Reaction of 2,4,6-Triazido-1,3,5-triazine with Triphenylphosphane. Syntheses and Characterization of the Novel 2-Triphenylphosphanimino-4-azidotetrazolo[5,1-a]-[1,3,5]triazine and 2,4,6-Tris(triphenylphosphanimino)-1,3,5-triazine
Elmar Kessenich; Kurt Polborn; Axel Schulz; Inorganic Chemistry 40 (2001) 1102–1109; doi:10.1021/ic000526k

data_4319339
_publ_section_title
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 Reaction of 2,4,6-Triazido-1,3,5-triazine with Triphenylphosphane.
 Syntheses and Characterization of the Novel
 2-Triphenylphosphanimino-4-azidotetrazolo[5,1-a]-[1,3,5]triazine and
 2,4,6-Tris(triphenylphosphanimino)-1,3,5-triazine
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1102
_journal_page_last               1109
_journal_paper_doi               10.1021/ic000526k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C57 H45 N6 P3'
_chemical_formula_weight         906.90
_space_group_IT_number           2
_symmetry_cell_setting           anorthic
_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                108.990(15)
_cell_angle_beta                 91.612(13)
_cell_angle_gamma                111.66(2)
_cell_formula_units_Z            4
_cell_length_a                   14.705(3)
_cell_length_b                   17.705(4)
_cell_length_c                   21.528(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      9
_cell_volume                     4855.0(19)
_computing_cell_refinement       CAD4(Nonius,_1977)
_computing_data_collection       CAD4(Nonius,_1977)
_computing_data_reduction        process_MOLEN(Fair,_1990)
_computing_molecular_graphics    ZORTEP(Zsolnai,_1994)
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius_MACH3
_diffrn_measurement_method       \o-2\T-scan
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15650
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9853
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         15185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_obs          0.0636
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+7.5062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1637
_refine_ls_wR_factor_obs         0.1434
_reflns_number_observed          10676
_reflns_number_total             15185
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000526k_1.cif
_cod_data_source_block           kesse10
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+7.5062P] 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^)+(0.0561P)^2^+7.5062P] 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        4854.9(16)
_cod_database_code               4319339