Comparison of the Coordination of B12F12(2-), B12Cl12(2-), and B12H12(2-) to Na(+) in the Solid State: Crystal Structures and Thermal Behavior of Na2(B12F12), Na2(H2O)4(B12F12), Na2(B12Cl12), and Na2(H2O)6(B12Cl12).
Bukovsky, Eric V.; Peryshkov, Dmitry V.; Wu, Hui; Zhou, Wei; Tang, Wan Si; Jones, W. Matthew; Stavila, Vitalie; Udovic, Terrence J.; Strauss, Steven H.; Inorganic chemistry 56 (2017) 4369–4379; doi:10.1021/acs.inorgchem.6b02920

data_4345773
_publ_section_title
;
 Comparison of the Coordination of B12F12(2-), B12Cl12(2-), and B12H12(2-)
 to Na(+) in the Solid State: Crystal Structures and Thermal Behavior of
 Na2(B12F12), Na2(H2O)4(B12F12), Na2(B12Cl12), and Na2(H2O)6(B12Cl12).
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4369
_journal_page_last               4379
_journal_paper_doi               10.1021/acs.inorgchem.6b02920
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'B12 F12, 4(H2 O), 2(Na)'
_chemical_formula_sum            'B12 F12 H8 Na2 O4'
_chemical_formula_weight         475.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                96.813(3)
_cell_angle_beta                 96.479(3)
_cell_angle_gamma                91.347(4)
_cell_formula_units_Z            4
_cell_length_a                   10.6491(10)
_cell_length_b                   10.8501(10)
_cell_length_c                   13.8432(11)
_cell_measurement_reflns_used    4997
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      4.61
_cell_volume                     1577.0(2)
_computing_cell_refinement       'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_data_collection       'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_data_reduction        'APEX2, v. 2.0-2, Bruker AXS, 2006'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'APEX2, v. 2.0-2, Bruker AXS, 2006'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker Kappa APEX2 diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34246
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_min         1.892
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.7234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Sheldrick, G. M., SADABS, v. 2.10, Bruker AXS, Madison, WI

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         6672
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1005P)^2^+2.5025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3591
_reflns_number_total             6672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02920_si_005.cif
_cod_data_source_block           ss300
_cod_database_code               4345773
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              94191
_shelx_hkl_checksum              71931