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_4064098
_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            'C43 H77 B9 N5 O2 Y'
_chemical_formula_weight         882.30
_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                96.541(8)
_cell_angle_beta                 93.202(8)
_cell_angle_gamma                106.821(8)
_cell_formula_units_Z            2
_cell_length_a                   10.125(5)
_cell_length_b                   12.243(5)
_cell_length_c                   20.164(9)
_cell_measurement_reflns_used    1009
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.02
_cell_volume                     2366.6(19)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD 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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       '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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.1476
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12950
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.5686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_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 one 
 molecule of THF per asymmetric unit.
;
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                4864
_reflns_number_total             8297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011243_si_001.cif
_cod_data_source_block           altr99
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2366.7(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064098