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_7044300
_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
'C27 H33 Cl4 N5 U, 0.8(C4 H8 O), 0.2(C4 H10 O)'
_chemical_formula_sum            'C31 H41.4 Cl4 N5 O U'
_chemical_formula_weight         879.92
_chemical_name_systematic
;
 ? 
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 102.9240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8297(2)
_cell_length_b                   19.9918(3)
_cell_length_c                   17.9909(3)
_cell_measurement_reflns_used    9009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.54
_cell_volume                     3445.89(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      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker Smart APEX-II CCD'
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52273
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         2.409
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.052
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1376 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.6958.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1722
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethylether, tetrahydrofuran'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 5520 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         13913
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0290P)^2^+0.4548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                12666
_reflns_number_total             13913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02947k1.cif
_cod_data_source_block           sa1210
_cod_original_formula_sum        'C31 H41.40 Cl4 N5 O U'
_cod_database_code               7044300
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.353
_shelx_estimated_absorpt_t_min   0.225
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C211-C212 = C214-C215
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.003
and sigma for terminal atoms of 0.006
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.003
and sigma for terminal atoms of 0.006
C211 \\sim C212 \\sim O213 \\sim C214 \\sim C215: within 2A with sigma of 0.003
and sigma for terminal atoms of 0.006
Uanis(C19) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of
0.003 and sigma for terminal atoms of 0.006
Uanis(O100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(O200) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C211) \\sim Ueq, Uanis(C212) \\sim Ueq, Uanis(O213) \\sim Ueq,
Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
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: O200(0.6) C201(0.6) H20A(0.6) H20B(0.6) C202(0.6) H20C(0.6)
 H20D(0.6) C203(0.6) H20E(0.6) H20F(0.6) C204(0.6) H20G(0.6) H20H(0.6)
 C211(0.4) H21C(0.4) H21D(0.4) H21E(0.4) C212(0.4) H21F(0.4) H21G(0.4)
 O213(0.4) C214(0.4) H21H(0.4) H21I(0.4) C215(0.4) H21J(0.4) H21K(0.4) H21L(0.4)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C23(H23), C39(H39), C50(H50)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C40(H40A,
 H40B), C41(H41A,H41B), C48(H48A,H48B), C49(H49A,H49B), C101(H10A,H10B),
 C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C201(H20A,H20B), C202(H20C,
 H20D), C203(H20E,H20F), C204(H20G,H20H), C212(H21F,H21G), C214(H21H,H21I)
6.c Me refined with riding coordinates:
 C211(H21C,H21D,H21E), C215(H21J,H21K,H21L)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C5(H5A), C6(H6), C7(H7), N7(H7A), N10(H10), C32(H32),
 C33(H33), C34(H34)
6.e 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), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              39001
_olex2_submission_special_instructions 'No special instructions were received'