Electroactive Ligands: The First Metal Complexes of Tetrathiafulvenyl-Acetylacetonate
Julien Massue; Nathalie Bellec; Stéphanie Chopin; Eric Levillain; Thierry Roisnel; Rodolphe Clérac; Dominique Lorcy; Inorganic Chemistry 44 (2005) 8740–8748; doi:10.1021/ic051017r

data_4310083
_publ_section_title
;
Electroactive Ligands: The First Metal Complexes of
Tetrathiafulvenyl-Acetylacetonate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8740
_journal_page_last               8748
_journal_paper_doi               10.1021/ic051017r
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H40 N2 Ni1 O4 S16'
_chemical_formula_sum            'C38 H40 N2 Ni O4 S16'
_chemical_formula_weight         1160.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-08-30T11:54:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.220(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.883(5)
_cell_length_b                   23.837(5)
_cell_length_c                   12.395(5)
_cell_measurement_reflns_used    32424
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     2912(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.311636E-1
_diffrn_orient_matrix_UB_12      0.283414E-1
_diffrn_orient_matrix_UB_13      0.522457E-1
_diffrn_orient_matrix_UB_21      -0.410959E-1
_diffrn_orient_matrix_UB_22      0.228441E-1
_diffrn_orient_matrix_UB_23      -0.616642E-1
_diffrn_orient_matrix_UB_31      -0.873745E-1
_diffrn_orient_matrix_UB_32      -0.20853E-1
_diffrn_orient_matrix_UB_33      0.34552E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33137
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  1.0483
_exptl_absorpt_correction_T_min  0.6592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0042(10)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.072
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+2.4999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                4911
_reflns_number_total             6553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051017rsi20050830_120707.cif
_cod_data_source_block           c19
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4310083