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_1560618
_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         'H2 O11 Se2 U, C2 H8 N, H3 O'
_chemical_formula_sum            'C2 H13 N O12 Se2 U'
_chemical_formula_weight         639.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                79.559(15)
_cell_angle_beta                 89.272(16)
_cell_angle_gamma                82.356(16)
_cell_formula_units_Z            2
_cell_length_a                   7.5635(15)
_cell_length_b                   7.6188(15)
_cell_length_c                   12.101(2)
_cell_measurement_reflns_used    6709
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      1.71
_cell_volume                     679.6(2)
_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_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.956
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_number            5568
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.711
_exptl_absorpt_coefficient_mu    17.351
_exptl_absorpt_correction_T_max  0.3403
_exptl_absorpt_correction_T_min  0.2037
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-AREA'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    3.123
_exptl_crystal_description       lamina
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.975
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0259P)^2^+0.4551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2552
_reflns_number_total             2874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2017-247-105.cif
_cod_data_source_block           Compound_4_isk218c_pl
_cod_database_code               1560618
_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,H) groups, All O(H,H,H) groups
2.a Riding coordinates:
 O7(H7A,H7B), O11(H11A,H11B,H11C)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;