#------------------------------------------------------------------------------ #$Date: 2014-07-23 12:49:31 +0300 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100802.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_1100802 _chemical_formula_sum 'C17 H30 Cl F6 N6 O3 P3 Ru' _chemical_formula_weight 709.90 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 26.2152(19) _cell_length_b 14.9540(11) _cell_length_c 6.4535(5) _cell_measurement_reflns_used ? _cell_measurement_temperature 123(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 2529.9(3) _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.0845 _diffrn_reflns_av_sigmaI/netI 0.1061 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 14733 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_min 1.55 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 1432 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(4) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 338 _refine_ls_number_reflns 5488 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.928 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0471 _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^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.0984 _reflns_number_gt 3830 _reflns_number_total 5488 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 1100802 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.487140(17) 0.28176(3) 0.46164(6) 0.01026(11) Uani 1 1 d . . . P1 P 0.42100(6) 0.21910(10) 0.2885(2) 0.0108(3) Uani 1 1 d . . . P2 P 0.55227(6) 0.21814(10) 0.2838(2) 0.0111(3) Uani 1 1 d . . . P3 P 0.29328(7) 0.49840(11) 1.2764(3) 0.0186(4) Uani 1 1 d . . . Cl1 Cl 0.48665(6) 0.14645(9) 0.6807(2) 0.0150(3) Uani 1 1 d . . . N1 N 0.36758(19) 0.0701(3) 0.1556(8) 0.0130(11) Uani 1 1 d . . . N2 N 0.31606(19) 0.1871(3) 0.3217(7) 0.0122(11) Uani 1 1 d . . . N3 N 0.35000(17) 0.2097(3) -0.0265(10) 0.0135(10) Uani 1 1 d . . . N4 N 0.60748(19) 0.0718(3) 0.1457(8) 0.0136(12) Uani 1 1 d . . . N5 N 0.6571(2) 0.1931(3) 0.3023(8) 0.0131(11) Uani 1 1 d . . . H5N H 0.691(3) 0.203(4) 0.362(10) 0.03(2) Uiso 1 1 d . . . N6 N 0.62118(15) 0.2133(3) -0.0435(10) 0.0127(9) Uani 1 1 d . . . F1 F 0.34376(13) 0.4617(2) 1.4113(5) 0.0229(9) Uani 1 1 d . . . F2 F 0.26266(14) 0.4005(2) 1.3271(6) 0.0240(9) Uani 1 1 d . . . F3 F 0.26829(14) 0.5427(2) 1.4931(6) 0.0290(10) Uani 1 1 d . . . F4 F 0.24290(14) 0.5342(2) 1.1391(6) 0.0227(9) Uani 1 1 d . . . F5 F 0.31739(15) 0.4514(3) 1.0572(5) 0.0240(9) Uani 1 1 d . . . F6 F 0.32397(13) 0.5953(2) 1.2224(6) 0.0214(9) Uani 1 1 d . . . C1 C 0.4173(2) 0.0977(4) 0.2418(10) 0.0137(14) Uani 1 1 d . . . H1A H 0.4447 0.0802 0.1444 0.016 Uiso 1 1 calc R . . H1B H 0.4232 0.0658 0.3740 0.016 Uiso 1 1 calc R . . C2 C 0.3600(2) 0.2326(4) 0.4278(9) 0.0106(14) Uani 1 1 d . . . H2A H 0.3636 0.2079 0.5693 0.013 Uiso 1 1 calc R . . H2B H 0.3523 0.2972 0.4409 0.013 Uiso 1 1 calc R . . C3 C 0.3977(2) 0.2575(4) 0.0328(9) 0.0147(15) Uani 1 1 d . . . H3A H 0.3911 0.3226 0.0379 0.018 Uiso 1 1 calc R . . H3B H 0.4243 0.2465 -0.0733 0.018 Uiso 1 1 calc R . . C4 C 0.3259(2) 0.0878(4) 0.2963(9) 0.0143(14) Uani 1 1 d . . . H4A H 0.3339 0.0615 0.4333 0.017 Uiso 1 1 calc R . . H4B H 0.2946 0.0586 0.2434 0.017 Uiso 1 1 calc R . . C5 C 0.3577(2) 0.1133(3) -0.0453(12) 0.0138(12) Uani 1 1 d . . . H5A H 0.3869 0.1019 -0.1390 0.017 Uiso 1 1 calc R . . H5B H 0.3270 0.0861 -0.1087 0.017 Uiso 1 1 calc R . . C6 C 0.3077(2) 0.2269(4) 0.1071(9) 0.0147(14) Uani 1 1 d . . . H6A H 0.2764 0.2010 0.0457 0.018 Uiso 1 1 calc R . . H6B H 0.3027 0.2923 0.1196 0.018 Uiso 1 1 calc R . . C7 C 0.5575(2) 0.0959(4) 0.2366(10) 0.0160(14) Uani 1 1 d . . . H7A H 0.5529 0.0636 0.3692 0.019 Uiso 1 1 calc R . . H7B H 0.5299 0.0770 0.1414 0.019 Uiso 1 1 calc R . . C8 C 0.6132(2) 0.2346(4) 0.4189(9) 0.0128(15) Uani 1 1 d . . . H8A H 0.6196 0.2994 0.4359 0.015 Uiso 1 1 calc R . . H8B H 0.6111 0.2076 0.5587 0.015 Uiso 1 1 calc R . . C9 C 0.5733(2) 0.2575(4) 0.0253(9) 0.0155(15) Uani 1 1 d . . . H9A H 0.5461 0.2453 -0.0771 0.019 Uiso 1 1 calc R . . H9B H 0.5788 0.3229 0.0303 0.019 Uiso 1 1 calc R . . C10 C 0.6498(2) 0.0920(4) 0.2793(10) 0.0160(14) Uani 1 1 d . . . H10A H 0.6813 0.0653 0.2214 0.019 Uiso 1 1 calc R . . H10B H 0.6438 0.0653 0.4174 0.019 Uiso 1 1 calc R . . C11 C 0.6153(2) 0.1158(3) -0.0546(12) 0.0169(13) Uani 1 1 d . . . H11A H 0.5859 0.1019 -0.1454 0.020 Uiso 1 1 calc R . . H11B H 0.6462 0.0902 -0.1203 0.020 Uiso 1 1 calc R . . C12 C 0.6640(2) 0.2338(4) 0.0866(9) 0.0148(15) Uani 1 1 d . . . H12A H 0.6676 0.2995 0.0988 0.018 Uiso 1 1 calc R . . H12B H 0.6955 0.2099 0.0229 0.018 Uiso 1 1 calc R . . C13 C 0.4447(2) 0.3937(4) 0.6103(10) 0.0149(15) Uani 1 1 d . . . H13A H 0.4087 0.3916 0.6611 0.018 Uiso 1 1 calc R . . C14 C 0.4882(3) 0.3774(4) 0.7281(10) 0.0162(13) Uani 1 1 d . . . H14A H 0.4885 0.3602 0.8778 0.019 Uiso 1 1 calc R . . C15 C 0.5316(3) 0.3922(4) 0.6063(10) 0.0177(15) Uani 1 1 d . . . H15A H 0.5678 0.3890 0.6540 0.021 Uiso 1 1 calc R . . C16 C 0.5146(3) 0.4170(4) 0.4045(9) 0.0172(15) Uani 1 1 d . . . H16A H 0.5367 0.4364 0.2865 0.021 Uiso 1 1 calc R . . C17 C 0.4607(3) 0.4166(4) 0.4073(9) 0.0148(15) Uani 1 1 d . . . H17A H 0.4380 0.4362 0.2914 0.018 Uiso 1 1 calc R . . O1W O 0.36676(17) 0.5620(3) 0.7667(7) 0.0226(11) Uani 1 1 d . . . O2W O 0.74774(17) 0.1141(3) 0.7693(7) 0.0217(11) Uani 1 1 d . . . O3W O 0.73222(15) 0.2693(3) 0.5583(6) 0.0141(10) Uani 1 1 d . . . 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 Ru1 0.0093(2) 0.00893(19) 0.0125(2) -0.0012(2) 0.0002(4) -0.0003(2) P1 0.0093(8) 0.0107(7) 0.0123(8) -0.0006(7) 0.0004(7) -0.0004(7) P2 0.0090(8) 0.0108(8) 0.0135(8) 0.0002(7) -0.0004(7) 0.0002(7) P3 0.0166(9) 0.0203(8) 0.0187(8) 0.0007(7) -0.0008(8) 0.0015(7) Cl1 0.0159(8) 0.0151(7) 0.0139(7) 0.0008(5) -0.0009(8) -0.0004(7) N1 0.012(3) 0.014(3) 0.013(3) 0.005(2) -0.002(2) -0.002(2) N2 0.011(3) 0.015(2) 0.011(3) -0.002(2) -0.004(2) 0.000(2) N3 0.013(2) 0.017(2) 0.010(2) 0.003(3) -0.005(3) -0.005(2) N4 0.009(3) 0.014(3) 0.017(3) 0.000(2) 0.001(2) 0.001(2) N5 0.007(3) 0.017(3) 0.016(3) 0.004(2) -0.002(2) 0.001(2) N6 0.009(2) 0.017(2) 0.012(2) 0.002(3) -0.004(3) 0.000(2) F1 0.017(2) 0.025(2) 0.027(3) -0.0026(16) -0.0072(17) 0.0067(16) F2 0.018(2) 0.0217(19) 0.032(2) 0.0090(17) 0.0006(18) -0.0008(17) F3 0.031(2) 0.037(2) 0.019(2) -0.0029(19) 0.006(2) 0.0147(17) F4 0.015(2) 0.026(2) 0.026(2) 0.0088(18) -0.0090(18) -0.0057(17) F5 0.034(2) 0.023(2) 0.0157(19) -0.0019(16) 0.0063(18) 0.0010(19) F6 0.015(2) 0.0155(19) 0.034(2) 0.0033(16) -0.0051(17) -0.0036(16) C1 0.010(3) 0.010(3) 0.021(4) 0.001(3) -0.001(3) 0.003(3) C2 0.008(3) 0.015(3) 0.008(4) -0.002(3) 0.001(3) -0.002(2) C3 0.017(4) 0.017(3) 0.010(3) 0.002(2) -0.001(3) -0.006(3) C4 0.017(4) 0.017(3) 0.009(3) 0.000(3) 0.000(3) -0.007(3) C5 0.013(3) 0.018(3) 0.009(3) -0.001(3) 0.002(4) 0.000(2) C6 0.018(4) 0.017(3) 0.010(3) 0.002(3) -0.002(3) 0.001(3) C7 0.011(3) 0.013(3) 0.023(4) 0.000(3) 0.005(3) 0.000(3) C8 0.012(3) 0.012(3) 0.014(4) -0.001(2) -0.003(3) -0.002(2) C9 0.014(3) 0.013(3) 0.019(4) -0.001(2) -0.001(3) 0.002(3) C10 0.015(3) 0.017(3) 0.016(3) 0.002(3) -0.003(3) 0.005(3) C11 0.011(3) 0.019(3) 0.020(4) -0.006(3) -0.001(4) 0.001(2) C12 0.012(3) 0.019(4) 0.013(3) -0.001(3) 0.006(3) -0.002(3) C13 0.011(4) 0.012(3) 0.022(4) -0.007(3) -0.001(3) 0.003(3) C14 0.016(3) 0.007(3) 0.026(4) -0.008(2) 0.001(3) -0.003(3) C15 0.016(4) 0.011(3) 0.026(4) -0.007(3) 0.007(3) -0.003(3) C16 0.016(3) 0.010(3) 0.026(4) -0.004(2) 0.005(3) -0.001(3) C17 0.015(3) 0.013(3) 0.017(4) -0.002(2) -0.003(3) 0.002(3) O1W 0.020(3) 0.022(2) 0.026(3) 0.001(2) 0.000(2) -0.004(2) O2W 0.024(3) 0.022(2) 0.019(2) -0.002(2) 0.001(2) 0.006(2) O3W 0.012(2) 0.014(3) 0.016(2) -0.0003(16) 0.0002(19) -0.0026(19) 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' P P 0.1023 0.0942 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _journal_paper_doi 10.1021/om048987r