Synthesis and Characterization of the High-Pressure Nickel Borate γ-NiB4O7.
Schmitt, Martin K.; Janka, Oliver; Niehaus, Oliver; Dresselhaus, Thomas; Pöttgen, Rainer; Pielnhofer, Florian; Weihrich, Richard; Krzhizhanovskaya, Maria; Filatov, Stanislav; Bubnova, Rimma; Bayarjargal, Lkhamsuren; Winkler, Björn; Glaum, Robert; Huppertz, Hubert; Inorganic chemistry 56 (2017) 4217–4228; doi:10.1021/acs.inorgchem.7b00243

data_4345610
_publ_section_title
;
 Synthesis and Characterization of the High-Pressure Nickel Borate
 \g-NiB4O7.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4217
_journal_page_last               4228
_journal_paper_doi               10.1021/acs.inorgchem.7b00243
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'B4 Ni O7'
_chemical_formula_sum            'B4 Ni O7'
_chemical_formula_weight         213.95
_chemical_name_common            'Nickel tetraborate'
_chemical_name_systematic        NiB4O7
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   4.256(2)
_cell_length_b                   4.256(2)
_cell_length_c                   34.905(2)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.039
_cell_measurement_theta_min      3.502
_cell_volume                     547.5(4)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    SHELXS-2013/1
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0080
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            27860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.039
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    5.286
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-like
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 207 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.6816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.362
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                790
_reflns_number_total             801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00243_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        547.5(5)
_cod_database_code               4345610
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              31736
_shelx_hkl_checksum              18200