Accessing the +IV Oxidation State in Molecular Complexes of Praseodymium.
Willauer, Aurélien R; Palumbo, Chad T.; Fadaei-Tirani, Farzaneh; Zivkovic, Ivica; Douair, Iskander; Maron, Laurent; Mazzanti, Marinella; Journal of the American Chemical Society 142 (2020) 5538–5542; doi:10.1021/jacs.0c01204

data_4134388
_publ_section_title
;
 Accessing the +IV Oxidation State in Molecular Complexes of Praseodymium.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5538
_journal_page_last               5542
_journal_paper_doi               10.1021/jacs.0c01204
_journal_volume                  142
_journal_year                    2020
_chemical_formula_sum            'C84 H84 K O7 Pr Si4'
_chemical_formula_weight         1497.88
_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_method           SHELXL-2018/3
_cell_angle_alpha                83.344(5)
_cell_angle_beta                 81.037(5)
_cell_angle_gamma                64.588(6)
_cell_formula_units_Z            2
_cell_length_a                   13.1036(8)
_cell_length_b                   14.9076(10)
_cell_length_c                   22.4578(12)
_cell_measurement_reflns_used    6926
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5740
_cell_measurement_theta_min      3.7190
_cell_volume                     3908.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Mercury 4.3.0 (CCDC, 2019)'
_computing_publication_material  'CIFTab (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (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 0.961
_diffrn_measured_fraction_theta_max 0.939
_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   -110.00 -66.00   1.00   10.00    --  -40.66-140.00 134.00   44
  2  \w    -73.00 -48.00   1.00   10.00    --  -40.66 129.00  20.00   25
  3  \w    -78.00 -53.00   1.00   10.00    --  -40.66 140.00-166.00   25
  4  \w     40.00  65.00   1.00   10.00    --   40.66-129.00 -52.00   25
  5  \w     44.00  70.00   1.00   10.00    --   40.66-140.00 134.00   26
  6  \w     47.00 110.00   1.00   40.00    --  105.15-129.00 -52.00   63
  7  \w    117.00 172.00   1.00   40.00    --  105.15 140.00-166.00   55
  8  \w     55.00  80.00   1.00   40.00    --  105.15-140.00 134.00   25
  9  \w     96.00 124.00   1.00   40.00    --  105.15 129.00  20.00   28
 10  \w   -112.00 -14.00   1.00   10.00    --  -40.66 -57.00  30.00   98
 11  \w   -112.00 -16.00   1.00   10.00    --  -40.66 -38.00 120.00   96
 12  \w     47.00  90.00   1.00   10.00    --   40.66-125.00   0.00   43
 13  \w     18.00 106.00   1.00   10.00    --   40.66  38.00 -30.00   88
 14  \w      7.00  74.00   1.00   10.00    --   40.66 -99.00-150.00   67
 15  \w    121.00 148.00   1.00   40.00    --  105.15  77.00-120.00   27
 16  \w     25.00  97.00   1.00   40.00    --  105.15 -94.00 120.00   72
 17  \w     33.00 134.00   1.00   40.00    --  105.15 -61.00 -90.00  101
 18  \w     46.00  72.00   1.00   40.00    --  105.15-111.00   0.00   26
 19  \w    110.00 178.00   1.00   40.00    --  105.15 111.00 -30.00   68
 20  \w     79.00 108.00   1.00   40.00    --  105.15-111.00   0.00   29
 21  \w     91.00 177.00   1.00   40.00    --  105.15  45.00  60.00   86
 22  \w    104.00 177.00   1.00   40.00    --  105.15  77.00  90.00   73
 23  \w     30.00  75.00   1.00   40.00    --  105.15-111.00-150.00   45
 24  \w     29.00  55.00   1.00   40.00    --  105.15 -94.00  30.00   26
 25  \w     76.00 109.00   1.00   40.00    --  105.15-111.00-150.00   33
 26  \w     73.00 104.00   1.00   40.00    --  105.15 -94.00  30.00   31
 27  \w    103.00 175.00   1.00   40.00    --  105.15  77.00   0.00   72
 28  \w     48.00  77.00   1.00   40.00    --  105.15 -45.00  90.00   29
 29  \w     85.00 178.00   1.00   40.00    --  105.15  30.00 150.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16598
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.832
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.254
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       plate
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.071
_refine_diff_density_max         5.287
_refine_diff_density_min         -2.552
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         16598
_refine_ls_number_restraints     1293
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2981
_refine_ls_wR_factor_ref         0.3102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11824
_reflns_number_total             16598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01204_si_004.cif
_cod_data_source_block           aw369_sq
_cod_depositor_comments
'Adding full bibliography for 4134387--4134389.cif.'
_cod_database_code               4134388
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.315
_shelx_estimated_absorpt_t_max   0.665
_shelx_res_checksum              5218
_shelx_hkl_checksum              36824
_shelx_fab_checksum              81835