Crystal structures of three uranyl-acetate-bipyridine complexes crystallized from hydraulic fracking fluid.
Whittington, Abigail A.; Keimowitz, Alison R.; Tanski, Joseph M.; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229623010288

data_2312366
_publ_section_title
;
 Crystal structures of three uranyl-acetate-bipyridine complexes
 crystallized from hydraulic fracking fluid.
;
_journal_coeditor_code           EQ3014
_journal_issue                   1
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229623010288
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'(C10 H9 N2)2 [U3 (C2 H3 O2)2 O8 (O H)2], C10 H8 N2, H2 O'
_chemical_formula_moiety
'2(C10 H9 N2 +), C4 H8 O14 U3 2-, C10 H8 N2, H2 O'
_chemical_formula_sum            'C34 H36 N6 O15 U3'
_chemical_formula_weight         1482.78
_chemical_name_systematic
;<i>catena</i>-Poly[bis(2,3'-bipyridinium)
[di-\m-acetato-\m~3~-hydroxido-\m-hydroxido-di-\m~3~-oxido-hexaoxidotriuranium(VI)]--2,3'-bipyridine--water (1/1/1)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.4120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8090(13)
_cell_length_b                   12.6324(12)
_cell_length_c                   23.699(2)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    125.(2)
_cell_measurement_theta_max      30.4568
_cell_measurement_theta_min      2.3920
_cell_volume                     4021.3(6)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2008),
OLEX2 (Dolomanov <i>et al.</i>,  2009), and
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      125.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            98670
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.50
_diffrn_source_voltage           45
_exptl_absorpt_coefficient_mu    12.127
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS: Bruker, 2013)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.541
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         12285
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                8925
_reflns_number_total             12285
_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_hkl_checksum              13845
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