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_4088082
_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         'C48 H84 Al2 Sm2, 4(C7 H8)'
_chemical_formula_sum            'C76 H116 Al2 Sm2'
_chemical_formula_weight         1384.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                106.392(2)
_cell_angle_beta                 100.659(2)
_cell_angle_gamma                111.773(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1956(15)
_cell_length_b                   12.6663(16)
_cell_length_c                   15.014(3)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.53
_cell_volume                     1793.8(5)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27211
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.818
_diffrn_reflns_theta_min         1.875
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_crystal_colour            orange/yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       'melted block'
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.897
_exptl_crystal_size_mid          0.566
_exptl_crystal_size_min          0.296
_exptl_transmission_factor_max   0.4315
_exptl_transmission_factor_min   0.2273
_refine_diff_density_max         4.646
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9265
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+8.9798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8855
_reflns_number_total             9265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00837_si_002.cif
_cod_data_source_block           Compound7a
_cod_database_code               4088082
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.313
_shelx_estimated_absorpt_t_max   0.636
_shelx_res_checksum              88492
_shelx_hkl_checksum              16599