C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
Palumbo, Chad T.; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b12804

data_4134061
_publ_section_title
;
 C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12804
_journal_year                    2020
_chemical_formula_moiety         'C32 H88 N5 O2 Si8 U2'
_chemical_formula_sum            'C32 H88 N5 O2 Si8 U2'
_chemical_formula_weight         1275.85
_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             2019-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                115.042(4)
_cell_angle_beta                 97.311(4)
_cell_angle_gamma                99.560(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1841(5)
_cell_length_b                   11.6216(6)
_cell_length_c                   11.9725(4)
_cell_measurement_reflns_used    4403
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6840
_cell_measurement_theta_min      4.0690
_cell_volume                     1355.87(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_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   -114.00 -19.00   1.00    6.00    --  -42.88 -57.00-120.00   95
  2  \w   -106.00 -79.00   1.00    6.00    --  -42.88 -99.00-180.00   27
  3  \w    -87.00  -2.00   1.00    6.00    --  -42.88 125.00  90.00   85
  4  \w   -121.00 -81.00   1.00    6.00    --  -42.88 -99.00 -30.00   40
  5  \w    -70.00  28.00   1.00    6.00    --  -42.88  57.00  30.00   98
  6  \w     34.00 132.00   1.00   24.00    --  105.68 -45.00 120.00   98
  7  \w     62.00 127.00   1.00   24.00    --  105.68 -61.00-150.00   65
  8  \w     37.00 138.00   1.00   24.00    --  105.68 -77.00   0.00  101
  9  \w    145.00 173.00   1.00   24.00    --  105.68  77.00  60.00   28
 10  \w     74.00 101.00   1.00   24.00    --  105.68  77.00  60.00   27
 11  \w     37.00  63.00   1.00   24.00    --  105.68-125.00  30.00   26
 12  \w     76.00 111.00   1.00   24.00    --  105.68-125.00  30.00   35
 13  \w     38.00 117.00   1.00   24.00    --  105.68-125.00-180.00   79
 14  \w     95.00 138.00   1.00   24.00    --  105.68 125.00-150.00   43
 15  \w    111.00 177.00   1.00   24.00    --  105.68  45.00-180.00   66
 16  \w     62.00 109.00   1.00   24.00    --  105.68 -94.00-150.00   47
 17  \w    105.00 132.00   1.00   24.00    --  105.68 125.00  60.00   27
 18  \w     42.00 174.00   1.00   24.00    --  105.68   0.00 -30.00  132
;
_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      0.0448109000
_diffrn_orient_matrix_UB_12      0.1394976000
_diffrn_orient_matrix_UB_13      0.0149322000
_diffrn_orient_matrix_UB_21      -0.1357209000
_diffrn_orient_matrix_UB_22      0.0109589000
_diffrn_orient_matrix_UB_23      -0.0191934000
_diffrn_orient_matrix_UB_31      0.0093209000
_diffrn_orient_matrix_UB_32      0.0565003000
_diffrn_orient_matrix_UB_33      0.1435859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9701
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.608
_diffrn_reflns_theta_min         4.110
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.598
_exptl_absorpt_correction_T_max  0.631
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018).
 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 dark black'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             627
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.036
_refine_diff_density_max         2.020
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0267P)^2^+3.9713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4709
_reflns_number_total             5277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12804_si_002.cif
_cod_data_source_block           ctp418
_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 
;
_cod_original_cell_volume        1355.88(11)
_cod_database_code               4134061
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C32 H88 N O6 Si8 U2'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C34A = O1-C31A = O1-C34B = O1-C31B
 1.436 with sigma of 0.02
 C34A-C33A = C32A-C31A = C34B-C33B = C32B-C31B
 1.532 with sigma of 0.02
 C34A-C32A = C33A-C31A = C34B-C32B = C33B-C31B
 2.38 with sigma of 0.04
 C33A-C32A = C33B-C32B
 1.536 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C31A \\sim C31B \\sim C32A \\sim C32B \\sim C33A \\sim C33B \\sim C34A
\\sim C34B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=
 Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C31B(H31C,H31D), C32A(H32A,H32B), C32B(H32C,H32D), C33A(H33A,
 H33B), C33B(H33C,H33D), C34A(H34A,H34B), C34B(H34C,H34D)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_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 1.314
_oxdiff_exptl_absorpt_empirical_full_min 0.706