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_1561819
_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         '0.5(O52.67 Se10 U6), H2 O, 3(C4 H12 N)'
_chemical_formula_sum            'C12 H38 N3 O27.33 Se5 U3'
_chemical_formula_weight         1770.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 97.510(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.941(2)
_cell_length_b                   19.300(4)
_cell_length_c                   11.377(3)
_cell_measurement_reflns_used    1596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.30
_cell_measurement_theta_min      2.30
_cell_volume                     1946.4(8)
_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      293(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  0.1196
_diffrn_reflns_av_unetI/netI     0.1609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18435
_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         27.492
_diffrn_reflns_theta_min         2.091
_exptl_absorpt_coefficient_mu    17.217
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    3.021
_exptl_crystal_description       plate
_exptl_crystal_F_000             1591
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.733
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0091P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2459
_reflns_number_total             4597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CompVI_last.cif
_cod_data_source_block           Compound_VI
_cod_original_cell_volume        1946.5(7)
_cod_database_code               1561819
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C5-N2
 1.57 with sigma of 0.02
 C5-C6
 1.53 with sigma of 0.02
 H3B-H6A_$1
 1.95 with sigma of 0.02
 H17-O13
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16) = Uanis(O15)
Uanis(C3) = Uanis(C4) = Uanis(C1) = Uanis(C2)
Uanis(N2) = Uanis(C5) = Uanis(C6)
4. Others
 Fixed Sof: O16(0.16666)
5.a Everything fixed:
 H17
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C3(H3A,H3B), N2(H2D,H2E), C5(H5A,H5B)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_cod_database_fobs_code 1561819