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_2022219
_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          'C8 H20 N +, C8 H12 B N4 O8 -, 6.375H2 O'
_chemical_formula_moiety         'C8 H20 N +, C8 H12 B N4 O8 -, 6.375(H2 O)'
_chemical_formula_sum            'C16 H44.75 B N5 O14.375'
_chemical_formula_weight         548.125
_chemical_name_systematic
;
Tetraethylazanium
2,3,7,8-tetracarboxamido-1,4,6,9-tetraoxa-5\l^4^-boraspiro[4.4]nonane
6.375-hydrate
;
_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     iterative
_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            8
_cell_length_a                   10.40272(13)
_cell_length_b                   17.5277(3)
_cell_length_c                   30.9259(4)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1940
_cell_measurement_theta_min      4.9320
_cell_volume                     5638.90(14)
_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
;
olex2.solve (Bourhis <i>et al.</i>, 2015)
;
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.959
_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  0.0199
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17424
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.689
_diffrn_reflns_theta_min         4.484
_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    0.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             2366
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.207
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4250 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         11082
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0424P)^2^+0.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                10345
_reflns_number_total             11082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fm3065sup1.cif
_cod_data_source_block           aris40cult
_cod_original_cell_volume        5638.90(13)
_cod_original_formula_sum        'C16 H44.75 B1 N5 O14.375'
_cod_database_code               2022219
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.954
_shelx_hkl_checksum              89634
_shelx_res_checksum              99199
_cod_database_fobs_code 2022219