Ln(III) methyl and methylidene complexes stabilized by a bulky hydrotris(pyrazolyl)borate ligand.
Zimmermann, Melanie; Takats, Josef; Kiel, Gong; Törnroos, Karl W; Anwander, Reiner; Chemical communications (Cambridge, England)  (2008) 612–614; doi:10.1039/b713378b

data_7102860
_publ_section_title
;
 Ln(III) methyl and methylidene complexes stabilized by a bulky
 hydrotris(pyrazolyl)borate ligand.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              612
_journal_page_last               614
_journal_paper_doi               10.1039/b713378b
_journal_year                    2008
_chemical_formula_moiety         'C25 H43 Al B N6, C14 H40 Al4 Y'
_chemical_formula_sum            'C39 H83 Al5 B N6 Y'
_chemical_formula_weight         870.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.6427(17)
_cell_length_b                   9.5879(6)
_cell_length_c                   18.0884(11)
_cell_measurement_reflns_used    5634
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      21.09
_cell_measurement_theta_min      2.23
_cell_volume                     5140.9(5)
_computing_cell_refinement
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_molecular_graphics
;
Brandenburg, K. (2005). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn,
Germany.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_computing_structure_solution
;
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean '48 \um'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-AXS SMART 2K CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2173
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49108
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  0.816505
_exptl_absorpt_correction_T_min  0.816505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2003). SADABS. Version 2004/1. University of
G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7423
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0000P)^2^+8.4848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                4683
_reflns_number_total             7423
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b713378b.txt
_cod_data_source_block           Compound3
_cod_database_code               7102860