Activation of carbon dioxide by new mixed sandwich uranium(iii) complexes incorporating cyclooctatetraenyl and pyrrolide, phospholide, or arsolide ligands
Kahan, Rachel J.; Cloke, F. Geoffrey N.; Roe, S. Mark; Nief, François; New J. Chem. 39 (2015) 7602–; doi:10.1039/C5NJ00590F

data_7054810
_publ_section_title
;
 Activation of carbon dioxide by new mixed sandwich uranium(iii) complexes
 incorporating cyclooctatetraenyl and pyrrolide, phospholide, or arsolide
 ligands
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              7602
_journal_paper_doi               10.1039/C5NJ00590F
_journal_volume                  39
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38  H68  N1 O1 Si2 U1'
_chemical_formula_sum            'C38 H68 N O Si2 U'
_chemical_formula_weight         849.14
_chemical_name_systematic
;
 1.THF
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
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_audit_creation_date             2015-02-27T13:49:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-04-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.366(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8517(2)
_cell_length_b                   14.9317(2)
_cell_length_c                   22.2479(3)
_cell_measurement_reflns_used    11478
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.0560
_cell_measurement_theta_min      3.9570
_cell_measurement_wavelength     1.54184
_cell_volume                     3936.00(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.845
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.845
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21216
_diffrn_reflns_point_group_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.153
_diffrn_reflns_theta_min         3.565
_diffrn_standards_interval_count 120
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.386
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.4839
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
'CrysAlisPro, Agilent Technologies 1.171.36.32'
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.613
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+29.9826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                5389
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00590f2.cif
_cod_data_source_block           1THF
_cod_depositor_comments
'Adding full bibliography for 7054809--7054814.cif.'
_cod_original_sg_symbol_H-M      P121/n1
_cod_database_code               7054810
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.79