Carbon dioxide reduction by dinuclear Yb(ii) and Sm(ii) complexes supported by siloxide ligands.
Willauer, Aurélien R; Toniolo, Davide; Fadaei-Tirani, Farzaneh; Yang, Yan; Laurent, Maron; Mazzanti, Marinella; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6100–6110; doi:10.1039/c9dt00554d

data_7049336
_publ_section_title
;
 Carbon dioxide reduction by dinuclear Yb(ii) and Sm(ii) complexes
 supported by siloxide ligands.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6100
_journal_page_last               6110
_journal_paper_doi               10.1039/c9dt00554d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H108 O16 Si4 Sm2'
_chemical_formula_sum            'C48 H108 O16 Si4 Sm2'
_chemical_formula_weight         1354.40
_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
;
2019-02-04 deposited with the CCDC.    2019-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                88.122(4)
_cell_angle_beta                 89.315(4)
_cell_angle_gamma                65.093(6)
_cell_formula_units_Z            2
_cell_length_a                   12.9099(7)
_cell_length_b                   14.0475(9)
_cell_length_c                   20.4106(8)
_cell_measurement_reflns_used    9147
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.8640
_cell_measurement_theta_min      3.4820
_cell_volume                     3355.4(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    '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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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   -102.00 -18.00   1.00    5.00    --  -40.91 -38.00 150.00   84
  2  \w   -114.00 -16.00   1.00    5.00    --  -40.91 -38.00-120.00   98
  3  \w    -64.00  30.00   1.00    5.00    --  -40.91  38.00  60.00   94
  4  \w     49.00  92.00   1.00    5.00    --   40.91-125.00-120.00   43
  5  \w     -7.00  55.00   1.00    5.00    --   40.91 -38.00  60.00   62
  6  \w     55.00  89.00   1.00    5.00    --   40.91-125.00  60.00   34
  7  \w     55.00  95.00   1.00   20.00    --  110.60 -94.00-180.00   40
  8  \w     40.00 114.00   1.00   20.00    --  110.60-111.00 -90.00   74
  9  \w     50.00 105.00   1.00   20.00    --  110.60 -94.00   0.00   55
 10  \w    131.00 172.00   1.00   20.00    --  110.60  77.00-120.00   41
 11  \w     32.00 159.00   1.00   20.00    --  110.60 -15.00 150.00  127
 12  \w    107.00 140.00   1.00   20.00    --  110.60 -77.00 -60.00   33
 13  \w     46.00 115.00   1.00   20.00    --  110.60-111.00 120.00   69
 14  \w     50.00 131.00   1.00   20.00    --  110.60 -45.00-150.00   81
 15  \w    119.00 177.00   1.00   20.00    --  110.60  45.00 -30.00   58
 16  \w     76.00 126.00   1.00   20.00    --  110.60 178.00-120.00   50
 17  \w     39.00  91.00   1.00   20.00    --  110.60 -45.00  90.00   52
 18  \w     96.00 123.00   1.00   20.00    --  110.60 -45.00  90.00   27
 19  \w     66.00 107.00   1.00   20.00    --  110.60 -94.00 -60.00   41
 20  \w     39.00 134.00   1.00   20.00    --  110.60 -30.00 -60.00   95
;
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24633
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.957
_diffrn_reflns_theta_min         3.471
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.134
_exptl_absorpt_correction_T_max  0.379
_exptl_absorpt_correction_T_min  0.080
_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 green'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.253
_refine_diff_density_max         2.033
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         13518
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1058P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9968
_reflns_number_total             13518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00554d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7049336--7049339.cif.'
_cod_database_code               7049336
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              55805