Four-electron reduction chemistry using a uranium(iii) phosphido complex.
Rungthanaphatsophon, Pokpong; Barnes, Charles L.; Kelley, Steven P.; Walensky, Justin R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8189–8192; doi:10.1039/c8dt01406j

data_7046549
_publ_section_title
;
 Four-electron reduction chemistry using a uranium(iii) phosphido complex.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8189
_journal_page_last               8192
_journal_paper_doi               10.1039/c8dt01406j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C78 H117 N6 U3, 0.5(C5)'
_chemical_formula_sum            'C80.5 H117 N6 U3'
_chemical_formula_weight         1882.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-03-12 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8226(9)
_cell_length_b                   23.0418(10)
_cell_length_c                   19.0030(9)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.33
_cell_volume                     8241.7(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  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            121252
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.362
_diffrn_reflns_theta_min         2.319
_exptl_absorpt_coefficient_mu    5.922
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.4120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3672
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.194
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.440(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     914
_refine_ls_number_reflns         20577
_refine_ls_number_restraints     1390
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0322P)^2^+18.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                17059
_reflns_number_total             20577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01406j2.cif
_cod_data_source_block           final_a
_cod_depositor_comments
'Adding full bibliography for 7046548--7046550.cif.'
_cod_original_formula_sum        'C80.50 H117 N6 U3'
_cod_database_code               7046549
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.375
_shelx_estimated_absorpt_t_max   0.721
_shelx_res_checksum              34325