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_4335866
_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 Dy6 F24 N4 O36 P12 S16'
_chemical_formula_weight         3474.41
_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                 100.879(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.8740(10)
_cell_length_b                   26.4810(10)
_cell_length_c                   14.6840(10)
_cell_measurement_reflns_used    13867
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_cell_volume                     13698.8(12)
_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_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 0.982
_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
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13941
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.703
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       stick
_exptl_crystal_F_000             6600
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Last refinements revealed several electronicp eaks per unit cell corresponding
to disordered CH2Cl2 molecules. These disordered solvents were removed using
SQUEEZE process. Formula is given considering none of these these molecules. 
;
_refine_diff_density_max         1.606
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         13941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                8050
_reflns_number_total             13941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012839_si_002_1.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        13698.8(11)
_cod_database_code               4335866