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_4310130
_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 Eu F5 N3'
_chemical_formula_weight         953.92
_chemical_melting_point          '80-120deg.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)europium(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                96.206(16)
_cell_angle_beta                 93.326(17)
_cell_angle_gamma                106.806(19)
_cell_formula_units_Z            2
_cell_length_a                   9.043(2)
_cell_length_b                   11.166(3)
_cell_length_c                   23.368(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2235.6(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10905
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        <1.5%
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.5004
_exptl_absorpt_correction_T_min  0.4278
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'deep orange'
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.55
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.376
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         10256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.376
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                9558
_reflns_number_total             10256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0514602si20050826_114842_1.cif
_cod_data_source_block           2
_cod_database_code               4310130