Difluorodioxophosphate-Based Hollow Hexanuclear Lanthanide(III) Clusters Decorated with Tetrathiafulvalene Ligands
Tamyris T. da Cunha; Fabrice Pointillart; Boris Le Guennic; Cynthia L. M. Pereira; Stéphane Golhen; Olivier Cador; Lahcène Ouahab; Inorganic Chemistry 52 (2013) 9711–9713; doi:10.1021/ic4012839

data_4335867
_publ_section_title
;
 Difluorodioxophosphate-Based Hollow Hexanuclear Lanthanide(III) Clusters
 Decorated with Tetrathiafulvalene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9711
_journal_page_last               9713
_journal_paper_doi               10.1021/ic4012839
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C40 H46 F24 N4 O36 P12 S16 Yb6'
_chemical_formula_weight         3537.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.895(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.7804(17)
_cell_length_b                   26.4651(12)
_cell_length_c                   14.4391(7)
_cell_measurement_reflns_used    5316
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      2.55
_cell_volume                     13379.2(11)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0916
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57618
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    4.634
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       stick
_exptl_crystal_F_000             6696
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Last refinements revealed one CH2Cl2 molecule and several electronic
peaks per unit cell. These disordered solvents were removed using SQUEEZE
process. Formula is given considering none of these these molecules.
;
_refine_diff_density_max         2.159
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.462
_refine_ls_extinction_coef       0.000461(19)
_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   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         15350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0808P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                7111
_reflns_number_total             15350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012839_si_002_2.cif
_cod_data_source_block           shelxl
_cod_database_code               4335867