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_4310080
_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           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-11-15T12:35:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 107.370(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   19.953(5)
_cell_length_b                   9.397(5)
_cell_length_c                   28.325(5)
_cell_measurement_reflns_used    32148
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     5069(3)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      -0.292526E-1
_diffrn_orient_matrix_UB_12      0.568957E-1
_diffrn_orient_matrix_UB_13      0.162845E-1
_diffrn_orient_matrix_UB_21      -0.425905E-1
_diffrn_orient_matrix_UB_22      -0.547906E-1
_diffrn_orient_matrix_UB_23      -0.187635E-1
_diffrn_orient_matrix_UB_31      0.93836E-2
_diffrn_orient_matrix_UB_32      -0.713173E-1
_diffrn_orient_matrix_UB_33      0.274069E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30277
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.8848
_exptl_absorpt_correction_T_min  0.7093
_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    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+4.7547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                4303
_reflns_number_total             5815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051017rsi20050622_054911.cif
_cod_data_source_block           acacni2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4310080