#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003313.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_2003313 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 575 _journal_page_last 578 _publ_section_title ; Bis(triethylammonium) Bis(2-mercaptobenzoato-O,S)dioxomolybdate(VI) ; _chemical_formula_moiety '2C6 H16 N 1+ Mo O2 , 2C7 H4 O2 S1 2-' _chemical_formula_sum 'C26 H40 Mo N2 O6 S2' _chemical_formula_weight 636.66 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 11.832(3) _cell_length_b 14.050(3) _cell_length_c 18.049(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3000.5(11) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 12.5 _exptl_absorpt_coefficient_mu 0.616 _cell_measurement_temperature 293(2) _exptl_crystal_description Prismatic _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour Orange _chemical_compound_source ? _diffrn_measurement_device 'Siemens R3m difractometer' _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.072 _exptl_absorpt_correction_T_max 0.094 _diffrn_reflns_number 2680 _reflns_number_total 2680 _reflns_number_observed 2273 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_theta_max 24.04 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0330 _refine_ls_wR_factor_obs 0.0800 _refine_ls_wR_factor_all 0.0879 _refine_ls_goodness_of_fit_obs 1.045 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_number_reflns 2680 _refine_ls_number_parameters 335 _refine_ls_hydrogen_treatment 'H atoms refined as a riding model' _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0505P)^2^+1.2564P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.035 _refine_diff_density_max 0.325 _refine_diff_density_min -0.356 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag "C" "C" "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" 0.0033 0.001 "H" "H" "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" 0.0000 0.000 "N" "N" "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" 0.0061 0.003 "O" "O" "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" 0.0106 0.006 "S" "S" "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" 0.1246 0.123 "Mo" "Mo" "International Tables Vol C Tables 4.2.6.8 and 6.1.1.4" -1.6832 0. _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881 _refine_ls_abs_structure_Flack 0.27(7) ; P3/P4-PC Diffractometer Program (Siemens, 1991) ; ; P3/P4-PC Diffractometer Program (Siemens, 1991) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Mo1 1 0.24870(5) 0.47995(3) 0.14600(3) 0.0451(2) S1 1 0.18931(15) 0.56099(12) 0.25962(9) 0.0570(4) S2 1 0.33665(14) 0.41886(12) 0.03158(9) 0.0547(4) N1 1 0.3612(4) 0.7306(4) -0.0637(3) 0.0602(14) H1A 1 0.3363 0.7422 -0.0175 0.080 N2 1 0.5575(4) 0.6267(3) 0.3109(3) 0.0530(13) H2A 1 0.5714 0.6066 0.2645 0.080 O1 1 0.1253(4) 0.4709(4) 0.0982(3) 0.0681(13) O2 1 0.2492(5) 0.3821(3) 0.2013(2) 0.0659(11) O3 1 0.2688(4) 0.6233(3) 0.1082(2) 0.0608(12) O4 1 0.2966(4) 0.7722(3) 0.0794(2) 0.0654(13) O5 1 0.4225(3) 0.5093(3) 0.1729(2) 0.0561(11) O6 1 0.6024(4) 0.5483(3) 0.1780(2) 0.0652(13) C1 1 0.2574(6) 0.7099(4) 0.1220(3) 0.0471(13) C2 1 0.1917(5) 0.7417(4) 0.1886(3) 0.0454(14) C3 1 0.1619(6) 0.8383(4) 0.1909(4) 0.059(2) H3A 1 0.1892 0.8807 0.1533 0.080 C4 1 0.0925(7) 0.8739(6) 0.2467(5) 0.076(2) H4A 1 0.0732 0.9403 0.2479 0.080 C5 1 0.0524(7) 0.8136(6) 0.3005(5) 0.076(2) H5A 1 0.0022 0.8371 0.3381 0.080 C6 1 0.0840(6) 0.7196(5) 0.3002(4) 0.062(2) H6A 1 0.0571 0.6785 0.3388 0.080 C7 1 0.1541(5) 0.6821(4) 0.2453(3) 0.0477(14) C8 1 0.5239(5) 0.4998(4) 0.1511(3) 0.0469(15) C9 1 0.5542(5) 0.4249(4) 0.0959(3) 0.0412(13) C10 1 0.6654(5) 0.3918(5) 0.0967(3) 0.052(2) H10A 1 0.7175 0.4179 0.1321 0.080 C11 1 0.7024(6) 0.3227(5) 0.0484(4) 0.066(2) H11A 1 0.7798 0.3022 0.0493 0.080 C12 1 0.6274(6) 0.2834(5) -0.0007(4) 0.061(2) H12A 1 0.6521 0.2337 -0.0334 0.080 C13 1 0.5159(6) 0.3150(5) -0.0036(3) 0.056(2) H13A 1 0.4645 0.2882 -0.0391 0.080 C14 1 0.4787(5) 0.3858(4) 0.0454(3) 0.0416(13) C15 1 0.2616(6) 0.7148(6) -0.1116(4) 0.098(3) H15A 1 0.2886 0.7003 -0.1605 0.080 H15B 1 0.2189 0.7728 -0.1147 0.080 C16 1 0.1850(8) 0.6356(6) -0.0865(5) 0.102(3) H16A 1 0.1236 0.6295 -0.1209 0.080 H16B 1 0.2263 0.5769 -0.0846 0.080 H16C 1 0.1558 0.6502 -0.0382 0.080 C17 1 0.4311(7) 0.6434(5) -0.0623(5) 0.107(3) H17A 1 0.4622 0.6337 -0.1109 0.080 H17B 1 0.3837 0.5899 -0.0511 0.080 C18 1 0.5264(7) 0.6474(7) -0.0065(5) 0.111(4) H18A 1 0.5685 0.5891 -0.0086 0.080 H18B 1 0.5754 0.6998 -0.0180 0.080 H18C 1 0.4960 0.6555 0.0424 0.080 C19 1 0.4286(6) 0.8127(4) -0.0886(5) 0.095(3) H19A 1 0.4535 0.8013 -0.1385 0.080 H19B 1 0.4945 0.8182 -0.0579 0.080 C20 1 0.3646(4) 0.9049(4) -0.0851(4) 0.114(3) H20A 1 0.4123 0.9558 -0.1020 0.080 H20B 1 0.2995 0.9003 -0.1166 0.080 H20C 1 0.3409 0.9174 -0.0352 0.080 C21 1 0.6640(4) 0.6698(4) 0.3372(4) 0.068(2) H21A 1 0.6548 0.6856 0.3886 0.080 H21B 1 0.6767 0.7280 0.3107 0.080 C22 1 0.7666(6) 0.6071(7) 0.3289(6) 0.118(4) H22A 1 0.8314 0.6403 0.3477 0.080 H22B 1 0.7560 0.5493 0.3564 0.080 H22C 1 0.7781 0.5923 0.2775 0.080 C23 1 0.4658(5) 0.6980(4) 0.3043(4) 0.063(2) H23A 1 0.4589 0.7308 0.3507 0.080 H23B 1 0.3958 0.6655 0.2951 0.080 C24 1 0.4856(7) 0.7693(5) 0.2434(4) 0.077(2) H24A 1 0.4238 0.8135 0.2421 0.080 H24B 1 0.5547 0.8030 0.2529 0.080 H24C 1 0.4909 0.7371 0.1966 0.080 C25 1 0.5214(8) 0.5407(4) 0.3525(3) 0.084(2) H25A 1 0.5791 0.4929 0.3490 0.080 H25B 1 0.4545 0.5155 0.3296 0.080 C26 1 0.4948(11) 0.5587(7) 0.4329(4) 0.124(4) H26A 1 0.4715 0.5004 0.4560 0.080 H26B 1 0.5617 0.5821 0.4569 0.080 H26C 1 0.4355 0.6050 0.4372 0.080 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Mo1 0.0382(2) 0.0000(3) 0.0006(3) 0.0418(2) -0.0004(2) 0.0555(3) S1 0.0608(10) 0.0055(8) 0.0175(8) 0.0570(9) 0.0060(8) 0.0533(9) S2 0.0487(8) 0.0017(8) -0.0105(7) 0.0617(10) -0.0145(8) 0.0537(9) N1 0.054(3) 0.000(3) 0.010(3) 0.072(4) 0.016(3) 0.054(3) N2 0.067(3) -0.011(3) 0.000(3) 0.046(3) -0.008(2) 0.046(3) O1 0.045(2) 0.003(2) -0.012(2) 0.081(3) 0.000(3) 0.079(3) O2 0.071(3) 0.005(3) 0.001(3) 0.047(2) 0.009(2) 0.079(3) O3 0.082(4) 0.009(2) 0.022(3) 0.042(2) 0.003(2) 0.058(2) O4 0.085(3) -0.001(2) 0.012(2) 0.053(3) 0.008(2) 0.058(2) O5 0.043(2) 0.001(2) 0.000(2) 0.070(3) -0.026(2) 0.056(2) O6 0.046(2) -0.011(2) 0.000(2) 0.082(3) -0.031(3) 0.067(3) C1 0.043(3) 0.002(4) -0.005(3) 0.047(3) 0.003(3) 0.051(3) C2 0.040(3) 0.004(3) -0.011(3) 0.048(3) -0.008(3) 0.048(3) C3 0.067(4) 0.003(3) -0.013(4) 0.049(4) -0.010(3) 0.062(4) C4 0.075(5) 0.029(4) -0.022(5) 0.063(5) -0.031(5) 0.091(6) C5 0.068(5) 0.014(4) 0.009(4) 0.090(6) -0.029(5) 0.070(5) C6 0.055(4) 0.007(4) 0.013(4) 0.072(5) -0.010(4) 0.060(4) C7 0.040(3) 0.004(3) -0.005(3) 0.053(4) -0.006(3) 0.050(3) C8 0.040(3) -0.002(3) 0.001(3) 0.056(4) -0.002(3) 0.045(3) C9 0.042(3) 0.000(3) 0.003(2) 0.046(3) 0.000(3) 0.036(3) C10 0.045(3) 0.008(3) 0.004(3) 0.064(4) 0.000(3) 0.047(3) C11 0.048(3) 0.012(3) 0.012(4) 0.075(5) -0.001(4) 0.075(4) C12 0.072(5) 0.014(4) 0.023(4) 0.057(4) -0.008(3) 0.055(4) C13 0.070(5) -0.005(4) 0.005(3) 0.061(4) -0.012(3) 0.038(3) C14 0.046(3) -0.001(3) 0.003(3) 0.044(3) 0.001(3) 0.035(3) C15 0.101(7) -0.036(7) 0.000(6) 0.114(7) 0.002(5) 0.080(5) C16 0.103(7) -0.026(6) -0.028(6) 0.105(7) 0.005(6) 0.097(6) C17 0.111(8) 0.013(6) 0.051(7) 0.097(7) 0.017(6) 0.114(7) C18 0.072(6) 0.012(6) 0.013(6) 0.139(9) 0.073(7) 0.123(8) C19 0.086(6) -0.014(6) 0.006(5) 0.103(7) 0.024(6) 0.096(6) C20 0.091(7) -0.014(6) -0.022(7) 0.088(6) 0.015(7) 0.162(10) C21 0.065(4) -0.014(4) -0.015(4) 0.059(4) -0.013(4) 0.080(5) C22 0.080(6) 0.012(6) -0.034(6) 0.133(8) -0.057(7) 0.141(8) C23 0.064(4) -0.006(4) 0.001(4) 0.065(4) -0.012(4) 0.060(4) C24 0.081(5) 0.001(4) -0.022(4) 0.077(5) -0.003(4) 0.073(5) C25 0.119(7) -0.023(5) -0.001(5) 0.065(5) 0.005(4) 0.067(4) C26 0.190(12) -0.033(8) 0.022(7) 0.097(7) 0.013(6) 0.083(6)