Uranium(iv) cyclobutadienyl sandwich compounds: synthesis, structure and chemical bonding.
Tsoureas, Nikolaos; Mansikkamäki, Akseli; Layfield, Richard A.; Chemical communications (Cambridge, England) 56 (2020) 944–947; doi:10.1039/c9cc09018e

data_7125701
_publ_section_title
;
 Uranium(iv) cyclobutadienyl sandwich compounds: synthesis, structure and
 chemical bonding.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              944
_journal_page_last               947
_journal_paper_doi               10.1039/c9cc09018e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C24 H64 B3 K O2 Si4 U'
_chemical_formula_sum            'C24 H64 B3 K O2 Si4 U'
_chemical_formula_weight         794.57
_chemical_name_systematic        2
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_audit_creation_date             2019-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.572(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5143(5)
_cell_length_b                   15.8092(8)
_cell_length_c                   16.0534(5)
_cell_measurement_reflns_used    5660
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.3540
_cell_measurement_theta_min      3.9760
_cell_volume                     3903.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_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 n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -71.00  88.00   0.50    1.00    --    0.00  10.00-120.00  318
  2  \w    -19.00   6.00   0.50    1.00    --    5.00  36.00 -89.00   50
  3  \w   -106.00 -73.00   0.50    4.00    --  -90.00  36.00 -89.00   66
  4  \w   -175.00-128.00   0.50    4.00    --  -90.00  36.00 -89.00   94
  5  \w    -68.00 -22.00   0.50    4.00    --  -90.00  39.00  30.00   92
  6  \w   -179.00-107.00   0.50    4.00    --  -90.00  30.00   0.00  144
  7  \w    -88.00  -2.00   0.50    4.00    --  -90.00  30.00   0.00  172
  8  \w   -121.00  -3.00   0.50    4.00    --  -90.00  39.00-180.00  236
  9  \w   -178.00-148.00   0.50    4.00    --  -90.00  10.00-180.00   60
 10  \w   -178.00  -2.00   0.50    4.00    --  -90.00  49.00 150.00  352
 11  \w   -106.00 -80.00   0.50    4.00    --  -90.00  10.00-180.00   52
 12  \w    -61.00  -2.00   0.50    4.00    --  -90.00  10.00-180.00  118
 13  \w   -178.00-149.00   0.50    4.00    --  -90.00  49.00 120.00   58
 14  \w   -105.00 -64.00   0.50    4.00    --  -90.00  49.00 120.00   82
 15  \w   -111.00 -85.00   0.50    4.00    --  -90.00   0.00-180.00   52
 16  \w   -179.00-102.00   0.50    4.00    --  -90.00  39.00  30.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005830000
_diffrn_orient_matrix_UB_12      0.0570368000
_diffrn_orient_matrix_UB_13      -0.0779094000
_diffrn_orient_matrix_UB_21      -0.1001817000
_diffrn_orient_matrix_UB_22      -0.0000172000
_diffrn_orient_matrix_UB_23      -0.0120411000
_diffrn_orient_matrix_UB_31      0.0003850000
_diffrn_orient_matrix_UB_32      0.0789825000
_diffrn_orient_matrix_UB_33      0.0561992000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14621
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.359
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
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    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.600
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         14621
_refine_ls_number_restraints     887
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.0991
_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^)+(0.1969P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2690
_refine_ls_wR_factor_ref         0.3009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7876
_reflns_number_total             14621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09018e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7125700--7125702.cif.'
_cod_database_code               7125701
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C96 H228 B12 K4 O8 Si16 U4 '
_chemical_oxdiff_usercomment     NTL12p63
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5120(19)
 0.4880(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 H16B-H5A
 -1.8 with sigma of 0.02
 C17-C18 \\sim C18-C19 \\sim C19-C20
 with sigma of 0.02
 O2-C17 \\sim O2-C20
 with sigma of 0.02
 O2-C18 \\sim O2-C19
 with sigma of 0.04
 C18-C20 \\sim C17-C19
 with sigma of 0.04
 C0AA-C1AA \\sim C1AA-C7AA \\sim C7AA-C8AA
 with sigma of 0.02
 O1-C0AA \\sim O1-C8AA
 with sigma of 0.02
 O1-C1AA \\sim O1-C7AA
 with sigma of 0.04
 C1AA-C8AA \\sim C0AA-C7AA
 with sigma of 0.04
 K1-O1 \\sim K1-O1A
 with sigma of 0.02
 O1-C0AA \\sim O1A-C1A
 with sigma of 0.02
 O1-C8AA \\sim O1A-C9A
 with sigma of 0.02
 C0AA-C1AA \\sim C1A-C2A
 with sigma of 0.02
 C1AA-C7AA \\sim C2A-C7A
 with sigma of 0.02
 C7AA-C8AA \\sim C7A-C9A
 with sigma of 0.02
 K1-C0AA \\sim K1-C1A
 with sigma of 0.04
 K1-C8AA \\sim K1-C9A
 with sigma of 0.04
 O1-C1AA \\sim O1A-C2A
 with sigma of 0.04
 O1-C7AA \\sim O1A-C7A
 with sigma of 0.04
 C0AA-C7AA \\sim C1A-C7A
 with sigma of 0.04
 C0AA-C8AA \\sim C1A-C9A
 with sigma of 0.04
 C1AA-C8AA \\sim C2A-C9A
 with sigma of 0.04
 C4-C15 \\sim C4-C14 \\sim C4-C16 \\sim C15-C14 \\sim C15-C16 \\sim C14-C16
 with sigma of 0.04
 Si3-C4 \\sim Si3-C15 \\sim Si3-C14 \\sim Si3-C16
 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(O1A)=Sof(C1A)=Sof(H1AC)=Sof(H1AD)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C7A)=Sof(H7AC)=Sof(H7AD)=1-FVAR(1)
 Sof(O1)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(C7AA)=
 Sof(H7AA)=Sof(H7AB)=Sof(C8AA)=Sof(H8AA)=Sof(H8AB)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C0AA(H0AA,
 H0AB), C1AA(H1AA,H1AB), C7AA(H7AA,H7AB), C8AA(H8AA,H8AB), C9A(H9AA,H9AB),
 C1A(H1AC,H1AD), C2A(H2AA,H2AB), C7A(H7AC,H7AD)
8.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C5(H5A,H5B,H5C)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C7(H7A,H7B,
 H7C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              90384
_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 4.580
_oxdiff_exptl_absorpt_empirical_full_min 0.185
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 15.7246\% 
 around [0.96 -0.13 -0.23] (reciprocal) or [0.99 -0.13 -0.09] (direct)
;