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_4064096
_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 N4 O3 Y'
_chemical_formula_weight         911.33
_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                96.415(3)
_cell_angle_beta                 92.025(3)
_cell_angle_gamma                98.546(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1838(4)
_cell_length_b                   11.7374(4)
_cell_length_c                   21.4661(8)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1888
_cell_measurement_theta_min      2.1867
_cell_volume                     2517.97(16)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.36 (release 16-03-2009 CrysAlis171 .NET) 
(compiled Mar 16 2009,17:39:00) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.36 (release 16-03-2009 CrysAlis171 .NET) 
(compiled Mar 16 2009,17:39:00) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.36 (release 16-03-2009 CrysAlis171 .NET) 
(compiled Mar 16 2009,17:39:00) 
;
_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      150(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_sigmaI/netI    0.2115
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64833
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.36 (release 16-03-2009 CrysAlis171 .NET) 
(compiled Mar 16 2009,17:39:00) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_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         0.987
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment
;
The hydrogens of the boron atoms B1, B2 and B3 were refined freely
but with a common isotropic temperature factor.
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     538
_refine_ls_number_reflns         10623
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                5388
_reflns_number_total             10623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011243_si_001.cif
_cod_data_source_block           altr27
_cod_database_code               4064096