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_1565766
_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                105.819(11)
_cell_angle_beta                 101.357(13)
_cell_angle_gamma                102.575(11)
_cell_formula_units_Z            1
_cell_length_a                   10.180(7)
_cell_length_b                   11.235(7)
_cell_length_c                   16.804(12)
_cell_measurement_reflns_used    2166
_cell_measurement_temperature    295
_cell_measurement_theta_max      21.80
_cell_measurement_theta_min      2.18
_cell_volume                     1736(2)
_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      295
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2248
_diffrn_reflns_av_unetI/netI     0.2880
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.901
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21392
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.430
_diffrn_reflns_theta_min         2.175
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.056
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0401 after correction.
The Ratio of minimum to maximum transmission is 0.6920.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.845
_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         2.412
_refine_diff_density_min         -2.963
_refine_diff_density_rms         0.259
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         10352
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.2463
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2965
_reflns_number_total             10352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119089.cif
_cod_data_source_block           fin
_cod_database_code               1565766
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.271
_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
 C16A-C15A
 1.5 with sigma of 0.02
 C16A-C14A
 2.4 with sigma of 0.02
 C14A-C15A
 1.3 with sigma of 0.02
 C14-C15
 1.3 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(N2) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uiso(C14A) = Uiso(C14)
Uanis(O13) = Uanis(O14)
Uiso(C16A) = Uiso(C16) = Uiso(C15) = Uiso(C15A)
4. Others
 Fixed Sof: C15A(0.5) H15A(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5) O13(0.5)
 H13(0.5) O14(0.5) H14B(0.5) C14A(0.5) H14A(0.5)
5.a Riding coordinates:
 O12(H12D,H12E), O13(H13), O14(H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C15A(H15A), C14(H14),
 C15(H15), N1(H1), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), N2(H2A),
 C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C14A(H14A)
5.c 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              29060