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_4317930
_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            'C42 H48 Al6 N6'
_chemical_formula_weight         798.74
_chemical_melting_point          245
_chemical_name_systematic
;
  Compound 1
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.7457(13)
_cell_length_b                   15.7457(13)
_cell_length_c                   14.949(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3209.7(6)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'STOE AED2'
_diffrn_measurement_method       'profile fitted'
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2020
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         4.18
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.70
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_obs          0.0334
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0890
_refine_ls_wR_factor_obs         0.0861
_reflns_number_observed          786
_reflns_number_total             848
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011101g_1.cif
_cod_data_source_block           roe949
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.8700P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.8700P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3209.8(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4317930