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_7707404
_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         'C29 H51 Cl O P U'
_chemical_formula_sum            'C29 H51 Cl O P U'
_chemical_formula_weight         720.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2020-11-08 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.30130(10)
_cell_length_b                   11.9655(2)
_cell_length_c                   29.1545(4)
_cell_measurement_reflns_used    9530
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      73.1730
_cell_measurement_theta_min      3.9890
_cell_volume                     3593.40(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      100.02(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 0.969
_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    -70.00 -21.00   1.00    1.00    --  -41.49  57.00 150.00   49
  2  \w   -115.00 -16.00   1.00    1.00    --  -41.49 -57.00 -30.00   99
  3  \w    -46.00 -17.00   1.00    1.00    --  -41.49 -37.00-150.00   29
  4  \w   -114.00 -50.00   1.00    1.00    --  -41.49 -37.00-150.00   64
  5  \w     46.00 124.00   1.00    1.00    --  107.19 -30.00  60.00   78
  6  \w    104.00 135.00   1.00    1.00    --  107.19  45.00 -30.00   31
  7  \w     48.00  80.00   1.00    1.00    --  107.19 -61.00 -60.00   32
  8  \w     83.00 164.00   1.00    1.00    --  107.19  61.00  90.00   81
  9  \w     61.00  87.00   1.00    1.00    --  107.19 -94.00 -30.00   26
 10  \w     32.00  58.00   1.00    1.00    --  107.19 -94.00 -30.00   26
 11  \w    102.00 136.00   1.00    1.00    --  107.19 -61.00 -60.00   34
 12  \w    114.00 178.00   1.00    1.00    --  107.19 125.00 150.00   64
 13  \w     86.00 162.00   1.00    1.00    --  107.19  30.00  30.00   76
;
_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      -0.0558121000
_diffrn_orient_matrix_UB_12      -0.1174319000
_diffrn_orient_matrix_UB_13      0.0087310000
_diffrn_orient_matrix_UB_21      0.1008082000
_diffrn_orient_matrix_UB_22      -0.0183190000
_diffrn_orient_matrix_UB_23      0.0387006000
_diffrn_orient_matrix_UB_31      -0.0952718000
_diffrn_orient_matrix_UB_32      0.0495545000
_diffrn_orient_matrix_UB_33      0.0349205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            14337
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.410
_diffrn_reflns_theta_min         3.994
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6645
_reflns_number_total             7007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00742d2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7707402--7707416.cif.'
_cod_original_cell_volume        3593.41(9)
_cod_database_code               7707404
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1P1Cl1Si1U1
_reflns_odcompleteness_completeness 99.93
_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. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21')=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=Sof(C22')=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C16(H16), C18(H18)
4.b 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), C20'(H20D,H20E,H20F), C21'(H21D,H21E,H21F),
 C22'(H22D,H22E,H22F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              5635
_shelx_hkl_checksum              73222
_shelx_fab_checksum              49027
_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 2.934
_oxdiff_exptl_absorpt_empirical_full_min 0.570