Synthesis and Characterization of Uranium(IV) Tetrachloro Complexes in Bis-Pyrazolylpyridine Ligand Environments
Korzekwa, Jana; Scheurer, Andreas; Heinemann, Frank; Meyer, Karsten; Dalton Trans.  (2017) –; doi:10.1039/C7DT02947K

data_7044301
_publ_section_title
;
 Synthesis and Characterization of Uranium(IV) Tetrachloro Complexes in
 Bis-Pyrazolylpyridine Ligand Environments
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02947K
_journal_year                    2017
_chemical_formula_moiety         '2(C21 H29 Cl4 N5 U), 0.5(C4 H10 O)'
_chemical_formula_sum            'C44 H63 Cl8 N10 O0.5 U2'
_chemical_formula_weight         1499.70
_chemical_name_systematic
;
 ? 
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-05 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.689(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.109(3)
_cell_length_b                   11.7208(13)
_cell_length_c                   17.7957(19)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.87
_cell_volume                     5573.7(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50007
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.311
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.228
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2884
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethylether, tetrahydrofuran'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         13278
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0264P)^2^+13.3275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11111
_reflns_number_total             13278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02947k1.cif
_cod_data_source_block           sa1207
_cod_original_cell_volume        5573.8(11)
_cod_original_formula_sum        'C44 H63 Cl8 N10 O0.50 U2'
_cod_database_code               7044301
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.369
_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. Restrained distances
 C101-C102 = C104-C105
 1.54 with sigma of 0.02
 O103-C102 = O103-C104
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C101 \\sim C102 \\sim O103 \\sim C104 \\sim C105: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(O103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{C105, C104, O103, C102, C101} sigma for 1-2: 0.02, 1-3: 0.04
as
{C101, C102, O103, C104, C105}
5. Others
 Fixed Sof: C101(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C102(0.5) H10D(0.5)
 H10E(0.5) O103(0.5) C104(0.5) H10F(0.5) H10G(0.5) C105(0.5) H10H(0.5)
 H10I(0.5) H10J(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E), C104(H10F,H10G)
6.b Me refined with riding coordinates:
 C101(H10A,H10B,H10C), C105(H10H,H10I,H10J)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C10(H10), C23(H23), C26(H26), C27(H27),
 C28(H28), C31(H31)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              32691
_olex2_submission_special_instructions 'No special instructions were received'