Latent Porosity in Potassium Dodecafluoro-closo-dodecaborate(2-). Structures and Rapid Room Temperature Interconversions of Crystalline K2B12F12, K2(H2O)2B12F12, and K2(H2O)4B12F12 in the Presence of Water Vapor
Dmitry V. Peryshkov; Alexey A. Popov; Steven H. Strauss; Journal of the American Chemical Society 132 (2010) 13902–13913; doi:10.1021/ja105522d

data_4103153
_publ_contact_author_address
;
Colorado State University
Fort Collins
Colorado
80523
USA
;
_publ_contact_author_email       steven.strauss@colostate.edu
_publ_contact_author_fax         +1-(970)-491-1801
_publ_contact_author_name        'S.H. Strauss'
_publ_contact_author_phone       +1-(970)-491-5104
_publ_section_title
;
 Latent Porosity in Potassium Dodecafluoro-closo-dodecaborate(2-).
 Structures and Rapid Room Temperature Interconversions of Crystalline
 K2B12F12, K2(H2O)2B12F12, and K2(H2O)4B12F12 in the Presence of Water
 Vapor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13902
_journal_page_last               13913
_journal_paper_doi               10.1021/ja105522d
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'B12 F12, 2(H2 O), 2(K)'
_chemical_formula_sum            'B12 F12 H4 K2 O2'
_chemical_formula_weight         471.95
_chemical_name_common
'potassium dodecafluoro-closo-dodecaborate(2-) dihydrate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.7300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2955(2)
_cell_length_b                   11.2522(3)
_cell_length_c                   9.2269(2)
_cell_measurement_reflns_used    9461
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      35.06
_cell_measurement_theta_min      2.87
_cell_volume                     735.80(3)
_computing_cell_refinement       'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_data_collection       'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_data_reduction        'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_molecular_graphics    'SHELXTL, v. 6.12 UNIX, Bruker AXS'
_computing_publication_material  'SHELXTL, v. 6.12 UNIX, Bruker AXS'
_computing_structure_refinement  'SHELXTL, v. 6.12 UNIX, Bruker AXS'
_computing_structure_solution    'SHELXTL, v. 6.12 UNIX, Bruker AXS'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX2 diffractometer'
_diffrn_measurement_method       'omega and phi 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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0100
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33744
_diffrn_reflns_theta_full        35.06
_diffrn_reflns_theta_max         35.06
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Sheldrick, G. M., SADABS, v. 2.10, Bruker AXS, Madison, WI

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.552
_exptl_crystal_size_mid          0.547
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0307P)^2^+0.1304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                3093
_reflns_number_total             3259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105522d_si_002.cif
_cod_data_source_block           ss232
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4103153