A tetranuclear samarium(ii) inverse sandwich from direct reduction of toluene by a samarium(ii) siloxide.
Kelly, Rory P.; Toniolo, Davide; Tirani, Farzaneh Fadaei; Maron, Laurent; Mazzanti, Marinella; Chemical communications (Cambridge, England) 54 (2018) 10268–10271; doi:10.1039/c8cc04169e

data_7122128
_publ_section_title
;
 A tetranuclear samarium(ii) inverse sandwich from direct reduction of
 toluene by a samarium(ii) siloxide.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10268
_journal_page_last               10271
_journal_paper_doi               10.1039/c8cc04169e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C60 H135 K O20 Si5 Sm2'
_chemical_formula_sum            'C60 H135 K O20 Si5 Sm2'
_chemical_formula_weight         1656.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-05-15 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                80.979(7)
_cell_angle_beta                 87.169(9)
_cell_angle_gamma                80.361(8)
_cell_formula_units_Z            2
_cell_length_a                   13.9095(16)
_cell_length_b                   15.4386(11)
_cell_length_c                   21.897(3)
_cell_measurement_reflns_used    142
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     4577.2(9)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Mercury 3.10 (CCDC, 2017)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0968
_diffrn_reflns_av_unetI/netI     0.1356
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63685
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.729
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0922 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.7854.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.223
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         20583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0460P)^2^+16.9946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12714
_reflns_number_total             20583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04169e2.cif
_cod_data_source_block           rk3-60
_cod_depositor_comments
'Adding full bibliography for 7122128--7122131.cif.'
_cod_original_cell_volume        4577.3(8)
_cod_database_code               7122128
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.894
_shelx_res_checksum              68666
_shelx_fab_checksum              1526
_publcif_funding_html
;
;