Synthesis of Carbaalane Halogen Derivatives
Andreas Stasch; Herbert W. Roesky; Denis Vidovic; Jörg Magull; Hans-Georg Schmidt; Mathias Noltemeyer; Inorganic Chemistry 43 (2004) 3625–3630; doi:10.1021/ic035460i

data_4311099
_publ_section_title
;
 Synthesis of Carbaalane Halogen Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3625
_journal_page_last               3630
_journal_paper_doi               10.1021/ic035460i
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C54 H108 Al8 I6 N2 Si6'
_chemical_formula_weight         1931.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.4323(10)
_cell_length_b                   15.4323(10)
_cell_length_c                   29.624(2)
_cell_measurement_temperature    133(2)
_cell_volume                     6109.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            22379
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_T_max  0.6353
_exptl_absorpt_correction_T_min  0.4353
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.000073(18)
_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   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0153
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+10.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0380
_reflns_number_gt                2366
_reflns_number_total             2479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035460isi20040216_055410_1.cif
_cod_data_source_block           r1118_cmpd11
_cod_original_cell_volume        6109.8(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4311099