#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010367.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_2010367 loop_ _publ_author_name 'Gordon, J.C.' 'Poli, R.' _publ_section_title ; A Tetranuclear Butterfly Cluster of Molybdenum, [PPh~4~]~2~[Mo~4~I~11~] ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 14 _journal_page_last 18 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C48 H40 I11 Mo4 P2' _chemical_formula_weight 2458.5 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source 'TEXSAN (Molecular Structure Corporation,year?' _cell_angle_alpha 94.72(3) _cell_angle_beta 91.80(5) _cell_angle_gamma 107.98(5) _cell_formula_units_Z 2 _cell_length_a 10.474(6) _cell_length_b 12.862(5) _cell_length_c 23.882(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 13.5 _cell_measurement_theta_min 8.5 _cell_volume 3044(3) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.003 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 8368 _diffrn_reflns_theta_max 22.5 _diffrn_standards_decay_% -0.2 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.391 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_type empirical _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.68 _exptl_crystal_density_meas 2.56 _exptl_crystal_description plate _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.91 _refine_diff_density_min -2.45 _refine_ls_goodness_of_fit_obs 2.97 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 586 _refine_ls_number_reflns 5900 _refine_ls_R_factor_obs 0.060 _refine_ls_shift/esd_max 0.47 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 1/\s^2^(|F~o~|) _refine_ls_wR_factor_obs 0.078 _reflns_number_observed 5900 _reflns_number_total 7938 _reflns_observed_criterion F~o~>6\s(F~o~) _[local]_cod_data_source_file gr1011.cif _[local]_cod_data_source_block gr1011_structure_1_of_1 _cod_original_cell_volume 3044(5) _cod_database_code 2010367 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z I(1) .0085(2) -.01710(10) .71882(8) I(2) .63230(10) .35830(10) .75412(8) I(3) .1386(2) .4661(2) .59111(8) I(4) .1514(2) .41970(10) .93927(7) I(13) -.0786(2) .24590(10) .67591(8) I(14) -.0635(2) .20880(10) .82592(8) I(23) .4226(2) .5420(2) .70010(10) I(24) .4364(2) .51990(10) .84860(8) I(34) .0843(2) .51890(10) .77417(8) I(123) .28880(10) .22690(10) .65588(6) I(124) .30270(10) .19580(10) .82728(7) Mo(1) .1183(2) .21450(10) .74476(8) Mo(2) .3646(2) .36360(10) .75694(8) Mo(3) .1751(2) .39180(10) .69709(8) Mo(4) .1827(2) .37010(10) .82332(9) P(1) .7544(5) .1533(4) .0669(3) P(2) .3888(6) .1828(4) .4381(3) C(10) .698(2) .2290(10) .0177(9) C(11) .580(2) .251(2) .0230(10) C(12) .533(2) .305(2) -.0180(10) C(13) .611(3) .339(2) -.0620(10) C(14) .731(3) .318(2) -.0660(10) C(15) .772(2) .261(2) -.0280(10) C(20) .629(2) .112(2) .1160(10) C(21) .543(2) -.0010(10) .1170(10) C(22) .441(2) -.026(2) .1530(10) C(23) .422(2) .054(2) .1910(10) C(24) .499(2) .156(2) .1930(10) C(25) .608(2) .189(2) .1560(10) C(30) .904(2) .2380(10) .1050(10) C(31) .952(2) .199(2) .1520(10) C(32) 1.080(2) .254(2) .1780(10) C(33) 1.156(2) .343(2) .1600(10) C(34) 1.116(2) .388(2) .1140(10) C(35) .989(2) .333(2) .0880(10) C(40) .784(2) .0370(10) .0310(10) C(41) .738(2) .005(2) -.0220(10) C(42) .759(3) -.090(2) -.0500(10) C(43) .827(2) -.149(2) -.0220(10) C(44) .875(2) -.115(2) .0310(10) C(45) .853(2) -.023(2) .0580(10) C(50) .504(2) .269(2) .4910(10) C(51) .484(2) .359(2) .5200(10) C(52) .569(3) .410(2) .5660(10) C(53) .674(3) .376(2) .5810(10) C(54) .700(3) .292(3) .552(2) C(55) .614(3) .237(2) .5060(10) C(60) .477(2) .131(2) .3840(10) C(61) .438(2) .023(2) .3640(10) C(62) .508(3) -.016(2) .3250(10) C(63) .619(4) .051(3) .3060(10) C(64) .664(3) .166(3) .329(2) C(65) .589(3) .198(2) .3680(10) C(70) .277(2) .0710(10) .4719(9) C(71) .308(2) .051(2) .5210(10) C(72) .218(3) -.038(2) .5470(10) C(73) .106(3) -.108(2) .514(2) C(74) .080(2) -.085(2) .4660(10) C(75) .162(2) .006(2) .4420(10) C(80) .287(2) .256(2) .4030(10) C(81) .293(3) .277(2) .3520(10) C(82) .218(3) .330(2) .3270(10) C(83) .130(4) .362(2) .357(2) C(84) .114(3) .345(2) .412(2) C(85) .196(2) .288(2) .4370(10) H11 .5276 .2293 .0558 H12 .4445 .3142 -.0164 H13 .5804 .3786 -.0895 H14 .7888 .3462 -.0969 H15 .8539 .2425 -.0324 H21 .5593 -.0579 .0908 H22 .3822 -.1004 .1520 H23 .3513 .0339 .2179 H24 .4805 .2100 .2178 H25 .6687 .2631 .1596 H31 .8967 .1343 .1665 H32 1.1100 .2249 .2107 H33 1.2435 .3786 .1780 H34 1.1735 .4544 .1015 H35 .9593 .3641 .0559 H41 .6879 .0463 -.0401 H42 .7268 -.1112 -.0893 H43 .8409 -.2128 -.0413 H44 .9233 -.1551 .0494 H45 .8879 .0002 .0974 H51 .4099 .3839 .5085 H52 .5538 .4703 .5877 H53 .7369 .4137 .6125 H54 .7753 .2697 .5631 H55 .6336 .1789 .4837 H61 .3562 -.0279 .3768 H62 .4769 -.0933 .3119 H63 .6676 .0237 .2777 H64 .7466 .2152 .3164 H65 .6208 .2768 .3835 H71 .3938 .0953 .5397 H72 .2387 -.0474 .5872 H73 .0490 -.1750 .5287 H74 -.0035 -.1300 .4471 H75 .1397 .0224 .4045 H81 .3570 .2529 .3297 H82 .2270 .3428 .2862 H83 .0762 .4027 .3409 H84 .0471 .3690 .4336 H85 .1890 .2705 .4757 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag I(1) Mo(1) 2.848(3) yes I(2) Mo(2) 2.829(3) yes I(3) Mo(3) 2.833(3) yes I(4) Mo(4) 2.843(3) yes I(13) Mo(1) 2.744(3) yes I(13) Mo(3) 2.743(3) yes I(14) Mo(1) 2.749(3) yes I(14) Mo(4) 2.773(3) yes I(23) Mo(2) 2.681(3) yes I(23) Mo(3) 2.707(3) yes I(24) Mo(2) 2.764(3) yes I(24) Mo(4) 2.772(3) yes I(34) Mo(3) 2.745(3) yes I(34) Mo(4) 2.760(3) yes I(123) Mo(1) 2.800(3) yes I(123) Mo(2) 2.804(3) yes I(123) Mo(3) 2.859(2) yes I(124) Mo(1) 2.793(3) yes I(124) Mo(2) 2.775(2) yes I(124) Mo(4) 2.895(3) yes Mo(1) Mo(2) 2.688(3) yes Mo(1) Mo(3) 2.547(3) yes Mo(1) Mo(4) 2.540(3) yes Mo(2) Mo(3) 2.543(3) yes Mo(2) Mo(4) 2.533(3) yes Mo(3) Mo(4) 3.051(3) yes P(1) C(10) 1.78(2) yes P(1) C(20) 1.78(2) yes P(1) C(30) 1.78(2) yes P(1) C(40) 1.78(2) yes P(2) C(50) 1.78(2) yes P(2) C(60) 1.81(2) yes P(2) C(70) 1.82(2) yes P(2) C(80) 1.86(2) yes C(10) C(11) 1.36(3) no C(10) C(15) 1.37(3) no C(11) H11 0.979 no C(11) C(12) 1.40(3) no C(12) H12 0.978 no C(12) C(13) 1.37(3) no C(13) H13 0.968 no C(13) C(14) 1.37(3) no C(14) H14 0.986 no C(14) C(15) 1.36(3) no C(15) H15 0.961 no C(20) C(25) 1.39(3) no C(20) C(21) 1.45(3) no C(21) H21 0.981 no C(21) C(22) 1.37(3) no C(22) H22 0.965 no C(22) C(23) 1.39(3) no C(23) H23 0.974 no C(23) C(24) 1.30(3) no C(24) H24 0.952 no C(24) C(25) 1.44(3) no C(25) H25 0.968 no C(30) C(35) 1.38(3) no C(30) C(31) 1.41(3) no C(31) H31 0.958 no C(31) C(32) 1.40(3) no C(32) H32 0.979 no C(32) C(33) 1.29(3) no C(33) H33 0.958 no C(33) C(34) 1.39(3) no C(34) H34 0.964 no C(34) C(35) 1.39(3) no C(35) H35 0.969 no C(40) C(41) 1.33(3) no C(40) C(45) 1.39(3) no C(41) H41 0.966 no C(41) C(42) 1.43(3) no C(42) H42 0.976 no C(42) C(43) 1.39(4) no C(43) H43 0.954 no C(43) C(44) 1.34(3) no C(44) H44 0.955 no C(44) C(45) 1.38(3) no C(45) H45 0.980 no C(50) C(51) 1.37(3) no C(50) C(55) 1.38(3) no C(51) H51 0.965 no C(51) C(52) 1.36(3) no C(52) H52 0.962 no C(52) C(53) 1.36(4) no C(53) H53 0.973 no C(53) C(54) 1.34(4) no C(54) H54 0.960 no C(54) C(55) 1.39(4) no C(55) H55 0.963 no C(60) C(65) 1.32(3) no C(60) C(61) 1.36(3) no C(61) H61 0.977 no C(61) C(62) 1.36(4) no C(62) H62 0.968 no C(62) C(63) 1.33(4) no C(63) H63 0.972 no C(63) C(64) 1.45(4) no C(64) H64 0.972 no C(64) C(65) 1.36(4) no C(65) H65 0.997 no C(70) C(71) 1.28(3) no C(70) C(75) 1.38(3) no C(71) H71 0.973 no C(71) C(72) 1.44(3) no C(72) H72 1.008 no C(72) C(73) 1.40(4) no C(73) H73 0.990 no C(73) C(74) 1.24(4) no C(74) H74 0.963 no C(74) C(75) 1.40(3) no C(75) H75 0.980 no C(80) C(81) 1.27(3) no C(80) C(85) 1.40(3) no C(81) H81 0.974 no C(81) C(82) 1.36(4) no C(82) H82 0.993 no C(82) C(83) 1.34(5) no C(83) H83 0.973 no C(83) C(84) 1.36(5) no C(84) H84 0.987 no C(84) C(85) 1.43(4) no C(85) H85 0.966 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Mo(1) I(13) Mo(3) 55.31(7) yes Mo(1) I(14) Mo(4) 54.76(7) yes Mo(2) I(23) Mo(3) 56.31(8) yes Mo(2) I(24) Mo(4) 54.45(7) yes Mo(3) I(34) Mo(4) 67.31(7) yes Mo(1) I(123) Mo(2) 57.33(7) yes Mo(1) I(123) Mo(3) 53.48(6) yes Mo(2) I(123) Mo(3) 53.35(6) yes Mo(1) I(124) Mo(2) 57.73(7) yes Mo(1) I(124) Mo(4) 53.00(6) yes Mo(2) I(124) Mo(4) 53.02(6) yes Mo(2) Mo(1) Mo(3) 58.05(8) yes Mo(2) Mo(1) Mo(4) 57.87(8) yes Mo(2) Mo(1) I(1) 136.75(9) yes Mo(2) Mo(1) I(13) 120.32(9) yes Mo(2) Mo(1) I(14) 120.50(10) yes Mo(2) Mo(1) I(123) 61.42(7) yes Mo(2) Mo(1) I(124) 60.80(7) yes Mo(3) Mo(1) Mo(4) 73.72(8) yes Mo(3) Mo(1) I(1) 140.60(10) yes Mo(3) Mo(1) I(13) 62.32(8) yes Mo(3) Mo(1) I(14) 112.00(10) yes Mo(3) Mo(1) I(123) 64.45(7) yes Mo(3) Mo(1) I(124) 117.80(9) yes Mo(4) Mo(1) I(1) 145.00(10) yes Mo(4) Mo(1) I(13) 107.70(10) yes Mo(4) Mo(1) I(14) 63.10(8) yes Mo(4) Mo(1) I(123) 117.91(9) yes Mo(4) Mo(1) I(124) 65.55(8) yes I(1) Mo(1) I(13) 90.35(9) yes I(1) Mo(1) I(14) 90.47(8) yes I(1) Mo(1) I(123) 90.52(8) yes I(1) Mo(1) I(124) 93.29(8) yes I(13) Mo(1) I(14) 83.50(8) yes I(13) Mo(1) I(124) 171.80(10) yes I(13) Mo(1) I(123) 91.51(9) yes I(14) Mo(1) I(124) 89.17(9) yes I(14) Mo(1) I(123) 174.92(9) yes I(123) Mo(1) I(124) 95.75(8) yes Mo(1) Mo(2) Mo(4) 58.12(8) yes Mo(1) Mo(2) Mo(3) 58.20(7) yes Mo(1) Mo(2) I(2) 136.02(8) yes Mo(1) Mo(2) I(23) 120.40(10) yes Mo(1) Mo(2) I(24) 120.80(10) yes Mo(1) Mo(2) I(124) 61.47(7) yes Mo(1) Mo(2) I(123) 61.25(8) yes Mo(3) Mo(2) Mo(4) 73.91(8) yes Mo(3) Mo(2) I(2) 142.90(10) yes Mo(3) Mo(2) I(23) 62.36(9) yes Mo(3) Mo(2) I(24) 109.99(9) yes Mo(3) Mo(2) I(124) 118.6(9) yes Mo(3) Mo(2) I(123) 64.43(8) yes Mo(4) Mo(2) I(2) 142.70(10) yes Mo(4) Mo(2) I(23) 108.80(10) yes Mo(4) Mo(2) I(24) 62.95(8) yes Mo(4) Mo(2) I(123) 117.98(9) yes Mo(4) Mo(2) I(124) 65.92(7) yes I(2) Mo(2) I(23) 91.60(10) yes I(2) Mo(2) I(24) 90.48(9) yes I(2) Mo(2) I(123) 91.82(9) yes I(2) Mo(2) I(124) 90.59(8) yes I(23) Mo(2) I(24) 82.31(9) yes I(23) Mo(2) I(124) 173.00(10) yes I(23) Mo(2) I(123) 90.60(10) yes I(24) Mo(2) I(123) 172.58(8) yes I(24) Mo(2) I(124) 90.97(8) yes I(124) Mo(2) I(123) 96.05(7) yes Mo(1) Mo(3) Mo(2) 63.76(8) yes Mo(1) Mo(3) Mo(4) 53.03(7) yes Mo(1) Mo(3) I(3) 140.00(10) yes Mo(1) Mo(3) I(13) 62.37(8) yes Mo(1) Mo(3) I(23) 124.90(10) yes Mo(1) Mo(3) I(34) 99.67(9) yes Mo(1) Mo(3) I(123) 62.06(7) yes Mo(2) Mo(3) Mo(4) 52.89(7) yes Mo(2) Mo(3) I(3) 138.10(10) yes Mo(2) Mo(3) I(13) 126.07(9) yes Mo(2) Mo(3) I(23) 61.32(8) yes Mo(2) Mo(3) I(34) 99.63(9) yes Mo(2) Mo(3) I(123) 62.22(7) yes Mo(4) Mo(3) I(3) 162.34(9) yes Mo(4) Mo(3) I(13) 94.71(9) yes Mo(4) Mo(3) I(23) 94.60(10) yes Mo(4) Mo(3) I(34) 56.57(6) yes Mo(4) Mo(3) I(123) 101.43(7) yes I(3) Mo(3) I(13) 86.34(9) yes I(3) Mo(3) I(23) 84.40(10) yes I(3) Mo(3) I(34) 105.81(8) yes I(3) Mo(3) I(123) 96.18(8) yes I(13) Mo(3) I(23) 170.60(10) yes I(13) Mo(3) I(34) 91.45(9) yes I(13) Mo(3) I(123) 90.28(8) yes I(23) Mo(3) I(34) 92.80(10) yes I(23) Mo(3) I(123) 88.88(9) yes I(34) Mo(3) I(123) 158.00(8) yes Mo(1) Mo(4) Mo(2) 64.00(8) yes Mo(1) Mo(4) Mo(3) 53.25(7) yes Mo(1) Mo(4) I(4) 142.51(9) yes Mo(1) Mo(4) I(14) 62.15(8) yes Mo(1) Mo(4) I(24) 126.40(10) yes Mo(1) Mo(4) I(34) 99.47(9) yes Mo(1) Mo(4) I(124) 61.44(7) yes Mo(2) Mo(4) Mo(3) 53.20(7) yes Mo(2) Mo(4) I(4) 140.20(10) yes Mo(2) Mo(4) I(14) 125.60(10) yes Mo(2) Mo(4) I(24) 62.61(8) yes Mo(2) Mo(4) I(34) 99.50(9) yes Mo(2) Mo(4) I(124) 61.07(7) yes Mo(3) Mo(4) I(4) 157.75(8) yes Mo(3) Mo(4) I(14) 97.82(9) yes Mo(3) Mo(4) I(24) 96.49(9) yes Mo(3) Mo(4) I(34) 56.12(6) yes Mo(3) Mo(4) I(124) 100.54(8) yes I(4) Mo(4) I(14) 85.00(9) yes I(4) Mo(4) I(24) 82.67(9) yes I(4) Mo(4) I(34) 101.67(8) yes I(4) Mo(4) I(124) 101.65(8) yes I(14) Mo(4) I(24) 165.50(10) yes I(14) Mo(4) I(34) 96.18(9) yes I(14) Mo(4) I(124) 86.67(8) yes I(24) Mo(4) I(34) 93.80(8) yes I(24) Mo(4) I(124) 88.34(8) yes I(34) Mo(4) I(124) 156.70(10) yes C(30) P(1) C(40) 110.0(10) no C(30) P(1) C(20) 108.0(10) no C(30) P(1) C(10) 110.0(10) no C(40) P(1) C(20) 111.0(10) no C(40) P(1) C(10) 110.0(10) no C(20) P(1) C(10) 109.0(10) no C(50) P(2) C(60) 111.0(10) no C(50) P(2) C(70) 107.0(10) no C(50) P(2) C(80) 112.0(10) no C(60) P(2) C(70) 111.0(10) no C(60) P(2) C(80) 107.0(10) no C(70) P(2) C(80) 109.0(10) no C(11) C(10) C(15) 120(2) no C(11) C(10) P(1) 121(2) no C(15) C(10) P(1) 119(2) no C(10) C(11) C(12) 120(2) no C(13) C(12) C(11) 119(2) no C(12) C(13) C(14) 120(2) no C(15) C(14) C(13) 121(2) no C(14) C(15) C(10) 120(2) no C(25) C(20) C(21) 117(2) no C(25) C(20) P(1) 121(2) no C(21) C(20) P(1) 123(2) no C(22) C(21) C(20) 120(2) no C(21) C(22) C(23) 121(2) no C(24) C(23) C(22) 120(2) no C(23) C(24) C(25) 122(2) no C(20) C(25) C(24) 120(2) no C(35) C(30) C(31) 115(2) no C(35) C(30) P(1) 125(2) no C(31) C(30) P(1) 119.0(10) no C(32) C(31) C(30) 121(2) no C(33) C(32) C(31) 121(2) no C(32) C(33) C(34) 122(2) no C(33) C(34) C(35) 118(2) no C(30) C(35) C(34) 123(2) no C(41) C(40) C(45) 119(2) no C(41) C(40) P(1) 120(2) no C(45) C(40) P(1) 121(2) no C(40) C(41) C(42) 119(2) no C(43) C(42) C(41) 121(3) no C(44) C(43) C(42) 119(2) no C(43) C(44) C(45) 121(2) no C(44) C(45) C(40) 121(2) no C(51) C(50) C(55) 120(2) no C(51) C(50) P(2) 124(2) no C(55) C(50) P(2) 116(2) no C(52) C(51) C(50) 118(2) no C(53) C(52) C(51) 122(2) no C(54) C(53) C(52) 121(3) no C(53) C(54) C(55) 119(3) no C(50) C(55) C(54) 120(2) no C(65) C(60) C(61) 119(2) no C(65) C(60) P(2) 118(2) no C(61) C(60) P(2) 122(2) no C(62) C(61) C(60) 122(2) no C(63) C(62) C(61) 120(3) no C(62) C(63) C(64) 119(3) no C(65) C(64) C(63) 117(3) no C(60) C(65) C(64) 123(3) no C(71) C(70) C(75) 121(2) no C(71) C(70) P(2) 121(2) no C(75) C(70) P(2) 118(2) no C(70) C(71) C(72) 120(2) no C(73) C(72) C(71) 118(3) no C(74) C(73) C(72) 120(3) no C(73) C(74) C(75) 122(2) no C(70) C(75) C(74) 119(2) no C(81) C(80) C(85) 121(2) no C(81) C(80) P(2) 125(2) no C(85) C(80) P(2) 115(2) no C(80) C(81) C(82) 124(3) no C(83) C(82) C(81) 118(3) no C(82) C(83) C(84) 123(3) no C(83) C(84) C(85) 117(3) no C(80) C(85) C(84) 118(3) no