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_1558115
_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 H58 N2 P Si2 U'
_chemical_formula_sum            'C35 H58 N2 P Si2 U'
_chemical_formula_weight         832.01
_chemical_name_systematic
Bis(pentamethylcyclopentadienyl)-P-trimethylsilyl-P-methylphosphimido-trimethylsilylimidouranium(VI)
_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
_audit_creation_date             2019-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                82.061(4)
_cell_angle_beta                 76.900(6)
_cell_angle_gamma                65.055(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8231(11)
_cell_length_b                   11.2078(13)
_cell_length_c                   19.039(3)
_cell_measurement_reflns_used    9332
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.24
_cell_volume                     1849.0(4)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            101517
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.754
_diffrn_reflns_theta_min         2.241
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.522
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.3992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1229 before and 0.0790 after correction. The Ratio of minimum to maximum transmission is 0.7087. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       prism
_exptl_crystal_F_000             834
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         11.865
_refine_diff_density_min         -8.609
_refine_diff_density_rms         0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         9335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+109.0689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8560
_reflns_number_total             9335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02261f2.cif
_cod_data_source_block           m2_a
_cod_depositor_comments
;Adding full bibliography for 1558114--1558116.cif.

 Adding full bibliography for 1558114--1558116.cif.
;
_cod_database_code               1558115
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.591
_shelx_estimated_absorpt_t_min   0.480
_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:
 C29(H29)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C),
 C16(H16A,H16B,H16C), C6(H6A,H6B,H6C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              12836
_olex2_submission_special_instructions 'No special instructions were received'