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_4134389
_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_moiety
'C72 H162 Cl3 K3 O24 Pr2 Si6, 2(C6 H18 O Si2)'
_chemical_formula_sum            'C84 H198 Cl3 K3 O26 Pr2 Si10'
_chemical_formula_weight         2410.78
_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_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.9196(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.6668(3)
_cell_length_b                   15.04611(14)
_cell_length_c                   33.6749(3)
_cell_measurement_reflns_used    29108
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      73.3470
_cell_measurement_theta_min      3.5350
_cell_volume                     12935.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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    -62.00  34.00   1.00    3.00    --  -40.66  38.00   0.00   96
  2  \w   -113.00 -22.00   1.00    3.00    --  -40.66 -57.00  60.00   91
  3  \w    -68.00  26.00   1.00    3.00    --  -40.66  57.00-150.00   94
  4  \w     26.00  71.00   1.00    3.00    --   40.66-125.00 -90.00   45
  5  \w     23.00  82.00   1.00    3.00    --   40.66 -99.00   0.00   59
  6  \w    124.00 174.00   1.00   12.00    --  107.03 125.00  60.00   50
  7  \w     66.00 114.00   1.00   12.00    --  107.03-125.00 -60.00   48
  8  \w     78.00 177.00   1.00   12.00    --  107.03  77.00  30.00   99
  9  \w     86.00 112.00   1.00   12.00    --  107.03  45.00-120.00   26
 10  \w     85.00 115.00   1.00   12.00    --  107.03-125.00-180.00   30
 11  \w     88.00 178.00   1.00   12.00    --  107.03  45.00  90.00   90
 12  \w     39.00  66.00   1.00   12.00    --  107.03-125.00  60.00   27
 13  \w     90.00 116.00   1.00   12.00    --  107.03-125.00  60.00   26
 14  \w     63.00 127.00   1.00   12.00    --  107.03 -61.00  60.00   64
 15  \w     84.00 168.00   1.00   12.00    --  107.03  30.00-180.00   84
 16  \w     32.00 139.00   1.00   12.00    --  107.03 -77.00 -30.00  107
 17  \w    139.00 168.00   1.00   12.00    --  107.03  61.00 120.00   29
 18  \w    105.00 172.00   1.00   12.00    --  107.03 125.00 -30.00   67
 19  \w     78.00 117.00   1.00   12.00    --  107.03  61.00 120.00   39
;
_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_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            42821
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.620
_diffrn_reflns_theta_min         2.638
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.492
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.238
_exptl_crystal_description       prism
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.302
_refine_diff_density_max         1.772
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         12853
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+22.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12627
_reflns_number_total             12853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01204_si_003.cif
_cod_data_source_block           aw315
_cod_depositor_comments
'Adding full bibliography for 4134387--4134389.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4134389
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.127
_shelx_estimated_absorpt_t_max   0.184
_shelx_res_checksum              65455
_shelx_hkl_checksum              83548