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_4345282
_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         'C6 H6 B12 Cl11 N, 2(C24 H20 P)'
_chemical_formula_sum            'C54 H46 B12 Cl11 N P2'
_chemical_formula_weight         1290.53
_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
_audit_creation_date             2016-06-10
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                101.214(3)
_cell_angle_beta                 100.711(3)
_cell_angle_gamma                108.423(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8703(3)
_cell_length_b                   12.9055(4)
_cell_length_c                   21.9887(9)
_cell_measurement_reflns_used    6925
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      28.8670
_cell_measurement_theta_min      2.3250
_cell_volume                     3022.1(2)
_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
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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_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      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.689
_diffrn_measurement_details
;
  1 omega   19.00   44.50   0.7500   68.8350
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -19.0000   60.0000 34

  2 omega   -3.00   50.25   0.7500   68.8350
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000   90.0000 71

  3 omega  -43.00   38.00   0.7500   68.8350
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -19.0000  150.0000 108

  4 omega    9.00   47.25   0.7500   68.8350
omega____ theta____ kappa____ phi______ frames
    -       15.2805   57.0000    0.0000 51

  5 omega  -56.00  -29.00   0.7500   68.8350
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -19.0000   60.0000 36

  6 omega   10.00   42.25   0.7500   68.8350
omega____ theta____ kappa____ phi______ frames
    -       15.2805  -99.0000 -150.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0527297000
_diffrn_orient_matrix_UB_12      -0.0242017000
_diffrn_orient_matrix_UB_13      -0.0267372000
_diffrn_orient_matrix_UB_21      -0.0230421000
_diffrn_orient_matrix_UB_22      0.0415874000
_diffrn_orient_matrix_UB_23      0.0126492000
_diffrn_orient_matrix_UB_31      0.0309366000
_diffrn_orient_matrix_UB_32      0.0361710000
_diffrn_orient_matrix_UB_33      -0.0170034000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.869
_diffrn_reflns_Laue_measured_fraction_max 0.689
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16753
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.689
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.531
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
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    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         11634
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+2.1537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8081
_reflns_number_total             11634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03006_si_005.cif
_cod_data_source_block           223pph4
_cod_depositor_comments
'Adding full bibliography for 4345279--4345283.cif.'
_cod_original_cell_volume        3022.13(19)
_cod_database_code               4345282
_chemical_oxdiff_formula         C24H20PB12Cl11C3H5N
_reflns_odcompleteness_completeness 85.55
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C48B) \\sim Ueq, Uanis(C47B) \\sim Ueq, Uanis(C45B) \\sim Ueq,
Uanis(C44B) \\sim Ueq, Uanis(C46B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(Cl2B)=Sof(Cl5B)=Sof(Cl6B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(C5B)=Sof(C43B)=Sof(C44B)=Sof(H44B)=Sof(C45B)=Sof(H45B)=Sof(C46B)=
 Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48B)=1-FVAR(1)
 Sof(Cl2A)=Sof(Cl5A)=Sof(Cl6A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=FVAR(1)
 Sof(C49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52A)=
 Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=1-FVAR(2)
 Sof(C49B)=Sof(C50B)=Sof(H50B)=Sof(C51B)=Sof(H51B)=Sof(C52B)=Sof(H52B)=
 Sof(C53B)=Sof(H53B)=Sof(C54B)=Sof(H54B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C4A(H4AA,H4AB), C4B(H4BA,H4BB)
4.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A),
 C48A(H48A), C44B(H44B), C45B(H45B), C46B(H46B), C47B(H47B), C48B(H48B),
 C50A(H50A), C51A(H51A), C52A(H52A), C53A(H53A), C54A(H54A), C50B(H50B),
 C51B(H51B), C52B(H52B), C53B(H53B), C54B(H54B), 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), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30)
4.c Fitted hexagon refined as free rotating group:
 C43A(C44A,C45A,C46A,C47A,C48A), C43B(C44B,C45B,C46B,C47B,C48B), C49A(C50A,
 C51A,C52A,C53A,C54A), C49B(C50B,C51B,C52B,C53B,C54B)
4.d :
 C3(H3), C6(H6)
;
_shelx_res_checksum              89264
_shelx_hkl_checksum              88674
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'