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_7107193
_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            'C95 H111 B2 Lu N2 O4'
_chemical_formula_weight         1541.45
_chemical_name_common            ((Ph-NCN)Lu(THF)4)(BPh4)2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 91.444(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5937(15)
_cell_length_b                   40.384(4)
_cell_length_c                   28.730(3)
_cell_measurement_reflns_used    395
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.4
_cell_volume                     16927(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  'SHELXH-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_sigmaI/netI    0.1422
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            92044
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.8385
_exptl_absorpt_correction_T_min  0.7507
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             6464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
One disordered THF molecules per formual unit of [(Ph-NCN)Lu(THF)4][BPh4]2
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         2.186
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1875
_refine_ls_number_reflns         29679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                17139
_reflns_number_total             29679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14949k.txt
_cod_data_source_block           6-Lu
_cod_original_cell_volume        16926(3)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7107193