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_1567210
_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         'C96 H234 K6 N10 O24 Si14 U4, 4[C7H8]'
_chemical_formula_sum            'C96 H234 K6 N10 O24 Si14 U4'
_chemical_formula_weight         3492.90
_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             2022-01-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-14 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                93.8055(9)
_cell_angle_beta                 91.6994(9)
_cell_angle_gamma                112.1353(11)
_cell_formula_units_Z            1
_cell_length_a                   13.65686(16)
_cell_length_b                   17.9610(2)
_cell_length_c                   20.0238(2)
_cell_measurement_reflns_used    37904
_cell_measurement_temperature    140.00(10)
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_cell_measurement_theta_min      2.2410
_cell_volume                     4531.67(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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 0.998
_diffrn_measured_fraction_theta_max 0.951
_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     42.00 112.00   0.50    0.40    --   81.22   0.00-120.00  140
  2  \w     62.00 109.00   0.50    0.40    --   59.56  30.00 -90.00   94
  3  \w     82.00 127.00   0.50    0.40    --   81.22  30.00 -60.00   90
  4  \w     73.00 117.00   0.50    0.40    --   71.88  30.00 150.00   88
  5  \w    -79.00 -53.00   0.50    0.40    --  -62.28 159.00 110.00   52
  6  \w   -106.00 -81.00   0.50    0.40    --  -76.11 159.00 110.00   50
  7  \w    -86.00 -61.00   0.50    0.40    --  -71.26 118.00 -42.00   50
  8  \w   -103.00 -73.00   0.50    0.40    --  -76.11 118.00 -42.00   60
  9  \w    -77.00 -52.00   0.50    0.40    --  -62.28 118.00 -42.00   50
 10  \w     10.00  36.00   0.50    0.40    --   59.56 -30.00  60.00   52
 11  \w     10.00  36.00   0.50    0.40    --   59.56 -30.00 120.00   52
 12  \w     10.00  35.00   0.50    0.40    --   59.56 -30.00  90.00   50
 13  \w     11.00  36.00   0.50    0.40    --   59.56 -30.00  30.00   50
 14  \w     10.00  35.00   0.50    0.40    --   59.56 -30.00   0.00   50
 15  \w     12.00  37.00   0.50    0.40    --   59.56 -30.00 -90.00   50
 16  \w     35.00  79.00   0.50    0.40    --   59.56-159.00  78.00   88
 17  \w     55.00  80.00   0.50    0.40    --   73.45-159.00  78.00   50
 18  \w     63.00  88.00   0.50    0.40    --   81.22-159.00  78.00   50
 19  \w     87.00 112.00   0.50    0.40    --   81.22-125.00  90.00   50
 20  \w     41.00  68.00   0.50    0.40    --   81.22-125.00  90.00   54
 21  \w     38.00 111.00   0.50    0.40    --   81.22-125.00   0.00  146
 22  \w     87.00 112.00   0.50    0.40    --   81.22-125.00 -30.00   50
 23  \w     48.00  74.00   0.50    0.40    --   81.22-125.00 -30.00   52
 24  \w     18.00  67.00   0.50    0.40    --   59.56-118.00-128.00   98
 25  \w     41.00  66.00   0.50    0.40    --   81.22-125.00-180.00   50
 26  \w     87.00 112.00   0.50    0.40    --   81.22-125.00-180.00   50
 27  \w     74.00 108.00   0.50    0.40    --   81.22-118.00-128.00   68
 28  \w     29.00 101.00   0.50    0.40    --   73.45-118.00-128.00  144
 29  \w     42.00  70.00   0.50    0.40    --   81.22 -95.00-120.00   56
 30  \w     35.00  80.00   0.50    0.40    --   71.88 -95.00 -90.00   90
 31  \w     25.00  67.00   0.50    0.40    --   59.56 -95.00 -60.00   84
 32  \w     32.00  63.00   0.50    0.40    --   71.88 -95.00   0.00   62
 33  \w     50.00  80.00   0.50    0.40    --   81.22 -95.00  60.00   60
 34  \w     52.00  91.00   0.50    0.40    --   81.22 -95.00 120.00   78
 35  \w     38.00  81.00   0.50    0.40    --   73.45 -95.00 150.00   86
 36  \w     58.00  84.00   0.50    0.40    --   73.45 -95.00  90.00   52
 37  \w     34.00  60.00   0.50    0.40    --   71.88 -95.00  90.00   52
 38  \w     38.00  68.00   0.50    0.40    --   73.45 -95.00  30.00   60
 39  \w     35.00  64.00   0.50    0.40    --   73.45 -95.00-180.00   58
 40  \w     81.00 108.00   0.50    0.40    --   81.22 125.00   0.00   54
 41  \w     59.00  84.00   0.50    0.40    --   73.45 159.00 110.00   50
 42  \w     87.00 112.00   0.50    0.40    --   81.22 159.00 110.00   50
 43  \w     98.00 126.00   0.50    0.40    --   81.22 125.00-150.00   56
 44  \w   -115.00 -73.00   0.50    0.40    --  -71.26 -30.00 -60.00   84
 45  \w   -113.00 -77.00   0.50    0.40    --  -76.11 -30.00-150.00   72
 46  \w   -125.00 -82.00   0.50    0.40    --  -76.11 -30.00 -90.00   86
 47  \w   -121.00 -95.00   0.50    0.40    --  -76.11 -30.00 120.00   52
 48  \w    -81.00 -55.00   0.50    0.40    --  -62.28-159.00  78.00   52
 49  \w   -122.00 -82.00   0.50    0.40    --  -76.11-125.00 120.00   80
 50  \w    -92.00 -67.00   0.50    0.40    --  -71.26-159.00  78.00   50
 51  \w   -106.00 -81.00   0.50    0.40    --  -76.11-159.00  78.00   50
 52  \w   -118.00 -92.00   0.50    0.40    --  -76.11-125.00 -60.00   52
 53  \w   -121.00 -74.00   0.50    0.40    --  -76.11-125.00 -90.00   94
 54  \w   -120.00 -75.00   0.50    0.40    --  -76.11-125.00-150.00   90
;
_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      -0.0294701000
_diffrn_orient_matrix_UB_12      0.0748469000
_diffrn_orient_matrix_UB_13      0.0062981000
_diffrn_orient_matrix_UB_21      0.0063875000
_diffrn_orient_matrix_UB_22      0.0057712000
_diffrn_orient_matrix_UB_23      -0.0762778000
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_diffrn_orient_matrix_UB_32      -0.0547674000
_diffrn_orient_matrix_UB_33      -0.0104066000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69706
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.346
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.441
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.200
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (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 yellow'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             1750
_exptl_crystal_size_max          0.17
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_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.034
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         17830
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_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0415
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_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+1.2538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14821
_reflns_number_total             17830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-533b
_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        4531.68(9)
_cod_database_code               1567210
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C96 H234 K6 N10 O24 Si14 U4'
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.226
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C52A-C49 = C49-C52B
 1.52 with sigma of 0.01
 C9-C12 = C9-C11
 1.52 with sigma of 0.01
3. 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
4. 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
5. Others
 Sof(O43B)=Sof(O44B)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(O43A)=Sof(O44A)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
6.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), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), 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), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), 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), C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16752
_shelx_hkl_checksum              20872
_shelx_fab_checksum              58690
_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 2.016
_oxdiff_exptl_absorpt_empirical_full_min 0.404