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_1560031
_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         'C28 H52 O Si4 U, C24 H44 Si4 U'
_chemical_formula_sum            'C52 H96 O Si8 U2'
_chemical_formula_weight         1438.06
_chemical_name_common            1
_chemical_name_systematic        1
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-03
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5444(3)
_cell_length_b                   18.4631(4)
_cell_length_c                   31.5083(7)
_cell_measurement_reflns_used    14898
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      71.3630
_cell_measurement_theta_min      4.7890
_cell_volume                     6134.1(3)
_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_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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     35.00 109.00   1.00   15.00    --   36.79 178.00 -30.00   74
  2  \w    -35.00  66.00   1.00   15.00    --   36.79 -19.00  90.00  101
  3  \w     35.00 109.00   1.00   15.00    --   36.79 178.00  90.00   74
  4  \w     40.00 125.00   1.00   32.50    --  107.00 -61.00 -60.00   85
  5  \w     89.00 174.00   1.00   32.50    --  107.00  61.00  60.00   85
  6  \w     37.00  87.00   1.00   32.50    --  107.00-111.00 150.00   50
  7  \w     36.00 145.00   1.00   32.50    --  107.00 -15.00 120.00  109
  8  \w     80.00 175.00   1.00   32.50    --  107.00  77.00-120.00   95
  9  \w     36.00 145.00   1.00   32.50    --  107.00 -15.00  30.00  109
 10  \w     10.00 104.00   1.00   15.00    --   36.79  77.00-150.00   94
 11  \w     10.00 104.00   1.00   15.00    --   36.79  77.00  90.00   94
 12  \w     69.00 178.00   1.00   32.50    --  107.00  15.00-180.00  109
 13  \w     38.00  84.00   1.00   32.50    --  107.00 -95.00-120.00   46
;
_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      0.0033887000
_diffrn_orient_matrix_UB_12      0.0443114000
_diffrn_orient_matrix_UB_13      -0.0414784000
_diffrn_orient_matrix_UB_21      0.1146954000
_diffrn_orient_matrix_UB_22      -0.0445620000
_diffrn_orient_matrix_UB_23      -0.0153695000
_diffrn_orient_matrix_UB_31      -0.0903694000
_diffrn_orient_matrix_UB_32      -0.0549798000
_diffrn_orient_matrix_UB_33      -0.0207849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            34384
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.580
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70619
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             2848
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-heptane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 4615 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.039(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                11145
_reflns_number_total             11753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05199c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1560031--1560036.cif.'
_cod_database_code               1560031
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C52 H96 O Si8 U2 '
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.137
_reflns_odcompleteness_completeness 99.87
_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:
 C49(H49A,H49B), C51(H51A,H51B), C50(H50A,H50B), C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C20(H20), C14(H14), C9(H9), C16(H16), C19(H19), C12(H12), C17(H17),
 C24(H24), C13(H13), C15(H15), C21(H21), C10(H10), C22(H22), C23(H23), C18(H18)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C33(H33A,H33B,
 H33C), C39(H39A,H39B,H39C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C), C30(H30A,H30B,H30C),
 C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C), C31(H31A,H31B,
 H31C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C26(H26A,H26B,H26C), C36(H36A,
 H36B,H36C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C),
 C42(H42A,H42B,H42C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              13396
_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 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.687