Analysis of Phase Transition Pathways in X3H(SO4)2 (X = Rb, NH4, K, Na): Variable Temperature Single-Crystal X-ray Diffraction Studies#
Diptikanta Swain; Tayur N. Guru Row; Inorganic Chemistry 46 (2007) 4411–4421; doi:10.1021/ic061901x

data_4307408
_publ_contact_author_address
;
Solid State and Structural Chemistry Unit
Indian Institute of Science
Bangalore 560 012. Karnataka.
INDIA.
;
_publ_contact_author_email       ssctng@sscu.iisc.ernet.in
_publ_contact_author_fax         '(91)803601310 '
_publ_contact_author_name
;
 'Prof. T. N. Guru Row'
;
_publ_contact_author_phone       (91)802932796
_publ_section_title
;
Analysis of Phase Transition Pathways in X3H(SO4)2 (X = Rb, NH4, K, Na):
Variable Temperature Single-Crystal X-ray Diffraction Studies#
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4411
_journal_page_last               4421
_journal_paper_doi               10.1021/ic061901x
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'see text'
_chemical_formula_moiety         'H O8 Rb3 S2'
_chemical_formula_sum            'H O8 Rb3 S2'
_chemical_formula_weight         449.54
_chemical_name_systematic
; 
 Trirubidium Hydrogen bisulfate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 114.577(7)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   20.480(10)
_cell_length_b                   11.815(6)
_cell_length_c                   16.387(8)
_cell_measurement_reflns_used    5250
_cell_measurement_temperature    425(2)
_cell_measurement_theta_max      28.4646
_cell_measurement_theta_min      0.9333
_cell_volume                     3606(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Farrugia, 1999)'
_computing_publication_material
'WinGx (Farrugia, 1999) and PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      425(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17400
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    16.694
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.155
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.305
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.579
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.691
_refine_ls_extinction_coef       0.0025(5)
_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   1.321
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.1169
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4349
_refine_ls_wR_factor_ref         0.4728
_reflns_number_gt                1179
_reflns_number_total             3316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061901x-file011.cif
_cod_data_source_block           data152m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4307408