Copper-Promoted Cyanation of a Boron Cluster: Synthesis, X-ray Structure, and Reactivity of 12-CN-closo-CHB11H10-
Aaron J. Rosenbaum; Douglas H. Juers; Marcus A. Juhasz; Inorganic Chemistry 52 (2013) 10717–10719; doi:10.1021/ic4015306

data_4336237
_publ_contact_author_address
;
Whitman College
Department of Chemistry
345 Boyer Ave
Walla Walla, WA 99362
;
_publ_contact_author_email       juhaszma@whitman.edu
_publ_contact_author_name        'Marcus A. Juhasz'
_publ_contact_author_phone       509-527-5207
_publ_section_title
;
 Copper-Promoted Cyanation of a Boron Cluster: Synthesis, X-ray Structure,
 and Reactivity of 12-CN-closo-CHB11H10-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10717
_journal_page_last               10719
_journal_paper_doi               10.1021/ic4015306
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C2 H11 B11 N, C8 H20 N'
_chemical_formula_sum            'C10 H31 B11 N2'
_chemical_formula_weight         298.44
_chemical_name_systematic
'tetraethylammonium 12-cyano-1-carba-closo-dodecaborate (Et4NCB11H11CN)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-06-18
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.0290(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.85709(18)
_cell_length_b                   10.5712(2)
_cell_length_c                   10.0588(2)
_cell_measurement_reflns_used    6916
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      66.9557
_cell_measurement_theta_min      4.1786
_cell_volume                     941.65(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
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olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      298(1)
_diffrn_detector_area_resol_mean 8.3552
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details
;
  1 omega -107.00  -81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.3121  -99.0000    0.0000 26

  2 omega   23.00  115.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121   57.0000 -150.0000 92

  3 omega   20.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121   57.0000  150.0000 46

  4 omega  -32.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121  -37.0000  -90.0000 100

  5 omega  -22.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121  -57.0000   60.0000 84

  6 omega -167.00  -77.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -64.0000  117.0000 90

  7 omega -160.00  -98.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -45.0000   60.0000 62

  8 omega  -89.00  -62.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -73.0000  162.0000 27

  9 omega -147.00  -62.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -77.0000 -150.0000 85

 10 omega -126.00 -100.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000   15.0000    0.0000 26

 11 omega -170.00 -127.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -73.0000  162.0000 43

 12 omega  -91.00  -61.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -77.0000  150.0000 30

 13 omega  -86.00  -60.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000   15.0000    0.0000 26

 14 omega -166.00 -101.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -66.0000  175.0000 65

 15 omega  -96.00  -67.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -66.0000  175.0000 29

 16 omega   47.00   74.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -45.0000   90.0000 27

 17 omega   79.00  178.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000   30.0000  -30.0000 99

 18 omega   38.00   77.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -45.0000  -60.0000 39

 19 omega   35.00   67.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -30.0000   60.0000 32

 20 omega   44.00  100.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -94.0000   90.0000 56

 21 omega   36.00   69.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -30.0000  -30.0000 33

 22 omega   33.00   67.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -30.0000   30.0000 34

 23 omega -120.00  -73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.3121 -125.0000    0.0000 47

 24 omega  -99.00   -2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.3121  125.0000 -180.0000 97

 25 omega   16.00  116.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121   57.0000  -60.0000 100

 26 omega   10.00  122.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121   77.0000  120.0000 112

 27 omega    2.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121 -125.0000   60.0000 97

 28 omega   10.00  122.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121   77.0000   30.0000 112

 29 omega -173.00  -62.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -76.0000  -49.0000 111

 30 omega -174.00  -61.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -77.0000 -130.0000 113

 31 omega -174.00  -61.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -77.0000   90.0000 113

 32 omega -171.00  -63.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -70.0000  -22.0000 108

 33 omega -171.00  -63.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -72.0000   39.0000 108

 34 omega -170.00  -64.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -67.0000    5.0000 106

 35 omega -174.00  -61.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -77.0000  -90.0000 113

 36 omega -171.00  -63.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      -95.0000  -70.0000  174.0000 108

 37 omega   24.00  109.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -94.0000 -180.0000 85

 38 omega   24.00  109.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -94.0000 -120.0000 85

 39 omega   24.00  109.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -94.0000  -30.0000 85

 40 omega   32.00   69.00   1.0000   27.8000
omega____ theta____ kappa____ phi______ frames
    -      109.0000  -30.0000 -120.0000 37

 41 omega   16.00  110.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3121   57.0000    0.0000 94
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0071857000
_diffrn_orient_matrix_UB_12      0.0709917000
_diffrn_orient_matrix_UB_13      -0.1336857000
_diffrn_orient_matrix_UB_21      0.1609949000
_diffrn_orient_matrix_UB_22      -0.0452718000
_diffrn_orient_matrix_UB_23      -0.0307593000
_diffrn_orient_matrix_UB_31      -0.0655844000
_diffrn_orient_matrix_UB_32      -0.1189734000
_diffrn_orient_matrix_UB_33      -0.0680619000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_number            17648
_diffrn_reflns_theta_full        67.0677
_diffrn_reflns_theta_max         67.07
_diffrn_reflns_theta_min         4.40
_diffrn_source                   'Nova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.0520
_exptl_crystal_description       prism
_exptl_crystal_F_000             320.6550
_exptl_crystal_preparation
'Rxn of 12-I-CB11H11 with CuCN in DMF using microwave irradiation.'
_exptl_crystal_recrystallization_method
'Slow evaporation of a saturated solution of compound in acetonitrile/water'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.1112
_refine_diff_density_min         -0.1656
_refine_diff_density_rms         0.0304
_refine_ls_d_res_high            0.8371
_refine_ls_d_res_low             10.0572
_refine_ls_goodness_of_fit_ref   0.9778
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9778
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1446
_reflns_Friedel_coverage         1.000
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              12
_reflns_limit_l_min              -11
_reflns_number_gt                2924
_reflns_number_total             3366
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic4015306_si_001.cif
_cod_data_source_block           AR-065c
_cod_database_code               4336237
_cod_database_fobs_code          4336237
_chemical_oxdiff_formula         C10N2B11H31
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;