Solution versus Solid-State Structure of Ytterbium Heterobimetallic Catalysts
Lorenzo Di Bari; Moreno Lelli; Guido Pintacuda; Gennaro Pescitelli; Fabio Marchetti; Piero Salvadori; Journal of the American Chemical Society 125 (2003) 5549–5558; doi:10.1021/ja0297640

data_4113713
_publ_section_title
;
 Solution versus Solid-State Structure of Ytterbium Heterobimetallic
 Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5549
_journal_page_last               5558
_journal_paper_doi               10.1021/ja0297640
_journal_volume                  125
_journal_year                    2003
_chemical_formula_iupac          'Yb Na3 (C20 H12 O2)3.6(C4 H8 O)'
_chemical_formula_moiety         'C84 H84 Na3 O12 Yb'
_chemical_formula_sum            'C84 H84 Na3 O12 Yb'
_chemical_formula_weight         1527.52
_chemical_name_systematic
;
 Ytterbium(iii)trisodiumtris-(S)-1,1'-bis(2-naphtoate) tetrahydrofurane solvate
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-02-16T19:54:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.2860(10)
_cell_length_b                   15.2860(10)
_cell_length_c                   18.709(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.06
_cell_measurement_theta_min      7.54
_cell_volume                     3785.9(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WINGX-1.64 (Farrugia, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5672
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.18
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_T_max  0.7956
_exptl_absorpt_correction_T_min  0.7360
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker AXS SHELXTL VER.5.1 (1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.34
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2459
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                1604
_reflns_number_total             2459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0297640si20030207_054057.cif
_cod_data_source_block           ybnaf
_cod_database_code               4113713