#------------------------------------------------------------------------------
#$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/31/2003169.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_2003169
loop_
_publ_author_name
'Luc Van Oostenryck'
'Bernard Tinant'
'Jean-Paul Declercq'
'Jean-Pierre Dutasta'
_publ_section_title
;
A Macrobicyclic Thiophosphonamide Polyether Ligand
;
_journal_coeditor_code           HU1098
_journal_issue                   1
_journal_name_full               'Acta Crystallographica C'
_journal_page_first              80
_journal_page_last               84
_journal_paper_doi               10.1107/S0108270194003914
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C29 H35 N2 O5 P S'
_chemical_formula_sum            'C29 H35 N2 O5 P S'
_chemical_formula_weight         554.62
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.674(3)
_cell_length_b                   20.023(4)
_cell_length_c                   11.494(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      2.5
_cell_volume                     2900.3(12)
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71069
_exptl_absorpt_coefficient_mu    0.207
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.211
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_shift/esd_max         -0.001
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2003169
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_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
C1 0.0343(10) -0.0011(9) -0.0005(9) 0.0503(12) 0.0127(10) 0.0434(12)
N2 0.0338(9) -0.0016(7) 0.0015(7) 0.0455(10) 0.0074(8) 0.0428(10)
C3 0.0499(13) -0.0090(11) -0.0037(12) 0.0561(15) 0.0222(13) 0.074(2)
C4 0.075(2) 0.0040(14) -0.027(2) 0.047(2) -0.004(2) 0.113(3)
C5 0.0579(15) 0.0095(12) -0.0027(12) 0.0570(15) -0.0171(12) 0.062(2)
N6 0.0333(9) 0.0039(7) 0.0001(7) 0.0456(10) -0.0055(8) 0.0415(9)
C7 0.0296(10) -0.0002(9) 0.0019(9) 0.0462(12) -0.0086(10) 0.0504(12)
C8 0.0435(13) -0.0043(12) 0.0086(11) 0.071(2) -0.0067(12) 0.0543(14)
C9 0.0383(13) -0.0013(13) 0.0192(13) 0.093(2) -0.021(2) 0.081(2)
C10 0.0360(13) 0.0112(12) -0.0036(14) 0.076(2) -0.024(2) 0.092(2)
C11 0.0476(13) 0.0134(11) -0.0077(12) 0.0575(15) -0.0074(13) 0.067(2)
C12 0.0393(11) 0.0051(9) -0.0004(10) 0.0461(12) -0.0042(10) 0.0513(13)
O13 0.0512(9) 0.0152(9) 0.0054(7) 0.0775(12) 0.0120(8) 0.0466(9)
C14 0.071(2) 0.0204(14) -0.0006(13) 0.069(2) 0.0081(13) 0.0506(14)
C15 0.094(2) 0.014(2) 0.0136(15) 0.066(2) 0.0182(14) 0.058(2)
O16 0.0822(13) 0.0111(11) 0.0281(10) 0.0714(13) 0.0114(10) 0.0641(11)
C17 0.090(2) 0.007(2) 0.034(2) 0.099(2) 0.023(2) 0.071(2)
C18 0.087(2) 0.012(2) 0.027(2) 0.107(3) 0.007(2) 0.055(2)
O19 0.0653(12) 0.0106(11) 0.0201(10) 0.104(2) 0.0104(11) 0.0675(12)
C20 0.066(2) -0.0012(14) 0.0096(13) 0.077(2) -0.0035(14) 0.056(2)
C21 0.083(2) 0.003(2) -0.001(2) 0.066(2) -0.013(2) 0.078(2)
O22 0.0761(13) 0.0067(10) -0.0045(10) 0.0670(12) -0.0095(10) 0.0684(12)
C23 0.069(2) 0.031(2) 0.001(2) 0.086(2) -0.013(2) 0.078(2)
C24 0.0514(15) 0.0234(15) 0.0088(13) 0.090(2) -0.006(2) 0.068(2)
O25 0.0405(8) 0.0124(8) 0.0041(7) 0.0718(11) -0.0033(9) 0.0588(10)
C26 0.0403(12) 0.0019(10) -0.0017(10) 0.0584(14) 0.0070(11) 0.0477(13)
C27 0.0382(12) 0.0036(12) 0.0013(12) 0.082(2) 0.0108(15) 0.074(2)
C28 0.0477(15) -0.0117(14) -0.0184(14) 0.082(2) 0.004(2) 0.083(2)
C29 0.062(2) -0.0054(14) -0.0176(14) 0.068(2) -0.0021(14) 0.068(2)
C30 0.0515(13) -0.0002(11) -0.0040(11) 0.0558(14) 0.0045(11) 0.0507(13)
P31 0.0309(3) 0.0024(2) 0.0033(2) 0.0441(3) -0.0020(2) 0.0408(3)
S32 0.0462(3) 0.0063(3) 0.0040(3) 0.0761(5) -0.0323(4) 0.0724(4)
C33 0.0354(11) 0.0021(9) -0.0006(9) 0.0514(13) 0.0150(11) 0.0537(13)
C34 0.064(2) 0.0152(14) 0.0261(13) 0.077(2) 0.0233(14) 0.064(2)
C35 0.078(2) 0.028(2) 0.043(2) 0.131(3) 0.051(2) 0.087(2)
C36 0.059(2) 0.000(2) 0.023(2) 0.134(4) 0.073(3) 0.119(3)
C37 0.070(2) -0.023(2) -0.012(2) 0.077(2) 0.054(2) 0.126(3)
C38 0.0528(15) -0.0069(12) -0.0084(14) 0.056(2) 0.0164(14) 0.088(2)
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
C1 1 0.1505(2) 0.39840(11) 0.0528(2) 0.0430(5)
N2 1 0.25703(13) 0.41084(9) 0.10272(15) 0.0409(4)
C3 1 0.3060(2) 0.47596(13) 0.0853(2) 0.0606(7)
H3A 1 0.2533(2) 0.50590(13) 0.0464(2) 0.085(2)
H3B 1 0.3624(2) 0.47061(13) 0.0352(2) 0.085(2)
C4 1 0.3508(3) 0.50617(14) 0.2003(3) 0.0811(9)
H4A 1 0.4004(3) 0.54118(14) 0.1851(3) 0.085(2)
H4B 1 0.2935(3) 0.52661(14) 0.2372(3) 0.085(2)
C5 1 0.4059(2) 0.45701(13) 0.2828(2) 0.0597(7)
H5A 1 0.4714(2) 0.47664(13) 0.3189(2) 0.085(2)
H5B 1 0.3614(2) 0.44733(13) 0.3444(2) 0.085(2)
N6 1 0.43065(13) 0.39406(9) 0.22482(15) 0.0404(4)
C7 1 0.5363(2) 0.36838(11) 0.2493(2) 0.0422(5)
C8 1 0.6061(2) 0.37151(14) 0.1657(2) 0.0560(6)
H8 1 0.5842(2) 0.38994(14) 0.0929(2) 0.085(2)
C9 1 0.7095(2) 0.3473(2) 0.1893(3) 0.0697(8)
H9 1 0.7563(2) 0.3489(2) 0.1322(3) 0.085(2)
C10 1 0.7412(2) 0.3211(2) 0.2969(3) 0.0690(8)
H10 1 0.8099(2) 0.3048(2) 0.3125(3) 0.085(2)
C11 1 0.6739(2) 0.31843(13) 0.3825(2) 0.0585(6)
H11 1 0.6974(2) 0.30116(13) 0.4558(2) 0.085(2)
C12 1 0.5702(2) 0.34165(11) 0.3593(2) 0.0459(5)
O13 1 0.49632(13) 0.34053(9) 0.43701(14) 0.0584(5)
C14 1 0.5297(2) 0.31799(15) 0.5534(2) 0.0641(7)
H14A 1 0.5797(2) 0.34946(15) 0.5925(2) 0.085(2)
H14B 1 0.5644(2) 0.27491(15) 0.5509(2) 0.085(2)
C15 1 0.4347(3) 0.3124(2) 0.6178(2) 0.0722(8)
H15A 1 0.3782(3) 0.2901(2) 0.5690(2) 0.085(2)
H15B 1 0.4516(3) 0.2858(2) 0.6878(2) 0.085(2)
O16 1 0.4003(2) 0.37632(10) 0.6490(2) 0.0711(5)
C17 1 0.3165(3) 0.3720(2) 0.7218(3) 0.0849(10)
H17A 1 0.3410(3) 0.3483(2) 0.7933(3) 0.085(2)
H17B 1 0.2577(3) 0.3472(2) 0.6818(3) 0.085(2)
C18 1 0.2800(3) 0.4408(2) 0.7512(3) 0.0817(9)
H18A 1 0.2435(3) 0.4381(2) 0.8211(3) 0.085(2)
H18B 1 0.3418(3) 0.4690(2) 0.7691(3) 0.085(2)
O19 1 0.2124(2) 0.47107(11) 0.6623(2) 0.0780(6)
C20 1 0.2653(2) 0.5030(2) 0.5765(2) 0.0660(7)
H20A 1 0.2973(2) 0.4698(2) 0.5298(2) 0.085(2)
H20B 1 0.3215(2) 0.5310(2) 0.6139(2) 0.085(2)
C21 1 0.1903(3) 0.5445(2) 0.4998(3) 0.0763(8)
H21A 1 0.1449(3) 0.5693(2) 0.5473(3) 0.085(2)
H21B 1 0.2297(3) 0.5764(2) 0.4578(3) 0.085(2)
O22 1 0.1284(2) 0.50509(10) 0.4205(2) 0.0714(5)
C23 1 0.0599(2) 0.5441(2) 0.3403(3) 0.0781(9)
H23A 1 0.1004(2) 0.5789(2) 0.3064(3) 0.085(2)
H23B 1 0.0056(2) 0.5653(2) 0.3811(3) 0.085(2)
C24 1 0.0104(2) 0.5002(2) 0.2477(2) 0.0696(8)
H24A 1 -0.0253(2) 0.4632(2) 0.2816(2) 0.085(2)
H24B 1 -0.0414(2) 0.5248(2) 0.1962(2) 0.085(2)
O25 1 0.09359(12) 0.47589(9) 0.18402(15) 0.0571(4)
C26 1 0.0664(2) 0.43083(13) 0.0976(2) 0.0492(6)
C27 1 -0.0377(2) 0.4166(2) 0.0533(3) 0.0651(7)
H27 1 -0.0940(2) 0.4379(2) 0.0835(3) 0.085(2)
C28 1 -0.0565(2) 0.3707(2) -0.0357(3) 0.0726(8)
H28 1 -0.1261(2) 0.3609(2) -0.0647(3) 0.085(2)
C29 1 0.0245(2) 0.33947(15) -0.0821(3) 0.0679(7)
H29 1 0.0104(2) 0.30913(15) -0.1430(3) 0.085(2)
C30 1 0.1282(2) 0.35316(12) -0.0379(2) 0.0533(6)
H30 1 0.1837(2) 0.33172(12) -0.0695(2) 0.085(2)
P31 1 0.33351(4) 0.34850(3) 0.15775(5) 0.0386(2)
S32 1 0.38609(5) 0.28272(4) 0.05509(6) 0.0651(2)
C33 1 0.2528(2) 0.30994(12) 0.2601(2) 0.0472(5)
C34 1 0.1959(2) 0.3491(2) 0.3304(2) 0.0670(8)
H34 1 0.1980(2) 0.3954(2) 0.3241(2) 0.085(2)
C35 1 0.1360(3) 0.3199(2) 0.4101(3) 0.0965(12)
H35 1 0.0992(3) 0.3468(2) 0.4579(3) 0.085(2)
C36 1 0.1299(3) 0.2532(2) 0.4197(4) 0.1028(14)
H36 1 0.0889(3) 0.2342(2) 0.4734(4) 0.085(2)
C37 1 0.1844(3) 0.2133(2) 0.3499(4) 0.0928(12)
H37 1 0.1792(3) 0.1671(2) 0.3557(4) 0.085(2)
C38 1 0.2477(2) 0.24121(14) 0.2697(3) 0.0667(7)
H38 1 0.2858(2) 0.21393(14) 0.2237(3) 0.085(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000
N N 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003
O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006
P P 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.094
S S 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.123