Divergent uranium- versus phosphorus-based reduction of Me3SiN3 with steric modification of phosphido ligands
Ward, Robert J.; Rungthanaphatsophon, Pokpong; Rosal, Iker del; Kelley, Steven P.; Maron, Laurent; Walensky, Justin R.; Chemical Science 11 (2020) 5830–5835; doi:10.1039/D0SC02261F

data_1558116
_publ_section_title
;
 Divergent uranium- versus phosphorus-based reduction of Me3SiN3 with
 steric modification of phosphido ligands
;
_journal_issue                   22
_journal_name_full               'Chemical Science'
_journal_page_first              5830
_journal_page_last               5835
_journal_paper_doi               10.1039/D0SC02261F
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C33 H56 N P Si2 U'
_chemical_formula_sum            'C33 H56 N P Si2 U'
_chemical_formula_weight         791.96
_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     heavy
_audit_creation_date             2018-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-28 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                85.363(2)
_cell_angle_beta                 89.696(2)
_cell_angle_gamma                85.317(2)
_cell_formula_units_Z            4
_cell_length_a                   10.6409(6)
_cell_length_b                   16.5027(9)
_cell_length_c                   20.4856(11)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.26
_cell_volume                     3573.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53696
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.463
_diffrn_reflns_theta_min         2.263
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.675
_exptl_absorpt_correction_T_max  0.5634
_exptl_absorpt_correction_T_min  0.4445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0844 before and 0.0578 after correction. The Ratio of minimum to maximum transmission is 0.7890. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         17966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.0720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13437
_reflns_number_total             17966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02261f2.cif
_cod_data_source_block           pr_6043_0m_a
_cod_depositor_comments
;Adding full bibliography for 1558114--1558116.cif.

 Adding full bibliography for 1558114--1558116.cif.
;
_cod_database_code               1558116
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.545
_shelx_estimated_absorpt_t_min   0.364
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C27B(H27B), C24B(H24B), C23B(H23B), C27A(H27), C23A(H23), C26A(H26),
 C26B(H26B), C25B(H25B), C24A(H24), C25A(H25)
2.b Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C6B(H6BA,H6BB,H6BC), C6A(H8A,H8B,
 H8C), C17B(H17D,H17E,H17F), C18A(H19A,H19B,H19C), C16B(H16D,H16E,H16F),
 C32B(H32D,H32E,H32F), C7B(H7BA,H7BB,H7BC), C33B(H33D,H33E,H33F), C28A(H32A,
 H32B,H32C), C8B(H8BA,H8BB,H8BC), C31B(H31D,H31E,H31F), C16A(H17A,H17B,H17C),
 C17A(H18A,H18B,H18C), C28B(H28D,H28E,H28F), C9B(H9BA,H9BB,H9BC), C33A(H30A,
 H30B,H30C), C29B(H29D,H29E,H29F), C8A(H10A,H10B,H10C), C31A(H29A,H29B,H29C),
 C32A(H28A,H28B,H28C), C19A(H20A,H20B,H20C), C30A(H31A,H31B,H31C), C10A(H7A,H7B,
 H7C), C10B(H10D,H10E,H10F), C7A(H9A,H9B,H9C), C9A(H6A,H6B,H6C), C20B(H20D,H20E,
 H20F), C30B(H30D,H30E,H30F), C20A(H16A,H16B,H16C), C19B(H19D,H19E,H19F),
 C29A(H33A,H33B,H33C), C18B(H18D,H18E,H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'