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_7707884
_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         'C25 H51 Cl O P Si4 U'
_chemical_formula_sum            'C25 H51 Cl O P Si4 U'
_chemical_formula_weight         784.46
_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             2020-11-01
_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                90
_cell_angle_beta                 92.176(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5325(3)
_cell_length_b                   12.6083(3)
_cell_length_c                   30.1952(7)
_cell_measurement_reflns_used    11836
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.5930
_cell_measurement_theta_min      2.8940
_cell_volume                     4006.94(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_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    -82.00 -57.00   0.50    0.56    --  -47.70 134.00 -26.00   50
  2  \w   -116.00 -91.00   0.50    0.56    --  -47.70-135.00  86.00   50
  3  \w    -99.00 -74.00   0.50    0.56    --  -47.70-134.00 -94.00   50
  4  \w     24.00  93.00   0.50    0.56    --   47.70-134.00 -94.00  138
  5  \w     71.00  96.00   0.50    0.56    --   47.70 134.00 -26.00   50
  6  \w     37.00  62.00   0.50    0.56    --   47.70-135.00  86.00   50
  7  \w   -144.00 -95.00   0.50    1.00    -- -102.00-135.00  86.00   98
  8  \w   -101.00 -76.00   0.50    1.00    -- -102.00 135.00 152.00   50
  9  \w   -123.00 -77.00   0.50    1.00    -- -102.00 134.00 -26.00   92
 10  \w     54.00  79.00   0.50    1.00    --  104.75-135.00  86.00   50
 11  \w     99.00 124.00   0.50    1.00    --  104.75 135.00 152.00   50
 12  \w     54.00  79.00   0.50    1.00    --  104.75-134.00 -94.00   50
 13  \w   -119.00 -73.00   0.50    0.56    --  -47.70-125.00-150.00   92
 14  \w    -24.00  58.00   0.50    0.56    --   47.70 -37.00 -60.00  164
 15  \w     36.00  75.00   0.50    0.56    --   47.70  37.00  90.00   78
 16  \w     81.00 118.00   0.50    0.56    --   47.70  37.00  90.00   74
 17  \w   -115.00 -52.00   0.50    1.00    -- -102.00 125.00-150.00  126
 18  \w   -175.00 -88.00   0.50    1.00    -- -102.00 -15.00  60.00  174
 19  \w     47.00 108.00   0.50    1.00    --  104.75 -94.00  60.00  122
 20  \w     64.00  99.00   0.50    1.00    --  104.75 -94.00-180.00   70
 21  \w    121.00 176.00   0.50    1.00    --  104.75  45.00 -30.00  110
 22  \w     41.00 114.00   0.50    1.00    --  104.75 -45.00-150.00  146
 23  \w     34.00 118.00   0.50    1.00    --  104.75 -30.00  30.00  168
;
_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      0.1252483000
_diffrn_orient_matrix_UB_12      0.0611450000
_diffrn_orient_matrix_UB_13      0.0082130000
_diffrn_orient_matrix_UB_21      0.0722306000
_diffrn_orient_matrix_UB_22      -0.1057743000
_diffrn_orient_matrix_UB_23      0.0054786000
_diffrn_orient_matrix_UB_31      0.0228533000
_diffrn_orient_matrix_UB_32      -0.0012261000
_diffrn_orient_matrix_UB_33      -0.0500922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28157
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.707
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+12.6932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7202
_reflns_number_total             8002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707884
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1Si1U1P1O1
_shelx_estimated_absorpt_t_max   0.343
_shelx_estimated_absorpt_t_min   0.234
_diffrn_oxdiff_digest_frames
;
019e4d2a0031bc14aaa9ee276727eec02b021024ecb
;
_diffrn_oxdiff_digest_hkl
;
01e61a82261f21aed5794364d0c3a121ae88ca
;
_reflns_odcompleteness_completeness 99.67
_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(C17A) = Uanis(C17B) = Uanis(C18A) = Uanis(C18B) = Uanis(C19A) =
Uanis(C19B)
3. Others
 Fixed Sof: C17A(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18A(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C19A(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C17B(0.5)
 H17D(0.5) H17E(0.5) H17F(0.5) C18B(0.5) H18D(0.5) H18E(0.5) H18F(0.5)
 C19B(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20A(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22A(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C20B(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C21B(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5)
 Si3A(0.5) Si4A(0.5) Si3B(0.5) Si4B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16)
4.b 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), C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C),
 C19A(H19A,H19B,H19C), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F), C19B(H19D,
 H19E,H19F), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C),
 C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              84337
_shelx_hkl_checksum              67570
_shelx_fab_checksum              7865
_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 3.121
_oxdiff_exptl_absorpt_empirical_full_min 0.690