#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003169.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 _journal_name_full 'Acta Crystallographica' _journal_volume C51 _journal_year 1995 _journal_page_first 53 _journal_page_last 57 _publ_section_title ; Folding onto Copper(II) of a Flexible Bis-chelating 4-Acyl-pyrazol-5-olate ; loop_ _publ_author_name 'Geneviève J. Goetz-Grandmont' 'Abdelkader Tayeb' 'Dominique Matt' 'Jean-Pierre Brunette' 'Loic Toupet' _chemical_formula_sum 'C30 H32 N4 O4 Cu1' _chemical_formula_weight 576.2 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 12.955(4) _cell_length_b 14.217(6) _cell_length_c 16.494(9) _cell_angle_alpha 98.82(5) _cell_angle_beta 112.57(5) _cell_angle_gamma 101.15(3) _cell_volume 2664(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 0.862 _cell_measurement_temperature 120 _exptl_crystal_description 'Plate' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour 'Dark green' loop_ _publ_author_name 'Luc Van Oostenryck' 'Bernard Tinant' 'Jean-Paul Declercq' 'Jean-Pierre Dutasta' _chemical_formula_moiety 'C29 H35 N2 O5 P S' _chemical_formula_sum 'C29 H35 N2 O5 P S' _chemical_formula_weight 554.62 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' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 12.674(3) _cell_length_b 20.023(4) _cell_length_c 11.494(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.11(2) _cell_angle_gamma 90.00 _cell_volume 2900.3(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 12.5 _exptl_absorpt_coefficient_mu 0.207 _cell_measurement_temperature 293(2) _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_colour ? _refine_ls_shift/esd_max -0.001 _refine_diff_density_max 0.618 _refine_diff_density_min -0.211 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 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_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)