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_7707887
_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         'C48 H78 N2 O P2 Si4 U, C6 H6'
_chemical_formula_sum            'C54 H84 N2 O P2 Si4 U'
_chemical_formula_weight         1189.56
_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             2020-12-08
_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                90.1150(10)
_cell_angle_beta                 106.883(2)
_cell_angle_gamma                103.328(2)
_cell_formula_units_Z            4
_cell_length_a                   15.2105(4)
_cell_length_b                   18.7372(4)
_cell_length_c                   22.0699(2)
_cell_measurement_reflns_used    26371
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2740
_cell_measurement_theta_min      3.6600
_cell_volume                     5840.7(2)
_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 0.997
_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     36.00 112.00   0.50    0.62    --   46.95  21.00  82.00  152
  2  \w     92.00 177.00   0.50    0.80    --  104.75  30.00  90.00  170
  3  \w     94.00 167.00   0.50    0.80    --  104.75  21.00  82.00  146
  4  \w     94.00 178.00   0.50    0.80    --  104.75  15.00   0.00  168
  5  \w    125.00 169.00   0.50    0.80    --  104.75  30.00-180.00   88
  6  \w     93.00 118.00   0.50    0.80    --  104.75  30.00-180.00   50
  7  \w    -23.00   2.00   0.50    0.62    --  -46.95  21.00  82.00   50
  8  \w    -59.00 -32.00   0.50    0.80    -- -102.00  61.00 150.00   54
  9  \w    -68.00 -29.00   0.50    0.80    -- -102.00  61.00 -60.00   78
 10  \w    -40.00   3.00   0.50    0.62    --  -46.95  37.00  90.00   86
 11  \w    -20.00  28.00   0.50    0.62    --   46.95 -19.00  60.00   96
 12  \w     -3.00  27.00   0.50    0.62    --   46.95 -19.00 120.00   60
 13  \w    -27.00  -1.00   0.50    0.62    --   46.95 -19.00 150.00   52
 14  \w    -10.00  29.00   0.50    0.62    --   46.95 -21.00 -84.00   78
 15  \w    -23.00  62.00   0.50    0.62    --   46.95 -57.00-180.00  170
 16  \w     34.00 104.00   0.50    0.80    --  104.75 -94.00 -60.00  140
 17  \w     32.00  96.00   0.50    0.80    --  104.75-125.00   0.00  128
 18  \w     38.00  64.00   0.50    0.80    --  104.75-125.00 -60.00   52
 19  \w     67.00  94.00   0.50    0.80    --  104.75 -94.00 -90.00   54
 20  \w     65.00 116.00   0.50    0.80    --  104.75-125.00 -60.00  102
 21  \w     35.00  98.00   0.50    0.80    --  104.75 -94.00   0.00  126
 22  \w     76.00 103.00   0.50    0.80    --  104.75 -94.00 120.00   54
 23  \w     16.00  93.00   0.50    0.62    --   46.95-125.00 -30.00  154
 24  \w     40.00 105.00   0.50    0.80    --  104.75 -94.00-180.00  130
 25  \w     36.00 107.00   0.50    0.80    --  104.75 -77.00-180.00  142
 26  \w     36.00  61.00   0.50    0.80    --  104.75 -61.00 -60.00   50
 27  \w     36.00 104.00   0.50    0.80    --  104.75 -77.00   0.00  136
 28  \w     34.00  81.00   0.50    0.80    --  104.75 -77.00  90.00   94
 29  \w     33.00  58.00   0.50    0.80    --  104.75 -61.00  60.00   50
 30  \w     36.00  67.00   0.50    0.80    --  104.75 -61.00   0.00   62
 31  \w     34.00  67.00   0.50    0.80    --  104.75 -61.00-180.00   66
 32  \w   -111.00 -71.00   0.50    0.62    --  -46.95-125.00   0.00   80
 33  \w   -103.00 -77.00   0.50    0.80    -- -102.00-125.00   0.00   52
 34  \w   -166.00-122.00   0.50    0.80    -- -102.00-125.00   0.00   88
 35  \w   -153.00 -85.00   0.50    0.80    -- -102.00 -94.00 -90.00  136
 36  \w   -130.00 -94.00   0.50    0.80    -- -102.00 -45.00-120.00   72
 37  \w   -137.00-111.00   0.50    0.80    -- -102.00 -21.00 -84.00   52
 38  \w   -114.00 -34.00   0.50    0.62    --  -46.95 -21.00 -84.00  160
 39  \w   -165.00 -89.00   0.50    0.80    -- -102.00 -30.00 150.00  152
 40  \w   -117.00 -88.00   0.50    0.80    -- -102.00 125.00   0.00   58
 41  \w   -117.00 -70.00   0.50    0.80    -- -102.00 125.00  60.00   94
 42  \w    -71.00 -30.00   0.50    0.80    -- -102.00 125.00 120.00   82
 43  \w   -117.00 -74.00   0.50    0.80    -- -102.00 125.00 120.00   86
 44  \w    -57.00 -30.00   0.50    0.80    -- -102.00 125.00-180.00   54
 45  \w   -117.00 -91.00   0.50    0.80    -- -102.00 125.00-180.00   52
;
_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      -0.0949664000
_diffrn_orient_matrix_UB_12      0.0226126000
_diffrn_orient_matrix_UB_13      -0.0198416000
_diffrn_orient_matrix_UB_21      -0.0531819000
_diffrn_orient_matrix_UB_22      -0.0806375000
_diffrn_orient_matrix_UB_23      -0.0000384000
_diffrn_orient_matrix_UB_31      0.0070849000
_diffrn_orient_matrix_UB_32      0.0128477000
_diffrn_orient_matrix_UB_33      0.0704065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23549
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.545
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42757
_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    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         7.224
_refine_diff_density_min         -3.169
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         23549
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0914P)^2^+47.2795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20457
_reflns_number_total             23549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound13
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707887
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1Si1P1U1
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.453
_diffrn_oxdiff_digest_frames
;
01e89900c0c2f49c2b4590e7076968f90004256f949
;
_diffrn_oxdiff_digest_hkl
;
0170babb066adac4363617eef194daca8f427a
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.767(2)
 0.233(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C79) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C37(H37), C40(H40), C43(H43), C85(H85), C88(H88), C91(H91)
4.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C94(H94A,H94B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C25(H25),
 C26(H26), C27(H27), C28(H28), C33(H33), C35(H35), N3(H3), C50(H50), C52(H52),
 C53(H53), C61(H61), C63(H63), C64(H64), C73(H73), C74(H74), C75(H75), C76(H76),
  C81(H81), C83(H83), C97(H97), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108)
4.d 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), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C86(H86A,H86B,H86C), C87(H87A,H87B,
 H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C93(H93A,
 H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              60868
_shelx_hkl_checksum              35868
_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 2.103
_oxdiff_exptl_absorpt_empirical_full_min 0.720