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_7029312
_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         'C18 H26 B10 N2 O4'
_chemical_formula_sum            'C18 H26 B10 N2 O4'
_chemical_formula_weight         442.51
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-28
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.225(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9013(10)
_cell_length_b                   15.5194(10)
_cell_length_c                   14.2472(10)
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9854
_cell_measurement_theta_min      2.5307
_cell_volume                     2385.6(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
;
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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -9.00   67.00   1.0000   10.0200
omega____ theta____ kappa____ phi______ frames
    -       17.7486   77.0000 -150.0000 76

  2 omega   -8.00   88.00   1.0000   10.0200
omega____ theta____ kappa____ phi______ frames
    -       17.7486   77.0000  -30.0000 96

  3 omega  -39.00   -2.00   1.0000   10.0200
omega____ theta____ kappa____ phi______ frames
    -      -18.9986   77.0000   90.0000 37

  4 omega   32.00   80.00   1.0000   10.0200
omega____ theta____ kappa____ phi______ frames
    -       17.7486 -179.0000   90.0000 48

  5 omega  -51.00   39.00   1.0000   10.0200
omega____ theta____ kappa____ phi______ frames
    -       17.7486  -57.0000 -150.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0595775000
_diffrn_orient_matrix_UB_12      0.0153957000
_diffrn_orient_matrix_UB_13      0.0062526000
_diffrn_orient_matrix_UB_21      0.0268760000
_diffrn_orient_matrix_UB_22      0.0244304000
_diffrn_orient_matrix_UB_23      0.0396647000
_diffrn_orient_matrix_UB_31      0.0072619000
_diffrn_orient_matrix_UB_32      0.0354728000
_diffrn_orient_matrix_UB_33      -0.0302120000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14790
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45335
_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_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.048
_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     309
_refine_ls_number_reflns         4877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0882P)^2^+0.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                2825
_reflns_number_total             4877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52785a.txt
_cod_data_source_block           130130_ny_wyf_36c
_cod_database_code               7029312
_chemical_oxdiff_formula         'C H B N O'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H1A of B1, H2A of B2, H5 of C5, H3 of B3, H10 of B10, H9 of B9, H14 of C14,
  H4A of B4, H6 of C6, H2 of N2, H1 of N1, H15 of C15, H5A of B5, H6A of B6, H8
  of C8, H17 of C17, H4 of C4, H13 of C13, H8A of B8, H7 of B7
 At 1.5 times of:
  {H18A,H18B,H18C} of C18, {H9A,H9B,H9C} of C9
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C4(H4), C17(H17), C8(H8), C6(H6), C5(H5), C15(H15), C13(H13),
 C14(H14)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C)
2.c Boron cage BH refined with riding coordinates:
 B4(H4A), B3(H3), B2(H2A), B6(H6A), B5(H5A), B1(H1A), B10(H10), B9(H9),
 B8(H8A), B7(H7)
;