Synthesis, bonding properties and ether activation reactivity of cyclobutadienyl-ligated hybrid uranocenes
Tsoureas, Nikolaos; Mansikkamäki, Akseli; Layfield, Richard A.; Chemical Science 12 (2021) 2948–2954; doi:10.1039/D0SC05199C

data_1560035
_publ_section_title
;
 Synthesis, bonding properties and ether activation reactivity of
 cyclobutadienyl-ligated hybrid uranocenes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2948
_journal_page_last               2954
_journal_paper_doi               10.1039/D0SC05199C
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C24 H44 Si4 U'
_chemical_formula_sum            'C24 H44 Si4 U'
_chemical_formula_weight         682.98
_chemical_name_common            3
_chemical_name_systematic        C24H44Si4U
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-11 deposited with the CCDC.	2021-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   31.8409(2)
_cell_length_b                   31.8409(2)
_cell_length_c                   11.02340(10)
_cell_measurement_reflns_used    14553
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.1220
_cell_measurement_theta_min      3.9110
_cell_volume                     11176.00(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (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                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -30.00  18.00   1.00    2.50    --    0.00  77.00-150.00   48
  2  \w    -30.00  18.00   1.00    2.50    --    0.00  77.00 -30.00   48
  3  \w    -30.00  18.00   1.00    2.50    --    0.00  77.00-180.00   48
  4  \w    -30.00  18.00   1.00    2.50    --    0.00  77.00 -90.00   48
  5  \w     76.00 126.00   1.00    5.00    --   54.50 125.00-180.00   50
  6  \w     76.00 126.00   1.00    5.00    --   54.50 125.00-150.00   50
  7  \w    -18.00 127.00   1.00    5.00    --   54.50   0.00-150.00  145
  8  \w      1.00  87.00   1.00    5.00    --   54.50-125.00  60.00   86
  9  \w     37.00  84.00   1.00   10.00    --  109.01-111.00  90.00   47
 10  \w     37.00  83.00   1.00   10.00    --  109.01-108.00 -26.00   46
 11  \w     86.00 176.00   1.00   10.00    --  109.01  64.00  60.00   90
 12  \w     84.00 178.00   1.00   10.00    --  109.01  38.00 150.00   94
 13  \w     37.00  84.00   1.00   10.00    --  109.01-111.00 150.00   47
 14  \w     87.00 178.00   1.00   10.00    --  109.01  50.00-150.00   91
 15  \w     39.00 139.00   1.00   10.00    --  109.01 -77.00 -30.00  100
 16  \w     37.00  84.00   1.00   10.00    --  109.01-111.00 120.00   47
 17  \w     37.00  84.00   1.00   10.00    --  109.01-111.00-150.00   47
 18  \w    -39.00  30.00   1.00    2.50    --    0.00 -77.00-120.00   69
 19  \w    -30.00  18.00   1.00    2.50    --    0.00  77.00  90.00   48
 20  \w   -123.00 -33.00   1.00    5.00    --  -54.50 -57.00   0.00   90
 21  \w     76.00 126.00   1.00    5.00    --   54.50 125.00 -90.00   50
 22  \w     33.00 123.00   1.00    5.00    --   54.50  57.00 -90.00   90
 23  \w     76.00 126.00   1.00    5.00    --   54.50 125.00 -30.00   50
 24  \w     80.00 178.00   1.00   10.00    --  109.01  77.00   0.00   98
 25  \w     37.00  64.00   1.00   10.00    --  109.01-111.00 -90.00   27
 26  \w     84.00 178.00   1.00   10.00    --  109.01  38.00 -60.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0434574000
_diffrn_orient_matrix_UB_12      0.0210474000
_diffrn_orient_matrix_UB_13      -0.0100842000
_diffrn_orient_matrix_UB_21      0.0179480000
_diffrn_orient_matrix_UB_22      -0.0403736000
_diffrn_orient_matrix_UB_23      -0.0569224000
_diffrn_orient_matrix_UB_31      -0.0114719000
_diffrn_orient_matrix_UB_32      0.0164094000
_diffrn_orient_matrix_UB_33      -0.1271491000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39719
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.327
_diffrn_reflns_theta_min         3.927
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.048
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       plate
_exptl_crystal_F_000             5376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-heptane'
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+24.8677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4857
_reflns_number_total             5417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05199c2.cif
_cod_data_source_block           C24H44Si4U
_cod_depositor_comments
'Adding full bibliography for 1560031--1560036.cif.'
_cod_original_cell_volume        11176.00(17)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1560035
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C24 H44 Si4 U '
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.080
_reflns_odcompleteness_completeness 99.96
_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:
 C5(H5), C12(H12), C6(H6), C11(H11), C7(H7), C10(H10), C9(H9), C8(H8)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C15(H15A,H15B,
 H15C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C16(H16A,H16B,H16C), C22(H22A,
 H22B,H22C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              77086
_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 1.628
_oxdiff_exptl_absorpt_empirical_full_min 0.420