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_4064095
_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            'C37 H64 B9 N4 O Sc'
_chemical_formula_weight         723.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.464(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9306(4)
_cell_length_b                   15.8819(4)
_cell_length_c                   18.9486(4)
_cell_measurement_reflns_used    17341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2104
_cell_measurement_theta_min      2.1263
_cell_volume                     4146.61(18)
_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      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0884
_diffrn_reflns_av_sigmaI/netI    0.1195
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112296
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98515
_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    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_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     495
_refine_ls_number_reflns         9470
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                5184
_reflns_number_total             9470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011243_si_001.cif
_cod_data_source_block           altr29
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4064095