#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/44/4114479.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_4114479
loop_
_publ_author_name
'June-Ho Jung'
'Julia C. Pomeroy'
'Hongming Zhang'
'Patty Wisian-Neilson'
_publ_section_title
;
 Isolation and Characterization of Nongeminal Cyclic
 Methylphenylphosphazene Tetramers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15537
_journal_page_last               15542
_journal_paper_doi               10.1021/ja0374168
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C28 H32 N4 P4'
_chemical_formula_weight         548.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.967(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3078(6)
_cell_length_b                   15.5628(7)
_cell_length_c                   14.3446(7)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2856.2(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.025
_diffrn_reflns_av_sigmaI/netI    0.044
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5192
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        12.96
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  n/a
_exptl_absorpt_correction_T_min  n/a
_exptl_absorpt_correction_type   n/a
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rods
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.23
_refine_diff_density_rms         0.04
_refine_ls_extinction_coef       0.0007(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0532P)²+0.8535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                3901
_reflns_number_total             4963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0374168si20030720_085114.cif
_cod_data_source_block           jh-trmet4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.8535P] 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^)+(0.0532P)^2^+0.8535P] 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               4114479
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
_atom_site_refinement_flags
P1 P 0.98039(5) 0.17339(4) 0.18415(4) 0.03932(17) Uani 1 d .
P2 P 0.90853(5) -0.00144(4) 0.13713(4) 0.03841(17) Uani 1 d .
P3 P 0.80462(5) 0.02078(4) 0.28775(4) 0.03816(17) Uani 1 d .
P4 P 0.78787(5) 0.20073(4) 0.23847(5) 0.04140(18) Uani 1 d .
N1 N 0.94032(15) 0.09370(13) 0.11423(14) 0.0429(5) Uani 1 d .
N2 N 0.88749(15) -0.02095(13) 0.23953(14) 0.0453(5) Uani 1 d .
N3 N 0.74391(16) 0.10613(13) 0.24387(16) 0.0474(5) Uani 1 d .
N4 N 0.90811(16) 0.21408(14) 0.24485(17) 0.0509(5) Uani 1 d .
C1 C 1.0119(2) 0.25564(19) 0.1087(2) 0.0612(8) Uani 1 d .
H1A H 1.0351 0.3063 0.1468 0.092 Uiso 1 calc R
H1B H 0.9510 0.2690 0.0569 0.092 Uiso 1 calc R
H1C H 1.0665 0.2355 0.0822 0.092 Uiso 1 calc R
C2 C 1.0088(2) -0.07568(18) 0.1289(2) 0.0561(7) Uani 1 d .
H2A H 0.9871 -0.1331 0.1382 0.084 Uiso 1 calc R
H2B H 1.0721 -0.0625 0.1779 0.084 Uiso 1 calc R
H2C H 1.0207 -0.0711 0.0660 0.084 Uiso 1 calc R
C3 C 0.8726(2) 0.0328(2) 0.41475(18) 0.0578(7) Uani 1 d .
H3A H 0.8248 0.0532 0.4491 0.087 Uiso 1 calc R
H3B H 0.9286 0.0733 0.4218 0.087 Uiso 1 calc R
H3C H 0.9005 -0.0218 0.4407 0.087 Uiso 1 calc R
C4 C 0.7648(2) 0.26627(19) 0.3342(2) 0.0586(7) Uani 1 d .
H4A H 0.6924 0.2629 0.3328 0.088 Uiso 1 calc R
H4B H 0.7827 0.3248 0.3251 0.088 Uiso 1 calc R
H4C H 0.8071 0.2459 0.3957 0.088 Uiso 1 calc R
C11 C 1.10332(17) 0.14834(15) 0.27312(17) 0.0408(5) Uani 1 d .
C12 C 1.1830(2) 0.10705(19) 0.2451(2) 0.0578(7) Uani 1 d .
H12 H 1.1741 0.0935 0.1802 0.069 Uiso 1 calc R
C13 C 1.2754(2) 0.0860(2) 0.3132(3) 0.0720(9) Uani 1 d .
H13 H 1.3276 0.0574 0.2938 0.086 Uiso 1 calc R
C14 C 1.2907(2) 0.1069(2) 0.4093(2) 0.0710(9) Uani 1 d .
H14 H 1.3534 0.0934 0.4544 0.085 Uiso 1 calc R
C15 C 1.2132(2) 0.1478(2) 0.4382(2) 0.0661(8) Uani 1 d .
H15 H 1.2231 0.1616 0.5032 0.079 Uiso 1 calc R
C16 C 1.1197(2) 0.16864(17) 0.37040(19) 0.0522(6) Uani 1 d .
H16 H 1.0675 0.1966 0.3905 0.063 Uiso 1 calc R
C21 C 0.79488(19) -0.02882(15) 0.03889(17) 0.0417(5) Uani 1 d .
C22 C 0.7397(2) 0.03317(18) -0.02342(19) 0.0541(7) Uani 1 d .
H22 H 0.7650 0.0892 -0.0190 0.065 Uiso 1 calc R
C23 C 0.6474(2) 0.0132(2) -0.0923(2) 0.0737(9) Uani 1 d .
H23 H 0.6109 0.0557 -0.1335 0.088 Uiso 1 calc R
C24 C 0.6097(3) -0.0691(3) -0.0999(2) 0.0772(10) Uani 1 d .
H24 H 0.5473 -0.0824 -0.1458 0.093 Uiso 1 calc R
C25 C 0.6639(3) -0.1322(2) -0.0396(2) 0.0736(9) Uani 1 d .
H25 H 0.6389 -0.1883 -0.0454 0.088 Uiso 1 calc R
C26 C 0.7555(2) -0.11212(18) 0.0297(2) 0.0592(7) Uani 1 d .
H26 H 0.7915 -0.1549 0.0708 0.071 Uiso 1 calc R
C31 C 0.70222(18) -0.05671(15) 0.28729(16) 0.0392(5) Uani 1 d .
C32 C 0.6126(2) -0.03023(19) 0.31146(19) 0.0511(6) Uani 1 d .
H32 H 0.6032 0.0276 0.3232 0.061 Uiso 1 calc R
C33 C 0.5375(2) -0.0895(2) 0.3181(2) 0.0659(8) Uani 1 d .
H33 H 0.4783 -0.0715 0.3352 0.079 Uiso 1 calc R
C34 C 0.5499(2) -0.1751(2) 0.2997(2) 0.0708(9) Uani 1 d .
H34 H 0.4994 -0.2149 0.3046 0.085 Uiso 1 calc R
C35 C 0.6370(2) -0.20140(19) 0.2742(2) 0.0672(8) Uani 1 d .
H35 H 0.6448 -0.2590 0.2607 0.081 Uiso 1 calc R
C36 C 0.7135(2) -0.14269(17) 0.2685(2) 0.0523(6) Uani 1 d .
H36 H 0.7727 -0.1613 0.2519 0.063 Uiso 1 calc R
C41 C 0.70367(17) 0.24780(16) 0.12903(17) 0.0423(6) Uani 1 d .
C42 C 0.7166(2) 0.33303(18) 0.1049(2) 0.0574(7) Uani 1 d .
H42 H 0.7696 0.3658 0.1450 0.069 Uiso 1 calc R
C43 C 0.6517(3) 0.3695(2) 0.0220(2) 0.0698(9) Uani 1 d .
H43 H 0.6613 0.4265 0.0068 0.084 Uiso 1 calc R
C44 C 0.5732(3) 0.3217(2) -0.0377(2) 0.0710(9) Uani 1 d .
H44 H 0.5295 0.3464 -0.0931 0.085 Uiso 1 calc R
C45 C 0.5593(2) 0.2376(2) -0.0157(2) 0.0678(8) Uani 1 d .
H45 H 0.5063 0.2054 -0.0565 0.081 Uiso 1 calc R
C46 C 0.62368(19) 0.20027(19) 0.0672(2) 0.0524(6) Uani 1 d .
H46 H 0.6135 0.1432 0.0816 0.063 Uiso 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_publ_flag
N1 P1 N4 120.36(11) y
N1 P1 C1 105.57(13) y
N4 P1 C1 108.76(14) y
N1 P1 C11 110.84(11) y
N4 P1 C11 105.25(11) y
C1 P1 C11 105.13(12) y
N1 P2 N2 119.21(11) y
N1 P2 C2 109.84(12) y
N2 P2 C2 105.07(12) y
N1 P2 C21 105.63(11) y
N2 P2 C21 110.51(11) y
C2 P2 C21 105.91(13) y
N2 P3 N3 120.35(11) y
N2 P3 C3 105.39(12) y
N3 P3 C3 111.81(13) y
N2 P3 C31 109.62(11) y
N3 P3 C31 104.70(11) y
C3 P3 C31 103.83(12) y
N4 P4 N3 119.64(11) y
N4 P4 C4 105.16(12) y
N3 P4 C4 110.11(13) y
N4 P4 C41 111.66(12) y
N3 P4 C41 105.52(11) y
C4 P4 C41 103.69(13) y
P1 N1 P2 130.83(13) y
P3 N2 P2 129.72(13) y
P3 N3 P4 129.56(13) y
P4 N4 P1 131.65(14) y
C16 C11 C12 118.3(2) ?
C16 C11 P1 121.25(19) ?
C12 C11 P1 120.43(19) ?
C13 C12 C11 120.4(3) ?
C14 C13 C12 120.6(3) ?
C15 C14 C13 119.8(3) ?
C14 C15 C16 120.0(3) ?
C11 C16 C15 120.9(3) ?
C22 C21 C26 118.1(2) ?
C22 C21 P2 121.37(19) ?
C26 C21 P2 120.3(2) ?
C21 C22 C23 121.0(3) ?
C24 C23 C22 120.0(3) ?
C23 C24 C25 120.1(3) ?
C24 C25 C26 119.9(3) ?
C25 C26 C21 120.9(3) ?
C36 C31 C32 118.8(2) ?
C36 C31 P3 121.44(19) ?
C32 C31 P3 119.7(2) ?
C33 C32 C31 120.3(3) ?
C34 C33 C32 120.3(3) ?
C35 C34 C33 119.7(3) ?
C34 C35 C36 120.5(3) ?
C31 C36 C35 120.4(3) ?
C42 C41 C46 118.1(2) ?
C42 C41 P4 120.7(2) ?
C46 C41 P4 121.2(2) ?
C43 C42 C41 120.9(3) ?
C44 C43 C42 120.0(3) ?
C45 C44 C43 120.1(3) ?
C44 C45 C46 120.4(3) ?
C45 C46 C41 120.4(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P1 N1 1.592(2) y
P1 N4 1.595(2) y
P1 C1 1.799(3) y
P1 C11 1.819(2) y
P2 N1 1.599(2) y
P2 N2 1.598(2) y
P2 C2 1.793(3) y
P2 C21 1.812(2) y
P3 N2 1.593(2) y
P3 N3 1.592(2) y
P3 C3 1.807(3) y
P3 C31 1.818(2) y
P4 N4 1.591(2) y
P4 N3 1.594(2) y
P4 C4 1.803(3) y
P4 C41 1.814(2) y
C11 C16 1.388(3) ?
C11 C12 1.391(4) ?
C12 C13 1.383(4) ?
C13 C14 1.376(5) ?
C14 C15 1.370(5) ?
C15 C16 1.390(4) ?
C21 C22 1.381(4) ?
C21 C26 1.391(3) ?
C22 C23 1.384(4) ?
C23 C24 1.370(5) ?
C24 C25 1.374(5) ?
C25 C26 1.381(4) ?
C31 C36 1.381(4) ?
C31 C32 1.393(3) ?
C32 C33 1.383(4) ?
C33 C34 1.377(5) ?
C34 C35 1.370(5) ?
C35 C36 1.388(4) ?
C41 C42 1.393(4) ?
C41 C46 1.396(4) ?
C42 C43 1.385(4) ?
C43 C44 1.374(5) ?
C44 C45 1.371(5) ?
C45 C46 1.387(4) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4414222
