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_1561817
_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         '2(O18 Se3 U2), 6(H2 O), H3 O, 3(C2 H8 N)'
_chemical_formula_sum            'C6 H39 N3 O43 Se6 U4'
_chemical_formula_weight         2267.28
_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   mixed
_cell_angle_alpha                90
_cell_angle_beta                 120.39(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.451(5)
_cell_length_b                   31.126(5)
_cell_length_c                   14.197(4)
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      34.39
_cell_measurement_theta_min      2.21
_cell_volume                     4746(3)
_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  0.0963
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34682
_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         27.499
_diffrn_reflns_theta_min         1.308
_exptl_absorpt_coefficient_mu    18.323
_exptl_absorpt_correction_T_max  0.5431
_exptl_absorpt_correction_T_min  0.2318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.608
_refine_diff_density_min         -4.340
_refine_diff_density_rms         0.332
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         10896
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0431P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5379
_reflns_number_total             10896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CompIV_last.cif
_cod_data_source_block           Compound_IV
_cod_database_code               1561817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, {H41A,H41B} of O41, {H42A,H42B} of O42, All O(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H40A,H40B} of O40, {H39A,H39B} of O39, {H38A,H38B} of
  O38, {H37A,H37B} of O37
2. Restrained distances
 O37-H37A = O37-H37B
 0.9 with sigma of 0.05
 H37A-H37B
 1.5 with sigma of 0.1
 O40-H40A = O40-H40B
 0.9 with sigma of 0.05
 H40A-H40B
 1.5 with sigma of 0.1
 O41-H41A = O41-H41B
 1 with sigma of 0.05
 H41A-H41B
 1.6 with sigma of 0.1
 O43-H43A = O43-H43B = O43-H43C
 1 with sigma of 0.05
 H43A-H43B = H43A-H43C = H43B-H43C
 1.6 with sigma of 0.1
 H38B-O21
 2 with sigma of 0.02
 O42_$1-H42A_$1 = O42_$1-H42B_$1
 0.9 with sigma of 0.02
 H42B_$1-H42A_$1
 1.6 with sigma of 0.02
 H37A-H43C_$2
 1.9 with sigma of 0.02
 H43A-H43B
 1.8 with sigma of 0.02
 H38A-O39
 2 with sigma of 0.02
 H39A-O33
 1.9 with sigma of 0.02
 O39-H39A
 0.9 with sigma of 0.02
 H39A-H1B_$1
 1.9 with sigma of 0.02
 H39B-H38A
 1.7 with sigma of 0.02
 O39-H39B
 0.6 with sigma of 0.02
 H43A-H42A
 1.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N1) = Uanis(C2)
Uanis(C3) = Uanis(N2) = Uanis(C4)
Uanis(C6) = Uanis(N3) = Uanis(C5)
Uanis(O29) = Uanis(O17)
4.a Everything fixed:
 H38A, H38B, H39A, H39B, H42A, H42B, H6A, H6B, H6C
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2D,H2E), N3(H3D,H3E)
4.c Me refined with everything fixed:
 C2(H2A,H2B,H2C)
4.d Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_cod_database_fobs_code 1561817