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_1565792
_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         'C92 H78 N O5 P Pr Si4, 1[C7H8]'
_chemical_formula_sum            'C92 H78 N O5 P Pr Si4'
_chemical_formula_weight         1561.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-22 deposited with the CCDC.	2021-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3627(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.39059(14)
_cell_length_b                   21.1314(2)
_cell_length_c                   28.0674(3)
_cell_measurement_reflns_used    37935
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.3080
_cell_measurement_theta_min      2.5810
_cell_volume                     8532.69(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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     64.00 109.00   0.50    0.50    --   59.82  30.00-120.00   90
  2  \w     78.00 105.00   0.50    0.50    --   59.82  30.00 -90.00   54
  3  \w     75.00 102.00   0.50    0.50    --   59.82  30.00 -30.00   54
  4  \w     78.00 106.00   0.50    0.50    --   59.82  30.00 150.00   56
  5  \w     61.00 109.00   0.50    0.50    --   59.82  30.00 120.00   96
  6  \w     11.00  37.00   0.50    0.50    --   59.82 -30.00 120.00   52
  7  \w   -109.00 -83.00   0.50    0.50    --  -62.25 -30.00  30.00   52
  8  \w   -106.00 -40.00   0.50    0.50    --  -71.33 -15.00 150.00  132
  9  \w   -114.00 -79.00   0.50    0.50    --  -71.33 -30.00 120.00   70
 10  \w     33.00  72.00   0.50    2.00    --   71.95 -95.00  60.00   78
 11  \w     32.00  72.00   0.50    2.00    --   71.95 -95.00 150.00   80
 12  \w     41.00  84.00   0.50    2.00    --   73.61 -95.00  90.00   86
 13  \w     35.00  61.00   0.50    2.00    --   73.61 -95.00 -30.00   52
 14  \w     78.00 122.00   0.50    2.00    --   73.61  30.00-180.00   88
 15  \w   -106.00 -37.00   0.50    2.00    --  -76.05 125.00 150.00  138
 16  \w   -108.00 -78.00   0.50    2.00    --  -76.05 -30.00   0.00   60
 17  \w   -124.00 -78.00   0.50    2.00    --  -76.05 -30.00 -30.00   92
 18  \w   -107.00 -37.00   0.50    2.00    --  -76.05 125.00-150.00  140
 19  \w   -107.00 -44.00   0.50    2.00    --  -76.05 125.00 -60.00  126
 20  \w   -123.00 -43.00   0.50    2.00    --  -76.05 -15.00-120.00  160
 21  \w   -120.00 -78.00   0.50    2.00    --  -76.05-125.00 -90.00   84
 22  \w     41.00  70.00   0.50    2.00    --   81.25 -95.00 120.00   58
 23  \w     86.00 111.00   0.50    2.00    --   81.25-125.00-150.00   50
 24  \w     44.00  75.00   0.50    2.00    --   81.25-125.00-150.00   62
 25  \w     41.00  69.00   0.50    2.00    --   81.25 -95.00-120.00   56
 26  \w     79.00 123.00   0.50    2.00    --   81.25 125.00  30.00   88
 27  \w     91.00 123.00   0.50    2.00    --   81.25 125.00 120.00   64
 28  \w     84.00 110.00   0.50    2.00    --   81.25-125.00 120.00   52
 29  \w     35.00 111.00   0.50    2.00    --   81.25-125.00  60.00  152
 30  \w     39.00  65.00   0.50    2.00    --   81.25-125.00 120.00   52
 31  \w    101.00 127.00   0.50    2.00    --   81.25 125.00-120.00   52
 32  \w     39.00 111.00   0.50    2.00    --   81.25-125.00 -30.00  144
 33  \w     81.00 111.00   0.50    2.00    --   81.25-125.00-180.00   60
 34  \w     84.00 109.00   0.50    2.00    --   81.25-125.00   0.00   50
 35  \w     43.00  75.00   0.50    2.00    --   81.25-125.00   0.00   64
 36  \w     91.00 116.00   0.50    2.00    --   81.25 125.00  90.00   50
 37  \w     99.00 126.00   0.50    2.00    --   81.25 125.00-180.00   54
 38  \w     41.00  66.00   0.50    2.00    --   81.25 -95.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1039181000
_diffrn_orient_matrix_UB_12      -0.0132737000
_diffrn_orient_matrix_UB_13      0.0100640000
_diffrn_orient_matrix_UB_21      0.0257945000
_diffrn_orient_matrix_UB_22      0.0587053000
_diffrn_orient_matrix_UB_23      -0.0294269000
_diffrn_orient_matrix_UB_31      -0.0032392000
_diffrn_orient_matrix_UB_32      0.0410717000
_diffrn_orient_matrix_UB_33      0.0452578000
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            107006
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.357
_diffrn_reflns_theta_min         2.618
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.484
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
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 intense orange'
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       plate
_exptl_crystal_F_000             3228
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         17163
_refine_ls_number_restraints     1757
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+7.4935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14419
_reflns_number_total             17163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05517h2.cif
_cod_data_source_block           aw844
_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        8532.71(14)
_cod_database_code               1565792
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C92 H78 N O5 P Pr Si4'
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.610
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 Si4-C79A \\sim Si4-C79B
 with sigma of 0.02
 P1-C1A \\sim P1-C1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C6A \\sim C5A \\sim C4A \\sim C3A \\sim C2A \\sim C1B \\sim C2B \\sim
C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim
C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim
C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79A \\sim C84A \\sim C83A \\sim C82A
\\sim C81A \\sim C80A \\sim C79B \\sim C84B \\sim C83B \\sim C82B \\sim C81B
\\sim C80B \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim
C91 \\sim C92: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=
 Sof(H3A)=Sof(C2A)=Sof(H2A)=FVAR(1)
 Sof(C79B)=Sof(C84B)=Sof(H84B)=Sof(C83B)=Sof(H83B)=Sof(C82B)=Sof(H82B)=
 Sof(C81B)=Sof(H81B)=Sof(C80B)=Sof(H80B)=1-FVAR(2)
 Sof(C79A)=Sof(C84A)=Sof(H84A)=Sof(C83A)=Sof(H83A)=Sof(C82A)=Sof(H82A)=
 Sof(C81A)=Sof(H81A)=Sof(C80A)=Sof(H80A)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A), 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), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 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), C84A(H84A), C83A(H83A), C82A(H82A), C81A(H81A),
 C80A(H80A), C84B(H84B), C83B(H83B), C82B(H82B), C81B(H81B), C80B(H80B),
 C86(H86), C87(H87), C88(H88), C89(H89), C90(H90)
6.b Fitted hexagon refined as free rotating group:
 C1A(C6A,C5A,C4A,C3A,C2A), C1B(C2B,C3B,C4B,C5B,C6B), C79A(C84A,C83A,C82A,C81A,
 C80A), C79B(C84B,C83B,C82B,C81B,C80B)
6.c Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94639
_shelx_hkl_checksum              74778
_shelx_fab_checksum              38365
_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 1.826
_oxdiff_exptl_absorpt_empirical_full_min 0.656