Cationic terminal hydrido rare earth complexes bearing an amidinate ancillary ligand
Jianhua Cheng; Zhaomin Hou; Chem.Commun. 48 (2012) 814–; doi:10.1039/c1cc14949k

data_7107191
_publ_section_title
;
 Cationic terminal hydrido rare earth complexes bearing an amidinate
 ancillary ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              814
_journal_paper_doi               10.1039/c1cc14949k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C67 H84 B Lu N2 O3'
_chemical_formula_weight         1151.14
_chemical_name_common            ((Ph-NCN)LuH(THF)3)(BPh4)
_chemical_properties_physical    air-sensitive
_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                 92.748(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.966(6)
_cell_length_b                   11.804(3)
_cell_length_c                   27.217(7)
_cell_measurement_reflns_used    875
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.75
_cell_volume                     6728(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35869
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_recrystallization_method THF/Hexane
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
Two disorder THF molecule per formual unit of [(Ph-NCN)LuH(THF)3][BPh4]
were not modelled and the disordered density was taken into account
using the SQUEEZE/PLATON procedure.
(Sluis, P. van der; Spek, A. L. Acta Crystallogr.
1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta
Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3.
PLATON - a multipurpose crystallographic tool. Utrecht University,
Utrecht, The Netherlands).
;
_refine_diff_density_max         2.582
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         11829
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+12.2743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                9644
_reflns_number_total             11829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14949k.txt
_cod_data_source_block           3-Lu
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7107191