Crystal structures of uranyl complexes with isobutyrate and isovalerate anions
Savchenkov, Anton V.; Vologzhanina, Anna V.; Dmitrienko, Artem O.; Zubavichus, Yan V.; Pushkin, Denis V.; Serezhkina, Larisa B.; Serezhkin, Viktor N.; Dalton Transactions  (2018) –; doi:10.1039/C7DT04042C

data_7045294
_publ_section_title
;
 Crystal structures of uranyl complexes with isobutyrate and isovalerate
 anions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04042C
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H27 O8 U1, H4 N1'
_chemical_formula_sum            'C15 H31 N O8 U'
_chemical_formula_weight         591.44
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-13 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6458(12)
_cell_length_b                   12.6458(12)
_cell_length_c                   12.6458(12)
_cell_measurement_reflns_used    9555
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.28
_cell_volume                     2022.3(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1682
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19814
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.865
_diffrn_reflns_theta_min         2.278
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.064
_exptl_absorpt_correction_T_max  0.2974
_exptl_absorpt_correction_T_min  0.0618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1667 before and 0.0950 after correction. The Ratio of minimum to maximum transmission is 0.2078. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.915
_refine_diff_density_min         -2.791
_refine_diff_density_rms         0.282
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.24(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1934
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+93.9420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                1539
_reflns_number_total             1934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04042c2.cif
_cod_data_source_block           a
_cod_original_cell_volume        2022.3(6)
_cod_database_code               7045294
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.76(6)
 0.24(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uiso(C3A) = Uiso(C3B)
Uiso(C2A) = Uiso(C2B)
Uiso(C5B) = Uiso(C5A)
Uiso(C4A) = Uiso(C4B)
4. Others
 Fixed Sof: C2B(0.5) H2BA(0.5) H2BB(0.5) C3B(0.5) H3B(0.5) C4B(0.5) H4BA(0.5)
 H4BB(0.5) H4BC(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) H5BC(0.5) C2A(0.5) H2AA(0.5)
 H2AB(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5A(0.5)
 H5AA(0.5) H5AB(0.5) H5AC(0.5)
5.a Riding coordinates:
 N1(H1A,H1B)
5.b Ternary CH refined with riding coordinates:
 C3B(H3B), C3A(H3A)
5.c Secondary CH2 refined with riding coordinates:
 C2B(H2BA,H2BB), C2A(H2AA,H2AB)
5.d Idealised Me refined as rotating group:
 C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,
 H5AC)
;
_shelx_res_checksum              8222
_olex2_submission_special_instructions 'No special instructions were received'