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_1561820
_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 Se10 U6), C2 H8 N, 1.5(C4 N2)'
_chemical_formula_sum            'C8 H8 N4 O26 Se5 U3'
_chemical_formula_weight         1685.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                   11.6591(11)
_cell_length_b                   14.9556(17)
_cell_length_c                   22.194(2)
_cell_measurement_reflns_used    6939
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.96
_cell_measurement_theta_min      1.64
_cell_volume                     3869.9(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.462
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.462
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10991
_diffrn_reflns_point_group_measured_fraction_full 0.462
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.552
_diffrn_reflns_theta_min         1.642
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.310
_exptl_absorpt_correction_T_max  0.8261
_exptl_absorpt_correction_T_min  0.3798
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    2.892
_exptl_crystal_description       plate
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1221
_reflns_number_total             1680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CompVII_last.cif
_cod_data_source_block           Compound_VII
_cod_original_cell_volume        3870.0(7)
_cod_database_code               1561820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) = Uanis(O14)
3. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) C1(0.5) H1C(0.5) H1D(0.5) H1E(0.5)
 C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) N2(0.5) N3(0.5) C7(0.5) C8(0.5)
4.a Everything fixed:
 H2A, H2B, H2C
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_cod_database_fobs_code 1561820