#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:46:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178915 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/44/4114480.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_4114480
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           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.738(1)
_cell_length_b                   10.766(1)
_cell_length_c                   19.522(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2887.4(5)
_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 0.879
_diffrn_measured_fraction_theta_max 0.879
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3241
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        6.69
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.285
_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    1.262
_exptl_crystal_description       plates
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.21
_refine_diff_density_rms         0.04
_refine_ls_extinction_coef       0.0025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0530P)²+0.9090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.102
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                2001
_reflns_number_total             2530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0374168si20030720_085156.cif
_cod_data_source_block           jh-ttrn15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.9090P] 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^)+(0.0530P)^2^+0.9090P] 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               4114480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.54851(5) -0.04069(6) 0.39830(3) 0.0411(2) Uani 1 d .
P2 P 0.46790(4) 0.17129(5) 0.47152(3) 0.03821(19) Uani 1 d .
N1 N 0.47904(17) 0.0751(2) 0.40997(10) 0.0514(5) Uani 1 d .
N2 N 0.41673(14) 0.12422(18) 0.53966(9) 0.0436(5) Uani 1 d .
C1 C 0.4879(2) -0.1339(3) 0.33442(14) 0.0630(8) Uani 1 d .
H1A H 0.4778 -0.0851 0.2939 0.095 Uiso 1 calc R
H1B H 0.4263 -0.1614 0.3519 0.095 Uiso 1 calc R
H1C H 0.5275 -0.2047 0.3235 0.095 Uiso 1 calc R
C2 C 0.5817(2) 0.2456(3) 0.49053(17) 0.0656(8) Uani 1 d .
H2A H 0.6098 0.2770 0.4490 0.098 Uiso 1 calc R
H2B H 0.6252 0.1864 0.5109 0.098 Uiso 1 calc R
H2C H 0.5709 0.3129 0.5218 0.098 Uiso 1 calc R
C11 C 0.66000(19) 0.0092(2) 0.35644(11) 0.0466(6) Uani 1 d .
C12 C 0.7452(2) -0.0565(3) 0.36378(14) 0.0588(7) Uani 1 d .
H12 H 0.7462 -0.1268 0.3914 0.071 Uiso 1 calc R
C13 C 0.8292(2) -0.0196(4) 0.33085(16) 0.0770(9) Uani 1 d .
H13 H 0.8866 -0.0639 0.3370 0.092 Uiso 1 calc R
C14 C 0.8275(3) 0.0836(4) 0.28874(18) 0.0857(11) Uani 1 d .
H14 H 0.8836 0.1079 0.2657 0.103 Uiso 1 calc R
C15 C 0.7439(3) 0.1495(3) 0.28091(17) 0.0873(12) Uani 1 d .
H15 H 0.7430 0.2192 0.2527 0.105 Uiso 1 calc R
C16 C 0.6602(3) 0.1134(3) 0.31463(15) 0.0709(9) Uani 1 d .
H16 H 0.6034 0.1594 0.3093 0.085 Uiso 1 calc R
C21 C 0.39205(16) 0.2938(2) 0.43814(12) 0.0390(5) Uani 1 d .
C22 C 0.3883(2) 0.3161(3) 0.36806(13) 0.0575(7) Uani 1 d .
H22 H 0.4225 0.2651 0.3381 0.069 Uiso 1 calc R
C23 C 0.3340(2) 0.4135(3) 0.34283(14) 0.0708(9) Uani 1 d .
H23 H 0.3324 0.4282 0.2959 0.085 Uiso 1 calc R
C24 C 0.2822(2) 0.4890(3) 0.38613(14) 0.0595(7) Uani 1 d .
H24 H 0.2450 0.5538 0.3687 0.071 Uiso 1 calc R
C25 C 0.2859(2) 0.4680(3) 0.45544(14) 0.0570(7) Uani 1 d .
H25 H 0.2517 0.5196 0.4851 0.068 Uiso 1 calc R
C26 C 0.34004(18) 0.3709(2) 0.48137(13) 0.0490(6) Uani 1 d .
H26 H 0.3416 0.3572 0.5284 0.059 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_site_symmetry_1
_geom_angle_publ_flag
N2 P1 N1 121.23(11) 5_656 y
N2 P1 C1 110.63(13) 5_656 y
N1 P1 C1 105.00(13) . y
N2 P1 C11 104.95(11) 5_656 y
N1 P1 C11 109.81(12) . y
C1 P1 C11 104.03(13) . y
N2 P2 N1 117.85(11) . y
N2 P2 C2 110.77(13) . y
N1 P2 C2 111.20(14) . y
N2 P2 C21 106.29(10) . y
N1 P2 C21 104.96(11) . y
C2 P2 C21 104.61(13) . y
P1 N1 P2 132.58(14) . y
P1 N2 P2 133.56(13) 5_656 y
C12 C11 C16 118.4(3) . ?
C12 C11 P1 121.23(19) . ?
C16 C11 P1 120.4(2) . ?
C11 C12 C13 121.0(3) . ?
C12 C13 C14 119.6(3) . ?
C15 C14 C13 120.0(3) . ?
C14 C15 C16 120.2(3) . ?
C15 C16 C11 120.7(3) . ?
C26 C21 C22 118.5(2) . ?
C26 C21 P2 121.15(18) . ?
C22 C21 P2 120.26(18) . ?
C23 C22 C21 120.2(2) . ?
C24 C23 C22 120.7(3) . ?
C23 C24 C25 119.4(2) . ?
C24 C25 C26 120.4(2) . ?
C25 C26 C21 120.6(2) . ?
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 N2 1.5822(2) 5_656 y
P1 N1 1.587(2) . y
P1 C1 1.804(3) . y
P1 C11 1.817(2) . y
P2 N2 1.588(2) . y
P2 N1 1.593(2) . y
P2 C2 1.795(3) . y
P2 C21 1.803(2) . y
N2 P1 1.5822(19) 5_656 ?
C11 C12 1.375(4) . ?
C11 C16 1.387(4) . ?
C12 C13 1.379(4) . ?
C13 C14 1.382(5) . ?
C14 C15 1.359(5) . ?
C15 C16 1.380(5) . ?
C21 C26 1.383(3) . ?
C21 C22 1.390(3) . ?
C22 C23 1.378(4) . ?
C23 C24 1.371(4) . ?
C24 C25 1.373(4) . ?
C25 C26 1.379(3) . ?
