Chiral anionic layers in tartramide spiroborate salts and variable solvation for [N<i>R</i>~4~][B(TarNH~2~)~2~] (<i>R</i> = Et, Pr or Bu)
Soecipto, Aristyo; Wong, Lawrence W.-Y.; Sung, Herman H.-Y.; Williams, Ian D.; Acta Crystallographica Section C 76 (2020) 695–705; doi:10.1107/S2053229620008384

data_2022221
_publ_section_title
;
 Chiral anionic layers in tartramide spiroborate salts and variable
 solvation for [N<i>R</i>~4~][B(TarNH~2~)~2~] (<i>R</i> = Et, Pr or Bu)
;
_journal_coeditor_code           FM3065
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              695
_journal_page_last               705
_journal_paper_doi               10.1107/S2053229620008384
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C15 H27 N2 +, C8 H12 B N4 O8 -, C2 H6 O'
_chemical_formula_moiety         'C15 H27 N2 +, C8 H12 B N4 O8 -, C2 H6 O'
_chemical_formula_sum            'C25 H45 B N6 O9'
_chemical_formula_weight         584.48
_chemical_name_common
;
Sparteinium spiroborate ethanol monosolvate
;
_chemical_name_systematic
;
7-Aza-15-azoniatetracyclo[7.7.1.0^2,7^.0^10,15^]heptadecane
2,3,7,8-tetracarboxamido-1,4,6,9-tetraoxa-5\l^4^-boraspiro[4.4]nonane
ethanol monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.41666(15)
_cell_length_b                   15.3809(2)
_cell_length_c                   18.0053(3)
_cell_measurement_reflns_used    12885
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.3980
_cell_measurement_theta_min      3.7490
_cell_volume                     2884.77(7)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19437
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.780
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.168
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2133 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0408P)^2^+0.3459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                4990
_reflns_number_total             5201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fm3065sup1.cif
_cod_data_source_block           aris52cult
_cod_original_cell_volume        2884.76(7)
_cod_database_code               2022221
_cod_database_fobs_code          2022221
_shelx_hkl_checksum              87462
_shelx_res_checksum              23504