Alkoxy substituted halogenated closo-dodecaborates as anions for ionic liquids.
Jenne, Carsten; Kirsch, Christoph; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13119–13124; doi:10.1039/c5dt01633a

data_7035519
_publ_section_title
;
 Alkoxy substituted halogenated closo-dodecaborates as anions for ionic
 liquids.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13119
_journal_page_last               13124
_journal_paper_doi               10.1039/c5dt01633a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C8 H17 B12 Br11 O, 2(C24 H20 P), C4 H10 O'
_chemical_formula_sum            'C60 H67 B12 Br11 O2 P2'
_chemical_formula_weight         1890.81
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-27
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
;
2015-04-02 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.517(2)
_cell_angle_beta                 77.871(2)
_cell_angle_gamma                73.201(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0812(4)
_cell_length_b                   16.9930(5)
_cell_length_c                   18.4910(4)
_cell_measurement_reflns_used    14399
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.9120
_cell_measurement_theta_min      2.4990
_cell_volume                     3550.54(19)
_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
;
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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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 0.833
_diffrn_measurement_details
;
  1 omega    2.00   77.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000   60.0000 75

  2 omega   14.00   79.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000  -30.0000 65

  3 omega    6.00   71.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000  -90.0000 65

  4 omega   -4.00   83.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805   77.0000   90.0000 87

  5 omega  -24.00   12.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   77.0000  -30.0000 36

  6 omega  -34.00   -3.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -57.0000  120.0000 31

  7 omega  -49.00   27.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -37.0000  150.0000 76

  8 omega   20.00   52.00   1.0000   95.1650
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000 -180.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0555065000
_diffrn_orient_matrix_UB_12      -0.0210114000
_diffrn_orient_matrix_UB_13      0.0083347000
_diffrn_orient_matrix_UB_21      -0.0117731000
_diffrn_orient_matrix_UB_22      -0.0381310000
_diffrn_orient_matrix_UB_23      -0.0033839000
_diffrn_orient_matrix_UB_31      0.0267973000
_diffrn_orient_matrix_UB_32      -0.0028746000
_diffrn_orient_matrix_UB_33      -0.0382180000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35549
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49403
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1836
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN/diethyl ether'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         16534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+2.6280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                11894
_reflns_number_total             16534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01633a2.cif
_cod_data_source_block           169pph
_cod_depositor_comments
'Adding full bibliography for 7035514--7035519.cif.'
_cod_original_cell_volume        3550.54(18)
_cod_database_code               7035519
_chemical_oxdiff_formula         B12Cl11OC56H57P2
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C2(H2), C3(H3), C4(H4),
 C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24)
2.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'