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_7707885
_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         '2(C31 H56 O P S Si4 U), 1.5(C6 H6)'
_chemical_formula_sum            'C71 H121 O2 P2 S2 Si8 U2'
_chemical_formula_weight         1833.51
_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             2020-12-22
_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                81.9380(10)
_cell_angle_beta                 76.4210(10)
_cell_angle_gamma                71.8010(10)
_cell_formula_units_Z            2
_cell_length_a                   12.21870(10)
_cell_length_b                   17.1216(2)
_cell_length_c                   22.5679(2)
_cell_measurement_reflns_used    32501
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1970
_cell_measurement_theta_min      3.2110
_cell_volume                     4348.28(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.961
_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    133.00 159.00   0.50    0.05    --  104.75  15.00  90.00   52
  2  \w     91.00 131.00   0.50    0.05    --  104.75  15.00  90.00   80
  3  \w    103.00 172.00   0.50    0.05    --  104.75  15.00-150.00  138
  4  \w    149.00 177.00   0.50    0.05    --  104.75 125.00-150.00   56
  5  \w     84.00 136.00   0.50    0.05    --  104.75 125.00-150.00  104
  6  \w     77.00 102.00   0.50    0.05    --  104.75 125.00 -30.00   50
  7  \w    124.00 150.00   0.50    0.05    --  104.75 125.00 -30.00   52
  8  \w     80.00 168.00   0.50    0.05    --  104.75  81.00 -87.00  176
  9  \w     54.00  98.00   0.50    0.05    --   46.95  81.00 -87.00   88
 10  \w     37.00  70.00   0.50    0.05    --  104.75 -61.00 -30.00   66
 11  \w     32.00  58.00   0.50    0.05    --  104.75 -61.00 -60.00   52
 12  \w     35.00 106.00   0.50    0.05    --  104.75 -77.00 -30.00  142
 13  \w     33.00  73.00   0.50    0.05    --  104.75 -61.00  60.00   80
 14  \w    -24.00  18.00   0.50    0.05    --   46.95 -19.00 150.00   84
 15  \w     63.00 129.00   0.50    0.05    --  104.75 -81.00 149.00  132
 16  \w     76.00 115.00   0.50    0.05    --  104.75-125.00  60.00   78
 17  \w     75.00 111.00   0.50    0.05    --  104.75-125.00   0.00   72
 18  \w     32.00  67.00   0.50    0.05    --  104.75-125.00   0.00   70
 19  \w     33.00 113.00   0.50    0.05    --  104.75-125.00 -60.00  160
 20  \w     42.00 116.00   0.50    0.05    --  104.75-125.00-120.00  148
 21  \w     62.00 100.00   0.50    0.05    --  104.75 -94.00 -90.00   76
 22  \w     22.00  94.00   0.50    0.05    --   46.95-125.00  30.00  144
 23  \w     45.00  71.00   0.50    0.05    --  104.75-125.00  60.00   52
 24  \w     89.00 116.00   0.50    0.05    --  104.75-125.00 120.00   54
 25  \w    -24.00  62.00   0.50    0.05    --   46.95 -81.00 149.00  172
 26  \w   -107.00 -29.00   0.50    0.05    -- -102.00 125.00 120.00  156
 27  \w    -95.00 -70.00   0.50    0.05    -- -102.00  77.00  30.00   50
 28  \w    -68.00 -32.00   0.50    0.05    -- -102.00  61.00 -30.00   72
 29  \w    -87.00 -62.00   0.50    0.05    -- -102.00  81.00 -87.00   50
 30  \w    -66.00 -41.00   0.50    0.05    -- -102.00  61.00-150.00   50
 31  \w     -5.00  24.00   0.50    0.05    --  -46.95  19.00 -90.00   58
 32  \w    -24.00  27.00   0.50    0.05    --  -46.95  19.00-180.00  102
 33  \w   -102.00 -72.00   0.50    0.05    -- -102.00  77.00-180.00   60
 34  \w    -66.00  25.00   0.50    0.05    --  -46.95  81.00 -87.00  182
 35  \w    -68.00 -31.00   0.50    0.05    -- -102.00  61.00 120.00   74
 36  \w   -120.00 -34.00   0.50    0.05    --  -46.95 -19.00 120.00  172
 37  \w   -135.00 -89.00   0.50    0.05    -- -102.00 -30.00   0.00   92
 38  \w   -169.00-143.00   0.50    0.05    -- -102.00 -30.00   0.00   52
 39  \w   -162.00 -85.00   0.50    0.05    -- -102.00 -61.00-150.00  154
 40  \w   -170.00 -73.00   0.50    0.05    -- -102.00-125.00 -60.00  194
 41  \w    -95.00 -70.00   0.50    0.05    --  -46.95 -81.00 149.00   50
 42  \w   -161.00 -83.00   0.50    0.05    -- -102.00 -81.00 149.00  156
;
_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      0.0439073000
_diffrn_orient_matrix_UB_12      -0.0612171000
_diffrn_orient_matrix_UB_13      0.0521992000
_diffrn_orient_matrix_UB_21      0.0101453000
_diffrn_orient_matrix_UB_22      0.0712657000
_diffrn_orient_matrix_UB_23      0.0311235000
_diffrn_orient_matrix_UB_31      -0.1278338000
_diffrn_orient_matrix_UB_32      0.0138601000
_diffrn_orient_matrix_UB_33      0.0355577000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60961
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.402
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18931
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             1842
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.248
_refine_diff_density_min         -3.512
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         17572
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0571P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15289
_reflns_number_total             17572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707885
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1S1P1Si1O1
_shelx_estimated_absorpt_t_max   0.255
_shelx_estimated_absorpt_t_min   0.188
_diffrn_oxdiff_digest_frames
;
01b628db11b8503cc66477c19e9771650304102b710
;
_diffrn_oxdiff_digest_hkl
;
01ccac46c32d6f37f49fc5fb3f6b7bcc22d833
;
_reflns_odcompleteness_completeness 99.91
_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(C53A) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C53A) = Uanis(C53) = Uanis(C51A) = Uanis(C51) = Uanis(C52A) = Uanis(C52)
3. Others
 Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52A)=Sof(H52D)=Sof(H52E)=
 Sof(H52F)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(1)
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C35(H35), C36(H36), C44(H44), C46(H46), C47(H47), C55(H55),
 C56(H56), C57(H57), C58(H58), C59(H59), C2(H2), C4(H4), C5(H5), C13(H13),
 C15(H15), C16(H16), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C63(H63),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71)
4.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C51A(H51D,H51E,H51F),
 C52(H52A,H52B,H52C), C52A(H52D,H52E,H52F), C53(H53A,H53B,H53C), C53A(H53D,H53E,
 H53F), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), 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),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              9202
_shelx_hkl_checksum              8544
_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 5.496
_oxdiff_exptl_absorpt_empirical_full_min 0.438