Accessing Decaphenylmetallocenes of Ytterbium, Calcium, and Barium by Desolvation of Solvent-Separated Ion Pairs: Overcoming Adverse Solubility Properties#
Deacon, Glen B.; Forsyth, Craig M.; Jaroschik, Florian; Junk, Peter C.; Kay, Danielle L.; Maschmeyer, Thomas; Masters, Anthony F.; Wang, Jun; Field, Leslie D.; Organometallics 27 (2008) 4772–; doi:10.1021/om800501z

data_4071984
_publ_section_title
;
 Accessing Decaphenylmetallocenes of Ytterbium, Calcium, and Barium by
 Desolvation of Solvent-Separated Ion Pairs: Overcoming Adverse Solubility
 Properties#
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4772
_journal_paper_doi               10.1021/om800501z
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         '2(C24 H48 O6 Yb), 4(C35 H25), 7(C4 H8 O)'
_chemical_formula_sum            'C216 H252 O19 Yb2'
_chemical_formula_weight         3498.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.845(1)
_cell_angle_beta                 75.352(1)
_cell_angle_gamma                88.167(1)
_cell_formula_units_Z            1
_cell_length_a                   14.1148(2)
_cell_length_b                   14.1430(2)
_cell_length_c                   24.0136(6)
_cell_measurement_temperature    123(2)
_cell_volume                     4564.87(15)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KAPPA CCD'
_diffrn_measurement_method       'phi and omega 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  0.0968
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50345
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         15873
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                11479
_reflns_number_total             15873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800501z_si_004.cif
_cod_data_source_block           ybph52ab
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4071984