12-Membered borophosphate rings in KNi~5~[P~6~B~6~O~23~(OH)~13~]
Yakubovich, Olga V.; Steele, Ian M.; Massa, Werner; Dimitrova, Olga V.; Acta Crystallographica Section C 65 (2009) i94–i98; doi:10.1107/S0108270109044217

data_2017431
_publ_section_title
;
 12-Membered borophosphate rings in KNi~5~[P~6~B~6~O~23~(OH)~13~]
;
_journal_coeditor_code           FN3039
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i94
_journal_page_last               i98
_journal_paper_doi               10.1107/S0108270109044217
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'K Ni5 [P6 B6 O23 (O H)13]'
_chemical_formula_moiety         'B12 H26 Ni10 O72 P12, 2(K)'
_chemical_formula_sum            'B12 H26 K2 Ni10 O72 P12'
_chemical_formula_weight         2344.67
_chemical_name_common            'Borophosphate hydroxide'
_chemical_name_systematic
;
Potassium pentanickel hexaborophosphate tridecahydroxide
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.467(2)
_cell_length_b                   13.467(2)
_cell_length_c                   13.467(2)
_cell_measurement_reflns_used    1017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.734
_cell_measurement_theta_min      2.620
_cell_volume                     2442.4(6)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27118
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    4.517
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    3.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.575
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1012
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0217P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                821
_reflns_number_total             1012
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3039.cif
_cod_data_source_block           I
_cod_original_cell_volume        2442.3(6)
_cod_database_code               2017431
_cod_database_fobs_code          2017431