#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/13/2001391.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_2001391
loop_
_publ_author_name
'Engelhardt, U.'
'Stromburg, B.'
_publ_section_title
;
 Phosphor(V)-Hydrazin-Sauerstoff-Achtring mit Boot-Sessel-Konformation
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1643
_journal_page_last               1646
_journal_paper_doi               10.1107/S0108270193001271
_journal_volume                  49
_journal_year                    1993
_chemical_formula_sum            'C24 H27 N4 O7 P3'
_chemical_formula_weight         576.423
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_type_scat_source
'Cromer & Mann (1968); Stewart, Davidson & Simpson (1965)'
_cell_angle_alpha                90.0
_cell_angle_beta                 110.780(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.450(2)
_cell_length_b                   9.781(2)
_cell_length_c                   17.818(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      17
_cell_measurement_theta_min      5
_cell_volume                     2680.4(7)
_diffrn_measurement_device       'CAD-4 (Enraf-Nonius)'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1789
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.2647
_exptl_absorpt_correction_type   keine
_exptl_crystal_colour            Farblos
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       Plättchen
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.39
_refine_ls_extinction_coef       1.60(10)
_refine_ls_extinction_method     'Isotrop (Larson, 1967)'
_refine_ls_goodness_of_fit_obs   1.58
_refine_ls_hydrogen_treatment    'H-Atome: siehe Text'
_refine_ls_number_parameters     385
_refine_ls_number_reflns         1666
_refine_ls_R_factor_obs          0.044
_refine_ls_shift/esd_max         0.2
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(Fₒ)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.023
_reflns_number_observed          1432
_reflns_number_total             1716
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sh1027.cif
_cod_data_source_block           sh1027_structure_1_of_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F~o~)' 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^(F~o~)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2680.0(10)
_cod_database_code               2001391
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
P(1) .5606 .2076(2) .4857 .0380(10)
P(2) .4677(2) -.0457(2) .4840(2) .0380(10)
P(3) .6975(2) -.1083(2) .4850(2) .0420(10)
O(1) .4921(3) .2901(5) .4290(3) .049(3)
O(2) .6214(3) .2815(5) .5628(3) .047(3)
O(3) .3841(3) -.0126(5) .4248(3) .048(3)
O(4) .4658(3) -.1222(4) .5613(3) .043(3)
O(5) .7807(3) -.1628(5) .5364(3) .057(3)
O(6) .6667(3) -.1465(4) .3921(3) .045(3)
O(7) .5280(3) .0823(4) .5243(3) .037(3)
N(1) .6256(4) .1388(5) .4437(3) .036(4)
N(2) .6955(4) .0593(5) .4961(3) .041(4)
N(3) .5304(4) -.1385(6) .4498(3) .039(4)
N(4) .6150(4) -.1697(6) .5085(3) .044(4)
C(1) .5956(5) .3443(7) .6227(4) .046(5)
C(2) .6626(6) .3799(8) .6907(5) .062(6)
C(3) .6417(7) .4460(10) .7518(6) .078(7)
C(4) .5592(8) .4710(10) .7428(6) .076(7)
C(5) .4941(6) .4350(10) .6743(6) .071(7)
C(6) .5108(5) .3704(8) .6124(5) .057(6)
C(7) .4332(5) -.0725(7) .6186(4) .038(4)
C(8) .4492(5) -.1519(8) .6847(5) .054(5)
C(9) .4196(6) -.1060(10) .7458(5) .061(6)
C(10) .3772(6) .0150(10) .7385(6) .065(6)
C(11) .3612(6) .0916(9) .6707(6) .062(7)
C(12) .3879(5) .0486(8) .6085(5) .050(5)
C(13) .7052(5) -.0966(7) .3385(4) .041(5)
C(14) .6503(5) -.0420(10) .2682(5) .056(6)
C(15) .6819(6) .0085(9) .2134(5) .065(7)
C(16) .7691(6) .0030(10) .2281(6) .071(7)
C(17) .8220(5) -.0550(10) .2974(7) .076(7)
C(18) .7914(5) -.1078(9) .3536(5) .054(5)
C(19) .6634(5) .2347(7) .3993(4) .055(5)
C(201) .7610(10) .248(2) .4640(10) .078(6)
C(202) .7570(10) .219(2) .4300(10) .048(5)
C(21) .7751(5) .1420(8) .5169(5) .069(6)
C(22) .4951(5) -.2641(7) .4030(5) .060(5)
C(231) .5250(10) -.373(2) .4640(10) .063(5)
C(232) .5640(10) -.377(2) .4500(10) .062(5)
C(24) .6143(5) -.3185(7) .5290(5) .065(6)
H(2) .724(4) .368(6) .685(3) ?
H(3) .692(4) .465(6) .794(4) ?
H(4) .537(4) .519(6) .776(4) ?
H(5) .438(4) .447(7) .669(4) ?
H(6) .444(4) .336(6) .547(3) ?
H(8) .484(4) -.234(7) .696(4) ?
H(9) .432(4) -.162(6) .795(4) ?
H(10) .368(4) .044(6) .797(4) ?
H(11) .336(4) .160(7) .664(4) ?
H(12) .378(4) .114(6) .560(4) ?
H(14) .599(4) -.027(7) .262(4) ?
H(15) .651(4) .042(6) .169(3) ?
H(16) .795(4) .038(6) .194(4) ?
H(17) .862(4) -.065(9) .306(5) ?
H(18) .824(4) -.153(6) .405(4) ?
H(19a) .663(6) .190(10) .347(5) ?
H(19b) .6326 .3247 .3889 ?
H(19c) .640(4) .213(7) .341(4) ?
H(19d) .6481 .3310 .4077 ?
H(20a) .8038 .2434 .4354 ?
H(20b) .7679 .3371 .4928 ?
H(20c) .7759 .1605 .3932 ?
H(20d) .7864 .3092 .4372 ?
H(21a) .7903 .1789 .5725 ?
H(21b) .8240 .0840 .5140 ?
H(21c) .7800 .2089 .5607 ?
H(21d) .8286 .0839 .5327 ?
H(22a) .430(4) -.261(7) .379(4) ?
H(22b) .5193 -.2772 .3592 ?
H(22c) .436(5) -.286(8) .403(4) ?
H(22d) .4925 -.2548 .3462 ?
H(23a) .4809 -.3891 .4896 ?
H(23b) .5352 -.4593 .4388 ?
H(23c) .5333 -.4622 .4564 ?
H(23d) .6034 -.3993 .4198 ?
H(24a) .665(5) -.367(9) .524(5) ?
H(24b) .6143 -.3306 .5848 ?
H(24c) .6745 -.3570 .5508 ?
H(24d) .585(4) -.334(7) .569(4) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) P(1) O(2) 116.7(5) yes
O(1) P(1) N(1) 112.0(10) yes
O(2) P(1) N(1) 106.0(10) yes
O(3) P(2) O(7) 115.5(3) yes
O(4) P(2) O(7) 100.4(3) yes
O(5) P(3) O(6) 116.8(3) yes
O(5) P(3) N(4) 112.2(3) yes
O(6) P(3) N(4) 100.9(3) yes
P(1) O(2) C(1) 126.0(10) yes
P(3) O(6) C(13) 124.7(4) yes
P(1) N(1) N(2) 115.3(7) yes
N(2) N(1) C(19) 107.3(5) yes
P(3) N(2) C(21) 121.4(5) yes
P(2) N(3) N(4) 114.6(5) yes
N(4) N(3) C(22) 108.4(5) yes
P(3) N(4) C(24) 119.2(6) yes
O(2) C(1) C(2) 114.6(7) yes
C(2) C(1) C(6) 122.4(8) yes
C(1) C(2) H(2) 112(3) yes
C(2) C(3) C(4) 120.6(9) yes
C(4) C(3) H(3) 130(5) yes
C(3) C(4) H(4) 129(4) yes
C(4) C(5) C(6) 122.0(10) yes
C(6) C(5) H(5) 118(4) yes
O(1) P(1) O(7) 115.0(10) yes
O(2) P(1) O(7) 101.0(10) yes
O(3) P(2) O(4) 115.8(3) yes
O(3) P(2) N(3) 114.4(3) yes
O(4) P(2) N(3) 105.8(3) yes
O(5) P(3) N(2) 110.1(3) yes
O(6) P(3) N(2) 110.2(3) yes
N(2) P(3) N(4) 105.9(4) yes
P(2) O(4) C(7) 127.2(4) yes
P(1) O(7) P(2) 131.3(7) yes
P(1) N(1) C(19) 116.2(6) yes
P(3) N(2) N(1) 120.5(4) yes
N(1) N(2) C(21) 107.7(5) yes
P(2) N(3) C(22) 119.6(5) yes
P(3) N(4) N(3) 113.8(5) yes
N(3) N(4) C(24) 107.0(5) yes
O(2) C(1) C(6) 122.9(6) yes
C(1) C(2) C(3) 117.6(9) yes
C(3) C(2) H(2) 129(3) yes
C(2) C(3) H(3) 109(5) yes
C(3) C(4) C(5) 120.0(10) yes
C(5) C(4) H(4) 111(4) yes
C(4) C(5) H(5) 120(4) yes
C(1) C(6) C(5) 117.5(7) yes
C(1) C(6) H(6) 124(3) yes
O(4) C(7) C(8) 115.3(7) yes
C(8) C(7) C(12) 122.3(8) yes
C(7) C(8) H(8) 126(4) yes
C(8) C(9) C(10) 120.5(9) yes
C(10) C(9) H(9) 120(4) yes
C(9) C(10) H(10) 111(3) yes
C(10) C(11) C(12) 121.4(9) yes
C(12) C(11) H(11) 116(6) yes
C(7) C(12) H(12) 124(4) yes
O(6) C(13) C(14) 116.6(7) yes
C(14) C(13) C(18) 121.3(8) yes
C(13) C(14) H(14) 120(5) yes
C(14) C(15) C(16) 119.68(8) yes
C(16) C(15) H(15) 117(5) yes
C(15) C(16) H(16) 124(4) yes
C(16) C(17) C(18) 122.6(9) yes
C(18) C(17) H(17) 112(9) yes
C(13) C(18) H(18) 114(4) yes
N(1) C(19) C(201) 99.9(9) yes
C(19) C(201) C(21) 108.0(10) yes
N(2) C(21) C(201) 109.1(9) yes
N(3) C(22) C(231) 102.8(8) yes
C(22) C(231) C(24) 106.0(10) yes
N(4) C(24) C(231) 103.1(8) yes
C(5) C(6) H(6) 119(3) yes
O(4) C(7) C(12) 122.3(7) yes
C(7) C(8) C(9) 118.3(8) yes
C(9) C(8) H(8) 116(4) yes
C(8) C(9) H(9) 120(4) yes
C(9) C(10) C(11) 120.0(10) yes
C(11) C(10) H(10) 129(3) yes
C(10) C(11) H(11) 123(6) yes
C(7) C(12) C(11) 117.7(8) yes
C(11) C(12) H(12) 118(4) yes
O(6) C(13) C(18) 122.0(6) yes
C(13) C(14) C(15) 120.5(8) yes
C(15) C(14) H(14) 118(5) yes
C(14) C(15) H(15) 124(5) yes
C(15) C(16) C(17) 119.0(10) yes
C(17) C(16) H(16) 117(4) yes
C(16) C(17) H(17) 125(9) yes
C(13) C(18) C(17) 117.1(7) yes
C(17) C(18) H(18) 129(4) yes
N(1) C(19) C(202) 108.5(9) yes
C(19) C(202) C(21) 103.0(10) yes
N(2) C(21) C(202) 99.3(8) yes
N(3) C(22) C(232) 102.6(8) yes
C(22) C(232) C(24) 107.0(10) yes
N(4) C(24) C(232) 101.2(9) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P(1) O(1) 1.460(10) yes
P(1) O(7) 1.59(2) yes
P(2) O(3) 1.442(5) yes
P(2) O(7) 1.600(4) yes
P(3) O(5) 1.451(5) yes
P(3) N(2) 1.653(6) yes
O(2) C(1) 1.410(10) yes
N(1) N(2) 1.428(7) yes
N(2) C(21) 1.470(10) yes
N(3) C(22) 1.483(9) yes
C(1) C(2) 1.360(10) yes
C(2) C(3) 1.41(2) yes
C(3) C(4) 1.33(2) yes
C(4) C(5) 1.360(10) yes
C(5) C(6) 1.380(10) yes
C(6) H(6) 1.32(5) yes
C(7) C(8) 1.360(10) yes
C(8) C(9) 1.410(10) yes
C(9) C(10) 1.360(10) yes
C(10) C(11) 1.370(10) yes
C(11) C(12) 1.390(10) yes
C(12) H(12) 1.04(6) yes
C(13) C(18) 1.350(10) yes
C(14) H(14) 0.82(7) yes
C(15) H(15) 0.84(5) yes
C(16) H(16) 0.92(7) yes
C(17) H(17) 0.62(7) yes
P(1) O(2) 1.560(10) yes
P(1) N(1) 1.65(2) yes
P(2) O(4) 1.578(6) yes
P(2) N(3) 1.645(7) yes
P(3) O(6) 1.595(6) yes
P(3) N(4) 1.668(7) yes
O(6) C(13) 1.410(10) yes
N(1) C(19) 1.500(10) yes
N(3) N(4) 1.445(7) yes
N(4) C(24) 1.502(9) yes
C(1) C(6) 1.370(10) yes
C(2) H(2) 1.07(7) yes
C(3) H(3) 0.92(5) yes
C(4) H(4) 0.92(8) yes
C(5) H(5) 0.91(7) yes
C(7) O(4) 1.400(10) yes
C(7) C(12) 1.380(10) yes
C(8) H(8) 0.96(6) yes
C(9) H(9) 0.99(6) yes
C(10) H(10) 1.14(7) yes
C(11) H(11) 0.77(7) yes
C(13) C(14) 1.360(10) yes
C(14) C(15) 1.350(10) yes
C(15) C(16) 1.360(10) yes
C(16) C(17) 1.360(10) yes
C(17) C(18) 1.37(2) yes
C(18) H(18) 0.99(6) yes
C(19) C(201) 1.61(2) yes
C(21) C(201) 1.37(2) yes
C(22) C(231) 1.47(2) yes
C(24) C(231) 1.60(2) yes
C(19) C(202) 1.44(2) yes
C(21) C(202) 1.65(2) yes
C(22) C(232) 1.59(2) yes
C(24) C(232) 1.48(2) yes
