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_4088076
_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         'C22 H51 N2 O Si4 Sm'
_chemical_formula_sum            'C22 H51 N2 O Si4 Sm'
_chemical_formula_weight         622.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.9580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2768(7)
_cell_length_b                   20.9232(14)
_cell_length_c                   14.4697(10)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      32.58
_cell_measurement_theta_min      2.41
_cell_volume                     3088.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.584
_diffrn_reflns_theta_min         1.947
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  0.7774
_exptl_absorpt_correction_T_min  0.3900
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         11256
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+1.1809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10778
_reflns_number_total             11256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00837_si_002.cif
_cod_data_source_block           Compound3a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088076
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.390
_shelx_estimated_absorpt_t_max   0.777
_shelx_res_checksum              71105
_shelx_hkl_checksum              28123