Yb(II) Triple-Decker Complex with the μ-Bridging Naphthalene Dianion [CpBn5Yb(DME)]2(μ-η4:η4-C10H8). Oxidative Substitution of [C10H8]2‒ by 1,4-Diphenylbuta-1,3-diene and P4 and Protonolysis of the Yb‒C10H8 Bond by PhPH2
Selikhov, Alexander N.; Mahrova, Tatyana V.; Cherkasov, Anton V.; Fukin, Georgy K.; Kirillov, Evgueni; Alvarez Lamsfus, Carlos; Maron, Laurent; Trifonov, Alexander A.; Organometallics 35 (2016) 2401–; doi:10.1021/acs.organomet.6b00428

data_4088784
_publ_section_title
;
 Yb(II) Triple-Decker Complex with the \m-Bridging Naphthalene Dianion
 [CpBn5Yb(DME)]2(\m-\h4:\h4-C10H8). Oxidative Substitution of [C10H8]2--
 by 1,4-Diphenylbuta-1,3-diene and P4 and Protonolysis of the Yb--C10H8
 Bond by PhPH2
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2401
_journal_paper_doi               10.1021/acs.organomet.6b00428
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C84 H80 O2 Yb, 0.5(C4 H10 O2)'
_chemical_formula_sum            'C86 H85 O3 Yb'
_chemical_formula_weight         1339.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                79.8680(10)
_cell_angle_beta                 84.4440(10)
_cell_angle_gamma                74.3150(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2669(3)
_cell_length_b                   15.7691(4)
_cell_length_c                   21.4030(6)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.18
_cell_volume                     3279.64(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Smart Apex (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34684
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.730
_diffrn_reflns_theta_min         1.358
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.478
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/2'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       prism
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.858
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         16794
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+2.0008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15356
_reflns_number_total             16794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00428_si_001.cif
_cod_data_source_block           ybcpbndme
_cod_database_code               4088784
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.641
_shelx_estimated_absorpt_t_max   0.820
_shelx_res_checksum              90958
_shelx_hkl_checksum              33563