Guanidinium dioxidobis(picolinato-κ^2^<i>N</i>,<i>O</i>)(picolinato-κ<i>O</i>)uranate(VI)
Mishkevich, Vitalii I.; Grigoriev, Mikhail S.; Fedosseev, Alexandre M.; Moisy, Philippe; Acta Crystallographica Section E 68 (2012) m1243–; doi:10.1107/S1600536812035465

data_2236149
_publ_section_title
;
 Guanidinium
 dioxidobis(picolinato-\k^2^<i>N</i>,<i>O</i>)(picolinato-\k<i>O</i>)uranate(VI)
;
_journal_coeditor_code           CV5297
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1243
_journal_paper_doi               10.1107/S1600536812035465
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C H6 N3) [U (C6 H4 N O2)3 O2]'
_chemical_formula_moiety         'C H6 N3 +, C18 H12 N3 O8 U -'
_chemical_formula_sum            'C19 H18 N6 O8 U'
_chemical_formula_weight         696.42
_chemical_name_systematic
;
Guanidinium
dioxidobis(picolinato-\k^2^<i>N</i>,<i>O</i>)(picolinato-\k<i>O</i>)uranate(VI)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           <i>SHELXL97</i>
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.3842(4)
_cell_length_b                   13.1678(3)
_cell_length_c                   21.2743(4)
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.901
_cell_measurement_theta_min      6.163
_cell_volume                     4589.80(18)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1998)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            77357
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         4.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.130
_exptl_absorpt_correction_T_max  0.7635
_exptl_absorpt_correction_T_min  0.3601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.706
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                3818
_reflns_number_total             6604
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5297.cif
_cod_data_source_block           I
_cod_database_code               2236149
_cod_database_fobs_code          2236149