Isolation and redox reactivity of cerium complexes in four redox states.
Hsueh, Fang-Che; Rajeshkumar, Thayalan; Maron, Laurent; Scopelliti, Rosario; Sienkiewicz, Andrzej; Mazzanti, Marinella; Chemical science 14 (2023) 6011–6021; doi:10.1039/d3sc01478a

data_1569056
_publ_section_title
;
 Isolation and redox reactivity of cerium complexes in four redox states.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              6011
_journal_page_last               6021
_journal_paper_doi               10.1039/d3sc01478a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C48 H69 Cl3 O6 Si3'
_chemical_formula_sum            'C48 H69 Cl3 O6 Si3'
_chemical_formula_weight         932.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                112.760(4)
_cell_angle_beta                 91.008(3)
_cell_angle_gamma                93.713(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7393(4)
_cell_length_b                   13.7546(5)
_cell_length_c                   14.7849(6)
_cell_measurement_reflns_used    11627
_cell_measurement_temperature    140.00(11)
_cell_measurement_theta_max      72.4870
_cell_measurement_theta_min      3.1680
_cell_volume                     2568.30(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_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   -115.00 -84.00   1.00    7.50    --  -43.13-139.00 -86.00   31
  2  \w    -52.00 -25.00   1.00    7.50    --  -43.13 131.00 159.00   27
  3  \w    -80.00 -55.00   1.00    7.50    --  -43.13 139.00 -25.00   25
  4  \w     46.00  73.00   1.00    7.50    --   43.13-131.00  88.00   27
  5  \w     58.00  97.00   1.00    7.50    --   43.13-139.00 -86.00   39
  6  \w     71.00  97.00   1.00   30.00    --  103.80-131.00  88.00   26
  7  \w    108.00 133.00   1.00   30.00    --  103.80 139.00 -25.00   25
  8  \w     36.00 121.00   1.00   30.00    --  103.80-139.00 -86.00   85
  9  \w    111.00 136.00   1.00   30.00    --  103.80 131.00 159.00   25
 10  \w   -115.00 -15.00   1.00    7.50    --  -43.13 -57.00-180.00  100
 11  \w   -116.00 -19.00   1.00    7.50    --  -43.13 -37.00 -90.00   97
 12  \w    -21.00  74.00   1.00    7.50    --   43.13 -77.00  60.00   95
 13  \w    104.00 150.00   1.00   30.00    --  103.80 111.00  30.00   46
 14  \w     50.00 107.00   1.00   30.00    --  103.80-111.00  90.00   57
 15  \w     44.00  70.00   1.00   30.00    --  103.80-111.00   0.00   26
 16  \w    121.00 176.00   1.00   30.00    --  103.80 111.00-120.00   55
 17  \w     45.00 108.00   1.00   30.00    --  103.80-111.00-180.00   63
 18  \w     89.00 117.00   1.00   30.00    --  103.80 178.00 -90.00   28
 19  \w     77.00 177.00   1.00   30.00    --  103.80  30.00-180.00  100
 20  \w    105.00 136.00   1.00   30.00    --  103.80 -77.00-120.00   31
 21  \w     35.00 104.00   1.00   30.00    --  103.80-111.00 -30.00   69
 22  \w     83.00 108.00   1.00   30.00    --  103.80-111.00   0.00   25
 23  \w     31.00  81.00   1.00   30.00    --  103.80 -77.00-120.00   50
 24  \w     29.00 128.00   1.00   30.00    --  103.80 -30.00 -60.00   99
 25  \w     99.00 147.00   1.00   30.00    --  103.80  45.00-150.00   48
 26  \w    104.00 135.00   1.00   30.00    --  103.80  77.00 -60.00   31
 27  \w     85.00 176.00   1.00   30.00    --  103.80  61.00  90.00   91
;
_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      -0.0632689000
_diffrn_orient_matrix_UB_12      -0.0938719000
_diffrn_orient_matrix_UB_13      -0.0754589000
_diffrn_orient_matrix_UB_21      0.0929334000
_diffrn_orient_matrix_UB_22      -0.0546329000
_diffrn_orient_matrix_UB_23      -0.0421552000
_diffrn_orient_matrix_UB_31      -0.0036562000
_diffrn_orient_matrix_UB_32      -0.0551880000
_diffrn_orient_matrix_UB_33      0.0729709000
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23460
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.784
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0496P)^2^+0.6680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8126
_reflns_number_total             9934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01478a2.cif
_cod_data_source_block           ah348
_cod_depositor_comments
'Adding full bibliography for 1569056--1569065.cif.'
_cod_original_cell_volume        2568.28(17)
_cod_database_code               1569056
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H69 O6 Si3 Cl3'
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.659
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C22(H22),
 C23(H23), C24(H24), C25(H25), C36(H36), C37(H37), C38(H38), C39(H39)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              42285
_shelx_hkl_checksum              82664
_olex2_date_sample_data_collection 2022-03-03
_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 1.377
_oxdiff_exptl_absorpt_empirical_full_min 0.747