Lanthanide Complexes of Boraamidinate Ligands: Synthesis and X-ray Structures of {[Li(THF)4][bamLnCl2(THF)]}2 (bam= [PhB(NDipp)2]2-; Ln = Y, Pr, Nd, Sm, Ho, Er, Yb) and {bamLnCl(THF)2}2 (Ln = Y, Sm)
Andrea M. Corrente; Tristram Chivers; Inorganic Chemistry 49 (2010) 2457–2463; doi:10.1021/ic9023184

data_4315071
_publ_contact_author_address
;
Department of Chemistry
University of Calgary, Calgary, Alberta 
T2N 1N4, Canada
;
_publ_contact_author_name        'Prof. T. Chivers'
_publ_section_title
;
 Lanthanide Complexes of Boraamidinate Ligands: Synthesis and X-ray
 Structures of {[Li(THF)4][bamLnCl2(THF)]}2 (bam= [PhB(NDipp)2]2-; Ln = Y,
 Pr, Nd, Sm, Ho, Er, Yb) and {bamLnCl(THF)2}2 (Ln = Y, Sm)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2457
_journal_page_last               2463
_journal_paper_doi               10.1021/ic9023184
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C38 H55 B Cl N2 O2 Y'
_chemical_formula_sum            'C38 H55 B Cl N2 O2 Y'
_chemical_formula_weight         707.01
_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                 93.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.690(3)
_cell_length_b                   15.867(3)
_cell_length_c                   18.516(4)
_cell_measurement_reflns_used    51912
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.55
_cell_volume                     4015.6(15)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi\omega scans'
_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  0.1061
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51912
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    1.550
_exptl_absorpt_correction_T_max  0.8860
_exptl_absorpt_correction_T_min  0.7896
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski and Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; Electron density in two regions were attributed to a disordered
  hexane molecule for which no suitable model could be found. 
  These regions of electron density were removed from the reflections 
  data using the program SQUEEZE (PLATON), leaving a total void of 
  496.2 angstroms cubed
;
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0351P)^2^+11.4662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                5363
_reflns_number_total             7069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9023184_si_001_8.cif
_cod_data_source_block           Compound10a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Integration'
changed to 'integration' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4015.7(14)
_cod_database_code               4315071