Synthesis of cyclo-2,4,6-Triarsa-1,3,5-triazanes from cyclo-2,4-Diarsa-1,3-diazanes Demonstrating the General Influence of Substituent Steric Strain on the Relative Stability of Pnictazane Oligomers
Neil Burford; Jeff C. Landry; Michael J. Ferguson; Robert McDonald; Inorganic Chemistry 44 (2005) 5897–5902; doi:10.1021/ic050532m

data_4309352
_publ_contact_author_address
;Department of Chemistry
Dalhousie University
Halifax, NS. CANADA
B3H 4J3
;
_publ_contact_author_email       neil.burford@dal.ca
_publ_contact_author_fax         902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       902-494-3190
_publ_section_title
;
Synthesis of cyclo-2,4,6-Triarsa-1,3,5-triazanes
from cyclo-2,4-Diarsa-1,3-diazanes Demonstrating the General Influence of
Substituent Steric Strain on the Relative Stability of Pnictazane Oligomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5897
_journal_page_last               5902
_journal_paper_doi               10.1021/ic050532m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H46 As2 Cl2 N2'
_chemical_formula_sum            'C36 H46 As2 Cl2 N2'
_chemical_formula_weight         727.49
_chemical_melting_point          505.5(15)
_chemical_name_common            'DippNAsCl Dimer'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   22.8454(16)
_cell_length_b                   10.2167(7)
_cell_length_c                   15.6939(11)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.414
_cell_measurement_theta_min      2.378
_cell_volume                     3663.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27542
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  0.5858
_exptl_absorpt_correction_T_min  0.4413
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.1181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                3316
_reflns_number_total             3983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050532msi20050407_085836_1.cif
_cod_data_source_block           dal0458
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value '504-507' changed to '505.5(15)' - took
average value and fixed precision.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 
;
_cod_database_code               4309352