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_7035518
_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         '2(C24 H20 P), C3 H7 B12 Br11 O, C2 H3 N'
_chemical_formula_sum            'C53 H50 B12 Br11 N O P2'
_chemical_formula_weight         1787.61
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 91.786(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8024(4)
_cell_length_b                   38.8526(14)
_cell_length_c                   13.9673(4)
_cell_measurement_reflns_used    11806
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5340
_cell_measurement_theta_min      2.4460
_cell_volume                     6401.6(4)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details
;
  1 omega    2.00   28.10   0.3000   30.4450
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   37.0000  -30.0000 87

  2 omega   13.00   80.20   0.3000   30.4450
omega____ theta____ kappa____ phi______ frames
    -       15.2805   77.0000   60.0000 224

  3 omega  -48.00  -21.00   0.3000   30.4450
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  111.0000 -151.0000 90

  4 omega  -54.00   44.10   0.3000   30.4450
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -19.0000   60.0000 327

  5 omega   -1.00   51.20   0.3000   30.4450
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000  -30.0000 174

  6 omega   -3.00   53.40   0.3000   30.4450
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000 -150.0000 188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0106040000
_diffrn_orient_matrix_UB_12      0.0170113000
_diffrn_orient_matrix_UB_13      0.0158529000
_diffrn_orient_matrix_UB_21      0.0057650000
_diffrn_orient_matrix_UB_22      -0.0055677000
_diffrn_orient_matrix_UB_23      0.0482825000
_diffrn_orient_matrix_UB_31      0.0588683000
_diffrn_orient_matrix_UB_32      0.0036284000
_diffrn_orient_matrix_UB_33      -0.0001884000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43395
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.44
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.973
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.58822
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_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         1.728
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         15102
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+8.8730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                11833
_reflns_number_total             15102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01633a2.cif
_cod_data_source_block           168pph42
_cod_depositor_comments
'Adding full bibliography for 7035514--7035519.cif.'
_cod_original_cell_volume        6401.7(4)
_cod_database_code               7035518
_chemical_oxdiff_formula         B12Br11OC51H47P2
_reflns_odcompleteness_completeness 99.89
_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(C25A) \\sim Ueq, Uanis(C25B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C25B) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.2
Uanis(C25A) \\sim Ueq, Uanis(C25B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.2
3. Others
 Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C37B)=Sof(C38B)=Sof(H38B)=
 Sof(C39B)=Sof(H39B)=Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=
 Sof(H42B)=1-FVAR(1)
 Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=
 Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30B)=Sof(C37A)=Sof(C38A)=Sof(H38A)=
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=
 Sof(H42A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B)
4.b Aromatic/amide H refined with riding coordinates:
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B), C30B(H30B), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A), C42A(H42A),
  C38B(H38B), C39B(H39B), C40B(H40B), C41B(H41B), C42B(H42B), 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)
4.c Fitted hexagon refined as free rotating group:
 C25A(C26A,C27A,C28A,C29A,C30A), C25B(C26B,C27B,C28B,C29B,C30B), C37A(C38A,
 C39A,C40A,C41A,C42A), C37B(C38B,C39B,C40B,C41B,C42B)
4.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C)
;
_olex2_submission_special_instructions 'No special instructions were received'