Synthesis and crystal structure of Ba26B12Si5N27 containing [Si2] dumbbells
Takayuki, Hashimoto; Yamane, Hisanori; Becker, Nils; Dronskowski, Richard; Journal of Solid State Chemistry 230 (2015) 390–396; doi:10.1016/j.jssc.2015.07.022

data_1561813
_publ_section_title
;
 Synthesis and crystal structure of Ba26B12Si5N27 containing [Si2]
 dumbbells
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              390
_journal_page_last               396
_journal_paper_doi               10.1016/j.jssc.2015.07.022
_journal_volume                  230
_journal_year                    2015
_chemical_formula_moiety
;
B8 N16, B16 N32, 16(B N2), B8
N16, 1.25(Si16),
6.000(N2), 104(Ba)
;
_chemical_formula_structural     Ba26N3(Si5)(BN2)12
_chemical_formula_sum            'B12 Ba26 N27 Si5'
_chemical_formula_weight         4219.28
_chemical_name_systematic
;
tridecabarium hexaboron tetrasilicon tetradecanitrogen
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6942(4)
_cell_length_b                   34.1437(6)
_cell_length_c                   10.04098(18)
_cell_measurement_reflns_used    23077
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.315
_cell_volume                     6066.2(2)
_computing_cell_refinement       'RAPID-AUTO (Rigaku/MSC, 2005)'
_computing_data_collection       'RAPID-AUTO (Rigaku/MSC, 2005)'
_computing_data_reduction        'RAPID-AUTO (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2008)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24017
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         3.317
_exptl_absorpt_coefficient_mu    16.686
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             7100
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 1543 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3466
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+46.5292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0382
_refine_ls_wR_factor_ref         0.0384
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3391
_reflns_number_total             3466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2015-230-390.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               1561813
_exptl_absorpt_special_details
; 
The crystal was sealed in a glass capirary with Ar gas. 
;
_shelx_res_checksum              8926
_shelx_hkl_checksum              70184