Ln(II)/Pb(II)‒Ln(III)/Pb(0) Redox Approach toward Rare-Earth-Metal Half-Sandwich Complexes
Bienfait, André M.; Wolf, Benjamin M.; Törnroos, Karl W.; Anwander, Reiner; Organometallics 34 (2015) 5734–; doi:10.1021/acs.organomet.5b00837

data_4088080
_publ_section_title
;
 Ln(II)/Pb(II)--Ln(III)/Pb(0) Redox Approach toward Rare-Earth-Metal
 Half-Sandwich Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5734
_journal_paper_doi               10.1021/acs.organomet.5b00837
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C18 H39 Al2 Sm'
_chemical_formula_sum            'C18 H39 Al2 Sm'
_chemical_formula_weight         459.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0888(10)
_cell_length_b                   14.3626(9)
_cell_length_c                   17.9890(11)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.38
_cell_volume                     4415.2(5)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.514
_diffrn_reflns_theta_min         2.171
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.734
_exptl_absorpt_correction_T_max  0.6975
_exptl_absorpt_correction_T_min  0.2568
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.683
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.142
_refine_diff_density_max         2.569
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         7347
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.1192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6377
_reflns_number_total             7347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00837_si_002.cif
_cod_data_source_block           Compound6a
_cod_database_code               4088080
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.257
_shelx_estimated_absorpt_t_max   0.697
_shelx_res_checksum              64938
_shelx_hkl_checksum              72431