Cyclopentadienyl-Like Ligand as a Reactive Site in Half-Sandwich Bis(amidinato) Rare-Earth-Metal Complexes: An Efficient Application in Catalytic Addition of Amines to Carbodiimides
Wei, Peng-Hui; Xu, Ling; Song, Li-Cheng; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 33 (2014) 2784–; doi:10.1021/om5002793

data_4083403
_publ_section_title
;
 Cyclopentadienyl-Like Ligand as a Reactive Site in Half-Sandwich
 Bis(amidinato) Rare-Earth-Metal Complexes: An Efficient Application in
 Catalytic Addition of Amines to Carbodiimides
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2784
_journal_paper_doi               10.1021/om5002793
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C50 H51 Dy N4 Si'
_chemical_formula_sum            'C50 H51 Dy N4 Si'
_chemical_formula_weight         898.53
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2013-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.78(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.870(2)
_cell_length_b                   17.823(4)
_cell_length_c                   22.817(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4356.2(16)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26166
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.917
_exptl_absorpt_coefficient_mu    1.781
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         8573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+2.0556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7475
_reflns_number_total             8573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5002793_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4083401--4083407.cif.'
_cod_original_cell_volume        4356.3(16)
_cod_database_code               4083403
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.717
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4A) = Uanis(C5A) = Uanis(C6A) = Uanis(C7A) = Uanis(C8A)
Uanis(C4) = Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C8)
Uanis(C39) = Uanis(C40) = Uanis(C39A) = Uanis(C44A)
3. Others
 Sof(Si1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=
 Sof(C8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=1-FVAR(1)
 Sof(Si1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(C5A)=Sof(C6A)=
 Sof(C7A)=Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=
 Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=
 Sof(H12D)=Sof(H12E)=Sof(H12F)=FVAR(1)
 Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=1-FVAR(2)
 Sof(C39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C40A(H40A),
 C41(H41), C41A(H41A), C42(H42), C42A(H42A), C43(H43), C43A(H43A), C44(H44),
 C44A(H44A), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC),
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C11(H11A,H11B,H11C), C11A(H11D,H11E,
 H11F), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              88586
_shelx_hkl_checksum              6192