Perylene salts of unsymmetrical nickel and gold dithiolene complexes with 3 ∶ 2 stoichiometry: conformational polymorphism and strong antiferromagnetic interactions
Olivier Jeannin; Marc Fourmigué; New Journal of Chemistry 30 (2006) 1774–; doi:10.1039/b608420f

data_7052368
_publ_section_title
;
 Perylene salts of unsymmetrical nickel and gold dithiolene complexes
 with 3 &#x2236; 2 stoichiometry: conformational polymorphism and
 strong antiferromagnetic interactions
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1774
_journal_paper_doi               10.1039/b608420f
_journal_volume                  30
_journal_year                    2006
_chemical_formula_moiety         '1.5(C20 H12), C8 F6 N2 Ni S4'
_chemical_formula_sum            'C38 H18 F6 N2 Ni S4'
_chemical_formula_weight         803.49
_chemical_name_common            (perylene)1.5,[Ni(tfadt)2]
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.253(13)
_cell_angle_beta                 103.614(14)
_cell_angle_gamma                94.149(14)
_cell_formula_units_Z            2
_cell_length_a                   10.8853(14)
_cell_length_b                   12.6566(14)
_cell_length_c                   13.1882(16)
_cell_measurement_reflns_used    6536
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      1.8
_cell_volume                     1594.4(4)
_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 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Rotation, phi incr. 1.8 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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15531
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.9650
_exptl_absorpt_correction_T_min  0.6801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of 8 x 8 x 8 = 512 sampling points was used
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         5735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                2597
_reflns_number_total             5735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608420f.txt
_cod_data_source_block           ojec111
_cod_original_cell_volume        1594.4(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052368
_exptl_absorpt_correction_t_ave  0.9137