The new high-pressure borate Co7B24O42(OH)2·2H2O—Formation of edge-sharing BO4 tetrahedra in a hydrated borate
Neumair, Stephanie C.; Kaindl, Reinhard; Huppertz, Hubert; Journal of Solid State Chemistry 185 (2012) 1–9; doi:10.1016/j.jssc.2011.10.028

data_1563076
_publ_section_title
;
 The new high-pressure borate Co7B24O42(OH)2&#x00B7;2H2O---Formation of
 edge-sharing BO4 tetrahedra in a hydrated borate
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               9
_journal_paper_doi               10.1016/j.jssc.2011.10.028
_journal_volume                  185
_journal_year                    2012
_chemical_formula_moiety         'B24 Co7 H6 O46'
_chemical_formula_sum            'B24 Co7 H6 O46'
_chemical_formula_weight         1414.00
_chemical_name_common            Cobaltborate
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b a m'
_atom_sites_solution_hydrogens   geom
_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                   8.1895(16)
_cell_length_b                   20.169(4)
_cell_length_c                   7.6988(15)
_cell_measurement_reflns_used    38695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      0.998
_cell_volume                     1271.6(4)
_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 (Brandenburg & Berndt, 1999)'
_computing_publication_material  'enCIFer (Allen et al., 2004) and SHELXL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_radiation_monochromator  'graded multilayer X-ray optics'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17310
_diffrn_reflns_theta_full        34.98
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    4.675
_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            violet
_exptl_crystal_density_diffrn    3.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1366
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.0003(3)
_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   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0273P)^2^+2.7078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                2230
_reflns_number_total             2967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2012-185-1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1271.7(4)
_cod_original_sg_symbol_H-M      Pbam
_cod_database_code               1563076