#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319786.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319786
loop_
_publ_author_name
'Rudolf J. Wehmschulte'
'Masood A. Khan'
'Shawn I. Hossain'
_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            'C48 H50 N8 P2'
_chemical_formula_weight         800.90
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.555(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.874(3)
_cell_length_b                   10.767(3)
_cell_length_c                   18.868(4)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.84
_cell_volume                     2164.3(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω 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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5420
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1381P)²+2.6849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2204
_reflns_number_gt                2998
_reflns_number_total             3785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0014538_1.cif
_cod_data_source_block           rw054e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        2164.2(9)
_cod_database_code               4319786
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.41866(8) 0.04974(7) 0.96874(4) 0.0216(3) Uani 1 1 d . . .
N1 N 0.4536(3) 0.0038(3) 1.05317(15) 0.0293(7) Uani 1 1 d . . .
N2 N 0.2850(3) -0.0117(3) 0.92050(19) 0.0386(8) Uani 1 1 d . . .
N3 N 0.2779(3) -0.1253(3) 0.91732(18) 0.0345(8) Uani 1 1 d . . .
N4 N 0.2615(4) -0.2278(3) 0.9113(2) 0.0569(11) Uani 1 1 d . . .
C1 C 0.0427(4) 0.0552(4) 1.1984(2) 0.0417(10) Uani 1 1 d . . .
H1C H -0.0038 -0.0177 1.1763 0.063 Uiso 1 1 calc R . .
H1D H -0.0165 0.1174 1.2096 0.063 Uiso 1 1 calc R . .
H1E H 0.1000 0.0304 1.2431 0.063 Uiso 1 1 calc R . .
C2 C 0.1171(3) 0.1098(3) 1.1466(2) 0.0320(8) Uani 1 1 d . . .
C3 C 0.2395(3) 0.1498(3) 1.1711(2) 0.0315(8) Uani 1 1 d . . .
H3A H 0.2761 0.1404 1.2209 0.038 Uiso 1 1 calc R . .
C4 C 0.3102(3) 0.2029(3) 1.12586(19) 0.0280(8) Uani 1 1 d . . .
C5 C 0.2571(3) 0.2162(3) 1.05284(18) 0.0256(7) Uani 1 1 d . . .
C6 C 0.1322(3) 0.1795(3) 1.02656(19) 0.0283(8) Uani 1 1 d . . .
C7 C 0.0653(3) 0.1259(3) 1.0743(2) 0.0334(8) Uani 1 1 d . . .
H7A H -0.0186 0.0996 1.0565 0.040 Uiso 1 1 calc R . .
C8 C 0.4424(3) 0.2436(4) 1.1567(2) 0.0374(9) Uani 1 1 d . . .
H8A H 0.4719 0.2985 1.1222 0.056 Uiso 1 1 calc R . .
H8B H 0.4970 0.1705 1.1658 0.056 Uiso 1 1 calc R . .
H8C H 0.4444 0.2882 1.2022 0.056 Uiso 1 1 calc R . .
C9 C 0.0677(3) 0.2013(4) 0.9492(2) 0.0373(9) Uani 1 1 d . . .
H9A H 0.1203 0.1693 0.9167 0.056 Uiso 1 1 calc R . .
H9B H 0.0543 0.2906 0.9409 0.056 Uiso 1 1 calc R . .
H9C H -0.0134 0.1584 0.9395 0.056 Uiso 1 1 calc R . .
C10 C 0.3244(3) 0.2783(3) 1.00050(18) 0.0248(7) Uani 1 1 d . . .
C11 C 0.3162(4) 0.4066(3) 0.9937(2) 0.0344(8) Uani 1 1 d . . .
H11A H 0.2772 0.4531 1.0259 0.041 Uiso 1 1 calc R . .
C12 C 0.3639(4) 0.4677(3) 0.9407(2) 0.0375(9) Uani 1 1 d . . .
H12A H 0.3612 0.5558 0.9382 0.045 Uiso 1 1 calc R . .
C13 C 0.4155(3) 0.4010(3) 0.8915(2) 0.0330(8) Uani 1 1 d . . .
H13A H 0.4444 0.4436 0.8539 0.040 Uiso 1 1 calc R . .
C14 C 0.4257(3) 0.2726(3) 0.89595(18) 0.0259(7) Uani 1 1 d . . .
C15 C 0.3851(3) 0.2121(3) 0.95320(17) 0.0220(7) Uani 1 1 d . . .
C16 C 0.4697(3) 0.2054(3) 0.83650(18) 0.0259(7) Uani 1 1 d . . .
C17 C 0.5968(3) 0.1926(3) 0.83510(19) 0.0290(8) Uani 1 1 d . . .
C18 C 0.6311(4) 0.1354(3) 0.7763(2) 0.0360(9) Uani 1 1 d . . .
H18A H 0.7179 0.1265 0.7758 0.043 Uiso 1 1 calc R . .
C19 C 0.5443(4) 0.0908(4) 0.7182(2) 0.0390(9) Uani 1 1 d . . .
C20 C 0.4191(4) 0.1040(4) 0.7209(2) 0.0395(9) Uani 1 1 d . . .
H20A H 0.3578 0.0727 0.6820 0.047 Uiso 1 1 calc R . .
C21 C 0.3791(3) 0.1614(4) 0.77838(19) 0.0322(8) Uani 1 1 d . . .
C22 C 0.6972(4) 0.2380(4) 0.8963(2) 0.0425(10) Uani 1 1 d . . .
H22A H 0.6598 0.2931 0.9275 0.064 Uiso 1 1 calc R . .
H22B H 0.7610 0.2836 0.8767 0.064 Uiso 1 1 calc R . .
H22C H 0.7364 0.1669 0.9245 0.064 Uiso 1 1 calc R . .
C23 C 0.2407(4) 0.1806(4) 0.7749(2) 0.0446(10) Uani 1 1 d . . .
H23A H 0.1928 0.1390 0.7319 0.067 Uiso 1 1 calc R . .
H23B H 0.2218 0.2697 0.7721 0.067 Uiso 1 1 calc R . .
H23C H 0.2174 0.1457 0.8183 0.067 Uiso 1 1 calc R . .
C24 C 0.5852(5) 0.0337(5) 0.6537(3) 0.0568(13) Uani 1 1 d . . .
H24A H 0.5402 -0.0445 0.6410 0.085 Uiso 1 1 calc R . .
H24B H 0.6757 0.0176 0.6656 0.085 Uiso 1 1 calc R . .
H24C H 0.5664 0.0911 0.6126 0.085 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N1 95.52(14) 3_657 . ?
N1 P1 N2 114.18(17) 3_657 . ?
N1 P1 N2 114.41(17) . . ?
N1 P1 C15 117.23(15) 3_657 . ?
N1 P1 C15 116.88(15) . . ?
N2 P1 C15 99.69(15) . . ?
N1 P1 P1 47.90(10) 3_657 3_657 ?
N1 P1 P1 47.62(10) . 3_657 ?
N2 P1 P1 127.74(12) . 3_657 ?
C15 P1 P1 132.57(12) . 3_657 ?
P1 N1 P1 84.48(14) 3_657 . ?
N3 N2 P1 117.1(3) . . ?
N4 N3 N2 174.2(4) . . ?
C7 C2 C3 117.7(3) . . ?
C7 C2 C1 121.7(4) . . ?
C3 C2 C1 120.5(4) . . ?
C4 C3 C2 122.5(3) . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 C8 119.2(3) . . ?
C5 C4 C8 121.9(3) . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 C10 122.6(3) . . ?
C6 C5 C10 117.2(3) . . ?
C7 C6 C5 118.8(3) . . ?
C7 C6 C9 119.3(3) . . ?
C5 C6 C9 121.8(3) . . ?
C2 C7 C6 122.0(3) . . ?
C11 C10 C15 118.4(3) . . ?
C11 C10 C5 118.3(3) . . ?
C15 C10 C5 123.0(3) . . ?
C12 C11 C10 121.0(3) . . ?
C13 C12 C11 120.1(3) . . ?
C12 C13 C14 121.0(3) . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 C16 118.1(3) . . ?
C15 C14 C16 123.3(3) . . ?
C14 C15 C10 120.8(3) . . ?
C14 C15 P1 119.4(2) . . ?
C10 C15 P1 119.7(2) . . ?
C17 C16 C21 119.7(3) . . ?
C17 C16 C14 122.0(3) . . ?
C21 C16 C14 118.1(3) . . ?
C18 C17 C16 119.1(3) . . ?
C18 C17 C22 119.3(3) . . ?
C16 C17 C22 121.6(3) . . ?
C19 C18 C17 122.6(4) . . ?
C20 C19 C18 117.2(4) . . ?
C20 C19 C24 121.6(4) . . ?
C18 C19 C24 121.1(4) . . ?
C19 C20 C21 122.6(4) . . ?
C20 C21 C16 118.7(3) . . ?
C20 C21 C23 119.5(4) . . ?
C16 C21 C23 121.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.631(3) 3_657 ?
P1 N1 1.639(3) . ?
P1 N2 1.687(3) . ?
P1 C15 1.798(3) . ?
P1 P1 2.1982(17) 3_657 ?
N1 P1 1.631(3) 3_657 ?
N2 N3 1.226(4) . ?
N3 N4 1.121(5) . ?
C1 C2 1.508(5) . ?
C2 C7 1.378(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.382(5) . ?
C4 C5 1.390(5) . ?
C4 C8 1.504(5) . ?
C5 C6 1.406(5) . ?
C5 C10 1.499(5) . ?
C6 C7 1.392(5) . ?
C6 C9 1.507(5) . ?
C10 C11 1.389(5) . ?
C10 C15 1.406(5) . ?
C11 C12 1.380(5) . ?
C12 C13 1.380(5) . ?
C13 C14 1.388(5) . ?
C14 C15 1.406(5) . ?
C14 C16 1.492(5) . ?
C16 C17 1.395(5) . ?
C16 C21 1.401(5) . ?
C17 C18 1.384(5) . ?
C17 C22 1.503(5) . ?
C18 C19 1.381(6) . ?
C19 C20 1.380(6) . ?
C19 C24 1.508(6) . ?
C20 C21 1.391(5) . ?
C21 C23 1.508(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P1 N1 P1 119.72(16) . . . 3_657 ?
C15 P1 N1 P1 -124.35(15) . . . 3_657 ?
N1 P1 N2 N3 51.7(4) 3_657 . . . ?
N1 P1 N2 N3 -57.0(4) . . . . ?
C15 P1 N2 N3 177.5(3) . . . . ?
P1 P1 N2 N3 -2.7(4) 3_657 . . . ?
P1 N2 N3 N4 176(4) . . . . ?
C7 C2 C3 C4 -0.9(5) . . . . ?
C1 C2 C3 C4 -178.5(3) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
C2 C3 C4 C8 -179.8(3) . . . . ?
C3 C4 C5 C6 2.0(5) . . . . ?
C8 C4 C5 C6 -178.6(3) . . . . ?
C3 C4 C5 C10 176.9(3) . . . . ?
C8 C4 C5 C10 -3.6(5) . . . . ?
C4 C5 C6 C7 -2.3(5) . . . . ?
C10 C5 C6 C7 -177.5(3) . . . . ?
C4 C5 C6 C9 175.1(3) . . . . ?
C10 C5 C6 C9 -0.1(5) . . . . ?
C3 C2 C7 C6 0.5(5) . . . . ?
C1 C2 C7 C6 178.1(3) . . . . ?
C5 C6 C7 C2 1.1(5) . . . . ?
C9 C6 C7 C2 -176.4(3) . . . . ?
C4 C5 C10 C11 -85.8(4) . . . . ?
C6 C5 C10 C11 89.3(4) . . . . ?
C4 C5 C10 C15 100.5(4) . . . . ?
C6 C5 C10 C15 -84.4(4) . . . . ?
C15 C10 C11 C12 1.4(6) . . . . ?
C5 C10 C11 C12 -172.6(3) . . . . ?
C10 C11 C12 C13 3.0(6) . . . . ?
C11 C12 C13 C14 -2.9(6) . . . . ?
C12 C13 C14 C15 -1.6(5) . . . . ?
C12 C13 C14 C16 173.6(3) . . . . ?
C13 C14 C15 C10 6.2(5) . . . . ?
C16 C14 C15 C10 -168.8(3) . . . . ?
C13 C14 C15 P1 -170.6(3) . . . . ?
C16 C14 C15 P1 14.4(4) . . . . ?
C11 C10 C15 C14 -6.1(5) . . . . ?
C5 C10 C15 C14 167.6(3) . . . . ?
C11 C10 C15 P1 170.7(3) . . . . ?
C5 C10 C15 P1 -15.6(4) . . . . ?
N1 P1 C15 C14 30.2(3) 3_657 . . . ?
N1 P1 C15 C14 142.6(3) . . . . ?
N2 P1 C15 C14 -93.6(3) . . . . ?
P1 P1 C15 C14 86.7(3) 3_657 . . . ?
N1 P1 C15 C10 -146.7(2) 3_657 . . . ?
N1 P1 C15 C10 -34.2(3) . . . . ?
N2 P1 C15 C10 89.6(3) . . . . ?
P1 P1 C15 C10 -90.1(3) 3_657 . . . ?
C13 C14 C16 C17 83.5(4) . . . . ?
C15 C14 C16 C17 -101.5(4) . . . . ?
C13 C14 C16 C21 -92.3(4) . . . . ?
C15 C14 C16 C21 82.7(4) . . . . ?
C21 C16 C17 C18 -0.6(5) . . . . ?
C14 C16 C17 C18 -176.3(3) . . . . ?
C21 C16 C17 C22 -179.8(3) . . . . ?
C14 C16 C17 C22 4.4(5) . . . . ?
C16 C17 C18 C19 0.4(6) . . . . ?
C22 C17 C18 C19 179.7(4) . . . . ?
C17 C18 C19 C20 -0.7(6) . . . . ?
C17 C18 C19 C24 177.5(4) . . . . ?
C18 C19 C20 C21 1.1(6) . . . . ?
C24 C19 C20 C21 -177.0(4) . . . . ?
C19 C20 C21 C16 -1.3(6) . . . . ?
C19 C20 C21 C23 175.6(4) . . . . ?
C17 C16 C21 C20 1.0(5) . . . . ?
C14 C16 C21 C20 176.9(3) . . . . ?
C17 C16 C21 C23 -175.8(3) . . . . ?
C14 C16 C21 C23 0.1(5) . . . . ?
