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_4311101
_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            'C96 H108 Al8 F6 N2'
_chemical_formula_weight         1619.68
_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                 102.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.642(2)
_cell_length_b                   31.900(6)
_cell_length_c                   11.986(2)
_cell_measurement_temperature    133(2)
_cell_volume                     4341.6(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.1153
_diffrn_reflns_av_sigmaI/netI    0.1474
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27552
_diffrn_reflns_theta_full        24.78
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.154
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                3777
_reflns_number_total             7294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035460isi20040216_055410_3.cif
_cod_data_source_block           as448_cmpd13
_cod_original_cell_volume        4341.5(15)
_cod_database_code               4311101