4-(2-Tetrathiafulvalenyl-ethenyl)pyridine (TTF-CH=CH-Py) Radical Cation Salts Containing Poly(β-diketonate) Rare Earth Complexes: Synthesis, Crystal Structure, Photoluminescent and Magnetic Properties
Fabrice Pointillart; Olivier Maury; Yann Le Gal; Stéphane Golhen; Olivier Cador; Lahcène Ouahab; Inorganic Chemistry 48 (2009) 7421–7429; doi:10.1021/ic901052b

data_4302881
_publ_contact_author_address
;Organom\'etalliques et Mat\'eriaux Mol\'eculaires
UMR 6226 CNRS-UR1 Sciences Chimiques de Rennes
Universit\'e de Rennes 1
35042, Rennes Cedex
France
;
_publ_contact_author_email       lacene.ouahab@univ-rennes1.fr
_publ_contact_author_fax         '+33(0)2 23 23 68 40'
_publ_contact_author_name        Ouahab
_publ_contact_author_phone       '+33(0)2 23 23 56 59'
_publ_section_title
;
4-(2-Tetrathiafulvalenyl-ethenyl)pyridine (TTF-CH=CH-Py) Radical
Cation Salts Containing Poly(\b-diketonate) Rare Earth Complexes:
Synthesis, Crystal Structure, Photoluminescent and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7421
_journal_page_last               7429
_journal_paper_doi               10.1021/ic901052b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C69 H39 F48 N2 Nd2 O19 S8'
_chemical_formula_weight         2656.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.3420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9926(3)
_cell_length_b                   12.1328(2)
_cell_length_c                   34.3105(4)
_cell_measurement_reflns_used    22706
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     9985.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare al, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            43330
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         22776
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1711
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2523
_reflns_number_gt                10476
_reflns_number_total             22776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901052b_si_002_1.cif
_cod_data_source_block           3
_cod_database_code               4302881