Synthesis and Structure of Rare-Earth-Metal Dicarbollide Complexes with an Imidazolin-2-iminato Ligand Featuring Very Short Metal−Nitrogen Bonds
Trambitas, Alexandra G.; Yang, Jingying; Melcher, Daniel; Daniliuc, Constantin G.; Jones, Peter G.; Xie, Zuowei; Tamm, Matthias; Organometallics 30 (2011) 1122–; doi:10.1021/om1011243

data_4064097
_publ_section_title
;
 Synthesis and Structure of Rare-Earth-Metal Dicarbollide Complexes with
 an Imidazolin-2-iminato Ligand Featuring Very Short Metal&#x2212;Nitrogen
 Bonds
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1122
_journal_paper_doi               10.1021/om1011243
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C45 H80 B9 Lu N4 O3'
_chemical_formula_weight         997.39
_chemical_name_systematic
; 
 ? 
;
_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                96.897(4)
_cell_angle_beta                 92.090(4)
_cell_angle_gamma                98.288(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1178(4)
_cell_length_b                   11.6476(4)
_cell_length_c                   21.4015(10)
_cell_measurement_reflns_used    22576
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.7004
_cell_measurement_theta_min      3.8636
_cell_volume                     2474.01(18)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) 
(compiled Nov  6 2009,16:24:50) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) 
(compiled Nov  6 2009,16:24:50) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) 
(compiled Nov  6 2009,16:24:50) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34042
_diffrn_reflns_theta_full        72.50
_diffrn_reflns_theta_max         75.96
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    4.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) 
(compiled Nov  6 2009,16:24:50) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
 One distorted molecule of THF, which could not be refined 
 satisfactorily, was removed using the program SQUEEZE (A.L. Spek, 
 University of Utrecht, Netherlands). The quoted formula and derived 
 parameters are based on a total of three molecules of THF
 (one coordinated, one free, one Squeezed) per asymmetric unit.
;
_refine_diff_density_max         1.039
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment
;
The hydrogens of the boron atoms B1, B2 and B3 were refined freely.
Bond lengths B-H were restrained equal with SADI.    
The hydrogen H29 of the C29 atom was refined freely.
The methyls were refined using a rigid model, other hydrogens riding. 
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         10191
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.7246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                9109
_reflns_number_total             10191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011243_si_001.cif
_cod_data_source_block           altr50
_cod_original_cell_volume        2474.01(17)
_cod_database_code               4064097