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_7054809
_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         'C68 H120 N2 Si4 U2'
_chemical_formula_sum            'C68 H120 N2 Si4 U2'
_chemical_formula_weight         1554.08
_chemical_name_systematic
;
 1
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2b'
_space_group_name_H-M_alt        'P b c 21'
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-02
_audit_creation_method
;
Olex2 1.2
(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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.54240(10)
_cell_length_b                   22.7691(3)
_cell_length_c                   24.9695(2)
_cell_measurement_reflns_used    11478
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.0560
_cell_measurement_theta_min      3.9570
_cell_volume                     7130.77(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies
Version 1.171.37.31 
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies
Version 1.171.37.31 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies
Version 1.171.37.31 
;
_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    'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            96143
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.624
_diffrn_standards_interval_count 120
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             3128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.869
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.414
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.267(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         15976
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0524P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.954
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.999
_reflns_number_gt                14154
_reflns_number_total             15976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00590f2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
Adding full bibliography for 7054809--7054814.cif.

2018-01-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H60 N Si2 U'
_cod_original_formula_weight         777.04
_cod_original_formula_moiety         '0.5(C68 H120 N2 Si4 U2)'
_cod_original_formula_units_Z            8
_cod_database_code               7054809
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.489
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.733(7) 0.267(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C23(H23), C82(H82), C26(H26), C70(H70), C67(H67), C32(H32), C79(H79),
 C29(H29), C73(H73), C20(H20), C76(H76), C17(H17)
3.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C72(H72A,H72B,H72C), C5(H5A,H5B,
 H5C), C83(H83A,H83B,H83C), C71(H71A,H71B,H71C), C22(H22A,H22B,H22C), C58(H58A,
 H58B,H58C), C31(H31A,H31B,H31C), C80(H80A,H80B,H80C), C55(H55A,H55B,H55C),
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C77(H77A,H77B,
 H77C), C75(H75A,H75B,H75C), C69(H69A,H69B,H69C), C78(H78A,H78B,H78C), C34(H34A,
 H34B,H34C), C30(H30A,H30B,H30C), C6(H6A,H6B,H6C), C33(H33A,H33B,H33C), C7(H7A,
 H7B,H7C), C28(H28A,H28B,H28C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C68(H68A,
 H68B,H68C), C74(H74A,H74B,H74C), C81(H81A,H81B,H81C), C57(H57A,H57B,H57C),
 C56(H56A,H56B,H56C), C84(H84A,H84B,H84C)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C60(H60), C15(H15), C13(H13), C61(H61), C11(H11),
 C63(H63), C65(H65), C64(H64), C66(H66), C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'