#------------------------------------------------------------------------------ #$Date: 2015-01-07 16:25:02 +0000 (Wed, 07 Jan 2015) $ #$Revision: 129439 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/00/4000006.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_4000006 _journal_name_full 'Chemistry of Materials' _journal_year 2000 _chemical_name_systematic ; Bis[3-methylamido-3',4'-ethylenedithiotetrathiafulvalene] chloride, water solvate ; _chemical_name_common '[EDT-TTF-CONHMe]2Cl.H2O' _chemical_melting_point ? _chemical_formula_moiety '[C10H9NOS6]2, Cl, H2O' _chemical_formula_sum 'C10 H9 Cl0.5 N O1.5 S6' _[local]_cod_chemical_formula_sum_orig 'C10 H9 Cl0.50 N O1.50 S6' _chemical_formula_weight 377.27 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.5376(10) _cell_length_b 11.4249(10) _cell_length_c 14.7464(10) _cell_angle_alpha 75.604(10) _cell_angle_beta 83.876(10) _cell_angle_gamma 83.047(10) _cell_volume 732.69(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2627 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.07 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method . _exptl_crystal_F_000 385 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8728 _exptl_absorpt_correction_T_max 0.9710 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _diffrn_ambient_temperature 293(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_type 'Stoe IPDS' _diffrn_measurement_method 'Oscillation, phi incr. 1.6' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7142 _diffrn_reflns_av_R_equivalents 0.1022 _diffrn_reflns_av_sigmaI/netI 0.1526 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.83 _reflns_number_total 2641 _reflns_number_gt 1249 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 2641 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 0.772 _refine_ls_restrained_S_all 0.772 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.003 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 S1 S 0.6350(3) 0.33469(11) 0.32785(9) 0.0340(4) Uani 1 1 d . . . S2 S 0.3736(3) 0.10604(10) 0.34944(9) 0.0378(4) Uani 1 1 d . . . S3 S 0.2705(3) 0.36665(10) 0.52458(9) 0.0357(4) Uani 1 1 d . . . S4 S 0.0357(3) 0.13312(10) 0.54650(9) 0.0354(4) Uani 1 1 d . . . S5 S -0.0393(3) 0.42209(10) 0.69368(9) 0.0410(4) Uani 1 1 d . . . S6 S -0.3074(4) 0.13853(12) 0.72857(9) 0.0446(4) Uani 1 1 d . . . C1 C 1.2091(13) 0.3165(5) 0.0116(3) 0.0536(17) Uani 1 1 d . . . H1A H 1.1060 0.3842 -0.0293 0.080 Uiso 1 1 calc R . . H1B H 1.2816 0.2558 -0.0223 0.080 Uiso 1 1 calc R . . H1C H 1.3738 0.3434 0.0341 0.080 Uiso 1 1 calc R . . C2 C 0.9302(12) 0.3184(4) 0.1612(3) 0.0321(14) Uani 1 1 d . . . C3 C 0.7246(11) 0.2564(4) 0.2393(3) 0.0286(13) Uani 1 1 d . . . C4 C 0.6053(11) 0.1525(4) 0.2500(3) 0.0340(14) Uani 1 1 d . . . H4 H 0.6459 0.1067 0.2052 0.041 Uiso 1 1 calc R . . C5 C 0.4005(11) 0.2303(4) 0.3964(3) 0.0299(13) Uani 1 1 d . . . C6 C 0.2557(10) 0.2429(4) 0.4778(3) 0.0298(13) Uani 1 1 d . . . C7 C 0.0250(11) 0.3202(4) 0.6226(3) 0.0259(12) Uani 1 1 d . . . C8 C -0.0786(11) 0.2118(4) 0.6332(3) 0.0273(13) Uani 1 1 d . . . C9 C -0.2711(13) 0.3457(4) 0.7917(3) 0.0496(17) Uani 1 1 d . . . H9A H -0.2421 0.3747 0.8463 0.059 Uiso 1 1 calc R . . H9B H -0.4778 0.3678 0.7782 0.059 Uiso 1 1 calc R . . C10 C -0.2142(13) 0.2105(4) 0.8156(3) 0.0475(16) Uani 1 1 d . . . H10A H -0.3275 0.1786 0.8743 0.057 Uiso 1 1 calc R . . H10B H -0.0049 0.1886 0.8256 0.057 Uiso 1 1 calc R . . N1 N 1.0074(10) 0.2656(3) 0.0903(3) 0.0422(12) Uani 1 1 d . . . H1 H 0.9352 0.1991 0.0913 0.051 Uiso 1 1 calc R . . O1 O 1.0240(8) 0.4120(3) 0.1660(2) 0.0525(11) Uani 1 1 d . . . Cl1 Cl 0.7106(5) 0.02724(16) 0.05938(13) 0.0683(11) Uani 0.603(10) 1 d P . . O2 O 0.7106(5) 0.02724(16) 0.05938(13) 0.0683(11) Uani 0.397(10) 1 d P . . 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 S1 0.0419(11) 0.0267(6) 0.0340(8) -0.0104(6) 0.0112(7) -0.0116(6) S2 0.0500(12) 0.0270(6) 0.0382(8) -0.0128(6) 0.0099(8) -0.0131(7) S3 0.0497(12) 0.0260(6) 0.0327(8) -0.0100(6) 0.0117(8) -0.0157(7) S4 0.0499(11) 0.0250(6) 0.0324(8) -0.0099(6) 0.0105(7) -0.0144(7) S5 0.0607(12) 0.0274(6) 0.0362(8) -0.0130(6) 0.0124(8) -0.0120(7) S6 0.0612(12) 0.0367(7) 0.0369(8) -0.0114(6) 0.0187(8) -0.0239(7) C1 0.059(5) 0.056(3) 0.040(3) -0.011(3) 0.016(3) -0.002(3) C2 0.031(4) 0.036(3) 0.030(3) -0.010(2) 0.005(3) -0.004(3) C3 0.034(4) 0.027(2) 0.026(3) -0.009(2) -0.003(3) -0.003(2) C4 0.043(4) 0.029(3) 0.034(3) -0.018(2) -0.001(3) 0.000(2) C5 0.036(4) 0.024(2) 0.029(3) -0.003(2) -0.001(3) -0.010(2) C6 0.028(4) 0.030(3) 0.030(3) -0.003(2) 0.002(3) -0.005(2) C7 0.028(4) 0.027(2) 0.021(3) -0.003(2) -0.002(2) -0.002(2) C8 0.025(4) 0.028(2) 0.025(3) -0.003(2) 0.009(2) -0.005(2) C9 0.065(5) 0.045(3) 0.038(3) -0.014(3) 0.022(3) -0.015(3) C10 0.069(5) 0.048(3) 0.023(3) -0.003(2) 0.005(3) -0.016(3) N1 0.058(4) 0.037(2) 0.033(2) -0.0128(19) 0.012(2) -0.012(2) O1 0.069(3) 0.046(2) 0.046(2) -0.0145(18) 0.020(2) -0.029(2) Cl1 0.079(2) 0.0614(14) 0.0572(16) -0.0089(10) 0.0108(12) -0.0013(11) O2 0.079(2) 0.0614(14) 0.0572(16) -0.0089(10) 0.0108(12) -0.0013(11) _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.290 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.068 _cod_database_code 4000006