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_4083407
_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         'C96 H88 Lu2 N10'
_chemical_formula_sum            'C96 H88 Lu2 N10'
_chemical_formula_weight         1731.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     iterative
_audit_creation_date             2014-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.706(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5804(5)
_cell_length_b                   26.6986(14)
_cell_length_c                   13.1122(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4753.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14978
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.366
_exptl_absorpt_coefficient_mu    2.110
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_correction_T_min  0.6776
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         1.788
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.300
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0180P)^2^+28.6550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6446
_reflns_number_total             7761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5002793_si_002.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 4083401--4083407.cif.'
_cod_database_code               4083407
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.045) H3(0.051) H4(0.063) H5A(0.063) H6(0.066) H7(0.056)
 H9(0.083) H10(0.113) H12(0.071) H13(0.055) H14A(0.179) H14B(0.179) H14C(0.179)
 H16(0.052) H17(0.056) H19(0.057) H20(0.051) H21A(0.092) H21B(0.092)
 H21C(0.092) H24(0.056) H25(0.088) H26(0.11) H27(0.103) H28(0.074) H30(0.047)
 H31(0.053) H33(0.051) H34(0.047) H35A(0.096) H35B(0.096) H35C(0.096)
 H37(0.058) H38(0.08) H40(0.066) H41(0.046) H42A(0.141) H42B(0.141) H42C(0.141)
 H44(0.049) H45(0.075) H46(0.125) H47(0.127) H48(0.086)
 Fixed X: H5(0.6264) H3(0.5936) H4(0.6607) H5A(0.7801) H6(0.8341) H7(0.7732)
 H9(0.7828) H10(0.949) H12(1.0099) H13(0.8458) H14A(1.12) H14B(1.1463)
 H14C(1.1199) H16(0.388) H17(0.2581) H19(0.3828) H20(0.5138) H21A(0.1595)
 H21B(0.2263) H21C(0.227) H24(0.6715) H25(0.7534) H26(0.8399) H27(0.8393)
 H28(0.7529) H30(0.6961) H31(0.8342) H33(0.9977) H34(0.8617) H35A(1.0138)
 H35B(1.0782) H35C(1.0185) H37(0.4853) H38(0.4298) H40(0.5103) H41(0.5703)
 H42A(0.4468) H42B(0.4586) H42C(0.3564) H44(0.5287) H45(0.5926) H46(0.7339)
 H47(0.7966) H48(0.7347)
 Fixed Y: H5(0.5344) H3(0.3527) H4(0.3328) H5A(0.3835) H6(0.4543) H7(0.4732)
 H9(0.3546) H10(0.3339) H12(0.472) H13(0.4943) H14A(0.3594) H14B(0.4155)
 H14C(0.3745) H16(0.3746) H17(0.3704) H19(0.479) H20(0.4833) H21A(0.4216)
 H21B(0.4485) H21C(0.3887) H24(0.3471) H25(0.2795) H26(0.2237) H27(0.2319)
 H28(0.2971) H30(0.4864) H31(0.5107) H33(0.4091) H34(0.3875) H35A(0.4557)
 H35B(0.4646) H35C(0.5101) H37(0.3052) H38(0.2246) H40(0.2369) H41(0.3167)
 H42A(0.1604) H42B(0.1463) H42C(0.1681) H44(0.5333) H45(0.5767) H46(0.6257)
 H47(0.639) H48(0.5954)
 Fixed Z: H5(-0.0855) H3(0.3558) H4(0.5166) H5A(0.5907) H6(0.5019) H7(0.3424)
 H9(0.1931) H10(0.1821) H12(0.0838) H13(0.0985) H14A(0.1758) H14B(0.1429)
 H14C(0.0577) H16(0.2007) H17(0.3171) H19(0.4828) H20(0.3695) H21A(0.4493)
 H21B(0.5346) H21C(0.5245) H24(-0.2762) H25(-0.3496) H26(-0.2476) H27(-0.0706)
 H28(0.0035) H30(-0.2372) H31(-0.3261) H33(-0.1762) H34(-0.0789) H35A(-0.3931)
 H35B(-0.2917) H35C(-0.3423) H37(-0.1393) H38(-0.1086) H40(0.1846) H41(0.1557)
 H42A(0.1328) H42B(0.015) H42C(0.055) H44(0.1653) H45(0.3041) H46(0.2877)
 H47(0.1238) H48(-0.0149)
;