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_1567207
_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         'C66 H162 K6 N6 O16 Si10 U2'
_chemical_formula_sum            'C66 H162 K6 N6 O16 Si10 U2'
_chemical_formula_weight         2287.57
_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             2022-03-17
_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                 99.035(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1020(6)
_cell_length_b                   29.9340(16)
_cell_length_c                   27.0037(8)
_cell_measurement_reflns_used    8043
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      71.0610
_cell_measurement_theta_min      3.1010
_cell_volume                     12055.9(9)
_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      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_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 -17.00   1.00   10.00    --  -43.01 -47.00 -31.00   98
  2  \w     -9.00  30.00   1.00   10.00    --  -43.01  47.00 117.00   39
  3  \w    -50.00 -10.00   1.00   10.00    --  -43.01  47.00 117.00   40
  4  \w     59.00 102.00   1.00   10.00    --   43.01  47.00 117.00   43
  5  \w     81.00 176.00   1.00   40.00    --  103.49  47.00 117.00   95
  6  \w     37.00  65.00   1.00   40.00    --  103.49 -47.00 -31.00   28
  7  \w     62.00  90.00   1.00   10.00    --   43.01-125.00 -90.00   28
  8  \w     28.00  97.00   1.00   10.00    --   43.01-125.00-180.00   69
  9  \w     -4.00  21.00   1.00   10.00    --   43.01 -47.00 -31.00   25
 10  \w     42.00  73.00   1.00   10.00    --   43.01-125.00-120.00   31
 11  \w     74.00 176.00   1.00   40.00    --  103.49  61.00-150.00  102
 12  \w    148.00 175.00   1.00   40.00    --  103.49 111.00 -30.00   27
 13  \w     68.00 101.00   1.00   40.00    --  103.49-111.00   0.00   33
 14  \w     79.00 106.00   1.00   40.00    --  103.49  45.00  60.00   27
 15  \w     81.00 108.00   1.00   40.00    --  103.49-111.00-180.00   27
 16  \w    126.00 161.00   1.00   40.00    --  103.49  45.00  60.00   35
 17  \w     74.00 162.00   1.00   40.00    --  103.49  61.00 150.00   88
 18  \w    125.00 172.00   1.00   40.00    --  103.49 111.00  30.00   47
;
_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      0.0495900000
_diffrn_orient_matrix_UB_12      0.0217442000
_diffrn_orient_matrix_UB_13      -0.0394775000
_diffrn_orient_matrix_UB_21      0.0685860000
_diffrn_orient_matrix_UB_22      0.0205124000
_diffrn_orient_matrix_UB_23      0.0421765000
_diffrn_orient_matrix_UB_31      0.0592670000
_diffrn_orient_matrix_UB_32      -0.0418810000
_diffrn_orient_matrix_UB_33      0.0001971000
_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  0.1130
_diffrn_reflns_av_unetI/netI     0.1393
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            63694
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.764
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.685
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.279
_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 pale green'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       prism
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         23143
_refine_ls_number_restraints     1527
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1006P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11669
_reflns_number_total             23143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-522b
_cod_depositor_comments
'Adding full bibliography for 1567201--1567212.cif.'
_cod_original_cell_volume        12055.8(9)
_cod_database_code               1567207
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H200 N20 O20 K6 Si10 U2'
_shelx_estimated_absorpt_t_max   0.522
_shelx_estimated_absorpt_t_min   0.175
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64-C61 = C63-C61 = C62-C61
 1.54 with sigma of 0.02
 C62-C64 \\sim C64-C63 \\sim C62-C63
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C87)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
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.a Ternary CH refined with riding coordinates:
 N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B)
5.c 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), 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), 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), C93(H93A,H93B,H93C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,
 H98B,H98C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 332 electrons were 
found in a volume of 2146\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.7[C6H14] per Asymmetric Unit 
which account for 340 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7623
_shelx_hkl_checksum              68774
_shelx_fab_checksum              48135
_olex2_date_sample_data_collection 2022-01-18
_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 2.464
_oxdiff_exptl_absorpt_empirical_full_min 0.499