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_4064099
_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            'C40 H70 B9 N4 O2 Y'
_chemical_formula_weight         825.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.138(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.348(6)
_cell_length_b                   17.036(3)
_cell_length_c                   17.959(3)
_cell_measurement_temperature    296(2)
_cell_volume                     10533(3)
_computing_cell_refinement       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_collection       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_reduction        'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_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  0.1076
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47014
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.7261
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.041
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
 One distorted molecule of THF and one half molecule of hexane, 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 one molecule of THF and half 
 molecule of hexane per asymmetric unit.
;
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00034(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9506
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2256
_reflns_number_gt                4313
_reflns_number_total             9506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011243_si_001.cif
_cod_data_source_block           altr98
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4064099