Solution Phase Mass Synthesis of 2D Atomic Layer with Hexagonal Boron Network.
Kambe, Tetsuya; Hosono, Reina; Imaoka, Shotaro; Kuzume, Akiyoshi; Yamamoto, Kimihisa; Journal of the American Chemical Society 141 (2019) 12984–12988; doi:10.1021/jacs.9b06110

data_4127852
_publ_section_title
;
 Solution Phase Mass Synthesis of 2D Atomic Layer with Hexagonal Boron
 Network.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12984
_journal_page_last               12988
_journal_paper_doi               10.1021/jacs.9b06110
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'B4.27 K O3'
_chemical_formula_sum            'B4.27 K O3'
_chemical_formula_weight         133.26
_space_group_crystal_system      hexagonal
_space_group_IT_number           189
_space_group_name_Hall           'P -6 -2'
_space_group_name_H-M_alt        'P -6 2 m'
_symmetry_space_group_name_Hall  'P -6 -2'
_symmetry_space_group_name_H-M   'P -6 2 m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            1
_cell_length_a                   6.0720(6)
_cell_length_b                   6.0720(6)
_cell_length_c                   3.4690(3)
_cell_measurement_reflns_used    188
_cell_measurement_temperature    100
_cell_measurement_theta_max      75.79
_cell_measurement_theta_min      12.78
_cell_volume                     110.764(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 5.0rc6'
_computing_publication_material  'CrystalStructure 5.0rc6 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            238
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        67.590
_diffrn_reflns_theta_max         67.590
_diffrn_reflns_theta_min         8.430
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.486
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             64.35
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.68
_refine_ls_abs_structure_details
;
 Flack x determined using 17 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_number_parameters     15
_refine_ls_number_reflns         78
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0992
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1806P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.279
_reflns_Friedel_fraction_full    0.486
_reflns_Friedel_fraction_max     0.486
_reflns_number_gt                78
_reflns_number_total             78
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9b06110_si_002.cif
_cod_data_source_block           xcalibur
_cod_database_code               4127852
_shelx_res_checksum              25648
_shelx_hkl_checksum              63661