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_4319347
_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            'C28 H79 Al5 N10 Si8'
_chemical_formula_weight         915.63
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9908(15)
_cell_length_b                   13.937(2)
_cell_length_c                   17.5586(10)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      5.22
_cell_volume                     5381.5(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      178(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       1
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_min         1.85
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
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_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.236
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.32(14)
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1122
_refine_ls_wR_factor_obs         0.0971
_reflns_number_observed          6015
_reflns_number_total             7178
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000636r_5.cif
_cod_data_source_block           rw957a(COMPOUND5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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^)+(0.0524P)^2^+0.0000P] 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^)+(0.0524P)^2^+0.0000P] 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        5381.7(8)
_cod_database_code               4319347