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_4345279
_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         'C12 H32 B12 Br6 N Na'
_chemical_formula_sum            'C12 H32 B12 Br6 N Na'
_chemical_formula_weight         822.55
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-22
_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                120
_cell_formula_units_Z            6
_cell_length_a                   21.8537(12)
_cell_length_b                   21.8537(12)
_cell_length_c                   12.5914(12)
_cell_measurement_reflns_used    2030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2430
_cell_measurement_theta_min      2.4610
_cell_volume                     5207.8(6)
_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    'SIR2004 (Burla et al., 2007)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -41.00   32.00   1.0000 1500.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -37.0000 -150.0000 73

  2 omega  -49.00   25.00   1.0000 1500.0000
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -19.0000  -30.0000 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0137787000
_diffrn_orient_matrix_UB_12      0.0366964000
_diffrn_orient_matrix_UB_13      0.0082315000
_diffrn_orient_matrix_UB_21      -0.0019862000
_diffrn_orient_matrix_UB_22      0.0046919000
_diffrn_orient_matrix_UB_23      -0.0554381000
_diffrn_orient_matrix_UB_31      -0.0347456000
_diffrn_orient_matrix_UB_32      -0.0058640000
_diffrn_orient_matrix_UB_33      0.0063889000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.1724
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16001
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        23.998
_diffrn_reflns_theta_max         23.998
_diffrn_reflns_theta_min         1.943
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54558
_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    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5345
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1073P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2503
_reflns_number_total             5345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03006_si_002.cif
_cod_data_source_block           257na
_cod_depositor_comments
'Adding full bibliography for 4345279--4345283.cif.'
_cod_original_cell_volume        5207.8(8)
_cod_database_code               4345279
_chemical_oxdiff_formula         NaB12Br6H5NC12H27
_reflns_odcompleteness_completeness 99.92
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C9B)
\\sim Ueq, Uanis(C7B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Fixed Sof: C9B(0.5) H9BA(0.5) H9BB(0.5) H10C(0.5) H10D(0.5) H10A(0.5)
 H10B(0.5) C11B(0.5) H11A(0.5) H11B(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) H6BC(0.5) H6BD(0.5)
 H6AA(0.5) H6AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5)
 H8BD(0.5) H8BE(0.5) H8BF(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H2AA(0.5) H2AB(0.5)
 H2BC(0.5) H2BD(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H4BD(0.5) H4BE(0.5) H4BF(0.5)
 H4AA(0.5) H4AB(0.5) H4AC(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C9A(0.5) H9AA(0.5)
 H9AB(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C1B(0.5)
 H1BA(0.5) H1BB(0.5) C3B(0.5) H3BA(0.5) H3BB(0.5) Br9A(0.5) Br9B(0.5) Br10(0.5)
 Br8B(0.5) Br8A(0.5) Br1(0.5) Na1(0.5) Na2(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C9B(H9BA,H9BB), C10(H10C,H10D), C10(H10A,H10B), C11B(H11A,H11B), C5B(H5BA,
 H5BB), C6(H6BC,H6BD), C6(H6AA,H6AB), C7A(H7AA,H7AB), C1A(H1AA,H1AB), C2(H2AA,
 H2AB), C2(H2BC,H2BD), C3A(H3AA,H3AB), C11A(H11C,H11D), C9A(H9AA,H9AB),
 C7B(H7BA,H7BB), C5A(H5AA,H5AB), C1B(H1BA,H1BB), C3B(H3BA,H3BB)
4.b Idealised Me refined as rotating group:
 C12(H12D,H12E,H12F), C12(H12A,H12B,H12C), C8(H8AA,H8AB,H8AC), C8(H8BD,H8BE,
 H8BF), C4(H4BD,H4BE,H4BF), C4(H4AA,H4AB,H4AC)
4.c Boron cage BH refined with riding coordinates:
 B2(H2), B6(H6), B5(H5), B4(H4), B3(H3)
;
_shelx_res_checksum              7749
_shelx_hkl_checksum              60753
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'