#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/44/4114481.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_4114481
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           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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.353(6)
_cell_angle_beta                 84.901(7)
_cell_angle_gamma                65.694(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2385(8)
_cell_length_b                   10.6957(8)
_cell_length_c                   16.4620(10)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1468.2(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.016
_diffrn_reflns_av_sigmaI/netI    0.045
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5486
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        8.25
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.281
_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    1.241
_exptl_crystal_description       plates
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.26
_refine_diff_density_rms         0.04
_refine_ls_extinction_coef       0.0019(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.063
_refine_ls_R_factor_gt           0.043
_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)+(0.0511P)²+0.4594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.108
_refine_ls_wR_factor_ref         0.116
_reflns_number_gt                3959
_reflns_number_total             5139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0374168si20030720_085218.cif
_cod_data_source_block           jh-ttrnz6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.4594P] 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^)+(0.0511P)^2^+0.4594P] 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               4114481
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.52061(8) 0.18155(7) 0.63089(4) 0.04060(18) Uani 1 d .
P2 P 0.60847(8) 0.10798(7) 0.80370(4) 0.04297(19) Uani 1 d .
P3 P 0.40309(8) 0.39260(7) 0.82871(4) 0.0461(2) Uani 1 d .
P4 P 0.43017(8) 0.46847(6) 0.65648(4) 0.03893(18) Uani 1 d .
N1 N 0.5630(3) 0.0912(2) 0.71712(14) 0.0554(6) Uani 1 d .
N2 N 0.5609(3) 0.2556(2) 0.83363(13) 0.0521(6) Uani 1 d .
N3 N 0.3332(2) 0.4656(2) 0.74144(13) 0.0463(5) Uani 1 d .
N4 N 0.5258(3) 0.3292(2) 0.61590(12) 0.0434(5) Uani 1 d .
C1 C 0.6535(4) 0.0834(3) 0.5539(2) 0.0628(8) Uani 1 d .
H1A H 0.6498 -0.0056 0.5577 0.094 Uiso 1 calc R
H1B H 0.7598 0.0721 0.5624 0.094 Uiso 1 calc R
H1C H 0.6218 0.1312 0.5006 0.094 Uiso 1 calc R
C2 C 0.5334(4) 0.0050(3) 0.8757(2) 0.0705(9) Uani 1 d .
H2A H 0.5686 0.0012 0.9295 0.106 Uiso 1 calc R
H2B H 0.5721 -0.0867 0.8598 0.106 Uiso 1 calc R
H2C H 0.4193 0.0455 0.8764 0.106 Uiso 1 calc R
C3 C 0.4474(4) 0.5077(3) 0.88195(19) 0.0691(9) Uani 1 d .
H3A H 0.3540 0.5915 0.8860 0.104 Uiso 1 calc R
H3B H 0.5307 0.5282 0.8524 0.104 Uiso 1 calc R
H3C H 0.4812 0.4649 0.9360 0.104 Uiso 1 calc R
C4 C 0.2872(4) 0.5896(3) 0.58575(17) 0.0597(8) Uani 1 d .
H4A H 0.2386 0.6776 0.6069 0.090 Uiso 1 calc R
H4B H 0.2071 0.5569 0.5789 0.090 Uiso 1 calc R
H4C H 0.3398 0.5988 0.5337 0.090 Uiso 1 calc R
C11 C 0.3289(3) 0.1904(3) 0.60645(15) 0.0434(6) Uani 1 d .
C12 C 0.2528(4) 0.1192(3) 0.6548(2) 0.0631(8) Uani 1 d .
H12 H 0.2988 0.0668 0.7028 0.076 Uiso 1 calc R
C13 C 0.1087(4) 0.1241(4) 0.6334(3) 0.0803(11) Uani 1 d .
H13 H 0.0592 0.0747 0.6667 0.096 Uiso 1 calc R
C14 C 0.0399(4) 0.2011(4) 0.5637(2) 0.0739(9) Uani 1 d .
H14 H -0.0568 0.2046 0.5492 0.089 Uiso 1 calc R
C15 C 0.1122(4) 0.2729(4) 0.5152(2) 0.0699(9) Uani 1 d .
H15 H 0.0646 0.3255 0.4676 0.084 Uiso 1 calc R
C16 C 0.2554(4) 0.2688(3) 0.53577(17) 0.0571(7) Uani 1 d .
H16 H 0.3033 0.3189 0.5020 0.069 Uiso 1 calc R
C21 C 0.8218(3) 0.0232(2) 0.81407(16) 0.0440(6) Uani 1 d .
C22 C 0.9110(3) -0.0954(3) 0.77743(19) 0.0575(7) Uani 1 d .
H22 H 0.8617 -0.1297 0.7448 0.069 Uiso 1 calc R
C23 C 1.0721(4) -0.1636(3) 0.7885(2) 0.0677(9) Uani 1 d .
H23 H 1.1299 -0.2448 0.7648 0.081 Uiso 1 calc R
C24 C 1.1467(4) -0.1128(4) 0.8338(2) 0.0753(10) Uani 1 d .
H24 H 1.2559 -0.1579 0.8401 0.090 Uiso 1 calc R
C25 C 1.0617(4) 0.0039(4) 0.8699(3) 0.0952(13) Uani 1 d .
H25 H 1.1127 0.0391 0.9010 0.114 Uiso 1 calc R
C26 C 0.8999(4) 0.0706(4) 0.8608(2) 0.0781(11) Uani 1 d .
H26 H 0.8426 0.1495 0.8869 0.094 Uiso 1 calc R
C31 C 0.2393(4) 0.3683(3) 0.88752(17) 0.0568(8) Uani 1 d .
C32 C 0.2537(5) 0.3157(4) 0.9688(2) 0.0985(15) Uani 1 d .
H32 H 0.3476 0.2944 0.9949 0.118 Uiso 1 calc R
C33 C 0.1283(6) 0.2945(4) 1.0120(3) 0.1155(19) Uani 1 d .
H33 H 0.1395 0.2580 1.0667 0.139 Uiso 1 calc R
C34 C -0.0086(6) 0.3259(4) 0.9760(3) 0.1078(17) Uani 1 d .
H34 H -0.0921 0.3118 1.0058 0.129 Uiso 1 calc R
C35 C -0.0248(6) 0.3779(6) 0.8965(3) 0.1172(17) Uani 1 d .
H35 H -0.1195 0.3995 0.8712 0.141 Uiso 1 calc R
C36 C 0.0996(4) 0.3993(4) 0.8523(2) 0.0817(11) Uani 1 d .
H36 H 0.0869 0.4355 0.7976 0.098 Uiso 1 calc R
C41 C 0.5740(3) 0.5400(3) 0.66609(15) 0.0441(6) Uani 1 d .
C42 C 0.7333(4) 0.4562(3) 0.66517(19) 0.0594(8) Uani 1 d .
H42 H 0.7663 0.3647 0.6552 0.071 Uiso 1 calc R
C43 C 0.8453(4) 0.5043(4) 0.6787(3) 0.0813(11) Uani 1 d .
H43 H 0.9526 0.4456 0.6779 0.098 Uiso 1 calc R
C44 C 0.7986(5) 0.6382(4) 0.6933(3) 0.0859(11) Uani 1 d .
H44 H 0.8742 0.6703 0.7031 0.103 Uiso 1 calc R
C45 C 0.6410(5) 0.7254(4) 0.6934(2) 0.0768(10) Uani 1 d .
H45 H 0.6100 0.8168 0.7031 0.092 Uiso 1 calc R
C46 C 0.5272(4) 0.6780(3) 0.67922(19) 0.0617(8) Uani 1 d .
H46 H 0.4203 0.7378 0.6785 0.074 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
N4 P1 N1 120.93(12) y
N4 P1 C1 105.75(13) y
N1 P1 C1 108.05(14) y
N4 P1 C11 111.13(12) y
N1 P1 C11 106.22(13) y
C1 P1 C11 103.39(13) y
N1 P2 N2 121.74(12) y
N1 P2 C2 105.05(16) y
N2 P2 C2 110.51(15) y
N1 P2 C21 110.21(13) y
N2 P2 C21 104.32(12) y
C2 P2 C21 103.70(13) y
N2 P3 N3 119.56(12) y
N2 P3 C3 103.94(14) y
N3 P3 C3 110.58(13) y
N2 P3 C31 111.79(13) y
N3 P3 C31 104.96(13) y
C3 P3 C31 105.25(15) y
N4 P4 N3 119.64(11) y
N4 P4 C4 109.09(13) y
N3 P4 C4 105.59(13) y
N4 P4 C41 105.59(11) y
N3 P4 C41 110.16(12) y
C4 P4 C41 106.06(14) y
P2 N1 P1 137.01(16) y
P3 N2 P2 133.07(16) y
P3 N3 P4 127.52(14) y
P1 N4 P4 132.89(14) y
C12 C11 C16 117.6(3) ?
C12 C11 P1 122.3(2) ?
C16 C11 P1 120.1(2) ?
C11 C12 C13 121.2(3) ?
C14 C13 C12 119.8(3) ?
C15 C14 C13 120.0(3) ?
C14 C15 C16 120.7(3) ?
C15 C16 C11 120.6(3) ?
C26 C21 C22 117.4(3) ?
C26 C21 P2 121.6(2) ?
C22 C21 P2 120.9(2) ?
C23 C22 C21 121.0(3) ?
C24 C23 C22 120.3(3) ?
C23 C24 C25 119.7(3) ?
C24 C25 C26 120.1(3) ?
C21 C26 C25 121.4(3) ?
C36 C31 C32 117.9(3) ?
C36 C31 P3 121.0(2) ?
C32 C31 P3 121.1(3) ?
C31 C32 C33 120.1(4) ?
C34 C33 C32 121.1(4) ?
C33 C34 C35 119.6(4) ?
C34 C35 C36 120.1(5) ?
C31 C36 C35 121.2(4) ?
C42 C41 C46 118.3(3) ?
C42 C41 P4 119.9(2) ?
C46 C41 P4 121.7(2) ?
C41 C42 C43 121.5(3) ?
C44 C43 C42 119.9(3) ?
C43 C44 C45 120.3(3) ?
C44 C45 C46 120.2(3) ?
C45 C46 C41 119.7(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P1 N4 1.586(2) y
P1 N1 1.589(2) y
P1 C1 1.797(3) y
P1 C11 1.813(3) y
P2 N1 1.574(2) y
P2 N2 1.590(2) y
P2 C2 1.799(3) y
P2 C21 1.812(3) y
P3 N2 1.584(2) y
P3 N3 1.594(2) y
P3 C3 1.793(3) y
P3 C31 1.814(3) y
P4 N4 1.588(2) y
P4 N3 1.596(2) y
P4 C4 1.800(3) y
P4 C41 1.812(3) y
C11 C12 1.374(4) ?
C11 C16 1.389(4) ?
C12 C13 1.385(4) ?
C13 C14 1.360(5) ?
C14 C15 1.355(5) ?
C15 C16 1.375(4) ?
C21 C26 1.368(4) ?
C21 C22 1.381(4) ?
C22 C23 1.378(4) ?
C23 C24 1.353(5) ?
C24 C25 1.356(5) ?
C25 C26 1.378(5) ?
C31 C36 1.357(5) ?
C31 C32 1.377(4) ?
C32 C33 1.387(6) ?
C33 C34 1.339(7) ?
C34 C35 1.348(6) ?
C35 C36 1.388(5) ?
C41 C42 1.372(4) ?
C41 C46 1.398(4) ?
C42 C43 1.377(4) ?
C43 C44 1.363(5) ?
C44 C45 1.368(5) ?
C45 C46 1.390(5) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4414222
