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_4311100
_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            'C63 H122 Al8 Br2.38 Cl1.62 N2 Si6'
_chemical_formula_weight         1539.62
_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                 90.59(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.732(3)
_cell_length_b                   12.9036(17)
_cell_length_c                   21.286(7)
_cell_measurement_temperature    200(2)
_cell_volume                     4320.8(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4701
_diffrn_reflns_theta_full        22.44
_diffrn_reflns_theta_max         22.44
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.6118
_exptl_absorpt_correction_T_min  0.5491
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1626
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4701
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0500P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                2897
_reflns_number_total             4701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035460isi20040216_055410_2.cif
_cod_data_source_block           r1011b_cmpd12
_cod_original_cell_volume        4320.9(16)
_cod_database_code               4311100