#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/05/2010575.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_2010575 loop_ _publ_author_name 'Boyd, Peter D. W.' 'Rickard, Clifton E. F.' 'Cavell, Kingsley J.' _publ_section_title ; [Bis(diphenylphosphino)alkane](pentane-2,4-dithionato) complexes of nickel(II) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e16 _journal_page_last e18 _journal_paper_doi 10.1107/S0108270199016078 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Ni1 (C26 H24 P2) (C5 H7 S2)] P1 F6' _chemical_formula_moiety 'C31 H31 Ni P2 S2, F6 P' _chemical_formula_sum 'C31 H31 F6 Ni P3 S2' _chemical_formula_weight 733.30 _chemical_name_systematic ; Pentane-2,4-dithione[bis(diphenylphosphino)ethane]nickel(II) hexafluorophosphate. ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 67.3860(10) _cell_angle_beta 76.1050(10) _cell_angle_gamma 72.0880(10) _cell_formula_units_Z 2 _cell_length_a 11.0458(2) _cell_length_b 13.4850(2) _cell_length_c 14.58280(10) _cell_measurement_reflns_used 5722 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 2 _cell_volume 1889.50(5) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 Sheldrick, (1997)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full .973 _diffrn_measured_fraction_theta_max .973 _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area-detector \w' _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 .029 _diffrn_reflns_av_sigmaI/netI .0411 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 17129 _diffrn_reflns_theta_full 26.16 _diffrn_reflns_theta_max 26.16 _diffrn_reflns_theta_min 1.53 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu .799 _exptl_absorpt_correction_T_max .924 _exptl_absorpt_correction_T_min .654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'Irregular fragment' _exptl_crystal_F_000 752 _exptl_crystal_size_max .58 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .10 _refine_diff_density_max .525 _refine_diff_density_min -.562 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 390 _refine_ls_number_reflns 7347 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all .052 _refine_ls_R_factor_gt .039 _refine_ls_shift/su_max .048 _refine_ls_shift/su_mean .002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1337P)^2^+4.2975P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .104 _reflns_number_gt 5871 _reflns_number_total 7347 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qb0153.cif _cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.1337P)^2^+4.2975P] where P = (Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1337P)^2^+4.2975P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2010575 _cod_database_fobs_code 2010575 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ni .17862(3) .20322(2) .16565(2) .03164(10) Uani d . 1 . . Ni P1 .39122(6) .17129(5) .14343(5) .03648(15) Uani d . 1 . . P P2 .21122(6) .02000(5) .20822(5) .03521(15) Uani d . 1 . . P S1 .17338(6) .37820(5) .10715(5) .04250(16) Uani d . 1 . . S S2 -.02490(6) .21214(5) .20673(5) .03737(15) Uani d . 1 . . S C1 .0351(3) .5869(2) .0929(2) .0555(7) Uani d . 1 . . C H1A -.0440 .6354 .0679 .083 Uiso calc R 1 . . H H1B .1070 .5995 .0401 .083 Uiso calc R 1 . . H H1C .0468 .6024 .1494 .083 Uiso calc R 1 . . H C2 .0278(2) .4665(2) .1262(2) .0399(6) Uani d . 1 . . C C3 -.0913(2) .4414(2) .1646(2) .0435(6) Uani d . 1 . . C H3A -.1602 .5017 .1694 .052 Uiso calc R 1 . . H C4 -.1236(2) .3400(2) .19707(19) .0391(6) Uani d . 1 . . C C5 -.2661(3) .3405(3) .2304(3) .0660(9) Uani d . 1 . . C H5A -.3170 .4041 .1846 .099 Uiso calc R 1 . . H H5B -.2911 .3445 .2976 .099 Uiso calc R 1 . . H H5C -.2805 .2732 .2301 .099 Uiso calc R 1 . . H C6 .4599(2) .0323(2) .1321(2) .0449(6) Uani d . 1 . . C H6A .4513 .0337 .0662 .054 Uiso calc R 1 . . H H6B .5513 .0078 .1397 .054 Uiso calc R 1 . . H C7 .3851(2) -.0461(2) .2155(2) .0475(7) Uani d . 1 . . C H7A .4055 -.0576 .2812 .057 Uiso calc R 1 . . H H7B .4074 -.1180 .2060 .057 Uiso calc R 1 . . H C11 .4673(2) .2662(2) .0341(2) .0443(6) Uani d . 1 . . C C12 .5402(3) .3300(2) .0418(3) .0549(7) Uani d . 1 . . C H12A .5530 .3240 .1054 .066 Uiso calc R 1 . . H C13 .5940(3) .4025(3) -.0440(3) .0732(10) Uani d . 1 . . C H13A .6442 .4445 -.0385 .088 Uiso calc R 1 . . H C14 .5734(4) .4128(3) -.1385(3) .0781(11) Uani d . 1 . . C H14A .6097 .4619 -.1964 .094 Uiso calc R 1 . . H C15 .4999(3) .3512(3) -.1474(3) .0744(10) Uani d . 1 . . C H15A .4862 .3586 -.2112 .089 Uiso calc R 1 . . H C16 .4462(3) .2782(3) -.0615(2) .0575(7) Uani d . 1 . . C H16A .3956 .2368 -.0675 .069 Uiso calc R 1 . . H C21 .4446(2) .1655(2) .2552(2) .0412(6) Uani d . 1 . . C C22 .5562(3) .0904(2) .2915(2) .0525(7) Uani d . 1 . . C H22A .6066 .0417 .2572 .063 Uiso calc R 1 . . H C23 .5934(3) .0867(3) .3779(3) .0674(9) Uani d . 1 . . C H23A .6689 .0361 .4012 .081 Uiso calc R 1 . . H C24 .5196(3) .1575(3) .4294(2) .0676(9) Uani d . 1 . . C H24A .5441 .1537 .4883 .081 Uiso calc R 1 . . H C25 .4103(4) .2334(4) .3944(3) .0786(11) Uani d . 1 . . C H25A .3612 .2823 .4289 .094 Uiso calc R 1 . . H C26 .3723(3) .2379(3) .3076(3) .0666(9) Uani d . 1 . . C H26A .2976 .2898 .2842 .080 Uiso calc R 1 . . H C31 .1251(2) -.0533(2) .32668(19) .0412(6) Uani d . 1 . . C C32 .1705(3) -.0757(3) .4167(2) .0653(9) Uani d . 1 . . C H32A .2451 -.0547 .4146 .078 Uiso calc R 1 . . H C33 .1059(4) -.1285(4) .5085(3) .0874(12) Uani d . 1 . . C H33A .1365 -.1423 .5681 .105 Uiso calc R 1 . . H C34 -.0032(4) -.1608(3) .5127(3) .0781(10) Uani d . 1 . . C H34A -.0447 -.1987 .5750 .094 Uiso calc R 1 . . H C35 -.0517(3) -.1376(3) .4248(2) .0630(8) Uani d . 1 . . C H35A -.1273 -.1577 .4279 .076 Uiso calc R 1 . . H C36 .0126(3) -.0840(2) .3319(2) .0510(7) Uani d . 1 . . C H36A -.0199 -.0685 .2726 .061 Uiso calc R 1 . . H C41 .1825(2) -.0180(2) .10884(19) .0374(5) Uani d . 1 . . C C42 .1872(3) -.1290(2) .1248(2) .0489(7) Uani d . 1 . . C H42A .1985 -.1832 .1881 .059 Uiso calc R 1 . . H C43 .1748(3) -.1579(3) .0455(3) .0573(8) Uani d . 1 . . C H43A .1766 -.2316 .0560 .069 Uiso calc R 1 . . H C44 .1600(3) -.0789(3) -.0480(2) .0556(8) Uani d . 1 . . C H44A .1527 -.0995 -.1008 .067 Uiso calc R 1 . . H C45 .1558(3) .0304(3) -.0649(2) .0505(7) Uani d . 1 . . C H45A .1456 .0838 -.1288 .061 Uiso calc R 1 . . H C46 .1668(2) .0610(2) .01360(19) .0414(6) Uani d . 1 . . C H46A .1637 .1352 .0023 .050 Uiso calc R 1 . . H P3 .72389(9) -.27755(7) .31028(6) .0623(2) Uani d . 1 . . P F1 .7095(3) -.15846(19) .3156(2) .1151(9) Uani d . 1 . . F F2 .6925(3) -.2157(2) .19706(16) .1129(9) Uani d . 1 . . F F3 .5729(2) -.2674(2) .3482(2) .1287(11) Uani d . 1 . . F F4 .7398(3) -.3954(2) .3034(2) .1217(10) Uani d . 1 . . F F5 .7509(2) -.3340(2) .42365(15) .1008(8) Uani d . 1 . . F F6 .8732(2) -.2835(2) .27195(18) .1025(8) Uani d . 1 . . F 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 Ni .02854(16) .02656(16) .04205(19) -.00393(11) -.00582(12) -.01546(13) P1 .0285(3) .0385(3) .0475(4) -.0041(2) -.0043(3) -.0237(3) P2 .0365(3) .0262(3) .0451(4) -.0021(2) -.0136(3) -.0138(3) S1 .0338(3) .0295(3) .0641(4) -.0073(2) -.0025(3) -.0184(3) S2 .0315(3) .0297(3) .0485(4) -.0066(2) -.0058(3) -.0111(3) C1 .0557(17) .0338(14) .080(2) -.0070(12) -.0090(15) -.0251(15) C2 .0430(14) .0313(13) .0489(15) -.0040(10) -.0072(11) -.0204(11) C3 .0376(14) .0369(14) .0532(16) .0009(11) -.0061(11) -.0201(12) C4 .0320(12) .0382(14) .0437(14) -.0029(10) -.0049(10) -.0148(11) C5 .0329(15) .0581(19) .099(3) -.0039(13) -.0051(15) -.0264(18) C6 .0342(13) .0459(15) .0624(17) .0034(11) -.0101(12) -.0346(14) C7 .0429(14) .0373(14) .0670(18) .0046(11) -.0226(13) -.0246(13) C11 .0289(12) .0466(15) .0543(16) -.0061(11) .0013(11) -.0202(13) C12 .0405(15) .0520(17) .073(2) -.0108(13) -.0014(14) -.0264(16) C13 .0509(18) .0510(19) .106(3) -.0145(15) .0120(19) -.026(2) C14 .067(2) .050(2) .076(3) -.0016(16) .0206(19) -.0049(18) C15 .069(2) .074(2) .053(2) -.0006(19) .0020(16) -.0125(18) C16 .0510(17) .0628(19) .0537(18) -.0077(14) -.0030(14) -.0215(15) C21 .0353(13) .0475(15) .0475(15) -.0124(11) -.0047(11) -.0219(12) C22 .0531(16) .0451(16) .0632(19) -.0065(13) -.0193(14) -.0199(14) C23 .069(2) .065(2) .073(2) -.0144(17) -.0354(18) -.0143(18) C24 .080(2) .083(2) .0517(19) -.031(2) -.0186(17) -.0208(18) C25 .074(2) .111(3) .070(2) -.009(2) -.0130(19) -.060(2) C26 .0500(17) .092(3) .071(2) .0025(16) -.0153(15) -.054(2) C31 .0502(15) .0283(12) .0438(15) -.0049(11) -.0147(12) -.0093(11) C32 .078(2) .070(2) .0506(18) -.0245(18) -.0194(16) -.0111(16) C33 .113(3) .099(3) .049(2) -.035(3) -.023(2) -.009(2) C34 .106(3) .070(2) .052(2) -.037(2) -.0024(19) -.0057(17) C35 .071(2) .0532(19) .065(2) -.0240(16) -.0043(16) -.0164(16) C36 .0588(17) .0431(16) .0517(17) -.0134(13) -.0126(13) -.0128(13) C41 .0346(12) .0328(13) .0501(15) -.0033(10) -.0098(11) -.0208(11) C42 .0518(16) .0363(14) .0649(18) -.0024(12) -.0173(14) -.0247(14) C43 .0454(16) .0519(18) .091(2) -.0061(13) -.0094(15) -.0454(18) C44 .0379(14) .081(2) .070(2) -.0157(14) -.0004(14) -.0528(19) C45 .0416(14) .074(2) .0433(15) -.0197(14) .0010(12) -.0271(15) C46 .0369(13) .0438(15) .0460(15) -.0109(11) -.0041(11) -.0177(12) P3 .0750(6) .0524(5) .0483(5) -.0028(4) -.0079(4) -.0152(4) F1 .171(3) .0544(13) .1117(19) .0039(14) -.0385(18) -.0316(13) F2 .151(2) .135(2) .0630(14) -.0781(19) -.0371(14) .0018(14) F3 .0768(16) .119(2) .121(2) -.0060(14) .0008(14) .0110(17) F4 .176(3) .0778(17) .124(2) -.0400(17) .0057(19) -.0558(16) F5 .128(2) .0852(16) .0539(12) .0173(14) -.0199(12) -.0149(11) F6 .0784(15) .112(2) .1011(18) -.0113(13) -.0007(13) -.0343(15) 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' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .3393 1.1124 '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 S2 Ni S1 99.53(2) S2 Ni P1 171.43(3) S1 Ni P1 87.53(3) S2 Ni P2 88.06(2) S1 Ni P2 171.04(3) P1 Ni P2 85.34(2) C11 P1 C21 108.08(12) C11 P1 C6 106.15(12) C21 P1 C6 105.96(12) C11 P1 Ni 117.84(9) C21 P1 Ni 109.72(8) C6 P1 Ni 108.44(8) C31 P2 C41 108.07(12) C31 P2 C7 106.11(13) C41 P2 C7 102.25(12) C31 P2 Ni 117.95(8) C41 P2 Ni 111.76(8) C7 P2 Ni 109.41(9) C2 S1 Ni 116.63(9) C4 S2 Ni 116.61(9) C3 C2 C1 118.6(2) C3 C2 S1 128.01(19) C1 C2 S1 113.39(19) C4 C3 C2 129.6(2) C3 C4 C5 117.1(2) C3 C4 S2 128.75(19) C5 C4 S2 114.19(19) C7 C6 P1 107.00(17) C6 C7 P2 106.99(18) C12 C11 C16 119.1(3) C12 C11 P1 122.8(2) C16 C11 P1 118.0(2) C13 C12 C11 120.3(3) C12 C13 C14 119.9(3) C15 C14 C13 120.5(3) C14 C15 C16 119.7(3) C15 C16 C11 120.4(3) C22 C21 C26 118.0(2) C22 C21 P1 122.1(2) C26 C21 P1 119.8(2) C23 C22 C21 120.9(3) C24 C23 C22 120.2(3) C25 C24 C23 120.2(3) C24 C25 C26 120.0(3) C25 C26 C21 120.7(3) C36 C31 C32 118.6(3) C36 C31 P2 122.7(2) C32 C31 P2 118.6(2) C33 C32 C31 120.5(3) C34 C33 C32 120.4(3) C33 C34 C35 120.2(3) C34 C35 C36 119.7(3) C31 C36 C35 120.5(3) C46 C41 C42 119.2(2) C46 C41 P2 120.23(18) C42 C41 P2 120.3(2) C43 C42 C41 119.5(3) C44 C43 C42 120.5(3) C43 C44 C45 120.6(3) C44 C45 C46 119.7(3) C41 C46 C45 120.5(3) F4 P3 F5 90.19(15) F4 P3 F1 179.09(16) F5 P3 F1 90.38(13) F4 P3 F6 91.25(15) F5 P3 F6 90.83(14) F1 P3 F6 88.03(16) F4 P3 F2 92.05(16) F5 P3 F2 177.39(15) F1 P3 F2 87.40(15) F6 P3 F2 90.46(14) F4 P3 F3 90.53(18) F5 P3 F3 89.60(15) F1 P3 F3 90.19(17) F6 P3 F3 178.17(16) F2 P3 F3 89.04(15) 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 Ni S2 . 2.1609(6) ? Ni S1 . 2.1658(7) ? Ni P1 . 2.2192(6) ? Ni P2 . 2.2361(6) ? P1 C11 . 1.826(3) ? P1 C21 . 1.829(3) ? P1 C6 . 1.849(2) ? P2 C31 . 1.828(3) ? P2 C41 . 1.832(2) ? P2 C7 . 1.862(3) ? S1 C2 . 1.715(2) ? S2 C4 . 1.707(2) ? C1 C2 . 1.528(4) ? C2 C3 . 1.391(4) ? C3 C4 . 1.393(4) ? C4 C5 . 1.530(4) ? C6 C7 . 1.532(4) ? C11 C12 . 1.395(4) ? C11 C16 . 1.409(4) ? C12 C13 . 1.391(5) ? C13 C14 . 1.397(6) ? C14 C15 . 1.383(6) ? C15 C16 . 1.394(5) ? C21 C22 . 1.399(4) ? C21 C26 . 1.406(4) ? C22 C23 . 1.395(4) ? C23 C24 . 1.385(5) ? C24 C25 . 1.379(5) ? C25 C26 . 1.401(4) ? C31 C36 . 1.403(4) ? C31 C32 . 1.408(4) ? C32 C33 . 1.389(5) ? C33 C34 . 1.383(5) ? C34 C35 . 1.395(5) ? C35 C36 . 1.402(4) ? C41 C46 . 1.399(4) ? C41 C42 . 1.409(3) ? C42 C43 . 1.401(4) ? C43 C44 . 1.379(5) ? C44 C45 . 1.387(4) ? C45 C46 . 1.398(4) ? P3 F4 . 1.583(2) ? P3 F5 . 1.591(2) ? P3 F1 . 1.595(2) ? P3 F6 . 1.596(2) ? P3 F2 . 1.606(2) ? P3 F3 . 1.607(3) ?