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_7029313
_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         'C11 H21 B10 N S'
_chemical_formula_sum            'C11 H21 B10 N S'
_chemical_formula_weight         307.45
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.802(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4931(16)
_cell_length_b                   18.880(2)
_cell_length_c                   8.6737(10)
_cell_measurement_reflns_used    2156
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6530
_cell_measurement_theta_min      4.1150
_cell_volume                     1759.4(4)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.8835
_diffrn_measurement_details
;
  1 omega  -35.00   88.00   1.0000   42.3700
omega____ theta____ kappa____ phi______ frames
    -       17.7426    0.0000  150.0000 123

  2 omega   35.00   94.00   1.0000   42.3700
omega____ theta____ kappa____ phi______ frames
    -       17.7426 -178.0000 -150.0000 59

  3 omega  -24.00   14.00   1.0000   42.3700
omega____ theta____ kappa____ phi______ frames
    -      -18.8363  -99.0000 -150.0000 38

  4 omega  -55.00    7.00   1.0000   42.3700
omega____ theta____ kappa____ phi______ frames
    -       17.7426  -37.0000  -30.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0255922000
_diffrn_orient_matrix_UB_12      0.0284053000
_diffrn_orient_matrix_UB_13      -0.0311150000
_diffrn_orient_matrix_UB_21      -0.0603859000
_diffrn_orient_matrix_UB_22      0.0146587000
_diffrn_orient_matrix_UB_23      -0.0376745000
_diffrn_orient_matrix_UB_31      0.0079838000
_diffrn_orient_matrix_UB_32      0.0197643000
_diffrn_orient_matrix_UB_33      0.0724914000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9305
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81786
_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            yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.3422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                2304
_reflns_number_total             3591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52785a.txt
_cod_data_source_block           130924_ny_wyf_68b
_cod_database_code               7029313
_chemical_oxdiff_formula         'C H N O B S'
_reflns_odcompleteness_completeness 99.60
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C8(H8), C6(H6), C9(H9)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
2.d Boron cage BH refined with riding coordinates:
 C1(H1A), B6(H6A), B3(H3), B7(H7), B11(H11), B10(H10), B5(H5A), B4(H4),
 B8(H8A), B12(H12), B9(H9A)
;