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_7707405
_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         'C52 H81 N O P2 U, C6 H6'
_chemical_formula_sum            'C58 H87 N O P2 U'
_chemical_formula_weight         1114.25
_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             2019-01-15
_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                88.637(2)
_cell_angle_beta                 88.144(3)
_cell_angle_gamma                66.662(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5859(4)
_cell_length_b                   13.4822(4)
_cell_length_c                   17.7155(5)
_cell_measurement_reflns_used    14331
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9630
_cell_measurement_theta_min      3.5610
_cell_volume                     2758.48(16)
_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    -53.00  -7.00   1.00    1.00    --  -41.49 125.00 -30.00   46
  2  \w    -76.00  43.00   1.00    1.00    --  -41.49   0.00-180.00  119
  3  \w    -47.00  28.00   1.00    1.00    --  -41.49  37.00-120.00   75
  4  \w     32.00  98.00   1.00    1.00    --   41.49-125.00   0.00   66
  5  \w     31.00  74.00   1.00    1.00    --   41.49-125.00-180.00   43
  6  \w     32.00 133.00   1.00    1.00    --  104.69 -61.00-180.00  101
  7  \w     66.00  98.00   1.00    1.00    --  104.69 -94.00 -60.00   32
  8  \w     30.00 135.00   1.00    1.00    --  104.69 -77.00 -30.00  105
  9  \w     93.00 119.00   1.00    1.00    --  104.69  45.00 -30.00   26
 10  \w     82.00 172.00   1.00    1.00    --  104.69  45.00 150.00   90
 11  \w    144.00 177.00   1.00    1.00    --  104.69  45.00 -30.00   33
 12  \w     65.00 116.00   1.00    1.00    --  104.69-125.00 150.00   51
 13  \w     29.00  98.00   1.00    1.00    --  104.69 -77.00 120.00   69
 14  \w     81.00 118.00   1.00    1.00    --  104.69-125.00 -90.00   37
 15  \w     34.00 133.00   1.00    1.00    --  104.69 -30.00 -30.00   99
 16  \w     32.00 148.00   1.00    1.00    --  104.69 -15.00 150.00  116
 17  \w     84.00 109.00   1.00    1.00    --  104.69 -94.00 -30.00   25
 18  \w     31.00  56.00   1.00    1.00    --  104.69 -94.00-180.00   25
;
_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      0.0360034000
_diffrn_orient_matrix_UB_12      -0.0771481000
_diffrn_orient_matrix_UB_13      0.0687650000
_diffrn_orient_matrix_UB_21      -0.1277164000
_diffrn_orient_matrix_UB_22      0.0197596000
_diffrn_orient_matrix_UB_23      0.0163984000
_diffrn_orient_matrix_UB_31      0.0132395000
_diffrn_orient_matrix_UB_32      -0.0956413000
_diffrn_orient_matrix_UB_33      -0.0507311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19743
_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         72.125
_diffrn_reflns_theta_min         3.571
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17261
_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    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.552
_refine_diff_density_min         -2.579
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         10577
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0618P)^2^+0.4419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10185
_reflns_number_total             10577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00742d2.cif
_cod_data_source_block           compound15
_cod_depositor_comments
'Adding full bibliography for 7707402--7707416.cif.'
_cod_original_cell_volume        2758.48(15)
_cod_database_code               7707405
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1
_shelx_estimated_absorpt_t_max   0.263
_shelx_estimated_absorpt_t_min   0.209
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C24, C25, C26, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C26 \\sim C24A \\sim C25A \\sim C26A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C24A)
\\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C26A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C41(H41), C44(H44), C47(H47)
5.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C37(H37), C39(H39), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58)
5.d 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), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              51590
_shelx_hkl_checksum              30108
_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 5.017
_oxdiff_exptl_absorpt_empirical_full_min 0.559