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_7125700
_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         'C16 H48 B3 Si4 U, C16 H31 Na O8'
_chemical_formula_sum            'C32 H79 B3 Na O8 Si4 U'
_chemical_formula_weight         997.76
_chemical_name_systematic        1
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   mixed
_audit_creation_date             2019-07-09
_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                 108.8680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3922(2)
_cell_length_b                   14.5028(2)
_cell_length_c                   20.3353(2)
_cell_measurement_reflns_used    11683
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.1830
_cell_measurement_theta_min      4.0580
_cell_volume                     4853.67(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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)'
_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 0.998
_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    -32.00  56.00   1.00   12.50    --   36.75 -38.00 120.00   88
  2  \w    -31.00  63.00   1.00   12.50    --   36.75 -77.00  30.00   94
  3  \w     35.00 109.00   1.00   12.50    --   36.75 178.00  60.00   74
  4  \w     36.00 145.00   1.00   25.00    --  107.00 -15.00 -90.00  109
  5  \w     38.00  84.00   1.00   25.00    --  107.00 -95.00 -60.00   46
  6  \w     39.00 124.00   1.00   25.00    --  107.00 -45.00  90.00   85
  7  \w     40.00 125.00   1.00   25.00    --  107.00 -61.00  30.00   85
  8  \w     39.00 124.00   1.00   25.00    --  107.00 -45.00 -90.00   85
  9  \w     36.00 145.00   1.00   25.00    --  107.00 -15.00  60.00  109
 10  \w     86.00 177.00   1.00   25.00    --  107.00  30.00 -60.00   91
 11  \w     10.00 104.00   1.00   12.50    --   36.75  77.00-120.00   94
 12  \w     10.00 104.00   1.00   12.50    --   36.75  77.00  90.00   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      -0.0284733000
_diffrn_orient_matrix_UB_12      0.0483643000
_diffrn_orient_matrix_UB_13      0.0555321000
_diffrn_orient_matrix_UB_21      0.0667315000
_diffrn_orient_matrix_UB_22      -0.0503447000
_diffrn_orient_matrix_UB_23      0.0576814000
_diffrn_orient_matrix_UB_31      0.0590990000
_diffrn_orient_matrix_UB_32      0.0800062000
_diffrn_orient_matrix_UB_33      0.0026085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23145
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         3.817
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light bronze'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       plate
_exptl_crystal_F_000             2036
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Dioxane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.001
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9180
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0529P)^2^+6.5672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8191
_reflns_number_total             9180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09018e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7125700--7125702.cif.'
_cod_database_code               7125700
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'B3 C34 Na1 O8 Si4 U1 H32 '
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.222
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C18A-C17A
 1.55 with sigma of 0.02
 C19A-C20A
 1.55 with sigma of 0.02
 C22A-C21A
 1.55 with sigma of 0.02
 C24A-C23A
 1.55 with sigma of 0.02
 O7-C17A
 1.42 with sigma of 0.02
 O7-C24A
 1.42 with sigma of 0.02
 O8-C23A
 1.42 with sigma of 0.02
 O8-C22A
 1.42 with sigma of 0.02
 O5-C21A
 1.42 with sigma of 0.02
 O5-C20A
 1.42 with sigma of 0.02
 O6-C18A
 1.42 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 C18A-C17A \\sim C18B-C17B
 with sigma of 0.02
 C19A-C20A \\sim C19B-C20B
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 O7-C17A \\sim O7-C17B
 with sigma of 0.02
 O7-C24A \\sim O7-C24B
 with sigma of 0.02
 O8-C23A \\sim O8-C23B
 with sigma of 0.02
 O8-C22A \\sim O8-C22B
 with sigma of 0.02
 O6-C18A \\sim O6-C18B
 with sigma of 0.02
 C19B-C18B \\sim C19A-C18A
 with sigma of 0.02
 O5-C21A \\sim O5-C21B
 with sigma of 0.02
 C21A-C22A \\sim C21B-C22B
 with sigma of 0.02
 C21A-C20A \\sim C21B-C20B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20A) = Uanis(C20B)
Uanis(C19A) = Uanis(C18A)
Uanis(C19B) = Uanis(C18B)
Uanis(C18A) = Uanis(C17A)
Uanis(C18B) = Uanis(C17B)
Uanis(C18A) = Uanis(C24A)
Uanis(C18B) = Uanis(C24B)
Uanis(C23B) = Uanis(C23A)
Uanis(C19A) = Uanis(C20A)
Uanis(C19A) = Uanis(C22A)
Uanis(C19B) = Uanis(C22B)
Uanis(C21B) = Uanis(C21A)
4. Others
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=
 Sof(H21C)=Sof(H21D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C23B)=Sof(H23C)=
 Sof(H23D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=
 Sof(C24B)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=
 Sof(H21A)=Sof(H21B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=
 Sof(C24A)=Sof(H24A)=Sof(H24B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C25(H25A,H25B), C30(H30A,
 H30B), C31(H31A,H31B), C26(H26A,H26B), C22A(H22A,H22B), C20A(H20A,H20B),
 C21A(H21A,H21B), C19A(H19A,H19B), C23A(H23A,H23B), C18A(H18A,H18B), C17A(H17A,
 H17B), C24A(H24A,H24B), C22B(H22C,H22D), C20B(H20C,H20D), C21B(H21C,H21D),
 C19B(H19C,H19D), C23B(H23C,H23D), C18B(H18C,H18D), C17B(H17C,H17D), C24B(H24C,
 H24D)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C),
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C),
  C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              65954
_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 2.923
_oxdiff_exptl_absorpt_empirical_full_min 0.645