Accelerated aging: a low energy, solvent-free alternative to solvothermal and mechanochemical synthesis of metal–organic materials
Cliffe, Matthew J.; Mottillo, Cristina; Stein, Robin S.; Bučar, Dejan-Krešimir; Friščić, Tomislav; Chemical Science 3 (2012) 2495–; doi:10.1039/c2sc20344h

data_1556346
_publ_section_title
;
 Accelerated aging: a low energy, solvent-free alternative to solvothermal
 and mechanochemical synthesis of metal--organic materials
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2495
_journal_paper_doi               10.1039/c2sc20344h
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety         '2(C3 H5 N2), S O4, 2(H2 O)'
_chemical_formula_sum            'C6 H14 N4 O6 S'
_chemical_formula_weight         270.27
_chemical_name_common            (H2im)2SO4.2H2O
_chemical_name_systematic
;
IMIDAZOLIUM SULFATE DIHYDRATE
;
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9553(6)
_cell_length_b                   7.9553(6)
_cell_length_c                   18.7605(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1187.29(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13642
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(9)
_refine_ls_extinction_coef       0.141(6)
_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   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.2289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                1373
_reflns_number_total             1440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20344h.txt
_cod_data_source_block           cm1
_cod_original_sg_symbol_H-M      P41212
_cod_database_code               1556346