#------------------------------------------------------------------------------
#$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003603.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003603
loop_
_publ_author_name
'Diefenbach, U.'
'Allcock, H. R.'
'Visscher, K. B.'
_publ_section_title
;
 Strukturuntersuchungen einer anorganisch-organischen Spiroverbindung
 aus Cyclotriphosphazen und 9,10-Diaminophenanthren
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1215
_journal_page_last               1218
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
' Synthese in unserem Labor, Kristalle aus THF/n-Hexan'
_chemical_formula_moiety         'C22 H26 Cl4 N5 O2 P3'
_chemical_formula_sum            'C22 H26 Cl4 N5 O2 P3'
_chemical_formula_weight         627.2
_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_type_scat_source
' Cromer & Mann (1968); Stewart, Davidson & Simpson (1965)'
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   15.279(6)
_cell_length_b                   16.864(6)
_cell_length_c                   10.424(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      1
_cell_volume                     2685.9(16)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.103
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4769
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        keine
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_type   keine
_exptl_crystal_colour            goldgelb
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      1.525
_exptl_crystal_density_method    '293 K'
_exptl_crystal_description       kubisch
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.71
_refine_ls_extinction_coef       2.3(2)
_refine_ls_extinction_method     isotrop
_refine_ls_goodness_of_fit_obs   1.9
_refine_ls_hydrogen_treatment    'refxyz [H(1)-H(6)]; noref [H(151)-H(182)]'
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1865
_refine_ls_R_factor_obs          0.054
_refine_ls_shift/esd_max         '0.05 > S/E'
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/\s^2^(F~o~)'
_refine_ls_wR_factor_obs         0.041
_reflns_number_observed          1225
_reflns_number_total             2437
_reflns_observed_criterion       Fo>4\s(Fo)
_[local]_cod_data_source_file    se1074.cif
_[local]_cod_data_source_block   se1074a
_cod_database_code               2003603
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2+y,1/2-z
x,-y,1/2+z
1/2-x,1/2+y,z
-x,-y,-z
1/2-x,1/2-y,1/2+z
-x,y,1/2-z
1/2+x,1/2-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
P(1) .50000 .7460(1) .25000 .044(1)
P(2) .57753(9) .60093(7) .1893(1) .046(1)
Cl(1) .68732(9) .57206(8) .2810(1) .067(1)
Cl(2) .6038(1) .55503(8) .0226(1) .068(1)
N(1) .5695(2) .6931(2) .1762(3) .044(2)
N(2) .50000 .5527(3) .25000 .056(4)
N(3) .4528(3) .8133(2) .1621(4) .049(3)
C(1) .4728(3) .8908(2) .2005(4) .045(3)
C(2) .4396(4) .9621(3) .1466(5) .046(3)
C(3) .3824(4) .9631(4) .0473(6) .059(4)
C(4) .3541(5) 1.0327(4) -.0034(6) .067(5)
C(5) .3841(5) 1.1040(4) .0450(7) .071(5)
C(6) .4386(4) 1.1053(3) .1433(6) .064(4)
C(7) .4702(3) 1.0343(3) .1990(4) .048(4)
O(1) .6286(3) .7478(3) .5562(4) .114(4)
C(15) .5952(6) .6783(4) .5922(8) .134(7)
C(16) .6404(7) .6535(5) .7059(9) .150(9)
C(17) .7088(6) .7081(5) .7231(7) .122(7)
C(18) .7026(5) .7658(4) .6204(8) .114(7)
H(1) .429(3) .803(2) .094(4) ?
H(3) .361(3) .919(2) .018(4) ?
H(4) .322(2) 1.032(2) -.066(3) ?
H(5) .373(3) 1.154(3) .012(4) ?
H(6) .469(3) 1.159(2) .176(4) ?
H(151) .5313 .6842 .6107 ?
H(152) .6036 .6382 .5226 ?
H(161) .6001 .6544 .7813 ?
H(162) .6645 .5988 .6945 ?
H(171) .7026 .7351 .8081 ?
H(172) .7665 .6803 .7192 ?
H(181) .6990 .8207 .6563 ?
H(182) .7545 .7617 .5624 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N(1) P(1) N(1) 7_655 111.5(2) yes
N(1) P(2) N(2) . 119.4(2) yes
P(2) N(2) P(2) 7_655 117.6(3) yes
P(1) N(3) C(1) . 113.1(3) yes
N(3) P(1) N(3) 7_655 91.6(3) yes
Cl(1) P(2) Cl(2) . 99.10(10) yes
P(1) N(1) P(2) . 124.7(2) yes
N(3) C(1) C(1) 7_655 111.1(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P(1) N(1) 1.586(4) yes
P(2) N(1) 1.565(3) yes
P(2) Cl(1) 1.991(2) yes
N(3) C(1) 1.401(6) yes
O(1) H(1) 2.03(4) yes
P(1) N(3) 1.627(4) yes
P(2) N(2) 1.570(3) yes
P(2) Cl(2) 1.944(2) yes
N(3) H(1) 0.81(4) yes
C(1) C(2) 1.421(6) no
C(2) C(3) 1.355(6) no
C(3) C(4) 1.358(9) no
C(4) C(5) 1.381(7) no
C(5) C(6) 1.321(10) no
C(6) C(7) 1.416(7) no
C(7) C(7) 1.400(7) no
O(1) C(18) 1.349(10) no
C(15) H(151) 1.000(9) no
C(16) C(17) 1.400(10) no
C(16) H(161) 1.000(10) no
C(17) H(171) 1.000(8) no
C(18) H(181) 1.00(7) no
O(1) H(1) 2.03(4) no
C(1) C(1) 1.325(6) no
C(2) C(7) 1.414(6) no
C(3) H(3) 0.87(4) no
C(4) H(4) 0.82(4) no
C(5) H(5) 0.93(4) no
C(6) H(6) 1.07(4) no
O(1) C(15) 1.333(9) no
C(15) C(16) 1.430(10) no
C(15) H(152) 1.000(8) no
C(16) H(162) 1.000(8) no
C(17) C(18) 1.450(10) no
C(17) H(172) 1.000(9) no
C(18) H(182) 1.000(8) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
P(1) N(1) P(2) N(2) . 16.1(3) yes
P(2) N(1) P(1) N(1) 7_655 -8.1(3) yes
N(1) P(2) N(2) P(2) 7_655 -7.5(2) yes
_journal_paper_doi 10.1107/S0108270194013636