#------------------------------------------------------------------------------
#$Date: 2021-09-06 15:06:12 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268877 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/01/7060196.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7060196
loop_
_publ_author_name
'Schopper, Nils'
'Sprenger, Jan A. P.'
'Zapf, Ludwig'
'Reiss, Guido J.'
'Ignat’ev, Nikolai V.'
'Finze, Maik'
_publ_section_title
;
 Alkoxycyanoborates: metal salts and low-viscosity ionic liquids
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14973
_journal_page_last               14987
_journal_paper_doi               10.1039/D0NJ04950F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C4 H5 B N3 Na O2'
_chemical_formula_sum            'C4 H5 B N3 Na O2'
_chemical_formula_weight         160.91
_chemical_name_systematic
; 
poly[m₂-aqua-(m₃-methoxy-tricyanoborato-k³N:N':N'')sodium(I)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-22 deposited with the CCDC.	2020-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.478(4)
_cell_angle_beta                 101.298(4)
_cell_angle_gamma                97.248(4)
_cell_formula_units_Z            2
_cell_length_a                   6.2298(3)
_cell_length_b                   8.0256(4)
_cell_length_c                   8.9101(4)
_cell_measurement_reflns_used    5564
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      32.1651
_cell_measurement_theta_min      3.3883
_cell_volume                     413.44(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    direct
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7746
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        29.994
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         4.136
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             164
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.332(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0300
_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/[σ²(Fo²)+(0.0160P)²+0.1000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2050
_reflns_number_total             2413
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj04950f2.cif
_cod_data_source_block           exp_166
_cod_depositor_comments
'Adding full bibliography for 7060196--7060200.cif.'
_cod_database_code               7060196
_shelx_shelxl_version_number     2018/3
_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'
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
Na Na 0.29065(6) 0.11164(5) 0.60816(4) 0.03358(12) Uani 1 1 d . . . . .
C1 C 0.31690(15) 0.14710(12) 0.26567(11) 0.03108(19) Uani 1 1 d . . . . .
C2 C 0.33092(17) 0.47442(13) 0.26640(12) 0.0353(2) Uani 1 1 d . . . . .
C3 C 0.19856(16) 0.22206(12) -0.00134(11) 0.0346(2) Uani 1 1 d . . . . .
C4 C -0.1836(2) 0.3388(2) 0.1256(2) 0.0724(5) Uani 1 1 d . . . . .
H4A H -0.324642 0.318547 0.152312 0.109 Uiso 0.65 1 calc R U P . .
H4B H -0.202147 0.288248 0.012222 0.109 Uiso 0.65 1 calc R U P . .
H4C H -0.128390 0.463204 0.155120 0.109 Uiso 0.65 1 calc R U P . .
H4D H -0.112144 0.394786 0.060790 0.109 Uiso 0.35 1 calc R U P . .
H4E H -0.234639 0.425085 0.200881 0.109 Uiso 0.35 1 calc R U P . .
H4F H -0.308396 0.250128 0.057983 0.109 Uiso 0.35 1 calc R U P . .
B1 B 0.18957(16) 0.27544(13) 0.18457(12) 0.02752(19) Uani 1 1 d . . . . .
N1 N 0.40534(15) 0.05652(12) 0.32405(11) 0.0424(2) Uani 1 1 d . . . . .
N2 N 0.42512(19) 0.61502(13) 0.32363(13) 0.0550(3) Uani 1 1 d . . . . .
N3 N 0.20768(18) 0.18659(14) -0.13179(11) 0.0525(3) Uani 1 1 d . . . . .
O1 O -0.03022(11) 0.26010(10) 0.20946(9) 0.04067(19) Uani 1 1 d . . . . .
O2 O -0.05805(13) 0.18443(11) 0.49053(10) 0.04134(19) Uani 1 1 d . . . . .
H1 H -0.068(2) 0.215(2) 0.404(2) 0.067(4) Uiso 1 1 d . . . . .
H2 H -0.124(3) 0.244(2) 0.543(2) 0.085(6) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N3 Na O2 90.63(4) 1_556 . ?
N3 Na O2 95.66(4) 1_556 2_556 ?
O2 Na O2 80.97(3) . 2_556 ?
N3 Na N2 93.58(4) 1_556 2_666 ?
O2 Na N2 105.22(4) . 2_666 ?
O2 Na N2 168.83(4) 2_556 2_666 ?
N3 Na N1 96.44(3) 1_556 2_656 ?
O2 Na N1 162.54(3) . 2_656 ?
O2 Na N1 82.46(3) 2_556 2_656 ?
N2 Na N1 90.30(4) 2_666 2_656 ?
N3 Na N1 174.94(4) 1_556 . ?
O2 Na N1 89.92(3) . . ?
O2 Na N1 89.39(3) 2_556 . ?
N2 Na N1 81.42(3) 2_666 . ?
N1 Na N1 84.44(3) 2_656 . ?
N3 Na Na 94.15(3) 1_556 2_556 ?
O2 Na Na 40.73(2) . 2_556 ?
O2 Na Na 40.24(2) 2_556 2_556 ?
N2 Na Na 145.08(3) 2_666 2_556 ?
N1 Na Na 122.49(3) 2_656 2_556 ?
N1 Na Na 89.55(2) . 2_556 ?
N3 Na Na 140.13(3) 1_556 2_656 ?
O2 Na Na 128.44(3) . 2_656 ?
O2 Na Na 84.66(2) 2_556 2_656 ?
N2 Na Na 84.23(3) 2_666 2_656 ?
N1 Na Na 43.93(2) 2_656 2_656 ?
N1 Na Na 40.51(2) . 2_656 ?
Na Na Na 110.187(19) 2_556 2_656 ?
N1 C1 B1 179.26(10) . . ?
N2 C2 B1 178.36(11) . . ?
N3 C3 B1 178.90(11) . . ?
O1 C4 H4A 109.5 . . ?
O1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C4 H4D 109.5 . . ?
H4A C4 H4D 141.1 . . ?
H4B C4 H4D 56.3 . . ?
H4C C4 H4D 56.3 . . ?
O1 C4 H4E 109.5 . . ?
H4A C4 H4E 56.3 . . ?
H4B C4 H4E 141.1 . . ?
H4C C4 H4E 56.3 . . ?
H4D C4 H4E 109.5 . . ?
O1 C4 H4F 109.5 . . ?
H4A C4 H4F 56.3 . . ?
H4B C4 H4F 56.3 . . ?
H4C C4 H4F 141.1 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
O1 B1 C1 108.31(7) . . ?
O1 B1 C3 114.19(8) . . ?
C1 B1 C3 107.61(7) . . ?
O1 B1 C2 111.97(8) . . ?
C1 B1 C2 108.09(7) . . ?
C3 B1 C2 106.44(7) . . ?
C1 N1 Na 157.18(8) . 2_656 ?
C1 N1 Na 103.83(7) . . ?
Na N1 Na 95.56(3) 2_656 . ?
C2 N2 Na 161.68(10) . 2_666 ?
C3 N3 Na 170.60(10) . 1_554 ?
C4 O1 B1 117.78(8) . . ?
Na O2 Na 99.03(3) . 2_556 ?
Na O2 H1 118.8(10) . . ?
Na O2 H1 102.1(10) 2_556 . ?
Na O2 H2 122.1(13) . . ?
Na O2 H2 105.5(13) 2_556 . ?
H1 O2 H2 106.1(15) . . ?
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
Na N3 2.4087(10) 1_556 ?
Na O2 2.4318(9) . ?
Na O2 2.4567(9) 2_556 ?
Na N2 2.4907(11) 2_666 ?
Na N1 2.5308(9) 2_656 ?
Na N1 2.7028(10) . ?
Na Na 3.7182(8) 2_556 ?
Na Na 3.8775(8) 2_656 ?
C1 N1 1.1372(12) . ?
C1 B1 1.6097(13) . ?
C2 N2 1.1341(13) . ?
C2 B1 1.6215(14) . ?
C3 N3 1.1352(13) . ?
C3 B1 1.6107(13) . ?
C4 O1 1.4129(13) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C4 H4F 0.9600 . ?
B1 O1 1.4249(12) . ?
O2 H1 0.860(17) . ?
O2 H2 0.794(19) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H1 O1 0.860(17) 1.917(17) 2.7615(11) 166.7(14) . yes
