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_4080935
_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         'C46 H62 N7 O2 Yb, C4 H8 O'
_chemical_formula_sum            'C50 H70 N7 O3 Yb'
_chemical_formula_weight         990.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.087(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1512(3)
_cell_length_b                   15.0219(4)
_cell_length_c                   24.6389(7)
_cell_measurement_reflns_used    12943
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.5165
_cell_measurement_theta_min      3.0857
_cell_volume                     4830.4(2)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.4692
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27419
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.984
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         3.070
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8969
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0396P)^2^+28.6789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                6529
_reflns_number_total             8969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400200f_si_001.cif
_cod_data_source_block           complex4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080935