Reactions of AlH3.NMe3 with Nitriles: Structural Characterization and Substitution Reactions of Hexameric Aluminum Imides
N. Dastagiri Reddy; Herbert W. Roesky; Mathias Noltemeyer; Hans-Georg Schmidt; Inorganic Chemistry 41 (2002) 2374–2378; doi:10.1021/ic011101g

data_4317933
_publ_section_title
;
 Reactions of AlH3.NMe3 with Nitriles: Structural Characterization and
 Substitution Reactions of Hexameric Aluminum Imides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2374
_journal_page_last               2378
_journal_paper_doi               10.1021/ic011101g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C97 H80 Al6 N6'
_chemical_formula_weight         1491.55
_chemical_melting_point          293
_chemical_name_systematic
;
  Compound 5
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.842(5)
_cell_length_b                   15.443(3)
_cell_length_c                   20.699(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     7945(3)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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    0.0188
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8878
_diffrn_reflns_theta_full        27.73
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.9240
_exptl_absorpt_correction_T_min  0.8778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8878
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0896
_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^)+(0.0002P)^2^+77.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                8102
_reflns_number_total             8878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011101g_4.cif
_cod_data_source_block           ready
_cod_database_code               4317933