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_1565793
_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         'C80 H76 Ce O6 Si4, C4 H8 O, 2[C4 H8 O]'
_chemical_formula_sum            'C84 H84 Ce O7 Si4'
_chemical_formula_weight         1457.99
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-04
_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                 95.951(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5246(6)
_cell_length_b                   23.1693(9)
_cell_length_c                   21.7608(8)
_cell_measurement_reflns_used    4650
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      70.8280
_cell_measurement_theta_min      3.6620
_cell_volume                     8286.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(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 0.988
_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    -96.00 -10.00   1.00   10.00    --  -43.01 -77.00-120.00   86
  2  \w   -117.00 -87.00   1.00   10.00    --  -43.01 -99.00 -30.00   30
  3  \w   -111.00 -79.00   1.00   10.00    --  -43.01 -99.00   0.00   32
  4  \w   -123.00 -98.00   1.00   10.00    --  -43.01 -99.00 -60.00   25
  5  \w    -70.00  27.00   1.00   10.00    --  -43.01  57.00  30.00   97
  6  \w     23.00  85.00   1.00   10.00    --   43.01-125.00-180.00   62
  7  \w     82.00 169.00   1.00   40.00    --  103.80  45.00   0.00   87
  8  \w     42.00 110.00   1.00   40.00    --  103.80-111.00 -90.00   68
  9  \w     23.00 145.00   1.00   40.00    --  103.80 -15.00-180.00  122
 10  \w     34.00 126.00   1.00   40.00    --  103.80 -30.00  60.00   92
 11  \w     34.00 124.00   1.00   40.00    --  103.80 -30.00 -30.00   90
 12  \w     32.00  73.00   1.00   40.00    --  103.80 -94.00 -60.00   41
 13  \w     83.00 112.00   1.00   40.00    --  103.80-111.00-180.00   29
 14  \w     42.00 103.00   1.00   40.00    --  103.80-111.00 120.00   61
 15  \w     86.00 112.00   1.00   40.00    --  103.80-111.00  30.00   26
 16  \w     36.00  63.00   1.00   40.00    --  103.80-111.00  30.00   27
 17  \w     42.00 131.00   1.00   40.00    --  103.80 -77.00 -60.00   89
 18  \w     51.00 131.00   1.00   40.00    --  103.80 -61.00  90.00   80
;
_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      -0.0820052000
_diffrn_orient_matrix_UB_12      -0.0309137000
_diffrn_orient_matrix_UB_13      -0.0158626000
_diffrn_orient_matrix_UB_21      -0.0453069000
_diffrn_orient_matrix_UB_22      0.0571539000
_diffrn_orient_matrix_UB_23      0.0083015000
_diffrn_orient_matrix_UB_31      0.0033987000
_diffrn_orient_matrix_UB_32      0.0139456000
_diffrn_orient_matrix_UB_33      -0.0689126000
_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  0.1352
_diffrn_reflns_av_unetI/netI     0.1193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.554
_diffrn_reflns_theta_min         3.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.180
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
 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    1.169
_exptl_crystal_description       needle
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         8133
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0724P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6071
_reflns_number_total             8133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05517h2.cif
_cod_data_source_block           aw541
_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_database_code               1565793
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C92 H100 Ce O9 Si4'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim C42 \\sim C41: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C42(H42A,
 H42B), C41(H41A,H41B)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C30(H30), C17(H17), C12(H12), C16(H16), C6(H6), C36(H36), C26(H26),
 C5(H5), C8(H8), C29(H29), C27(H27), C28(H28), C2(H2), C4(H4), C24(H24),
 C15(H15), C14(H14), C11(H11), C9(H9), C35(H35), C20(H20), C3(H3), C10(H10),
 C34(H34), C32(H32), C22(H22), C23(H23), C21(H21), C33(H33)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61394
_shelx_hkl_checksum              14838
_shelx_fab_checksum              87003
_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 3.323
_oxdiff_exptl_absorpt_empirical_full_min 0.306