#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/22/7052228.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_7052228
loop_
_publ_author_name
'Kumar, K. V. P. Pavan'
'Kumar, N. Satish'
'Kumara Swamy, K. C.'
_publ_section_title
;
 Structurally diverse penta- and hexacoordinate phosphorus compounds
 from the reaction of diethyl or diisopropyl azodicarboxylates with
 phosphorus(iii) compounds
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              717
_journal_paper_doi               10.1039/b514839a
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C33 H50 N3 O6 P S'
_chemical_formula_weight         647.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.2570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9655(9)
_cell_length_b                   22.0001(17)
_cell_length_c                   13.9870(11)
_cell_measurement_temperature    273(2)
_cell_volume                     3671.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34926
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.9494
_exptl_absorpt_correction_type   'EMPIRICAL, SADABS'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLES
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0642P)²+1.0733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                5040
_reflns_number_total             6468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514839a.txt
_cod_data_source_block           compd15
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P_21/n
_cod_database_code               7052228
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'
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
P P 0.18329(4) 0.17382(2) 0.91226(3) 0.03535(13) Uani 1 1 d . . .
S S -0.02786(4) 0.20703(2) 0.75727(4) 0.04802(15) Uani 1 1 d . . .
O3 O 0.31072(10) 0.18566(5) 0.96183(9) 0.0397(3) Uani 1 1 d . . .
O1 O 0.19240(10) 0.14405(5) 0.80742(8) 0.0405(3) Uani 1 1 d . . .
N1 N 0.19922(12) 0.09707(6) 0.95769(11) 0.0388(3) Uani 1 1 d . . .
O6 O 0.04166(11) 0.06465(6) 0.88186(10) 0.0511(3) Uani 1 1 d . . .
N2 N 0.30804(12) 0.08492(7) 1.00009(12) 0.0435(4) Uani 1 1 d . . .
O2 O 0.18858(9) 0.24484(5) 0.86863(9) 0.0389(3) Uani 1 1 d . . .
N3 N 0.08099(12) 0.18872(7) 0.97810(11) 0.0417(4) Uani 1 1 d . . .
H H 0.0504 0.2235 0.9660 0.050 Uiso 1 1 calc R . .
O4 O 0.46435(10) 0.14631(6) 1.03359(10) 0.0505(3) Uani 1 1 d . . .
C23 C 0.14206(16) 0.04697(8) 0.92170(14) 0.0445(4) Uani 1 1 d . . .
C17 C 0.10901(15) 0.29022(8) 0.85866(12) 0.0377(4) Uani 1 1 d . . .
C6 C 0.08395(16) 0.19744(8) 0.68194(13) 0.0429(4) Uani 1 1 d . . .
O5 O 0.17320(13) -0.00475(6) 0.92809(13) 0.0700(5) Uani 1 1 d . . .
C27 C 0.36047(15) 0.13472(8) 0.99961(13) 0.0406(4) Uani 1 1 d . . .
C1 C 0.18180(16) 0.16786(8) 0.71503(13) 0.0406(4) Uani 1 1 d . . .
C12 C 0.00580(15) 0.27912(8) 0.80780(13) 0.0414(4) Uani 1 1 d . . .
C16 C 0.13532(16) 0.34868(8) 0.89496(13) 0.0412(4) Uani 1 1 d . . .
C15 C 0.05177(17) 0.39278(9) 0.88026(14) 0.0494(5) Uani 1 1 d . . .
H15 H 0.0671 0.4317 0.9034 0.059 Uiso 1 1 calc R . .
C2 C 0.26718(16) 0.15534(9) 0.65434(13) 0.0452(4) Uani 1 1 d . . .
C13 C -0.07387(16) 0.32493(9) 0.79657(15) 0.0488(5) Uani 1 1 d . . .
H13 H -0.1428 0.3169 0.7638 0.059 Uiso 1 1 calc R . .
C14 C -0.05187(18) 0.38216(9) 0.83356(15) 0.0523(5) Uani 1 1 d . . .
C3 C 0.24811(18) 0.17629(10) 0.56020(15) 0.0540(5) Uani 1 1 d . . .
H3 H 0.3028 0.1688 0.5178 0.065 Uiso 1 1 calc R . .
C5 C 0.07074(18) 0.21746(9) 0.58767(14) 0.0513(5) Uani 1 1 d . . .
H5 H 0.0055 0.2378 0.5661 0.062 Uiso 1 1 calc R . .
C31 C 0.02944(17) 0.15487(10) 1.05471(15) 0.0506(5) Uani 1 1 d . . .
H31 H 0.0267 0.1117 1.0377 0.061 Uiso 1 1 calc R . .
C28 C 0.53661(16) 0.09358(9) 1.05815(15) 0.0491(5) Uani 1 1 d . . .
H28 H 0.4942 0.0628 1.0908 0.059 Uiso 1 1 calc R . .
C7 C 0.37652(18) 0.12226(10) 0.68751(15) 0.0540(5) Uani 1 1 d . . .
C32 C 0.0971(3) 0.16201(15) 1.14876(18) 0.0883(9) Uani 1 1 d . . .
H32A H 0.1705 0.1452 1.1438 0.132 Uiso 1 1 calc R . .
H32B H 0.0607 0.1410 1.1980 0.132 Uiso 1 1 calc R . .
H32C H 0.1035 0.2044 1.1647 0.132 Uiso 1 1 calc R . .
C18 C 0.24880(18) 0.36403(9) 0.94747(16) 0.0545(5) Uani 1 1 d . . .
C30 C 0.5766(2) 0.06770(11) 0.96850(17) 0.0664(6) Uani 1 1 d . . .
H30A H 0.5135 0.0552 0.9268 0.100 Uiso 1 1 calc R . .
H30B H 0.6238 0.0332 0.9839 0.100 Uiso 1 1 calc R . .
H30C H 0.6185 0.0980 0.9369 0.100 Uiso 1 1 calc R . .
C20 C 0.2616(2) 0.32903(11) 1.04292(17) 0.0684(7) Uani 1 1 d . . .
H20A H 0.2002 0.3388 1.0806 0.103 Uiso 1 1 calc R . .
H20B H 0.3309 0.3403 1.0774 0.103 Uiso 1 1 calc R . .
H20C H 0.2618 0.2861 1.0303 0.103 Uiso 1 1 calc R . .
C9 C 0.3537(2) 0.06147(10) 0.73625(18) 0.0659(6) Uani 1 1 d . . .
H9A H 0.2993 0.0388 0.6969 0.099 Uiso 1 1 calc R . .
H9B H 0.3256 0.0690 0.7977 0.099 Uiso 1 1 calc R . .
H9C H 0.4221 0.0386 0.7446 0.099 Uiso 1 1 calc R . .
C4 C 0.15281(19) 0.20757(10) 0.52594(14) 0.0552(5) Uani 1 1 d . . .
C19 C 0.2583(2) 0.43176(11) 0.9731(2) 0.0851(9) Uani 1 1 d . . .
H19A H 0.2491 0.4556 0.9156 0.128 Uiso 1 1 calc R . .
H19B H 0.3306 0.4397 1.0050 0.128 Uiso 1 1 calc R . .
H19C H 0.2010 0.4423 1.0147 0.128 Uiso 1 1 calc R . .
C24 C -0.0284(2) 0.01936(11) 0.83186(19) 0.0665(6) Uani 1 1 d . . .
H24 H -0.0226 -0.0192 0.8669 0.080 Uiso 1 1 calc R . .
C29 C 0.62995(19) 0.11758(12) 1.12546(17) 0.0654(6) Uani 1 1 d . . .
H29A H 0.6696 0.1488 1.0940 0.098 Uiso 1 1 calc R . .
H29B H 0.6806 0.0851 1.1441 0.098 Uiso 1 1 calc R . .
H29C H 0.5993 0.1342 1.1814 0.098 Uiso 1 1 calc R . .
C22 C -0.1377(2) 0.43242(12) 0.8197(2) 0.0826(8) Uani 1 1 d . . .
H22A H -0.1119 0.4676 0.8555 0.124 Uiso 1 1 calc R . .
H22B H -0.2076 0.4190 0.8419 0.124 Uiso 1 1 calc R . .
H22C H -0.1482 0.4426 0.7529 0.124 Uiso 1 1 calc R . .
C25 C -0.1455(2) 0.04301(15) 0.8313(2) 0.0978(10) Uani 1 1 d . . .
H25A H -0.1649 0.0487 0.8961 0.147 Uiso 1 1 calc R . .
H25B H -0.1962 0.0144 0.7995 0.147 Uiso 1 1 calc R . .
H25C H -0.1506 0.0812 0.7980 0.147 Uiso 1 1 calc R . .
C21 C 0.3447(2) 0.34812(12) 0.8854(2) 0.0753(7) Uani 1 1 d . . .
H21A H 0.3459 0.3050 0.8749 0.113 Uiso 1 1 calc R . .
H21B H 0.4146 0.3607 0.9175 0.113 Uiso 1 1 calc R . .
H21C H 0.3337 0.3687 0.8249 0.113 Uiso 1 1 calc R . .
C8 C 0.44727(19) 0.16383(12) 0.75624(17) 0.0666(6) Uani 1 1 d . . .
H8A H 0.5155 0.1434 0.7776 0.100 Uiso 1 1 calc R . .
H8B H 0.4059 0.1734 0.8105 0.100 Uiso 1 1 calc R . .
H8C H 0.4646 0.2006 0.7236 0.100 Uiso 1 1 calc R . .
C33 C -0.0881(2) 0.17764(15) 1.0597(2) 0.0949(10) Uani 1 1 d . . .
H33A H -0.0867 0.2204 1.0734 0.142 Uiso 1 1 calc R . .
H33B H -0.1232 0.1564 1.1094 0.142 Uiso 1 1 calc R . .
H33C H -0.1298 0.1707 0.9993 0.142 Uiso 1 1 calc R . .
C11 C 0.1403(2) 0.22996(14) 0.42332(16) 0.0814(8) Uani 1 1 d . . .
H11A H 0.0720 0.2527 0.4132 0.122 Uiso 1 1 calc R . .
H11B H 0.1382 0.1958 0.3805 0.122 Uiso 1 1 calc R . .
H11C H 0.2027 0.2555 0.4113 0.122 Uiso 1 1 calc R . .
C10 C 0.4467(2) 0.10803(15) 0.60278(19) 0.0883(9) Uani 1 1 d . . .
H10A H 0.5145 0.0877 0.6258 0.133 Uiso 1 1 calc R . .
H10B H 0.4650 0.1452 0.5716 0.133 Uiso 1 1 calc R . .
H10C H 0.4045 0.0823 0.5580 0.133 Uiso 1 1 calc R . .
C26 C 0.0108(3) 0.0110(2) 0.7335(2) 0.1240(14) Uani 1 1 d . . .
H26A H 0.0055 0.0489 0.6996 0.186 Uiso 1 1 calc R . .
H26B H -0.0353 -0.0188 0.6993 0.186 Uiso 1 1 calc R . .
H26C H 0.0872 -0.0026 0.7385 0.186 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O1 P N3 134.63(8) . . ?
O1 P O3 108.84(7) . . ?
N3 P O3 116.34(8) . . ?
O1 P O2 92.31(6) . . ?
N3 P O2 93.94(7) . . ?
O3 P O2 86.98(6) . . ?
O1 P N1 85.88(7) . . ?
N3 P N1 93.07(7) . . ?
O3 P N1 85.97(6) . . ?
O2 P N1 171.72(7) . . ?
C12 S C6 100.61(9) . . ?
C27 O3 P 113.49(11) . . ?
C1 O1 P 133.01(11) . . ?
C23 N1 N2 114.81(14) . . ?
C23 N1 P 125.72(12) . . ?
N2 N1 P 113.15(11) . . ?
C23 O6 C24 117.97(16) . . ?
C27 N2 N1 106.01(14) . . ?
C17 O2 P 131.71(11) . . ?
C31 N3 P 133.22(13) . . ?
C27 O4 C28 116.88(14) . . ?
O5 C23 O6 124.68(18) . . ?
O5 C23 N1 126.24(18) . . ?
O6 C23 N1 108.99(15) . . ?
O2 C17 C12 120.08(16) . . ?
O2 C17 C16 119.33(16) . . ?
C12 C17 C16 120.47(16) . . ?
C5 C6 C1 119.93(18) . . ?
C5 C6 S 119.23(15) . . ?
C1 C6 S 120.78(14) . . ?
N2 C27 O4 128.28(16) . . ?
N2 C27 O3 120.97(16) . . ?
O4 C27 O3 110.74(15) . . ?
C6 C1 O1 120.16(16) . . ?
C6 C1 C2 121.61(17) . . ?
O1 C1 C2 117.89(16) . . ?
C13 C12 C17 120.22(18) . . ?
C13 C12 S 118.11(15) . . ?
C17 C12 S 121.66(14) . . ?
C15 C16 C17 116.25(17) . . ?
C15 C16 C18 121.07(17) . . ?
C17 C16 C18 122.67(16) . . ?
C14 C15 C16 124.11(19) . . ?
C3 C2 C1 115.46(18) . . ?
C3 C2 C7 121.06(18) . . ?
C1 C2 C7 123.47(17) . . ?
C14 C13 C12 120.66(19) . . ?
C15 C14 C13 118.21(18) . . ?
C15 C14 C22 121.0(2) . . ?
C13 C14 C22 120.7(2) . . ?
C4 C3 C2 124.2(2) . . ?
C4 C5 C6 120.74(19) . . ?
N3 C31 C33 107.99(18) . . ?
N3 C31 C32 110.84(19) . . ?
C33 C31 C32 111.8(2) . . ?
O4 C28 C30 108.97(17) . . ?
O4 C28 C29 105.41(16) . . ?
C30 C28 C29 113.06(18) . . ?
C10 C7 C9 106.9(2) . . ?
C10 C7 C8 107.3(2) . . ?
C9 C7 C8 110.42(19) . . ?
C10 C7 C2 111.43(18) . . ?
C9 C7 C2 111.77(18) . . ?
C8 C7 C2 108.92(18) . . ?
C21 C18 C16 110.66(18) . . ?
C21 C18 C19 108.0(2) . . ?
C16 C18 C19 111.91(18) . . ?
C21 C18 C20 110.30(19) . . ?
C16 C18 C20 109.46(18) . . ?
C19 C18 C20 106.4(2) . . ?
C5 C4 C3 118.03(19) . . ?
C5 C4 C11 121.3(2) . . ?
C3 C4 C11 120.7(2) . . ?
O6 C24 C25 105.8(2) . . ?
O6 C24 C26 108.6(2) . . ?
C25 C24 C26 113.3(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
P O1 1.6171(13) . ?
P N3 1.6190(15) . ?
P O3 1.6481(12) . ?
P O2 1.6803(12) . ?
P N1 1.8092(15) . ?
S C12 1.7705(19) . ?
S C6 1.776(2) . ?
O3 C27 1.358(2) . ?
O1 C1 1.391(2) . ?
N1 C23 1.373(2) . ?
N1 N2 1.416(2) . ?
O6 C23 1.344(2) . ?
O6 C24 1.448(2) . ?
N2 C27 1.263(2) . ?
O2 C17 1.379(2) . ?
N3 C31 1.477(2) . ?
O4 C27 1.322(2) . ?
O4 C28 1.472(2) . ?
C23 O5 1.199(2) . ?
C17 C12 1.400(3) . ?
C17 C16 1.410(3) . ?
C6 C5 1.388(3) . ?
C6 C1 1.389(3) . ?
C1 C2 1.403(3) . ?
C12 C13 1.388(3) . ?
C16 C15 1.397(3) . ?
C16 C18 1.533(3) . ?
C15 C14 1.378(3) . ?
C2 C3 1.398(3) . ?
C2 C7 1.538(3) . ?
C13 C14 1.379(3) . ?
C14 C22 1.512(3) . ?
C3 C4 1.386(3) . ?
C5 C4 1.372(3) . ?
C31 C33 1.500(3) . ?
C31 C32 1.501(3) . ?
C28 C30 1.488(3) . ?
C28 C29 1.502(3) . ?
C7 C10 1.535(3) . ?
C7 C9 1.535(3) . ?
C7 C8 1.535(3) . ?
C18 C21 1.530(3) . ?
C18 C19 1.535(3) . ?
C18 C20 1.539(3) . ?
C4 C11 1.514(3) . ?
C24 C25 1.494(4) . ?
C24 C26 1.498(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21141781
