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_7126256
_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 H40 B2 F30 N6 Na2 O4'
_chemical_formula_sum            'C52 H40 B2 F30 N6 Na2 O4'
_chemical_formula_weight         1450.50
_chemical_name_systematic
Bis((tris(pentafluorophenyl)borylazido)-bis(diethyl-ether)-sodium)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_chemical_temperature_decomposition 410
_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             2019-08-26
_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                70.9380(10)
_cell_angle_beta                 81.4520(10)
_cell_angle_gamma                72.2550(10)
_cell_formula_units_Z            1
_cell_length_a                   11.1153(4)
_cell_length_b                   11.7453(4)
_cell_length_c                   12.4529(4)
_cell_measurement_reflns_used    20441
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.097
_cell_measurement_theta_min      1.976
_cell_volume                     1461.32(9)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20441
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         1.976
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0427P)^2^+0.5239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5483
_reflns_number_total             5943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01356k2.cif
_cod_data_source_block           mab_4_163_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 '410
(decomp.)'. The value '410 (decomp.)' was changed to '410'.

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

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

 Adding full bibliography for 7126254--7126256.cif.
;
_cod_database_code               7126256
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.972
_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. Rigid bond restraints
 N1, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C122)
4. Others
 Sof(C121)=Sof(H12A)=Sof(H12B)=Sof(C122)=Sof(H12C)=Sof(H12D)=Sof(H12E)=1-FVAR(1)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C25(H25A,H25B), C23(H23A,H23B), C21(H21A,H21B), C121(H12A,H12B)
5.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C20(H20A,H20B,
 H20C), C122(H12C,H12D,H12E)
;
_shelx_res_checksum              89221
_olex2_submission_special_instructions 'No special instructions were received'