Activation of carbon suboxide (C<sub>3</sub>O<sub>2</sub>) by U(iii) to form a cyclobutane-1,3-dione ring.
Tsoureas, Nikolaos; Cloke, F Geoffrey N; Chemical communications (Cambridge, England) 54 (2018) 8830–8833; doi:10.1039/c8cc04391d

data_7121988
_publ_section_title
;
 Activation of carbon suboxide (C<sub>3</sub>O<sub>2</sub>) by U(iii) to
 form a cyclobutane-1,3-dione ring.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8830
_journal_page_last               8833
_journal_paper_doi               10.1039/c8cc04391d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C50 H78 O Si6 U2 . C4H12Si1'
_chemical_formula_sum            'C54 H90 O Si7 U2'
_chemical_formula_weight         1427.94
_chemical_name_common            4
_chemical_name_systematic        4
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                87.990(3)
_cell_angle_beta                 89.525(3)
_cell_angle_gamma                72.969(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0648(4)
_cell_length_b                   14.3955(7)
_cell_length_c                   25.3043(8)
_cell_measurement_reflns_used    10038
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.1360
_cell_measurement_theta_min      3.7010
_cell_volume                     3155.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Dirdif 2008 (P.T. Beurskens, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16655
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.710
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    15.847
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.23695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Light Brown'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: SiMe4'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.702
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         11156
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0654P)^2^+9.0572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9792
_reflns_number_total             11156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04391d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7121987--7121988.cif.'
_cod_database_code               7121988
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.087
_shelx_estimated_absorpt_t_max   0.742
_oxdiff_exptl_absorpt_empirical_full_min 0.586
_oxdiff_exptl_absorpt_empirical_full_max 2.539
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              73443