Tris(tetrahydrofuran-κ<i>O</i>)tris[tris(thiophen-2-yl)methanolato-κ<i>O</i>]terbium(III) tetrahydrofuran monosolvate
Veith, Michael; Belot, Celine; Huch, Volker; Acta Crystallographica Section E 67 (2011) m1712–; doi:10.1107/S160053681104623X

data_2232871
_publ_section_title
;
 Tris(tetrahydrofuran-\k<i>O</i>)tris[tris(thiophen-2-yl)methanolato-\k<i>O</i>]terbium(III)
 tetrahydrofuran monosolvate
;
_journal_coeditor_code           NC2251
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1712
_journal_paper_doi               10.1107/S160053681104623X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Tb (C13 H9 O S3)3 (C4 H8 O)3], C4 H8 O'
_chemical_formula_moiety         'C51 H51 O6 S9 Tb, C4 H8 O'
_chemical_formula_sum            'C55 H59 O7 S9 Tb'
_chemical_formula_weight         1279.48
_chemical_name_systematic
;
Tris(tetrahydrofuran-\k<i>O</i>)tris[tris(thiophen-2-yl)methanolato-
\k<i>O</i>]terbium(III) tetrahydrofuran monosolvate
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.9131(4)
_cell_length_b                   13.9131(4)
_cell_length_c                   24.6789(7)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      31.97
_cell_measurement_theta_min      2.93
_cell_volume                     4137.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      132(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            28927
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  0.6934
_exptl_absorpt_correction_T_min  0.5927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.630
_refine_ls_abs_structure_details 'Flack (1983), 3011 Friedel pairs'
_refine_ls_abs_structure_Flack   0.089(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6212
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                6197
_reflns_number_total             6212
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nc2251.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2232871
_cod_database_fobs_code          2232871