Remarkable cage deboronation and rearrangement of a closo-1,12-dicarbadodecaborane to form a neutral nido-7,9-dicarbaundecaborane
Joseph A. Ioppolo; Mohan Bhadbhade; Mark A. Fox; Louis M. Rendina; Chem.Commun. 49 (2013) 3312–; doi:10.1039/c3cc41173g

data_7109091
_publ_section_title
;
 Remarkable cage deboronation and rearrangement of a
 closo-1,12-dicarbadodecaborane to form a neutral
 nido-7,9-dicarbaundecaborane
;
_journal_name_full               Chem.Commun.
_journal_page_first              3312
_journal_paper_doi               10.1039/c3cc41173g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C29.5 H35 B9 O P2'
_chemical_formula_weight         564.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.844(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2083(5)
_cell_length_b                   11.6030(4)
_cell_length_c                   17.4061(6)
_cell_measurement_reflns_used    3816
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.403
_cell_measurement_theta_min      2.459
_cell_volume                     3064.60(18)
_computing_cell_refinement
;
APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA)
;
_computing_data_collection
;
APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_data_reduction
;
APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_molecular_graphics    'SHELXTL-Plus. Sheldrick, G. M. (2008)'
_computing_structure_refinement  'SHELXL-97. Sheldrick, G. M. (2008)'
_computing_structure_solution    'SHELXS-97. Sheldrick, G. M. (2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Area Detector'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22964
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_correction_T_min  0.9573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0441P)^2^+1.9015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                3914
_reflns_number_total             5374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc41173g.txt
_cod_data_source_block           joseph3p21byc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C29.50 H35 B9 O P2'
_cod_database_code               7109091