Cation assisted binding and cleavage of dinitrogen by uranium complexes
Jori, Nadir; Rajeshkumar, Thayalan; Scopelliti, Rosario; Z̆ivković, Ivica; Sienkiewicz, Andrzej; Maron, Laurent; Mazzanti, Marinella; Chemical Science 13 (2022) 9232–9242; doi:10.1039/D2SC02530B

data_1567305
_publ_section_title
;
 Cation assisted binding and cleavage of dinitrogen by uranium complexes
;
_journal_issue                   32
_journal_name_full               'Chemical Science'
_journal_page_first              9232
_journal_page_last               9242
_journal_paper_doi               10.1039/D2SC02530B
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C72 H162 Cs2 O25 Si6 U2'
_chemical_formula_sum            'C72 H162 Cs2 O25 Si6 U2'
_chemical_formula_weight         2338.455
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_Int_Tables_number      88
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-28 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.3833(4)
_cell_length_b                   25.3833(4)
_cell_length_c                   65.6666(17)
_cell_measurement_reflns_used    14002
_cell_measurement_temperature    140.1(5)
_cell_measurement_theta_max      72.6430
_cell_measurement_theta_min      2.7820
_cell_volume                     42309.8(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.1(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_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   -118.00  -7.00   0.75    5.00    --  -40.85 -19.00  90.00  148
  2  \w    -90.00  -3.00   0.75    5.00    --  -40.85 125.00-180.00  116
  3  \w   -113.00 -26.00   0.75    5.00    --  -40.85 -38.00  30.00  116
  4  \w     31.00  61.00   0.75    5.00    --   40.85-125.00   0.00   40
  5  \w     42.00  96.00   0.75    5.00    --   40.85-125.00  90.00   72
  6  \w      5.00  31.25   0.75    5.00    --   40.85 -99.00   0.00   35
  7  \w     34.00 118.00   0.75   20.00    --  107.03-125.00-150.00  112
  8  \w     79.00 176.50   0.75   20.00    --  107.03  30.00  90.00  130
  9  \w     41.00 125.00   0.75   20.00    --  107.03 -61.00-180.00  112
 10  \w    102.00 172.50   0.75   20.00    --  107.03  30.00   0.00   94
 11  \w     96.00 135.00   0.75   20.00    --  107.03 125.00   0.00   52
 12  \w    153.00 178.50   0.75   20.00    --  107.03 125.00   0.00   34
 13  \w     29.00  97.25   0.75   20.00    --  107.03 -94.00  90.00   91
 14  \w    107.00 132.50   0.75   20.00    --  107.03 -45.00  60.00   34
 15  \w     81.00 114.00   0.75   20.00    --  107.03-125.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0165033000
_diffrn_orient_matrix_UB_12      0.0015797000
_diffrn_orient_matrix_UB_13      -0.0225788000
_diffrn_orient_matrix_UB_21      0.0560390000
_diffrn_orient_matrix_UB_22      -0.0176677000
_diffrn_orient_matrix_UB_23      0.0059343000
_diffrn_orient_matrix_UB_31      -0.0165905000
_diffrn_orient_matrix_UB_32      -0.0579706000
_diffrn_orient_matrix_UB_33      -0.0024375000
_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  0.1469
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            113244
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9991
_diffrn_reflns_theta_full        66.5982
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         2.67
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.977
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.56a (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    1.468
_exptl_crystal_description       plate
_exptl_crystal_F_000             18687.403
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.7267
_refine_diff_density_min         -2.6391
_refine_diff_density_rms         0.3188
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             16.5767
_refine_ls_goodness_of_fit_ref   1.0072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    229
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         18706
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.0037
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              30
_reflns_limit_h_min              0
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              78
_reflns_limit_l_min              0
_reflns_number_gt                12278
_reflns_number_total             18706
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc02530b2.cif
_cod_data_source_block           NJ189n2
_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 1567298--1567305.cif.
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1567305
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C72 H162 Cs2 O25 Si6 U2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C92-C89 = C104-C101 = C102-C101 = C3A-C1 = C2A-C1 = C4A-C1 = C1-C4B = C1-C3B =
  C1-C2B
 1.54 with sigma of 0.01
 C2A-C4A \\sim C4A-C3A \\sim C3A-C2A \\sim C4B-C3B \\sim C3B-C2B \\sim C4B-C3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C101 \\sim C102 \\sim C103 \\sim C104:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C1 \\sim C2A \\sim C2B \\sim C3A \\sim C3B \\sim C4A \\sim C4B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C2B)=Sof(H2Ba)=Sof(H2Bb)=Sof(H2Bc)=Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(H3Bc)=
 Sof(C4B)=Sof(H4Ba)=Sof(H4Bb)=Sof(H4Bc)=1-FVAR(1)
 Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=
 Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C2A(H2Aa,H2Ab,H2Ac), C2B(H2Ba,H2Bb,H2Bc), C3A(H3Aa,H3Ab,H3Ac), C3B(H3Ba,H3Bb,
 H3Bc), C4A(H4Aa,H4Ab,H4Ac), C4B(H4Ba,H4Bb,H4Bc), C6(H6a,H6b,H6c), C7(H7a,H7b,
 H7c), C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,
 H12c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C26(H26a,
 H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C30(H30a,H30b,H30c),
 C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C42(H42a,H42b,H42c), C43(H43a,H43b,
 H43c), C44(H44a,H44b,H44c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,
 H48b,H48c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C52(H52a,H52b,H52c),
 C62(H62a,H62b,H62c), C63(H63a,H63b,H63c), C64(H64a,H64b,H64c), C66(H66a,H66b,
 H66c), C67(H67a,H67b,H67c), C68(H68a,H68b,H68c), C70(H70a,H70b,H70c), C71(H71a,
 H71b,H71c), C72(H72a,H72b,H72c), C82(H82a,H82b,H82c), C83(H83a,H83b,H83c),
 C84(H84a,H84b,H84c), C86(H86a,H86b,H86c), C87(H87a,H87b,H87c), C88(H88a,H88b,
 H88c), C90(H90a,H90b,H90c), C91(H91a,H91b,H91c), C92(H92a,H92b,H92c),
 C102(H10d,H10e,H10f), C103(H10g,H10h,H10i), C104(H10j,H10k,H10l), C106(H10m,
 H10n,H10o), C107(H10p,H10q,H10r), C108(H10s,H10t,H10u), C110(H11d,H11e,H11f),
 C111(H11g,H11h,H11i), C112(H11j,H11k,H11l)
;
_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 4.051
_oxdiff_exptl_absorpt_empirical_full_min 0.320