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_1567202
_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 K3 N5 O16 Si8 U2, C7 H8'
_chemical_formula_sum            'C67 H152 K3 N5 O16 Si8 U2'
_chemical_formula_weight         2102.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-03-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.7630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5895(2)
_cell_length_b                   26.3839(4)
_cell_length_c                   21.3250(3)
_cell_measurement_reflns_used    24436
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.3950
_cell_measurement_theta_min      3.9500
_cell_volume                     9753.2(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -81.00 -46.00   1.00    7.00    --  -40.91 100.00  55.00   35
  2  \w    -40.00 -14.00   1.00    7.00    --  -40.91 100.00  55.00   26
  3  \w    104.00 167.00   1.00   28.00    --  105.15 100.00  55.00   63
  4  \w     60.00 107.00   1.00   28.00    --  105.15-100.00 -50.00   47
  5  \w   -110.00 -83.00   1.00    7.00    --  -40.91 -57.00-120.00   27
  6  \w    -65.00 -13.00   1.00    7.00    --  -40.91 -57.00-120.00   52
  7  \w   -113.00 -43.00   1.00    7.00    --  -40.91 -57.00 120.00   70
  8  \w    -60.00  33.00   1.00    7.00    --  -40.91  38.00 -90.00   93
  9  \w    -81.00 -24.00   1.00    7.00    --  -40.91 125.00 150.00   57
 10  \w    -32.00  64.00   1.00    7.00    --   40.91 -38.00 -30.00   96
 11  \w     29.00  59.00   1.00    7.00    --   40.91-100.00 -50.00   30
 12  \w     30.00  73.00   1.00    7.00    --   40.91-125.00-180.00   43
 13  \w     66.00 109.00   1.00   28.00    --  105.15-111.00-120.00   43
 14  \w     68.00 109.00   1.00   28.00    --  105.15-111.00 150.00   41
 15  \w    106.00 169.00   1.00   28.00    --  105.15 111.00   0.00   63
 16  \w     80.00 107.00   1.00   28.00    --  105.15  45.00 150.00   27
 17  \w     86.00 178.00   1.00   28.00    --  105.15  45.00 120.00   92
 18  \w    142.00 174.00   1.00   28.00    --  105.15 111.00  30.00   32
 19  \w     33.00 130.00   1.00   28.00    --  105.15 -45.00 -30.00   97
 20  \w    104.00 175.00   1.00   28.00    --  105.15 111.00 -60.00   71
 21  \w    126.00 161.00   1.00   28.00    --  105.15 111.00  90.00   35
 22  \w     38.00 106.00   1.00   28.00    --  105.15 -94.00   0.00   68
 23  \w     67.00  97.00   1.00   28.00    --  105.15-111.00  90.00   30
 24  \w    109.00 165.00   1.00   28.00    --  105.15  77.00  30.00   56
 25  \w    147.00 174.00   1.00   28.00    --  105.15  45.00 150.00   27
 26  \w     83.00 173.00   1.00   28.00    --  105.15  45.00-180.00   90
 27  \w     33.00  72.00   1.00   28.00    --  105.15 -61.00  90.00   39
;
_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      0.0271742000
_diffrn_orient_matrix_UB_12      0.0553865000
_diffrn_orient_matrix_UB_13      -0.0025113000
_diffrn_orient_matrix_UB_21      0.0134954000
_diffrn_orient_matrix_UB_22      0.0024321000
_diffrn_orient_matrix_UB_23      0.0732124000
_diffrn_orient_matrix_UB_31      0.0834963000
_diffrn_orient_matrix_UB_32      -0.0184232000
_diffrn_orient_matrix_UB_33      0.0021669000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27008
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.829
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.804
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.199
_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,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.084
_refine_diff_density_max         7.103
_refine_diff_density_min         -5.766
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         27008
_refine_ls_number_restraints     1245
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.1007
_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^)+(0.1397P)^2^+158.2848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2701
_refine_ls_wR_factor_ref         0.2894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18989
_reflns_number_total             27008
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9678\% 
around [0.71 -0.02 0.71] (reciprocal) or [0.81 -0.01 0.59] (direct)
;
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-486
_cod_depositor_comments
'Adding full bibliography for 1567201--1567212.cif.'
_cod_database_code               1567202
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C67 H142 N5 O16 Si8 K3 U2'
_shelx_estimated_absorpt_t_max   0.437
_shelx_estimated_absorpt_t_min   0.207
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8912(19)
 0.1088(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C23-C21 = C22-C21 = C24-C21
 1.54 with sigma of 0.02
 O22-C21
 1.43 with sigma of 0.02
 C8-C5 \\sim C11-C5 \\sim C7-C5 \\sim C10-C5 \\sim C6-C5 \\sim C9-C5
 with sigma of 0.02
 C11-C10 \\sim C10-C9 \\sim C9-C11
 with sigma of 0.02
 C8-C7 \\sim C7-C6 \\sim C6-C8
 with sigma of 0.02
 C23-C24 \\sim C24-C22 \\sim C22-C23
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C94(H94), C95(H95), C96(H96), C97(H97), C98(H98)
7.b 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), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), 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), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C99(H99A,H99B,H99C)
;
_shelx_res_checksum              85206
_shelx_hkl_checksum              37746
_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 3.021
_oxdiff_exptl_absorpt_empirical_full_min 0.344
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2