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_1567211
_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         '0.5(C72 H180 K2 N4 O16 Si12 U2)'
_chemical_formula_sum            'C36 H90 K N2 O8 Si6 U'
_chemical_formula_weight         1124.76
_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             2022-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-25 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                66.602(3)
_cell_angle_beta                 83.686(3)
_cell_angle_gamma                85.153(3)
_cell_formula_units_Z            4
_cell_length_a                   13.5839(4)
_cell_length_b                   20.4057(6)
_cell_length_c                   22.3874(7)
_cell_measurement_reflns_used    26738
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      76.5270
_cell_measurement_theta_min      3.2190
_cell_volume                     5655.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (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      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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   -115.00 -90.00   1.00    2.50    --  -43.01-137.00 126.00   25
  2  \w    -90.00 -14.00   1.00    2.50    --  -43.01 132.00  12.00   76
  3  \w    -78.00 -53.00   1.00    2.50    --  -43.01 137.00-171.00   25
  4  \w     66.00  91.00   1.00    2.50    --   43.01-132.00 -57.00   25
  5  \w     46.00  71.00   1.00    2.50    --   43.01-137.00 126.00   25
  6  \w     56.00  81.00   1.00   10.00    --  112.00-137.00 126.00   25
  7  \w    136.00 178.00   1.00   10.00    --  112.00 132.00  12.00   42
  8  \w    133.00 158.00   1.00   10.00    --  112.00 137.00-171.00   25
  9  \w     51.00  77.00   1.00   10.00    --  112.00-132.00 -57.00   26
 10  \w    -66.00  27.00   1.00    2.50    --  -43.01  37.00 -60.00   93
 11  \w    -74.00  -6.00   1.00    2.50    --  -43.01 125.00 -60.00   68
 12  \w   -111.00 -20.00   1.00    2.50    --  -43.01 -37.00 120.00   91
 13  \w     20.00 111.00   1.00    2.50    --   43.01  37.00-120.00   91
 14  \w    145.00 177.00   1.00   10.00    --  112.00  45.00  60.00   32
 15  \w     83.00 140.00   1.00   10.00    --  112.00 178.00 120.00   57
 16  \w     39.00  92.00   1.00   10.00    --  112.00 -45.00-120.00   53
 17  \w     37.00  68.00   1.00   10.00    --  112.00-111.00   0.00   31
 18  \w     85.00 177.00   1.00   10.00    --  112.00  30.00-120.00   92
 19  \w     84.00 109.00   1.00   10.00    --  112.00-111.00   0.00   25
 20  \w     83.00 109.00   1.00   10.00    --  112.00 -77.00 120.00   26
 21  \w    136.00 162.00   1.00   10.00    --  112.00 111.00 -30.00   26
 22  \w     37.00 109.00   1.00   10.00    --  112.00-111.00 150.00   72
 23  \w    113.00 178.00   1.00   10.00    --  112.00  77.00 -90.00   65
 24  \w    138.00 174.00   1.00   10.00    --  112.00  77.00 150.00   36
 25  \w     40.00 109.00   1.00   10.00    --  112.00-111.00-150.00   69
 26  \w     98.00 144.00   1.00   10.00    --  112.00 -77.00-120.00   46
 27  \w    116.00 142.00   1.00   10.00    --  112.00  61.00  90.00   26
 28  \w    149.00 174.00   1.00   10.00    --  112.00  61.00  90.00   25
 29  \w     36.00  62.00   1.00   10.00    --  112.00 -77.00-120.00   26
 30  \w     68.00 109.00   1.00   10.00    --  112.00-111.00  60.00   41
 31  \w     86.00 124.00   1.00   10.00    --  112.00  45.00  60.00   38
 32  \w    110.00 137.00   1.00   10.00    --  112.00 -45.00-120.00   27
 33  \w     94.00 119.00   1.00   10.00    --  112.00 -61.00  60.00   25
 34  \w    112.00 138.00   1.00   10.00    --  112.00 -77.00 120.00   26
 35  \w     84.00 117.00   1.00   10.00    --  112.00  30.00-150.00   33
 36  \w    130.00 156.00   1.00   10.00    --  112.00  30.00-150.00   26
 37  \w     71.00 106.00   1.00   10.00    --  112.00-111.00 -60.00   35
 38  \w     39.00 109.00   1.00   10.00    --  112.00-111.00  90.00   70
 39  \w     42.00 109.00   1.00   10.00    --  112.00-111.00 120.00   67
 40  \w    118.00 177.00   1.00   10.00    --  112.00  30.00 150.00   59
;
_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      0.0553884000
_diffrn_orient_matrix_UB_12      0.0289904000
_diffrn_orient_matrix_UB_13      0.0402059000
_diffrn_orient_matrix_UB_21      -0.0951654000
_diffrn_orient_matrix_UB_22      -0.0032644000
_diffrn_orient_matrix_UB_23      0.0452140000
_diffrn_orient_matrix_UB_31      0.0303539000
_diffrn_orient_matrix_UB_32      -0.0770025000
_diffrn_orient_matrix_UB_33      0.0447286000
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.895
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.277
_exptl_absorpt_correction_T_max  0.470
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       plate
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         23386
_refine_ls_number_restraints     1029
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0275P)^2^+4.5321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19717
_reflns_number_total             23386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk417
_cod_depositor_comments
'Adding full bibliography for 1567201--1567212.cif.'
_cod_database_code               1567211
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C39 H90 N2 O8 Si6 K1 U1'
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.240
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
K1 \\sim K2 \\sim K3 \\sim K4: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. 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
4. Others
 Sof(K2)=1-FVAR(1)
 Sof(K1)=FVAR(1)
 Sof(K4)=1-FVAR(2)
 Sof(K3)=FVAR(2)
5.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), 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), 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), 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), C93(H93A,H93B,
 H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C97(H97A,
 H97B,H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C100(H10D,H10E,H10F),
 C101(H10G,H10H,H10I), C102(H10J,H10K,H10L), C103(H10M,H10N,H10O), C104(H10P,
 H10Q,H10R)
;
_shelx_res_checksum              20199
_shelx_hkl_checksum              14218
_olex2_date_sample_data_collection 2021-08-17
_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 2.465
_oxdiff_exptl_absorpt_empirical_full_min 0.561