Structure, reactivity and luminescence studies of triphenylsiloxide complexes of tetravalent lanthanides
Willauer, Aurélien R.; Douair, Iskander; Chauvin, Anne-Sophie; Fadaei-Tirani, Farzaneh; Bünzli, Jean-Claude G.; Maron, Laurent; Mazzanti, Marinella; Chemical Science 13 (2022) 681–691; doi:10.1039/D1SC05517H

data_1565796
_publ_section_title
;
 Structure, reactivity and luminescence studies of triphenylsiloxide
 complexes of tetravalent lanthanides
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              681
_journal_page_last               691
_journal_paper_doi               10.1039/D1SC05517H
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C90 H75 K2 Nd O5 Si5, 3(C7 H8), 1[C7H8]'
_chemical_formula_sum            'C111 H99 K2 Nd O5 Si5'
_chemical_formula_weight         1875.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_audit_update_record
;
2021-08-22 deposited with the CCDC.	2021-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2121(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0352(2)
_cell_length_b                   23.9418(2)
_cell_length_c                   22.3713(3)
_cell_measurement_reflns_used    25521
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.5550
_cell_measurement_theta_min      3.4800
_cell_volume                     10187.83(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (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 0.985
_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    -82.00 -39.00   1.00    9.00    --  -40.66 108.00-155.00   43
  2  \w     24.00  78.00   1.00    9.00    --   40.66-108.00 107.00   54
  3  \w    117.00 142.00   1.00   36.00    --  109.35 108.00-155.00   25
  4  \w     40.00  88.00   1.00   36.00    --  109.35-108.00 107.00   48
  5  \w    -70.00  -6.00   1.00    9.00    --  -40.66 125.00 -90.00   64
  6  \w    -53.00 -10.00   1.00    9.00    --  -40.66 125.00-150.00   43
  7  \w   -115.00 -24.00   1.00    9.00    --  -40.66 -38.00  60.00   91
  8  \w   -112.00 -18.00   1.00    9.00    --  -40.66 -38.00 150.00   94
  9  \w     37.00 110.00   1.00    9.00    --   40.66  57.00   0.00   73
 10  \w    105.00 132.00   1.00   36.00    --  109.35 -77.00-120.00   27
 11  \w     53.00  79.00   1.00   36.00    --  109.35 -77.00-120.00   26
 12  \w    103.00 175.00   1.00   36.00    --  109.35  77.00 -90.00   72
 13  \w     38.00 109.00   1.00   36.00    --  109.35-111.00 150.00   71
 14  \w     95.00 177.00   1.00   36.00    --  109.35  45.00-120.00   82
 15  \w     33.00 108.00   1.00   36.00    --  109.35-111.00 -30.00   75
 16  \w     37.00 108.00   1.00   36.00    --  109.35-111.00  60.00   71
 17  \w    122.00 152.00   1.00   36.00    --  109.35 111.00-180.00   30
 18  \w    111.00 159.00   1.00   36.00    --  109.35 111.00  90.00   48
 19  \w     36.00 109.00   1.00   36.00    --  109.35-111.00-150.00   73
 20  \w     87.00 177.00   1.00   36.00    --  109.35  45.00-180.00   90
 21  \w     82.00 109.00   1.00   36.00    --  109.35-111.00-120.00   27
 22  \w    145.00 170.00   1.00   36.00    --  109.35 111.00 -90.00   25
 23  \w     42.00 135.00   1.00   36.00    --  109.35 -45.00 150.00   93
 24  \w    104.00 178.00   1.00   36.00    --  109.35  77.00 120.00   74
;
_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      0.0041215000
_diffrn_orient_matrix_UB_12      -0.0570905000
_diffrn_orient_matrix_UB_13      -0.0313791000
_diffrn_orient_matrix_UB_21      0.0467412000
_diffrn_orient_matrix_UB_22      0.0257811000
_diffrn_orient_matrix_UB_23      -0.0475225000
_diffrn_orient_matrix_UB_31      0.0660410000
_diffrn_orient_matrix_UB_32      -0.0146134000
_diffrn_orient_matrix_UB_33      0.0388192000
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83289
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.881
_diffrn_reflns_theta_min         2.992
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.576
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             3892
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.045
_refine_diff_density_max         3.837
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1182
_refine_ls_number_reflns         20610
_refine_ls_number_restraints     392
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0782P)^2^+7.1585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17408
_reflns_number_total             20610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05517h2.cif
_cod_data_source_block           aw611
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1565790--1565796.cif.
;
_cod_original_cell_volume        10187.8(2)
_cod_database_code               1565796
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C118 H107 K2 Nd O5 Si5'
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.368
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-C25B \\sim Si2-C25A
 with sigma of 0.01
 Si1-C1A \\sim Si1-C1B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C2A \\sim C2B \\sim C3A \\sim C3B \\sim C4A \\sim C4B \\sim
C5A \\sim C5B \\sim C6A \\sim C6B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C25A \\sim C25B \\sim C26A \\sim C26B \\sim C27A \\sim C27B \\sim C28A \\sim
C28B \\sim C29A \\sim C29B \\sim C30A \\sim C30B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=
 Sof(H5B)=Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=FVAR(1)
 Sof(C25B)=Sof(C30B)=Sof(H30B)=Sof(C29B)=Sof(H29B)=Sof(C28B)=Sof(H28B)=
 Sof(C27B)=Sof(H27B)=Sof(C26B)=Sof(H26B)=1-FVAR(2)
 Sof(C25A)=Sof(C30A)=Sof(H30A)=Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=
 Sof(C27A)=Sof(H27A)=Sof(C26A)=Sof(H26A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C2B(H2B), C3B(H3B),
 C4B(H4B), C5B(H5B), C6B(H6B), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C30A(H30A), C29A(H29A), C28A(H28A), C27A(H27A),
 C26A(H26A), C30B(H30B), C29B(H29B), C28B(H28B), C27B(H27B), C26B(H26B),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
 C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
  C77(H77), C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94),
  C95(H95), C96(H96), C99(H99), C100(H100), C101(H101), C102(H102), C103(H103),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110)
5.b Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C1B(C2B,C3B,C4B,C5B,C6B), C25A(C30A,C29A,C28A,C27A,
 C26A), C25B(C30B,C29B,C28B,C27B,C26B)
5.c Idealised Me refined as rotating group:
 C97(H97A,H97B,H97C), C104(H10A,H10B,H10C), C111(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88632
_shelx_hkl_checksum              31667
_shelx_fab_checksum              96333
_olex2_date_sample_data_collection 2020-02-25
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.761
_oxdiff_exptl_absorpt_empirical_full_min 0.635