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_7054811
_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_formula_moiety         'C38 H68 O P Si2 U'
_chemical_formula_sum            'C38 H68 O P Si2 U'
_chemical_formula_weight         866.10
_chemical_name_common            2THF
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.568(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8847(7)
_cell_length_b                   14.9475(8)
_cell_length_c                   22.5236(14)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.7710
_cell_measurement_theta_min      3.6600
_cell_volume                     4001.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega  -46.00   55.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   19.0000 -120.0000 101

  2 omega  -88.00  -49.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295 -178.0000  -60.0000 39

  3 omega  -53.00    6.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295  -77.0000 -150.0000 59

  4 omega  -26.00   53.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   38.0000  120.0000 79

  5 omega  -79.00    1.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295  -57.0000  -60.0000 80

  6 omega  -26.00   -1.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7545  105.0000  171.0000 25

  7 omega   27.00   56.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7545  -99.0000  120.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0515873000
_diffrn_orient_matrix_UB_12      -0.0014749000
_diffrn_orient_matrix_UB_13      0.0159227000
_diffrn_orient_matrix_UB_21      -0.0276183000
_diffrn_orient_matrix_UB_22      -0.0151540000
_diffrn_orient_matrix_UB_23      -0.0259925000
_diffrn_orient_matrix_UB_31      0.0110264000
_diffrn_orient_matrix_UB_32      -0.0449511000
_diffrn_orient_matrix_UB_33      0.0082602000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mo/Ka
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34897
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.374
_diffrn_reflns_theta_min         3.429
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             1756
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         9625
_refine_ls_number_restraints     615
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+2.1311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7914
_reflns_number_total             9625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00590f2.cif
_cod_data_source_block           2THF
_cod_depositor_comments
'Adding full bibliography for 7054809--7054814.cif.'
_cod_database_code               7054811
_chemical_oxdiff_formula         'C38 H68 O1 P1 Si2 U1'
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.181
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Rigid bond restraints
 P1, C30, C29, C28, C27, C34, C33, C32, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P1A, C30A, C29A, C28A, C27A, C34A, C33A, C32A, C31A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
P1 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C34 \\sim C33 \\sim C32 \\sim
C31: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
P1A \\sim C30A \\sim C29A \\sim C28A \\sim C27A \\sim C34A \\sim C33A \\sim
C32A \\sim C31A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 P1A, C30A, C29A, C28A, C27A, C34A, C33A, C32A, C31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, C27, C28, C29, C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C35, C36, C37, C38, O1, Si1, Si2,
 U1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P1A)=Sof(C30A)=Sof(C29A)=Sof(C28A)=Sof(C27A)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C32A)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=1-FVAR(1)
 Sof(P1)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C15(H15),
 C18(H18), C21(H21), C24(H24)
6.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C31(H31D,H31E,H31F), C32(H32D,H32E,H32F), C33(H33D,H33E,
 H33F), C34(H34D,H34E,H34F), C34A(H34A,H34B,H34C), C33A(H33A,H33B,H33C),
 C32A(H32A,H32B,H32C), C31A(H31A,H31B,H31C)
;
_shelx_res_checksum              64062
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'