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_7707886
_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         'C34 H62 N O P Si4 U'
_chemical_formula_sum            'C34 H62 N O P Si4 U'
_chemical_formula_weight         882.20
_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             2019-03-27
_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                 93.183(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8316(3)
_cell_length_b                   20.3339(4)
_cell_length_c                   15.0866(3)
_cell_measurement_reflns_used    5307
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.6090
_cell_measurement_theta_min      3.6430
_cell_volume                     4236.57(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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   -110.00 -13.00   1.00    3.03    --  -39.49 -57.00 120.00   97
  2  \w    -47.00  35.00   1.00    3.03    --  -39.49  37.00 -90.00   82
  3  \w   -124.00 -85.00   1.00    3.03    --  -39.49 178.00 150.00   39
  4  \w    150.00 177.00   1.00    3.00    --  104.69 125.00 150.00   27
  5  \w     83.00 110.00   1.00    3.00    --  104.69-125.00-180.00   27
  6  \w     29.00 133.00   1.00    3.00    --  104.69 -30.00  30.00  104
  7  \w     23.00 107.00   1.00    3.00    --  104.69 -94.00 -60.00   84
  8  \w     79.00 170.00   1.00    3.00    --  104.69  45.00-150.00   91
  9  \w     47.00 117.00   1.00    3.00    --  104.69 -45.00 -60.00   70
 10  \w     75.00 133.00   1.00    3.00    --  104.69 -30.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0441222000
_diffrn_orient_matrix_UB_12      -0.0148973000
_diffrn_orient_matrix_UB_13      0.0938429000
_diffrn_orient_matrix_UB_21      -0.1005933000
_diffrn_orient_matrix_UB_22      0.0077470000
_diffrn_orient_matrix_UB_23      0.0379145000
_diffrn_orient_matrix_UB_31      -0.0192582000
_diffrn_orient_matrix_UB_32      -0.0738619000
_diffrn_orient_matrix_UB_33      -0.0149852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.857
_diffrn_reflns_theta_min         3.652
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.639
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6471
_reflns_number_total             8116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound16
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707886
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1P1U1Si1
_shelx_estimated_absorpt_t_max   0.370
_shelx_estimated_absorpt_t_min   0.370
_reflns_odcompleteness_completeness 99.90
_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), C28(H28), C30(H30)
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), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              7939
_shelx_hkl_checksum              14400
_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 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.826