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_7707412
_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 N O P2 U'
_chemical_formula_sum            'C44 H74 N O P2 U'
_chemical_formula_weight         933.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-17
_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                90
_cell_angle_beta                 90.1840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.99370(10)
_cell_length_b                   27.2685(2)
_cell_length_c                   15.12480(10)
_cell_measurement_reflns_used    21559
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.9260
_cell_measurement_theta_min      4.3300
_cell_volume                     4534.12(6)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_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    -60.00  32.00   1.00    1.00    --  -41.49  37.00  60.00   92
  2  \w    -93.00 -67.00   1.00    1.00    --  -41.49 -37.00 120.00   26
  3  \w     47.00  87.00   1.00    1.00    --   41.49-125.00  60.00   40
  4  \w      2.00  70.00   1.00    1.00    --   41.49 -99.00-180.00   68
  5  \w     30.00  56.00   1.00    1.00    --   41.49-125.00 -30.00   26
  6  \w     84.00 128.00   1.00    1.00    --  104.69  77.00 -30.00   44
  7  \w    120.00 146.00   1.00    1.00    --  104.69  45.00-150.00   26
  8  \w     95.00 171.00   1.00    1.00    --  104.69  77.00 -90.00   76
  9  \w     25.00 100.00   1.00    1.00    --  104.69 -94.00-180.00   75
 10  \w     61.00 124.00   1.00    1.00    --  104.69 -61.00-150.00   63
 11  \w     94.00 175.00   1.00    1.00    --  104.69 125.00-180.00   81
 12  \w     89.00 115.00   1.00    1.00    --  104.69  45.00-150.00   26
 13  \w     82.00 127.00   1.00    1.00    --  104.69  45.00 -90.00   45
 14  \w     -1.00  30.00   1.00    1.00    --  -41.74  57.00 150.00   31
 15  \w    -58.00  30.00   1.00    1.00    --  -41.74  57.00 -90.00   88
 16  \w    -69.00 -41.00   1.00    1.00    --  -41.74  57.00 150.00   28
 17  \w   -110.00 -71.00   1.00    1.00    --  -41.74 -57.00 120.00   39
 18  \w     89.00 132.00   1.00    1.00    --  104.69 -30.00 -30.00   43
 19  \w     59.00 105.00   1.00    1.00    --  104.69-111.00   0.00   46
 20  \w     94.00 137.00   1.00    1.00    --  104.69 -77.00   0.00   43
 21  \w     31.00  83.00   1.00    1.00    --  104.69-111.00  30.00   52
 22  \w     35.00  62.00   1.00    1.00    --  104.69 -30.00 -30.00   27
 23  \w     62.00  87.00   1.00    1.00    --  104.69 178.00-120.00   25
 24  \w    108.00 148.00   1.00    1.00    --  104.69 178.00-120.00   40
;
_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      0.1149234000
_diffrn_orient_matrix_UB_12      -0.0288775000
_diffrn_orient_matrix_UB_13      0.0264423000
_diffrn_orient_matrix_UB_21      0.0162611000
_diffrn_orient_matrix_UB_22      0.0332218000
_diffrn_orient_matrix_UB_23      0.0815223000
_diffrn_orient_matrix_UB_31      -0.0785192000
_diffrn_orient_matrix_UB_32      -0.0354185000
_diffrn_orient_matrix_UB_33      0.0550359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30427
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.345
_diffrn_reflns_theta_min         4.336
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41652
_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            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+4.4548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8492
_reflns_number_total             8686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00742d2.cif
_cod_data_source_block           compound20
_cod_depositor_comments
'Adding full bibliography for 7707402--7707416.cif.'
_cod_database_code               7707412
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1
_shelx_estimated_absorpt_t_max   0.218
_shelx_estimated_absorpt_t_min   0.170
_reflns_odcompleteness_completeness 99.13
_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.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C31(H31)
2.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              49366
_shelx_hkl_checksum              43295
_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 1.812
_oxdiff_exptl_absorpt_empirical_full_min 0.644