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_7126254
_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         'C136 H232 N12 U4, 1.82(C2.74 H6.58)'
_chemical_formula_sum            'C141 H244 N12 U4'
_chemical_formula_weight         3059.59
_chemical_name_systematic
'Tetrakis(bis(1,2,3,4-tetra(isopropyl)cyclopentadienyl)-azido-uranium(iii)) n-pentane solvate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_chemical_temperature_decomposition 407
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-11
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7855(5)
_cell_length_b                   20.7855(5)
_cell_length_c                   35.3744(10)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.21
_cell_volume                     15283.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    SHELXT-2014
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            104285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         1.500
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.272
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.3804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       Block
_exptl_crystal_F_000             6168
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.029(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         14035
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0164P)^2^+38.8932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                11893
_reflns_number_total             14035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01356k2.cif
_cod_data_source_block           mab_iii_181_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 '407
(decomp.)'. The value '407 (decomp.)' was changed to '407'.

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

 Adding full bibliography for 7126254--7126256.cif.
;
_cod_original_cell_volume        15283.0(9)
_cod_database_code               7126254
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.427
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.971(9)
 0.029(9)
2. 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
3. Shared sites
{C69, C69'}
{C71, C71'}
4. Restrained distances
 C60'-C61'
 1.54 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C69) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C52) = Uanis(C52')
Uanis(C53) = Uanis(C53')
Uanis(C54) = Uanis(C54')
Uanis(C55) = Uanis(C55')
Uanis(C56) = Uanis(C56')
Uanis(C57) = Uanis(C57')
Uanis(C58) = Uanis(C58')
Uanis(C59) = Uanis(C59')
Uanis(C60) = Uanis(C60')
Uanis(C61) = Uanis(C61')
Uanis(C62) = Uanis(C62')
Uanis(C64) = Uanis(C64')
Uanis(C65) = Uanis(C65')
Uanis(C66) = Uanis(C66')
Uanis(C67) = Uanis(C67')
6. Others
 Sof(C70')=Sof(H70C)=Sof(H70D)=Sof(C69')=Sof(H69D)=Sof(H69E)=Sof(H69F)=1-FVAR(1)
 Sof(C71')=Sof(H71C)=Sof(H71D)=0.5*(1-FVAR(2))
 Sof(C71)=Sof(H71A)=Sof(H71B)=0.5*FVAR(2)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=FVAR(1)
 Sof(C55')=Sof(C54')=Sof(H54')=Sof(C53')=Sof(C52')=Sof(C56')=Sof(C60')=
 Sof(H60')=Sof(C66')=Sof(H66')=Sof(C57')=Sof(H57')=Sof(C63')=Sof(H63')=
 Sof(C58')=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C61')=Sof(H61D)=Sof(H61E)=
 Sof(H61F)=Sof(C68')=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C62')=Sof(H62D)=
 Sof(H62E)=Sof(H62F)=Sof(C65')=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C67')=
 Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C64')=Sof(H64D)=Sof(H64E)=Sof(H64F)=
 Sof(C59')=Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(2)
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C60)=Sof(H60)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(H65A)=
 Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 Sof(C57)=Sof(H57)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C12(H12), C15(H15), C23(H23), C26(H26), C29(H29), C32(H32),
 C40(H40), C43(H43), C46(H46), C60(H60), C63(H63), C66(H66), C57(H57), C49(H49),
  C60'(H60'), C66'(H66'), C57'(H57'), C63'(H63')
7.b Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C71(H71A,H71B), C70'(H70C,H70D), C71'(H71C,H71D)
7.c Me refined with riding coordinates:
 C69'(H69D,H69E,H69F)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18), C35(H35), C52(H52), C54'(H54')
7.e Fitted pentagon refined as free rotating group:
 C52(C53,C54,C55,C56), C55'(C54',C53',C52',C56')
7.f Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C58'(H58D,H58E,H58F),
 C61'(H61D,H61E,H61F), C68'(H68D,H68E,H68F), C62'(H62D,H62E,H62F), C65'(H65D,
 H65E,H65F), C67'(H67D,H67E,H67F), C64'(H64D,H64E,H64F), C59'(H59D,H59E,H59F),
 C69(H69A,H69B,H69C)
;
_shelx_res_checksum              62374
_shelx_fab_checksum              23614
_olex2_submission_special_instructions 'No special instructions were received'