#------------------------------------------------------------------------------
#$Date: 2017-03-24 12:00:48 +0200 (Fri, 24 Mar 2017) $
#$Revision: 194474 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/40/2014090.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2014090
loop_
_publ_author_name
'Hong-Xia Zhang'
'Shou-Tian Zheng'
'Guo-Yu Yang'
_publ_section_title
;
 Tetramethylammonium pentaborate 0.25-hydrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o545
_journal_page_last               o546
_journal_paper_doi               10.1107/S0108270104013915
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C4 H12 N + , B5 H4 O10 - , 0.25H2 O'
_chemical_formula_moiety         'B5 H4 O10, C4 H12 N, 0.062(O4)'
_chemical_formula_sum            'C4 H16 B5 N O10.25'
_chemical_formula_weight         296.23
_chemical_name_systematic
;
Tetramethylammonium pentaborate hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.281(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2623(4)
_cell_length_b                   16.8814(7)
_cell_length_c                   9.2119(5)
_cell_measurement_reflns_used    57
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.41
_cell_volume                     1431.73(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT and SHELXTL (Bruker, 1999)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4012
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.213
_refine_ls_extinction_coef       0.011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0671P)²+1.0501P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                1654
_reflns_number_total             2538
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            av1187.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-24

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2014090
_cod_database_fobs_code          2014090
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
_atom_site_attached_hydrogens
O1 0.8486(2) 0.57705(13) 0.1955(2) 0.0390(6) Uani d . 1 . . O 0
O2 1.0888(3) 0.53732(16) 0.2093(3) 0.0529(7) Uani d . 1 . . O 0
O3 1.0043(2) 0.63342(14) 0.0344(3) 0.0462(7) Uani d . 1 . . O 0
O4 0.9200(3) 0.72546(18) -0.1411(3) 0.0591(8) Uani d . 1 . . O 0
O5 0.7570(2) 0.67133(13) 0.0127(2) 0.0392(6) Uani d . 1 . . O 0
O6 0.6910(2) 0.68090(13) 0.2551(2) 0.0407(6) Uani d . 1 . . O 0
O7 0.5300(3) 0.7418(2) 0.4023(4) 0.0803(11) Uani d . 1 . . O 0
O8 0.4480(2) 0.63774(16) 0.2525(3) 0.0597(8) Uani d . 1 . . O 0
O9 0.3570(2) 0.53304(17) 0.1089(3) 0.0543(8) Uani d . 1 . . O 0
O10 0.5992(2) 0.57430(12) 0.0974(2) 0.0370(6) Uani d . 1 . . O 0
OW 0.649(2) 0.8871(12) 0.143(2) 0.135(6) Uani d P 0.25 . . O 2
B1 0.9795(4) 0.5822(2) 0.1457(4) 0.0364(9) Uani d . 1 . . B 0
B2 0.8906(4) 0.6768(2) -0.0314(4) 0.0378(9) Uani d . 1 . . B 0
B3 0.7253(4) 0.6256(2) 0.1413(4) 0.0321(8) Uani d . 1 . . B 0
B4 0.5600(4) 0.6874(3) 0.3036(5) 0.0468(11) Uani d . 1 . . B 0
B5 0.4718(4) 0.5813(2) 0.1516(4) 0.0386(9) Uani d . 1 . . B 0
N 0.2069(4) 0.87837(19) 0.1203(3) 0.0565(9) Uani d . 1 . . N 0
C1 0.2401(6) 0.8739(3) 0.2795(5) 0.0878(16) Uani d . 1 . . C 0
H1A 0.3415 0.8627 0.3035 0.132 Uiso calc R 1 . . H 0
H1B 0.1835 0.8324 0.3169 0.132 Uiso calc R 1 . . H 0
H1C 0.2170 0.9235 0.3223 0.132 Uiso calc R 1 . . H 0
C2 0.2907(7) 0.9435(3) 0.0630(6) 0.107(2) Uani d . 1 . . C 0
H2B 0.3927 0.9328 0.0838 0.160 Uiso calc R 1 . . H 0
H2C 0.2679 0.9923 0.1087 0.160 Uiso calc R 1 . . H 0
H2D 0.2661 0.9476 -0.0406 0.160 Uiso calc R 1 . . H 0
C3 0.0482(5) 0.8967(3) 0.0870(6) 0.0860(15) Uani d . 1 . . C 0
H3A 0.0264 0.9453 0.1340 0.129 Uiso calc R 1 . . H 0
H3B -0.0080 0.8545 0.1224 0.129 Uiso calc R 1 . . H 0
H3C 0.0246 0.9019 -0.0166 0.129 Uiso calc R 1 . . H 0
C4 0.2369(6) 0.8033(3) 0.0465(7) 0.108(2) Uani d . 1 . . C 0
H4B 0.3382 0.7906 0.0660 0.163 Uiso calc R 1 . . H 0
H4C 0.2119 0.8090 -0.0569 0.163 Uiso calc R 1 . . H 0
H4D 0.1801 0.7615 0.0824 0.163 Uiso calc R 1 . . H 0
H2 1.172(4) 0.539(2) 0.174(4) 0.052(11) Uiso d . 1 . . H 0
H4 0.853(5) 0.750(3) -0.178(5) 0.070(15) Uiso d . 1 . . H 0
H7 0.602(6) 0.765(3) 0.429(6) 0.11(2) Uiso d . 1 . . H 0
H9 0.371(5) 0.503(3) 0.046(5) 0.082(16) Uiso d . 1 . . H 0
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 for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
H H 0.0000 0.0000
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
B B 0.0013 0.0007
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
N N 0.0061 0.0033
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
O O 0.0106 0.0060
; International Tables for Crystallography (1992).
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_publ_flag
B1 O1 B3 123.4(3) ?
B1 O2 H2 118(2) ?
B2 O3 B1 118.8(3) ?
B2 O4 H4 115(3) ?
B2 O5 B3 123.3(3) ?
B4 O6 B3 124.4(3) ?
B4 O7 H7 109(4) ?
B5 O8 B4 119.1(3) ?
B5 O9 H9 114(3) ?
B5 O10 B3 123.5(3) ?
O2 B1 O1 118.5(3) ?
O2 B1 O3 119.9(3) ?
O1 B1 O3 121.6(3) ?
O5 B2 O4 122.2(3) ?
O5 B2 O3 121.2(3) ?
O4 B2 O3 116.6(3) ?
O1 B3 O6 109.7(3) ?
O1 B3 O5 110.9(2) ?
O6 B3 O5 108.7(3) ?
O1 B3 O10 109.5(3) ?
O6 B3 O10 110.1(2) ?
O5 B3 O10 108.0(3) ?
O6 B4 O7 122.9(3) ?
O6 B4 O8 120.7(3) ?
O7 B4 O8 116.3(3) ?
O10 B5 O9 122.2(3) ?
O10 B5 O8 122.1(3) ?
O9 B5 O8 115.8(3) ?
C1 N C2 109.6(4) ?
C1 N C4 112.7(4) ?
C2 N C4 109.9(4) ?
C1 N C3 108.0(3) ?
C2 N C3 108.4(4) ?
C4 N C3 108.2(4) ?
N C1 H1A 109.5 ?
N C1 H1B 109.5 ?
H1A C1 H1B 109.5 ?
N C1 H1C 109.5 ?
H1A C1 H1C 109.5 ?
H1B C1 H1C 109.5 ?
N C2 H2B 109.5 ?
N C2 H2C 109.5 ?
H2B C2 H2C 109.5 ?
N C2 H2D 109.5 ?
H2B C2 H2D 109.5 ?
H2C C2 H2D 109.5 ?
N C3 H3A 109.5 ?
N C3 H3B 109.5 ?
H3A C3 H3B 109.5 ?
N C3 H3C 109.5 ?
H3A C3 H3C 109.5 ?
H3B C3 H3C 109.5 ?
N C4 H4B 109.5 ?
N C4 H4C 109.5 ?
H4B C4 H4C 109.5 ?
N C4 H4D 109.5 ?
H4B C4 H4D 109.5 ?
H4C C4 H4D 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 B1 . 1.346(4) ?
O1 B3 . 1.449(4) ?
O2 B1 . 1.346(4) ?
O2 H2 . 0.87(4) ?
O3 B2 . 1.368(4) ?
O3 B1 . 1.379(4) ?
O4 B2 . 1.354(4) ?
O4 H4 . 0.79(5) ?
O5 B2 . 1.347(4) ?
O5 B3 . 1.470(4) ?
O6 B4 . 1.342(4) ?
O6 B3 . 1.465(4) ?
O7 B4 . 1.342(5) ?
O7 H7 . 0.79(6) ?
O8 B5 . 1.366(4) ?
O8 B4 . 1.377(5) ?
O9 B5 . 1.363(4) ?
O9 H9 . 0.79(5) ?
O10 B5 . 1.336(4) ?
O10 B3 . 1.474(4) ?
N C1 . 1.467(5) ?
N C2 . 1.476(6) ?
N C4 . 1.479(5) ?
N C3 . 1.500(5) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C2 H2B . 0.9600 ?
C2 H2C . 0.9600 ?
C2 H2D . 0.9600 ?
C3 H3A . 0.9600 ?
C3 H3B . 0.9600 ?
C3 H3C . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C4 H4D . 0.9600 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O2 H2 O9 1_655 0.87(4) 1.88(4) 2.745(3) 174(4)
O4 H4 O6 4_575 0.79(5) 1.94(5) 2.733(4) 173(5)
O7 H7 O5 4_576 0.79(6) 1.89(6) 2.671(4) 171(6)
O9 H9 O10 3_665 0.79(5) 1.90(5) 2.688(3) 176(5)
