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_7044302
_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_absolute_configuration ad
_chemical_formula_moiety         'C29 H37 Cl4 N5 U, 0.25(C8 H16 O2)'
_chemical_formula_sum            'C31 H41 Cl4 N5 O0.5 U'
_chemical_formula_weight         871.52
_chemical_name_systematic
;
 ? 
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-05
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6426(11)
_cell_length_b                   28.025(2)
_cell_length_c                   17.5300(14)
_cell_measurement_reflns_used    9289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.08
_cell_measurement_theta_min      2.39
_cell_volume                     6702.3(9)
_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      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            180788
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.686
_diffrn_reflns_theta_min         1.453
_exptl_absorpt_coefficient_mu    5.193
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1211 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.7549.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethylether, tetrahydrofuran'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 6265 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         18080
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0191P)^2^+2.2318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                15376
_reflns_number_total             18080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02947k1.cif
_cod_data_source_block           sa1301
_cod_original_cell_volume        6702.4(9)
_cod_original_formula_sum        'C31 H41 Cl4 N5 O0.50 U'
_cod_database_code               7044302
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.408
_shelx_estimated_absorpt_t_min   0.219
_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 = C102-C103 = C103-C104
 1.51 with sigma of 0.02
 C201-C202 = C202-C203 = C203-C204
 1.51 with sigma of 0.02
 O100-C101 = O100-C104 = O200-C201 = O200-C204
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(O100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O200) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Same fragment restrains
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
{O200, C204, C203, C202, C201} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C202, C203, C204}
5. Others
 Fixed Sof: O100(0.5) C101(0.5) H10A(0.5) H10B(0.5) C102(0.5) H10C(0.5)
 H10D(0.5) C103(0.5) H10E(0.5) H10F(0.5) C104(0.5) H10G(0.5) H10H(0.5)
 O200(0.5) C201(0.5) H20A(0.5) H20B(0.5) C202(0.5) H20C(0.5) H20D(0.5)
 C203(0.5) H20E(0.5) H20F(0.5) C204(0.5) H20G(0.5) H20H(0.5)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C23(H23), C41(H41), C52(H52)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C42(H42A,
 H42B), C43(H43A,H43B), C50(H50A,H50B), C51(H51A,H51B), C101(H10A,H10B),
 C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C201(H20A,H20B), C202(H20C,
 H20D), C203(H20E,H20F), C204(H20G,H20H)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C34(H34), C35(H35), C36(H36)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              19753
_olex2_submission_special_instructions 'No special instructions were received'