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_7122129
_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         'C52 H118 O18 Si4 Sm2, C4 H10 O2'
_chemical_formula_sum            'C56 H128 O20 Si4 Sm2'
_chemical_formula_weight         1534.64
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.49276(16)
_cell_length_b                   13.49276(16)
_cell_length_c                   73.6861(7)
_cell_measurement_reflns_used    26128
_cell_measurement_temperature    90.0(3)
_cell_measurement_theta_max      74.9820
_cell_measurement_theta_min      3.5900
_cell_volume                     11617.6(2)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_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  0.1104
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       54
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            84451
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.075
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.347
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.170
_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            'metallic dark black'
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Flack x determined using 3214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         12570
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0819
_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^)+(0.0375P)^2^+156.8031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.551
_reflns_Friedel_fraction_full    0.601
_reflns_Friedel_fraction_max     0.558
_reflns_number_gt                12086
_reflns_number_total             12570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04169e2.cif
_cod_data_source_block           aw57
_cod_depositor_comments
'Adding full bibliography for 7122128--7122131.cif.'
_cod_original_cell_volume        11617.6(3)
_cod_database_code               7122129
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.111
_shelx_estimated_absorpt_t_max   0.724
_shelx_res_checksum              33147
_publcif_funding_html
;
;