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_4307399
_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         '3(H4.02 N), 6(H3 O4 S), H9.06 N6 '
_chemical_formula_sum            'H13 N3 O8 S2'
_chemical_formula_weight         237.31
_chemical_name_systematic        ' ?'
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      166
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   5.9061(4)
_cell_length_b                   5.9061(4)
_cell_length_c                   22.608(3)
_cell_measurement_reflns_used    568
_cell_measurement_temperature    420(2)
_cell_measurement_theta_max      27.568
_cell_measurement_theta_min      0.8569
_cell_volume                     682.96(11)
_computing_cell_refinement       'Bruker SMART V5.628, (Bruker, 2004)'
_computing_data_collection       'Bruker SMART V5.628, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT V6.45a, (Bruker, 2004)'
_computing_molecular_graphics
'DIAMOND. version 2.1c (Brandenburg, K. 1999)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL V6.14 (Bruker, 2000)'
_diffrn_ambient_temperature      420(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0089
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            2360
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.9139
_exptl_absorpt_correction_T_min  0.8622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0856P)^2^+1.8921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                208
_reflns_number_total             224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061901x-file002.cif
_cod_data_source_block           nh43hs350m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 

2017-09-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'H39.12 N9 O24 S6'
_cod_original_formula_weight         741.94
_cod_original_formula_moiety         '3(H4.02 N), 6(H3 O4 S), H9.06 N6 '
_cod_original_formula_units_Z            1
_cod_original_cell_volume        682.94(12)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4307399