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#------------------------------------------------------------------------------
#$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006199.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_2006199
_journal_name_full 'Acta Crystallographica Section C'
_journal_year 1997
_journal_volume 53
_journal_page_first 773
_journal_page_last 775
_publ_section_title
;
A Tricyclic Phosphorus(V)-Hydrazine System with Twist Conformation of the
Central Heterocycle
;
_space_group_IT_number 14
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_[local]_cod_cif_authors_sg_H-M 'P 21/n'
loop_
_publ_author_name
'Engelhardt, Udo'
'Rosefid, Mehdi'
_chemical_formula_sum 'C15 H21 N4 O2 P S'
_chemical_formula_weight 352.14
_chemical_melting_point '112\%C'
_symmetry_cell_setting monoclinic
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x+1/2,y+1/2,-z+1/2'
'-x,-y,-z'
'x+1/2,-y+1/2,z+1/2'
_cell_length_a 8.002(5)
_cell_length_b 12.286(2)
_cell_length_c 17.380(4)
_cell_angle_alpha 90.0
_cell_angle_beta 91.10(2)
_cell_angle_gamma 90.0
_cell_volume 1708.0(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 293
_exptl_crystal_density_diffrn 1.371
_diffrn_ambient_temperature '293 K'
_refine_ls_R_factor_obs .048
_refine_ls_wR_factor_obs .029
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_type_symbol
S .12237(9) .59818(5) .24318(4) .0595(5) Ueq ? ? ? ? ?
P2 .31535(9) .64953(5) .19106(4) .0451(4) Ueq ? ? ? ? ?
O1 .4067(2) .56070(10)
.14000(10)
.0580(10)
Ueq ? ? ? ? ?
O2 .6413(2) .91770(10)
.14430(10)
.0730(10)
Ueq ? ? ? ? ?
N1 .2815(3) .7554(2) .13470(10)
.0440(10)
Ueq ? ? ? ? ?
N3 .4800(3) .69130(10)
.24330(10)
.0470(10)
Ueq ? ? ? ? ?
N8 .5317(3) .8005(2) .23200(10)
.056(2) Ueq ? ? ? ? ?
N10 .4346(3) .7983(2) .10670(10)
.0500(10)
Ueq ? ? ? ? ?
C1 .3258(3) .4863(2) .0905(2) .051(2) Ueq ? ? ? ? ?
C2 .3157(4) .3804(2) .1129(2) .064(2) Ueq ? ? ? ? ?
C3 .2502(5) .3046(3) .0609(3) .085(3) Ueq ? ? ? ? ?
C8 .1995(5) .3355(4) -.0104(3) .096(3) Ueq ? ? ? ? ?
C10 .2066(6) .4434(4) -.0305(2) .112(3) Ueq ? ? ? ? ?
C15 .2730(5) .5185(3) .0200(2) .089(3) Ueq ? ? ? ? ?
C4 .6198(4) .6200(2) .2653(2) .059(2) Ueq ? ? ? ? ?
C5 .7062(5) .6634(3) .3368(2) .067(2) Ueq ? ? ? ? ?
C6 .7622(4) .7794(3) .3248(2) .060(2) Ueq ? ? ? ? ?
C7 .6164(4) .8483(2) .2986(2) .059(2) Ueq ? ? ? ? ?
C9 .5451(3) .8446(2) .1600(2) .058(2) Ueq ? ? ? ? ?
C11 .4075(4) .8547(3) .0328(2) .062(2) Ueq ? ? ? ? ?
C12 .2788(5) .9448(2) .0403(2) .066(3) Ueq ? ? ? ? ?
C13 .1178(4) .9000(3) .0728(2) .065(2) Ueq ? ? ? ? ?
C14 .1533(4) .8397(2) .1477(2) .053(2) Ueq ? ? ? ? ?
H2 .347(4) .362(2) .1600(10)
.080(10)
Uiso ? ? ? ? ?
H3 .249(4) .240(2) .072(2) .090(10)
Uiso ? ? ? ? ?
H8 .156(4) .283(3) -.047(2) .130(10)
Uiso ? ? ? ? ?
H10 .167(4) .465(3) -.088(2) .15(2) Uiso ? ? ? ? ?
H15 .266(4) .593(3) .009(2) .130(10)
Uiso ? ? ? ? ?
H41 .572(3) .545(2) .2730(10)
.077(9) Uiso ? ? ? ? ?
H42 .694(3) .617(2) .2190(10)
.070(9) Uiso ? ? ? ? ?
H51 .623(3) .664(2) .3790(10)
.068(9) Uiso ? ? ? ? ?
H52 .791(3) .616(2) .3480(10)
.071(9) Uiso ? ? ? ? ?
H61 .810(3) .807(2) .3750(10)
.058(8) Uiso ? ? ? ? ?
H62 .847(3) .778(2) .2860(10)
.080(10)
Uiso ? ? ? ? ?
H71 .534(3) .854(2) .3420(10)
.090(10)
Uiso ? ? ? ? ?
H72 .648(3) .918(2) .2810(10)
.080(10)
Uiso ? ? ? ? ?
H111 .364(3) .796(2) -.0030(10)
.052(7) Uiso ? ? ? ? ?
H112 .524(3) .881(2) .0210(10)
.063(8) Uiso ? ? ? ? ?
H121 .251(3) .982(2) -.0110(10)
.058(7) Uiso ? ? ? ? ?
H122 .333(3) .998(2) .0760(10)
.061(8) Uiso ? ? ? ? ?
H131 .069(3) .845(2) .0320(10)
.080(10)
Uiso ? ? ? ? ?
H132 .034(3) .956(2) .0810(10)
.090(10)
Uiso ? ? ? ? ?
H141 .058(3) .805(2) .1630(10)
.055(8) Uiso ? ? ? ? ?
H142 .195(3) .890(2) .1900(10)
.051(7) Uiso ? ? ? ? ?
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
S .0595(5) .0467(4) .0723(5) -.0100(4) .0100(4) .0091(4) U
P2 .0497(4) .0325(3) .0531(4) -.0044(3) .0015(3) -.0005(3) U
O1 .0530(10)
.0460(10)
.0750(10)
-.0072(9) .0040(10)
-.0168(9) U
O2 .0700(10)
.0570(10)
.0910(10)
-.0300(10)
.0010(10)
.0060(10)
U
N1 .0480(10)
.0390(10)
.0460(10)
-.0070(10)
.0000(10)
.0039(9) U
N3 .0510(10)
.0320(10)
.0590(10)
-.0030(10)
-.0080(10)
.0020(10)
U
N8 .068(2) .0340(10)
.0660(10)
-.0120(10)
-.0250(10)
.0050(10)
U
N10 .0550(10)
.0460(10)
.0500(10)
-.0120(10)
.0050(10)
.0050(10)
U
C1 .051(2) .042(2) .059(2) -.0050(10)
.0030(10)
-.0100(10)
U
C2 .074(2) .046(2) .073(2) .001(2) .004(2) -.004(2) U
C3 .096(3) .044(2) .115(3) -.018(2) .028(3) -.024(2) U
C8 .100(3) .104(3) .084(3) -.035(3) .011(2) -.046(3) U
C10 .166(4) .102(3) .069(3) -.023(3) -.021(3) -.011(2) U
C15 .141(4) .059(2) .068(2) -.009(2) -.015(2) .000(2) U
C4 .070(2) .041(2) .067(2) .008(2) -.012(2) .0000(10)
U
C5 .077(3) .055(2) .069(2) .017(2) -.023(2) .000(2) U
C6 .055(2) .065(2) .060(2) .005(2) -.013(2) -.010(2) U
C7 .065(2) .042(2) .069(2) -.002(2) -.019(2) -.005(2) U
C9 .051(2) .0390(10)
.065(2) -.0030(10)
-.0010(10)
.0000(10)
U
C11 .079(2) .061(2) .046(2) -.018(2) .005(2) .004(2) U
C12 .097(3) .048(2) .054(2) -.010(2) -.012(2) .014(2) U
C13 .071(2) .058(2) .068(2) .005(2) -.008(2) .014(2) U
C14 .056(2) .049(2) .055(2) -.005(2) .002(2) .005(2) U
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S P2 1.9130(10)
yes
P2 O1 1.594(2) yes
P2 N1 1.647(2) yes
P2 N3 1.663(2) yes
N1 N10 1.429(3) yes
N1 C14 1.479(4) no
N3 N8 1.420(3) yes
N3 C4 1.468(4) no
O1 C1 1.404(3) no
O2 C9 1.218(3) yes
N8 C7 1.453(4) no
N8 C9 1.370(3) yes
N10 C11 1.471(4) no
N10 C9 1.390(3) yes
C1 C2 1.361(4) no
C1 C15 1.348(4) no
C2 C3 1.392(5) no
C3 C8 1.351(6) no
C8 C10 1.373(6) no
C10 C15 1.372(6) no
C C(phenyl)mean 1.370(10)
no
C4 C5 1.507(5) no
C5 C6 1.510(5) no
C6 C7 1.504(5) no
C11 C12 1.520(5) no
C12 C13 1.520(5) no
C13 C14 1.519(4) no
C C(hexahydropyridazine)mean 1.513(7) no
C2 H2 .88(3) no
C3 H3 .82(3) no
C8 H8 .97(3) no
C10 H10 1.08(3) no
C15 H15 .94(3) no
C4 H41 1.00(2) no
C4 H42 1.01(2) no
C5 H51 1.00(2) no
C5 H52 .91(3) no
C6 H61 1.01(2) no
C6 H62 .96(3) no
C7 H71 1.02(3) no
C7 H72 .95(3) no
C11 H111 1.01(2) no
C11 H112 1.01(2) no
C12 H121 1.03(2) no
C12 H122 .99(2) no
C13 H131 1.06(2) no
C13 H132 .98(3) no
C14 H141 .91(2) no
C14 H142 1.01(2) no
_cod_database_code 2006199
|
