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_7121987
_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         'C106 H156 O6 Si12 U4'
_chemical_formula_sum            'C106 H156 O6 Si12 U4'
_chemical_formula_weight         2815.50
_chemical_name_common            3
_chemical_name_systematic        3
_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-2016/6
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                101.395(3)
_cell_angle_beta                 104.401(3)
_cell_angle_gamma                111.570(3)
_cell_formula_units_Z            1
_cell_length_a                   12.6651(4)
_cell_length_b                   16.1115(5)
_cell_length_c                   19.1954(6)
_cell_measurement_reflns_used    11293
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.1220
_cell_measurement_theta_min      4.3540
_cell_volume                     3341.6(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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution
;
DirDiff 2008 (P.T. Beurskens, G. Beurskens, R. de Gelder, S. Garcia-Granda, R.O. Gould, and J.M.M. Smits (2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18388
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.850
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    14.816
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.79504
_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            Brown-red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-heptane'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
A highly dissordered molecule of crystallisation solvent (n-heptane) could not be properly modelled. This disorder
was treated using the SQUEEZE routine in PLATON.
;
_refine_diff_density_max         0.796
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         11780
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+2.9683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10282
_reflns_number_total             11780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04391d2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121987--7121988.cif.
;
_cod_database_code               7121987
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.095
_shelx_estimated_absorpt_t_max   0.349
_oxdiff_exptl_absorpt_empirical_full_min 0.864
_oxdiff_exptl_absorpt_empirical_full_max 1.384
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              91521