Borane reaction chemistry. Alkyne insertion reactions into boron-containing clusters. Products from the thermolysis of [6,9-(2-HCC‒C5H4N)2-arachno-B10H12]
Bould, Jonathan; Laromaine, Anna; Bullen, Neil J.; Viñas, Clara; Thornton-Pett, Mark; Sillanpää, Reijo; Kivekäs, Raikko; Kennedy, John D.; Teixidor, Francesc; Dalton Transactions  (2008) 1552–1563; doi:10.1039/b715845a

data_7003381
_publ_section_title
;
 Borane reaction chemistry. Alkyne insertion reactions into
 boron-containing clusters. Products from the thermolysis of
 [6,9-(2-HC&#xE002;C--C5H4N)2-arachno-B10H12]
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              1552
_journal_page_last               1563
_journal_paper_doi               10.1039/b715845a
_journal_year                    2008
_chemical_formula_moiety         'C7 H16 B9 N'
_chemical_formula_sum            'C7 H16 B9 N'
_chemical_formula_weight         211.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.5520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.4462(2)
_cell_length_b                   18.0969(5)
_cell_length_c                   14.8241(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2452.84(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24295
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.055
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0445P)^2^+1.1087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                3885
_reflns_number_total             4763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715845a.txt
_cod_data_source_block           jb273
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7003381