Synthesis and reactivity of the uranium phosphinidene metallocene [η<sup>5</sup>-1,3-(Me<sub>3</sub>Si)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>U(P-2,4,6-<sup>i</sup>Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>)(OPMe<sub>3</sub>): influence of the coordinated Lewis base.
Wang, Shichun; Heng, Yi; Li, Tongyu; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12502–12516; doi:10.1039/d1dt02149d

data_7707889
_publ_section_title
;
 Synthesis and reactivity of the uranium phosphinidene metallocene
 [\h<sup>5</sup>-1,3-(Me<sub>3</sub>Si)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>U(&#xE001;P-2,4,6-<sup>i</sup>Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>)(OPMe<sub>3</sub>):
 influence of the coordinated Lewis base.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12502
_journal_page_last               12516
_journal_paper_doi               10.1039/d1dt02149d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C47 H79 N O P2 Si4 U'
_chemical_formula_sum            'C47 H79 N O P2 Si4 U'
_chemical_formula_weight         1086.44
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                101.5020(10)
_cell_angle_beta                 101.4470(10)
_cell_angle_gamma                98.3560(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5160(2)
_cell_length_b                   14.2653(2)
_cell_length_c                   17.15030(10)
_cell_measurement_reflns_used    28423
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3730
_cell_measurement_theta_min      3.6710
_cell_volume                     2655.32(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_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    -27.00  28.00   0.50    0.05    --   46.95 -21.00 -10.00  110
  2  \w     29.00  61.00   0.50    0.05    --   46.95 -57.00 -60.00   64
  3  \w     29.00  95.00   0.50    0.05    --   46.95-125.00-150.00  132
  4  \w     70.00  95.00   0.50    0.05    --   46.95-125.00 -30.00   50
  5  \w     41.00  67.00   0.50    0.05    --  104.75-125.00-150.00   52
  6  \w     44.00  70.00   0.50    0.05    --  104.75 -94.00-120.00   52
  7  \w     75.00 101.00   0.50    0.05    --  104.75 -94.00-120.00   52
  8  \w     90.00 117.00   0.50    0.05    --  104.75-125.00-150.00   54
  9  \w     77.00 103.00   0.50    0.05    --  104.75 -94.00   0.00   52
 10  \w     35.00  61.00   0.50    0.05    --  104.75 -94.00   0.00   52
 11  \w     32.00 102.00   0.50    0.05    --  104.75 -77.00 -60.00  140
 12  \w     33.00  69.00   0.50    0.05    --  104.75 -61.00-180.00   72
 13  \w     40.00  65.00   0.50    0.05    --  104.75 -61.00-120.00   50
 14  \w     44.00 117.00   0.50    0.05    --  104.75-125.00 -30.00  146
 15  \w     41.00 108.00   0.50    0.05    --  104.75 -94.00  90.00  134
 16  \w     43.00 119.00   0.50    0.05    --   46.95  21.00 155.00  152
 17  \w     92.00 178.00   0.50    0.05    --  104.75  21.00 155.00  172
 18  \w     99.00 174.00   0.50    0.05    --  104.75  45.00  60.00  150
 19  \w    137.00 163.00   0.50    0.05    --  104.75  45.00   0.00   52
 20  \w     32.00 103.00   0.50    0.05    --  104.75 -77.00   0.00  142
 21  \w     37.00  63.00   0.50    0.05    --  104.75 -61.00   0.00   52
 22  \w     35.00  72.00   0.50    0.05    --  104.75 -61.00 120.00   74
 23  \w     44.00  73.00   0.50    0.05    --  104.75 -61.00 150.00   58
 24  \w    -20.00  23.00   0.50    0.05    --   46.95 -57.00 -60.00   86
 25  \w    -24.00  62.00   0.50    0.05    --   46.95 -57.00-120.00  172
 26  \w    -16.00  24.00   0.50    0.05    --  -46.95  21.00 155.00   80
 27  \w   -117.00 -77.00   0.50    0.05    --  -46.95-125.00 -30.00   80
 28  \w   -120.00 -41.00   0.50    0.05    --  -46.95 -21.00 -10.00  158
 29  \w    -67.00 -32.00   0.50    0.05    -- -102.00  61.00 150.00   70
 30  \w    -71.00 -29.00   0.50    0.05    -- -102.00 125.00  60.00   84
 31  \w    -55.00 -30.00   0.50    0.05    -- -102.00 125.00 150.00   50
 32  \w   -115.00 -81.00   0.50    0.05    -- -102.00 125.00  60.00   68
 33  \w   -117.00 -75.00   0.50    0.05    -- -102.00 125.00 150.00   84
 34  \w   -175.00 -91.00   0.50    0.05    -- -102.00 -21.00 -10.00  168
 35  \w   -152.00 -89.00   0.50    0.05    -- -102.00 -45.00-120.00  126
 36  \w    -68.00 -43.00   0.50    0.05    -- -102.00  61.00-180.00   50
 37  \w    -95.00 -69.00   0.50    0.05    -- -102.00 125.00-150.00   52
 38  \w    -56.00 -31.00   0.50    0.05    -- -102.00 125.00-150.00   50
 39  \w   -116.00 -80.00   0.50    0.05    -- -102.00 125.00 -60.00   72
 40  \w   -168.00 -95.00   0.50    0.05    -- -102.00 -15.00 -60.00  146
 41  \w   -169.00 -93.00   0.50    0.05    -- -102.00 -45.00  60.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1214840000
_diffrn_orient_matrix_UB_12      -0.0346863000
_diffrn_orient_matrix_UB_13      0.0077613000
_diffrn_orient_matrix_UB_21      -0.0555188000
_diffrn_orient_matrix_UB_22      -0.0912340000
_diffrn_orient_matrix_UB_23      0.0249070000
_diffrn_orient_matrix_UB_31      -0.0388090000
_diffrn_orient_matrix_UB_32      -0.0555541000
_diffrn_orient_matrix_UB_33      -0.0906185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.387
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.329
_refine_diff_density_min         -2.110
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         10732
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0343P)^2^+3.2640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10433
_reflns_number_total             10732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707889
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1Si1
_shelx_estimated_absorpt_t_max   0.308
_shelx_estimated_absorpt_t_min   0.233
_diffrn_oxdiff_digest_frames
;
019ca7d7a06fe2384d09abbc8d446d2e41038122970
;
_diffrn_oxdiff_digest_hkl
;
01eabe9461eca126c9f52e95adc8d7b31ac5bc
;
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 C33-C39 \\sim C33-C39A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C39-C41 \\sim C39A-C41A
 with sigma of 0.02
 C33-C40 \\sim C33-C40A
 with sigma of 0.04
 C33-C41 \\sim C33-C41A
 with sigma of 0.04
 C40-C41 \\sim C40A-C41A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C41A \\sim C40 \\sim C40A \\sim C41: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C39 \\sim C39A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=
 Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C36(H36), C39(H39), C42(H42), C39A(H39A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C32(H32), C34(H34)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C40A(H40D,H40E,H40F), C41A(H41D,H41E,
 H41F)
;
_shelx_res_checksum              39360
_shelx_hkl_checksum              35606
_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 2.175
_oxdiff_exptl_absorpt_empirical_full_min 0.669