Salt-Free Synthesis of Samarium-Aluminum Mixed-Metal Alkoxides: X-ray Crystal Structures of {[(i-Pr-O)(i-Bu)Al(μ-O-i-Pr)2Sm(O-i-Pr)(HO-i-Pr)](μ-O-i-Pr)}2, [(THF)2Sm(O-t-Bu)2(μ-O-t-Bu)2Al(i-Bu)2], Sm(OAr)3(THF)3 (Ar = 2,4,6-Me3C6H2), [Nd(μ-OAr)(OAr)2(py)2]2 (Ar = 2,4,6-Me3C6H2), and (ArO)3Sm[(μ-O-t-Bu)2Al2(O-t-Bu)4] (Ar = 2,6-i-Pr2C6H3)
Garth R. Giesbrecht; John C. Gordon; David L. Clark; Brian L. Scott; John G. Watkin; Kenneth J. Young; Inorganic Chemistry 41 (2002) 6372–6379; doi:10.1021/ic0203116

data_4318887
_publ_section_title
;
 Salt-Free Synthesis of Samarium-Aluminum Mixed-Metal Alkoxides: X-ray
 Crystal Structures of
 {[(i-Pr-O)(i-Bu)Al(\m-O-i-Pr)2Sm(O-i-Pr)(HO-i-Pr)](\m-O-i-Pr)}2,
 [(THF)2Sm(O-t-Bu)2(\m-O-t-Bu)2Al(i-Bu)2], Sm(OAr)3(THF)3 (Ar =
 2,4,6-Me3C6H2), [Nd(\m-OAr)(OAr)2(py)2]2 (Ar = 2,4,6-Me3C6H2), and
 (ArO)3Sm[(\m-O-t-Bu)2Al2(O-t-Bu)4] (Ar = 2,6-i-Pr2C6H3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6372
_journal_page_last               6379
_journal_paper_doi               10.1021/ic0203116
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C42 H40 O6 Sm'
_chemical_formula_weight         791.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   16.5822(9)
_cell_length_b                   15.5668(9)
_cell_length_c                   29.9017(18)
_cell_measurement_temperature    203(2)
_cell_volume                     7718.6(8)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       '\w and \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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5577
_diffrn_reflns_theta_full        23.45
_diffrn_reflns_theta_max         23.45
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                4092
_reflns_number_total             5577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203116_3.cif
_cod_data_source_block           ccd231a
_cod_database_code               4318887