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_4345283
_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_absolute_configuration unk
_chemical_formula_moiety         'C6 H20 B12 Br6 N, C3 H10 N, C2 H3 N'
_chemical_formula_sum            'C11 H33 B12 Br6 N3'
_chemical_formula_weight         816.58
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2497(2)
_cell_length_b                   14.5802(3)
_cell_length_c                   19.2110(4)
_cell_measurement_reflns_used    5634
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.1490
_cell_measurement_theta_min      2.3930
_cell_volume                     2870.94(10)
_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
;
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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_details
;
  1 omega    3.00   53.00   1.0000  126.8150
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000   90.0000 50

  2 omega  -43.00   23.00   1.0000  126.8150
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -57.0000 -120.0000 66

  3 omega  -22.00   29.00   1.0000  126.8150
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -19.0000  -60.0000 51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0164398000
_diffrn_orient_matrix_UB_12      -0.0077728000
_diffrn_orient_matrix_UB_13      0.0353790000
_diffrn_orient_matrix_UB_21      -0.0054573000
_diffrn_orient_matrix_UB_22      0.0479863000
_diffrn_orient_matrix_UB_23      0.0054192000
_diffrn_orient_matrix_UB_31      -0.0669667000
_diffrn_orient_matrix_UB_32      -0.0020125000
_diffrn_orient_matrix_UB_33      -0.0091173000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10430
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.461
_diffrn_reflns_theta_min         2.120
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77791
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 2123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         6405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.673
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.731
_reflns_number_gt                5733
_reflns_number_total             6405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03006_si_003.cif
_cod_data_source_block           259
_cod_depositor_comments
'Adding full bibliography for 4345279--4345283.cif.'
_cod_original_cell_volume        2870.93(9)
_cod_database_code               4345283
_chemical_oxdiff_formula         NC3H10B12Br6H5NC6H15
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
2.c Boron cage BH refined with riding coordinates:
 B2(H2), B6(H6), B5(H5), B4(H4), B3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'