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_1567212
_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 K2 N3 O16 Si8 U2, C6 H14'
_chemical_formula_sum            'C66 H158 K2 N3 O16 Si8 U2'
_chemical_formula_weight         2028.92
_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             2022-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-12 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8994(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.10134(10)
_cell_length_b                   30.68723(18)
_cell_length_c                   46.2387(3)
_cell_measurement_reflns_used    110276
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.7490
_cell_measurement_theta_min      2.4850
_cell_volume                     19983.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     52.00  87.00   0.50    1.00    --   48.00  72.00 -88.86   70
  2  \w     50.00  86.00   0.50    1.00    --   48.00  76.00  64.00   72
  3  \w     56.00  91.00   0.50    1.00    --   52.00  72.00 -44.90   70
  4  \w     61.00  96.00   0.50    1.00    --   56.00  70.00 -37.82   70
  5  \w     11.00  37.00   0.50    1.00    --   59.87 -30.00-180.00   52
  6  \w     11.00  37.00   0.50    1.00    --   59.87 -30.00 120.00   52
  7  \w     11.00  37.00   0.50    1.00    --   59.87 -30.00-150.00   52
  8  \w   -100.00 -65.00   0.50    1.00    --  -60.00 -69.00  95.67   70
  9  \w   -110.00 -73.00   0.50    1.00    --  -64.00 -51.00 127.90   74
 10  \w   -114.00 -77.00   0.50    1.00    --  -68.00 -52.00 171.13   74
 11  \w   -115.00 -77.00   0.50    1.00    --  -68.00 -48.00-139.60   76
 12  \w     32.00  83.00   0.50    2.00    --   71.88 -95.00   0.00  102
 13  \w   -112.00 -76.00   0.50    1.00    --  -72.00 -71.00  69.71   72
 14  \w     34.00  84.00   0.50    2.00    --   73.64 -95.00 -60.00  100
 15  \w     75.00 123.00   0.50    2.00    --   73.64  30.00   0.00   96
 16  \w     34.00  84.00   0.50    2.00    --   73.64 -95.00  30.00  100
 17  \w     34.00  84.00   0.50    2.00    --   73.64 -95.00-150.00  100
 18  \w   -107.00 -30.00   0.50    2.00    --  -76.11 125.00-120.00  154
 19  \w   -122.00 -74.00   0.50    2.00    --  -76.11-125.00   0.00   96
 20  \w   -107.00 -30.00   0.50    2.00    --  -76.11 125.00  90.00  154
 21  \w   -115.00 -79.00   0.50    2.00    --  -76.55 -74.00  50.87   72
 22  \w   -120.00 -84.00   0.50    2.00    --  -76.55 -61.00  20.29   72
 23  \w   -121.00 -84.00   0.50    2.00    --  -76.55 -58.00-168.14   74
 24  \w   -124.00 -86.00   0.50    2.00    --  -76.55 -44.00 -95.30   76
 25  \w     35.00 112.00   0.50    2.00    --   81.22-125.00 150.00  154
 26  \w     79.00 127.00   0.50    2.00    --   81.22 125.00-180.00   96
 27  \w     35.00 112.00   0.50    2.00    --   81.22-125.00-150.00  154
 28  \w     79.00 127.00   0.50    2.00    --   81.22 125.00  60.00   96
 29  \w     41.00  92.00   0.50    2.00    --   81.22 -95.00  60.00  102
 30  \w     79.00 127.00   0.50    2.00    --   81.22 125.00 120.00   96
 31  \w     35.00 112.00   0.50    2.00    --   81.22-125.00  60.00  154
 32  \w     41.00  92.00   0.50    2.00    --   81.22 -95.00-120.00  102
 33  \w     35.00 112.00   0.50    2.00    --   81.22-125.00-120.00  154
 34  \w     79.00 127.00   0.50    2.00    --   81.22 125.00 -30.00   96
 35  \w     79.00 127.00   0.50    2.00    --   81.22 125.00  30.00   96
 36  \w     35.00 112.00   0.50    2.00    --   81.22-125.00   0.00  154
 37  \w     35.00 112.00   0.50    2.00    --   81.22-125.00 -30.00  154
 38  \w      6.00  33.00   0.50    1.00    --   16.00  94.00  50.43   54
 39  \w     15.00  42.00   0.50    1.00    --   20.00  86.00 -11.78   54
 40  \w     16.00  42.00   0.50    1.00    --   20.00  85.00 135.68   52
 41  \w     15.00  42.00   0.50    1.00    --   20.00  86.00 -85.09   54
 42  \w     11.00  40.00   0.50    1.00    --   20.00  92.00-173.12   58
 43  \w     42.00  78.00   0.50    1.00    --   40.00  75.00  22.78   72
 44  \w     41.00  77.00   0.50    1.00    --   40.00  77.00-153.76   72
 45  \w     47.00  83.00   0.50    1.00    --   44.00  73.00 143.50   72
 46  \w   -114.00 -83.00   0.50    2.00    --  -76.00 -75.00-128.75   62
 47  \w   -122.00 -74.00   0.50    2.00    --  -76.11-125.00-180.00   96
 48  \w   -121.00 -85.00   0.50    2.00    --  -76.55 -55.00  -7.37   72
 49  \w     79.00 127.00   0.50    2.00    --   81.22 125.00-150.00   96
;
_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      -0.1092504000
_diffrn_orient_matrix_UB_12      -0.0007280000
_diffrn_orient_matrix_UB_13      -0.0000479000
_diffrn_orient_matrix_UB_21      -0.0050965000
_diffrn_orient_matrix_UB_22      0.0325032000
_diffrn_orient_matrix_UB_23      -0.0254274000
_diffrn_orient_matrix_UB_31      -0.0022875000
_diffrn_orient_matrix_UB_32      -0.0382349000
_diffrn_orient_matrix_UB_33      -0.0216077000
_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  0.1273
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            355501
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         2.395
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.128
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (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 intense red'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       plate
_exptl_crystal_F_000             8296
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.025
_refine_diff_density_max         10.736
_refine_diff_density_min         -5.880
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1856
_refine_ls_number_reflns         35299
_refine_ls_number_restraints     3229
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0839
_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^)+(0.0984P)^2^+465.3323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29878
_reflns_number_total             35299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-464
_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_database_code               1567212
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C64 H154 Cs K N3 O17 Si8 U2'
_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
 C201-C202 = C202-C203 = C203-C204 = C204-C205 = C205-C206
 1.52 with sigma of 0.02
 C212-C211 = C211-C210 = C210-C209 = C209-C208 = C208-C207
 1.52 with sigma of 0.02
 C52-C49 = C50-C49 = C51-C49 = C22-C21 = C23-C21 = C7-C5 = C6-C5 = C25-C27 =
 C152-C149 = C151-C149 = C150-C149 = C29-C30 = C29-C32 = C45-C46 = C45-C47 =
 C45-C48 = C65-C66 = C65-C68 = C69-C70 = C141-C143 = C141-C144 = C141-C142 =
 C145-C146 = C145-C147 = C145-C148 = C161-C162 = C165-C166 = C165-C167 = C161-
 C163 = C161-C164 = C121-C123 = C121-C122 = C101-C104 = C25-C26 = C5-C8
 1.52 with sigma of 0.01
 C212-C210 = C209-C207
 2.53 with sigma of 0.04
 C211-C209 = C210-C208
 2.54 with sigma of 0.04
 C201-C203 = C204-C206
 2.53 with sigma of 0.04
 C202-C204 = C203-C205
 2.54 with sigma of 0.04
 C52-C50 \\sim C50-C51 \\sim C51-C52
 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
Uanis(K1) = Uanis(K4B)
Uanis(K1) = Uanis(K3A)
Uanis(K1) = Uanis(K3B)
Uanis(K1) = Uanis(K4A)
Uanis(K1) = Uanis(K2)
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(K4B)=1-FVAR(1)
 Sof(K4A)=FVAR(1)
 Sof(K3B)=1-FVAR(2)
 Sof(K3A)=FVAR(2)
 Sof(O43B)=Sof(O44B)=1-FVAR(3)
 Sof(O43A)=Sof(O44A)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C202(H20D,H20E), C203(H20F,H20G), C204(H20H,H20I), C205(H20J,H20K), C208(H20R,
 H20S), C209(H20T,H20U), C210(H21A,H21B), C211(H21C,H21D)
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), 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), C102(H10D,H10E,
 H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C106(H10M,H10N,H10O),
 C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C110(H11D,H11E,H11F), C111(H11G,
 H11H,H11I), C112(H11J,H11K,H11L), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I),
 C124(H12J,H12K,H12L), C126(H12M,H12N,H12O), C127(H12P,H12Q,H12R), C128(H12S,
 H12T,H12U), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I),
 C142(H14A,H14B,H14C), C143(H14D,H14E,H14F), C144(H14G,H14H,H14I), C146(H14J,
 H14K,H14L), C147(H14M,H14N,H14O), C148(H14P,H14Q,H14R), C150(H15A,H15B,H15C),
 C151(H15D,H15E,H15F), C152(H15G,H15H,H15I), C162(H16A,H16B,H16C), C163(H16D,
 H16E,H16F), C164(H16G,H16H,H16I), C166(H16J,H16K,H16L), C167(H16M,H16N,H16O),
 C168(H16P,H16Q,H16R), C170(H17A,H17B,H17C), C171(H17D,H17E,H17F), C172(H17G,
 H17H,H17I), C181(H18A,H18B,H18C), C182(H18D,H18E,H18F), C183(H18G,H18H,H18I),
 C184(H18J,H18K,H18L), C185(H18M,H18N,H18O), C186(H18P,H18Q,H18R), C187(H18S,
 H18T,H18U), C188(H18V,H18W,H18X), C189(H18Y,H,HA), C190(H19A,H19B,H19C),
 C191(H19D,H19E,H19F), C192(H19G,H19H,H19I), C201(H20A,H20B,H20C), C206(H20L,
 H20M,H20N), C207(H20O,H20P,H20Q), C212(H21E,H21F,H21G)
;
_shelx_res_checksum              91462
_shelx_hkl_checksum              59445
_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 10.080
_oxdiff_exptl_absorpt_empirical_full_min 0.253