Hydrothermal synthesis and characterization of the first mixed alkali borate-nitrate K3Na[B6O9(OH)3]NO3
Ortner, Teresa S.; Wurst, Klaus; Perfler, Lukas; Tribus, Martina; Huppertz, Hubert; Journal of Solid State Chemistry 221 (2015) 66–72; doi:10.1016/j.jssc.2014.09.016

data_1562141
_publ_section_title
;
 Hydrothermal synthesis and characterization of the first mixed alkali
 borate-nitrate K3Na[B6O9(OH)3]NO3
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              66
_journal_page_last               72
_journal_paper_doi               10.1016/j.jssc.2014.09.016
_journal_volume                  221
_journal_year                    2015
_chemical_formula_moiety         'B6 H3 O12 (N O3), 3(K), 1(Na)'
_chemical_formula_sum            'B6 H3 K3 N Na O15'
_chemical_formula_weight         462.18
_chemical_name_common            Potassium-sodiumhydroxoborate-nitrate
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      58
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.208(3)
_cell_length_b                   9.1067(18)
_cell_length_c                   12.325(3)
_cell_measurement_reflns_used    23999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.785
_cell_measurement_theta_min      0.998
_cell_volume                     1482.5(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
'DIAMOND Version 3.2i(Brandenburg & Putz, 2012)'
_computing_publication_material
;
enCIFer 1.4 (Allen et al., 2004) and SHELXL-2013 (Sheldrick, 2013)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18303
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.998
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Z. Otwinowski, W. Minor, Vol. 276:
Macromolecular Crystallography A, p.307-326, 1997, Academic Press (New York).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0010(11)
_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   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2898
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+0.4791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                2193
_reflns_number_total             2898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2015-221-66.cif
_cod_data_source_block           E
_cod_original_cell_volume        1482.4(5)
_cod_database_code               1562141