#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:46:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178915 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/44/4114478.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_4114478
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           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   20.7790(10)
_cell_length_b                   8.2761(5)
_cell_length_c                   16.4341(9)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2826.2(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker XSCANS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_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  0.000
_diffrn_reflns_av_sigmaI/netI    0.033
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2475
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        6.15
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.292
_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    1.289
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.20
_refine_diff_density_rms         0.04
_refine_ls_extinction_coef       0.0064(11)
_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         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.036
_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)+(0.0505P)²+1.0780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.096
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                2060
_reflns_number_total             2475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0374168si20030720_085045.cif
_cod_data_source_block           jh-csmet3
_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^)+(0.0505P)^2^+1.0780P] 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^)+(0.0505P)^2^+1.0780P] 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               4114478
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, 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 0.08255(2) 0.13316(6) 0.31187(3) 0.03209(18) Uani 1 d .
P2 P -0.05142(2) 0.06825(6) 0.35575(3) 0.03323(19) Uani 1 d .
N1 N 0.01649(8) 0.1565(2) 0.35918(10) 0.0406(4) Uani 1 d .
N2 N -0.08381(8) 0.0272(2) 0.26961(10) 0.0368(4) Uani 1 d .
C1 C 0.14010(12) 0.0403(3) 0.37920(14) 0.0513(6) Uani 1 d .
H1A H 0.1813 0.0351 0.3528 0.077 Uiso 1 calc R
H1B H 0.1260 -0.0669 0.3926 0.077 Uiso 1 calc R
H1C H 0.1437 0.1033 0.4281 0.077 Uiso 1 calc R
C2 C -0.04998(12) -0.1212(3) 0.40945(15) 0.0508(6) Uani 1 d .
H2A H -0.0921 -0.1687 0.4085 0.076 Uiso 1 calc R
H2B H -0.0372 -0.1031 0.4648 0.076 Uiso 1 calc R
H2C H -0.0199 -0.1929 0.3837 0.076 Uiso 1 calc R
C11 C 0.11301(10) 0.3346(2) 0.29211(12) 0.0346(5) Uani 1 d .
C12 C 0.17555(11) 0.3559(3) 0.26287(16) 0.0519(6) Uani 1 d .
H12 H 0.2029 0.2672 0.2587 0.062 Uiso 1 calc R
C13 C 0.19724(13) 0.5061(3) 0.24022(18) 0.0625(7) Uani 1 d .
H13 H 0.2391 0.5183 0.2211 0.075 Uiso 1 calc R
C14 C 0.15774(14) 0.6377(3) 0.24554(18) 0.0619(7) Uani 1 d .
H14 H 0.1725 0.7389 0.2296 0.074 Uiso 1 calc R
C15 C 0.09590(13) 0.6200(3) 0.27459(17) 0.0574(7) Uani 1 d .
H15 H 0.0690 0.7094 0.2785 0.069 Uiso 1 calc R
C16 C 0.07401(11) 0.4698(3) 0.29783(14) 0.0444(5) Uani 1 d .
H16 H 0.0323 0.4591 0.3177 0.053 Uiso 1 calc R
C21 C -0.10411(10) 0.1966(3) 0.41557(12) 0.0398(5) Uani 1 d .
C22 C -0.08189(13) 0.3357(3) 0.45286(15) 0.0545(6) Uani 1 d .
H22 H -0.0389 0.3650 0.4473 0.065 Uiso 1 calc R
C23 C -0.12297(17) 0.4320(4) 0.49845(18) 0.0751(9) Uani 1 d .
H23 H -0.1073 0.5251 0.5233 0.090 Uiso 1 calc R
C24 C -0.18646(18) 0.3908(5) 0.5071(2) 0.0833(10) Uani 1 d .
H24 H -0.2138 0.4553 0.5380 0.100 Uiso 1 calc R
C25 C -0.20972(14) 0.2544(5) 0.46991(19) 0.0771(10) Uani 1 d .
H25 H -0.2529 0.2272 0.4753 0.093 Uiso 1 calc R
C26 C -0.16912(11) 0.1566(3) 0.42433(16) 0.0568(7) Uani 1 d .
H26 H -0.1852 0.0641 0.3995 0.068 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_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N2 119.32(9) . 3 y
N1 P1 C1 108.94(11) . . y
N2 P1 C1 105.64(10) 3 . y
N1 P1 C11 106.12(10) . . y
N2 P1 C11 110.37(9) 3 . y
C1 P1 C11 105.70(11) . . y
N1 P2 N2 120.07(9) . . y
N1 P2 C2 111.59(11) . . y
N2 P2 C2 104.80(10) . . y
N1 P2 C21 104.33(10) . . y
N2 P2 C21 110.42(9) . . y
C2 P2 C21 104.73(11) . . y
P2 N1 P1 133.92(12) . . y
P1 N2 P2 128.00(11) 3 . y
C16 C11 C12 117.8(2) . . ?
C16 C11 P1 121.78(16) . . ?
C12 C11 P1 120.16(17) . . ?
C13 C12 C11 120.8(2) . . ?
C14 C13 C12 120.4(2) . . ?
C13 C14 C15 119.8(2) . . ?
C16 C15 C14 120.0(2) . . ?
C15 C16 C11 121.1(2) . . ?
C22 C21 C26 118.3(2) . . ?
C22 C21 P2 121.71(18) . . ?
C26 C21 P2 120.03(19) . . ?
C21 C22 C23 120.8(3) . . ?
C24 C23 C22 120.3(3) . . ?
C23 C24 C25 119.9(3) . . ?
C24 C25 C26 120.4(3) . . ?
C25 C26 C21 120.3(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 1.5894(17) . y
P1 N2 1.6006(17) 3 y
P1 C1 1.801(2) . y
P1 C11 1.813(2) . y
P2 N1 1.5898(18) . y
P2 N2 1.6038(17) . y
P2 C2 1.800(2) . y
P2 C21 1.815(2) . y
N2 P1 1.6007(17) 3 ?
C11 C16 1.385(3) . ?
C11 C12 1.397(3) . ?
C12 C13 1.374(3) . ?
C13 C14 1.367(4) . ?
C14 C15 1.378(4) . ?
C15 C16 1.378(3) . ?
C21 C22 1.384(3) . ?
C21 C26 1.398(3) . ?
C22 C23 1.388(4) . ?
C23 C24 1.370(5) . ?
C24 C25 1.372(5) . ?
C25 C26 1.388(4) . ?
