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_4088782
_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         'C132 H135 O6 P7 Yb3, 3(C7 H8)'
_chemical_formula_sum            'C153 H159 O6 P7 Yb3'
_chemical_formula_weight         2829.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 97.3890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0777(10)
_cell_length_b                   28.066(2)
_cell_length_c                   17.2223(12)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.28
_cell_volume                     6748.1(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73323
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.149
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.200
_exptl_absorpt_correction_T_max  0.6148
_exptl_absorpt_correction_T_min  0.4709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.345
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 11335 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1379
_refine_ls_number_reflns         36134
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0459
_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\^)+(0.0422P)\^2\^] where P=(Fo\^2\^+2Fc\^2\^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                28734
_reflns_number_total             36134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00428_si_001.cif
_cod_data_source_block           ybp7cpbn
_cod_original_cell_volume        6748.0(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4088782
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.406
_shelx_estimated_absorpt_t_max   0.680
_shelx_res_checksum              54138
_shelx_hkl_checksum              38649