4f Gadolinium(III) Complex Involving Tetrathiafulvalene-amido-2-pyrimidine-1-oxide as a Ligand
Fabrice Pointillart; Yann Le Gal; Stéphane Golhen; Olivier Cador; Lahcène Ouahab; Inorganic Chemistry 48 (2009) 4631–4633; doi:10.1021/ic9003966

data_4302244
_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       lahcene.ouahab@univ-rennes1.fr
_publ_contact_author_fax         '+33 2 23 23 68 40'
_publ_contact_author_name        'Lahc\`ene Ouahab'
_publ_contact_author_phone       '+33 2 23 23 56 59'
_publ_section_title
;
4f Gadolinium(III) Complex Involving
Tetrathiafulvalene-amido-2-pyrimidine-1-oxide as a Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4631
_journal_page_last               4633
_journal_paper_doi               10.1021/ic9003966
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'[Gd(C5 O2 F6 H)3(C11 N3 O2 S4 H7)3] (CH2Cl2) 0.5(C6H14)'
_chemical_formula_sum            'C52 H33 Cl2 F18 Gd N9 O12 S12'
_chemical_formula_weight         1930.74
_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                 107.297(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.066(5)
_cell_length_b                   14.879(5)
_cell_length_c                   26.377(5)
_cell_measurement_reflns_used    24793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      0.998
_cell_volume                     7519(3)
_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    'SIR97 (Altomare al, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_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
_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  0.1411
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48390
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         15951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.2021
_refine_ls_R_factor_gt           0.0981
_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^)+(0.0848P)^2^+28.2440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2505
_reflns_number_gt                7673
_reflns_number_total             15951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003966_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302244