#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/95/4319568.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_4319568
loop_
_publ_author_name
'Anil J. Elias'
'Brendan Twamley'
'Jean'ne M. Shreeve'
_publ_section_title
;
 Syntheses and Experimental Studies on the Relative Stabilities of Spiro,
 Ansa, and Bridged Derivatives of Cyclic Tetrameric Fluorophosphazene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2120
_journal_page_last               2126
_journal_paper_doi               10.1021/ic001294s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C4 H4 F10 N4 O2 P4'
_chemical_formula_weight         453.99
_chemical_name_common            spiro-[(CF2CH2O)2PHN][F2PN]3
_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            8
_cell_length_a                   12.8938(2)
_cell_length_b                   10.2999(2)
_cell_length_c                   20.96840(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      1.94
_cell_volume                     2784.71(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Siemens SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18868
_diffrn_reflns_theta_full        29.05
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        '< 0.01%'
_diffrn_standards_interval_count 'beginning and end'
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.8495
_exptl_absorpt_correction_T_min  0.7982
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0249P)²+7.1538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2986
_reflns_number_total             3468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001294s_1.cif
_cod_data_source_block           bt100
_cod_database_code               4319568
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.09369(6) -0.12174(9) 0.37538(4) 0.0235(2) Uani 1 1 d . . .
P2 P 0.05769(7) -0.32029(9) 0.40267(4) 0.0250(2) Uani 1 1 d . . .
P3 P 0.20496(7) -0.12272(9) 0.44258(4) 0.0244(2) Uani 1 1 d . . .
P4 P 0.05566(7) 0.07258(9) 0.41097(4) 0.02228(19) Uani 1 1 d . . .
N1 N -0.0374(2) -0.2557(3) 0.37185(16) 0.0348(7) Uani 1 1 d . . .
N2 N 0.1375(2) -0.2464(3) 0.44414(14) 0.0281(6) Uani 1 1 d . . .
N3 N 0.1637(2) 0.0136(3) 0.42515(15) 0.0306(7) Uani 1 1 d . . .
N4 N -0.0454(2) -0.0080(3) 0.41488(13) 0.0261(6) Uani 1 1 d . . .
O1 O -0.20478(18) -0.1550(3) 0.40194(12) 0.0300(6) Uani 1 1 d . . .
O2 O -0.11270(18) -0.0672(2) 0.30592(11) 0.0271(5) Uani 1 1 d . . .
F1 F -0.43875(17) -0.0790(3) 0.32048(12) 0.0498(7) Uani 1 1 d . . .
F2 F -0.35138(18) -0.2600(2) 0.32852(11) 0.0411(6) Uani 1 1 d . . .
F3 F -0.33590(18) -0.1528(2) 0.21436(11) 0.0441(6) Uani 1 1 d . . .
F4 F -0.28875(19) 0.0329(2) 0.25503(12) 0.0440(6) Uani 1 1 d . . .
F5 F 0.06473(16) 0.1438(2) 0.34710(10) 0.0346(5) Uani 1 1 d . . .
F6 F 0.04152(17) 0.1893(2) 0.45507(11) 0.0357(5) Uani 1 1 d . . .
F7 F 0.25871(18) -0.1145(2) 0.50744(10) 0.0410(6) Uani 1 1 d . . .
F8 F 0.30121(16) -0.1462(2) 0.40117(11) 0.0373(5) Uani 1 1 d . . .
F9 F 0.0219(2) -0.4350(2) 0.44347(12) 0.0456(6) Uani 1 1 d . . .
F10 F 0.11433(17) -0.3959(2) 0.35026(11) 0.0381(5) Uani 1 1 d . . .
C1 C -0.2943(3) -0.0790(4) 0.38660(17) 0.0295(8) Uani 1 1 d . . .
H1A H -0.2742 0.0132 0.3814 0.035 Uiso 1 1 calc R . .
H1B H -0.3455 -0.0846 0.4217 0.035 Uiso 1 1 calc R . .
C2 C -0.3421(3) -0.1291(4) 0.32523(18) 0.0307(8) Uani 1 1 d . . .
C3 C -0.2833(3) -0.0976(3) 0.26390(17) 0.0291(8) Uani 1 1 d . . .
C4 C -0.1714(3) -0.1407(3) 0.26022(16) 0.0271(7) Uani 1 1 d . . .
H4A H -0.1661 -0.2346 0.2698 0.033 Uiso 1 1 calc R . .
H4B H -0.1439 -0.1257 0.2168 0.033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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 N4 120.17(17) . . ?
N1 P1 O1 104.34(16) . . ?
N4 P1 O1 109.72(15) . . ?
N1 P1 O2 110.04(16) . . ?
N4 P1 O2 106.46(15) . . ?
O1 P1 O2 105.20(13) . . ?
F9 P2 F10 98.76(14) . . ?
F9 P2 N1 109.19(17) . . ?
F10 P2 N1 107.36(16) . . ?
F9 P2 N2 105.44(15) . . ?
F10 P2 N2 109.64(15) . . ?
N1 P2 N2 123.63(17) . . ?
F7 P3 F8 98.37(13) . . ?
F7 P3 N2 106.39(15) . . ?
F8 P3 N2 109.77(15) . . ?
F7 P3 N3 108.45(16) . . ?
F8 P3 N3 106.75(15) . . ?
N2 P3 N3 124.11(16) . . ?
F6 P4 F5 99.28(13) . . ?
F6 P4 N4 106.82(14) . . ?
F5 P4 N4 111.56(15) . . ?
F6 P4 N3 107.45(16) . . ?
F5 P4 N3 106.69(15) . . ?
N4 P4 N3 122.50(17) . . ?
P2 N1 P1 137.2(2) . . ?
P3 N2 P2 140.3(2) . . ?
P3 N3 P4 135.4(2) . . ?
P4 N4 P1 135.1(2) . . ?
C1 O1 P1 122.3(2) . . ?
C4 O2 P1 120.6(2) . . ?
O1 C1 C2 109.4(3) . . ?
F1 C2 F2 107.5(3) . . ?
F1 C2 C1 107.9(3) . . ?
F2 C2 C1 109.3(3) . . ?
F1 C2 C3 108.3(3) . . ?
F2 C2 C3 107.3(3) . . ?
C1 C2 C3 116.1(3) . . ?
F4 C3 F3 106.4(3) . . ?
F4 C3 C4 109.5(3) . . ?
F3 C3 C4 108.2(3) . . ?
F4 C3 C2 107.4(3) . . ?
F3 C3 C2 107.8(3) . . ?
C4 C3 C2 117.0(3) . . ?
O2 C4 C3 108.3(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 1.561(3) . ?
P1 N4 1.564(3) . ?
P1 O1 1.575(2) . ?
P1 O2 1.580(2) . ?
P2 F9 1.530(2) . ?
P2 F10 1.532(2) . ?
P2 N1 1.537(3) . ?
P2 N2 1.548(3) . ?
P3 F7 1.529(2) . ?
P3 F8 1.534(2) . ?
P3 N2 1.543(3) . ?
P3 N3 1.546(3) . ?
P4 F6 1.528(2) . ?
P4 F5 1.532(2) . ?
P4 N4 1.547(3) . ?
P4 N3 1.548(3) . ?
O1 C1 1.431(4) . ?
O2 C4 1.437(4) . ?
F1 C2 1.353(4) . ?
F2 C2 1.356(4) . ?
F3 C3 1.365(4) . ?
F4 C3 1.358(4) . ?
C1 C2 1.517(5) . ?
C2 C3 1.527(5) . ?
C3 C4 1.512(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661084
