Novel Aluminum Hydride Derivatives from the Reaction of H~3~Al.NMe~3~ with the Cyclosilazanes [Me~2~SiNH]~3~ and [Me~2~SiNH]~4~
Ulrike Fooken; Masood A. Khan; Rudolf. J. Wehmschulte; Inorganic Chemistry 40 (2001) 1316–1322; doi:10.1021/ic000636r

data_4319343
_publ_contact_author_address
;       Department of Chemistry and Biochemistry
         University of Oklahoma
         620 Parrington Oval, Room 208
         Norman, OK 73019
;
_publ_contact_author_email       rjwehmschulte@ou.edu
_publ_contact_author_fax         '405 325 6111'
_publ_contact_author_name        'Rudolf J. Wehmschulte'
_publ_contact_author_phone       '405 325 2388'
_publ_section_title
;
 Novel Aluminum Hydride Derivatives from the Reaction of H~3~Al.NMe~3~
 with the Cyclosilazanes [Me~2~SiNH]~3~ and [Me~2~SiNH]~4~
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1316
_journal_page_last               1322
_journal_paper_doi               10.1021/ic000636r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C23.5 H79.5 Al6 N10 Si8'
_chemical_formula_weight         889.07
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                75.199(14)
_cell_angle_beta                 82.330(13)
_cell_angle_gamma                86.936(15)
_cell_formula_units_Z            2
_cell_length_a                   13.094(2)
_cell_length_b                   13.111(3)
_cell_length_c                   16.595(3)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      15.78
_cell_measurement_theta_min      3.75
_cell_volume                     2729.2(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       prism
_exptl_crystal_F_000             961
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         9492
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_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_obs          0.0614
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+0.9470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1977
_refine_ls_wR_factor_obs         0.1581
_reflns_number_observed          6815
_reflns_number_total             9512
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000636r_1.cif
_cod_data_source_block           rw956a(COMPOUND6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+0.9470P] 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^)+(0.1080P)^2^+0.9470P] 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        2729.3(8)
_cod_original_formula_sum        'C23.50 H79.50 Al6 N10 Si8'
_cod_database_code               4319343