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_7122131
_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         'C79 H169 K2 O24 Si6 Sm2'
_chemical_formula_sum            'C79 H169 K2 O24 Si6 Sm2'
_chemical_formula_weight         2050.57
_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     dual
_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                80.512(5)
_cell_angle_beta                 72.563(6)
_cell_angle_gamma                64.969(6)
_cell_formula_units_Z            1
_cell_length_a                   13.3255(8)
_cell_length_b                   13.4570(8)
_cell_length_c                   19.2064(12)
_cell_measurement_reflns_used    4181
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.3210
_cell_measurement_theta_min      3.7510
_cell_volume                     2974.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -112.00 -18.00   1.00   20.00    --  -42.88 -57.00 120.00   94
  2  \w    -56.00  22.00   1.00   20.00    --  -42.88  57.00  60.00   78
  3  \w    -67.00  30.00   1.00   20.00    --  -42.88  57.00 -90.00   97
  4  \w     56.00  96.00   1.00   20.00    --   42.88-125.00  60.00   40
  5  \w     38.00 114.00   1.00   20.00    --   42.88  37.00   0.00   76
  6  \w     39.00 125.00   1.00   80.00    --  109.26 -45.00 -60.00   86
  7  \w     78.00 138.00   1.00   80.00    --  109.26 -61.00  90.00   60
  8  \w     89.00 116.00   1.00   80.00    --  109.26 -77.00-120.00   27
  9  \w     60.00 108.00   1.00   80.00    --  109.26 -94.00-120.00   48
 10  \w     37.00 124.00   1.00   80.00    --  109.26 -45.00-150.00   87
 11  \w     61.00 114.00   1.00   80.00    --  109.26-111.00  60.00   53
 12  \w     39.00 135.00   1.00   80.00    --  109.26 -45.00  60.00   96
 13  \w     83.00 108.00   1.00   80.00    --  109.26 -94.00 -60.00   25
 14  \w     78.00 106.00   1.00   80.00    --  109.26 -94.00-180.00   28
 15  \w    121.00 169.00   1.00   80.00    --  109.26  30.00  90.00   48
 16  \w     74.00 116.00   1.00   80.00    --  109.26-111.00 120.00   42
 17  \w    100.00 172.00   1.00   80.00    --  109.26 111.00-150.00   72
 18  \w    121.00 148.00   1.00   80.00    --  109.26 111.00   0.00   27
 19  \w     35.00 170.00   1.00   80.00    --  109.26   0.00  60.00  135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.151
_diffrn_reflns_theta_min         3.629
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.981
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             1081
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.163
_refine_diff_density_max         2.761
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         12278
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0731
_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^)+(0.1200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7202
_reflns_number_total             12278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04169e2.cif
_cod_data_source_block           dt211_sq
_cod_depositor_comments
'Adding full bibliography for 7122128--7122131.cif.'
_cod_database_code               7122131
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.151
_shelx_estimated_absorpt_t_max   0.322
_shelx_res_checksum              39341
_shelx_fab_checksum              9073