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_7035517
_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 Cl11 O, 2(C24 H20 P)'
_chemical_formula_sum            'C56 H57 B12 Cl11 O P2'
_chemical_formula_weight         1327.62
_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
_audit_creation_date             2015-05-22
_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
;
2015-05-26 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                93.883(2)
_cell_angle_beta                 103.004(3)
_cell_angle_gamma                102.370(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1721(4)
_cell_length_b                   16.4910(5)
_cell_length_c                   17.4760(5)
_cell_measurement_reflns_used    11614
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.2160
_cell_measurement_theta_min      2.4190
_cell_volume                     3313.79(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_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -1.00   66.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   57.0000  -30.0000 67

  2 omega   -1.00   82.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   77.0000    0.0000 83

  3 omega   30.00   82.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   77.0000  150.0000 52

  4 omega  -10.00   19.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   77.0000  150.0000 29

  5 omega  -52.00   32.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367  -57.0000   60.0000 84

  6 omega    2.00   67.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   57.0000 -120.0000 65

  7 omega   -4.00   47.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367   37.0000 -150.0000 51

  8 omega  -36.00   -6.00   1.0000   32.1350
omega____ theta____ kappa____ phi______ frames
    -       15.4367  -57.0000 -180.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0535866000
_diffrn_orient_matrix_UB_12      0.0146749000
_diffrn_orient_matrix_UB_13      0.0286011000
_diffrn_orient_matrix_UB_21      -0.0249191000
_diffrn_orient_matrix_UB_22      0.0274784000
_diffrn_orient_matrix_UB_23      0.0198853000
_diffrn_orient_matrix_UB_31      -0.0171858000
_diffrn_orient_matrix_UB_32      -0.0315873000
_diffrn_orient_matrix_UB_33      0.0234064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29031
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.371
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis 171.NET) (complied 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    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12967
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+7.0634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10977
_reflns_number_total             12967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01633a2.cif
_cod_data_source_block           172pph4
_cod_depositor_comments
'Adding full bibliography for 7035514--7035519.cif.'
_cod_original_cell_volume        3313.78(17)
_cod_database_code               7035517
_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. Shared sites
{O2, Cl2}
3. Restrained distances
 C49-C50 \\sim C50-C51 \\sim C51-C52 \\sim C52-C53 \\sim C53-C54 \\sim C54-C55
\\sim C55-C56
 with sigma of 0.0001
 C57-C58 \\sim C58-C59 \\sim C59-C60 \\sim C61-C60 \\sim C64-C63 \\sim C61-C62
\\sim C62-C63
 with sigma of 0.0001
4. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C60) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) = Uanis(Cl2)
5. Rigid body (RIGU) restrains
 C49, C50, C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(B1B)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=
 Sof(H64B)=Sof(H64C)=Sof(Cl1)=Sof(O2)=1-FVAR(1)
 Sof(B1A)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=
 Sof(H56B)=Sof(H56C)=Sof(Cl2)=Sof(O1)=FVAR(1)
7.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), C58(H58A,H58B),
 C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
7.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)
7.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              74073
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'