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_7707890
_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      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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-01
_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                 92.6930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.66930(10)
_cell_length_b                   11.4991(2)
_cell_length_c                   39.0487(4)
_cell_measurement_reflns_used    25902
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3850
_cell_measurement_theta_min      3.8750
_cell_volume                     5234.02(11)
_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 0.994
_diffrn_measured_fraction_theta_max 0.950
_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     68.00 158.00   0.50    0.32    --  104.75 136.00  -5.00  180
  2  \w    102.00 128.00   0.50    0.32    --  104.75 133.00 176.00   52
  3  \w     95.00 177.00   0.50    0.32    --  104.75  15.00   0.00  164
  4  \w    -24.00  29.00   0.50    0.20    --  -46.95  19.00 -90.00  106
  5  \w    -89.00 -63.00   0.50    0.32    -- -102.00  77.00-180.00   52
  6  \w    -19.00   7.00   0.50    0.20    --  -46.95  19.00 -60.00   52
  7  \w    -68.00 -34.00   0.50    0.32    -- -102.00  61.00  30.00   68
  8  \w    -66.00 -29.00   0.50    0.32    -- -102.00  61.00 -30.00   74
  9  \w    -69.00 -44.00   0.50    0.32    -- -102.00  61.00 -60.00   50
 10  \w   -175.00-111.00   0.50    0.32    -- -102.00 -15.00-180.00  128
 11  \w    -97.00 -70.00   0.50    0.20    --  -46.95-133.00 107.00   54
 12  \w   -107.00 -75.00   0.50    0.20    --  -46.95-125.00  60.00   64
 13  \w   -111.00 -85.00   0.50    0.20    --  -46.95-136.00 -69.00   52
 14  \w   -112.00 -86.00   0.50    0.20    --  -46.95-125.00-180.00   52
 15  \w    -82.00 -56.00   0.50    0.20    --  -46.95 133.00 176.00   52
 16  \w   -120.00 -95.00   0.50    0.32    -- -102.00-136.00 -69.00   50
 17  \w   -169.00-144.00   0.50    0.32    -- -102.00 -94.00-150.00   50
 18  \w   -145.00-120.00   0.50    0.32    -- -102.00-133.00 107.00   50
 19  \w    -27.00  27.00   0.50    0.20    --   46.95 -19.00-120.00  108
 20  \w     32.00  65.00   0.50    0.32    --  104.75 -61.00  60.00   66
 21  \w     32.00  58.00   0.50    0.32    --  104.75 -61.00 120.00   52
 22  \w     38.00  72.00   0.50    0.32    --  104.75 -61.00 150.00   68
 23  \w     84.00 109.00   0.50    0.32    --  104.75 -94.00 -60.00   50
 24  \w     39.00  91.00   0.50    0.20    --   46.95-133.00 107.00  104
 25  \w     92.00 122.00   0.50    0.32    --  104.75-136.00 -69.00   60
 26  \w     57.00 121.00   0.50    0.32    --  104.75-133.00 107.00  128
 27  \w     45.00 107.00   0.50    0.32    --  104.75 -94.00 120.00  124
;
_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      0.0812656000
_diffrn_orient_matrix_UB_12      -0.1056256000
_diffrn_orient_matrix_UB_13      0.0004126000
_diffrn_orient_matrix_UB_21      0.1042294000
_diffrn_orient_matrix_UB_22      0.0824180000
_diffrn_orient_matrix_UB_23      0.0013535000
_diffrn_orient_matrix_UB_31      0.0017146000
_diffrn_orient_matrix_UB_32      -0.0017168000
_diffrn_orient_matrix_UB_33      0.0394614000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36497
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.582
_diffrn_reflns_theta_min         3.907
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.424
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64098
_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    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         10471
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+27.4536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9425
_reflns_number_total             10471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound14
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707890
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1S1U1Si1
_shelx_estimated_absorpt_t_max   0.422
_shelx_estimated_absorpt_t_min   0.304
_diffrn_oxdiff_digest_frames
;
010f37448ded9aa93c85ec79dcb2cc063602110cb37
;
_diffrn_oxdiff_digest_hkl
;
01136d5725848a1a2760a19b20e9ec57a39766
;
_reflns_odcompleteness_completeness 99.77
_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(C4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C41) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C36(H36), C39(H39), C42(H42)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C32(H32), C34(H34)
3.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)
;
_shelx_res_checksum              21605
_shelx_hkl_checksum              4387
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.528