Fragmentation, catenation, and direct functionalisation of white phosphorus by a uranium(IV)-silyl-phosphino-carbene complex.
Boronski, Josef T.; Seed, John A.; Wooles, Ashley J.; Liddle, Stephen T.; Chemical communications (Cambridge, England) 57 (2021) 5090–5093; doi:10.1039/d1cc01741a

data_7128208
_publ_section_title
;
 Fragmentation, catenation, and direct functionalisation of white
 phosphorus by a uranium(IV)-silyl-phosphino-carbene complex.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5090
_journal_page_last               5093
_journal_paper_doi               10.1039/d1cc01741a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C94 H114 N4 P10 Si6 U2, 2(C6 H6)'
_chemical_formula_sum            'C106 H126 N4 P10 Si6 U2'
_chemical_formula_weight         2410.40
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-03 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                113.276(2)
_cell_angle_beta                 106.9110(10)
_cell_angle_gamma                90.1380(10)
_cell_formula_units_Z            1
_cell_length_a                   13.8687(2)
_cell_length_b                   14.1074(3)
_cell_length_c                   15.5642(2)
_cell_measurement_reflns_used    24470
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0390
_cell_measurement_theta_min      3.2090
_cell_volume                     2652.39(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.948
_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     67.00 133.00   0.50    0.50    --   44.80  20.00-180.00  132
  2  \w     79.00 128.00   0.50    0.50    --   44.80  60.00 -30.00   98
  3  \w     68.00 123.00   0.50    0.50    --   44.80  60.00-120.00  110
  4  \w    -45.00 134.00   0.50    0.50    --   44.80  60.00 150.00  358
  5  \w     42.00  68.00   0.50    0.50    --   44.80  20.00 -60.00   52
  6  \w     85.00 110.00   0.50    0.50    --   44.80  20.00 -60.00   50
  7  \w     -8.00  19.00   0.50    0.50    --   44.80  20.00 -60.00   54
  8  \w    -45.00  40.00   0.50    0.50    --   44.80  60.00 -30.00  170
  9  \w    -45.00  28.00   0.50    0.50    --   44.80  60.00-120.00  146
 10  \w     20.00 197.00   0.50    0.50    --  108.20  50.00  30.00  354
 11  \w    125.00 164.00   0.50    0.50    --  108.20  50.00  90.00   78
 12  \w    103.00 132.00   0.50    0.50    --  108.20  50.00-150.00   58
 13  \w     37.00  63.00   0.50    0.50    --  108.20  50.00-120.00   52
 14  \w     75.00 152.00   0.50    0.50    --  108.20  50.00-120.00  154
 15  \w     20.00 189.00   0.50    0.50    --  108.20  50.00 -90.00  338
 16  \w    151.00 187.00   0.50    0.50    --  108.20  50.00 -30.00   72
 17  \w    143.00 170.00   0.50    0.50    --  108.20  50.00   0.00   54
 18  \w     22.00 143.00   0.50    0.50    --  108.20  50.00 -30.00  242
 19  \w    135.00 194.00   0.50    0.50    --  108.20  50.00 120.00  118
 20  \w     35.00 193.00   0.50    0.50    --  108.20  50.00  60.00  316
 21  \w     31.00 182.00   0.50    0.50    --  108.20   0.00 -60.00  302
 22  \w     85.00 198.00   0.50    0.50    --  108.20  50.00-180.00  226
 23  \w    124.00 174.00   0.50    0.50    --  108.20  50.00 -60.00  100
 24  \w     28.00  66.00   0.50    0.50    --  108.20  50.00-180.00   76
 25  \w    142.00 169.00   0.50    0.50    --  108.20  50.00-150.00   54
 26  \w     62.00 123.00   0.50    0.50    --  108.20  50.00 120.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1052960000
_diffrn_orient_matrix_UB_12      0.0503120000
_diffrn_orient_matrix_UB_13      0.0767514000
_diffrn_orient_matrix_UB_21      0.0491445000
_diffrn_orient_matrix_UB_22      -0.0387628000
_diffrn_orient_matrix_UB_23      -0.0826262000
_diffrn_orient_matrix_UB_31      -0.0149010000
_diffrn_orient_matrix_UB_32      0.1017580000
_diffrn_orient_matrix_UB_33      -0.0139969000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33479
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.370
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.968
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.273
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0413P)^2^+3.4972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10386
_reflns_number_total             10551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01741a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7128206--7128208.cif.'
_cod_database_code               7128208
_manchester_internal_diff_code   lstl231
_manchester_internal_stl_name    UJB32
_manchester_internal_coll_client JB
_manchester_internal_coll_date   29/01/2019
_manchester_internal_process_date 29/01/2019
_manchester_internal_process_user JB
_manchester_internal_solution_date 29/01/2019
_manchester_internal_solution_user JB
_manchester_internal_refinement_date 29/01/2019
_manchester_internal_refinement_user JB
_manchester_internal_validation_date 29/01/2019
_manchester_internal_validation_user JB
_manchester_internal_archive_date 31/01/2019
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C53 H63 U P5 Si3 N2'
_chemical_oxdiff_usercomment     jb
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.410
_reflns_odcompleteness_completeness 98.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              47882
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.362
_oxdiff_exptl_absorpt_empirical_full_min 0.719