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_4134387
_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         'C76 H66 N2 O4 Pr Si4, 0.5(C2 H3 N)'
_chemical_formula_sum            'C77 H67.5 N2.5 O4 Pr Si4'
_chemical_formula_weight         1345.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-19
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_b                   24.2398(3)
_cell_length_c                   25.1777(3)
_cell_measurement_reflns_used    82582
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      32.4210
_cell_measurement_theta_min      2.9430
_cell_volume                     13718.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (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
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_diffrn_measured_fraction_theta_max 0.998
_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    -42.00  15.00   1.00   35.00    --  -17.94 -77.00  60.00   57
  2  \w    -28.00  15.00   1.00   35.00    --  -17.94 -77.00-180.00   43
  3  \w    -53.00  51.00   1.00   35.00    --   18.87 -19.00-120.00  104
  4  \w    -41.00  41.00   1.00   35.00    --   18.87 -37.00   0.00   82
  5  \w     10.00  90.00   1.00   35.00    --   18.87  37.00 -30.00   80
  6  \w     -3.00  93.00   1.00   35.00    --   18.87  37.00  60.00   96
  7  \w      8.00  77.00   1.00   35.00    --   18.87-128.00-118.56   69
  8  \w     -5.00  79.00   1.00   35.00    --   18.87  37.00-120.00   84
  9  \w     40.00  74.00   1.00   35.00    --   20.00-122.00  -9.48   34
 10  \w     -2.00  71.00   1.00   35.00    --   20.00-116.00 144.08   73
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
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_diffrn_orient_matrix_UB_12      -0.0202382000
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_diffrn_orient_matrix_UB_21      0.0299637000
_diffrn_orient_matrix_UB_22      -0.0090523000
_diffrn_orient_matrix_UB_23      0.0013922000
_diffrn_orient_matrix_UB_31      -0.0078813000
_diffrn_orient_matrix_UB_32      -0.0190917000
_diffrn_orient_matrix_UB_33      0.0201509000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            202106
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (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 intense red'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prism
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.131
_refine_diff_density_max         5.499
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.463(10)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1600
_refine_ls_number_reflns         24214
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0736P)^2^+8.0986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22118
_reflns_number_total             24214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01204_si_002.cif
_cod_data_source_block           2-PrPh_AW550
_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/ACS/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 4134387--4134389.cif.

2020-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C154 H135 N5 O8 Pr2 Si8'
_cod_original_formula_weight         2690.20
_cod_original_formula_moiety         '2(C76 H66 N2 O4 Pr Si4), C2 H3 N'
_cod_original_formula_units_Z            4
_cod_database_code               4134387
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C77 H67 N2.50 O4 Pr Si4'
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.822
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.537(10)
 0.463(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
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 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), C78(H78), C79(H79),
  C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87),
 C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
  C98(H98), C99(H99), C100(H100), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C120(H120), C121(H121), C122(H122), C123(H123), C124(H124), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C138(H138), C139(H139), C140(H140),
 C141(H141), C142(H142), C144(H144), C145(H145), C146(H146), C147(H147),
 C148(H148)
3.b Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C150(H15A,H15B,H15C), C152(H15D,
 H15E,H15F), C154(H15G,H15H,H15I)
;
_shelx_res_checksum              78090
_shelx_hkl_checksum              77406
_olex2_date_sample_data_collection 2019-12-18
_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 1.295
_oxdiff_exptl_absorpt_empirical_full_min 0.827