Between Ni(mnt)2 and Ni(tfd)2i Dithiolene Complexes: the Unsymmetrical 2-(Trifluoromethyl)acrylonitrile-1,2-dithiolate and Its Nickel Complexes
Olivier Jeannin; Jacques Delaunay; Frédéric Barrière; Marc Fourmigué; Inorganic Chemistry 44 (2005) 9763–9770; doi:10.1021/ic051226b

data_4310241
_publ_section_title
;
Between Ni(mnt)2 and Ni(tfd)2i Dithiolene Complexes: the Unsymmetrical
2-(Trifluoromethyl)acrylonitrile-1,2-dithiolate and Its Nickel Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9763
_journal_page_last               9770
_journal_paper_doi               10.1021/ic051226b
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C24 H36 F6 N3 Ni S4'
_chemical_formula_weight         667.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.175(5)
_cell_length_b                   8.6412(17)
_cell_length_c                   16.091(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      1.75
_cell_volume                     3117.8(13)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1.5 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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14649
_diffrn_reflns_theta_full        25.78
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.7694
_exptl_absorpt_correction_T_min  0.6864
_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    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0441
_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/[\s^2^(Fo^2^)+(0.0768P)^2^+4.4429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                2261
_reflns_number_total             2876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051226bsi20050722_112444_4.cif
_cod_data_source_block           oj109
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3117.8(11)
_cod_database_code               4310241