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_7707411
_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         'C49 H83 N O P2 U'
_chemical_formula_sum            'C49 H83 N O P2 U'
_chemical_formula_weight         1002.13
_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             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                71.805(5)
_cell_angle_beta                 79.054(5)
_cell_angle_gamma                89.350(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3562(7)
_cell_length_b                   13.6804(7)
_cell_length_c                   17.5534(9)
_cell_measurement_reflns_used    13216
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.7950
_cell_measurement_theta_min      3.9340
_cell_volume                     2540.2(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.976
_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   -120.00  -2.00   1.00    1.00    --  -41.49 -19.00-180.00  118
  2  \w   -116.00 -42.00   1.00    1.00    --  -41.49 -37.00 120.00   74
  3  \w    -84.00 -12.00   1.00    1.00    --  -41.49 125.00 -90.00   72
  4  \w     23.00  49.00   1.00    1.00    --   41.49-125.00  90.00   26
  5  \w     39.00  93.00   1.00    1.00    --   41.49-125.00-180.00   54
  6  \w     94.00 137.00   1.00    1.00    --  104.69 -77.00 -60.00   43
  7  \w     25.00  81.00   1.00    1.00    --  104.69 -94.00-120.00   56
  8  \w     34.00 131.00   1.00    1.00    --  104.69 -45.00-120.00   97
  9  \w     89.00 175.00   1.00    1.00    --  104.69  45.00  90.00   86
 10  \w    149.00 178.00   1.00    1.00    --  104.69  98.00 -75.00   29
 11  \w     95.00 120.00   1.00    1.00    --  104.69 125.00 -60.00   25
 12  \w    145.00 177.00   1.00    1.00    --  104.69 125.00 -60.00   32
 13  \w     95.00 151.00   1.00    1.00    --  104.69  45.00  60.00   56
 14  \w     96.00 144.00   1.00    1.00    --  104.69 125.00 150.00   48
 15  \w     36.00  63.00   1.00    1.00    --  104.69-125.00 -60.00   27
 16  \w     72.00 150.00   1.00    1.00    --  104.69  77.00 120.00   78
 17  \w     75.00 118.00   1.00    1.00    --  104.69-125.00 -60.00   43
 18  \w     44.00 133.00   1.00    1.00    --  104.69 -30.00  90.00   89
 19  \w     59.00 106.00   1.00    1.00    --  104.69 -94.00 -30.00   47
 20  \w     33.00 118.00   1.00    1.00    --  104.69-125.00 150.00   85
;
_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      -0.0053018000
_diffrn_orient_matrix_UB_12      0.1110042000
_diffrn_orient_matrix_UB_13      -0.0565324000
_diffrn_orient_matrix_UB_21      0.0894929000
_diffrn_orient_matrix_UB_22      -0.0243722000
_diffrn_orient_matrix_UB_23      -0.0686254000
_diffrn_orient_matrix_UB_31      -0.1053688000
_diffrn_orient_matrix_UB_32      -0.0342713000
_diffrn_orient_matrix_UB_33      -0.0311817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.025
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20383
_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    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.618
_refine_diff_density_min         -2.126
_refine_diff_density_rms         0.130
_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     511
_refine_ls_number_reflns         9733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0443P)^2^+0.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9510
_reflns_number_total             9733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00742d2.cif
_cod_data_source_block           compound14
_cod_depositor_comments
'Adding full bibliography for 7707402--7707416.cif.'
_cod_database_code               7707411
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1
_shelx_estimated_absorpt_t_max   0.244
_shelx_estimated_absorpt_t_min   0.193
_reflns_odcompleteness_completeness 99.92
_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:
 C38(H38), C41(H41), C44(H44)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C34(H34), C36(H36)
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), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              85785
_shelx_hkl_checksum              91499
_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 2.903
_oxdiff_exptl_absorpt_empirical_full_min 0.603