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_7122130
_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 H170 O24 Si6 Sm4'
_chemical_formula_sum            'C79 H170 O24 Si6 Sm4'
_chemical_formula_weight         2274.08
_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-2017/1
_audit_update_record
;
2018-05-15 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                81.584(4)
_cell_angle_beta                 73.829(4)
_cell_angle_gamma                65.648(4)
_cell_formula_units_Z            1
_cell_length_a                   13.2055(6)
_cell_length_b                   13.2859(6)
_cell_length_c                   19.3107(10)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.5000
_cell_measurement_theta_min      4.2660
_cell_volume                     2962.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_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    133.00 176.00   1.00   20.00    --  111.85  45.00   0.00   43
  2  \w     84.00 112.00   1.00   20.00    --  111.85  61.00-150.00   28
  3  \w    107.00 134.00   1.00   20.00    --  111.85 -30.00-180.00   27
  4  \w     80.00 136.00   1.00   20.00    --  111.85 -61.00-180.00   56
  5  \w     82.00 109.00   1.00   20.00    --  111.85-125.00-150.00   27
  6  \w     65.00 135.00   1.00   20.00    --  111.85 -77.00 -90.00   70
  7  \w     81.00 128.00   1.00   20.00    --  111.85 -42.00 -25.00   47
  8  \w     97.00 122.00   1.00   20.00    --  111.85-125.00  30.00   25
  9  \w     63.00 138.00   1.00   20.00    --  111.85 -61.00  60.00   75
 10  \w     85.00 178.00   1.00   20.00    --  111.85  15.00  90.00   93
 11  \w     84.00 178.00   1.00   20.00    --  111.85  30.00 150.00   94
 12  \w     55.00  83.00   1.00    5.00    --   40.66-125.00 150.00   28
 13  \w     33.00 108.00   1.00   20.00    --  111.85 -94.00  60.00   75
 14  \w     38.00  66.00   1.00   20.00    --  111.85 -42.00 -25.00   28
 15  \w     49.00 122.00   1.00   20.00    --  111.85-125.00 -90.00   73
 16  \w     44.00  71.00   1.00   20.00    --  111.85-125.00-150.00   27
 17  \w     37.00  90.00   1.00   20.00    --  111.85 -30.00-180.00   53
 18  \w     39.00  70.00   1.00   20.00    --  111.85-125.00  30.00   31
 19  \w    -65.00  33.00   1.00    5.00    --  -40.66  38.00 150.00   98
 20  \w    -94.00  -6.00   1.00    5.00    --  -40.66 125.00-120.00   88
 21  \w    -59.00  32.00   1.00    5.00    --  -40.66  57.00-120.00   91
 22  \w   -108.00 -18.00   1.00    5.00    --  -40.66 -38.00 -30.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_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_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.187
_diffrn_reflns_theta_min         3.654
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.673
_exptl_absorpt_correction_T_max  0.305
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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            'metallic intense black'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.143
_refine_diff_density_max         3.245
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         11997
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0917P)^2^+2.0447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10583
_reflns_number_total             11997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04169e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7122128--7122131.cif.'
_cod_database_code               7122130
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              15114
_shelx_fab_checksum              22948