Reactivity studies involving a Lewis base supported terminal uranium phosphinidene metallocene [η<sup>5</sup>-1,3-(Me<sub>3</sub>C)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>U([double bond, length as m-dash]P-2,4,6-<sup>i</sup>Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>)(OPMe<sub>3</sub>).
Wang, Deqiang; Wang, Shichun; Li, Tongyu; Heng, Yi; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8349–8363; doi:10.1039/d1dt00742d

data_7707403
_publ_section_title
;
 Reactivity studies involving a Lewis base supported terminal uranium
 phosphinidene metallocene
 [\h<sup>5</sup>-1,3-(Me<sub>3</sub>C)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>U([double
 bond, length as
 m-dash]P-2,4,6-<sup>i</sup>Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>)(OPMe<sub>3</sub>).
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8349
_journal_page_last               8363
_journal_paper_doi               10.1039/d1dt00742d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C44 H74 O P2 U'
_chemical_formula_sum            'C44 H74 O P2 U'
_chemical_formula_weight         919.00
_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             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-08 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                77.525(4)
_cell_angle_beta                 76.193(4)
_cell_angle_gamma                75.636(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2470(4)
_cell_length_b                   13.8930(6)
_cell_length_c                   15.3588(8)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.5330
_cell_measurement_theta_min      4.5930
_cell_volume                     2226.10(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -93.00 -64.00   1.00    1.00    --  -41.49 125.00  90.00   29
  2  \w    -34.00  -7.00   1.00    1.00    --  -41.49 125.00  90.00   27
  3  \w    -70.00  28.00   1.00    1.00    --  -41.49  57.00  30.00   98
  4  \w    -50.00  -2.00   1.00    1.00    --  -41.49 125.00 120.00   48
  5  \w   -112.00 -21.00   1.00    1.00    --  -41.49 -57.00-120.00   91
  6  \w    -22.00  69.00   1.00    1.00    --   41.49 -57.00  90.00   91
  7  \w     30.00 113.00   1.00    1.00    --  104.69-112.00  12.00   83
  8  \w     33.00  63.00   1.00    1.00    --  104.69 -61.00-150.00   30
  9  \w     45.00 122.00   1.00    1.00    --  104.69 -77.00   0.00   77
 10  \w     41.00 130.00   1.00    1.00    --  104.69 -45.00  90.00   89
 11  \w     63.00  89.00   1.00    1.00    --  104.69 -94.00 -60.00   26
 12  \w     38.00 124.00   1.00    1.00    --  104.69 -45.00   0.00   86
 13  \w     79.00 109.00   1.00    1.00    --  104.69 -94.00  90.00   30
 14  \w     61.00  90.00   1.00    1.00    --  104.69 -94.00-180.00   29
 15  \w     46.00 110.00   1.00    1.00    --  104.69 -45.00-150.00   64
 16  \w    108.00 171.00   1.00    1.00    --  104.69  77.00 150.00   63
 17  \w     63.00 109.00   1.00    1.00    --  104.69 -94.00-150.00   46
 18  \w     18.00 173.00   1.00    1.00    --  104.69   0.00 150.00  155
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0626566000
_diffrn_orient_matrix_UB_12      0.0490512000
_diffrn_orient_matrix_UB_13      0.0529389000
_diffrn_orient_matrix_UB_21      -0.0433269000
_diffrn_orient_matrix_UB_22      -0.0702688000
_diffrn_orient_matrix_UB_23      0.0881431000
_diffrn_orient_matrix_UB_31      0.1224147000
_diffrn_orient_matrix_UB_32      -0.0783148000
_diffrn_orient_matrix_UB_33      -0.0200439000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.136
_diffrn_reflns_theta_min         4.098
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.592
_refine_diff_density_min         -2.570
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8521
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+6.2820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7941
_reflns_number_total             8521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00742d2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7707402--7707416.cif.'
_cod_database_code               7707403
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1
_shelx_estimated_absorpt_t_max   0.214
_shelx_estimated_absorpt_t_min   0.214
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 C42, C43, C44, P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C42 \\sim C43 \\sim C44 \\sim P2: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C42) = Uanis(C44)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C39(H39)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C31(H31)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              96678
_shelx_hkl_checksum              95284
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.958
_oxdiff_exptl_absorpt_empirical_full_min 0.401