Synthesis, structure, and reactivity of 13-vertex carboranes and 14-vertex metallacarboranes.
Deng, Liang; Chan, Hoi-Shan; Xie, Zuowei; Journal of the American Chemical Society 128 (2006) 5219–5230; doi:10.1021/ja0605772

data_4101460
_publ_section_title
;
 Synthesis, structure, and reactivity of 13-vertex carboranes and
 14-vertex metallacarboranes.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5219
_journal_page_last               5230
_journal_paper_doi               10.1021/ja0605772
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C43 H65 B11 Ni O3 P2'
_chemical_formula_weight         869.51
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           triclinic
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 77.9940(10)
_cell_angle_gamma                68.8430(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0023(10)
_cell_length_b                   11.6631(10)
_cell_length_c                   20.3879(18)
_cell_measurement_reflns_used    2637
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.95
_cell_measurement_theta_min      2.62
_cell_volume                     2380.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7856
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8281
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                5366
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0605772si20060125_040455.cif
_cod_data_source_block           18
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_cod_database_code               4101460