#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:22:36 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 180075 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/21/7052160.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_7052160
loop_
_publ_author_name
'Mitsushiro Nomura'
'Marc Fourmigué'
_publ_section_title
;
 The contrasted structural and magnetic behaviour of two
 single-component paramagnetic dithiolene complexes
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              528
_journal_paper_doi               10.1039/b700278e
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety         CpNi(bddt)
_chemical_formula_sum            'C11 H13 Ni S4'
_chemical_formula_weight         332.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.406(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5803(12)
_cell_length_b                   11.9991(15)
_cell_length_c                   12.9458(18)
_cell_measurement_reflns_used    4012
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.85
_cell_volume                     1331.7(3)
_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 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, phi. incr. 1.8'
_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  0.1253
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10111
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_T_max  0.8128
_exptl_absorpt_correction_T_min  0.7308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0454
_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)+(0.0303P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                1330
_reflns_number_total             2413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700278e.txt
_cod_data_source_block           mn165abs
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7052160
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ni1 Ni 0.13928(8) 0.82079(5) 0.86837(6) 0.0416(2) Uani 1 1 d . . .
S1 S -0.01953(17) 0.77575(12) 0.98361(11) 0.0454(4) Uani 1 1 d . . .
S2 S 0.00892(17) 0.73300(12) 0.75124(12) 0.0448(4) Uani 1 1 d . . .
S3 S -0.31645(17) 0.65132(12) 0.99024(12) 0.0482(4) Uani 1 1 d . . .
S4 S -0.29884(17) 0.62027(11) 0.73427(12) 0.0452(4) Uani 1 1 d . . .
C1 C -0.1641(6) 0.7016(4) 0.9152(4) 0.0387(13) Uani 1 1 d . . .
C2 C -0.1545(6) 0.6863(4) 0.8134(4) 0.0389(13) Uani 1 1 d . . .
C3 C -0.2720(7) 0.5044(4) 1.0063(4) 0.0481(15) Uani 1 1 d . . .
H3A H -0.1640 0.4983 1.0309 0.058 Uiso 1 1 calc R . .
H3B H -0.3356 0.4758 1.0605 0.058 Uiso 1 1 calc R . .
C4 C -0.2949(7) 0.4287(4) 0.9131(5) 0.0508(16) Uani 1 1 d . . .
H4A H -0.3027 0.3527 0.9380 0.061 Uiso 1 1 calc R . .
H4B H -0.3942 0.4473 0.8788 0.061 Uiso 1 1 calc R . .
C5 C -0.1714(7) 0.4315(4) 0.8331(4) 0.0446(15) Uani 1 1 d . . .
H5A H -0.0834 0.4744 0.8608 0.053 Uiso 1 1 calc R . .
H5B H -0.1352 0.3559 0.8224 0.053 Uiso 1 1 calc R . .
C6 C -0.2215(7) 0.4799(4) 0.7292(4) 0.0452(15) Uani 1 1 d . . .
H6A H -0.3004 0.4317 0.6971 0.054 Uiso 1 1 calc R . .
H6B H -0.1326 0.4799 0.6853 0.054 Uiso 1 1 calc R . .
C7 C 0.2563(8) 0.9637(6) 0.9264(7) 0.072(2) Uani 1 1 d . . .
H7 H 0.2157 1.0121 0.9746 0.086 Uiso 1 1 calc R . .
C8 C 0.2380(8) 0.9733(6) 0.8207(8) 0.076(2) Uani 1 1 d . . .
H8 H 0.1860 1.0304 0.7849 0.091 Uiso 1 1 calc R . .
C9 C 0.3106(8) 0.8831(7) 0.7770(5) 0.071(2) Uani 1 1 d . . .
H9 H 0.3111 0.8669 0.7068 0.085 Uiso 1 1 calc R . .
C10 C 0.3845(6) 0.8193(5) 0.8576(5) 0.0525(16) Uani 1 1 d . . .
H10 H 0.4464 0.7565 0.8500 0.063 Uiso 1 1 calc R . .
C11 C 0.3463(7) 0.8690(5) 0.9494(5) 0.0607(19) Uani 1 1 d . . .
H11 H 0.3755 0.8437 1.0153 0.073 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'
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'
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
C9 Ni1 C11 65.2(3) . . ?
C9 Ni1 C7 64.5(3) . . ?
C11 Ni1 C7 38.8(2) . . ?
C9 Ni1 C10 39.7(2) . . ?
C11 Ni1 C10 38.2(2) . . ?
C7 Ni1 C10 64.5(3) . . ?
C9 Ni1 C8 38.5(3) . . ?
C11 Ni1 C8 64.5(3) . . ?
C7 Ni1 C8 38.0(3) . . ?
C10 Ni1 C8 65.0(3) . . ?
C9 Ni1 S2 97.9(2) . . ?
C11 Ni1 S2 154.0(2) . . ?
C7 Ni1 S2 152.3(2) . . ?
C10 Ni1 S2 116.37(19) . . ?
C8 Ni1 S2 115.1(3) . . ?
C9 Ni1 S1 169.7(2) . . ?
C11 Ni1 S1 105.8(2) . . ?
C7 Ni1 S1 105.4(2) . . ?
C10 Ni1 S1 135.32(18) . . ?
C8 Ni1 S1 134.2(3) . . ?
S2 Ni1 S1 92.34(6) . . ?
C1 S1 Ni1 103.7(2) . . ?
C2 S2 Ni1 103.90(19) . . ?
C1 S3 C3 103.8(3) . . ?
C2 S4 C6 100.9(2) . . ?
C2 C1 S1 120.1(4) . . ?
C2 C1 S3 124.9(4) . . ?
S1 C1 S3 115.0(3) . . ?
C1 C2 S2 119.7(4) . . ?
C1 C2 S4 124.4(4) . . ?
S2 C2 S4 115.9(3) . . ?
C4 C3 S3 118.2(4) . . ?
C5 C4 C3 117.4(5) . . ?
C6 C5 C4 115.9(5) . . ?
C5 C6 S4 114.6(4) . . ?
C8 C7 C11 108.5(7) . . ?
C8 C7 Ni1 71.4(4) . . ?
C11 C7 Ni1 70.4(3) . . ?
C7 C8 C9 107.9(6) . . ?
C7 C8 Ni1 70.6(4) . . ?
C9 C8 Ni1 68.6(4) . . ?
C8 C9 C10 108.5(7) . . ?
C8 C9 Ni1 72.9(4) . . ?
C10 C9 Ni1 72.0(4) . . ?
C11 C10 C9 106.5(6) . . ?
C11 C10 Ni1 70.5(3) . . ?
C9 C10 Ni1 68.3(3) . . ?
C10 C11 C7 108.5(6) . . ?
C10 C11 Ni1 71.3(3) . . ?
C7 C11 Ni1 70.8(3) . . ?
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 C9 2.065(7) . ?
Ni1 C11 2.105(6) . ?
Ni1 C7 2.110(6) . ?
Ni1 C10 2.114(5) . ?
Ni1 C8 2.120(6) . ?
Ni1 S2 2.1255(16) . ?
Ni1 S1 2.1320(18) . ?
S1 C1 1.738(5) . ?
S2 C2 1.739(6) . ?
S3 C1 1.768(6) . ?
S3 C3 1.813(5) . ?
S4 C2 1.762(5) . ?
S4 C6 1.813(5) . ?
C1 C2 1.337(7) . ?
C3 C4 1.516(7) . ?
C4 C5 1.513(8) . ?
C5 C6 1.511(7) . ?
C7 C8 1.376(10) . ?
C7 C11 1.399(9) . ?
C8 C9 1.381(10) . ?
C9 C10 1.422(8) . ?
C10 C11 1.381(8) . ?
