A Bromine Adduct of 2,3,6,7,14,15-Hexamethyl-9,10-distibatriptycene. The First Stibonium‒Stiborate Zwitterion
Yosuke Uchiyama; Gaku Yamamoto; Chemistry Letters 34 (2005) 966–; doi:10.1246/cl.2005.966

data_8000057
_publ_section_title
;
 A Bromine Adduct of 2,3,6,7,14,15-Hexamethyl-9,10-distibatriptycene.
 The First Stibonium--Stiborate Zwitterion
;
_journal_issue                   7
_journal_name_full               'Chemistry Letters'
_journal_page_first              966
_journal_paper_doi               10.1246/cl.2005.966
_journal_volume                  34
_journal_year                    2005
_chemical_formula_moiety         'C24 H24 Br4 Sb2, C H Cl3'
_chemical_formula_sum            'C25 H25 Br4 Cl3 Sb2'
_chemical_formula_weight         994.94
_chemical_melting_point          203.5(5)
_chemical_name_common            'bromine adduct'
_chemical_name_systematic
; 
9,9,9,10-tetrabromo-2,3,6,7,14,15-hexamethyl-9,10-
distibatriptycene 
;
_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                90.0000(7)
_cell_angle_beta                 100.1844(8)
_cell_angle_gamma                90.0000(7)
_cell_formula_units_Z            4
_cell_length_a                   11.0798(4)
_cell_length_b                   18.9219(7)
_cell_length_c                   14.3459(8)
_cell_measurement_temperature    113(2)
_cell_volume                     2960.2(2)
_computing_cell_refinement       Crystalclear
_computing_data_collection       Crystalclear
_computing_data_reduction        YadokariXG
_computing_molecular_graphics    'ORTEP-III ver.1.0.3'
_computing_publication_material  YadaokariXG
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19685
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    7.510
_exptl_absorpt_correction_T_max  0.3151
_exptl_absorpt_correction_T_min  0.3151
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                5585
_reflns_number_total             5973
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '203-204' was changed to '203.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               8000057