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_7045293
_publ_section_title
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 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 unk
_chemical_formula_moiety         'C12 H21 Cs O8 U'
_chemical_formula_sum            'C12 H21 Cs O8 U'
_chemical_formula_weight         663.83
_chemical_name_common
'cesium tris(iso-butyrato-O,O')-dioxo-uranium(vi)'
_chemical_name_systematic
'cesium tris(2-methylpropanoato-O,O')-dioxo-uranium(vi)'
_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'
_audit_creation_method
'Olex2: 2016.02.16 svn.r3265 GCC:4.1.0 on Linux64, Python: 2.7.2, wxWidgets: 3.0.2 for OlexSys'
_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                   12.39075(4)
_cell_length_b                   12.39075(4)
_cell_length_c                   12.39075(4)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    295
_cell_measurement_theta_max      48.5
_cell_measurement_theta_min      2.9
_cell_volume                     1902.360(11)
_computing_cell_refinement       'TOPAS 4.2 (Coelho, 2003; Bruker, 2009)'
_computing_data_collection       'Bruker XRD Commander 2.6 (Bruker, 2007)'
_computing_data_reduction        'TOPAS 4.2 (Coelho, 2003; Bruker, 2009)'
_computing_molecular_graphics    'OLEX2 1.2 (Dolomanov et al., 2009, 2)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'TOPAS 4.2 (Coelho, 2003; Bruker, 2009)'
_computing_structure_solution    'FOX 1.9.7.0 (Favre-Nicolin, Cerny, 2002)'
_diffrn_ambient_temperature      295
_diffrn_detector                 '1D linear'
_diffrn_detector_type
;
Bruker LynxEye compound silicon strip 1D linear detector 
;
_diffrn_measurement_device_type  'Bruker D8 Advance Vario'
_diffrn_radiation_monochromator  'Ge 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_wavelength     1.54060
_diffrn_reflns_limit_h_max       -100
_diffrn_reflns_limit_h_min       100
_diffrn_reflns_limit_k_max       -100
_diffrn_reflns_limit_k_min       100
_diffrn_reflns_limit_l_max       -100
_diffrn_reflns_limit_l_min       100
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.318
_pd_block_diffractogram_id       final
_pd_char_colour                  yellow
_pd_char_particle_morphology     round
_pd_meas_2theta_range_inc        0.0105
_pd_meas_2theta_range_max        96.9656
_pd_meas_2theta_range_min        5.800000
_pd_meas_number_of_points        8701
_pd_meas_scan_method             cont
_pd_proc_2theta_range_inc        0.0105
_pd_proc_2theta_range_max        96.9656
_pd_proc_2theta_range_min        5.600000
_pd_proc_ls_background_function
;
19th order Chebyshev polynomial 
;
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_prof_R_factor        0.0215
_pd_proc_ls_prof_wR_expected     0.0192
_pd_proc_ls_prof_wR_factor       0.0296
_pd_proc_wavelength              1.54060
_pd_spec_mounting
;
deposited on sticky tape 
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.482
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     66
_refine_ls_number_restraints     27
_refine_ls_R_I_factor            0.0112
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_details     1/Y~i~
_refine_ls_weighting_scheme      calc
_cod_data_source_file            c7dt04042c2.cif
_cod_data_source_block           final
_cod_database_code               7045293
_olex2_refinement_description
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1. Others
 Fixed Sof: U1(0.333) O1(0.333) O2(0.333) C3(0.5) C3B(0.5) C4(0.5) C4B(0.5)
 Cs2(0.333) H3BA(0.5) H3BB(0.5) H2A(0.5) H2B(0.5) H3BC(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) H4BA(0.5) H4A(0.5) H4B(0.5) H4C(0.5) H4BB(0.5) H4BC(0.5)
 Fixed Uiso: U1(0.05) O1(0.05) O2(0.05) O3(0.05) O4(0.05) C1(0.05) C2(0.05)
 C3(0.05) C3B(0.05) C4(0.05) C4B(0.05) Cs2(0.05) H3BA(0.05) H3BB(0.05)
 H2A(0.06) H2B(0.06) H3BC(0.05) H3A(0.05) H3B(0.05) H3C(0.05) H4BA(0.05)
 H4A(0.05) H4B(0.05) H4C(0.05) H4BB(0.05) H4BC(0.05)
 Fixed X: U1(0.54912) O1(0.4673) O2(0.6308) O3(0.7105) O4(0.6634) C1(0.7253)
 C2(0.804) C3(0.901) C3B(0.898) C4(0.762) C4B(0.841) Cs2(0.82913) H3BA(0.878)
 H3BB(0.957) H2A(0.83226) H2B(0.76518) H3BC(0.92) H3A(0.923) H3B(0.959)
 H3C(0.88) H4BA(0.78) H4A(0.729) H4B(0.82) H4C(0.708) H4BB(0.872) H4BC(0.894)
 Fixed Y: U1(0.95088) O1(1.0327) O2(0.8692) O3(1.0109) O4(1.1072) C1(1.0863)
 C2(1.18) C3(1.143) C3B(1.18) C4(1.29) C4B(1.161) Cs2(0.82913) H3BA(1.215)
 H3BB(1.219) H2A(1.19119) H2B(1.24877) H3BC(1.108) H3A(1.073) H3B(1.193)
 H3C(1.142) H4BA(1.166) H4A(1.289) H4B(1.34) H4C(1.311) H4BB(1.09) H4BC(1.214)
 Fixed Z: U1(0.04912) O1(-0.0327) O2(0.1308) O3(-0.0536) O4(0.0876) C1(0.009)
 C2(-0.006) C3(-0.067) C3B(0.073) C4(-0.036) C4B(-0.118) Cs2(-0.17087)
 H3BA(0.139) H3BB(0.04) H2A(0.06702) H2B(-0.00172) H3BC(0.088) H3A(-0.044) H3B(-
 0.059) H3C(-0.144) H4BA(-0.165) H4A(-0.106) H4B(-0.035) H4C(0.016) H4BB(-
 0.123) H4BC(-0.139)
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