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_7049338
_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 O36 Si8 Yb4, 1[C6H14]'
_chemical_formula_sum            'C98 H216 O36 Si8 Yb4'
_chemical_formula_weight         2887.57
_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_date             2018-10-02
_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                72.6073(17)
_cell_angle_beta                 80.2421(15)
_cell_angle_gamma                79.3717(13)
_cell_formula_units_Z            1
_cell_length_a                   13.1265(2)
_cell_length_b                   15.6137(3)
_cell_length_c                   18.8708(4)
_cell_measurement_reflns_used    21837
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      76.3010
_cell_measurement_theta_min      4.1890
_cell_volume                     3600.42(12)
_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      140.01(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 0.987
_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   -113.00 -85.00   1.00    1.00    --  -42.88 -99.00 120.00   28
  2  \w   -112.00 -19.00   1.00    1.00    --  -42.88 -57.00 -30.00   93
  3  \w   -124.00 -84.00   1.00    1.00    --  -42.88 -99.00  90.00   40
  4  \w   -117.00 -81.00   1.00    1.00    --  -42.88 -99.00  30.00   36
  5  \w    -70.00  29.00   1.00    1.00    --  -42.88  57.00 120.00   99
  6  \w     25.00  96.00   1.00    1.00    --   42.88-125.00 -60.00   71
  7  \w     24.00  71.00   1.00    1.00    --   42.88-125.00-150.00   47
  8  \w     78.00 138.00   1.00    4.00    --  112.00 -45.00  30.00   60
  9  \w     44.00 119.00   1.00    4.00    --  112.00 -61.00 -60.00   75
 10  \w     64.00  94.00   1.00    4.00    --  112.00 -77.00  90.00   30
 11  \w     53.00  82.00   1.00    4.00    --  112.00 -94.00  30.00   29
 12  \w     45.00  79.00   1.00    4.00    --  112.00 -61.00 150.00   34
 13  \w     90.00 125.00   1.00    4.00    --  112.00  61.00  60.00   35
 14  \w     84.00 111.00   1.00    4.00    --  112.00-111.00  60.00   27
 15  \w     36.00  62.00   1.00    4.00    --  112.00-111.00-150.00   26
 16  \w     38.00 127.00   1.00    4.00    --  112.00 -30.00 150.00   89
 17  \w     95.00 166.00   1.00    4.00    --  112.00  45.00 120.00   71
 18  \w     86.00 113.00   1.00    4.00    --  112.00-111.00 120.00   27
 19  \w     76.00 105.00   1.00    4.00    --  112.00 -94.00-120.00   29
 20  \w     97.00 128.00   1.00    4.00    --  112.00 -61.00-180.00   31
 21  \w     37.00 131.00   1.00    4.00    --  112.00 -30.00 -90.00   94
 22  \w     79.00 113.00   1.00    4.00    --  112.00-111.00   0.00   34
 23  \w     41.00 113.00   1.00    4.00    --  112.00-111.00-180.00   72
 24  \w     36.00 113.00   1.00    4.00    --  112.00-111.00  90.00   77
 25  \w    116.00 167.00   1.00    4.00    --  112.00  45.00 -90.00   51
 26  \w     98.00 139.00   1.00    4.00    --  112.00 -61.00 150.00   41
 27  \w    101.00 126.00   1.00    4.00    --  112.00 -77.00  90.00   25
 28  \w     56.00 113.00   1.00    4.00    --  112.00-111.00-120.00   57
 29  \w     36.00 112.00   1.00    4.00    --  112.00-111.00 -30.00   76
 30  \w    125.00 175.00   1.00    4.00    --  112.00 111.00-150.00   50
 31  \w     38.00 172.00   1.00    4.00    --  112.00   0.00 -90.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0930348000
_diffrn_orient_matrix_UB_12      -0.0764875000
_diffrn_orient_matrix_UB_13      0.0146951000
_diffrn_orient_matrix_UB_21      0.0090014000
_diffrn_orient_matrix_UB_22      0.0216241000
_diffrn_orient_matrix_UB_23      0.0729951000
_diffrn_orient_matrix_UB_31      -0.0757483000
_diffrn_orient_matrix_UB_32      -0.0677742000
_diffrn_orient_matrix_UB_33      0.0434139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38077
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.616
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.768
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.196
_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 yellow'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         14966
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.1235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14260
_reflns_number_total             14966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00554d2.cif
_cod_data_source_block           aw175
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7049336--7049339.cif.
;
_cod_original_cell_volume        3600.41(12)
_cod_database_code               7049338
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C104 H230 O36 Si8 Yb4'
_reflns_odcompleteness_completeness 99.97
_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
 C46A-C45 \\sim C46B-C45 \\sim C47A-C45 \\sim C47B-C45 \\sim C48A-C45 \\sim
C48B-C45
 with sigma of 0.02
 C46A-C47A \\sim C47A-C48A \\sim C48A-C46A \\sim C46B-C47B \\sim C47B-C48B
\\sim C48B-C46B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C46A \\sim C46B \\sim C47A \\sim C47B \\sim C48A \\sim C48B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47B)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47A)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=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), C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F),
 C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F), C48A(H48A,H48B,H48C), C48B(H48D,
 H48E,H48F), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 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 1.478
_oxdiff_exptl_absorpt_empirical_full_min 0.751