#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000350.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_5000350 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C18 H35 Cl4 N3 O Ru S' _[local]_cod_chemical_formula_sum_orig 'C18 H35 Cl4 N3 O1 Ru1 S1' _chemical_formula_moiety 'C17 H33 Cl2 N3 O1 Ru1 S1 , C1 H2 Cl2' _chemical_formula_weight 584.442 _cell_length_a 13.353(2) _cell_length_b 11.228(1) _cell_length_c 17.536(2) _cell_angle_alpha 90 _cell_angle_beta 109.30(1) _cell_angle_gamma 90 _cell_volume 2481.3(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 65 _cell_measurement_theta_min 9.52 _cell_measurement_theta_max 10.55 _cell_measurement_temperature 110 _exptl_crystal_colour orange _exptl_crystal_description 'triangular prism' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.1614 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.81 _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_crystal_treatment ; The single crystal used for the data collection was obtained by cleaving a very large crystal. The crystal shattered upon cleaving, leaving pieces with uneven surfaces. The one selected for investigation was an irregular triangular prism. _diffrn_radiation_type ; _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 110 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11184 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_min 3.05495 _diffrn_reflns_theta_max 27.5831 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 4 _diffrn_standards_decay_% -1.5 _diffrn_standards_interval_count 300 _reflns_number_total 5738 _reflns_number_gt 4782 _reflns_threshold_expression F^2^>2.0\s(F^2^) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.42 0.836 'International Tables Vol. IV (1974) Table 2.2B' Cl Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' S S 0.11 0.124 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 4782 _refine_ls_number_parameters 254 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.00000012(5) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.05F)^2^ _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_ref 0.0319 _refine_ls_goodness_of_fit_ref 1.0201 _refine_ls_shift/su_max 0.0063 _refine_diff_density_max 0.32 _refine_diff_density_min -0.2 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_disorder_group _atom_site_disorder_assembly Ru1 Ru 0.219778(14) 0.106588(16) 0.406701(11) 0.01247(7) Uani 1 0 . Cl2 Cl 0.37969(4) 0.21465(5) 0.48643(3) 0.01833(18) Uani 1 0 . Cl3 Cl 0.17438(5) 0.26012(5) 0.30088(3) 0.01745(18) Uani 1 0 . S4 S 0.07398(5) 0.00393(5) 0.34613(4) 0.01513(18) Uani 1 0 . O5 O -0.00132(14) -0.00272(16) 0.39313(11) 0.0221(6) Uani 1 0 . C6 C -0.0065(2) 0.0498(2) 0.24747(16) 0.0229(8) Uani 1 0 . C7 C 0.0892(2) -0.1496(2) 0.32318(15) 0.0196(8) Uani 1 0 . N8 N 0.34225(16) 0.00651(18) 0.37288(12) 0.0173(7) Uani 1 0 . C9 C 0.3487(2) -0.1143(2) 0.40938(15) 0.0193(8) Uani 1 0 . C10 C 0.31936(19) -0.1110(2) 0.48526(15) 0.0190(8) Uani 1 0 . C11 C 0.3453(2) -0.1994(2) 0.54348(16) 0.0237(8) Uani 1 0 . C12 C 0.3141(2) -0.1865(3) 0.61083(17) 0.0261(9) Uani 1 0 . C13 C 0.2628(2) -0.0829(2) 0.62126(16) 0.0235(8) Uani 1 0 . C14 C 0.24071(19) 0.0035(2) 0.56204(15) 0.0184(8) Uani 1 0 . N15 N 0.26430(15) -0.01436(18) 0.49406(12) 0.0154(6) Uani 1 0 . C16 C 0.1963(2) 0.1250(2) 0.56848(15) 0.0211(8) Uani 1 0 . N17 N 0.13439(16) 0.17055(19) 0.48646(12) 0.0182(7) Uani 1 0 . C18 C 0.3678(2) 0.0062(2) 0.29427(15) 0.0191(8) Uani 1 0 . C19 C 0.4610(2) -0.0770(3) 0.30059(17) 0.0270(9) Uani 1 0 . C20 C 0.3992(2) 0.1339(3) 0.28131(17) 0.0256(9) Uani 1 0 . C21 C 0.2704(2) -0.0300(3) 0.22471(15) 0.0236(9) Uani 1 0 . C22 C 0.0902(2) 0.2954(2) 0.48789(15) 0.0198(8) Uani 1 0 . C23 C 0.0458(2) 0.3073(3) 0.55785(17) 0.0273(9) Uani 1 0 . C24 C -0.0015(2) 0.3094(2) 0.40864(16) 0.0233(9) Uani 1 0 . C25 C 0.1753(2) 0.3886(2) 0.49461(17) 0.0251(9) Uani 1 0 . C26 C 0.3819(2) 0.4636(3) 0.36687(19) 0.0319(10) Uani 1 0 . Cl27 Cl 0.51491(6) 0.51373(8) 0.40187(4) 0.0392(3) Uani 1 0 . Cl28 Cl 0.29171(7) 0.58297(7) 0.35152(5) 0.0431(3) Uani 1 0 . H1 H -0.0224 0.1323 0.2482 0.0356 Uiso 1 0 . H2 H 0.0306 0.0365 0.2104 0.0356 Uiso 1 0 . H3 H -0.0706 0.0054 0.2312 0.0356 Uiso 1 0 . H4 H 0.0215 -0.1865 0.304 0.0322 Uiso 1 0 . H5 H 0.1222 -0.1541 0.2829 0.0322 Uiso 1 0 . H6 H 0.1321 -0.1892 0.3706 0.0322 Uiso 1 0 . H7 H 0.405 0.0417 0.4085 0.0297 Uiso 1 0 . H8 H 0.3014 -0.1661 0.3715 0.0316 Uiso 1 0 . H9 H 0.4192 -0.1433 0.4223 0.0316 Uiso 1 0 . H10 H 0.3838 -0.2678 0.5373 0.0363 Uiso 1 0 . H11 H 0.3279 -0.2482 0.6501 0.0387 Uiso 1 0 . H12 H 0.2435 -0.0718 0.6683 0.0362 Uiso 1 0 . H13 H 0.1512 0.12 0.6005 0.0336 Uiso 1 0 . H14 H 0.2531 0.1783 0.5934 0.0336 Uiso 1 0 . H15 H 0.0725 0.1222 0.4716 0.0306 Uiso 1 0 . H16 H 0.4419 -0.1565 0.3086 0.0396 Uiso 1 0 . H17 H 0.478 -0.0729 0.2522 0.0396 Uiso 1 0 . H18 H 0.5208 -0.0537 0.345 0.0396 Uiso 1 0 . H19 H 0.4603 0.1565 0.3249 0.038 Uiso 1 0 . H20 H 0.4143 0.1382 0.2321 0.038 Uiso 1 0 . H21 H 0.3423 0.1863 0.2788 0.038 Uiso 1 0 . H22 H 0.2134 0.0223 0.2222 0.0361 Uiso 1 0 . H23 H 0.2854 -0.0259 0.1755 0.0361 Uiso 1 0 . H24 H 0.2509 -0.1092 0.2329 0.0361 Uiso 1 0 . H25 H 0.1016 0.298 0.6077 0.0398 Uiso 1 0 . H26 H 0.0145 0.3837 0.556 0.0398 Uiso 1 0 . H27 H -0.0064 0.2476 0.553 0.0398 Uiso 1 0 . H28 H -0.0334 0.3855 0.4073 0.0361 Uiso 1 0 . H29 H 0.0244 0.3026 0.3645 0.0361 Uiso 1 0 . H30 H -0.0528 0.2491 0.4047 0.0361 Uiso 1 0 . H31 H 0.2315 0.3784 0.5443 0.0377 Uiso 1 0 . H32 H 0.2019 0.3795 0.451 0.0377 Uiso 1 0 . H33 H 0.1456 0.4658 0.4929 0.0377 Uiso 1 0 . H34 H 0.3695 0.4222 0.3173 0.0448 Uiso 1 0 . H35 H 0.3711 0.4106 0.4058 0.0448 Uiso 1 0 .