Syntheses and structural characterization of o-carboranylamides with direct cage-amide bond.
Nie, Yong; Wang, Yafeng; Miao, Jinling; Bian, Deqian; Zhang, Zhenwei; Cui, Yu; Sun, Guoxin; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5083–5094; doi:10.1039/c3dt52785a

data_7029310
_publ_section_title
;
 Syntheses and structural characterization of o-carboranylamides with
 direct cage-amide bond.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5083
_journal_page_last               5094
_journal_paper_doi               10.1039/c3dt52785a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C9 H16 B10 I N O'
_chemical_formula_sum            'C9 H16 B10 I N O'
_chemical_formula_weight         389.23
_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             2013-08-24
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.334(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2249(2)
_cell_length_b                   22.8107(10)
_cell_length_c                   10.5504(4)
_cell_measurement_reflns_used    5548
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1990
_cell_measurement_theta_min      3.4690
_cell_volume                     1640.70(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9254
_diffrn_measurement_details
;
  1 omega  -23.00   86.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.7426   19.0000   90.0000 109

  2 omega    9.00   47.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -      -18.8363   57.0000 -180.0000 38

  3 omega   32.00   57.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.7426 -178.0000  120.0000 25

  4 omega  -50.00  -22.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.5863  -57.0000  -30.0000 28

  5 omega   36.00   91.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.5863  178.0000    0.0000 55

  6 omega    9.00   39.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.5863  -57.0000   30.0000 30

  7 omega   15.00   79.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.5863   37.0000  150.0000 64

  8 omega   47.00   87.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.5863  178.0000 -120.0000 40

  9 omega  -21.00   19.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -      -18.6801  -99.0000  -30.0000 40

 10 omega  -36.00   -4.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -      -18.6801  -57.0000  -90.0000 32

 11 omega  -11.00   16.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -      -18.6801  -99.0000 -150.0000 27

 12 omega  -25.00    6.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -      -18.6801  -99.0000 -180.0000 31

 13 omega  -51.00   39.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -       17.5863  -57.0000    0.0000 90

 14 omega  -87.00  -42.00   1.0000    7.5500
omega____ theta____ kappa____ phi______ frames
    -      -18.6801  -57.0000 -120.0000 45
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0946145000
_diffrn_orient_matrix_UB_12      0.0061049000
_diffrn_orient_matrix_UB_13      -0.0460460000
_diffrn_orient_matrix_UB_21      -0.0038887000
_diffrn_orient_matrix_UB_22      0.0260806000
_diffrn_orient_matrix_UB_23      0.0356848000
_diffrn_orient_matrix_UB_31      0.0430491000
_diffrn_orient_matrix_UB_32      0.0158024000
_diffrn_orient_matrix_UB_33      -0.0410126000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19725
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0310P)^2^+1.6385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                2721
_reflns_number_total             3340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52785a.txt
_cod_data_source_block           130823_ny_wyf_65a
_cod_original_cell_volume        1640.71(11)
_cod_database_code               7029310
_chemical_oxdiff_formula         'C H N O B I'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C8(H8), C5(H5), C6(H6), C9(H9)
2.b Boron cage BH refined with riding coordinates:
 C1(H1A), B11(H11), B6(H6A), B12(H12), B7(H7), B5(H5A), B10(H10), B3(H3),
 B9(H9A), B4(H4), B8(H8A)
;