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_7035516
_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         'C3 H7 B12 Cl11 O, 2(C24 H20 P)'
_chemical_formula_sum            'C51 H47 B12 Cl11 O P2'
_chemical_formula_weight         1257.50
_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
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-02 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                113.9658(17)
_cell_angle_beta                 90.7492(14)
_cell_angle_gamma                94.0845(13)
_cell_formula_units_Z            6
_cell_length_a                   11.27145(18)
_cell_length_b                   28.4714(5)
_cell_length_c                   30.0522(5)
_cell_measurement_reflns_used    26236
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.2630
_cell_measurement_theta_min      2.1310
_cell_volume                     8781.0(3)
_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  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_details
;
  1 omega   28.00   54.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   57.0000  -30.0000 26

  2 omega   29.00   83.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000  -60.0000 54

  3 omega   54.00   82.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000 -180.0000 28

  4 omega   -7.00   71.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805   77.0000 -120.0000 78

  5 omega    0.00   46.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000   30.0000 46

  6 omega    0.00   82.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000  150.0000 82

  7 omega  -16.00   10.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   57.0000  -30.0000 26

  8 omega  -34.00    6.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -57.0000 -120.0000 40

  9 omega  -46.00   41.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -77.0000   30.0000 87

 10 omega   17.00   48.00   1.0000  153.1550
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000   90.0000 31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0048395000
_diffrn_orient_matrix_UB_12      0.0111927000
_diffrn_orient_matrix_UB_13      0.0256595000
_diffrn_orient_matrix_UB_21      0.0242832000
_diffrn_orient_matrix_UB_22      -0.0216308000
_diffrn_orient_matrix_UB_23      0.0015359000
_diffrn_orient_matrix_UB_31      0.0581000000
_diffrn_orient_matrix_UB_32      0.0124643000
_diffrn_orient_matrix_UB_33      0.0027908000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            91326
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88614
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3828
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN/diethyl ether'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.656
_refine_diff_density_min         -1.868
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2083
_refine_ls_number_reflns         40498
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0497P)^2^+31.8295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                30630
_reflns_number_total             40498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01633a2.cif
_cod_data_source_block           171pph4b2
_cod_depositor_comments
'Adding full bibliography for 7035514--7035519.cif.'
_cod_database_code               7035516
_chemical_oxdiff_formula         B12Cl11OC51H47P2
_reflns_odcompleteness_completeness 99.86
_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. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C145) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.2
Uanis(O1) \\sim Ueq, Uanis(C145) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
3.a Secondary CH2 refined with riding coordinates:
 C145(H14A,H14B), C146(H14C,H14D), C148(H14H,H14I), C149(H14J,H14K), C151(H15D,
 H15E), C152(H15F,H15G)
3.b Aromatic/amide H refined with riding coordinates:
 C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), 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), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), 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), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
 C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C86(H86), C87(H87), C88(H88),
  C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96)
3.c Idealised Me refined as rotating group:
 C147(H14E,H14F,H14G), C150(H15A,H15B,H15C), C153(H15H,H15I,H15J)
;
_olex2_submission_special_instructions 'No special instructions were received'