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_7707891
_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         'C28 H60 O2 P2 Si4 U, C11 H21 Si2, 3(C6 H6)'
_chemical_formula_sum            'C57 H99 O2 P2 Si6 U'
_chemical_formula_weight         1284.87
_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             2020-12-08
_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                 101.9840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.13300(10)
_cell_length_b                   25.2117(2)
_cell_length_c                   22.3666(2)
_cell_measurement_reflns_used    28457
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      3.4770
_cell_volume                     6692.69(10)
_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 0.959
_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     51.00  76.00   0.50    0.07    --   46.95  58.00-115.00   50
  2  \w     90.00 174.00   0.50    0.27    --  104.75  58.00-115.00  168
  3  \w     92.00 177.00   0.50    0.27    --  104.75  45.00-180.00  170
  4  \w     68.00 108.00   0.50    0.27    --  104.75 -77.00 -90.00   80
  5  \w     43.00  72.00   0.50    0.27    --  104.75 -61.00-120.00   58
  6  \w     32.00  71.00   0.50    0.27    --  104.75 -61.00 -60.00   78
  7  \w     33.00  68.00   0.50    0.27    --  104.75 -61.00 -90.00   70
  8  \w     77.00 102.00   0.50    0.27    --  104.75 -94.00  90.00   50
  9  \w     33.00  69.00   0.50    0.27    --  104.75 -58.00 103.00   72
 10  \w     43.00  69.00   0.50    0.27    --  104.75 -94.00  90.00   52
 11  \w    -23.00  56.00   0.50    0.07    --   46.95 -58.00 103.00  158
 12  \w    117.00 161.00   0.50    0.27    --  104.75  61.00 150.00   88
 13  \w    -60.00  26.00   0.50    0.07    --  -46.95  58.00-115.00  172
 14  \w    -57.00 -30.00   0.50    0.27    -- -102.00  58.00-115.00   54
 15  \w    -97.00 -31.00   0.50    0.27    -- -102.00  77.00-150.00  132
 16  \w    -61.00 -35.00   0.50    0.27    -- -102.00  61.00  90.00   52
 17  \w   -116.00 -44.00   0.50    0.07    --  -46.95 -58.00 103.00  144
 18  \w   -117.00 -71.00   0.50    0.07    --  -46.95-125.00-120.00   92
 19  \w   -117.00 -87.00   0.50    0.07    --  -46.95-125.00-150.00   60
 20  \w   -170.00 -93.00   0.50    0.27    -- -102.00 -45.00   0.00  154
 21  \w   -171.00-146.00   0.50    0.27    -- -102.00 -58.00 103.00   50
 22  \w   -170.00-105.00   0.50    0.27    -- -102.00 -30.00 -30.00  130
;
_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      -0.0420668000
_diffrn_orient_matrix_UB_12      -0.0421621000
_diffrn_orient_matrix_UB_13      0.0398043000
_diffrn_orient_matrix_UB_21      -0.1196811000
_diffrn_orient_matrix_UB_22      0.0046691000
_diffrn_orient_matrix_UB_23      -0.0396606000
_diffrn_orient_matrix_UB_31      0.0276521000
_diffrn_orient_matrix_UB_32      -0.0439740000
_diffrn_orient_matrix_UB_33      -0.0424149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47682
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.549
_diffrn_reflns_theta_min         3.506
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62788
_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    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.575
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.000048(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         13506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+4.0406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11624
_reflns_number_total             13506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707891
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1Si1U1
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.481
_diffrn_oxdiff_digest_frames
;
01fd877b98525a5af043507b202ca3a61800050a1df
;
_diffrn_oxdiff_digest_hkl
;
018d028ecdb45aa017ac439c232a7e23044e2b
;
_reflns_odcompleteness_completeness 99.81
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C30(H30), C31(H31),
 C33(H33), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57)
2.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), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              97749
_shelx_hkl_checksum              35159
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.834