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_1558114
_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         'C35 H59 N2 P Si2 U'
_chemical_formula_sum            'C35 H59 N2 P Si2 U'
_chemical_formula_weight         833.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2018-02-28 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.155(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0922(13)
_cell_length_b                   11.4805(6)
_cell_length_c                   18.3590(11)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.34
_cell_volume                     3661.7(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.345
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.567
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.4544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0901 before and 0.0692 after correction.
The Ratio of minimum to maximum transmission is 0.8067.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.149(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7456
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0224
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0404
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6935
_reflns_number_total             7456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02261f2.cif
_cod_data_source_block           final_m_b
_cod_depositor_comments
;Adding full bibliography for 1558114--1558116.cif.

 Adding full bibliography for 1558114--1558116.cif.
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1558114
_shelxl_version_number           2014-3
_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:
 C28(H28), C26(H26)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C9(H9A,H9B,H9C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C32(H32A,
 H32B,H32C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C7(H7A,
 H7B,H7C), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C21(H21A,H21B,H21C),
 C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'