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_7046550
_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_absolute_configuration ad
_chemical_formula_moiety         'C26 H48 N2 Si2 U'
_chemical_formula_sum            'C26 H48 N2 Si2 U'
_chemical_formula_weight         682.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-09 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2573(14)
_cell_length_b                   14.8359(16)
_cell_length_c                   15.4478(17)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.45
_cell_volume                     3038.3(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_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  0.0181
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24124
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.436
_exptl_absorpt_correction_T_max  0.3343
_exptl_absorpt_correction_T_min  0.1999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1289 before and 0.0495 after correction. The Ratio of minimum to maximum transmission is 0.5980. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7482
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+4.0732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                7236
_reflns_number_total             7482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt01406j2.cif
_cod_data_source_block           pr4143
_cod_depositor_comments
'Adding full bibliography for 7046548--7046550.cif.'
_cod_database_code               7046550
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C14') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(C1')=Sof(C2')=Sof(C3')=Sof(C4')=Sof(C5')=Sof(C6')=Sof(H6'A)=Sof(H6'B)=
 Sof(H6'C)=Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(H7'C)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=
 Sof(H8'C)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=Sof(C10')=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(C11')=Sof(C12')=Sof(C13')=Sof(C14')=Sof(C15')=Sof(C16')=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17')=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18')=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19')=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=FVAR(2)
4.a Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C6'(H6'A,H6'B,H6'C), C7'(H7'A,H7'B,H7'C), C8'(H8'A,H8'B,H8'C),
 C9'(H9'A,H9'B,H9'C), C10'(H10D,H10E,H10F), C16'(H16D,H16E,H16F), C17'(H17D,
 H17E,H17F), C18'(H18D,H18E,H18F), C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F)
4.b Cp* refined as free rotating group:
 C1(C2,C3,C4,C5,C6,C7,C8,C9,C10), C11(C12,C13,C14,C15,C16,C17,C18,C19,C20),
 C1'(C2',C3',C4',C5',C6',C7',C8',C9',C10'), C11'(C12',C13',C14',C15',C16',C17',
 C18',C19',C20')
;
_olex2_submission_special_instructions 'No special instructions were received'