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_7707888
_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 H85 N O P2 Si4 U'
_chemical_formula_sum            'C47 H85 N O P2 Si4 U'
_chemical_formula_weight         1092.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-02-07
_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                 100.4882(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0980(4)
_cell_length_b                   11.5929(2)
_cell_length_c                   21.5294(4)
_cell_measurement_reflns_used    23986
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1840
_cell_measurement_theta_min      4.0890
_cell_volume                     5423.25(17)
_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    'olex2.solve (Bourhis et al., 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 0.950
_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     67.00  92.00   0.50    0.09    --   46.95  56.00 121.00   50
  2  \w     94.00 177.00   0.50    0.20    --  104.75  56.00 121.00  166
  3  \w    120.00 175.00   0.50    0.20    --  104.75  30.00-120.00  110
  4  \w     96.00 154.00   0.50    0.20    --  104.75  45.00-180.00  116
  5  \w    -18.00  26.00   0.50    0.09    --  -46.95  56.00 121.00   88
  6  \w   -103.00 -56.00   0.50    0.20    -- -102.00  77.00 -30.00   94
  7  \w    -69.00 -44.00   0.50    0.20    -- -102.00  61.00 -60.00   50
  8  \w    -69.00 -34.00   0.50    0.20    -- -102.00  61.00 -90.00   70
  9  \w    -68.00 -29.00   0.50    0.20    -- -102.00  61.00-180.00   78
 10  \w    -69.00 -32.00   0.50    0.20    -- -102.00  61.00-120.00   74
 11  \w    -62.00 -29.00   0.50    0.20    -- -102.00  56.00 121.00   66
 12  \w    -61.00 -35.00   0.50    0.09    --  -46.95  56.00 121.00   52
 13  \w   -173.00-144.00   0.50    0.20    -- -102.00 -56.00 -21.00   58
 14  \w   -175.00-143.00   0.50    0.20    -- -102.00 -15.00-120.00   64
 15  \w   -129.00-103.00   0.50    0.20    -- -102.00 -15.00-120.00   52
 16  \w   -118.00 -35.00   0.50    0.09    --  -46.95 -56.00 -21.00  166
 17  \w   -155.00 -96.00   0.50    0.20    -- -102.00 -45.00  60.00  118
 18  \w   -118.00 -72.00   0.50    0.09    --  -46.95-125.00  90.00   92
 19  \w   -118.00 -72.00   0.50    0.09    --  -46.95-125.00 -30.00   92
 20  \w    -20.00  47.00   0.50    0.09    --   46.95 -56.00 -21.00  134
 21  \w    -15.00  25.00   0.50    0.09    --   46.95 -19.00-180.00   80
 22  \w     35.00  71.00   0.50    0.20    --  104.75 -61.00-120.00   72
 23  \w     32.00  66.00   0.50    0.20    --  104.75 -56.00 -21.00   68
 24  \w     45.00  70.00   0.50    0.20    --  104.75 -61.00   0.00   50
 25  \w     46.00 102.00   0.50    0.20    --  104.75 -94.00 -60.00  112
 26  \w     84.00 109.00   0.50    0.20    --  104.75 -94.00  60.00   50
 27  \w     46.00  72.00   0.50    0.20    --  104.75 -94.00  60.00   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      -0.0432199000
_diffrn_orient_matrix_UB_12      0.0571754000
_diffrn_orient_matrix_UB_13      0.0396027000
_diffrn_orient_matrix_UB_21      -0.0312787000
_diffrn_orient_matrix_UB_22      0.0684193000
_diffrn_orient_matrix_UB_23      -0.0584989000
_diffrn_orient_matrix_UB_31      -0.0466542000
_diffrn_orient_matrix_UB_32      -0.0985367000
_diffrn_orient_matrix_UB_33      -0.0175681000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10819
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.729
_diffrn_reflns_theta_min         4.069
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26976
_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    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.275
_refine_diff_density_min         -2.011
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         10819
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+91.0861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9844
_reflns_number_total             10819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound15
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_original_cell_volume        5423.24(18)
_cod_database_code               7707888
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1Si1
_shelx_estimated_absorpt_t_max   0.314
_shelx_estimated_absorpt_t_min   0.238
_diffrn_oxdiff_digest_frames
;
01fff46e9c14aea7b91e88e66247f304b6022744f6c
;
_diffrn_oxdiff_digest_hkl
;
01c18a59019a6167b780e3f83726accbf8b945
;
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.845(2)
 0.155(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C23(H23), C36(H36), C39(H39), C42(H42)
4.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C32(H32), C34(H34)
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), 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              23922
_shelx_hkl_checksum              35146
_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 2.657
_oxdiff_exptl_absorpt_empirical_full_min 0.517