#------------------------------------------------------------------------------ #$Date: 2011-01-02 22:00:31 +0200 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2000014.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_2000014 loop_ _publ_author_name 'Jin, Song' 'Popp, Friedrich' 'Boettcher, Shannon W.' 'Yuan, Min' 'Oertel, Catherine M.' 'DiSalvo, Francis J.' _publ_section_title ; Synthesis, characterization and properties of Mo6S8(4-tert-butylpyridine)6 and related M6S8L6 cluster complexes (M = Mo, W) ; _journal_issue 16 _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _journal_page_first 3096 _journal_year 2002 _chemical_formula_moiety 'Mo6 S8 (CH5N)6' _chemical_formula_sum 'C6 H30 Mo6 N6 S8' _chemical_formula_weight 1018.48 _chemical_name_common 'molybdenum sulfide cluster with' _chemical_name_systematic ; octakis(mu!3$-sulfido)-hexakis(methylamine) -hexa-molybdenum ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 116.821(2) _cell_angle_beta 103.418(2) _cell_angle_gamma 106.402(2) _cell_formula_units_Z 1 _cell_length_a 9.0965(10) _cell_length_b 9.1746(10) _cell_length_c 9.5609(10) _cell_measurement_temperature 173(2) _cell_volume 619.97(12) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'BRUKER SMART' _computing_data_reduction SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6962 _diffrn_reflns_theta_full 27.88 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_min 2.57 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.623 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.461776 _exptl_absorpt_correction_type empirical _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.728 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_method 'not measured' _exptl_crystal_description wedge _exptl_crystal_F_000 488 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.050 _refine_diff_density_min -1.372 _refine_diff_density_rms 0.256 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 2882 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.127 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0401 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1023 _refine_ls_wR_factor_ref 0.1092 _reflns_number_gt 2349 _reflns_number_total 2882 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b202246j.txt _[local]_cod_data_source_block final_3 _[local]_cod_cif_authors_sg_H-M P-1 _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 ; _cod_database_code 2000014 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.44204(6) 0.63172(6) 0.41187(6) 0.01048(14) Uani 1 1 d . . . Mo2 Mo 0.69786(5) 0.55082(6) 0.46539(6) 0.01049(14) Uani 1 1 d . . . Mo3 Mo 0.38476(6) 0.28777(6) 0.27617(6) 0.01054(14) Uani 1 1 d . . . S4 S 0.52446(18) 0.4738(2) 0.18378(19) 0.0167(3) Uani 1 1 d . . . S5 S 0.62932(17) 0.22537(19) 0.34162(19) 0.0152(3) Uani 1 1 d . . . S6 S 0.15447(17) 0.37724(19) 0.24544(18) 0.0144(3) Uani 1 1 d . . . S7 S 0.26593(17) 0.13390(19) 0.40437(19) 0.0154(3) Uani 1 1 d . . . N8 N 0.3853(6) 0.7912(7) 0.2966(7) 0.0206(12) Uani 1 1 d . . . H8A H 0.351(2) 0.849(3) 0.348(3) 0.025 Uiso 1 1 calc R . . H8B H 0.466(5) 0.853(4) 0.3088(10) 0.025 Uiso 1 1 calc R . . C9 C 0.2679(8) 0.6884(10) 0.1129(8) 0.0292(16) Uani 1 1 d . . . H9A H 0.2554 0.7740 0.0820 0.044 Uiso 1 1 calc R . . H9B H 0.1576 0.6079 0.0938 0.044 Uiso 1 1 calc R . . H9C H 0.3128 0.6150 0.0410 0.044 Uiso 1 1 calc R . . N10 N 0.9332(6) 0.6069(7) 0.4109(7) 0.0205(12) Uani 1 1 d . . . H10A H 1.018(4) 0.652(2) 0.503(5) 0.025 Uiso 1 1 calc R . . H10B H 0.9248(7) 0.505(5) 0.336(4) 0.025 Uiso 1 1 calc R . . C11 C 0.9688(8) 0.7282(9) 0.3498(9) 0.0278(15) Uani 1 1 d . . . H11A H 1.0721 0.7403 0.3317 0.042 Uiso 1 1 calc R . . H11B H 0.9838 0.8486 0.4363 0.042 Uiso 1 1 calc R . . H11C H 0.8742 0.6767 0.2408 0.042 Uiso 1 1 calc R . . N12 N 0.2443(6) 0.0377(7) -0.0035(6) 0.0213(12) Uani 1 1 d . . . H12A H 0.302(4) -0.003(3) -0.0240(14) 0.026 Uiso 1 1 calc R . . H12B H 0.172(4) -0.031(4) -0.0085(7) 0.026 Uiso 1 1 calc R . . C13 C 0.1780(8) 0.0684(9) -0.1378(8) 0.0279(15) Uani 1 1 d . . . H13A H 0.1210 -0.0475 -0.2510 0.042 Uiso 1 1 calc R . . H13B H 0.2714 0.1553 -0.1364 0.042 Uiso 1 1 calc R . . H13C H 0.0975 0.1178 -0.1157 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0111(2) 0.0107(2) 0.0132(3) 0.0079(2) 0.00683(19) 0.00567(18) Mo2 0.0103(2) 0.0107(2) 0.0135(3) 0.0074(2) 0.00743(19) 0.00525(18) Mo3 0.0108(2) 0.0100(2) 0.0112(3) 0.0055(2) 0.00575(18) 0.00467(18) S4 0.0209(7) 0.0218(7) 0.0143(7) 0.0123(6) 0.0120(6) 0.0100(6) S5 0.0155(7) 0.0136(7) 0.0179(8) 0.0074(6) 0.0095(6) 0.0087(5) S6 0.0110(6) 0.0165(7) 0.0155(7) 0.0088(6) 0.0041(5) 0.0073(5) S7 0.0137(7) 0.0101(6) 0.0207(8) 0.0085(6) 0.0078(6) 0.0027(5) N8 0.027(3) 0.021(3) 0.026(3) 0.018(2) 0.012(2) 0.015(2) C9 0.033(4) 0.039(4) 0.024(4) 0.021(3) 0.011(3) 0.021(3) N10 0.021(3) 0.021(3) 0.025(3) 0.014(2) 0.016(2) 0.009(2) C11 0.032(4) 0.028(4) 0.037(4) 0.024(3) 0.024(3) 0.012(3) N12 0.024(3) 0.017(2) 0.018(3) 0.008(2) 0.008(2) 0.009(2) C13 0.033(4) 0.027(3) 0.020(4) 0.011(3) 0.005(3) 0.017(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Mo1 S4 89.74(14) . . ? N8 Mo1 S7 91.49(13) . 2_666 ? S4 Mo1 S7 90.20(5) . 2_666 ? N8 Mo1 S6 95.51(13) . . ? S4 Mo1 S6 90.65(5) . . ? S7 Mo1 S6 172.95(5) 2_666 . ? N8 Mo1 S5 96.84(14) . 2_666 ? S4 Mo1 S5 173.36(5) . 2_666 ? S7 Mo1 S5 88.75(5) 2_666 2_666 ? S6 Mo1 S5 89.60(5) . 2_666 ? N8 Mo1 Mo3 133.54(13) . . ? S4 Mo1 Mo3 57.32(4) . . ? S7 Mo1 Mo3 117.64(4) 2_666 . ? S6 Mo1 Mo3 57.44(4) . . ? S5 Mo1 Mo3 117.68(4) 2_666 . ? N8 Mo1 Mo2 130.99(13) . . ? S4 Mo1 Mo2 57.04(4) . . ? S7 Mo1 Mo2 57.65(4) 2_666 . ? S6 Mo1 Mo2 117.43(4) . . ? S5 Mo1 Mo2 117.19(4) 2_666 . ? Mo3 Mo1 Mo2 60.052(18) . . ? N8 Mo1 Mo2 139.09(13) . 2_666 ? S4 Mo1 Mo2 117.41(4) . 2_666 ? S7 Mo1 Mo2 116.60(4) 2_666 2_666 ? S6 Mo1 Mo2 57.01(4) . 2_666 ? S5 Mo1 Mo2 57.57(4) 2_666 2_666 ? Mo3 Mo1 Mo2 60.147(19) . 2_666 ? Mo2 Mo1 Mo2 89.89(2) . 2_666 ? N8 Mo1 Mo3 136.24(13) . 2_666 ? S4 Mo1 Mo3 117.03(4) . 2_666 ? S7 Mo1 Mo3 57.02(4) 2_666 2_666 ? S6 Mo1 Mo3 116.58(4) . 2_666 ? S5 Mo1 Mo3 57.18(4) 2_666 2_666 ? Mo3 Mo1 Mo3 89.96(2) . 2_666 ? Mo2 Mo1 Mo3 60.027(18) . 2_666 ? Mo2 Mo1 Mo3 59.600(18) 2_666 2_666 ? N10 Mo2 S4 90.79(14) . . ? N10 Mo2 S6 95.26(14) . 2_666 ? S4 Mo2 S6 173.95(5) . 2_666 ? N10 Mo2 S7 94.48(14) . 2_666 ? S4 Mo2 S7 89.90(5) . 2_666 ? S6 Mo2 S7 89.46(5) 2_666 2_666 ? N10 Mo2 S5 92.75(13) . . ? S4 Mo2 S5 90.02(5) . . ? S6 Mo2 S5 89.86(5) 2_666 . ? S7 Mo2 S5 172.77(5) 2_666 . ? N10 Mo2 Mo1 133.57(14) . . ? S4 Mo2 Mo1 57.18(4) . . ? S6 Mo2 Mo1 117.75(4) 2_666 . ? S7 Mo2 Mo1 57.05(3) 2_666 . ? S5 Mo2 Mo1 117.26(4) . . ? N10 Mo2 Mo3 132.76(13) . . ? S4 Mo2 Mo3 57.31(4) . . ? S6 Mo2 Mo3 117.89(4) 2_666 . ? S7 Mo2 Mo3 116.90(4) 2_666 . ? S5 Mo2 Mo3 57.39(4) . . ? Mo1 Mo2 Mo3 59.911(19) . . ? N10 Mo2 Mo3 137.16(13) . 2_666 ? S4 Mo2 Mo3 117.49(4) . 2_666 ? S6 Mo2 Mo3 57.42(4) 2_666 2_666 ? S7 Mo2 Mo3 56.96(4) 2_666 2_666 ? S5 Mo2 Mo3 116.97(4) . 2_666 ? Mo1 Mo2 Mo3 60.353(18) . 2_666 ? Mo3 Mo2 Mo3 90.06(2) . 2_666 ? N10 Mo2 Mo1 136.25(14) . 2_666 ? S4 Mo2 Mo1 117.59(4) . 2_666 ? S6 Mo2 Mo1 57.60(4) 2_666 2_666 ? S7 Mo2 Mo1 116.53(4) 2_666 2_666 ? S5 Mo2 Mo1 57.39(4) . 2_666 ? Mo1 Mo2 Mo1 90.11(2) . 2_666 ? Mo3 Mo2 Mo1 60.316(19) . 2_666 ? Mo3 Mo2 Mo1 59.615(19) 2_666 2_666 ? N12 Mo3 S4 90.69(14) . . ? N12 Mo3 S7 96.22(14) . . ? S4 Mo3 S7 173.07(5) . . ? N12 Mo3 S6 91.85(14) . . ? S4 Mo3 S6 90.73(5) . . ? S7 Mo3 S6 89.60(5) . . ? N12 Mo3 S5 94.51(14) . . ? S4 Mo3 S5 90.08(5) . . ? S7 Mo3 S5 88.84(5) . . ? S6 Mo3 S5 173.58(5) . . ? N12 Mo3 Mo1 131.80(14) . . ? S4 Mo3 Mo1 57.13(4) . . ? S7 Mo3 Mo1 117.67(4) . . ? S6 Mo3 Mo1 57.75(3) . . ? S5 Mo3 Mo1 117.81(4) . . ? N12 Mo3 Mo2 133.91(13) . . ? S4 Mo3 Mo2 56.97(4) . . ? S7 Mo3 Mo2 116.99(4) . . ? S6 Mo3 Mo2 117.71(4) . . ? S5 Mo3 Mo2 57.82(4) . . ? Mo1 Mo3 Mo2 60.037(18) . . ? N12 Mo3 Mo2 136.01(13) . 2_666 ? S4 Mo3 Mo2 117.30(4) . 2_666 ? S7 Mo3 Mo2 57.47(4) . 2_666 ? S6 Mo3 Mo2 57.13(4) . 2_666 ? S5 Mo3 Mo2 117.03(4) . 2_666 ? Mo1 Mo3 Mo2 60.237(17) . 2_666 ? Mo2 Mo3 Mo2 89.94(2) . 2_666 ? N12 Mo3 Mo1 138.14(14) . 2_666 ? S4 Mo3 Mo1 117.01(4) . 2_666 ? S7 Mo3 Mo1 56.93(4) . 2_666 ? S6 Mo3 Mo1 116.73(4) . 2_666 ? S5 Mo3 Mo1 57.42(4) . 2_666 ? Mo1 Mo3 Mo1 90.04(2) . 2_666 ? Mo2 Mo3 Mo1 60.081(18) . 2_666 ? Mo2 Mo3 Mo1 59.621(19) 2_666 2_666 ? Mo2 S4 Mo1 65.78(4) . . ? Mo2 S4 Mo3 65.71(4) . . ? Mo1 S4 Mo3 65.55(4) . . ? Mo3 S5 Mo1 65.39(4) . 2_666 ? Mo3 S5 Mo2 64.79(4) . . ? Mo1 S5 Mo2 65.04(4) 2_666 . ? Mo2 S6 Mo3 65.45(4) 2_666 . ? Mo2 S6 Mo1 65.39(4) 2_666 . ? Mo3 S6 Mo1 64.81(4) . . ? Mo1 S7 Mo3 66.06(4) 2_666 . ? Mo1 S7 Mo2 65.30(4) 2_666 2_666 ? Mo3 S7 Mo2 65.57(4) . 2_666 ? C9 N8 Mo1 118.6(4) . . ? C11 N10 Mo2 117.9(4) . . ? C13 N12 Mo3 116.9(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N8 2.289(5) . ? Mo1 S4 2.4369(15) . ? Mo1 S7 2.4426(14) 2_666 ? Mo1 S6 2.4683(14) . ? Mo1 S5 2.4693(15) 2_666 ? Mo1 Mo3 2.6412(7) . ? Mo1 Mo2 2.6445(7) . ? Mo1 Mo2 2.6578(7) 2_666 ? Mo1 Mo3 2.6642(7) 2_666 ? Mo2 N10 2.293(5) . ? Mo2 S4 2.4329(16) . ? Mo2 S6 2.4521(15) 2_666 ? Mo2 S7 2.4590(15) 2_666 ? Mo2 S5 2.4743(15) . ? Mo2 Mo3 2.6449(7) . ? Mo2 Mo3 2.6555(7) 2_666 ? Mo2 Mo1 2.6578(7) 2_666 ? Mo3 N12 2.295(5) . ? Mo3 S4 2.4422(15) . ? Mo3 S7 2.4450(15) . ? Mo3 S6 2.4600(14) . ? Mo3 S5 2.4627(15) . ? Mo3 Mo2 2.6554(7) 2_666 ? Mo3 Mo1 2.6641(7) 2_666 ? S5 Mo1 2.4692(15) 2_666 ? S6 Mo2 2.4521(15) 2_666 ? S7 Mo1 2.4426(14) 2_666 ? S7 Mo2 2.4591(15) 2_666 ? N8 C9 1.477(8) . ? N10 C11 1.468(8) . ? N12 C13 1.468(8) . ?