#------------------------------------------------------------------------------ #$Date: 2011-04-30 08:20:42 +0300 (Sat, 30 Apr 2011) $ #$Revision: 18458 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2000024.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_2000024 _publ_contact_author ; Prof. Francis J. DiSalvo Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853 ; _publ_contact_author_email fjd3@cornell.edu _publ_contact_author_fax '607-255-4137' _publ_contact_author_phone '607-255-7238' loop_ _publ_author_name 'Song Jin' 'D. Venkataraman' 'Francis J. DiSalvo' _publ_author_address ; Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853 ; _publ_section_title ; Ligand Substitution Reactions of W6S8L6 with Tricyclohexylphosphine (L = 4-tert-Butylpyridine or n-Butylamine): 31P NMR and Structural Studies of W6S8(PCy3)n(4-tert-butylpyridine)6-n (0 < n <= 6) Complexes ; _journal_name_full 'Inorganic Chemistry' _journal_volume 39 _journal_page_first 2747 _journal_page_last 2757 _journal_year 2000 _chemical_formula_sum 'C24 H66 N6 S8 W6' _space_group_IT_number 12 _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _[local]_cod_cif_authors_sg_H-M 'C 2/m' _cell_volume 2471.769 _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.416 _exptl_crystal_description 'blocks' _exptl_crystal_preparation 'acetonitrile' _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_gt 0.0768 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2+y,z 3 x,-y,z 4 1/2+x,1/2-y,z 5 -x,-y,-z 6 -1/2-x,-1/2-y,-z 7 -x,y,-z 8 -1/2-x,-1/2+y,-z _cell_length_a 10.0667(11) _cell_length_b 17.699(2) _cell_length_c 14.374(2) _cell_angle_alpha 90 _cell_angle_beta 105.171(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 S 1.02 W 1.37 _cod_database_code 2000024 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 14.264 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4047 _exptl_absorpt_correction_T_max 0.9279 _exptl_absorpt_process_details ; SADABS ; _exptl_special_details ; sealed in a capillary with mother liquid ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD Diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 5274 _diffrn_reflns_av_R_equivalents 0.1166 _diffrn_reflns_av_sigmaI/netI 0.1367 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 23.28 _reflns_number_total 1831 _reflns_number_observed 998 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1831 _refine_ls_number_parameters 72 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_obs 0.0768 _refine_ls_wR_factor_all 0.2482 _refine_ls_wR_factor_obs 0.2022 _refine_ls_goodness_of_fit_all 1.092 _refine_ls_goodness_of_fit_obs 1.211 _refine_ls_restrained_S_all 1.089 _refine_ls_restrained_S_obs 1.206 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W -0.8170(2) 0.5000 0.57673(15) 0.0405(7) Uani 1 d S . W2 W -0.95535(14) 0.42511(8) 0.42114(10) 0.0419(6) Uani 1 d . . S1 S -0.7478(12) 0.5000 0.4248(10) 0.046(3) Uani 1 d S . S2 S -0.9112(15) 0.5000 0.7173(10) 0.060(4) Uani 1 d S . S3 S -1.1667(9) 0.3613(6) 0.4316(7) 0.057(3) Uani 1 d . . N1 N -0.5979(50) 0.5000 0.6605(34) 0.087(16) Uiso 1 d SD . H1A H -0.5579(50) 0.4592 0.6421(34) 0.104 Uiso 0.50 calc PR . H1B H -0.5579(50) 0.5408 0.6421(34) 0.104 Uiso 0.50 calc PR . N2 N -0.9094(36) 0.3348(22) 0.3201(25) 0.090(11) Uiso 1 d D . H2A H -0.8722(36) 0.2960(22) 0.3587(25) 0.108 Uiso 1 calc R . H2B H -0.9924(36) 0.3186(22) 0.2855(25) 0.108 Uiso 1 calc R . C1 C -0.5615(62) 0.5000 0.7687(35) 0.116(26) Uiso 1 d SD . H1B H -0.6012(62) 0.4557 0.7907(35) 0.140 Uiso 0.50 calc PR . H1C H -0.6012(62) 0.5443 0.7907(35) 0.140 Uiso 0.50 calc PR . C2 C -0.4062(61) 0.5000 0.8129(47) 0.111(25) Uiso 1 d SD . H2B H -0.3707(61) 0.4561 0.7868(47) 0.133 Uiso 0.50 calc PR . H2C H -0.3707(61) 0.5439 0.7868(47) 0.133 Uiso 0.50 calc PR . C3 C -0.3386(81) 0.5000 0.9199(48) 0.130(30) Uiso 1 d SD . H3A H -0.3764(81) 0.4563 0.9446(48) 0.156 Uiso 0.50 calc PR . H3B H -0.3764(81) 0.5437 0.9446(48) 0.156 Uiso 0.50 calc PR . C4 C -0.1875(85) 0.5000 0.9725(80) 0.263(66) Uiso 1 d SD . H4A H -0.1775(85) 0.5000 1.0407(80) 0.394 Uiso 1 calc SR . H4B H -0.1445(85) 0.5443 0.9550(80) 0.394 Uiso 0.50 calc PR . H4C H -0.1445(85) 0.4557 0.9550(80) 0.394 Uiso 0.50 calc PR . C5 C -0.8238(75) 0.3414(51) 0.2485(48) 0.255(43) Uiso 1 d D . H5A H -0.7298(75) 0.3455(51) 0.2879(48) 0.306 Uiso 1 calc R . H5B H -0.8467(75) 0.3907(51) 0.2193(48) 0.306 Uiso 1 calc R . C6 C -0.8146(67) 0.2905(39) 0.1656(50) 0.169(28) Uiso 1 d D . H6A H -0.8323(67) 0.3203(39) 0.1070(50) 0.203 Uiso 1 calc R . H6B H -0.7216(67) 0.2708(39) 0.1780(50) 0.203 Uiso 1 calc R . C7 C -0.9144(68) 0.2247(40) 0.1497(59) 0.216(38) Uiso 1 d D . H7A H -1.0062(68) 0.2389(40) 0.1129(59) 0.259 Uiso 1 calc R . H7B H -0.9183(68) 0.2006(40) 0.2095(59) 0.259 Uiso 1 calc R . C8 C -0.8390(52) 0.1768(36) 0.0912(38) 0.146(23) Uiso 1 d D . H8A H -0.8878(52) 0.1302(36) 0.0732(38) 0.219 Uiso 1 calc R . H8B H -0.7475(52) 0.1662(36) 0.1295(38) 0.219 Uiso 1 calc R . H8C H -0.8344(52) 0.2038(36) 0.0343(38) 0.219 Uiso 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 W1 0.0293(12) 0.0473(14) 0.0444(14) 0.000 0.0085(10) 0.000 W2 0.0349(9) 0.0435(10) 0.0486(10) -0.0051(8) 0.0131(7) -0.0004(7) S1 0.037(7) 0.048(8) 0.057(9) 0.000 0.019(7) 0.000 S2 0.060(9) 0.070(10) 0.051(9) 0.000 0.015(8) 0.000 S3 0.052(6) 0.054(7) 0.067(7) -0.018(5) 0.018(6) -0.019(5) 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 W1 N1 2.22(5) . ? W1 S2 2.446(14) . ? W1 S1 2.459(13) . ? W1 S3 2.461(10) 2_356 ? W1 S3 2.461(10) 5_366 ? W1 W2 2.655(2) 2_356 ? W1 W2 2.655(2) 5_366 ? W1 W2 2.659(2) . ? W1 W2 2.659(2) 6_565 ? W2 N2 2.29(4) . ? W2 S3 2.430(10) 2_356 ? W2 S3 2.447(9) . ? W2 S1 2.463(10) . ? W2 S2 2.474(12) 5_366 ? W2 W2 2.648(3) 2_356 ? W2 W2 2.651(3) 6_565 ? W2 W1 2.655(2) 5_366 ? S1 W2 2.463(10) 6_565 ? S2 W2 2.474(12) 2_356 ? S2 W2 2.474(12) 5_366 ? S3 W2 2.430(10) 2_356 ? S3 W1 2.461(10) 5_366 ? N1 C1 1.50(2) . ? N2 C5 1.51(2) . ? C1 C2 1.53(3) . ? C2 C3 1.51(3) . ? C3 C4 1.51(3) . ? C5 C6 1.52(3) . ? C6 C7 1.51(3) . ? C7 C8 1.53(3) . ? 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 N1 W1 S2 95.6(13) . . ? N1 W1 S1 90.5(13) . . ? S2 W1 S1 173.9(4) . . ? N1 W1 S3 94.1(2) . 2_356 ? S2 W1 S3 90.3(2) . 2_356 ? S1 W1 S3 89.3(2) . 2_356 ? N1 W1 S3 94.1(2) . 5_366 ? S2 W1 S3 90.3(2) . 5_366 ? S1 W1 S3 89.3(2) . 5_366 ? S3 W1 S3 171.8(5) 2_356 5_366 ? N1 W1 W2 137.1(8) . 2_356 ? S2 W1 W2 57.9(3) . 2_356 ? S1 W1 W2 117.1(3) . 2_356 ? S3 W1 W2 57.0(2) 2_356 2_356 ? S3 W1 W2 116.8(2) 5_366 2_356 ? N1 W1 W2 137.1(8) . 5_366 ? S2 W1 W2 57.9(3) . 5_366 ? S1 W1 W2 117.1(3) . 5_366 ? S3 W1 W2 116.8(2) 2_356 5_366 ? S3 W1 W2 57.0(2) 5_366 5_366 ? W2 W1 W2 59.91(7) 2_356 5_366 ? N1 W1 W2 133.2(9) . . ? S2 W1 W2 117.6(3) . . ? S1 W1 W2 57.4(2) . . ? S3 W1 W2 56.5(2) 2_356 . ? S3 W1 W2 116.3(2) 5_366 . ? W2 W1 W2 59.80(7) 2_356 . ? W2 W1 W2 89.70(7) 5_366 . ? N1 W1 W2 133.2(9) . 6_565 ? S2 W1 W2 117.6(3) . 6_565 ? S1 W1 W2 57.4(2) . 6_565 ? S3 W1 W2 116.3(2) 2_356 6_565 ? S3 W1 W2 56.5(2) 5_366 6_565 ? W2 W1 W2 89.70(7) 2_356 6_565 ? W2 W1 W2 59.80(7) 5_366 6_565 ? W2 W1 W2 59.81(7) . 6_565 ? N2 W2 S3 95.1(9) . 2_356 ? N2 W2 S3 92.3(10) . . ? S3 W2 S3 88.9(4) 2_356 . ? N2 W2 S1 94.5(9) . . ? S3 W2 S1 89.9(4) 2_356 . ? S3 W2 S1 173.2(3) . . ? N2 W2 S2 91.2(9) . 5_366 ? S3 W2 S2 173.6(3) 2_356 5_366 ? S3 W2 S2 89.9(4) . 5_366 ? S1 W2 S2 90.5(4) . 5_366 ? N2 W2 W2 135.6(9) . 2_356 ? S3 W2 W2 57.4(2) 2_356 2_356 ? S3 W2 W2 56.8(2) . 2_356 ? S1 W2 W2 117.2(3) . 2_356 ? S2 W2 W2 117.0(3) 5_366 2_356 ? N2 W2 W2 134.3(9) . 6_565 ? S3 W2 W2 117.7(3) 2_356 6_565 ? S3 W2 W2 117.5(2) . 6_565 ? S1 W2 W2 57.44(15) . 6_565 ? S2 W2 W2 57.6(2) 5_366 6_565 ? W2 W2 W2 90.0 2_356 6_565 ? N2 W2 W1 132.5(9) . 5_366 ? S3 W2 W1 117.6(2) 2_356 5_366 ? S3 W2 W1 57.5(2) . 5_366 ? S1 W2 W1 117.5(2) . 5_366 ? S2 W2 W1 56.8(3) 5_366 5_366 ? W2 W2 W1 60.18(6) 2_356 5_366 ? W2 W2 W1 60.04(4) 6_565 5_366 ? N2 W2 W1 137.2(9) . . ? S3 W2 W1 57.6(3) 2_356 . ? S3 W2 W1 116.8(2) . . ? S1 W2 W1 57.2(3) . . ? S2 W2 W1 117.6(2) 5_366 . ? W2 W2 W1 60.03(6) 2_356 . ? W2 W2 W1 60.09(4) 6_565 . ? W1 W2 W1 90.30(7) 5_366 . ? W1 S1 W2 65.4(3) . . ? W1 S1 W2 65.4(3) . 6_565 ? W2 S1 W2 65.1(3) . 6_565 ? W1 S2 W2 65.3(3) . 2_356 ? W1 S2 W2 65.3(3) . 5_366 ? W2 S2 W2 64.8(4) 2_356 5_366 ? W2 S3 W2 65.8(2) 2_356 . ? W2 S3 W1 65.8(2) 2_356 5_366 ? W2 S3 W1 65.5(2) . 5_366 ? C1 N1 W1 120.0(37) . . ? C5 N2 W2 128.7(40) . . ? N1 C1 C2 112.1(50) . . ? C3 C2 C1 124.3(61) . . ? C2 C3 C4 129.5(80) . . ? N2 C5 C6 130.8(61) . . ? C7 C6 C5 113.6(59) . . ? C6 C7 C8 96.0(48) . . ? _refine_diff_density_max 2.541 _refine_diff_density_min -2.826 _refine_diff_density_rms 0.604