A Comparative Study of π-Arene-Bridged Lanthanum Arylamide and Aryloxide Dimers. Solution Behavior, Exchange Mechanisms, and X-ray Crystal Structures of La2(NH-2,6-iPr2C6H3)6, La(NH-2,6-iPr2C6H3)3(THF)3, and La(NH-2,6-iPr2C6H3)3(py)2
Garth R. Giesbrecht; John C. Gordon; David L. Clark; P. Jeffrey Hay; Brian L. Scott; C. Drew Tait; Journal of the American Chemical Society 126 (2004) 6387–6401; doi:10.1021/ja0398262

data_4112586
_publ_contact_author
;
John C. Gordon
MS J514
Los Alamos National Laboratory
Los Alamos, New Mexico  87545
;
_publ_contact_author_email       jgordon@lanl.gov
_publ_section_title
;
 A Comparative Study of \p-Arene-Bridged Lanthanum Arylamide and Aryloxide
 Dimers. Solution Behavior, Exchange Mechanisms, and X-ray Crystal
 Structures of La2(NH-2,6-iPr2C6H3)6, La(NH-2,6-iPr2C6H3)3(THF)3, and
 La(NH-2,6-iPr2C6H3)3(py)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6387
_journal_page_last               6401
_journal_paper_doi               10.1021/ja0398262
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C52 H86 La N3 O4'
_chemical_formula_weight         956.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 119.253(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.137(4)
_cell_length_b                   16.922(4)
_cell_length_c                   13.442(3)
_cell_measurement_temperature    203(2)
_cell_volume                     2607.1(12)
_computing_cell_refinement       'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_data_collection       'Siemens SMART (v. 4.202, Siemens 1996)'
_computing_data_reduction        'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_molecular_graphics    'Bruker AXS SHEXTL (v. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       '\f 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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16872
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.8888
_exptl_absorpt_correction_T_min  0.7820
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.037(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                8545
_reflns_number_total             9402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0398262si20031126_061303_2.cif
_cod_data_source_block           ccd716as
_cod_original_cell_volume        2607.3(11)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4112586