#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/18/2011810.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_2011810 loop_ _publ_author_name 'Burgess, John' 'Fawcett, John' 'Palma, Vitor' 'Gilani, Syeda R.' _publ_section_title ; Fluoro derivatives of bis(salicylideneaminato-N,O)copper(II) and -oxovanadium(IV) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 277 _journal_page_last 280 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu(C15 H8 F6 NO )2 ]' _chemical_formula_moiety 'C30 H16 Cu F12 N2 O2' _chemical_formula_sum 'C30 H16 Cu F12 N2 O2' _chemical_formula_weight 727.98 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 98.070(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.607(2) _cell_length_b 7.4230(10) _cell_length_c 27.109(2) _cell_measurement_reflns_used 39 _cell_measurement_temperature 290(2) _cell_measurement_theta_max 12.61 _cell_measurement_theta_min 5.38 _cell_volume 2910.3(6) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Fait, 1991)' _computing_data_reduction XSCANS _computing_molecular_graphics SHELXL97 _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 290(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .015 _diffrn_reflns_av_sigmaI/netI .0282 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 3159 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% <2 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .860 _exptl_absorpt_correction_T_max .838 _exptl_absorpt_correction_T_min .761 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (XEMP; SHELXL97) ; _exptl_crystal_colour red-brown _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1452 _exptl_crystal_size_max .47 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .33 _refine_diff_density_max .182 _refine_diff_density_min -.294 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 2566 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all .058 _refine_ls_R_factor_gt .039 _refine_ls_shift/su_max .003 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.4869P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .096 _reflns_number_gt 2013 _reflns_number_total 2566 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gg1032.cif _[local]_cod_data_source_block III _[local]_cod_cif_authors_sg_H-M 'C 2/c' _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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011810 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 .0000 .04523(7) .2500 .04873(18) Uani d S 1 . . Cu O1 .07155(14) -.0100(3) .20003(6) .0644(6) Uani d . 1 . . O N1 .10804(14) .1119(3) .29840(7) .0428(5) Uani d . 1 . . N F1 .2457(6) .0477(15) .4946(4) .141(5) Uani d P .68 A 1 F F2 .1175(6) .008(2) .5179(3) .166(5) Uani d P .68 A 1 F F3 .1671(11) -.1715(10) .4693(3) .173(4) Uani d P .68 A 1 F F1' .1640(14) .107(2) .5225(4) .121(6) Uani d P .32 A 2 F F2' .1169(11) -.133(3) .4888(7) .125(6) Uani d P .32 A 2 F F3' .2422(11) -.036(4) .4795(8) .134(9) Uani d P .32 A 2 F F4 -.1141(9) .5085(19) .3699(4) .135(5) Uani d P .60 B 1 F F5 -.0082(6) .6369(12) .4171(8) .158(4) Uani d P .60 B 1 F F6 -.0968(11) .462(2) .4450(5) .155(5) Uani d P .60 B 1 F F4' -.0423(19) .621(2) .3779(9) .162(8) Uani d P .40 B 2 F F5' -.1383(8) .440(4) .3940(12) .181(9) Uani d P .40 B 2 F F6' -.0524(15) .548(3) .4493(4) .124(6) Uani d P .40 B 2 F C1 .3113(2) .1352(4) .23410(13) .0676(9) Uani d . 1 . . C H1A .3522 .1719 .2617 .081 Uiso calc R 1 . . H C2 .3413(3) .1227(5) .18828(16) .0841(12) Uani d . 1 . . C H2A .4019 .1522 .1847 .101 Uiso calc R 1 . . H C3 .2805(3) .0657(6) .14766(15) .0870(12) Uani d . 1 . . C H3A .3008 .0573 .1167 .104 Uiso calc R 1 . . H C4 .1915(3) .0216(5) .15185(11) .0775(11) Uani d . 1 . . C H4A .1524 -.0174 .1238 .093 Uiso calc R 1 . . H C5 .1572(2) .0342(4) .19826(10) .0555(7) Uani d . 1 . . C C6 .21893(19) .0931(4) .23969(10) .0527(7) Uani d . 1 . . C C7 .19147(18) .1230(4) .28766(10) .0494(7) Uani d . 1 . . C H7A .2378 .1530 .3135 .059 Uiso calc R 1 . . H C8 .09357(16) .1553(4) .34829(9) .0416(6) Uani d . 1 . . C C9 .13664(17) .0633(4) .38885(9) .0493(6) Uani d . 1 . . C H9A .1784 -.0284 .3849 .059 Uiso calc R 1 . . H C10 .11714(19) .1089(4) .43604(9) .0547(7) Uani d . 1 A . C C11 .05585(19) .2440(4) .44253(10) .0586(8) Uani d . 1 . . C H11A .0435 .2737 .4743 .070 Uiso calc R 1 . . H C12 .01275(17) .3356(4) .40126(9) .0506(7) Uani d . 1 B . C C13 .02999(17) .2892(4) .35440(9) .0459(6) Uani d . 1 . . C H13A -.0011 .3478 .3267 .055 Uiso calc R 1 . . H C14 .1618(3) .0015(7) .48027(13) .0826(12) Uani d . 1 . . C C15 -.0527(3) .4862(6) .40737(14) .0764(10) Uani d . 1 . . C 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 Cu1 .0526(3) .0581(3) .0356(2) .000 .00683(18) .000 O1 .0607(13) .0915(17) .0407(10) .0219(11) .0059(9) -.0081(10) N1 .0478(12) .0451(13) .0365(10) .0029(10) .0099(9) -.0012(9) F1 .105(6) .175(8) .120(6) -.001(5) -.061(5) .036(5) F2 .144(6) .285(15) .076(5) .077(7) .044(5) .089(7) F3 .305(13) .092(4) .098(4) .041(7) -.054(6) .033(4) F1' .179(16) .141(11) .035(4) .055(9) -.013(7) .002(5) F2' .137(10) .125(14) .111(12) -.040(10) .013(7) .065(10) F3' .080(11) .22(2) .112(12) .074(12) .039(10) .101(15) F4 .121(9) .183(12) .091(4) .105(9) -.022(4) -.026(5) F5 .129(5) .073(4) .277(12) .010(3) .045(9) -.056(7) F6 .169(10) .174(11) .149(10) .089(7) .113(9) .035(7) F4' .23(2) .104(10) .179(12) .105(11) .129(13) .060(10) F5' .053(4) .205(17) .28(2) .034(7) .005(10) -.140(17) F6' .151(13) .137(13) .078(7) .057(8) -.005(7) -.066(9) C1 .070(2) .0483(18) .092(2) .0023(15) .0360(18) -.0063(17) C2 .089(3) .059(2) .119(3) .009(2) .068(3) .004(2) C3 .113(3) .081(3) .078(2) .037(2) .055(2) .018(2) C4 .097(3) .090(3) .0512(17) .040(2) .0274(17) .0098(17) C5 .069(2) .0529(17) .0472(15) .0237(16) .0178(13) .0061(14) C6 .0620(17) .0404(16) .0610(17) .0073(13) .0275(14) -.0012(13) C7 .0520(16) .0434(16) .0537(15) .0039(13) .0110(12) -.0017(13) C8 .0394(13) .0460(15) .0394(12) -.0006(12) .0055(10) -.0030(12) C9 .0429(14) .0576(18) .0472(14) .0066(14) .0060(11) .0022(14) C10 .0506(16) .071(2) .0414(14) .0005(15) .0024(12) .0063(13) C11 .0571(17) .082(2) .0385(14) .0010(16) .0117(12) -.0066(14) C12 .0455(15) .0581(18) .0487(15) .0047(13) .0090(12) -.0077(14) C13 .0458(14) .0489(16) .0420(13) .0003(13) .0032(11) .0005(12) C14 .083(3) .112(4) .052(2) .013(3) .0061(19) .018(2) C15 .078(3) .087(3) .067(2) .022(2) .020(2) -.008(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 2 1.8688(18) ? Cu1 O1 . 1.8688(18) ? Cu1 N1 . 1.969(2) ? Cu1 N1 2 1.969(2) ? O1 C5 . 1.300(4) ? N1 C7 . 1.295(3) ? N1 C8 . 1.435(3) ? F1 C14 . 1.279(9) ? F2 C14 . 1.285(8) ? F3 C14 . 1.323(8) ? F1' C14 . 1.381(13) ? F2' C14 . 1.234(13) ? F3' C14 . 1.210(15) ? F4 C15 . 1.268(8) ? F5 C15 . 1.302(8) ? F6 C15 . 1.292(8) ? F4' C15 . 1.300(11) ? F5' C15 . 1.297(13) ? F6' C15 . 1.226(9) ? C1 C2 . 1.377(4) ? C1 C6 . 1.413(4) ? C2 C3 . 1.381(5) ? C3 C4 . 1.360(5) ? C4 C5 . 1.421(4) ? C5 C6 . 1.408(4) ? C6 C7 . 1.431(3) ? C8 C9 . 1.370(3) ? C8 C13 . 1.386(3) ? C9 C10 . 1.391(4) ? C10 C11 . 1.372(4) ? C10 C14 . 1.510(4) ? C11 C12 . 1.383(4) ? C12 C13 . 1.373(3) ? C12 C15 . 1.496(4) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 Cu1 O1 2 . 154.66(15) O1 Cu1 N1 2 . 92.84(8) O1 Cu1 N1 . . 93.48(8) O1 Cu1 N1 2 2 93.48(8) O1 Cu1 N1 . 2 92.84(8) N1 Cu1 N1 . 2 150.87(13) C5 O1 Cu1 . . 127.60(19) C7 N1 C8 . . 117.8(2) C7 N1 Cu1 . . 123.90(18) C8 N1 Cu1 . . 118.32(15) C2 C1 C6 . . 120.8(3) C1 C2 C3 . . 119.3(3) C4 C3 C2 . . 121.5(3) C3 C4 C5 . . 121.2(4) O1 C5 C6 . . 124.1(2) O1 C5 C4 . . 118.5(3) C6 C5 C4 . . 117.4(3) C5 C6 C1 . . 119.8(3) C5 C6 C7 . . 122.9(2) C1 C6 C7 . . 117.2(3) N1 C7 C6 . . 126.0(3) C9 C8 C13 . . 120.1(2) C9 C8 N1 . . 122.2(2) C13 C8 N1 . . 117.6(2) C8 C9 C10 . . 119.1(3) C11 C10 C9 . . 121.2(3) C11 C10 C14 . . 120.1(3) C9 C10 C14 . . 118.7(3) C10 C11 C12 . . 119.1(2) C13 C12 C11 . . 120.2(3) C13 C12 C15 . . 119.6(3) C11 C12 C15 . . 120.2(3) C12 C13 C8 . . 120.2(2) F3' C14 F2' . . 111.2(13) F3' C14 F1 . . 34.6(16) F2' C14 F1 . . 132.2(8) F3' C14 F2 . . 128.4(9) F2' C14 F2 . . 62.5(8) F1 C14 F2 . . 108.4(7) F3' C14 F3 . . 71.7(13) F2' C14 F3 . . 46.2(8) F1 C14 F3 . . 104.2(7) F2 C14 F3 . . 105.5(7) F3' C14 F1' . . 103.5(13) F2' C14 F1' . . 104.6(10) F1 C14 F1' . . 71.7(8) F2 C14 F1' . . 43.7(6) F3 C14 F1' . . 137.7(7) F3' C14 C10 . . 114.9(7) F2' C14 C10 . . 113.2(7) F1 C14 C10 . . 112.9(6) F2 C14 C10 . . 113.7(5) F3 C14 C10 . . 111.5(4) F1' C14 C10 . . 108.5(7) F6' C15 F4 . . 127.2(7) F6' C15 F6 . . 41.9(7) F4 C15 F6 . . 106.0(7) F6' C15 F5' . . 103.5(9) F4 C15 F5' . . 42.8(12) F6 C15 F5' . . 67.4(10) F6' C15 F4' . . 107.3(9) F4 C15 F4' . . 62.5(11) F6 C15 F4' . . 134.8(7) F5' C15 F4' . . 102.9(11) F6' C15 F5 . . 63.6(7) F4 C15 F5 . . 109.1(8) F6 C15 F5 . . 104.4(7) F5' C15 F5 . . 135.8(11) F4' C15 F5 . . 50.7(9) F6' C15 C12 . . 117.6(7) F4 C15 C12 . . 113.6(5) F6 C15 C12 . . 112.4(6) F5' C15 C12 . . 112.3(9) F4' C15 C12 . . 112.0(5) F5 C15 C12 . . 110.8(4)