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_1561814
_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         'H2 O11 Se2 U, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H18 N2 O11 Se2 U'
_chemical_formula_weight         666.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5363(7)
_cell_length_b                   12.2021(11)
_cell_length_c                   16.7601(16)
_cell_measurement_reflns_used    5132
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      35.12
_cell_measurement_theta_min      2.96
_cell_volume                     1541.2(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13644
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.064
_exptl_absorpt_coefficient_mu    15.306
_exptl_absorpt_correction_T_max  0.3224
_exptl_absorpt_correction_T_min  0.1779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.339
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.188(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4117
_reflns_number_total             4492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CompI_last.cif
_cod_data_source_block           compound_I
_cod_database_code               1561814
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.812(14) 0.188(14)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 H11A-H11B
 1.5 with sigma of 0.02
 O11-H11A = O11-H11B
 0.9 with sigma of 0.02
 H11B-U1 = U1-H11A
 2.9 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 N2(H2D,H2E), N1(H1D,H1E)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_cod_database_fobs_code 1561814