Highly conjugated systems with pedal motion in uranyl crotonate compounds with 1,2-bis(4-pyridyl)ethylene as a neutral ligand or a counter cation
Savchenkov, Anton V.; Vologzhanina, Anna V.; Pushkin, Denis V.; Serezhkina, Larisa B.; Serezhkin, Viktor N.; Inorganica Chimica Acta 498 (2019) 119089–; doi:10.1016/j.ica.2019.119089

data_1565765
_publ_section_title
;
 Highly conjugated systems with pedal motion in uranyl crotonate compounds
 with 1,2-bis(4-pyridyl)ethylene as a neutral ligand or a counter cation
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119089
_journal_paper_doi               10.1016/j.ica.2019.119089
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety
'2(C12 H15 O8 U), C8 H14 O8 U, 2(H O), 2(C12 H12 N2)'
_chemical_formula_sum            'C56 H70 N4 O26 U3'
_chemical_formula_weight         1929.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                104.352(2)
_cell_angle_beta                 103.862(2)
_cell_angle_gamma                103.053(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1617(9)
_cell_length_b                   11.2210(10)
_cell_length_c                   16.7560(15)
_cell_measurement_reflns_used    4291
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.391
_cell_measurement_theta_min      2.016
_cell_volume                     1712.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23434
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.610
_diffrn_reflns_theta_min         1.966
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    7.154
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0916 before and 0.0411 after correction. The Ratio of minimum to maximum transmission is 0.7637. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       prism
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.895
_refine_diff_density_min         -2.128
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10446
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+1.0808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7146
_reflns_number_total             10446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119089.cif
_cod_data_source_block           mo_231_293_0m
_cod_database_code               1565765
_shelx_estimated_absorpt_t_max   0.507
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H12E-H12D
 1.3 with sigma of 0.02
 H12E-O12
 0.85 with sigma of 0.02
 H12D-O12
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(O13) = Uanis(O14)
4. Others
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=1-FVAR(1)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 FVAR(1)
 Fixed Sof: O13(0.5) H13(0.5) O14(0.5) H14B(0.5) C18A(0.45) H18A(0.45)
 C018(0.55) H018(0.55)
5.a Riding coordinates:
 O13(H13), O14(H14B)
5.b Rotating group:
 O12(H12D,H12E)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15),
 C14A(H14A), C15A(H15A), N1(H1), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), N2(H2A), C18A(H18A), C018(H018), C23(H23), C24(H24), C26(H26),
 C27(H27)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              27076