Lewis acid capping of a uranium(v) nitride via a uranium(iii) azide molecular square.
Boreen, Michael A.; Rao, Guodong; Villarreal, David G.; Watt, Fabian A.; Britt, R. David; Hohloch, Stephan; Arnold, John; Chemical communications (Cambridge, England) 56 (2020) 4535–4538; doi:10.1039/d0cc01356k

data_7126255
_publ_section_title
;
 Lewis acid capping of a uranium(v) nitride via a uranium(iii) azide
 molecular square.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4535
_journal_page_last               4538
_journal_paper_doi               10.1039/d0cc01356k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C52 H58 B F15 N U, C3.5 H4'
_chemical_formula_sum            'C55.5 H62 B F15 N U'
_chemical_formula_weight         1276.90
_chemical_name_systematic
'Bis(1,2,3,4-tetrakis(isopropyl)cyclopentadienyl)-(tris(pentafluorophenyl)borylnitrido)-uranium(v) toluene sovlate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_chemical_temperature_decomposition 427
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                100.421(2)
_cell_angle_beta                 97.392(2)
_cell_angle_gamma                116.686(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5562(5)
_cell_length_b                   13.4735(6)
_cell_length_c                   18.1929(8)
_cell_measurement_reflns_used    34714
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.042
_cell_measurement_theta_min      1.877
_cell_volume                     2626.3(2)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34714
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         1.877
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1268
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0081P)^2^+3.6030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9016
_reflns_number_total             9599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01356k2.cif
_cod_data_source_block           mab_v_001_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_temperature_decomposition' since the value had been '427
(decomp.)'. The value '427 (decomp.)' was changed to '427'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126254--7126256.cif.
;
_cod_original_formula_sum        'C55.50 H62 B F15 N U'
_cod_database_code               7126255
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.805
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C55, C57}
3. Others
 Fixed Sof: H53(0.5) H53A(0.5) H54(0.5) H54A(0.5) C55(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) H56C(0.5) C57(0.5) H57(0.5)
4.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C9(H9), C23(H23), C6(H6), C12(H12), C15(H15), C32(H32)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C1(H1), C53(H53), C53(H53A), C54(H54), C54(H54A), C57(H57)
4.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C27(H27A,H27B,H27C), C10(H10A,H10B,
 H10C), C8(H8A,H8B,H8C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C14(H14A,
 H14B,H14C), C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C),
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C33(H33A,H33B,H33C), C30(H30A,H30B,
 H30C), C7(H7A,H7B,H7C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              79135
_olex2_submission_special_instructions 'No special instructions were received'