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_1567203
_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             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                80.346(4)
_cell_angle_beta                 83.800(4)
_cell_angle_gamma                71.074(4)
_cell_formula_units_Z            2
_cell_length_a                   13.9128(5)
_cell_length_b                   16.1167(6)
_cell_length_c                   21.8294(10)
_cell_measurement_reflns_used    10090
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.5650
_cell_measurement_theta_min      3.2720
_cell_volume                     4557.0(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 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_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    -78.00  -9.00   1.00    7.50    --  -43.50 105.00-132.00   69
  2  \w     23.00  77.00   1.00    7.50    --   43.68-105.00 127.00   54
  3  \w     66.00 108.00   1.00   35.00    --  101.68-105.00 127.00   42
  4  \w    110.00 176.00   1.00   35.00    --  101.68 105.00-132.00   66
  5  \w   -114.00 -17.00   1.00    7.50    --  -43.50 -57.00 120.00   97
  6  \w   -115.00 -21.00   1.00    7.50    --  -43.50 -37.00   0.00   94
  7  \w    -53.00  21.00   1.00    7.50    --  -43.50  37.00 -30.00   74
  8  \w     67.00  94.00   1.00   35.00    --  101.68 -61.00 -60.00   27
  9  \w     36.00  63.00   1.00   35.00    --  101.68 -94.00-150.00   27
 10  \w    117.00 144.00   1.00   35.00    --  101.68  77.00-150.00   27
 11  \w    103.00 131.00   1.00   35.00    --  101.68  77.00-120.00   28
 12  \w     40.00  96.00   1.00   35.00    --  101.68-125.00   0.00   56
 13  \w     35.00 113.00   1.00   35.00    --  101.68-125.00  30.00   78
 14  \w     40.00 112.00   1.00   35.00    --  101.68-125.00  90.00   72
 15  \w    104.00 168.00   1.00   35.00    --  101.68 125.00 -60.00   64
 16  \w     54.00 106.00   1.00   35.00    --  101.68 -94.00-120.00   52
 17  \w    104.00 156.00   1.00   35.00    --  101.68  77.00  90.00   52
 18  \w    119.00 146.00   1.00   35.00    --  101.68  77.00 120.00   27
 19  \w     79.00 172.00   1.00   35.00    --  101.68  45.00-150.00   93
 20  \w     30.00  86.00   1.00   35.00    --  101.68 -45.00   0.00   56
 21  \w     96.00 121.00   1.00   35.00    --  101.68 -45.00   0.00   25
 22  \w     88.00 113.00   1.00   35.00    --  101.68-125.00-150.00   25
 23  \w     38.00 120.00   1.00   35.00    --  101.68 -45.00-180.00   82
 24  \w     75.00 172.00   1.00   35.00    --  101.68  61.00 150.00   97
;
_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      -0.0321768000
_diffrn_orient_matrix_UB_12      0.0089503000
_diffrn_orient_matrix_UB_13      0.0689700000
_diffrn_orient_matrix_UB_21      -0.0835878000
_diffrn_orient_matrix_UB_22      -0.0423769000
_diffrn_orient_matrix_UB_23      -0.0032569000
_diffrn_orient_matrix_UB_31      0.0756691000
_diffrn_orient_matrix_UB_32      -0.0924272000
_diffrn_orient_matrix_UB_33      0.0193441000
_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  0.0808
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41825
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.009
_diffrn_reflns_theta_min         2.928
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.423
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.218
_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 pale yellow'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       needle
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.122
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         17412
_refine_ls_number_restraints     588
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11289
_reflns_number_total             17412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-407b
_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               1567203
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C60 H144 Cs N3 O16 Si8 U2'
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.237
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
3. Others
 Sof(O62B)=Sof(O64B)=1-FVAR(1)
 Sof(O62A)=Sof(O64A)=FVAR(1)
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1)
4.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),
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C27A(H27A,H27B,H27C), C27B(H27D,
 H27E,H27F), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F), 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)
;
_shelx_res_checksum              50470
_shelx_hkl_checksum              71668
_olex2_date_sample_data_collection 2021-08-25
_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 2.338
_oxdiff_exptl_absorpt_empirical_full_min 0.487