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_4088084
_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         'C43 H71 Cl4 O3 Sm3'
_chemical_formula_sum            'C43 H71 Cl4 O3 Sm3'
_chemical_formula_weight         1228.84
_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                 91.1460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6202(6)
_cell_length_b                   19.9665(10)
_cell_length_c                   18.6483(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      32.09
_cell_measurement_theta_min      2.22
_cell_volume                     4698.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89483
_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         32.143
_diffrn_reflns_theta_min         1.909
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    3.963
_exptl_absorpt_correction_T_max  0.92652
_exptl_absorpt_correction_T_min  0.81023
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.9791
_exptl_transmission_factor_min   0.7867
_refine_diff_density_max         2.277
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         16495
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+8.6498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14741
_reflns_number_total             16495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00837_si_002.cif
_cod_data_source_block           Compound9
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088084
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81833
_shelx_hkl_checksum              81102