Synthesis and Structural Characterization of Mixed-Valent Ytterbium and Europium Complexes Supported by a Phenoxy(quinolinyl)amide Ligand
Jiang, Yinyin; Zhu, Xi; Chen, Muzi; Wang, Yaorong; Yao, Yingming; Wu, Bing; Shen, Qi; Organometallics 33 (2014) 1972–; doi:10.1021/om5000198

data_4083029
_publ_section_title
;
 Synthesis and Structural Characterization of Mixed-Valent Ytterbium and
 Europium Complexes Supported by a Phenoxy(quinolinyl)amide Ligand
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1972
_journal_paper_doi               10.1021/om5000198
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C34 H56 N3 O3 Si2 Sm, 0.5(C4 H10 O2)'
_chemical_formula_sum            'C36 H61 N3 O4 Si2 Sm'
_chemical_formula_weight         806.41
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   48.357(5)
_cell_length_b                   39.213(4)
_cell_length_c                   8.8404(7)
_cell_measurement_reflns_used    19685
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     16763(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22428
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         8328
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                7759
_reflns_number_total             8328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5000198_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4083026--4083029.cif.'
_cod_database_code               4083029