Topologically and geometrically flexible structural units in seven new organically templated uranyl selenates and selenite‒selenates
Gurzhiy, Vladislav V.; Kovrugin, Vadim M.; Tyumentseva, Olga S.; Mikhaylenko, Pavel A.; Krivovichev, Sergey V.; Tananaev, Ivan G.; Journal of Solid State Chemistry 229 (2015) 32–40; doi:10.1016/j.jssc.2015.04.040

data_1561816
_publ_section_title
;
 Topologically and geometrically flexible structural units in seven new
 organically templated uranyl selenates and selenite--selenates
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              32
_journal_page_last               40
_journal_paper_doi               10.1016/j.jssc.2015.04.040
_journal_volume                  229
_journal_year                    2015
_chemical_formula_moiety
'O33.86 Se6 U4, 0.5(O2), 0.5(N2 O6), 2(C4 H15 N3)'
_chemical_formula_sum            'C8 H30 N7 O37.86 Se6 U4'
_chemical_formula_weight         2256.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 98.0190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1679(4)
_cell_length_b                   10.9040(4)
_cell_length_c                   17.9913(6)
_cell_measurement_reflns_used    6752
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      2.62
_cell_volume                     2169.46(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23671
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    20.036
_exptl_absorpt_correction_T_max  0.3937
_exptl_absorpt_correction_T_min  0.1512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.824
_refine_diff_density_min         -1.997
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3855
_reflns_number_total             4988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CompIII_last.cif
_cod_data_source_block           Compound_III
_cod_database_code               1561816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 O19-N4
 1.25 with sigma of 0.02
 O21-N4 = O20-N4
 1.25 with sigma of 0.02
 Se3A-O7_$1 = Se3A-O3
 1.9 with sigma of 0.02
 Se3A-O12
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O20) = Uanis(O21) = Uanis(O19) = Uanis(N4)
Uanis(Se3) = Uanis(Se3A)
4. Others
 Sof(Se3A)=1-FVAR(1)
 Sof(Se3)=Sof(O16)=FVAR(1)
 Fixed Sof: O18(0.5) O19(0.5) O20(0.5) O21(0.5) N4(0.5)
5.a Secondary CH2 refined with everything fixed:
 N1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C2(H2C,H2D), C3(H3D,H3E), C4(H4A,H4B)
5.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
5.d Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C)
;
_cod_database_fobs_code 1561816