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_4311102
_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            'C82 H92 Al8 Br6 N2'
_chemical_formula_weight         1800.88
_chemical_name_systematic
; 
 ? 
;
_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                90.00
_cell_angle_beta                 95.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.822(2)
_cell_length_b                   15.823(3)
_cell_length_c                   21.216(4)
_cell_measurement_temperature    140(2)
_cell_volume                     3950.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1936
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57236
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    3.183
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.797
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6830
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                4564
_reflns_number_total             6830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035460isi20040216_055410_4.cif
_cod_data_source_block           r1117a_cmpd15
_cod_original_cell_volume        3949.9(14)
_cod_database_code               4311102