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_7045292
_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         '0.05(C240 H448 Na20 O174 U20)'
_chemical_formula_sum            'C12 H22.4 Na O8.7 U'
_chemical_formula_weight         566.92
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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            20
_cell_length_a                   21.051(4)
_cell_length_b                   21.361(4)
_cell_length_c                   21.402(4)
_cell_measurement_reflns_used    159
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.59
_cell_measurement_theta_min      3.82
_cell_volume                     9624(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    'SHELXT (Sheldrixk, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9699
_diffrn_reflns_av_R_equivalents  0.1457
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            100705
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        37.500
_diffrn_reflns_theta_max         38.483
_diffrn_reflns_theta_min         3.678
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.839
_exptl_absorpt_correction_T_max  0.158
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Scala
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_description       prism
_exptl_crystal_F_000             5340
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         4.514
_refine_diff_density_min         -2.925
_refine_diff_density_rms         0.258
_refine_ls_abs_structure_details
;
 Flack x determined using 5237 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.110(6)
_refine_ls_extinction_coef       0.00025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         20732
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                14289
_reflns_number_total             20732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04042c2.cif
_cod_data_source_block           u205
_cod_original_formula_sum        'C12 H22.40 Na O8.70 U'
_cod_database_code               7045292
_shelxl_version_number           2014-3
_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, All O(H,H) groups
2. Restrained distances
 C31-C30
 1.5 with sigma of 0.02
 O28-C37 = C37-O27
 1.23 with sigma of 0.02
 C38-C37
 1.5 with sigma of 0.02
 C8-C6 = C6-C7
 1.5 with sigma of 0.02
 C8-C7
 2.5 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.02
 C5-C8
 2.5 with sigma of 0.02
 C7-C5
 2.5 with sigma of 0.02
 C26-C28 = C26-C27 = C26-C25
 1.5 with sigma of 0.02
 C28-C25
 2.5 with sigma of 0.02
 C28-C27
 2.5 with sigma of 0.02
 C27-C25
 2.5 with sigma of 0.02
 O5-C5
 1.28 with sigma of 0.02
 O6-C5
 1.28 with sigma of 0.02
 O6-O5
 2.15 with sigma of 0.02
 C4A-C3A
 2.5 with sigma of 0.02
 C14-C16A
 1.5 with sigma of 0.02
 C14-C15A
 1.5 with sigma of 0.02
 C16-C14
 1.5 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.02
 C16-C13
 2.5 with sigma of 0.02
 C13-C15
 2.5 with sigma of 0.02
 C16A-C15A
 2.5 with sigma of 0.02
 C16-C15
 2.5 with sigma of 0.02
 C24A-C22 = C23-C22 = C23A-C22 = C24-C22
 1.5 with sigma of 0.02
 C24A-C23
 2.5 with sigma of 0.02
 C21-C24A
 2.5 with sigma of 0.02
 C26-C28A
 1.5 with sigma of 0.02
 C27A-C28A
 2.5 with sigma of 0.02
 C31A-C30 = C32A-C30
 1.5 with sigma of 0.02
 C32A-C31
 2.5 with sigma of 0.02
 C31A-C32A
 2.5 with sigma of 0.02
 C30-C29
 1.5 with sigma of 0.02
 C29-C31
 2.5 with sigma of 0.02
 C29-C31A
 2.5 with sigma of 0.02
 C11-C10
 1.5 with sigma of 0.02
 C12A-C11
 2.5 with sigma of 0.02
 C35-C34
 1.5 with sigma of 0.02
 C38-C39A
 1.5 with sigma of 0.02
 C38-C39
 1.5 with sigma of 0.02
 C38-C40
 1.5 with sigma of 0.02
 C38-C40A
 1.5 with sigma of 0.02
 C39-C37
 2.5 with sigma of 0.02
 C37-C39A
 2.5 with sigma of 0.02
 C37-C40A
 2.5 with sigma of 0.02
 C40-C37
 2.5 with sigma of 0.02
 C59A-C58
 1.5 with sigma of 0.02
 C60-C58
 1.5 with sigma of 0.02
 C59A-C60
 2.5 with sigma of 0.02
 C59A-C57
 2.5 with sigma of 0.02
 C60A-C59
 2.5 with sigma of 0.02
 C11A-C10
 1.5 with sigma of 0.02
 C58-C57
 1.5 with sigma of 0.02
 C32-C29
 2.5 with sigma of 0.02
 C54-C53
 1.5 with sigma of 0.02
 C3-C2 \\sim C3A-C2 \\sim C4-C2 \\sim C4A-C2
 with sigma of 0.02
 C43-C42 \\sim C44-C42
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(Na3) \\sim
Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(O25) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(Na4) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.008
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, : with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C34) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(C30)
\\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(C22) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.008
Uanis(O34) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O37)
\\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uanis(C25) \\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.008
Uanis(O18) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uiso(C4) = Uiso(C4A)
Uiso(C3) = Uiso(C3A)
Uiso(C12) = Uiso(C12A)
Uiso(C11) = Uiso(C11A)
Uiso(C16) = Uiso(C16A)
Uiso(C15) = Uiso(C15A)
Uiso(C23) = Uiso(C23A)
Uiso(C24) = Uiso(C24A)
Uiso(C28) = Uiso(C28A)
Uiso(C27) = Uiso(C27A)
Uiso(C31) = Uiso(C31A)
Uiso(C32) = Uiso(C32A)
Uiso(C39) = Uiso(C39A)
Uiso(C40) = Uiso(C40A)
Uanis(O6) = Uanis(O5) = Uanis(O1) = Uanis(O8)
4. Rigid body (RIGU) restrains
 O43, O27, Na4, O32, O23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C19, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C34, C36, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C44, C42, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C54, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O43(0.5) H43A(0.5) H43B(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) H10(0.5) H10A(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
 H14(0.5) H14A(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) H22(0.5) H22A(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) H26(0.5) H26A(0.5) C27(0.5) H27A(0.5)
 H27B(0.5) H27C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) H30A(0.5) H30(0.5)
 C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
 H38A(0.5) H38(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) H58(0.5) H58A(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5)
 C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
 C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C16A(0.5) H16D(0.5) H16E(0.5)
 H16F(0.5) C15A(0.5) H15D(0.5) H15E(0.5) H15F(0.5) C23A(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C28A(0.5)
 H28D(0.5) H28E(0.5) H28F(0.5) C27A(0.5) H27D(0.5) H27E(0.5) H27F(0.5)
 C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5) C32A(0.5) H32D(0.5) H32E(0.5)
 H32F(0.5) C39A(0.5) H39D(0.5) H39E(0.5) H39F(0.5) C40A(0.5) H40D(0.5)
 H40E(0.5) H40F(0.5) C59A(0.5) H59D(0.5) H59E(0.5) H59F(0.5) C60A(0.5)
 H60D(0.5) H60E(0.5) H60F(0.5)
 Fixed Uiso: C3(0.08) C4(0.08) C5(0.09) C6(0.09) C7(0.11) C8(0.11) C11(0.08)
 C12(0.08) C31(0.13) C32(0.13) C37(0.12) C38(0.12) C39(0.09) C40(0.09) C59(0.1)
 C60(0.1) C4A(0.08) C3A(0.08) C12A(0.08) C11A(0.08) C31A(0.13) C32A(0.13)
 C39A(0.09) C40A(0.09) C59A(0.1) C60A(0.1)
6.a Riding coordinates:
 O41(H41A,H41B), O42(H42A,H42B), O43(H43A,H43B), O44(H44A,H44B)
6.b Ternary CH refined with riding coordinates:
 C2(H2A), C2(H2B), C6(H6), C10(H10), C10(H10A), C14(H14), C14(H14A), C18(H18),
 C22(H22), C22(H22A), C26(H26), C26(H26A), C30(H30A), C30(H30), C34(H34),
 C38(H38A), C38(H38), C42(H42), C46(H46), C50(H50), C54(H54), C58(H58),
 C58(H58A)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C43(H43C,H43D,H43E), C44(H44C,H44D,H44E), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C4A(H4AA,H4AB,H4AC), C3A(H3AA,H3AB,H3AC), C12A(H12D,H12E,H12F), C11A(H11D,H11E,
 H11F), C16A(H16D,H16E,H16F), C15A(H15D,H15E,H15F), C23A(H23D,H23E,H23F),
 C24A(H24D,H24E,H24F), C28A(H28D,H28E,H28F), C27A(H27D,H27E,H27F), C31A(H31D,
 H31E,H31F), C32A(H32D,H32E,H32F), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F),
 C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F)
;
_shelx_res_checksum              48704
_olex2_submission_special_instructions 'No special instructions were received'