Dehydration-driven evolution of topological complexity in ethylamonium uranyl selenates
Gurzhiy, Vladislav V.; Krivovichev, Sergey V.; Tananaev, Ivan G.; Journal of Solid State Chemistry 247 (2017) 105–112; doi:10.1016/j.jssc.2017.01.005

data_1560616
_publ_section_title
;
 Dehydration-driven evolution of topological complexity in ethylamonium
 uranyl selenates
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              105
_journal_page_last               112
_journal_paper_doi               10.1016/j.jssc.2017.01.005
_journal_volume                  247
_journal_year                    2017
_chemical_formula_moiety         'H O14 Se3 U, 3(C2 H8 N)'
_chemical_formula_sum            'C6 H25 N3 O14 Se3 U'
_chemical_formula_weight         838.20
_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                 113.433(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7463(11)
_cell_length_b                   12.4261(7)
_cell_length_c                   14.9928(11)
_cell_measurement_reflns_used    9355
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      1.59
_cell_volume                     2178.8(3)
_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, 2015)'
_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 0.967
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      ' 90 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14994
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         1.741
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    12.526
_exptl_absorpt_correction_T_max  0.5485
_exptl_absorpt_correction_T_min  0.1382
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-AREA'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    2.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamina
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.975
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00068(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+10.0919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3622
_reflns_number_total             4344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2017-247-105.cif
_cod_data_source_block           Compound_2_isk218
_cod_database_code               1560616
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C4(H4A,H4B), C6(H6A,H6B)
2.b Tetrahedral OH refined with everything fixed:
 O10(H10)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C2(H2A,H2B,H2C), N2(H2D,H2E,H2F), C3(H3A,H3B,H3C), N3(H3D,
 H3E,H3F), C5(H5A,H5B,H5C)
;