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_7029309
_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 F N O'
_chemical_formula_sum            'C9 H16 B10 F N O'
_chemical_formula_weight         281.33
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                114.63(3)
_cell_angle_beta                 90.84(3)
_cell_angle_gamma                106.42(3)
_cell_formula_units_Z            2
_cell_length_a                   6.735(2)
_cell_length_b                   11.253(4)
_cell_length_c                   11.649(4)
_cell_measurement_reflns_used    1393
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9067
_cell_measurement_theta_min      3.1838
_cell_volume                     760.9(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -47.00   48.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043  -77.0000 -180.0000 95

  2 omega  -46.00   36.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043  -57.0000  -90.0000 82

  3 omega  -40.00   38.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043  -57.0000   30.0000 78

  4 omega   11.00   45.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043   54.0000   24.0000 34

  5 omega  -16.00   23.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -      -18.8543  -99.0000   60.0000 39

  6 omega  -24.00    4.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -      -18.8543  -99.0000 -120.0000 28

  7 omega   -4.00   86.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043   57.0000   90.0000 90

  8 omega   -4.00   21.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043   57.0000  -30.0000 25

  9 omega   -4.00   86.00   1.0000   21.8900
omega____ theta____ kappa____ phi______ frames
    -       17.6043   57.0000 -150.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0804559000
_diffrn_orient_matrix_UB_12      0.0294278000
_diffrn_orient_matrix_UB_13      -0.0279684000
_diffrn_orient_matrix_UB_21      0.0751071000
_diffrn_orient_matrix_UB_22      -0.0103540000
_diffrn_orient_matrix_UB_23      0.0350506000
_diffrn_orient_matrix_UB_31      -0.0149751000
_diffrn_orient_matrix_UB_32      -0.0661409000
_diffrn_orient_matrix_UB_33      -0.0508116000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7806
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74588
_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    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0899P)^2^+0.0084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                1870
_reflns_number_total             3110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52785a.txt
_cod_data_source_block           130305_ny_wyf_38a
_cod_original_cell_volume        760.9(4)
_cod_database_code               7029309
_chemical_oxdiff_formula         'C H N O B F'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H1 of N1, H9 of C9, H1A of C1, H5 of B5, H1B of B1, H7 of B7, H6 of C6, H9A
  of B9, H10 of B10, H8 of B8, H6A of B6, H8A of C8, H2 of B2, H4 of B4, H7A of
  C7, H3 of B3
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C9(H9), C6(H6), C8(H8A), C7(H7A)
2.b Boron cage BH refined with riding coordinates:
 C1(H1A), B5(H5), B1(H1B), B7(H7), B9(H9A), B10(H10), B8(H8), B6(H6A), B2(H2),
 B4(H4), B3(H3)
;