Palladium-Catalyzed Amination of 2-Iodo-para-carborane
Beletskaya, Irina P.; Bregadze, Vladimir I.; Kabytaev, Kuanysh Z.; Zhigareva, Galina G.; Petrovskii, Pavel V.; Glukhov, Ivan V.; Starikova, Zoya A.; Organometallics 26 (2007) 2340–; doi:10.1021/om0611756

data_4072978
_publ_contact_author             'Vladimir I. Bregadze'
_publ_section_title
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 Palladium-Catalyzed Amination of 2-Iodo-para-carborane
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_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2340
_journal_paper_doi               10.1021/om0611756
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         C2B10H11(C12H8N)
_chemical_formula_sum            'C14 H19 B10 N'
_chemical_formula_weight         309.40
_chemical_melting_point          166.5(5)
_chemical_name_common
1-(1,12-dicarba-closo-dodecaboran-2-yl)carbazole
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.420(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.922(4)
_cell_length_b                   7.835(2)
_cell_length_c                   15.145(4)
_cell_measurement_reflns_used    3478
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.74
_cell_volume                     1652.0(8)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12005
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   4(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0016P)^2^+1.1889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                4461
_reflns_number_total             6343
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0611756si20070213_010000.cif
_cod_data_source_block           bk1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '166-167' was changed to '166.5(5)' -
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1651.9(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4072978