Nitrogen activation and cleavage by a multimetallic uranium complex.
Keener, Megan; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Chemical science 13 (2022) 8025–8035; doi:10.1039/d2sc02997a

data_1567204
_publ_section_title
;
 Nitrogen activation and cleavage by a multimetallic uranium complex.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              8025
_journal_page_last               8035
_journal_paper_doi               10.1039/d2sc02997a
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C60 H144 Cs2 N3 O16 Si8 U2, 0.5[C6H14]'
_chemical_formula_sum            'C60 H144 Cs2 N3 O16 Si8 U2'
_chemical_formula_weight         2130.37
_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             2022-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-11 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                94.2273(11)
_cell_angle_beta                 97.0402(12)
_cell_angle_gamma                117.4870(16)
_cell_formula_units_Z            2
_cell_length_a                   13.7070(2)
_cell_length_b                   13.7678(2)
_cell_length_c                   29.7454(4)
_cell_measurement_reflns_used    26692
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.9390
_cell_measurement_theta_min      3.0000
_cell_volume                     4887.79(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.942
_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     75.00 119.00   0.50    1.00    --   73.64  30.00 -30.00   88
  2  \w     84.00 109.00   0.50    0.50    --   59.87  30.00-150.00   50
  3  \w     87.00 115.00   0.50    1.00    --   73.64  30.00-120.00   56
  4  \w     83.00 127.00   0.50    1.00    --   81.22  30.00 -90.00   88
  5  \w     39.00 119.00   0.50    1.00    --   71.88  15.00  30.00  160
  6  \w     83.00 130.00   0.50    1.00    --   81.22  30.00  30.00   94
  7  \w     79.00 122.00   0.50    1.00    --   73.64  30.00 120.00   86
  8  \w     64.00 109.00   0.50    0.50    --   59.87  30.00 150.00   90
  9  \w     11.00  37.00   0.50    0.50    --   59.87 -30.00-120.00   52
 10  \w     11.00  37.00   0.50    0.50    --   59.87 -30.00-180.00   52
 11  \w     12.00  37.00   0.50    0.50    --   59.87 -30.00-150.00   50
 12  \w     11.00  37.00   0.50    0.50    --   59.87 -30.00 -90.00   52
 13  \w     11.00  37.00   0.50    0.50    --   59.87 -30.00 -60.00   52
 14  \w     11.00  36.00   0.50    0.50    --   59.87 -30.00   0.00   50
 15  \w     45.00  79.00   0.50    1.00    --   81.22 -95.00 -60.00   68
 16  \w     77.00 112.00   0.50    1.00    --   81.22-125.00-120.00   70
 17  \w     87.00 112.00   0.50    1.00    --   81.22-125.00-180.00   50
 18  \w     35.00  60.00   0.50    1.00    --   81.22-125.00-180.00   50
 19  \w     35.00  74.00   0.50    1.00    --   81.22-125.00-120.00   78
 20  \w     72.00 105.00   0.50    1.00    --   81.22-112.00 -55.00   66
 21  \w     39.00  64.00   0.50    1.00    --   73.64-112.00 -55.00   50
 22  \w     48.00  89.00   0.50    1.00    --   81.22 -95.00-150.00   82
 23  \w     30.00  55.00   0.50    0.50    --   59.87-112.00 -55.00   50
 24  \w     29.00  62.00   0.50    1.00    --   71.88-112.00 -55.00   66
 25  \w     33.00  82.00   0.50    1.00    --   71.88 -95.00   0.00   98
 26  \w     36.00 112.00   0.50    1.00    --   81.22-125.00  60.00  152
 27  \w     86.00 111.00   0.50    1.00    --   81.22-125.00  90.00   50
 28  \w     42.00  78.00   0.50    1.00    --   81.22 -95.00 120.00   72
 29  \w     37.00  83.00   0.50    1.00    --   73.64 -95.00  60.00   92
 30  \w     34.00  83.00   0.50    1.00    --   71.88 -95.00-120.00   98
 31  \w     36.00  71.00   0.50    1.00    --   73.64 -95.00-180.00   70
 32  \w    -62.00 -29.00   0.50    0.50    --  -71.26 112.00  37.00   66
 33  \w    -45.00 -18.00   0.50    0.50    --  -62.28 112.00  37.00   54
 34  \w   -100.00 -33.00   0.50    1.00    --  -76.11 125.00  90.00  134
 35  \w    -89.00 -64.00   0.50    1.00    --  -76.11 112.00  37.00   50
 36  \w   -107.00 -39.00   0.50    1.00    --  -76.11 125.00 -90.00  136
 37  \w   -116.00 -38.00   0.50    0.50    --  -71.26 -15.00 120.00  156
 38  \w   -115.00 -81.00   0.50    1.00    --  -76.11 -30.00  90.00   68
 39  \w   -121.00 -95.00   0.50    0.50    --  -71.26 -30.00  30.00   52
 40  \w   -111.00 -83.00   0.50    1.00    --  -76.11 -30.00   0.00   56
 41  \w   -112.00 -78.00   0.50    1.00    --  -76.11 -30.00-150.00   68
 42  \w   -111.00 -75.00   0.50    1.00    --  -76.11-125.00 -60.00   72
 43  \w   -121.00 -85.00   0.50    1.00    --  -76.11-125.00  30.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0068655000
_diffrn_orient_matrix_UB_12      0.0164041000
_diffrn_orient_matrix_UB_13      0.0510892000
_diffrn_orient_matrix_UB_21      -0.0346308000
_diffrn_orient_matrix_UB_22      0.0897843000
_diffrn_orient_matrix_UB_23      -0.0083674000
_diffrn_orient_matrix_UB_31      -0.1237909000
_diffrn_orient_matrix_UB_32      -0.0890833000
_diffrn_orient_matrix_UB_33      -0.0102043000
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            66515
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.326
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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 light orange'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       plate
_exptl_crystal_F_000             2118
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.934
_refine_diff_density_min         -2.385
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         19075
_refine_ls_number_restraints     1521
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0537P)^2^+11.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15463
_reflns_number_total             19075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-538
_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 1567201--1567212.cif.
;
_cod_original_cell_volume        4887.77(14)
_cod_database_code               1567204
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C60 H144 Cs2 N3 O16 Si8 U2'
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.111
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), 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), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58663
_shelx_hkl_checksum              3645
_shelx_fab_checksum              89003
_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 3.399
_oxdiff_exptl_absorpt_empirical_full_min 0.415