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_7049339
_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         'C98 H216 O38 Si8 Sm4, 2[C6H14]'
_chemical_formula_sum            'C98 H216 O38 Si8 Sm4'
_chemical_formula_weight         2828.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-04 deposited with the CCDC.    2019-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.606(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.217(2)
_cell_length_b                   14.6315(7)
_cell_length_c                   30.140(2)
_cell_measurement_reflns_used    7665
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.7670
_cell_measurement_theta_min      3.2910
_cell_volume                     15088.6(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_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 0.965
_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    -68.00  32.00   1.00   10.00    --  -40.41  57.00  60.00  100
  2  \w   -103.00  -8.00   1.00   10.00    --  -40.41 -77.00 -90.00   95
  3  \w   -114.00 -13.00   1.00   10.00    --  -40.41 -57.00 150.00  101
  4  \w     27.00  54.00   1.00   10.00    --   40.41  38.00-180.00   27
  5  \w     24.00  81.00   1.00   10.00    --   40.41 -99.00  90.00   57
  6  \w     67.00 115.00   1.00   40.00    --  107.03-125.00-120.00   48
  7  \w     34.00 118.00   1.00   40.00    --  107.03-125.00   0.00   84
  8  \w     67.00 109.00   1.00   40.00    --  107.03 -94.00  30.00   42
  9  \w     85.00 113.00   1.00   40.00    --  107.03-125.00-180.00   28
 10  \w    115.00 171.00   1.00   40.00    --  107.03 125.00 120.00   56
 11  \w     32.00 114.00   1.00   40.00    --  107.03 -30.00-180.00   82
 12  \w    100.00 150.00   1.00   40.00    --  107.03 125.00 150.00   50
 13  \w     36.00 134.00   1.00   40.00    --  107.03 -61.00  30.00   98
 14  \w     81.00 165.00   1.00   40.00    --  107.03  45.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0279455000
_diffrn_orient_matrix_UB_12      0.0283823000
_diffrn_orient_matrix_UB_13      0.0371993000
_diffrn_orient_matrix_UB_21      -0.0256549000
_diffrn_orient_matrix_UB_22      0.0519624000
_diffrn_orient_matrix_UB_23      -0.0340174000
_diffrn_orient_matrix_UB_31      -0.0243159000
_diffrn_orient_matrix_UB_32      -0.0871041000
_diffrn_orient_matrix_UB_33      -0.0081656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            37370
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.626
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 pale colourless'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       plate
_exptl_crystal_F_000             5872
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.069
_refine_diff_density_max         2.324
_refine_diff_density_min         -2.707
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         12866
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0861P)^2^+139.9905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9253
_reflns_number_total             12866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00554d2.cif
_cod_data_source_block           aw170
_cod_depositor_comments
'Adding full bibliography for 7049336--7049339.cif.'
_cod_original_cell_volume        15088.5(16)
_cod_database_code               7049339
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C98 H216 O38 Si8 Sm4'
_reflns_odcompleteness_completeness 95.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C50A-C49 \\sim C51A-C49 \\sim C52A-C49 \\sim C50B-C49 \\sim C51B-C49 \\sim
C52B-C49
 with sigma of 0.02
 C50A-C51A \\sim C51A-C52A \\sim C52A-C50A \\sim C50B-C51B \\sim C51B-C52B
\\sim C52B-C50B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49 \\sim C50A \\sim C50B \\sim C51A \\sim C51B \\sim C52A \\sim C52B: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C50B)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C51B)=Sof(H51D)=Sof(H51E)=
 Sof(H51F)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51A)=Sof(H51A)=Sof(H51B)=
 Sof(H51C)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C50A(H50A,H50B,H50C), C50B(H50D,H50E,H50F), C51A(H51A,
 H51B,H51C), C51B(H51D,H51E,H51F), C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 4.938
_oxdiff_exptl_absorpt_empirical_full_min 0.180