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_7054813
_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         'C70 H120 N2 O5 Si4 U2'
_chemical_formula_sum            'C70 H120 N2 O5 Si4 U2'
_chemical_formula_weight         1658.09
_chemical_name_common            4
_chemical_name_systematic        4
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive, Oxygen-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_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                97.035(6)
_cell_angle_beta                 97.053(6)
_cell_angle_gamma                102.983(7)
_cell_formula_units_Z            2
_cell_length_a                   12.9610(9)
_cell_length_b                   14.6337(10)
_cell_length_c                   22.2106(16)
_cell_measurement_reflns_used    39042
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     4024.5(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_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_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47825
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.562
_diffrn_reflns_theta_min         2.430
_diffrn_source                   'Sealed Tube'
_diffrn_standards_interval_count 120
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.121
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.017
_refine_diff_density_min         -2.642
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         18150
_refine_ls_number_restraints     1119
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1107P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11223
_reflns_number_total             18150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00590f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7054809--7054814.cif.'
_cod_database_code               7054813
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C58) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
3. Rigid body (RIGU) restrains
 U2, C1, N1, O2, O3, C2, C5, U1, C3, C6, C4, C9, O1, O4, C47, C49, C50, C46,
 C48, C52, C51, C45, O5, C25, C20, C26, C24, C23, C21, C19, C22, C7, H6A, H6B,
 H6C, C8, H9A, H9B, H9C, C10, H47, H49, H50, H46, Si4, H52, H51, Si3, H25, H20,
 H26, H24, H23, H21, Si1, Si2, H7A, H7B, H7C, H8A, H8B, H8C, N2, C62, C65, C68,
 C53, C56, C59, C27, C30, C33, C36, C39, C42, C11, C14, H62, C63, C64, H65, C66,
  C67, H68, C69, C70, H53, C54, C55, H56, C57, C58, H59, C60, C61, H27, C28,
 C29, H30, C31, C32, H33, C34, C35, H36, C37, C38, H39, C40, C41, H42, C43, C44,
  C12, C15, C13, C18, H63A, H63B, H63C, H64A, H64B, H64C, H66A, H66B, H66C,
 H67A, H67B, H67C, H69A, H69B, H69C, H70A, H70B, H70C, H54A, H54B, H54C, H55A,
 H55B, H55C, H57A, H57B, H57C, H58A, H58B, H58C, H60A, H60B, H60C, H61A, H61B,
 H61C, H28A, H28B, H28C, H29A, H29B, H29C, H31A, H31B, H31C, H32A, H32B, H32C,
 H34A, H34B, H34C, H35A, H35B, H35C, H37A, H37B, H37C, H38A, H38B, H38C, H40A,
 H40B, H40C, H41A, H41B, H41C, H43A, H43B, H43C, H44A, H44B, H44C, C16, H15A,
 H15B, H15C, C17, H18A, H18B, H18C, H16A, H16B, H16C, H17A, H17B, H17C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C27(H27), C30(H30), C33(H33), C36(H36), C39(H39), C42(H42), C53(H53),
 C56(H56), C59(H59), C62(H62), C65(H65), C68(H68)
4.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C46(H46),
 C47(H47), C49(H49), C50(H50), C51(H51), C52(H52)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              90934
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'