data_KB(OCH3)4

_diffrn_radiation_monochromator   'Double crystal'
_diffrn_radiation_source   'Synchrotron'
_diffrn_measurement_device_type   'Mythen Detector'
_cell_measurement_temperature   298.65
_diffrn_ambient_temperature 298.65
_cell_measurement_reflns_used   187
_diffrn_radiation_wavelength   0.774863(1)
_diffrn_radiation_type   Synchrotron
_exptl_crystal_density_diffrn   1.12762
_exptl_absorpt_coefficient_mu 0.653
_cell_measurement_theta_min 1.5
_cell_measurement_theta_max 12.5
_exptl_crystal_F_000 1280
_cell_formula_units_Z   16
_symmetry_space_group_name_hall   'I 4bw -1bw'
_symmetry_cell_setting   tetragonal
_chemical_formula_weight   174.04
_chemical_formula_iupac   'K[B O (C H3)4]'
_chemical_formula_sum 'C4 H12 B K O4'
_chemical_formula_moiety 'K 1+, C4 H12 B O4 1-'
_publ_section_abstract
;
Research into the use of sodium tetraalkoxyborate salts for different
chemicaluses including synthetic catalysis, hydrogen storage, or battery
applicationshas been investigated, however, understanding of the structural,
thermal and electrochemical properties of these salts has been left in the
1950s and 1960s. A review of the synthesis, as well as a thorough
characterisation using 1H NMR, 11B NMR, 13C{1H} NMR, FTIR, XRD, in situ XRD,
DSC-TGA, RGA-MS, TPPA, and EIS has newly identified polymorphic phase changes
for Na[B(OMe)4], K[B(OMe)4], Li[B(OMe)4], Na[B(OEt)4], Na[B(OBu)4], and
Na[B(OiBu)4]. The newly solved space group for K[B(OMe)4] was identified as
I41/a (a = 22.33 Å, c = 7.649 Å, V = 3815 Å3, ρ = 1.13 g/cm3). Ionic
conductivity of the different salts was analysed, however it was found that
the longer alkyl chains had no measurable ionic conductivity compared to the
shorter chained samples, Na[B(OMe)4] and K[B(OMe)4] with 9.6 x 10-8 S cm-1 and
1.6 x 10-7 S cm-1, at 114 °C respectively.
;
_publ_section_keywords
;
solid-state electrolyte
alkoxyborate
;
_publ_contact_author_name 'Mark Paskevicius'
_publ_contact_author_email
;
mark.paskevicius@gmail.com
;
_publ_section_title
;
Alkali metal alkoxyborate ester salts; a contemporary look at old compounds
;
loop_
_chemical_name_mineral ?KB(OCH3)4?
_cell_length_a 22.337(2)
_cell_length_b 22.337(2)
_cell_length_c 7.648(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3815.6(4)
_symmetry_space_group_name_H-M I41/a
loop_
	_symmetry_equiv_pos_as_xyz
	 'x, y, z '
	 '-x+1/2, -y+1/2, z+1/2 '
	 '-y, x+1/2, z+1/4 '
	 '-y+1/2, x+1/2, -z+1/2 '
	 'y, -x, -z '
	 'y+1/2, -x, z-1/4 '
	 '-x, -y+1/2, -z+1/4 '
	 'x+1/2, y, -z-1/4 '
	 'x+1/2, y+1/2, z+1/2 '
	 '-x, -y, z '
	 '-y+1/2, x, z-1/4 '
	 '-y, x, -z '
	 'y+1/2, -x+1/2, -z+1/2 '
	 'y, -x+1/2, z+1/4 '
	 '-x+1/2, -y, -z-1/4 '
	 'x, y+1/2, -z+1/4 '
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
K1 K+1  16 0.55571	 0.80386  -0.28309 1 1
O1a O   16 -0.10932 -0.40823  -0.81685 1 1
O2a O   16 -0.16096 -0.34596  -0.63916 1 1
O3a O   16 -0.16557 -0.45347  -0.57363 1 1
O4a O   16 -0.21842 -0.42055  -0.80792 1 1
B1a B   16 -0.16349 -0.40716  -0.70913 1 1
C1a C   16 -0.09497 -0.46256  -0.9011  1 1
C2a C   16 -0.20536 -0.3291	  -0.51809 1 1
C3a C   16 -0.12085 -0.452	  -0.44434 1 1
C4a C   16 -0.22437 -0.38783  -0.96439 1 1

loop_
   _geom_bond_atom_site_label_1
   _geom_bond_atom_site_label_2
   _geom_bond_distance
   _geom_bond_site_symmetry_1
   _geom_bond_site_symmetry_2
   _geom_bond_publ_flag
  K1     K1     3.73631      1_555    5_664 yes
  K1     O1a    2.63356      1_555    3_555 yes
  K1     O2a    2.761        1_555    3_555 yes
  K1     O3a    3.11127      1_555   12_655 yes
  K1     O3a    2.62345      1_555   16_453 yes
  K1     O4a    2.88816      1_555   12_655 yes
  O1a    K1     2.63356      1_555    3_554 yes
  O1a    B1a    1.46403      1_555    1_555 yes
  O1a    C1a    1.41091      1_555    1_555 yes
  O2a    K1     2.761        1_555    3_554 yes
  O2a    B1a    1.46912      1_555    1_555 yes
  O2a    C2a    1.40812      1_555    1_555 yes
  O3a    K1     2.62345      1_555    6_443 yes
  O3a    K1     3.11127      1_555   10_534 yes
  O3a    B1a    1.46497      1_555    1_555 yes
  O3a    C3a    1.40593      1_555    1_555 yes
  O4a    K1     2.88816      1_555   10_534 yes
  O4a    B1a    1.47165      1_555    1_555 yes
  O4a    C4a    1.4085       1_555    1_555 yes
  B1a    O1a    1.46403      1_555    1_555 yes
  B1a    O2a    1.46912      1_555    1_555 yes
  B1a    O3a    1.46497      1_555    1_555 yes
  B1a    O4a    1.47165      1_555    1_555 yes
  C1a    O1a    1.41091      1_555    1_555 yes
  C2a    O2a    1.40812      1_555    1_555 yes
  C3a    O3a    1.40593      1_555    1_555 yes
  C4a    O4a    1.4085       1_555    1_555 yes

loop_
   _geom_angle_atom_site_label_1
   _geom_angle_atom_site_label_2
   _geom_angle_atom_site_label_3
   _geom_angle
   _geom_angle_site_symmetry_1
   _geom_angle_site_symmetry_2
   _geom_angle_site_symmetry_3
   _geom_angle_publ_flag
  K1     K1     O1a    146.727       5_664  1_555    3_555 yes
  K1     K1     O2a    159.479       5_664  1_555    3_555 yes
  O1a    K1     O2a    49.489        3_555  1_555    3_555 yes
  K1     K1     O3a    55.292        5_664  1_555   16_564 yes
  O1a    K1     O3a    97.15         3_555  1_555   16_564 yes
  O2a    K1     O3a    144.996       3_555  1_555   16_564 yes
  K1     O1a    B1a    107.829       3_554  1_555    1_555 yes
  K1     O1a    C1a    134.659       3_554  1_555    1_555 yes
  B1a    O1a    C1a    117.309       1_555  1_555    1_555 yes
  K1     O2a    B1a    101.798       3_554  1_555    1_555 yes
  K1     O2a    C2a    140.426       3_554  1_555    1_555 yes
  B1a    O2a    C2a    117.471       1_555  1_555    1_555 yes
  K1     O3a    B1a    109.114       6_554  1_555    1_555 yes
  K1     O3a    C3a    119.936       6_554  1_555    1_555 yes
  B1a    O3a    C3a    117.29        1_555  1_555    1_555 yes
  B1a    O4a    C4a    114.167       1_555  1_555    1_555 yes
  O1a    B1a    O2a    100.858       1_555  1_555    1_555 yes
  O1a    B1a    O3a    114.378       1_555  1_555    1_555 yes
  O2a    B1a    O3a    113.615       1_555  1_555    1_555 yes
  O1a    B1a    O4a    113.381       1_555  1_555    1_555 yes
  O2a    B1a    O4a    114.091       1_555  1_555    1_555 yes
  O3a    B1a    O4a    101.141       1_555  1_555    1_555 yes

