Bulky triazenide complexes of alumino- and gallohydrides
Alexander, Sean G.; Cole, Marcus L.; Forsyth, Craig M.; Furfari, Samantha K.; Konstas, Kristina; Dalton Transactions  (2009) 2326–2336; doi:10.1039/b817397d

data_7000829
_publ_section_title
;
 Bulky triazenide complexes of alumino- and gallohydrides
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2326
_journal_page_last               2336
_journal_paper_doi               10.1039/b817397d
_journal_year                    2009
_chemical_compound_source        Et2O
_chemical_formula_moiety         'C62 H64 Al N6'
_chemical_formula_sum            'C62 H64 Al N6'
_chemical_formula_weight         921.18
_chemical_melting_point          '426-430 (dec. 443)'
_chemical_name_common            (AlH(DmpN3pTol)2)
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      81
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1771(11)
_cell_length_b                   15.1771(11)
_cell_length_c                   11.6305(7)
_cell_measurement_reflns_used    20930
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      2.21
_cell_volume                     2679.0(3)
_computing_cell_refinement       'Bruker Scalepack'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20930
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9935
_exptl_absorpt_correction_T_min  0.9798
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker Scalepack'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         7151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0477P)^2^+0.2577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                5332
_reflns_number_total             7151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817397d.txt
_cod_data_source_block           Compound3b
_cod_database_code               7000829