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_4345281
_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 H25 B12 Cl6.4 N, C2 H3 N, C3 H9 N'
_chemical_formula_sum            'C14 H37 B12 Cl6.39 N3'
_chemical_formula_weight         603.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_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                 99.741(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1599(3)
_cell_length_b                   12.6988(4)
_cell_length_c                   13.4526(4)
_cell_measurement_reflns_used    3557
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.1290
_cell_measurement_theta_min      2.5930
_cell_volume                     1710.61(9)
_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
;
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      120.00(10)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   -7.00   25.00   1.0000   20.4350
omega____ theta____ kappa____ phi______ frames
    -       15.4367  -57.0000    0.0000 32

  2 omega   -9.00   82.00   1.0000   20.4350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   19.0000  -90.0000 91

  3 omega   45.00   72.00   1.0000   20.4350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   57.0000  -90.0000 27

  4 omega  -25.00    0.00   1.0000   20.4350
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   57.0000 -150.0000 25

  5 omega  -51.00   18.00   1.0000   20.4350
omega____ theta____ kappa____ phi______ frames
    -       15.4367  -57.0000  -30.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0439723000
_diffrn_orient_matrix_UB_12      0.0435193000
_diffrn_orient_matrix_UB_13      0.0101607000
_diffrn_orient_matrix_UB_21      0.0190113000
_diffrn_orient_matrix_UB_22      -0.0175322000
_diffrn_orient_matrix_UB_23      0.0504616000
_diffrn_orient_matrix_UB_31      0.0521621000
_diffrn_orient_matrix_UB_32      -0.0302865000
_diffrn_orient_matrix_UB_33      -0.0146514000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2811
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        23.994
_diffrn_reflns_theta_max         23.994
_diffrn_reflns_theta_min         2.221
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87094
_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    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             621
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2811
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+12.0343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2595
_reflns_number_total             2811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03006_si_004.cif
_cod_data_source_block           256e6nme
_cod_depositor_comments
'Adding full bibliography for 4345279--4345283.cif.'
_cod_original_cell_volume        1710.60(9)
_cod_database_code               4345281
_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. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(B5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C9(0.5) N3(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5)
4.a Riding coordinates:
 B3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C7(H7A,H7B,H7C)
4.d Boron cage BH refined with riding coordinates:
 B2(H2)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'