Synthesis of a Naphthalene-Bridged Bis(guanidinato)ytterbium(II) Complex and an Unexpected Pathway in Its Reaction with CH3CN,p-ClC6H4CH2CN, and Ph2CHCN
Wang, Chuanyong; Zhang, Xingmin; Xue, Mingqiang; Zhang, Yong; Shen, Qi; Organometallics 32 (2013) 3618–; doi:10.1021/om400200f

data_4080932
_publ_section_title
;
 Synthesis of a Naphthalene-Bridged Bis(guanidinato)ytterbium(II) Complex
 and an Unexpected Pathway in Its Reaction with CH3CN,p-ClC6H4CH2CN, and
 Ph2CHCN
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3618
_journal_paper_doi               10.1021/om400200f
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C56 H88 N12 O2 Yb2'
_chemical_formula_sum            'C56 H88 N12 O2 Yb2'
_chemical_formula_weight         1307.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.516(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.641(5)
_cell_length_b                   15.473(6)
_cell_length_c                   13.537(5)
_cell_measurement_reflns_used    12589
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      3.0
_cell_volume                     2857.1(19)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23075
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    3.304
_exptl_absorpt_correction_T_max  0.370
_exptl_absorpt_correction_T_min  0.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.220
_refine_diff_density_min         -2.418
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0983P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                4394
_reflns_number_total             5301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400200f_si_001.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        2857.0(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4080932