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_1567201
_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 Cs N3 O16 Si8 U2'
_chemical_formula_sum            'C60 H144 Cs N3 O16 Si8 U2'
_chemical_formula_weight         1997.46
_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             2021-08-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                107.3639(13)
_cell_angle_beta                 92.5382(12)
_cell_angle_gamma                108.1942(14)
_cell_formula_units_Z            2
_cell_length_a                   14.1418(2)
_cell_length_b                   16.3515(2)
_cell_length_c                   22.1403(3)
_cell_measurement_reflns_used    47489
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.1070
_cell_measurement_theta_min      2.2120
_cell_volume                     4588.44(12)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.986
_diffrn_measured_fraction_theta_max 0.948
_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     37.00  62.00   0.50    0.30    --   24.00  58.00  61.43   50
  2  \w     51.00  76.00   0.50    0.30    --   72.70   2.00  98.06   50
  3  \w     90.00 115.00   0.50    0.30    --   72.70  40.00  72.96   50
  4  \w     87.00 112.00   0.50    0.30    --   72.70  37.00  66.54   50
  5  \w     50.00  80.00   0.50    0.30    --   40.00  29.00-149.71   60
  6  \w    -93.00 -68.00   0.50    0.30    --  -72.70 115.00-130.69   50
  7  \w   -103.00 -78.00   0.50    0.30    --  -72.70 134.00-108.72   50
  8  \w    -68.00 -35.00   0.50    0.30    --  -72.70 134.00-108.72   66
  9  \w    -99.00 -52.00   0.50    0.30    --  -72.70 127.00  18.09   94
 10  \w    -89.00 -32.00   0.50    0.30    --  -66.62 125.00  60.00  114
 11  \w    -65.00 -38.00   0.50    0.30    --  -72.70 146.00 170.61   54
 12  \w    -98.00 -65.00   0.50    0.30    --  -72.70 125.00 137.59   66
 13  \w    -97.00 -36.00   0.50    0.30    --  -68.00 133.00  99.65  122
 14  \w    -90.00 -27.00   0.50    0.30    --  -66.62 125.00 -30.00  126
 15  \w    -91.00 -28.00   0.50    0.30    --  -66.62 125.00 -90.00  126
 16  \w    -91.00 -41.00   0.50    0.30    --  -66.62 125.00-150.00  100
 17  \w    -94.00 -60.00   0.50    0.30    --  -72.00 118.00-111.35   68
 18  \w    -94.00 -42.00   0.50    0.30    --  -72.70 118.00 -38.62  104
 19  \w    -94.00 -68.00   0.50    0.30    --  -72.70 117.00 -59.52   52
 20  \w    -94.00 -60.00   0.50    0.30    --  -72.70 117.00  -8.94   68
 21  \w    -94.00 -68.00   0.50    0.30    --  -72.70 117.00 105.73   52
 22  \w    -94.00 -69.00   0.50    0.30    --  -72.70 117.00  87.11   50
 23  \w    -89.00 -29.00   0.50    0.30    --  -68.00 116.00 164.04  120
 24  \w    -93.00 -67.00   0.50    0.30    --  -72.70 115.00 169.64   52
 25  \w   -110.00 -85.00   0.50    0.30    --  -72.70 -65.00   0.92   50
 26  \w    -99.00 -72.00   0.50    0.30    --  -56.00 -40.00-113.34   54
 27  \w   -116.00 -91.00   0.50    0.30    --  -72.70 -39.00 -38.43   50
 28  \w   -112.00 -87.00   0.50    0.30    --  -72.70 -37.00 -71.76   50
 29  \w   -116.00 -91.00   0.50    0.30    --  -72.70 -38.00-111.04   50
 30  \w   -117.00 -88.00   0.50    0.30    --  -72.70 -33.00-149.11   58
 31  \w    -81.00 -56.00   0.50    0.30    --  -40.00 -50.00  29.55   50
 32  \w   -115.00 -89.00   0.50    0.30    --  -72.70 -37.00 156.55   52
 33  \w   -114.00 -88.00   0.50    0.30    --  -72.70 -52.00 122.41   52
 34  \w    -75.00 -39.00   0.50    0.30    --  -66.62 -15.00 -90.00   72
 35  \w   -105.00 -54.00   0.50    0.30    --  -66.62 -15.00  30.00  102
 36  \w    -89.00 -40.00   0.50    0.30    --  -66.62 -15.00  60.00   98
 37  \w   -116.00 -91.00   0.50    0.30    --  -72.70 -39.00  91.12   50
 38  \w   -112.00 -82.00   0.50    0.30    --  -72.70-113.00-119.51   60
 39  \w    -99.00 -72.00   0.50    0.30    --  -66.62   0.00 -90.00   54
 40  \w   -101.00 -33.00   0.50    0.30    --  -66.62   0.00 -30.00  136
 41  \w    -65.00 -39.00   0.50    0.30    --  -66.62   0.00 -90.00   52
 42  \w    -59.00 -34.00   0.50    0.30    --  -72.70  54.00-116.44   50
 43  \w     32.00  57.00   0.50    0.30    --   72.70 -53.00  79.79   50
 44  \w     40.00 101.00   0.50    0.30    --   72.70-132.00 120.58  122
 45  \w     69.00  94.00   0.50    0.30    --   72.70-118.00 132.82   50
 46  \w     34.00  59.00   0.50    0.30    --   72.70 -57.00 136.26   50
 47  \w     37.00  91.00   0.50    0.30    --   72.70-115.00   8.27  108
 48  \w     32.00  94.00   0.50    0.30    --   72.70-117.00 -48.41  124
 49  \w     34.00  59.00   0.50    0.30    --   72.70-123.00 -79.91   50
 50  \w     66.00  97.00   0.50    0.30    --   72.70-123.00 -79.91   62
;
_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      -0.1147912000
_diffrn_orient_matrix_UB_12      -0.0297479000
_diffrn_orient_matrix_UB_13      -0.0190236000
_diffrn_orient_matrix_UB_21      0.0159417000
_diffrn_orient_matrix_UB_22      0.0139211000
_diffrn_orient_matrix_UB_23      -0.0651103000
_diffrn_orient_matrix_UB_31      -0.0052319000
_diffrn_orient_matrix_UB_32      -0.0997530000
_diffrn_orient_matrix_UB_33      -0.0289627000
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73042
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.609
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.324
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (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 light brown'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         17574
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0107P)^2^+12.8192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16403
_reflns_number_total             17574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-389
_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_original_cell_volume        4588.43(13)
_cod_database_code               1567201
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C60 H146 Cs1 N3 O16 Si8 U2'
_shelx_estimated_absorpt_t_max   0.534
_shelx_estimated_absorpt_t_min   0.239
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Si4 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
Cs1A \\sim Cs1B \\sim Cs1C: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
3. Others
 Fixed Sof: Cs1A(0.92) Cs1B(0.05) Cs1C(0.03)
4.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14C,
 H14B), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), 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), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60C,H60B)
;
_shelx_res_checksum              11915
_shelx_hkl_checksum              92433
_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 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.710