Improving the Solubility of Halogenated 1-Ammonio-closo-dodecaborate Anions.
Bertocco, Philipp; Derendorf, Janis; Jenne, Carsten; Kirsch, Christoph; Inorganic chemistry 56 (2017) 3459–3466; doi:10.1021/acs.inorgchem.6b03006

data_4345280
_publ_section_title
;
 Improving the Solubility of Halogenated 1-Ammonio-closo-dodecaborate
 Anions.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3459
_journal_page_last               3466
_journal_paper_doi               10.1021/acs.inorgchem.6b03006
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C9 H26 B12 Br6 N, C3 H10 N'
_chemical_formula_sum            'C12 H36 B12 Br6 N2'
_chemical_formula_weight         817.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0056(7)
_cell_length_b                   13.9177(6)
_cell_length_c                   12.0441(5)
_cell_measurement_reflns_used    4921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6760
_cell_measurement_theta_min      2.4760
_cell_volume                     3185.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -50.00   22.00   1.0000  569.2000
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -77.0000   90.0000 72

  2 omega   -1.00   31.00   1.0000  569.2000
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000    0.0000 32

  3 omega   -3.00   47.00   1.0000  569.2000
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000  -30.0000 50

  4 omega   16.00   47.00   1.0000  569.2000
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000 -180.0000 31

  5 omega  -68.00  -39.00   1.0000  569.2000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  -57.0000   60.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0146481000
_diffrn_orient_matrix_UB_12      -0.0462518000
_diffrn_orient_matrix_UB_13      0.0086441000
_diffrn_orient_matrix_UB_21      -0.0309407000
_diffrn_orient_matrix_UB_22      -0.0141878000
_diffrn_orient_matrix_UB_23      0.0284468000
_diffrn_orient_matrix_UB_31      -0.0149126000
_diffrn_orient_matrix_UB_32      -0.0158737000
_diffrn_orient_matrix_UB_33      -0.0508679000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12705
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.002
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
TITL 256 Br2 in Pca21 #29
CELL   19.0056   13.9177   12.0441     90.00     90.00     90.00
SPGR Pca21
C101 0.974 0.090 0.080 !       2.28 eA-3
C102 0.535 0.172 0.545 !       1.72 eA-3
Q103 0.645 0.081 0.490 !       1.46 eA-3
Q104 0.162 0.035 0.792 !       1.43 eA-3
C105 0.781 0.174 0.486 !       1.42 eA-3
Q106 0.341 0.966 0.205 !       1.39 eA-3
C107 0.829 0.067 0.311 !       1.38 eA-3
Q108 0.044 0.811 0.403 !       1.38 eA-3
C109 0.720 0.045 0.842 !       1.34 eA-3
C110 0.694 0.110 0.812 !       1.33 eA-3
C111 0.326 0.827 0.910 !       1.33 eA-3
Q112 0.849 0.123 0.424 !       1.31 eA-3
C113 0.128 0.844 0.587 !       1.30 eA-3
Q114 0.950 0.409 0.485 !       1.29 eA-3
Q115 0.592 0.079 0.814 !       1.23 eA-3
C116 0.742 0.218 0.343 !       1.22 eA-3
C117 0.305 0.985 0.270 !       1.22 eA-3
C118 0.281 0.857 0.394 !       1.19 eA-3
C119 0.732 0.139 0.515 !       1.18 eA-3
Q120 0.752 0.263 0.076 !       1.18 eA-3
Q121 0.140 0.781 0.388 !       1.17 eA-3
Q122 0.201 0.701 0.815 !       1.17 eA-3
C123 0.721 0.172 0.795 !       1.16 eA-3
C124 0.426 0.875 0.092 !       1.16 eA-3
C125 0.297 0.845 0.129 !       1.15 eA-3
C126 0.978 0.098-0.003 !       1.13 eA-3
C127 0.343 0.843 0.004 !       1.12 eA-3
C128 0.478 0.910 1.003 !       1.11 eA-3
Q129 0.137 0.782 0.542 !       1.11 eA-3
Q130 0.734 0.076 0.687 !       1.11 eA-3
C131 0.774 0.112 0.907 !       1.10 eA-3
Q132 0.509 0.140 0.472 !       1.09 eA-3
Q133 0.218 0.734 0.877 !       1.07 eA-3
C134 0.593 0.177 0.526 !       1.07 eA-3
C135 0.089 0.889 0.388 !       1.06 eA-3
Q136 0.030 0.129 0.783 !       1.06 eA-3
Q137 0.736 0.141 0.158 !       1.05 eA-3
Q138 0.092 0.120 0.501 !       1.04 eA-3
C139 0.334 0.827 0.342 !       1.04 eA-3
Q140 0.686 0.064 0.956 !       1.03 eA-3
Q141 0.099 0.837 0.828 !       1.03 eA-3
Q142 0.722 0.299 0.044 !       1.03 eA-3
Q143 0.683 0.232 0.384 !       1.03 eA-3
Q144 1.002 0.032 0.063 !       1.02 eA-3
Q145 0.025 0.264 0.612 !       1.02 eA-3
Q146 0.786 0.093 0.079 !       1.01 eA-3
Q147 0.533 0.906 0.094 !       1.01 eA-3
C148 0.193 0.812 0.549 !       1.00 eA-3
C149 0.682 0.061 0.754 !       0.99 eA-3
C150 0.241 0.818 0.715 !       0.99 eA-3
Q151 0.719 0.811 0.771 !       0.98 eA-3
Q152 0.530 0.949 0.565 !       0.97 eA-3
Q153 0.926 0.057 0.057 !       0.97 eA-3
Q154 0.017 0.250 0.729 !       0.97 eA-3
Q155 0.522 0.938-0.001 !       0.96 eA-3
Q156 0.754 0.252 0.919 !       0.96 eA-3
Q157 0.661 0.188 0.095 !       0.96 eA-3
Q158 1.007 0.921 0.642 !       0.96 eA-3
Q159 0.675 0.937 0.389 !       0.96 eA-3
Q160 0.095 0.719 0.220 !       0.95 eA-3
Q161 0.722 0.048 0.351 !       0.95 eA-3
Q162 0.577 0.966 0.738 !       0.94 eA-3
C163 0.098 0.874 0.465 !       0.94 eA-3
Q164 0.927 0.688 0.450 !       0.94 eA-3
Q165 0.557 0.748 0.986 !       0.94 eA-3
Q166 0.029 0.999 0.772 !       0.94 eA-3
Q167 0.670 0.793 0.890 !       0.94 eA-3
C168 0.081 0.894 0.684 !       0.93 eA-3
Q169 0.497 0.982 0.688 !       0.93 eA-3
Q170 0.249 0.341 0.796 !       0.93 eA-3
Q171 0.572 0.253 0.448 !       0.93 eA-3
Q172 0.389 0.453 0.454 !       0.93 eA-3
Q173 0.861 0.933 0.954 !       0.93 eA-3
Q174 0.742 0.047 0.766 !       0.93 eA-3
Q175 0.205 0.065 0.592 !       0.93 eA-3
Q176 0.401 0.720 0.817 !       0.93 eA-3
Q177 0.147 0.123 0.512 !       0.93 eA-3
Q178 0.330 0.825 0.500 !       0.92 eA-3
Q179 0.126 0.063 0.756 !       0.92 eA-3
Q180 0.606 0.168 0.409 !       0.92 eA-3
Q181 0.951 0.020 0.077 !       0.92 eA-3
Q182 0.235 0.748-0.001 !       0.92 eA-3
Q183 0.960 0.123 0.578 !       0.92 eA-3
Q184 0.998 0.795 0.825 !       0.91 eA-3
Q185 0.395 0.188 0.239 !       0.91 eA-3
C186 0.782 0.206 0.081 !       0.91 eA-3
Q187 0.386 0.672 0.748 !       0.91 eA-3
Q188 0.697 0.362 0.552 !       0.90 eA-3
Q189 0.173 0.639 0.345 !       0.90 eA-3
Q190 0.625 0.248 0.078 !       0.90 eA-3
Q191 0.234 0.984 0.013 !       0.90 eA-3
Q192 0.564 0.844 0.874 !       0.90 eA-3
Q193 0.945 0.845 0.236 !       0.90 eA-3
Q194 0.325 0.905 0.891 !       0.90 eA-3
Q195 0.042 0.877 0.917 !       0.89 eA-3
Q196 0.167 0.717 0.461 !       0.89 eA-3
Q197 0.223 0.049 0.029 !       0.89 eA-3
C198 0.130 0.910 0.685 !       0.89 eA-3
Q199 0.692 0.112 0.496 !       0.89 eA-3
;
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 1651 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5467
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.7226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4701
_reflns_number_total             5467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03006_si_006.cif
_cod_data_source_block           256br2_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4345279--4345283.cif.
;
_cod_database_code               4345280
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.630(19) 0.370(19)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(B7) \\sim Ueq, Uanis(B8) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 N2(H2C)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
4.d Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3), B4(H4), B5(H5), B6(H6)
;
_shelx_fab_checksum              73585
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'