08(19) 8_565 . ?
C7 Ni1 C4 65.21(17) . . ?
C8 Ni1 C4 38.71(12) . . ?
C8 Ni1 C4 8.5(3) 8_565 . ?
C6 Ni1 C4 64.1(2) . . ?
C6 Ni1 C4 71.39(16) 8_565 . ?
S1 Ni1 C4 156.6(3) . . ?
S2 Ni1 C4 100.70(17) . . ?
C4 Ni1 C4 34.4(7) 8_565 . ?
C7 Ni1 C5 64.7(3) 8_565 8_565 ?
C7 Ni1 C5 18.5(3) . 8_565 ?
C8 Ni1 C5 29.7(3) . 8_565 ?
C8 Ni1 C5 64.4(3) 8_565 8_565 ?
C6 Ni1 C5 57.1(4) . 8_565 ?
C6 Ni1 C5 38.0(2) 8_565 8_565 ?
S1 Ni1 C5 118.9(3) . 8_565 ?
S2 Ni1 C5 125.2(4) . 8_565 ?
C4 Ni1 C5 37.8(5) 8_565 8_565 ?
C4 Ni1 C5 64.9(3) . 8_565 ?
C7 Ni1 C5 18.54(18) 8_565 . ?
C7 Ni1 C5 64.69(19) . . ?
C8 Ni1 C5 64.4(2) . . ?
C8 Ni1 C5 29.7(3) 8_565 . ?
C6 Ni1 C5 38.02(14) . . ?
C6 Ni1 C5 57.1(2) 8_565 . ?
S1 Ni1 C5 118.9(2) . . ?
S2 Ni1 C5 125.18(12) . . ?
C4 Ni1 C5 64.9(5) 8_565 . ?
C4 Ni1 C5 37.79(17) . . ?
C5 Ni1 C5 76.5(4) 8_565 . ?
C2 S2 Ni1 100.81(11) . . ?
C2 S4 C3 96.63(16) . . ?
C1 S1 Ni1 100.84(11) . . ?
C1 S3 C3 96.06(17) . . ?
C2 C1 S1 122.1(3) . . ?
C2 C1 S3 117.5(2) . . ?
S1 C1 S3 120.39(19) . . ?
C1 C2 S2 121.3(3) . . ?
C1 C2 S4 117.1(2) . . ?
S2 C2 S4 121.63(19) . . ?
O1 C3 S4 124.2(3) . . ?
O1 C3 S3 123.0(3) . . ?
S4 C3 S3 112.78(19) . . ?
C5 C4 C8 108 . . ?
C5 C4 Ni1 72.2(2) . . ?
C8 C4 Ni1 67.7(4) . . ?
C4 C5 C6 108 . . ?
C4 C5 Ni1 70.00(16) . . ?
C6 C5 Ni1 68.8(3) . . ?
C7 C6 C5 108 . . ?
C7 C6 Ni1 67.9(3) . . ?
C5 C6 Ni1 73.2(4) . . ?
C8 C7 C6 108 . . ?
C8 C7 Ni1 70.8(2) . . ?
C6 C7 Ni1 72.9(3) . . ?
C7 C8 C4 108 . . ?
C7 C8 Ni1 69.5(3) . . ?
C4 C8 Ni1 73.6(4) . . ?
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
Ni1 C7 2.038(4) 8_565 ?
Ni1 C7 2.038(9) . ?
Ni1 C8 2.055(6) . ?
Ni1 C8 2.055(9) 8_565 ?
Ni1 C6 2.103(4) . ?
Ni1 C6 2.103(8) 8_565 ?
Ni1 S1 2.1379(10) . ?
Ni1 S2 2.1453(10) . ?
Ni1 C4 2.130(6) 8_565 ?
Ni1 C4 2.130(6) . ?
Ni1 C5 2.159(12) 8_565 ?
Ni1 C5 2.159(8) . ?
S2 C2 1.718(3) . ?
S4 C2 1.740(3) . ?
S4 C3 1.770(4) . ?
S1 C1 1.712(3) . ?
S3 C1 1.749(3) . ?
S3 C3 1.773(4) . ?
O1 C3 1.200(4) . ?
C1 C2 1.352(4) . ?
C4 C5 1.389(4) . ?
C4 C8 1.389(4) . ?
C5 C6 1.389(4) . ?
C6 C7 1.389(4) . ?
C7 C8 1.389(4) . ?
