Reaction of m-Terphenyldichlorophosphanes with Sodium Azide: Synthesis and Characterization of Stable Azidocyclophosphazenes
Rudolf J. Wehmschulte; Masood A. Khan; Shawn I. Hossain; Inorganic Chemistry 40 (2001) 2756–2762; doi:10.1021/ic0014538

data_4319787
_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
;
 Reaction of m-Terphenyldichlorophosphanes with Sodium Azide: Synthesis
 and Characterization of Stable Azidocyclophosphazenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2756
_journal_page_last               2762
_journal_paper_doi               10.1021/ic0014538
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C26 H29 Cl2 P'
_chemical_formula_weight         443.36
_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
_cell_angle_alpha                104.920(10)
_cell_angle_beta                 96.180(10)
_cell_angle_gamma                93.330(10)
_cell_formula_units_Z            4
_cell_length_a                   11.9310(10)
_cell_length_b                   12.135(2)
_cell_length_c                   17.230(2)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      4.68
_cell_volume                     2386.9(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS (Siemens 1994a)'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL (Siemens 1994b)'
_diffrn_ambient_temperature      173(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
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9558
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+1.3200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1144
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                6905
_reflns_number_total             8255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0014538_2.cif
_cod_data_source_block           rw921a
_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^)+(0.0489P)^2^+1.3200P] 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^)+(0.0489P)^2^+1.3200P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319787