#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008183.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_7008183
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_sum            'C8 H5 Ni S3 Se2'
_chemical_formula_weight         413.93
_chemical_name_common            CpNi(dsit)
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0750(12)
_cell_length_b                   7.9798(11)
_cell_length_c                   11.8369(19)
_cell_measurement_reflns_used    3386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      1.70
_cell_volume                     568.85(17)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       'Oscillation, phi incr. 2 deg.'
_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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4282
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    8.607
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_correction_T_min  0.1444
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.0076
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2090
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0283P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                1475
_reflns_number_total             2090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418756n.txt
_cod_data_source_block           mf344fac
_cod_original_cell_volume        568.85(16)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7008183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni -0.06424(18) 0.69392(15) 0.73183(9) 0.0328(3) Uani 1 1 d . . .
Se1 Se 0.06801(15) 0.77625(14) 0.57184(8) 0.0392(3) Uani 1 1 d . . .
Se2 Se -0.38571(15) 0.58984(14) 0.64348(8) 0.0407(3) Uani 1 1 d . . .
S1 S -0.1705(4) 0.7589(3) 0.3204(2) 0.0384(6) Uani 1 1 d . . .
S2 S -0.5665(4) 0.6020(4) 0.3806(2) 0.0408(6) Uani 1 1 d . . .
S3 S -0.5423(4) 0.6870(4) 0.1366(2) 0.0536(7) Uani 1 1 d . . .
C1 C -0.1736(13) 0.7223(11) 0.4643(7) 0.029(2) Uani 1 1 d . . .
C2 C -0.3615(15) 0.6507(11) 0.4930(8) 0.030(2) Uani 1 1 d . . .
C3 C -0.4299(15) 0.6843(14) 0.2743(8) 0.039(2) Uani 1 1 d . . .
C4 C 0.1973(18) 0.777(2) 0.8494(9) 0.058(3) Uani 1 1 d . . .
H4 H 0.3249 0.8276 0.8299 0.069 Uiso 1 1 calc R . .
C5 C 0.1796(19) 0.6081(19) 0.8623(9) 0.056(3) Uani 1 1 d . . .
H5 H 0.2883 0.5288 0.8535 0.067 Uiso 1 1 calc R . .
C6 C -0.028(3) 0.577(3) 0.8906(10) 0.107(7) Uani 1 1 d . . .
H6 H -0.0915 0.4734 0.9038 0.128 Uiso 1 1 calc R . .
C7 C -0.130(2) 0.747(3) 0.8951(9) 0.089(6) Uani 1 1 d . . .
H7 H -0.2711 0.7701 0.9141 0.107 Uiso 1 1 calc R . .
C8 C 0.018(3) 0.8633(19) 0.8669(11) 0.073(4) Uani 1 1 d . . .
H8 H -0.0022 0.9787 0.8611 0.088 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0347(6) 0.0418(7) 0.0210(7) -0.0028(6) -0.0004(5) -0.0002(6)
Se1 0.0321(5) 0.0565(6) 0.0280(6) 0.0021(5) 0.0000(4) -0.0116(5)
Se2 0.0378(5) 0.0577(6) 0.0264(5) 0.0059(5) 0.0037(4) -0.0123(5)
S1 0.0394(12) 0.0511(16) 0.0249(13) 0.0053(13) 0.0053(10) -0.0062(13)
S2 0.0391(12) 0.0527(17) 0.0286(14) -0.0025(14) -0.0025(10) -0.0108(14)
S3 0.0623(16) 0.0700(18) 0.0250(14) 0.0015(15) -0.0069(12) -0.0032(16)
C1 0.030(4) 0.031(6) 0.025(5) 0.003(4) 0.001(4) 0.004(4)
C2 0.038(5) 0.037(6) 0.014(4) 0.000(4) 0.004(4) -0.001(4)
C3 0.047(5) 0.040(5) 0.030(5) -0.006(5) 0.001(4) 0.010(5)
C4 0.045(6) 0.090(10) 0.033(6) 0.002(8) -0.014(5) -0.012(8)
C5 0.069(7) 0.056(8) 0.036(6) 0.006(7) -0.015(6) 0.014(7)
C6 0.168(18) 0.122(15) 0.022(7) 0.019(9) -0.021(9) -0.091(15)
C7 0.055(7) 0.20(2) 0.012(5) -0.014(9) 0.008(5) 0.017(11)
C8 0.088(10) 0.082(10) 0.043(8) -0.018(7) -0.022(7) 0.021(9)
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'
Ni Ni 0.3393 1.1124 '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'
Se Se -0.0929 2.2259 '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 Ni C4 62.2(5) . . ?
C7 Ni C6 42.3(6) . . ?
C4 Ni C6 63.9(5) . . ?
C7 Ni C8 38.1(6) . . ?
C4 Ni C8 37.1(5) . . ?
C6 Ni C8 67.5(6) . . ?
C7 Ni C5 65.6(5) . . ?
C4 Ni C5 37.9(4) . . ?
C6 Ni C5 38.2(5) . . ?
C8 Ni C5 65.1(5) . . ?
C7 Ni Se2 104.3(4) . . ?
C4 Ni Se2 165.8(3) . . ?
C6 Ni Se2 103.6(4) . . ?
C8 Ni Se2 134.1(4) . . ?
C5 Ni Se2 134.7(4) . . ?
C7 Ni Se1 149.4(7) . . ?
C4 Ni Se1 98.3(3) . . ?
C6 Ni Se1 152.0(6) . . ?
C8 Ni Se1 112.1(5) . . ?
C5 Ni Se1 114.6(4) . . ?
Se2 Ni Se1 95.78(5) . . ?
C1 Se1 Ni 99.9(3) . . ?
C2 Se2 Ni 100.1(3) . . ?
C3 S1 C1 97.3(4) . . ?
C3 S2 C2 96.2(4) . . ?
C2 C1 S1 115.8(7) . . ?
C2 C1 Se1 122.6(7) . . ?
S1 C1 Se1 121.6(5) . . ?
C1 C2 S2 116.2(7) . . ?
C1 C2 Se2 121.4(7) . . ?
S2 C2 Se2 122.1(5) . . ?
S3 C3 S1 123.1(6) . . ?
S3 C3 S2 122.6(6) . . ?
S1 C3 S2 114.3(5) . . ?
C8 C4 C5 114.7(13) . . ?
C8 C4 Ni 72.5(7) . . ?
C5 C4 Ni 72.3(7) . . ?
C4 C5 C6 107.3(14) . . ?
C4 C5 Ni 69.8(7) . . ?
C6 C5 Ni 70.0(7) . . ?
C5 C6 C7 103.9(13) . . ?
C5 C6 Ni 71.8(7) . . ?
C7 C6 Ni 68.3(7) . . ?
C8 C7 C6 108.6(12) . . ?
C8 C7 Ni 72.3(7) . . ?
C6 C7 Ni 69.4(7) . . ?
C4 C8 C7 105.5(15) . . ?
C4 C8 Ni 70.4(7) . . ?
C7 C8 Ni 69.6(8) . . ?
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
Ni C7 2.070(11) . ?
Ni C4 2.078(11) . ?
Ni C6 2.085(13) . ?
Ni C8 2.103(13) . ?
Ni C5 2.109(10) . ?
Ni Se2 2.2496(15) . ?
Ni Se1 2.2502(15) . ?
Se1 C1 1.862(8) . ?
Se2 C2 1.871(9) . ?
S1 C3 1.706(10) . ?
S1 C1 1.731(9) . ?
S2 C3 1.726(10) . ?
S2 C2 1.743(9) . ?
S3 C3 1.683(10) . ?
C1 C2 1.360(11) . ?
C4 C8 1.329(17) . ?
C4 C5 1.361(16) . ?
C5 C6 1.372(19) . ?
C6 C7 1.50(2) . ?
C7 C8 1.36(2) . ?
