Syntheses and Structures of Bis(azido)- and Bis(tert-butoxy)cyclodistibazanes
Dana C. Haagenson; Lothar Stahl; Richard J. Staples; Inorganic Chemistry 40 (2001) 4491–4493; doi:10.1021/ic010247c

data_4320095
_publ_section_title
;
 Syntheses and Structures of Bis(azido)- and
 Bis(tert-butoxy)cyclodistibazanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4491
_journal_page_last               4493
_journal_paper_doi               10.1021/ic010247c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C8 H18 N8 Sb2'
_chemical_formula_weight         469.80
_chemical_name_systematic
;
Bis(tert-butoxy)cyclodistibazanes
;
_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-97
_cell_angle_alpha                99.401(6)
_cell_angle_beta                 97.796(5)
_cell_angle_gamma                100.969(5)
_cell_formula_units_Z            1
_cell_length_a                   6.6242(9)
_cell_length_b                   6.9198(9)
_cell_length_c                   8.969(1)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      18.45
_cell_measurement_theta_min      2.29
_cell_volume                     392.25(9)
_computing_cell_refinement       'SMART (Bruker, V4.050, 1995)'
_computing_data_collection       'ASTRO (Bruker, V4.050, 1995)'
_computing_data_reduction        'SAINT (Bruker, V5.A06, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998, ver 5.10)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_method       '\w, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2461
_diffrn_reflns_theta_full        27.78
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.442
_exptl_absorpt_correction_T_max  0.9187
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Light_yellow
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                1474
_reflns_number_total             1581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010247c_2.cif
_cod_data_source_block           ls35a_COMPOUND_3
_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 
;
_cod_original_cell_volume        392.26(9)
_cod_database_code               4320095