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_1567205
_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         'C48 H126 K N5 O8 Si10 U2, C24 H48 K O6'
_chemical_formula_sum            'C72 H174 K2 N5 O14 Si10 U2'
_chemical_formula_weight         2169.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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
;
2022-05-24 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6235(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.57855(15)
_cell_length_b                   19.40862(16)
_cell_length_c                   26.9671(2)
_cell_measurement_reflns_used    35277
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5740
_cell_measurement_theta_min      3.4860
_cell_volume                     10766.37(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (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 0.989
_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 -16.00   1.00    6.00    --  -40.91 125.00 -30.00   26
  2  \w    -41.00  -6.00   1.00    6.00    --  -40.91 125.00  30.00   35
  3  \w    -54.00  28.00   1.00    6.00    --  -40.91  38.00 -60.00   82
  4  \w   -121.00  -8.00   1.00    6.00    --  -40.91 -19.00 120.00  113
  5  \w     35.00  97.00   1.00    6.00    --   40.91-125.00-180.00   62
  6  \w     29.00  97.00   1.00    6.00    --   40.91-125.00  60.00   68
  7  \w     69.00 109.00   1.00   24.00    --  105.15-111.00-120.00   40
  8  \w     97.00 122.00   1.00   24.00    --  105.15 -61.00 -30.00   25
  9  \w     66.00 109.00   1.00   24.00    --  105.15-111.00  60.00   43
 10  \w     35.00 109.00   1.00   24.00    --  105.15-111.00 -30.00   74
 11  \w     40.00  83.00   1.00   24.00    --  105.15 -61.00 -30.00   43
 12  \w     25.00 157.00   1.00   24.00    --  105.15 -15.00  30.00  132
 13  \w    115.00 147.00   1.00   24.00    --  105.15  77.00  90.00   32
 14  \w     82.00 109.00   1.00   24.00    --  105.15-111.00-180.00   27
 15  \w     37.00  66.00   1.00   24.00    --  105.15-111.00-180.00   29
 16  \w     63.00 127.00   1.00   24.00    --  105.15 178.00   0.00   64
 17  \w    113.00 140.00   1.00   24.00    --  105.15  77.00-180.00   27
 18  \w    152.00 178.00   1.00   24.00    --  105.15  77.00-180.00   26
 19  \w     48.00 131.00   1.00   24.00    --  105.15 -45.00 120.00   83
 20  \w     24.00 148.00   1.00   24.00    --  105.15 -15.00 -90.00  124
 21  \w    137.00 174.00   1.00   24.00    --  105.15 111.00  90.00   37
 22  \w     35.00 106.00   1.00   24.00    --  105.15 -94.00 120.00   71
;
_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      0.0242830000
_diffrn_orient_matrix_UB_12      0.0543922000
_diffrn_orient_matrix_UB_13      0.0377913000
_diffrn_orient_matrix_UB_21      -0.0335805000
_diffrn_orient_matrix_UB_22      -0.0393616000
_diffrn_orient_matrix_UB_23      0.0417526000
_diffrn_orient_matrix_UB_31      0.0623729000
_diffrn_orient_matrix_UB_32      -0.0423581000
_diffrn_orient_matrix_UB_33      0.0097257000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            80595
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.773
_diffrn_reflns_theta_min         3.130
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.559
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (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            'lustrous dark black'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             4460
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         21198
_refine_ls_number_restraints     1943
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+31.4553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18355
_reflns_number_total             21198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-183
_cod_depositor_comments
'Adding full bibliography for 1567201--1567212.cif.'
_cod_original_cell_volume        10766.38(15)
_cod_database_code               1567205
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H174 N5 O14 Si10 K2 U2'
_shelx_estimated_absorpt_t_max   0.471
_shelx_estimated_absorpt_t_min   0.185
_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
 C82-C81 = C83-C82 = C84-C83 = C104-C103 = C103-C102 = C102-C101 = C86-C85 =
 C87-C86 = C88-C87 = C96-C95 = C95-C94 = C94-C93 = C92-C91 = C90-C89 = C91-C90 =
  C99-C100 = C99-C98 = C98-C97
 1.54 with sigma of 0.02
 O31-C84 = O31-C81 = O35-C100 = O35-C97 = O33-C92 = O33-C89 = O34-C93 = O34-
 C96 = O32-C88 = O32-C85 = O36-C101 = O36-C104
 1.43 with sigma of 0.02
 Si2-O23 \\sim Si2-O26 \\sim Si2-O27 \\sim Si2-O24 \\sim Si2-O25
 with sigma of 0.02
 C34-C33 \\sim C35-C33 \\sim C36-C33 \\sim C22-C21 \\sim C24-C21 \\sim C23-C21
\\sim C43-C41 \\sim C42-C41
 \\sim C44-C41 \\sim C29-C31 \\sim C30-C29 \\sim C32-C29 \\sim C26-C25 \\sim
C27-C25 \\sim C37-C38 \\sim C40-
 C37 \\sim C28-C25 \\sim C39-C37
 with sigma of 0.02
 O23-C25 \\sim O27-C37 \\sim O24-C29 \\sim O25-C41 \\sim O26-C33 \\sim O22-C21
 with sigma of 0.02
 C31-C30 \\sim C30-C32 \\sim C31-C32
 with sigma of 0.02
 C43-C42 \\sim C42-C44 \\sim C43-C44
 with sigma of 0.02
 C38-C40 \\sim C40-C39 \\sim C38-C39
 with sigma of 0.02
 C26-C27 \\sim C27-C28 \\sim C26-C28
 with sigma of 0.02
 C34-C35 \\sim C35-C36 \\sim C34-C36
 with sigma of 0.02
 C22-C24 \\sim C24-C23 \\sim C22-C23
 with sigma of 0.02
 C11-C10 \\sim C10-C12 \\sim C11-C12
 with sigma of 0.02
 C11-C9 \\sim C10-C9 \\sim C12-C9 \\sim C14-C13 \\sim C15-C13 \\sim C16-C13
 with sigma of 0.02
 C15-C14 \\sim C14-C16 \\sim C15-C16
 with sigma of 0.02
 O4-C13 \\sim O4-C9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si2 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim C21 \\sim
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim
C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
O4 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C52) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C102)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. 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
5. Others
 Sof(O25)=Sof(O26)=Sof(O27)=Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=1-FVAR(1)
 Sof(O22)=Sof(O23)=Sof(O24)=Sof(C21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(2)
 Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,
 H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B),
 C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B),
  C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,
 H99B), C100(H10D,H10E), C101(H10F,H10G), C102(H10H,H10I), C103(H10J,H10K),
 C104(H10L,H10M)
6.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), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 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), C34(H34A,H34B,H34C), 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), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              69352
_shelx_hkl_checksum              14831
_olex2_date_sample_data_collection 2021-03-17
_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 3.334
_oxdiff_exptl_absorpt_empirical_full_min 0.524