Stabilization of Unsolvated Europium and Ytterbium Pentafluorophenyls by π-Bonding Encapsulation through a Sterically Crowded Triazenido Ligand
Sven-Oliver Hauber; Mark Niemeyer; Inorganic Chemistry 44 (2005) 8644–8646; doi:10.1021/ic0514602

data_4310131
_publ_contact_author_address
;
Institut f\"ur Anorganische Chemie
Universit\"at Stuttgart
Pfaffenwaldring 55
D-70569 Stuttgart
Germany
;
_publ_contact_author_email       niemeyer@iac.uni-stuttgart.de
_publ_contact_author_name        'Mark Niemeyer'
_publ_section_title
;
Stabilization of Unsolvated Europium and Ytterbium Pentafluorophenyls by
\p-Bonding Encapsulation through a Sterically Crowded Triazenido Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8644
_journal_page_last               8646
_journal_paper_doi               10.1021/ic0514602
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C51 H52 F5 N3 Yb'
_chemical_formula_weight         975.00
_chemical_melting_point          '80-165deg.C (dec.)'
_chemical_name_systematic
;
((1-(2',4',6'-triisopropylbiphenyl-2))
(3-(2,4,6,2'',4'',6''-hexamethyl-1,1':3';1''-terphenyl-2'))
(triazenido-N,N'))(pentafluorophenyl)ytterbium(II)
;
_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                96.91(3)
_cell_angle_beta                 93.71(3)
_cell_angle_gamma                106.93(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0770(18)
_cell_length_b                   11.114(2)
_cell_length_c                   23.416(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2231.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Siemens P3'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10167
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        '< 0.5%'
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                7365
_reflns_number_total             9552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0514602si20050826_114842_2.cif
_cod_data_source_block           3
_cod_original_cell_volume        2231.0(8)
_cod_database_code               4310131