# Electronic Supplementary Material (ESI) for Green Chemistry.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_grela_1
_database_code_depnum_ccdc_archive 'CCDC 2089072'
loop_
_audit_author_name
_audit_author_address
'Oksana Danylyuk'
;Institute of Physical Chemistry, Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2021-06-09 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        'Ammonium pentaborate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'N H4 [B5 O10 H4], 2(H2 O)'
_chemical_formula_sum            'H12 B5 N O12'
_chemical_formula_weight         272.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   11.3246(3)
_cell_length_b                   11.0147(3)
_cell_length_c                   9.1513(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1141.51(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    1531
_cell_measurement_theta_min      3.3940
_cell_measurement_theta_max      29.4580

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.158
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_reflns_number            2278
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.408
_diffrn_reflns_theta_max         30.096
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.762
_diffrn_reflns_point_group_measured_fraction_full 0.892
_reflns_number_total             1271
_reflns_number_gt                1217
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.593
_reflns_Friedel_fraction_max     0.603
_reflns_Friedel_fraction_full    0.769

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0411P)²+0.1907P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.2(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1271
_refine_ls_number_parameters     97
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0748
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.97253(12) 0.82333(13) 0.45156(18) 0.0158(3) Uani 1 1 d D . . . .
H1W1 H 0.998(2) 0.752(2) 0.434(3) 0.024 Uiso 1 1 d D U . . .
H2W1 H 1.004(2) 0.846(3) 0.530(3) 0.024 Uiso 1 1 d D U . . .
N1 N 0.0000 1.0000 0.2089(3) 0.0155(5) Uani 1 2 d DS T P . .
H1N1 H 0.028(2) 1.053(2) 0.265(3) 0.023 Uiso 1 1 d D U . . .
H2N1 H -0.057(2) 1.030(2) 0.159(3) 0.023 Uiso 1 1 d D U . . .
B2 B 0.5000 1.0000 0.2929(4) 0.0117(6) Uani 1 2 d S T P . .
O4 O 0.41794(12) 0.93195(12) 0.19822(16) 0.0131(3) Uani 1 1 d . . . . .
O3 O 0.56333(12) 0.91268(12) 0.38719(17) 0.0132(3) Uani 1 1 d . . . . .
O2 O 0.73656(12) 0.82123(13) 0.47804(18) 0.0187(4) Uani 1 1 d . . . . .
H2 H 0.8100 0.8251 0.4663 0.028 Uiso 1 1 calc R U . . .
O1 O 0.75314(14) 0.97019(13) 0.29580(18) 0.0159(3) Uani 1 1 d . . . . .
O5 O 0.22257(13) 0.88826(15) 0.11291(19) 0.0235(4) Uani 1 1 d . . . . .
H5 H 0.2586 0.8333 0.0675 0.035 Uiso 1 1 calc R U . . .
B1 B 0.68266(19) 0.90197(19) 0.3874(3) 0.0131(4) Uani 1 1 d . . . . .
B3 B 0.2993(2) 0.94789(19) 0.2015(3) 0.0146(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1W 0.0145(7) 0.0145(6) 0.0185(7) -0.0022(6) -0.0037(6) 0.0028(6)
N1 0.0107(12) 0.0207(12) 0.0152(12) 0.000 0.000 -0.0001(10)
B2 0.0088(13) 0.0134(13) 0.0128(13) 0.000 0.000 0.0009(11)
O4 0.0093(7) 0.0158(6) 0.0140(7) -0.0040(6) 0.0001(6) 0.0007(5)
O3 0.0105(6) 0.0136(6) 0.0155(7) 0.0037(5) 0.0001(6) 0.0006(5)
O2 0.0116(6) 0.0192(7) 0.0253(9) 0.0108(6) -0.0008(6) -0.0002(6)
O1 0.0098(6) 0.0174(6) 0.0206(7) 0.0090(6) 0.0010(6) 0.0008(5)
O5 0.0120(8) 0.0277(8) 0.0307(10) -0.0186(7) -0.0035(6) 0.0031(6)
B1 0.0133(10) 0.0118(9) 0.0142(10) 0.0012(8) -0.0008(10) -0.0013(8)
B3 0.0132(10) 0.0150(10) 0.0158(10) -0.0023(9) -0.0002(9) 0.0003(8)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B2 O4 1.475(2) 2_675 ?
B2 O4 1.475(2) . ?
B2 O3 1.478(2) . ?
B2 O3 1.478(2) 2_675 ?
O4 B3 1.355(3) . ?
O3 B1 1.356(3) . ?
O2 B1 1.361(3) . ?
O1 B1 1.380(3) . ?
O1 B3 1.383(3) 2_675 ?
O5 B3 1.358(3) . ?
B3 O1 1.383(3) 2_675 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 B2 O4 108.1(2) 2_675 . ?
O4 B2 O3 111.59(7) 2_675 . ?
O4 B2 O3 108.54(8) . . ?
O4 B2 O3 108.54(8) 2_675 2_675 ?
O4 B2 O3 111.59(7) . 2_675 ?
O3 B2 O3 108.5(2) . 2_675 ?
B3 O4 B2 123.07(15) . . ?
B1 O3 B2 122.75(15) . . ?
B1 O1 B3 119.07(17) . 2_675 ?
O3 B1 O2 120.32(18) . . ?
O3 B1 O1 121.85(19) . . ?
O2 B1 O1 117.82(18) . . ?
O4 B3 O5 123.96(19) . . ?
O4 B3 O1 121.64(19) . 2_675 ?
O5 B3 O1 114.39(18) . 2_675 ?

_refine_diff_density_max         0.181
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.052

_shelxl_version_number           2013-3

_shelx_res_file                  
;
TITL GRELA_1 in Aea2
CELL  0.71073  11.3246  11.0147   9.1513   90.000   90.000   90.000
ZERR     4.00   0.0003   0.0003   0.0003    0.000    0.000    0.000
LATT  -5
SYMM  - X, - Y,   Z
SYMM  1/2 + X, 1/2 - Y,   Z
SYMM  1/2 - X, 1/2 + Y,   Z
SFAC  B    N    O    H
UNIT  20   4    48   48
MERG   2
OMIT    -3.00 180.00
dfix 0.85 o1w h1w1 o1w h2w1 n1 h1n1 n1 h2n1
FMAP   2
PLAN   20
ACTA
BOND
L.S.   20
TEMP  -173.00
size 0.25 0.17 0.12
WGHT    0.041100    0.190700
FVAR       5.22661
mole 1
O1W   3    0.972535    0.823325    0.451555    11.00000    0.01450    0.01449 =
         0.01848   -0.00221   -0.00366    0.00279
H1W1  4    0.997937    0.752040    0.433991    11.00000   -1.50000
H2W1  4    1.003624    0.845532    0.529684    11.00000   -1.50000
mole 2

N1    2    0.000000    1.000000    0.208887    10.50000    0.01074    0.02070 =
         0.01520    0.00000    0.00000   -0.00012
H1N1  4    0.027900    1.053470    0.265272    11.00000   -1.50000
H2N1  4   -0.056655    1.029844    0.158858    11.00000   -1.50000
mole 3
B2    1    0.500000    1.000000    0.292884    10.50000    0.00884    0.01336 =
         0.01277    0.00000    0.00000    0.00091
O4    3    0.417936    0.931947    0.198216    11.00000    0.00932    0.01579 =
         0.01405   -0.00403    0.00006    0.00071
O3    3    0.563330    0.912684    0.387195    11.00000    0.01053    0.01357 =
         0.01546    0.00373    0.00007    0.00058
O2    3    0.736565    0.821234    0.478038    11.00000    0.01158    0.01917 =
         0.02525    0.01078   -0.00076   -0.00018
AFIX 147
H2    4    0.810033    0.825095    0.466287    11.00000   -1.50000
AFIX   0

O1    3    0.753136    0.970191    0.295797    11.00000    0.00981    0.01739 =
         0.02065    0.00904    0.00098    0.00076
O5    3    0.222573    0.888261    0.112913    11.00000    0.01196    0.02773 =
         0.03070   -0.01857   -0.00347    0.00309
AFIX 147
H5    4    0.258563    0.833267    0.067520    11.00000   -1.50000
AFIX   0
B1    1    0.682656    0.901966    0.387427    11.00000    0.01327    0.01181 =
         0.01418    0.00125   -0.00079   -0.00131
B3    1    0.299347    0.947893    0.201499    11.00000    0.01315    0.01496 =
         0.01579   -0.00234   -0.00021    0.00028
HKLF    4

REM  GRELA_1 in Aea2
REM R1 =  0.0297 for    1217 Fo > 4sig(Fo)  and  0.0314 for all    1271 data
REM     97 parameters refined using      5 restraints

END

WGHT      0.0384      0.1919

REM Highest difference peak  0.181,  deepest hole -0.222,  1-sigma level  0.052
Q1    1   0.8284  0.8134  0.2197  11.00000  0.05    0.18
Q2    1   0.0644  1.1310  0.1182  11.00000  0.05    0.17
Q3    1   0.8656  0.8512  0.6191  11.00000  0.05    0.17
Q4    1   0.6236  0.8137  0.1990  11.00000  0.05    0.17
Q5    1   0.3628  0.9648  0.1659  11.00000  0.05    0.16
Q6    1   1.0940  0.8056  0.3070  11.00000  0.05    0.16
Q7    1   0.9041  0.8222  0.4220  11.00000  0.05    0.16
Q8    1   0.2092  0.8293  0.1839  11.00000  0.05    0.15
Q9    1   0.0864  1.1888  0.2241  11.00000  0.05    0.14
Q10   1   0.4307  0.8517  0.2225  11.00000  0.05    0.14
Q11   1   0.1299  0.8451 -0.0476  11.00000  0.05    0.14
Q12   1   0.3608  0.9133  0.2427  11.00000  0.05    0.14
Q13   1   1.0912  0.6706  0.5407  11.00000  0.05    0.13
Q14   1   0.8443  0.6694  0.3663  11.00000  0.05    0.13
Q15   1   0.5626  0.8449  0.2724  11.00000  0.05    0.13
Q16   1   0.9567  0.7178  0.2971  11.00000  0.05    0.13
Q17   1   0.2763  0.7622  0.2170  11.00000  0.05    0.13
Q18   1   0.1613  0.8310  0.3161  11.00000  0.05    0.13
Q19   1   0.0195  1.2166  0.2004  11.00000  0.05    0.13
Q20   1   0.6095  0.8643  0.3480  11.00000  0.05    0.12
;
_shelx_res_checksum              42198
