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_1560032
_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         'C26 H50 O Si4 U'
_chemical_formula_sum            'C26 H50 O Si4 U'
_chemical_formula_weight         729.05
_chemical_name_common            5
_chemical_name_systematic        5
_chemical_properties_physical    Air-sensitive,Moisture-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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2021-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.001(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5935(3)
_cell_length_b                   9.9770(2)
_cell_length_c                   18.6747(4)
_cell_measurement_reflns_used    12622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.6840
_cell_measurement_theta_min      2.9160
_cell_volume                     3080.27(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_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    -88.00  86.00   1.00    2.00    --    0.00  41.00-162.00  174
  2  \w    -19.00   6.00   1.00    8.00    --    5.00  41.00-162.00   25
  3  \w   -178.00 -32.00   1.00    8.00    --  -89.00  41.00-162.00  146
  4  \w   -152.00 -76.00   1.00    8.00    --  -89.00  30.00 150.00   76
  5  \w    -63.00  -2.00   1.00    8.00    --  -89.00  30.00 150.00   61
  6  \w   -177.00-114.00   1.00    8.00    --  -89.00  40.00 -30.00   63
  7  \w   -109.00 -49.00   1.00    8.00    --  -89.00  40.00 -30.00   60
  8  \w    -25.00   0.00   1.00    8.00    --  -89.00  40.00 -30.00   25
  9  \w   -165.00  -5.00   1.00    8.00    --  -89.00  40.00  90.00  160
;
_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      0.0855177000
_diffrn_orient_matrix_UB_12      0.0305798000
_diffrn_orient_matrix_UB_13      0.0558884000
_diffrn_orient_matrix_UB_21      0.0362351000
_diffrn_orient_matrix_UB_22      -0.0949767000
_diffrn_orient_matrix_UB_23      -0.0448196000
_diffrn_orient_matrix_UB_31      0.0070654000
_diffrn_orient_matrix_UB_32      0.1180171000
_diffrn_orient_matrix_UB_33      -0.0506847000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16262
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.759
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethylether'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.367
_refine_diff_density_min         -1.994
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0723P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5317
_reflns_number_total             5495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05199c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1560031--1560036.cif.'
_cod_database_code               1560032
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H49 O Si4 U'
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.138
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C9(H9), C11(H11), C10(H10), C6(H6), C12(H12), C5(H5)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C13(H13A,H13B,
 H13C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C24(H24A,
 H24B,H24C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              19248
_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 2.307
_oxdiff_exptl_absorpt_empirical_full_min 0.460