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_7107192
_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            'C70 H90 B Lu N4 O2'
_chemical_formula_weight         1205.24
_chemical_name_common            ((Ph-NCN)Lu(NCN)(THF)2)(BPh4)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.098(7)
_cell_angle_beta                 86.501(6)
_cell_angle_gamma                80.166(6)
_cell_formula_units_Z            2
_cell_length_a                   12.306(4)
_cell_length_b                   12.971(5)
_cell_length_c                   23.504(8)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.63
_cell_volume                     3602(2)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.1515
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19316
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_T_max  0.6609
_exptl_absorpt_correction_T_min  0.6022
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_platon_squeeze_details
;
Two disordered THF molecules per formual unit of [(Ph-NCN)Lu(NCN)(THF)2][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         2.015
_refine_diff_density_min         -2.148
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         12412
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                8161
_reflns_number_total             12412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14949k.txt
_cod_data_source_block           5-Lu
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107192