Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Jon Dilworth' _publ_contact_author_address ; Department of Inorganic Chemistry University of Oxford Chemistry Research Lab 12 Mansfield Road Oxford OX1 3TA UNITED KINGDOM ; _publ_contact_author_email JON.DILWORTH@CHEM.OX.AC.UK _publ_section_title ; Preparation and characterization of diarylphosphazene and diarylphosphinohydrazide complexes of titanium, tungsten and ruthenium and phosphorylketimido complexes of rhenium ; loop_ _publ_author_name J.R.Dilworth 'Andrew R. Cowle' 'Alison K. Nairn' 'Alasdair Robbie' data_arc932 _database_code_depnum_ccdc_archive 'CCDC 255284' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; 1-dimethylphosphino-2,2-dimethylhydrazine ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #============================================================= _cell_length_a 16.4464(4) _cell_angle_alpha 90 _cell_length_b 8.4807(2) _cell_angle_beta 90 _cell_length_c 19.3755(4) _cell_angle_gamma 90 _cell_volume 2702.44(11) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C14 H17 N2 P ' _chemical_formula_moiety ' C14 H17 N2 P ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 244.28 _cell_measurement_reflns_used 19242 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.184 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.97 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 19242 _reflns_number_total 3069 # 3474 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_min 5.249 _diffrn_reflns_theta_max 27.485 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.485 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.20 _refine_diff_density_max 0.27 _refine_ls_number_reflns 2202 _refine_ls_number_restraints 0 _refine_ls_number_parameters 158 #_refine_ls_R_factor_ref 0.0358 _refine_ls_wR_factor_ref 0.0410 _refine_ls_goodness_of_fit_ref 1.0875 #_reflns_number_all 3069 _refine_ls_R_factor_all 0.0537 _refine_ls_wR_factor_all 0.0563 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 2202 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_gt 0.0410 _refine_ls_shift/su_max 0.002867 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.533 0.287 0.224 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type P1 P 0.36294(2) 0.40978(4) 0.40756(2) 0.0315 1.0000 Uani N1 N 0.28694(8) 0.33027(15) 0.36109(7) 0.0338 1.0000 Uani N2 N 0.21765(8) 0.43075(15) 0.35011(6) 0.0310 1.0000 Uani C1 C 0.19642(11) 0.4236(2) 0.27726(9) 0.0455 1.0000 Uani C2 C 0.14928(11) 0.3827(2) 0.39303(10) 0.0430 1.0000 Uani C3 C 0.44491(9) 0.27579(16) 0.38157(8) 0.0295 1.0000 Uani C4 C 0.49580(10) 0.19659(18) 0.42774(8) 0.0328 1.0000 Uani C5 C 0.56057(10) 0.1063(2) 0.40396(9) 0.0389 1.0000 Uani C6 C 0.57518(10) 0.0935(2) 0.33386(10) 0.0431 1.0000 Uani C7 C 0.52541(11) 0.1709(2) 0.28717(9) 0.0430 1.0000 Uani C8 C 0.46128(10) 0.2622(2) 0.31086(8) 0.0361 1.0000 Uani C9 C 0.34846(9) 0.35232(17) 0.49812(8) 0.0310 1.0000 Uani C10 C 0.39310(10) 0.4359(2) 0.54739(9) 0.0388 1.0000 Uani C11 C 0.38437(11) 0.4046(2) 0.61739(9) 0.0429 1.0000 Uani C12 C 0.32940(11) 0.2915(2) 0.63894(9) 0.0417 1.0000 Uani C13 C 0.28403(11) 0.2084(2) 0.59075(9) 0.0424 1.0000 Uani C14 C 0.29384(10) 0.23800(19) 0.52070(8) 0.0376 1.0000 Uani H1 H 0.2752(12) 0.229(2) 0.3621(10) 0.043(5) 1.0000 Uiso H11 H 0.1483 0.4927 0.2683 0.0546 1.0000 Uiso H12 H 0.2435 0.4608 0.2489 0.0546 1.0000 Uiso H13 H 0.1829 0.3124 0.2645 0.0546 1.0000 Uiso H21 H 0.1021 0.4543 0.3844 0.0516 1.0000 Uiso H22 H 0.1652 0.3888 0.4428 0.0516 1.0000 Uiso H23 H 0.1336 0.2719 0.3814 0.0516 1.0000 Uiso H41 H 0.4855 0.2049 0.4785 0.0394 1.0000 Uiso H51 H 0.5966 0.0505 0.4376 0.0467 1.0000 Uiso H61 H 0.6217 0.0284 0.3169 0.0518 1.0000 Uiso H71 H 0.5357 0.1609 0.2365 0.0515 1.0000 Uiso H81 H 0.4262 0.3192 0.2769 0.0433 1.0000 Uiso H101 H 0.4319 0.5196 0.5320 0.0466 1.0000 Uiso H111 H 0.4177 0.4635 0.6520 0.0515 1.0000 Uiso H121 H 0.3223 0.2696 0.6893 0.0501 1.0000 Uiso H131 H 0.2442 0.1270 0.6065 0.0509 1.0000 Uiso H141 H 0.2614 0.1767 0.4863 0.0451 1.0000 Uiso 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 P1 0.0344(2) 0.02176(18) 0.0383(2) -0.00075(15) -0.00547(17) -0.00019(15) N1 0.0320(7) 0.0243(6) 0.0451(7) -0.0031(5) -0.0094(6) 0.0056(5) N2 0.0302(6) 0.0295(6) 0.0335(6) 0.0018(5) -0.0021(5) 0.0075(5) C1 0.0438(9) 0.0571(10) 0.0356(8) 0.0006(8) -0.0080(7) 0.0105(9) C2 0.0423(9) 0.0330(8) 0.0536(10) 0.0060(7) 0.0106(8) 0.0082(7) C3 0.0284(7) 0.0236(7) 0.0366(7) 0.0003(6) -0.0023(6) -0.0061(5) C4 0.0329(8) 0.0314(7) 0.0343(7) -0.0008(6) -0.0041(6) -0.0018(6) C5 0.0322(8) 0.0396(8) 0.0449(9) -0.0018(7) -0.0048(7) 0.0041(7) C6 0.0324(8) 0.0472(9) 0.0498(9) -0.0085(8) 0.0037(7) 0.0020(8) C7 0.0387(9) 0.0527(10) 0.0375(8) -0.0042(8) 0.0051(7) -0.0059(8) C8 0.0347(8) 0.0381(8) 0.0355(8) 0.0045(7) -0.0020(6) -0.0052(7) C9 0.0299(7) 0.0252(7) 0.0380(8) -0.0051(6) -0.0029(6) 0.0019(6) C10 0.0320(8) 0.0412(9) 0.0432(9) -0.0147(7) 0.0038(7) -0.0065(7) C11 0.0406(9) 0.0484(10) 0.0397(8) -0.0142(8) 0.0007(7) -0.0019(8) C12 0.0422(9) 0.0454(9) 0.0376(8) -0.0021(7) -0.0008(7) 0.0039(8) C13 0.0422(9) 0.0387(8) 0.0463(9) 0.0079(7) -0.0071(8) -0.0050(7) C14 0.0397(9) 0.0300(7) 0.0431(8) 0.0027(7) -0.0114(7) -0.0042(7) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P1 . N1 . 1.6815(13) yes P1 . C3 . 1.8336(16) yes P1 . C9 . 1.8367(16) yes N1 . N2 . 1.4388(17) yes N1 . H1 . 0.88(2) no N2 . C1 . 1.455(2) yes N2 . C2 . 1.457(2) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . C4 . 1.397(2) yes C3 . C8 . 1.401(2) yes C4 . C5 . 1.390(2) yes C4 . H41 . 1.000 no C5 . C6 . 1.384(2) yes C5 . H51 . 1.000 no C6 . C7 . 1.385(3) yes C6 . H61 . 1.000 no C7 . C8 . 1.387(2) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.398(2) yes C9 . C14 . 1.392(2) yes C10 . C11 . 1.390(2) yes C10 . H101 . 1.000 no C11 . C12 . 1.382(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.388(2) yes C12 . H121 . 1.000 no C13 . C14 . 1.390(2) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . P1 . C3 . 98.69(7) yes N1 . P1 . C9 . 107.99(7) yes C3 . P1 . C9 . 101.14(7) yes P1 . N1 . N2 . 115.50(10) yes P1 . N1 . H1 . 122.8(13) no N2 . N1 . H1 . 114.1(13) no N1 . N2 . C1 . 107.98(12) yes N1 . N2 . C2 . 111.17(12) yes C1 . N2 . C2 . 110.90(14) yes N2 . C1 . H11 . 109.467 no N2 . C1 . H12 . 109.466 no H11 . C1 . H12 . 109.476 no N2 . C1 . H13 . 109.467 no H11 . C1 . H13 . 109.476 no H12 . C1 . H13 . 109.476 no N2 . C2 . H21 . 109.467 no N2 . C2 . H22 . 109.467 no H21 . C2 . H22 . 109.476 no N2 . C2 . H23 . 109.467 no H21 . C2 . H23 . 109.476 no H22 . C2 . H23 . 109.476 no P1 . C3 . C4 . 124.23(12) yes P1 . C3 . C8 . 117.44(11) yes C4 . C3 . C8 . 118.13(14) yes C3 . C4 . C5 . 120.77(15) yes C3 . C4 . H41 . 119.616 no C5 . C4 . H41 . 119.617 no C4 . C5 . C6 . 120.10(15) yes C4 . C5 . H51 . 119.951 no C6 . C5 . H51 . 119.951 no C5 . C6 . C7 . 120.09(15) yes C5 . C6 . H61 . 119.954 no C7 . C6 . H61 . 119.954 no C6 . C7 . C8 . 119.86(15) yes C6 . C7 . H71 . 120.072 no C8 . C7 . H71 . 120.072 no C3 . C8 . C7 . 121.05(15) yes C3 . C8 . H81 . 119.475 no C7 . C8 . H81 . 119.475 no P1 . C9 . C10 . 116.73(12) yes P1 . C9 . C14 . 124.65(12) yes C10 . C9 . C14 . 118.54(15) yes C9 . C10 . C11 . 121.01(15) yes C9 . C10 . H101 . 119.494 no C11 . C10 . H101 . 119.494 no C10 . C11 . C12 . 119.68(15) yes C10 . C11 . H111 . 120.159 no C12 . C11 . H111 . 120.159 no C11 . C12 . C13 . 120.04(16) yes C11 . C12 . H121 . 119.978 no C13 . C12 . H121 . 119.978 no C12 . C13 . C14 . 120.22(16) yes C12 . C13 . H131 . 119.891 no C14 . C13 . H131 . 119.892 no C9 . C14 . C13 . 120.49(15) yes C9 . C14 . H141 . 119.756 no C13 . C14 . H141 . 119.756 no data_arc942 _database_code_depnum_ccdc_archive 'CCDC 255285' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _chemical_absolute_configuration ad _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; The NH hydrogen atom was located in a difference Fourier map and its coordinates and isotropic displacement parameter subsequently refined. All other hydrogen atoms were positioned geometrically, the preferred orientation of the methyl group H241-H243 having been previously identified by examination of the Fourier map. ; #============================================================= _cell_length_a 14.7058(5) _cell_angle_alpha 90 _cell_length_b 16.8368(5) _cell_angle_beta 90 _cell_length_c 10.5355(4) _cell_angle_gamma 90 _cell_volume 2608.57(15) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C24 H31 B Cl F4 N2 P Ru ' _chemical_formula_moiety ' C24 H31 Cl1 N2 P Ru, B F4 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 601.82 _cell_measurement_reflns_used 18147 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' orange-yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.809 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.92 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 18147 _reflns_number_total 5587 # 5812 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_min 5.188 _diffrn_reflns_theta_max 27.462 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.462 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min -13 _reflns_limit_l_max 13 _refine_diff_density_min -0.66 _refine_diff_density_max 0.66 _refine_ls_number_reflns 4337 _refine_ls_number_restraints 1 _refine_ls_number_parameters 312 #_refine_ls_R_factor_ref 0.0343 _refine_ls_wR_factor_ref 0.0367 _refine_ls_goodness_of_fit_ref 1.1040 #_reflns_number_all 5587 _refine_ls_R_factor_all 0.0529 _refine_ls_wR_factor_all 0.0614 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4337 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_gt 0.0367 _refine_ls_shift/su_max 0.009429 _refine_ls_abs_structure_Flack 0.46(4) _refine_ls_abs_structure_details 'Flack, 2478 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.389 0.0439 0.113 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Ru1 Ru 0.615207(17) 0.409724(16) 0.46274(8) 0.0222 1.0000 Uani Cl1 Cl 0.52398(7) 0.51085(6) 0.36678(12) 0.0295 1.0000 Uani P1 P 0.48054(6) 0.33905(5) 0.47372(14) 0.0227 1.0000 Uani N1 N 0.4974(2) 0.3114(2) 0.3246(4) 0.0273 1.0000 Uani N2 N 0.5898(2) 0.3352(2) 0.2925(4) 0.0284 1.0000 Uani C1 C 0.5883(4) 0.3727(3) 0.1654(4) 0.0381 1.0000 Uani C2 C 0.6482(3) 0.2634(3) 0.2862(5) 0.0396 1.0000 Uani C3 C 0.3688(2) 0.3846(2) 0.4772(6) 0.0248 1.0000 Uani C4 C 0.3116(3) 0.3781(3) 0.3736(4) 0.0292 1.0000 Uani C5 C 0.2269(3) 0.4155(3) 0.3737(5) 0.0346 1.0000 Uani C6 C 0.2000(3) 0.4596(2) 0.4790(6) 0.0321 1.0000 Uani C7 C 0.2562(3) 0.4651(3) 0.5815(5) 0.0361 1.0000 Uani C8 C 0.3411(3) 0.4289(3) 0.5829(4) 0.0323 1.0000 Uani C9 C 0.4692(3) 0.2519(3) 0.5749(5) 0.0290 1.0000 Uani C10 C 0.4841(3) 0.1756(3) 0.5297(5) 0.0369 1.0000 Uani C11 C 0.4772(4) 0.1106(3) 0.6103(6) 0.0473 1.0000 Uani C12 C 0.4555(4) 0.1223(4) 0.7360(7) 0.0539 1.0000 Uani C13 C 0.4413(4) 0.1980(4) 0.7841(6) 0.0503 1.0000 Uani C14 C 0.4470(4) 0.2631(3) 0.7031(5) 0.0420 1.0000 Uani C15 C 0.7231(3) 0.5036(3) 0.5046(4) 0.0286 1.0000 Uani C16 C 0.6630(3) 0.4902(3) 0.6111(4) 0.0304 1.0000 Uani C17 C 0.6520(3) 0.4139(3) 0.6630(4) 0.0306 1.0000 Uani C18 C 0.6980(3) 0.3473(3) 0.6122(4) 0.0310 1.0000 Uani C19 C 0.7503(3) 0.3595(3) 0.5020(5) 0.0339 1.0000 Uani C20 C 0.7654(2) 0.4368(3) 0.4509(6) 0.0304 1.0000 Uani C21 C 0.7405(3) 0.5848(3) 0.4468(6) 0.0360 1.0000 Uani C22 C 0.8425(4) 0.6032(3) 0.4558(11) 0.0615 1.0000 Uani C23 C 0.6847(4) 0.6515(3) 0.5065(5) 0.0481 1.0000 Uani C24 C 0.6916(4) 0.2648(3) 0.6717(6) 0.0430 1.0000 Uani B1 B 0.4053(5) 0.1434(4) 0.1574(6) 0.0465 1.0000 Uani F1 F 0.3662(2) 0.1855(2) 0.2566(3) 0.0523 1.0000 Uani F2 F 0.4782(3) 0.1881(3) 0.1161(4) 0.0706 1.0000 Uani F3 F 0.4256(4) 0.0688(3) 0.2007(5) 0.0873 1.0000 Uani F4 F 0.3406(3) 0.1389(2) 0.0606(4) 0.0795 1.0000 Uani H1 H 0.474(3) 0.268(3) 0.288(5) 0.028(13) 1.0000 Uiso H11 H 0.6513 0.3895 0.1417 0.0457 1.0000 Uiso H12 H 0.5476 0.4202 0.1672 0.0457 1.0000 Uiso H13 H 0.5651 0.3337 0.1016 0.0457 1.0000 Uiso H21 H 0.7118 0.2793 0.2642 0.0475 1.0000 Uiso H22 H 0.6478 0.2360 0.3704 0.0475 1.0000 Uiso H23 H 0.6242 0.2265 0.2197 0.0475 1.0000 Uiso H41 H 0.3310 0.3464 0.2981 0.0351 1.0000 Uiso H51 H 0.1857 0.4106 0.2985 0.0415 1.0000 Uiso H61 H 0.1398 0.4872 0.4794 0.0385 1.0000 Uiso H71 H 0.2358 0.4959 0.6575 0.0433 1.0000 Uiso H81 H 0.3819 0.4345 0.6583 0.0387 1.0000 Uiso H101 H 0.5000 0.1674 0.4383 0.0443 1.0000 Uiso H111 H 0.4880 0.0558 0.5772 0.0568 1.0000 Uiso H121 H 0.4497 0.0753 0.7936 0.0647 1.0000 Uiso H131 H 0.4272 0.2057 0.8762 0.0603 1.0000 Uiso H141 H 0.4352 0.3177 0.7362 0.0504 1.0000 Uiso H161 H 0.6287 0.5359 0.6483 0.0365 1.0000 Uiso H171 H 0.6107 0.4065 0.7376 0.0367 1.0000 Uiso H191 H 0.7777 0.3126 0.4581 0.0407 1.0000 Uiso H201 H 0.8066 0.4435 0.3762 0.0364 1.0000 Uiso H211 H 0.7204 0.5824 0.3562 0.0431 1.0000 Uiso H221 H 0.8547 0.6566 0.4180 0.0738 1.0000 Uiso H222 H 0.8616 0.6031 0.5469 0.0738 1.0000 Uiso H223 H 0.8776 0.5619 0.4083 0.0738 1.0000 Uiso H231 H 0.6997 0.7030 0.4639 0.0578 1.0000 Uiso H232 H 0.6993 0.6554 0.5990 0.0578 1.0000 Uiso H233 H 0.6184 0.6399 0.4957 0.0578 1.0000 Uiso H241 H 0.7411 0.2582 0.7360 0.0516 1.0000 Uiso H242 H 0.6311 0.2585 0.7140 0.0516 1.0000 Uiso H243 H 0.6984 0.2235 0.6040 0.0516 1.0000 Uiso 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 0.01688(12) 0.02614(12) 0.02358(12) 0.0003(2) 0.0010(2) -0.00131(11) Cl1 0.0277(5) 0.0276(5) 0.0332(5) 0.0045(4) -0.0005(4) 0.0001(4) P1 0.0165(4) 0.0245(4) 0.0270(5) 0.0021(5) 0.0009(6) -0.0017(3) N1 0.0196(17) 0.0295(19) 0.033(2) -0.0065(16) 0.0039(14) -0.0054(15) N2 0.0242(18) 0.0281(19) 0.0329(19) -0.0003(15) 0.0048(15) -0.0034(14) C1 0.048(3) 0.040(3) 0.026(2) -0.0024(19) 0.009(2) -0.005(2) C2 0.029(3) 0.037(3) 0.053(3) -0.015(2) 0.004(2) 0.009(2) C3 0.0226(17) 0.0219(14) 0.030(3) 0.000(2) -0.005(2) -0.0028(12) C4 0.025(2) 0.036(2) 0.026(2) -0.0005(19) -0.0052(18) 0.0013(18) C5 0.027(2) 0.035(2) 0.042(3) 0.002(2) -0.007(2) 0.0027(19) C6 0.0221(18) 0.0261(17) 0.048(3) 0.003(2) 0.000(2) 0.0021(14) C7 0.033(2) 0.036(2) 0.039(3) -0.006(2) 0.003(2) 0.010(2) C8 0.034(2) 0.034(2) 0.029(2) -0.0071(18) -0.007(2) 0.003(2) C9 0.0170(19) 0.031(2) 0.039(2) 0.0079(19) -0.0027(17) 0.0007(17) C10 0.028(2) 0.033(2) 0.049(3) 0.012(2) -0.001(2) -0.0001(19) C11 0.030(3) 0.035(3) 0.077(4) 0.017(3) 0.002(3) 0.000(2) C12 0.043(3) 0.046(3) 0.073(4) 0.037(3) 0.004(3) 0.001(3) C13 0.041(3) 0.061(4) 0.049(3) 0.025(3) 0.016(3) 0.010(3) C14 0.036(3) 0.048(3) 0.042(3) 0.017(2) 0.011(2) 0.012(2) C15 0.023(2) 0.035(2) 0.028(2) -0.0032(16) -0.0046(15) -0.0132(17) C16 0.025(2) 0.041(2) 0.024(2) -0.0064(19) -0.0021(17) -0.0043(19) C17 0.026(2) 0.042(2) 0.024(2) 0.0094(19) -0.0064(17) -0.008(2) C18 0.021(2) 0.039(2) 0.033(2) 0.0069(19) -0.0087(17) -0.0001(18) C19 0.0175(18) 0.042(2) 0.043(3) 0.0038(19) -0.0033(17) 0.0062(17) C20 0.0143(16) 0.042(2) 0.035(3) -0.003(3) -0.003(2) -0.0033(13) C21 0.036(2) 0.039(2) 0.033(3) 0.001(2) 0.002(2) -0.0107(18) C22 0.041(2) 0.059(3) 0.085(4) 0.014(5) -0.001(5) -0.027(2) C23 0.064(4) 0.033(2) 0.047(3) -0.001(2) 0.009(2) -0.011(2) C24 0.030(3) 0.043(3) 0.055(3) 0.012(3) -0.006(2) 0.001(2) B1 0.056(4) 0.044(3) 0.039(3) -0.011(3) 0.010(3) -0.020(3) F1 0.0486(19) 0.0562(19) 0.0522(19) -0.0106(15) 0.0150(15) -0.0111(15) F2 0.054(2) 0.085(3) 0.073(3) -0.023(2) 0.023(2) -0.030(2) F3 0.100(3) 0.055(2) 0.107(4) -0.009(2) -0.002(3) 0.022(2) F4 0.108(3) 0.075(3) 0.056(2) -0.004(2) -0.018(2) -0.041(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . Cl1 . 2.3918(11) yes Ru1 . P1 . 2.3133(9) yes Ru1 . N2 . 2.221(4) yes Ru1 . C15 . 2.282(4) yes Ru1 . C16 . 2.184(4) yes Ru1 . C17 . 2.180(4) yes Ru1 . C18 . 2.251(4) yes Ru1 . C19 . 2.198(4) yes Ru1 . C20 . 2.259(4) yes P1 . N1 . 1.658(4) yes P1 . C3 . 1.813(4) yes P1 . C9 . 1.822(4) yes N1 . N2 . 1.457(5) yes N1 . H1 . 0.89(5) yes N2 . C1 . 1.480(6) yes N2 . C2 . 1.484(6) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . C4 . 1.383(7) yes C3 . C8 . 1.401(7) yes C4 . C5 . 1.395(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.393(7) yes C5 . H51 . 1.000 no C6 . C7 . 1.362(8) yes C6 . H61 . 1.000 no C7 . C8 . 1.390(7) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.387(7) yes C9 . C14 . 1.402(7) yes C10 . C11 . 1.388(7) yes C10 . H101 . 1.000 no C11 . C12 . 1.377(10) yes C11 . H111 . 1.000 no C12 . C13 . 1.387(10) yes C12 . H121 . 1.000 no C13 . C14 . 1.392(8) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.446(6) yes C15 . C20 . 1.404(6) yes C15 . C21 . 1.519(6) yes C16 . C17 . 1.406(7) yes C16 . H161 . 1.000 no C17 . C18 . 1.415(7) yes C17 . H171 . 1.000 no C18 . C19 . 1.408(7) yes C18 . C24 . 1.528(7) yes C19 . C20 . 1.425(7) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.534(6) yes C21 . C23 . 1.527(7) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no B1 . F1 . 1.388(7) yes B1 . F2 . 1.381(7) yes B1 . F3 . 1.369(9) yes B1 . F4 . 1.396(8) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ru1 . P1 . 84.67(4) yes Cl1 . Ru1 . N2 . 88.08(10) yes P1 . Ru1 . N2 . 66.79(10) yes Cl1 . Ru1 . C15 . 88.78(12) yes P1 . Ru1 . C15 . 160.33(12) yes N2 . Ru1 . C15 . 131.62(15) yes Cl1 . Ru1 . C16 . 92.37(13) yes P1 . Ru1 . C16 . 123.96(12) yes N2 . Ru1 . C16 . 169.24(15) yes C15 . Ru1 . C16 . 37.70(16) yes Cl1 . Ru1 . C17 . 121.70(14) yes P1 . Ru1 . C17 . 100.41(12) yes N2 . Ru1 . C17 . 147.35(16) yes C15 . Ru1 . C17 . 67.55(16) yes C16 . Ru1 . C17 . 37.58(17) yes Cl1 . Ru1 . C18 . 158.67(13) yes P1 . Ru1 . C18 . 100.84(12) yes N2 . Ru1 . C18 . 113.09(16) yes C15 . Ru1 . C18 . 79.16(16) yes C16 . Ru1 . C18 . 67.36(18) yes Cl1 . Ru1 . C19 . 149.32(13) yes P1 . Ru1 . C19 . 124.52(13) yes N2 . Ru1 . C19 . 94.96(16) yes C15 . Ru1 . C19 . 66.52(17) yes C16 . Ru1 . C19 . 79.23(18) yes Cl1 . Ru1 . C20 . 112.43(13) yes P1 . Ru1 . C20 . 160.68(11) yes N2 . Ru1 . C20 . 103.52(18) yes C15 . Ru1 . C20 . 36.02(16) yes C16 . Ru1 . C20 . 66.41(18) yes C17 . Ru1 . C18 . 37.21(18) yes C17 . Ru1 . C19 . 66.80(18) yes C18 . Ru1 . C19 . 36.88(17) yes C17 . Ru1 . C20 . 78.7(2) yes C18 . Ru1 . C20 . 66.65(18) yes C19 . Ru1 . C20 . 37.25(18) yes Ru1 . P1 . N1 . 88.24(13) yes Ru1 . P1 . C3 . 124.01(12) yes N1 . P1 . C3 . 105.9(2) yes Ru1 . P1 . C9 . 121.46(14) yes N1 . P1 . C9 . 110.0(2) yes C3 . P1 . C9 . 104.2(2) yes P1 . N1 . N2 . 106.4(3) yes P1 . N1 . H1 . 126(3) yes N2 . N1 . H1 . 119(3) yes Ru1 . N2 . N1 . 97.2(2) yes Ru1 . N2 . C1 . 119.5(3) yes N1 . N2 . C1 . 108.3(4) yes Ru1 . N2 . C2 . 113.5(3) yes N1 . N2 . C2 . 109.0(3) yes C1 . N2 . C2 . 108.4(4) yes N2 . C1 . H11 . 109.466 no N2 . C1 . H12 . 109.465 no H11 . C1 . H12 . 109.476 no N2 . C1 . H13 . 109.467 no H11 . C1 . H13 . 109.477 no H12 . C1 . H13 . 109.476 no N2 . C2 . H21 . 109.465 no N2 . C2 . H22 . 109.467 no H21 . C2 . H22 . 109.476 no N2 . C2 . H23 . 109.466 no H21 . C2 . H23 . 109.475 no H22 . C2 . H23 . 109.478 no P1 . C3 . C4 . 120.2(4) yes P1 . C3 . C8 . 120.3(4) yes C4 . C3 . C8 . 119.5(4) yes C3 . C4 . C5 . 120.5(4) yes C3 . C4 . H41 . 119.733 no C5 . C4 . H41 . 119.734 no C4 . C5 . C6 . 119.6(4) yes C4 . C5 . H51 . 120.209 no C6 . C5 . H51 . 120.209 no C5 . C6 . C7 . 119.8(4) yes C5 . C6 . H61 . 120.117 no C7 . C6 . H61 . 120.116 no C6 . C7 . C8 . 121.5(4) yes C6 . C7 . H71 . 119.242 no C8 . C7 . H71 . 119.241 no C3 . C8 . C7 . 119.1(4) yes C3 . C8 . H81 . 120.439 no C7 . C8 . H81 . 120.438 no P1 . C9 . C10 . 122.1(4) yes P1 . C9 . C14 . 118.5(4) yes C10 . C9 . C14 . 119.5(4) yes C9 . C10 . C11 . 120.5(5) yes C9 . C10 . H101 . 119.730 no C11 . C10 . H101 . 119.730 no C10 . C11 . C12 . 119.5(5) yes C10 . C11 . H111 . 120.232 no C12 . C11 . H111 . 120.232 no C11 . C12 . C13 . 121.2(5) yes C11 . C12 . H121 . 119.417 no C13 . C12 . H121 . 119.416 no C12 . C13 . C14 . 119.3(6) yes C12 . C13 . H131 . 120.331 no C14 . C13 . H131 . 120.331 no C9 . C14 . C13 . 119.9(5) yes C9 . C14 . H141 . 120.032 no C13 . C14 . H141 . 120.033 no Ru1 . C15 . C16 . 67.5(2) yes Ru1 . C15 . C20 . 71.1(2) yes C16 . C15 . C20 . 117.3(4) yes Ru1 . C15 . C21 . 131.6(3) yes C16 . C15 . C21 . 123.7(4) yes C20 . C15 . C21 . 119.0(4) yes Ru1 . C16 . C15 . 74.8(2) yes Ru1 . C16 . C17 . 71.0(2) yes C15 . C16 . C17 . 121.0(4) yes Ru1 . C16 . H161 . 126.596 no C15 . C16 . H161 . 119.508 no C17 . C16 . H161 . 119.508 no Ru1 . C17 . C16 . 71.4(2) yes Ru1 . C17 . C18 . 74.1(3) yes C16 . C17 . C18 . 121.4(4) yes Ru1 . C17 . H171 . 127.273 no C16 . C17 . H171 . 119.281 no C18 . C17 . H171 . 119.281 no Ru1 . C18 . C17 . 68.7(2) yes Ru1 . C18 . C19 . 69.5(2) yes C17 . C18 . C19 . 117.2(4) yes Ru1 . C18 . C24 . 132.7(3) yes C17 . C18 . C24 . 122.4(4) yes C19 . C18 . C24 . 120.3(4) yes Ru1 . C19 . C18 . 73.6(2) yes Ru1 . C19 . C20 . 73.7(2) yes C18 . C19 . C20 . 122.0(5) yes Ru1 . C19 . H191 . 125.504 no C18 . C19 . H191 . 118.998 no C20 . C19 . H191 . 118.997 no Ru1 . C20 . C15 . 72.9(2) yes Ru1 . C20 . C19 . 69.1(2) yes C15 . C20 . C19 . 120.7(5) yes Ru1 . C20 . H201 . 131.175 no C15 . C20 . H201 . 119.674 no C19 . C20 . H201 . 119.675 no C15 . C21 . C22 . 108.8(4) yes C15 . C21 . C23 . 114.0(5) yes C22 . C21 . C23 . 110.6(5) yes C15 . C21 . H211 . 107.201 no C22 . C21 . H211 . 110.857 no C23 . C21 . H211 . 105.310 no C21 . C22 . H221 . 109.467 no C21 . C22 . H222 . 109.466 no H221 . C22 . H222 . 109.476 no C21 . C22 . H223 . 109.467 no H221 . C22 . H223 . 109.475 no H222 . C22 . H223 . 109.476 no C21 . C23 . H231 . 109.469 no C21 . C23 . H232 . 109.466 no H231 . C23 . H232 . 109.476 no C21 . C23 . H233 . 109.467 no H231 . C23 . H233 . 109.475 no H232 . C23 . H233 . 109.474 no C18 . C24 . H241 . 109.466 no C18 . C24 . H242 . 109.466 no H241 . C24 . H242 . 109.475 no C18 . C24 . H243 . 109.467 no H241 . C24 . H243 . 109.476 no H242 . C24 . H243 . 109.477 no F1 . B1 . F2 . 106.2(5) yes F1 . B1 . F3 . 108.0(5) yes F2 . B1 . F3 . 115.9(7) yes F1 . B1 . F4 . 107.1(6) yes F2 . B1 . F4 . 109.2(5) yes F3 . B1 . F4 . 110.0(5) yes loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N1 H1 F1 0.89(5) 2.14(5) 2.954(5) 152(5) yes N1 H1 F2 0.89(5) 2.26(6) 3.034(5) 145(4) yes data_ARC1008 _database_code_depnum_ccdc_archive 'CCDC 255286' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; Coordinates, site occupancies and anisotropic displacement parameters were refined for the disordered carbon atoms. No geometric restraints were applied but similarity restraints were applied to the displacement parameters of disrectly-bonded pairs of atoms within the disordered isopropyl groups. The NH hydrogen atom was located in a difference Fourier map and its coordinates and isotropic displacement parameter subsequently refined. All other hydrogen atoms were positioned geometrically, the preferred orientations of the methyl group H271-H273 having been identified by examination of a difference Fourier map. ; #============================================================= _cell_length_a 29.8867(4) _cell_angle_alpha 90 _cell_length_b 10.3937(2) _cell_angle_beta 121.4595(7) _cell_length_c 23.4925(4) _cell_angle_gamma 90 _cell_volume 6224.88(19) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C28 H37 B Cl3 F4 N2 P Ru ' _chemical_formula_moiety ' C27 H35 Cl N2 P Ru, B F4, C H2 Cl2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 726.82 _cell_measurement_reflns_used 31308 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.859 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.89 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 31308 _reflns_number_total 7077 #7454 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min 5.111 _diffrn_reflns_theta_max 27.474 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.474 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -38 _reflns_limit_h_max 33 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _refine_diff_density_min -0.66 _refine_diff_density_max 1.06 _refine_ls_number_reflns 4437 _refine_ls_number_restraints 36 _refine_ls_number_parameters 431 #_refine_ls_R_factor_ref 0.0359 _refine_ls_wR_factor_ref 0.0409 _refine_ls_goodness_of_fit_ref 1.1179 #_reflns_number_all 7077 _refine_ls_R_factor_all 0.0690 _refine_ls_wR_factor_all 0.0743 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4437 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_gt 0.0409 _refine_ls_shift/su_max 0.008515 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.409 0.185 0.160 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group Ru1 Ru 0.339479(10) 0.65361(3) 0.299220(14) 0.0203 1.0000 Uani . . . . . Cl1 Cl 0.25717(3) 0.54507(10) 0.23642(5) 0.0379 1.0000 Uani . . . . . P1 P 0.32765(3) 0.65724(9) 0.38888(4) 0.0213 1.0000 Uani . . . . . N1 N 0.35306(14) 0.5098(3) 0.40855(19) 0.0324 1.0000 Uani . . . . . N2 N 0.37073(11) 0.4793(3) 0.36345(14) 0.0223 1.0000 Uani . . . . . C1 C 0.42961(13) 0.4719(4) 0.39963(18) 0.0259 1.0000 Uani . . . . . C2 C 0.45311(14) 0.3629(4) 0.44919(18) 0.0294 1.0000 Uani . . . . . C3 C 0.43001(15) 0.2335(4) 0.4164(2) 0.0360 1.0000 Uani . . . . . C4 C 0.37034(16) 0.2401(4) 0.3804(2) 0.0359 1.0000 Uani . . . . . C5 C 0.34896(14) 0.3506(4) 0.33099(19) 0.0302 1.0000 Uani . . . . . C6 C 0.36553(14) 0.7662(4) 0.45772(18) 0.0258 1.0000 Uani . . . . . C7 C 0.40981(14) 0.7245(4) 0.51734(19) 0.0307 1.0000 Uani . . . . . C8 C 0.43777(15) 0.8115(5) 0.5685(2) 0.0388 1.0000 Uani . . . . . C9 C 0.42284(17) 0.9388(5) 0.5613(2) 0.0400 1.0000 Uani . . . . . C10 C 0.37853(18) 0.9818(4) 0.5023(2) 0.0370 1.0000 Uani . . . . . C11 C 0.34976(15) 0.8950(4) 0.45098(19) 0.0315 1.0000 Uani . . . . . C12 C 0.26568(12) 0.6564(4) 0.38545(16) 0.0232 1.0000 Uani . . . . . C13 C 0.2656(3) 0.6586(10) 0.4457(4) 0.0303 0.514(15) Uani . . P 1 1 C14 C 0.2194(3) 0.6603(11) 0.4453(5) 0.0366 0.514(15) Uani . . P 1 1 C63 C 0.2597(3) 0.5758(12) 0.4292(5) 0.0347 0.486(15) Uani . . P 1 2 C64 C 0.2119(4) 0.5772(13) 0.4258(5) 0.0407 0.486(15) Uani . . P 1 2 C15 C 0.17181(15) 0.6600(5) 0.3839(2) 0.0432 1.0000 Uani . . . . . C16 C 0.1700(4) 0.6654(12) 0.3262(6) 0.0369 0.514(15) Uani . . P 1 1 C17 C 0.2158(4) 0.6667(12) 0.3247(5) 0.0303 0.514(15) Uani . . P 1 1 C66 C 0.1800(5) 0.7333(17) 0.3399(7) 0.0484 0.486(15) Uani . . P 1 2 C67 C 0.2275(4) 0.7307(16) 0.3419(6) 0.0378 0.486(15) Uani . . P 1 2 C18 C 0.32670(17) 0.7190(5) 0.1988(2) 0.0435 1.0000 Uani . U . . . C19 C 0.31461(16) 0.8170(4) 0.2306(2) 0.0392 1.0000 Uani . . . . . C20 C 0.35179(16) 0.8592(4) 0.2952(2) 0.0348 1.0000 Uani . . . . . C21 C 0.40244(15) 0.8045(4) 0.3311(2) 0.0298 1.0000 Uani . . . . . C22 C 0.41240(14) 0.6998(4) 0.3012(2) 0.0280 1.0000 Uani . . . . . C23 C 0.37573(16) 0.6579(4) 0.2355(2) 0.0335 1.0000 Uani . . . . . C24 C 0.2816(4) 0.6967(12) 0.1290(5) 0.0642 0.687(14) Uani . U P 2 1 C25 C 0.2876(4) 0.5686(14) 0.1036(5) 0.0719 0.687(14) Uani . U P 2 1 C26 C 0.2787(4) 0.8055(13) 0.0843(4) 0.0989 0.687(14) Uani . U P 2 1 C74 C 0.2959(8) 0.647(2) 0.1271(9) 0.0460 0.313(14) Uani . U P 2 2 C75 C 0.3033(6) 0.5013(15) 0.1219(7) 0.0317 0.313(14) Uani . U P 2 2 C76 C 0.2414(7) 0.701(2) 0.0941(8) 0.0605 0.313(14) Uani . U P 2 2 C27 C 0.44388(18) 0.8559(5) 0.3978(2) 0.0450 1.0000 Uani . . . . . B1 B 0.42645(18) 0.3577(5) 0.5916(2) 0.0342 1.0000 Uani . . . . . F1 F 0.38016(10) 0.3811(3) 0.53294(13) 0.0603 1.0000 Uani . . . . . F2 F 0.44582(14) 0.2391(3) 0.58688(19) 0.0728 1.0000 Uani . . . . . F3 F 0.46425(10) 0.4483(3) 0.60048(12) 0.0445 1.0000 Uani . . . . . F4 F 0.42130(11) 0.3550(3) 0.64577(13) 0.0585 1.0000 Uani . . . . . C28 C 0.5000 0.8828(7) 0.2500 0.0575 1.0000 Uani S T . . . Cl2 Cl 0.55034(7) 0.97626(17) 0.25600(10) 0.0809 1.0000 Uani . . . . . C29 C 0.5000 0.4321(6) 0.2500 0.0400 1.0000 Uani S T . . . Cl3 Cl 0.54799(5) 0.34015(15) 0.24873(8) 0.0682 1.0000 Uani . . . . . H1 H 0.362(2) 0.471(5) 0.443(3) 0.047(15) 1.0000 Uiso . . . . . H11 H 0.4443 0.5547 0.4241 0.0289 1.0000 Uiso . . . . . H12 H 0.4400 0.4607 0.3658 0.0289 1.0000 Uiso . . . . . H21 H 0.4919 0.3611 0.4684 0.0332 1.0000 Uiso . . . . . H22 H 0.4459 0.3776 0.4857 0.0332 1.0000 Uiso . . . . . H31 H 0.4433 0.1649 0.4513 0.0408 1.0000 Uiso . . . . . H32 H 0.4407 0.2132 0.3835 0.0408 1.0000 Uiso . . . . . H41 H 0.3599 0.2526 0.4141 0.0398 1.0000 Uiso . . . . . H42 H 0.3553 0.1575 0.3560 0.0398 1.0000 Uiso . . . . . H51 H 0.3583 0.3356 0.2964 0.0337 1.0000 Uiso . . . . . H52 H 0.3099 0.3527 0.3093 0.0337 1.0000 Uiso . . . . . H71 H 0.4211 0.6325 0.5228 0.0369 1.0000 Uiso . . . . . H81 H 0.4692 0.7817 0.6112 0.0449 1.0000 Uiso . . . . . H91 H 0.4438 1.0009 0.5984 0.0500 1.0000 Uiso . . . . . H101 H 0.3677 1.0741 0.4972 0.0487 1.0000 Uiso . . . . . H111 H 0.3176 0.9246 0.4090 0.0391 1.0000 Uiso . . . . . H131 H 0.2997 0.6589 0.4893 0.0390 0.5137 Uiso . . . 1 1 H141 H 0.2198 0.6617 0.4882 0.0502 0.5137 Uiso . . . 1 1 H631 H 0.2890 0.5191 0.4618 0.0421 0.4863 Uiso . . . 1 2 H641 H 0.2063 0.5165 0.4545 0.0540 0.4863 Uiso . . . 1 2 H151 H 0.1382 0.6556 0.3834 0.0570 1.0000 Uiso . . . . . H161 H 0.1353 0.6686 0.2834 0.0446 0.5137 Uiso . . . 1 1 H171 H 0.2140 0.6748 0.2811 0.0358 0.5137 Uiso . . . 1 1 H661 H 0.1510 0.7890 0.3062 0.0579 0.4863 Uiso . . . 1 2 H671 H 0.2324 0.7849 0.3104 0.0468 0.4863 Uiso . . . 1 2 H191 H 0.2789 0.8568 0.2065 0.0475 1.0000 Uiso . . . . . H201 H 0.3422 0.9293 0.3161 0.0475 1.0000 Uiso . . . . . H221 H 0.4466 0.6533 0.3273 0.0374 1.0000 Uiso . . . . . H231 H 0.3847 0.5853 0.2153 0.0471 1.0000 Uiso . . . . . H241 H 0.2481 0.6949 0.1289 0.0734 0.6869 Uiso . . . 2 1 H251 H 0.2573 0.5547 0.0571 0.0839 0.6869 Uiso . . . 2 1 H252 H 0.3210 0.5677 0.1036 0.0839 0.6869 Uiso . . . 2 1 H253 H 0.2883 0.4984 0.1332 0.0839 0.6869 Uiso . . . 2 1 H261 H 0.2486 0.7904 0.0379 0.1067 0.6869 Uiso . . . 2 1 H262 H 0.3120 0.8090 0.0842 0.1067 0.6869 Uiso . . . 2 1 H263 H 0.2735 0.8888 0.1014 0.1067 0.6869 Uiso . . . 2 1 H741 H 0.3131 0.6670 0.1013 0.0524 0.3131 Uiso . . . 2 2 H751 H 0.2814 0.4737 0.0742 0.0393 0.3131 Uiso . . . 2 2 H752 H 0.3410 0.4830 0.1388 0.0393 0.3131 Uiso . . . 2 2 H753 H 0.2922 0.4528 0.1492 0.0393 0.3131 Uiso . . . 2 2 H761 H 0.2194 0.6611 0.0489 0.0668 0.3131 Uiso . . . 2 2 H762 H 0.2426 0.7960 0.0894 0.0668 0.3131 Uiso . . . 2 2 H763 H 0.2259 0.6805 0.1218 0.0668 0.3131 Uiso . . . 2 2 H271 H 0.4647 0.9235 0.3915 0.0566 1.0000 Uiso . . . . . H272 H 0.4677 0.7842 0.4255 0.0566 1.0000 Uiso . . . . . H273 H 0.4269 0.8941 0.4210 0.0566 1.0000 Uiso . . . . . H281 H 0.5144 0.8272 0.2906 0.0603 1.0000 Uiso . . . . . H291 H 0.5172 0.4876 0.2907 0.0507 1.0000 Uiso . . . . . 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 0.01687(12) 0.02044(13) 0.02509(14) 0.00103(13) 0.01207(10) 0.00055(13) Cl1 0.0202(4) 0.0378(5) 0.0426(6) 0.0087(4) 0.0072(4) -0.0058(4) P1 0.0195(4) 0.0217(4) 0.0262(4) 0.0026(4) 0.0143(3) 0.0022(4) N1 0.047(2) 0.0269(17) 0.0390(19) 0.0089(15) 0.0330(17) 0.0113(15) N2 0.0206(14) 0.0211(14) 0.0273(15) -0.0011(12) 0.0140(12) 0.0010(12) C1 0.0172(15) 0.0256(18) 0.0295(19) 0.0006(15) 0.0084(14) 0.0014(14) C2 0.0221(16) 0.032(2) 0.0290(18) 0.0028(16) 0.0098(14) 0.0032(16) C3 0.0299(19) 0.029(2) 0.043(2) 0.0012(18) 0.0147(18) 0.0055(17) C4 0.033(2) 0.0201(18) 0.046(2) -0.0001(17) 0.0151(18) -0.0006(16) C5 0.0242(16) 0.0245(17) 0.0355(19) -0.0053(17) 0.0112(15) -0.0056(16) C6 0.0231(16) 0.0293(19) 0.0283(18) -0.0006(15) 0.0157(15) -0.0014(15) C7 0.0209(16) 0.041(2) 0.030(2) 0.0030(17) 0.0135(15) 0.0000(16) C8 0.0271(19) 0.054(3) 0.031(2) 0.0011(19) 0.0122(17) -0.0058(18) C9 0.039(2) 0.055(3) 0.031(2) -0.013(2) 0.0218(18) -0.018(2) C10 0.049(2) 0.032(2) 0.041(2) -0.0077(18) 0.031(2) -0.0086(19) C11 0.034(2) 0.033(2) 0.030(2) -0.0021(17) 0.0191(17) -0.0016(17) C12 0.0219(15) 0.0252(16) 0.0255(16) 0.0014(16) 0.0145(14) -0.0003(16) C13 0.036(4) 0.026(5) 0.035(4) -0.001(4) 0.023(3) -0.003(4) C14 0.043(4) 0.036(6) 0.046(5) 0.000(4) 0.034(4) -0.003(4) C63 0.023(4) 0.047(8) 0.035(5) 0.015(5) 0.016(4) 0.005(4) C64 0.038(5) 0.053(8) 0.044(5) 0.009(5) 0.031(4) -0.005(5) C15 0.0286(19) 0.058(3) 0.056(3) 0.010(2) 0.0309(19) 0.002(2) C16 0.017(4) 0.033(5) 0.061(6) 0.009(5) 0.021(4) 0.001(4) C17 0.021(4) 0.039(5) 0.029(4) -0.001(4) 0.012(3) -0.003(4) C66 0.024(5) 0.063(9) 0.058(7) 0.032(7) 0.021(5) 0.019(6) C67 0.018(4) 0.069(9) 0.029(5) 0.015(6) 0.015(4) 0.002(5) C18 0.043(2) 0.059(3) 0.0260(19) 0.0086(19) 0.0168(18) -0.014(2) C19 0.0305(19) 0.035(2) 0.054(3) 0.0259(19) 0.0227(19) 0.0087(17) C20 0.037(2) 0.0198(18) 0.062(3) 0.0049(18) 0.036(2) -0.0004(16) C21 0.0285(18) 0.0302(18) 0.037(2) 0.0002(16) 0.0218(17) -0.0078(15) C22 0.0228(16) 0.0299(18) 0.041(2) 0.0043(16) 0.0231(16) 0.0000(15) C23 0.046(2) 0.0330(19) 0.039(2) -0.0054(19) 0.0342(19) -0.009(2) C24 0.061(5) 0.090(6) 0.032(3) 0.002(4) 0.018(3) -0.020(4) C25 0.072(6) 0.097(8) 0.041(5) -0.016(5) 0.025(4) -0.035(6) C26 0.093(6) 0.134(8) 0.039(4) 0.026(5) 0.014(4) -0.023(6) C74 0.051(6) 0.055(7) 0.025(5) -0.005(5) 0.015(5) 0.011(5) C75 0.044(7) 0.033(7) 0.021(6) 0.005(5) 0.019(5) 0.009(5) C76 0.053(8) 0.075(9) 0.039(7) 0.001(7) 0.014(6) -0.003(7) C27 0.045(2) 0.049(3) 0.047(2) -0.014(2) 0.029(2) -0.027(2) B1 0.036(2) 0.039(2) 0.029(2) -0.001(2) 0.0183(18) -0.004(2) F1 0.0348(13) 0.101(2) 0.0364(14) 0.0247(15) 0.0121(11) 0.0016(15) F2 0.090(2) 0.0420(16) 0.096(3) -0.0060(17) 0.055(2) 0.0071(17) F3 0.0428(13) 0.0507(15) 0.0449(14) -0.0008(12) 0.0262(12) -0.0088(12) F4 0.0595(17) 0.088(2) 0.0401(14) 0.0050(15) 0.0343(13) -0.0054(17) C28 0.068(5) 0.038(4) 0.045(4) 0.0000 0.014(4) 0.0000 Cl2 0.0900(11) 0.0749(10) 0.1044(12) -0.0309(9) 0.0692(11) -0.0169(9) C29 0.037(3) 0.040(3) 0.049(4) 0.0000 0.027(3) 0.0000 Cl3 0.0445(6) 0.0671(9) 0.0999(11) -0.0064(8) 0.0426(7) 0.0101(7) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . C23 . 2.260(3) yes Ru1 . C22 . 2.208(3) yes Ru1 . C21 . 2.256(4) yes Ru1 . C20 . 2.179(4) yes Ru1 . C19 . 2.187(4) yes Ru1 . C18 . 2.288(4) yes Ru1 . N2 . 2.227(3) yes Ru1 . P1 . 2.3109(9) yes Ru1 . Cl1 . 2.3901(9) yes P1 . C12 . 1.811(3) yes P1 . C6 . 1.808(4) yes P1 . N1 . 1.665(3) yes N1 . H1 . 0.81(5) no N1 . N2 . 1.444(4) yes N2 . C5 . 1.508(5) yes N2 . C1 . 1.505(4) yes C1 . H12 . 1.000 no C1 . H11 . 1.000 no C1 . C2 . 1.510(5) yes C2 . H22 . 1.000 no C2 . H21 . 1.000 no C2 . C3 . 1.524(5) yes C3 . H32 . 1.000 no C3 . H31 . 1.000 no C3 . C4 . 1.525(5) yes C4 . H42 . 1.000 no C4 . H41 . 1.000 no C4 . C5 . 1.517(6) yes C5 . H52 . 1.000 no C5 . H51 . 1.000 no C6 . C11 . 1.401(5) yes C6 . C7 . 1.402(5) yes C7 . H71 . 1.000 no C7 . C8 . 1.383(6) yes C8 . H81 . 1.000 no C8 . C9 . 1.378(7) yes C9 . H91 . 1.000 no C9 . C10 . 1.399(6) yes C10 . H101 . 1.000 no C10 . C11 . 1.387(6) yes C11 . H111 . 1.000 no C12 . C17 . 1.432(10) yes C12 . C13 . 1.417(8) yes C12 . C67 . 1.314(11) yes C12 . C63 . 1.408(9) yes C13 . H131 . 1.000 no C13 . C14 . 1.375(11) yes C14 . H141 . 1.000 no C14 . C15 . 1.402(10) yes C63 . H631 . 1.000 no C63 . C64 . 1.389(11) yes C64 . H641 . 1.000 no C64 . C15 . 1.384(11) yes C15 . H151 . 1.000 no C15 . C16 . 1.328(13) yes C15 . H151 . 1.000 no C15 . C66 . 1.404(13) yes C16 . H161 . 1.000 no C16 . C17 . 1.388(13) yes C17 . H171 . 1.000 no C66 . H661 . 1.000 no C66 . C67 . 1.395(14) yes C67 . H671 . 1.000 no C18 . C24 . 1.500(10) yes C18 . C23 . 1.405(6) yes C18 . C19 . 1.417(7) yes C18 . C74 . 1.62(2) yes C18 . C23 . 1.405(6) yes C18 . C19 . 1.417(7) yes C19 . H191 . 1.000 no C19 . C20 . 1.403(6) yes C20 . H201 . 1.000 no C20 . C21 . 1.412(5) yes C21 . C27 . 1.499(6) yes C21 . C22 . 1.410(5) yes C22 . H221 . 1.000 no C22 . C23 . 1.417(6) yes C23 . H231 . 1.000 no C24 . H241 . 1.000 no C24 . C26 . 1.515(14) yes C24 . C25 . 1.508(16) yes C25 . H253 . 1.000 no C25 . H252 . 1.000 no C25 . H251 . 1.000 no C26 . H263 . 1.000 no C26 . H262 . 1.000 no C26 . H261 . 1.000 no C74 . H741 . 1.000 no C74 . C76 . 1.50(3) yes C74 . C75 . 1.55(2) yes C75 . H753 . 1.000 no C75 . H752 . 1.000 no C75 . H751 . 1.000 no C76 . H763 . 1.000 no C76 . H762 . 1.000 no C76 . H761 . 1.000 no C27 . H273 . 1.000 no C27 . H272 . 1.000 no C27 . H271 . 1.000 no B1 . F4 . 1.360(5) yes B1 . F3 . 1.400(5) yes B1 . F2 . 1.390(6) yes B1 . F1 . 1.372(5) yes C28 . H281 . 1.000 no C28 . Cl2 . 1.734(4) yes C28 . Cl2 5_655 1.734(4) yes C28 . H281 5_655 1.000 no C29 . H291 . 1.000 no C29 . Cl3 . 1.737(4) yes C29 . Cl3 5_655 1.737(4) yes C29 . H291 5_655 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C23 . Ru1 . C22 . 36.94(14) yes C23 . Ru1 . C21 . 66.51(14) yes C22 . Ru1 . C21 . 36.80(14) yes C23 . Ru1 . C20 . 78.54(15) yes C22 . Ru1 . C20 . 66.45(14) yes C21 . Ru1 . C20 . 37.07(14) yes C23 . Ru1 . C19 . 65.94(16) yes C22 . Ru1 . C19 . 78.39(14) yes C21 . Ru1 . C19 . 66.98(15) yes C20 . Ru1 . C19 . 37.50(17) yes C23 . Ru1 . C18 . 35.98(16) yes C22 . Ru1 . C18 . 65.72(15) yes C21 . Ru1 . C18 . 78.33(15) yes C20 . Ru1 . C18 . 66.73(17) yes C19 . Ru1 . C18 . 36.84(18) yes C23 . Ru1 . N2 . 106.76(13) yes C22 . Ru1 . N2 . 95.87(12) yes C21 . Ru1 . N2 . 110.99(12) yes C20 . Ru1 . N2 . 143.78(14) yes C19 . Ru1 . N2 . 172.70(14) yes C23 . Ru1 . P1 . 163.23(11) yes C22 . Ru1 . P1 . 126.59(10) yes C21 . Ru1 . P1 . 100.57(10) yes C20 . Ru1 . P1 . 97.67(11) yes C19 . Ru1 . P1 . 120.30(13) yes C23 . Ru1 . Cl1 . 107.17(11) yes C22 . Ru1 . Cl1 . 143.33(11) yes C21 . Ru1 . Cl1 . 160.82(10) yes C20 . Ru1 . Cl1 . 125.37(11) yes C19 . Ru1 . Cl1 . 93.84(11) yes C18 . Ru1 . N2 . 136.51(15) yes C18 . Ru1 . P1 . 155.87(14) yes N2 . Ru1 . P1 . 66.75(8) yes C18 . Ru1 . Cl1 . 86.53(11) yes N2 . Ru1 . Cl1 . 88.10(8) yes P1 . Ru1 . Cl1 . 88.43(4) yes C12 . P1 . C6 . 101.03(16) yes C12 . P1 . N1 . 108.39(17) yes C6 . P1 . N1 . 110.25(18) yes C12 . P1 . Ru1 . 126.77(11) yes C6 . P1 . Ru1 . 120.22(12) yes N1 . P1 . Ru1 . 88.48(12) yes H1 . N1 . N2 . 123(4) no H1 . N1 . P1 . 127(4) no N2 . N1 . P1 . 106.7(2) yes C5 . N2 . C1 . 108.0(3) yes C5 . N2 . N1 . 109.8(3) yes C1 . N2 . N1 . 111.4(3) yes C5 . N2 . Ru1 . 117.5(2) yes C1 . N2 . Ru1 . 112.2(2) yes N1 . N2 . Ru1 . 97.67(19) yes H12 . C1 . H11 . 109.467 no H12 . C1 . C2 . 108.276 no H11 . C1 . C2 . 108.276 no H12 . C1 . N2 . 108.276 no H11 . C1 . N2 . 108.276 no C2 . C1 . N2 . 114.2(3) yes H22 . C2 . H21 . 109.467 no H22 . C2 . C3 . 108.964 no H21 . C2 . C3 . 108.964 no H22 . C2 . C1 . 108.965 no H21 . C2 . C1 . 108.965 no C3 . C2 . C1 . 111.5(3) yes H32 . C3 . H31 . 109.467 no H32 . C3 . C4 . 109.507 no H31 . C3 . C4 . 109.507 no H32 . C3 . C2 . 109.507 no H31 . C3 . C2 . 109.507 no C4 . C3 . C2 . 109.3(3) yes H42 . C4 . H41 . 109.467 no H42 . C4 . C5 . 109.045 no H41 . C4 . C5 . 109.045 no H42 . C4 . C3 . 109.045 no H41 . C4 . C3 . 109.045 no C5 . C4 . C3 . 111.2(3) yes H52 . C5 . H51 . 109.467 no H52 . C5 . N2 . 108.656 no H51 . C5 . N2 . 108.656 no H52 . C5 . C4 . 108.656 no H51 . C5 . C4 . 108.656 no N2 . C5 . C4 . 112.7(3) yes C11 . C6 . C7 . 119.6(4) yes C11 . C6 . P1 . 118.7(3) yes C7 . C6 . P1 . 121.6(3) yes H71 . C7 . C8 . 120.213 no H71 . C7 . C6 . 120.213 no C8 . C7 . C6 . 119.6(4) yes H81 . C8 . C9 . 119.645 no H81 . C8 . C7 . 119.645 no C9 . C8 . C7 . 120.7(4) yes H91 . C9 . C10 . 119.785 no H91 . C9 . C8 . 119.785 no C10 . C9 . C8 . 120.4(4) yes H101 . C10 . C11 . 120.313 no H101 . C10 . C9 . 120.312 no C11 . C10 . C9 . 119.4(4) yes H111 . C11 . C10 . 119.871 no H111 . C11 . C6 . 119.871 no C10 . C11 . C6 . 120.3(4) yes C17 . C12 . C13 . 116.8(5) yes C17 . C12 . P1 . 123.5(4) yes C13 . C12 . P1 . 119.4(4) yes C67 . C12 . C63 . 121.9(6) yes C67 . C12 . P1 . 118.9(5) yes C63 . C12 . P1 . 119.2(4) yes H131 . C13 . C14 . 119.345 no H131 . C13 . C12 . 119.345 no C14 . C13 . C12 . 121.3(7) yes H141 . C14 . C15 . 120.605 no H141 . C14 . C13 . 120.605 no C15 . C14 . C13 . 118.8(7) yes H631 . C63 . C64 . 120.952 no H631 . C63 . C12 . 120.952 no C64 . C63 . C12 . 118.1(7) yes H641 . C64 . C15 . 119.027 no H641 . C64 . C63 . 119.026 no C15 . C64 . C63 . 121.9(7) yes H151 . C15 . C16 . 119.021 no H151 . C15 . C14 . 119.021 no C16 . C15 . C14 . 122.0(6) yes H151 . C15 . C66 . 125.261 no H151 . C15 . C64 . 118.055 no C66 . C15 . C64 . 116.3(6) yes H161 . C16 . C17 . 119.627 no H161 . C16 . C15 . 119.627 no C17 . C16 . C15 . 120.7(9) yes H171 . C17 . C16 . 119.970 no H171 . C17 . C12 . 119.970 no C16 . C17 . C12 . 120.1(8) yes H661 . C66 . C67 . 118.971 no H661 . C66 . C15 . 118.971 no C67 . C66 . C15 . 122.1(9) yes H671 . C67 . C12 . 120.291 no H671 . C67 . C66 . 120.290 no C12 . C67 . C66 . 119.4(9) yes C24 . C18 . C23 . 131.0(7) yes C24 . C18 . C19 . 110.8(6) yes C23 . C18 . C19 . 118.2(4) yes C24 . C18 . Ru1 . 130.7(4) yes C23 . C18 . Ru1 . 70.9(2) yes C19 . C18 . Ru1 . 67.7(2) yes C74 . C18 . C23 . 106.0(8) yes C74 . C18 . C19 . 135.7(8) yes C23 . C18 . C19 . 118.2(4) yes C74 . C18 . Ru1 . 129.4(8) yes C23 . C18 . Ru1 . 70.9(2) yes C19 . C18 . Ru1 . 67.7(2) yes H191 . C19 . C20 . 119.371 no H191 . C19 . C18 . 119.372 no C20 . C19 . C18 . 121.3(4) yes H191 . C19 . Ru1 . 126.125 no C20 . C19 . Ru1 . 70.9(2) yes C18 . C19 . Ru1 . 75.4(2) yes H201 . C20 . C21 . 119.400 no H201 . C20 . C19 . 119.401 no C21 . C20 . C19 . 121.2(4) yes H201 . C20 . Ru1 . 126.495 no C21 . C20 . Ru1 . 74.5(2) yes C19 . C20 . Ru1 . 71.6(2) yes C27 . C21 . C22 . 121.5(4) yes C27 . C21 . C20 . 121.7(4) yes C22 . C21 . C20 . 116.8(4) yes C27 . C21 . Ru1 . 133.3(3) yes C22 . C21 . Ru1 . 69.8(2) yes C20 . C21 . Ru1 . 68.5(2) yes H221 . C22 . C23 . 118.796 no H221 . C22 . C21 . 118.795 no C23 . C22 . C21 . 122.4(3) yes H221 . C22 . Ru1 . 126.149 no C23 . C22 . Ru1 . 73.5(2) yes C21 . C22 . Ru1 . 73.5(2) yes H231 . C23 . C18 . 120.121 no H231 . C23 . C22 . 120.122 no C18 . C23 . C22 . 119.8(4) yes H231 . C23 . Ru1 . 129.688 no C18 . C23 . Ru1 . 73.1(2) yes C22 . C23 . Ru1 . 69.53(19) yes H241 . C24 . C26 . 108.481 no H241 . C24 . C25 . 107.952 no C26 . C24 . C25 . 111.1(10) yes H241 . C24 . C18 . 109.527 no C26 . C24 . C18 . 109.6(8) yes C25 . C24 . C18 . 110.1(9) yes H253 . C25 . H252 . 109.477 no H253 . C25 . H251 . 109.476 no H252 . C25 . H251 . 109.476 no H253 . C25 . C24 . 109.466 no H252 . C25 . C24 . 109.467 no H251 . C25 . C24 . 109.466 no H263 . C26 . H262 . 109.468 no H263 . C26 . H261 . 109.470 no H262 . C26 . H261 . 109.480 no H263 . C26 . C24 . 109.466 no H262 . C26 . C24 . 109.471 no H261 . C26 . C24 . 109.472 no H741 . C74 . C76 . 111.951 no H741 . C74 . C75 . 90.745 no C76 . C74 . C75 . 118.9(18) yes H741 . C74 . C18 . 110.044 no C76 . C74 . C18 . 104.1(14) yes C75 . C74 . C18 . 120.4(13) yes H753 . C75 . H752 . 109.477 no H753 . C75 . H751 . 109.476 no H752 . C75 . H751 . 109.476 no H753 . C75 . C74 . 109.469 no H752 . C75 . C74 . 109.463 no H751 . C75 . C74 . 109.466 no H763 . C76 . H762 . 109.476 no H763 . C76 . H761 . 109.477 no H762 . C76 . H761 . 109.475 no H763 . C76 . C74 . 109.469 no H762 . C76 . C74 . 109.463 no H761 . C76 . C74 . 109.466 no H273 . C27 . H272 . 109.476 no H273 . C27 . H271 . 109.476 no H272 . C27 . H271 . 109.476 no H273 . C27 . C21 . 109.467 no H272 . C27 . C21 . 109.467 no H271 . C27 . C21 . 109.467 no F4 . B1 . F3 . 110.5(4) yes F4 . B1 . F2 . 108.1(4) yes F3 . B1 . F2 . 105.8(4) yes F4 . B1 . F1 . 113.3(4) yes F3 . B1 . F1 . 110.1(4) yes F2 . B1 . F1 . 108.7(4) yes H281 . C28 . Cl2 . 108.879 no H281 . C28 . Cl2 5_655 108.880 no Cl2 . C28 . Cl2 5_655 111.8(4) yes H281 . C28 . H281 5_655 109.467 no Cl2 . C28 . H281 5_655 108.879 no Cl2 5_655 C28 . H281 5_655 108.879 no H291 . C29 . Cl3 . 108.522 no H291 . C29 . Cl3 5_655 108.522 no Cl3 . C29 . Cl3 5_655 113.2(4) yes H291 . C29 . H291 5_655 109.466 no Cl3 . C29 . H291 5_655 108.522 no Cl3 5_655 C29 . H291 5_655 108.522 no loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N1 H1 F1 0.81(5) 2.11(5) 2.918(4) 173(5) yes data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 255287' _audit_creation_date 02-28-01 _audit_creation_method CRYSTALS_ver_12-03-99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 18.6983(7) _cell_angle_alpha 90 _cell_length_b 13.3095(5) _cell_angle_beta 91.6690(16) _cell_length_c 21.6881(9) _cell_angle_gamma 90 _cell_volume 5395.1(4) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C58 H55 Cl2 N5 O1 P3 Re1 ' _chemical_formula_moiety ' C52 H46 Cl2 N2 O P3 Re, 3(C2 H3 N) ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1188.14 _cell_measurement_reflns_used 28344 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' green ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2396.025 _exptl_absorpt_coefficient_mu 2.485 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.91 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 28344 _reflns_number_total 11979 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_gt 6747 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 27.43 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -24 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -1.73 _refine_diff_density_max 0.87 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6747 _refine_ls_number_parameters 618 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.0583 _refine_ls_goodness_of_fit_ref 1.0666 _refine_ls_shift/su_max 0.01132 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin (1979) 2.41 0.540 2.04 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _refine_special_details ; Two of the solvent molecules have been modelled as disordered over two sites. The coordinates of the C and N atoms have been refined subject to geometric restraint of C-N bonds to 1.13(1) A, C-C to 1.45(1) and N-C-C angle to 180 deg. A common isotropic thermal parameter has been refined for all four N atoms, and similarly for all four C(nitrile and four all four C(methyl) atoms. Site occupancies have been refined for each position, subject to a constraint of the sum of the occupancies of each pair of sites to 1 All hydrogen atoms were positioned geometrically, the preferred orientations of the methyl groups having been identified by examination of a difference Fourier map ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_disorder_assembly _atom_site_disorder_group Re1 0.339833(15) 0.03639(2) 0.605323(13) 0.0233 1.0000 Uani . . Cl1 0.2790(1) -0.11048(15) 0.64892(9) 0.0344 1.0000 Uani . . Cl2 0.4107(1) -0.07130(15) 0.54176(9) 0.0322 1.0000 Uani . . N1 0.3773(3) 0.1561(5) 0.5835(3) 0.0289 1.0000 Uani . . C1 0.4017(4) 0.2426(6) 0.5707(4) 0.0318 1.0000 Uani . . C2 0.4676(5) 0.2526(7) 0.5316(4) 0.0422 1.0000 Uani . . P1 0.35461(11) 0.34903(15) 0.60088(11) 0.0332 1.0000 Uani . . O1 0.2784(3) 0.3277(4) 0.6142(3) 0.0417 1.0000 Uani . . C3 0.4023(5) 0.3923(6) 0.6688(5) 0.0405 1.0000 Uani . . C4 0.3646(5) 0.4148(7) 0.7213(4) 0.0441 1.0000 Uani . . C5 0.4003(6) 0.4446(6) 0.7750(5) 0.0474 1.0000 Uani . . C6 0.4742(7) 0.4529(8) 0.7763(5) 0.0567 1.0000 Uani . . C7 0.5127(6) 0.4292(8) 0.7258(6) 0.0543 1.0000 Uani . . C8 0.4771(5) 0.4011(8) 0.6705(5) 0.0470 1.0000 Uani . . C9 0.3626(4) 0.4484(6) 0.5449(5) 0.0377 1.0000 Uani . . C10 0.3755(5) 0.5484(7) 0.5626(5) 0.0452 1.0000 Uani . . C11 0.3742(6) 0.6236(8) 0.5175(6) 0.0549 1.0000 Uani . . C12 0.3645(6) 0.5996(8) 0.4573(6) 0.0584 1.0000 Uani . . C13 0.3518(6) 0.5014(9) 0.4386(5) 0.0533 1.0000 Uani . . C14 0.3513(5) 0.4261(8) 0.4814(5) 0.0466 1.0000 Uani . . N2 0.2700(3) 0.1049(5) 0.6631(3) 0.0261 1.0000 Uani . . C15 0.2316(4) 0.1471(6) 0.6933(4) 0.0325 1.0000 Uani . . C16 0.1805(5) 0.1958(8) 0.7336(4) 0.0442 1.0000 Uani . . P2 0.4250(1) 0.01994(13) 0.69179(9) 0.0248 1.0000 Uani . . C17 0.5088(4) 0.0917(6) 0.6875(4) 0.0291 1.0000 Uani . . C18 0.5405(4) 0.1428(7) 0.7362(4) 0.0385 1.0000 Uani . . C19 0.6055(5) 0.1902(8) 0.7302(4) 0.0456 1.0000 Uani . . C20 0.6401(5) 0.1874(8) 0.6752(5) 0.0446 1.0000 Uani . . C21 0.6099(4) 0.1338(7) 0.6255(4) 0.0379 1.0000 Uani . . C22 0.5439(5) 0.0874(6) 0.6314(4) 0.0348 1.0000 Uani . . C23 0.4623(4) -0.1050(6) 0.7136(4) 0.0306 1.0000 Uani . . C24 0.5042(5) -0.1110(7) 0.7672(5) 0.0442 1.0000 Uani . . C25 0.5359(5) -0.2014(8) 0.7843(5) 0.0503 1.0000 Uani . . C26 0.5246(5) -0.2861(7) 0.7480(5) 0.0466 1.0000 Uani . . C27 0.4822(5) -0.2807(7) 0.6948(4) 0.0407 1.0000 Uani . . C28 0.4494(4) -0.1895(6) 0.6781(4) 0.0327 1.0000 Uani . . C29 0.3847(4) 0.0641(6) 0.7630(3) 0.0289 1.0000 Uani . . C30 0.3803(5) 0.1653(6) 0.7757(4) 0.0357 1.0000 Uani . . C31 0.3406(4) 0.2001(6) 0.8248(4) 0.0346 1.0000 Uani . . C32 0.3054(5) 0.1325(8) 0.8620(4) 0.0450 1.0000 Uani . . C33 0.3092(5) 0.0288(8) 0.8490(4) 0.0456 1.0000 Uani . . C34 0.3494(5) -0.0048(7) 0.7998(4) 0.0374 1.0000 Uani . . P3 0.2517(1) 0.04567(16) 0.52107(9) 0.0277 1.0000 Uani . . C35 0.2758(5) 0.1317(6) 0.4598(4) 0.0331 1.0000 Uani . . C36 0.3448(5) 0.1253(6) 0.4385(4) 0.0371 1.0000 Uani . . C37 0.3660(6) 0.1846(8) 0.3894(4) 0.0508 1.0000 Uani . . C38 0.3185(6) 0.2495(8) 0.3609(4) 0.0492 1.0000 Uani . . C39 0.2498(6) 0.2569(7) 0.3812(4) 0.0487 1.0000 Uani . . C40 0.2278(5) 0.1982(7) 0.4310(4) 0.0393 1.0000 Uani . . C41 0.2287(4) -0.0665(6) 0.4754(4) 0.0339 1.0000 Uani . . C42 0.1958(5) -0.0575(8) 0.4171(5) 0.0484 1.0000 Uani . . C43 0.1744(6) -0.1406(9) 0.3835(5) 0.0541 1.0000 Uani . . C44 0.1829(5) -0.2343(9) 0.4067(5) 0.0527 1.0000 Uani . . C45 0.2153(6) -0.2459(7) 0.4659(6) 0.0550 1.0000 Uani . . C46 0.2401(5) -0.1631(7) 0.4995(4) 0.0421 1.0000 Uani . . C47 0.1625(4) 0.0876(7) 0.5434(4) 0.0332 1.0000 Uani . . C48 0.1046(5) 0.0212(8) 0.5444(4) 0.0407 1.0000 Uani . . C49 0.0391(5) 0.0524(9) 0.5656(5) 0.0490 1.0000 Uani . . C50 0.0307(5) 0.1510(11) 0.5861(5) 0.0591 1.0000 Uani . . C51 0.0882(5) 0.2183(8) 0.5865(4) 0.0463 1.0000 Uani . . C52 0.1546(5) 0.1854(7) 0.5659(4) 0.0396 1.0000 Uani . . N3 0.3129(7) 0.4666(11) 0.2635(7) 0.0964 1.0000 Uani . . C53 0.2590(7) 0.5045(9) 0.2576(6) 0.0592 1.0000 Uani . . C54 0.1908(9) 0.5483(12) 0.2485(11) 0.1098 1.0000 Uani . . N4 0.069(4) 0.542(5) 0.414(3) 0.157(8) 0.29(2) Uiso 1 1 C55 0.106(3) 0.499(4) 0.446(3) 0.090(4) 0.29(2) Uiso 1 1 C56 0.155(4) 0.445(6) 0.488(4) 0.088(4) 0.29(2) Uiso 1 1 N104 0.1257(17) 0.496(2) 0.3826(11) 0.157(8) 0.71(2) Uiso 1 2 C155 0.1411(12) 0.4787(16) 0.432(1) 0.090(4) 0.71(2) Uiso 1 2 C156 0.1604(19) 0.457(3) 0.4959(11) 0.088(4) 0.71(2) Uiso 1 2 N5 0.061(2) 0.238(4) 0.3816(19) 0.157(8) 0.48(3) Uiso 2 1 C57 0.014(2) 0.257(3) 0.4119(16) 0.090(4) 0.48(3) Uiso 2 1 C58 -0.0445(17) 0.281(3) 0.4511(16) 0.088(4) 0.48(3) Uiso 2 1 N105 0.035(2) 0.193(3) 0.400(2) 0.157(8) 0.52(3) Uiso 2 2 C157 0.0094(15) 0.259(2) 0.4239(18) 0.090(4) 0.52(3) Uiso 2 2 C158 -0.0222(17) 0.343(2) 0.4548(15) 0.088(4) 0.52(3) Uiso 2 2 H21 0.4848 0.1843 0.5200 0.0509 1.0000 Uiso . . H22 0.5061 0.2885 0.5557 0.0509 1.0000 Uiso . . H23 0.4550 0.2916 0.4934 0.0509 1.0000 Uiso . . H41 0.3112 0.4093 0.7202 0.0533 1.0000 Uiso . . H51 0.3728 0.4601 0.8128 0.0570 1.0000 Uiso . . H61 0.4997 0.4766 0.8147 0.0678 1.0000 Uiso . . H71 0.5662 0.4319 0.7281 0.0650 1.0000 Uiso . . H81 0.5048 0.3876 0.6326 0.0564 1.0000 Uiso . . H101 0.3855 0.5656 0.6069 0.0542 1.0000 Uiso . . H111 0.3805 0.6955 0.5299 0.0660 1.0000 Uiso . . H121 0.3666 0.6538 0.4255 0.0699 1.0000 Uiso . . H131 0.3430 0.4858 0.3939 0.0638 1.0000 Uiso . . H141 0.3429 0.3551 0.4680 0.0556 1.0000 Uiso . . H161 0.1834 0.2703 0.7284 0.0534 1.0000 Uiso . . H162 0.1924 0.1779 0.7775 0.0534 1.0000 Uiso . . H163 0.1310 0.1724 0.7225 0.0534 1.0000 Uiso . . H181 0.5160 0.1456 0.7765 0.0462 1.0000 Uiso . . H191 0.6276 0.2270 0.7662 0.0545 1.0000 Uiso . . H201 0.6866 0.2234 0.6708 0.0535 1.0000 Uiso . . H211 0.6357 0.1290 0.5858 0.0455 1.0000 Uiso . . H221 0.5214 0.0507 0.5955 0.0417 1.0000 Uiso . . H241 0.5116 -0.0501 0.7936 0.0526 1.0000 Uiso . . H251 0.5668 -0.2055 0.8226 0.0600 1.0000 Uiso . . H261 0.5472 -0.3514 0.7604 0.0559 1.0000 Uiso . . H271 0.4750 -0.3416 0.6684 0.0490 1.0000 Uiso . . H281 0.4169 -0.1857 0.6407 0.0395 1.0000 Uiso . . H301 0.4060 0.2145 0.7494 0.0430 1.0000 Uiso . . H311 0.3375 0.2739 0.8333 0.0417 1.0000 Uiso . . H321 0.2775 0.1570 0.8977 0.0542 1.0000 Uiso . . H331 0.2832 -0.0206 0.8750 0.0548 1.0000 Uiso . . H341 0.3528 -0.0783 0.7908 0.0450 1.0000 Uiso . . H361 0.3797 0.0778 0.4586 0.0448 1.0000 Uiso . . H371 0.4161 0.1798 0.3747 0.0613 1.0000 Uiso . . H381 0.3339 0.2913 0.3254 0.0591 1.0000 Uiso . . H391 0.2152 0.3043 0.3605 0.0585 1.0000 Uiso . . H401 0.1779 0.2041 0.4458 0.0471 1.0000 Uiso . . H421 0.1875 0.0110 0.3993 0.0580 1.0000 Uiso . . H431 0.1522 -0.1315 0.3413 0.0644 1.0000 Uiso . . H441 0.1666 -0.2943 0.3823 0.0630 1.0000 Uiso . . H451 0.2204 -0.3147 0.4841 0.0661 1.0000 Uiso . . H461 0.2657 -0.1725 0.5402 0.0505 1.0000 Uiso . . H481 0.1106 -0.0494 0.5297 0.0488 1.0000 Uiso . . H491 -0.0021 0.0045 0.5662 0.0589 1.0000 Uiso . . H501 -0.0169 0.1738 0.6006 0.0709 1.0000 Uiso . . H511 0.0821 0.2888 0.6013 0.0555 1.0000 Uiso . . H521 0.1965 0.2321 0.5673 0.0476 1.0000 Uiso . . H541 0.1912 0.5936 0.2117 0.1307 1.0000 Uiso . . H542 0.1785 0.5882 0.2858 0.1307 1.0000 Uiso . . H543 0.1543 0.4943 0.2414 0.1307 1.0000 Uiso . . H561 0.1564 0.3726 0.4755 0.1059 0.29 Uiso 1 1 H562 0.1379 0.4506 0.5309 0.1059 0.29 Uiso 1 1 H563 0.2039 0.4745 0.4855 0.1059 0.29 Uiso 1 1 H1561 0.1802 0.5190 0.5161 0.1059 0.71 Uiso 1 2 H1562 0.1170 0.4345 0.5180 0.1059 0.71 Uiso 1 2 H1563 0.1973 0.4027 0.4976 0.1059 0.71 Uiso 1 2 H581 -0.0770 0.2217 0.4537 0.1059 0.48 Uiso 2 1 H582 -0.0256 0.2988 0.4933 0.1059 0.48 Uiso 2 1 H583 -0.0718 0.3395 0.4333 0.1059 0.48 Uiso 2 1 H1581 0.0110 0.4021 0.4533 0.1059 0.52 Uiso 2 2 H1582 -0.0307 0.3254 0.4988 0.1059 0.52 Uiso 2 2 H1583 -0.0688 0.3610 0.4337 0.1059 0.52 Uiso 2 2 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 Re1 0.02354(14) 0.02324(14) 0.02333(14) -0.00062(15) 0.00384(8) -0.00075(15) Cl1 0.034(1) 0.032(1) 0.038(1) 0.0057(8) 0.0050(8) -0.0065(8) Cl2 0.035(1) 0.0330(9) 0.0290(9) -0.0023(7) 0.0073(7) 0.0032(7) N1 0.028(3) 0.028(3) 0.031(3) -0.007(3) -0.001(3) 0.006(3) C1 0.028(4) 0.023(4) 0.044(5) 0.003(3) -0.000(3) -0.000(3) C2 0.042(5) 0.045(5) 0.041(5) 0.008(4) 0.014(4) 0.000(4) P1 0.0333(11) 0.0244(9) 0.0422(12) -0.0032(9) 0.0048(9) -0.0016(8) O1 0.039(3) 0.030(3) 0.057(4) -0.008(3) 0.010(3) -0.001(2) C3 0.049(5) 0.022(4) 0.050(5) -0.002(4) 0.002(4) 0.009(4) C4 0.059(6) 0.031(4) 0.043(5) 0.013(4) 0.017(4) 0.013(4) C5 0.071(7) 0.031(5) 0.041(5) 0.006(4) 0.009(4) 0.008(4) C6 0.082(8) 0.042(6) 0.045(5) 0.000(5) -0.008(5) 0.001(5) C7 0.044(5) 0.050(5) 0.068(7) -0.007(5) -0.006(5) 0.003(4) C8 0.039(5) 0.059(6) 0.043(5) 0.003(5) -0.001(4) 0.000(4) C9 0.027(4) 0.025(5) 0.061(6) 0.006(4) -0.003(4) -0.004(3) C10 0.048(5) 0.031(5) 0.057(6) -0.001(4) 0.002(4) 0.001(4) C11 0.053(6) 0.039(5) 0.073(8) 0.007(5) 0.008(5) -0.008(4) C12 0.044(6) 0.047(6) 0.083(9) 0.019(6) -0.002(5) 0.003(5) C13 0.056(6) 0.061(6) 0.043(6) 0.007(4) -0.003(5) 0.003(5) C14 0.042(5) 0.047(5) 0.050(6) 0.002(4) -0.008(4) -0.003(4) N2 0.021(3) 0.028(3) 0.029(3) -0.000(3) -0.001(2) 0.004(2) C15 0.029(4) 0.033(4) 0.035(4) 0.003(3) 0.002(3) -0.004(3) C16 0.040(5) 0.051(5) 0.043(5) -0.008(4) 0.013(4) 0.011(4) P2 0.0258(9) 0.0236(11) 0.0250(9) -0.0000(7) 0.0038(7) 0.0019(7) C17 0.029(4) 0.025(4) 0.034(4) -0.002(3) 0.002(3) 0.002(3) C18 0.032(4) 0.050(5) 0.033(4) 0.005(4) 0.002(3) 0.003(4) C19 0.039(5) 0.056(6) 0.041(5) -0.004(4) -0.004(4) -0.013(4) C20 0.035(5) 0.052(6) 0.046(5) 0.008(4) -0.001(4) -0.007(4) C21 0.026(4) 0.054(5) 0.033(4) 0.006(4) 0.000(3) -0.003(4) C22 0.039(4) 0.034(4) 0.031(4) -0.006(3) -0.002(3) 0.001(3) C23 0.027(4) 0.028(4) 0.037(4) 0.006(3) 0.001(3) 0.003(3) C24 0.044(5) 0.039(5) 0.049(5) -0.005(4) -0.016(4) 0.003(4) C25 0.044(5) 0.050(6) 0.056(6) 0.015(5) -0.013(4) 0.003(4) C26 0.045(5) 0.031(5) 0.063(6) 0.005(4) 0.003(5) 0.007(4) C27 0.045(5) 0.033(4) 0.044(5) 0.002(4) 0.012(4) 0.001(4) C28 0.033(4) 0.035(4) 0.031(4) 0.002(3) 0.014(3) -0.003(3) C29 0.029(4) 0.035(4) 0.023(3) -0.004(3) 0.003(3) 0.000(3) C30 0.040(4) 0.026(4) 0.042(5) 0.004(3) 0.008(4) -0.001(3) C31 0.035(4) 0.033(4) 0.036(4) -0.009(3) 0.008(3) 0.003(3) C32 0.043(5) 0.058(6) 0.034(5) -0.005(4) 0.014(4) 0.001(4) C33 0.052(5) 0.059(6) 0.026(4) 0.009(4) 0.007(3) -0.004(5) C34 0.043(5) 0.035(4) 0.034(4) 0.001(3) 0.006(4) -0.007(4) P3 0.0247(9) 0.032(1) 0.0267(9) 0.0001(9) 0.0030(7) -0.0001(8) C35 0.043(5) 0.031(4) 0.024(4) 0.002(3) -0.005(3) 0.001(3) C36 0.052(5) 0.025(4) 0.034(4) -0.000(3) 0.012(4) -0.003(3) C37 0.061(6) 0.061(6) 0.031(5) 0.017(4) 0.016(4) 0.006(5) C38 0.073(7) 0.051(6) 0.024(4) 0.007(4) 0.003(4) 0.002(5) C39 0.068(7) 0.044(5) 0.034(5) 0.009(4) 0.003(4) 0.006(5) C40 0.036(4) 0.055(5) 0.027(4) 0.006(4) -0.000(3) 0.015(4) C41 0.025(4) 0.039(4) 0.038(4) -0.003(3) 0.009(3) 0.004(3) C42 0.047(5) 0.055(6) 0.043(5) 0.002(4) -0.002(4) -0.006(4) C43 0.048(6) 0.067(7) 0.046(6) 0.002(5) -0.021(4) -0.009(5) C44 0.036(5) 0.073(7) 0.049(6) -0.022(5) -0.007(4) -0.008(5) C45 0.054(6) 0.037(5) 0.075(8) -0.010(5) 0.004(5) -0.006(4) C46 0.041(5) 0.046(5) 0.039(5) -0.004(4) 0.001(4) -0.002(4) C47 0.029(4) 0.044(5) 0.027(4) 0.003(3) 0.003(3) 0.006(3) C48 0.033(4) 0.060(6) 0.029(4) -0.006(4) -0.001(3) -0.004(4) C49 0.028(4) 0.076(7) 0.044(5) -0.010(5) 0.006(4) -0.002(4) C50 0.025(4) 0.12(1) 0.036(5) -0.002(6) -0.000(4) 0.009(5) C51 0.045(5) 0.064(6) 0.030(4) -0.002(4) 0.001(4) 0.018(5) C52 0.040(5) 0.047(5) 0.032(4) 0.004(4) 0.004(3) 0.010(4) N3 0.077(8) 0.10(1) 0.110(11) 0.013(8) -0.013(7) 0.003(8) C53 0.069(8) 0.046(5) 0.063(7) 0.003(5) -0.009(6) -0.002(5) C54 0.09(1) 0.07(1) 0.17(2) 0.009(11) -0.041(12) 0.015(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . Cl1 . 2.4637(19) yes Re1 . Cl2 . 2.4123(18) yes Re1 . N1 . 1.809(7) yes Re1 . N2 . 2.049(6) yes Re1 . P2 . 2.434(2) yes Re1 . P3 . 2.4284(19) yes N1 . C1 . 1.27(1) yes C1 . C2 . 1.522(11) yes C1 . P1 . 1.801(8) yes C2 . H21 . 1.00 no C2 . H22 . 1.00 no C2 . H23 . 1.000 no P1 . O1 . 1.489(6) yes P1 . C3 . 1.80(1) yes P1 . C9 . 1.806(9) yes C3 . C4 . 1.389(13) yes C3 . C8 . 1.402(13) yes C4 . C5 . 1.385(15) yes C4 . H41 . 1.00 no C5 . C6 . 1.387(16) yes C5 . H51 . 1.00 no C6 . C7 . 1.365(16) yes C6 . H61 . 1.000 no C7 . C8 . 1.406(15) yes C7 . H71 . 1.00 no C8 . H81 . 1.00 no C9 . C10 . 1.404(12) yes C9 . C14 . 1.417(14) yes C10 . C11 . 1.399(15) yes C10 . H101 . 1.000 no C11 . C12 . 1.351(18) yes C11 . H111 . 1.000 no C12 . C13 . 1.387(17) yes C12 . H121 . 1.000 no C13 . C14 . 1.367(15) yes C13 . H131 . 1.000 no C14 . H141 . 1.00 no N2 . C15 . 1.14(1) yes C15 . C16 . 1.465(12) yes C16 . H161 . 1.00 no C16 . H162 . 1.00 no C16 . H163 . 1.00 no P2 . C17 . 1.841(8) yes P2 . C23 . 1.859(8) yes P2 . C29 . 1.834(8) yes C17 . C18 . 1.376(12) yes C17 . C22 . 1.399(11) yes C18 . C19 . 1.379(12) yes C18 . H181 . 1.000 no C19 . C20 . 1.374(14) yes C19 . H191 . 1.000 no C20 . C21 . 1.398(14) yes C20 . H201 . 1.000 no C21 . C22 . 1.390(12) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C23 . C24 . 1.385(12) yes C23 . C28 . 1.380(12) yes C24 . C25 . 1.387(13) yes C24 . H241 . 1.000 no C25 . C26 . 1.387(15) yes C25 . H251 . 1.00 no C26 . C27 . 1.382(15) yes C26 . H261 . 1.000 no C27 . C28 . 1.403(12) yes C27 . H271 . 1.000 no C28 . H281 . 1.000 no C29 . C30 . 1.378(11) yes C29 . C34 . 1.395(12) yes C30 . C31 . 1.396(12) yes C30 . H301 . 1.000 no C31 . C32 . 1.387(13) yes C31 . H311 . 1.000 no C32 . C33 . 1.411(14) yes C32 . H321 . 1.000 no C33 . C34 . 1.397(12) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no P3 . C35 . 1.821(8) yes P3 . C41 . 1.835(9) yes P3 . C47 . 1.836(8) yes C35 . C36 . 1.385(12) yes C35 . C40 . 1.395(11) yes C36 . C37 . 1.393(12) yes C36 . H361 . 1.000 no C37 . C38 . 1.373(14) yes C37 . H371 . 1.00 no C38 . C39 . 1.374(15) yes C38 . H381 . 1.000 no C39 . C40 . 1.403(13) yes C39 . H391 . 1.00 no C40 . H401 . 1.000 no C41 . C42 . 1.395(13) yes C41 . C46 . 1.402(13) yes C42 . C43 . 1.379(15) yes C42 . H421 . 1.00 no C43 . C44 . 1.353(17) yes C43 . H431 . 1.00 no C44 . C45 . 1.413(17) yes C44 . H441 . 1.00 no C45 . C46 . 1.392(14) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C47 . C48 . 1.399(12) yes C47 . C52 . 1.400(13) yes C48 . C49 . 1.386(12) yes C48 . H481 . 1.00 no C49 . C50 . 1.395(17) yes C49 . H491 . 1.00 no C50 . C51 . 1.400(16) yes C50 . H501 . 1.000 no C51 . C52 . 1.401(12) yes C51 . H511 . 1.00 no C52 . H521 . 1.00 no N3 . C53 . 1.131(16) yes C53 . C54 . 1.41(2) yes C54 . H541 . 1.00 no C54 . H542 . 1.00 no C54 . H543 . 1.000 no N4 . C55 . 1.13(1) yes C55 . C56 . 1.45(1) yes C56 . H561 . 1.00 no C56 . H562 . 1.00 no C56 . H563 . 1.00 no N104 . C155 . 1.13(1) yes C155 . C156 . 1.44(1) yes C156 . H1561 . 1.00 no C156 . H1562 . 1.00 no C156 . H1563 . 1.00 no N5 . C57 . 1.13(1) yes C57 . C58 . 1.45(1) yes C58 . H581 . 1.00 no C58 . H582 . 1.00 no C58 . H583 . 1.00 no N105 . C157 . 1.13(1) yes C157 . C158 . 1.45(1) yes C158 . H1581 . 1.00 no C158 . H1582 . 1.00 no C158 . H1583 . 1.00 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Re1 . Cl2 . 90.88(7) yes Cl1 . Re1 . N1 . 170.3(2) yes Cl2 . Re1 . N1 . 98.6(2) yes Cl1 . Re1 . N2 . 79.01(18) yes Cl2 . Re1 . N2 . 169.80(18) yes N1 . Re1 . N2 . 91.5(3) yes Cl1 . Re1 . P2 . 86.08(6) yes Cl2 . Re1 . P2 . 91.66(6) yes N1 . Re1 . P2 . 91.8(2) yes N2 . Re1 . P2 . 89.03(17) yes Cl1 . Re1 . P3 . 91.06(7) yes Cl2 . Re1 . P3 . 88.43(7) yes N1 . Re1 . P3 . 91.0(2) yes N2 . Re1 . P3 . 90.38(17) yes P2 . Re1 . P3 . 177.13(7) yes Re1 . N1 . C1 . 176.6(6) yes N1 . C1 . C2 . 120.1(7) yes N1 . C1 . P1 . 116.8(6) yes C2 . C1 . P1 . 123.1(6) yes C1 . C2 . H21 . 109.5 no C1 . C2 . H22 . 109.5 no H21 . C2 . H22 . 109.5 no C1 . C2 . H23 . 109.5 no H21 . C2 . H23 . 109.5 no H22 . C2 . H23 . 109.5 no C1 . P1 . O1 . 113.6(4) yes C1 . P1 . C3 . 108.3(4) yes O1 . P1 . C3 . 111.0(4) yes C1 . P1 . C9 . 106.3(4) yes O1 . P1 . C9 . 111.6(4) yes C3 . P1 . C9 . 105.6(4) yes P1 . C3 . C4 . 119.3(8) yes P1 . C3 . C8 . 121.3(7) yes C4 . C3 . C8 . 119.4(9) yes C3 . C4 . C5 . 120.5(10) yes C3 . C4 . H41 . 119.7 no C5 . C4 . H41 . 119.7 no C4 . C5 . C6 . 119.7(9) yes C4 . C5 . H51 . 120.2 no C6 . C5 . H51 . 120.2 no C5 . C6 . C7 . 121.0(10) yes C5 . C6 . H61 . 119.5 no C7 . C6 . H61 . 119.5 no C6 . C7 . C8 . 119.9(10) yes C6 . C7 . H71 . 120.0 no C8 . C7 . H71 . 120.0 no C3 . C8 . C7 . 119.4(9) yes C3 . C8 . H81 . 120.3 no C7 . C8 . H81 . 120.3 no P1 . C9 . C10 . 121.8(8) yes P1 . C9 . C14 . 119.1(6) yes C10 . C9 . C14 . 119.0(9) yes C9 . C10 . C11 . 119.2(10) yes C9 . C10 . H101 . 120.4 no C11 . C10 . H101 . 120.4 no C10 . C11 . C12 . 120.4(10) yes C10 . C11 . H111 . 119.8 no C12 . C11 . H111 . 119.8 no C11 . C12 . C13 . 121.5(10) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 119.3 no C12 . C13 . C14 . 119.8(10) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C9 . C14 . C13 . 120.1(9) yes C9 . C14 . H141 . 119.9 no C13 . C14 . H141 . 119.9 no Re1 . N2 . C15 . 176.5(7) yes N2 . C15 . C16 . 176.6(9) yes C15 . C16 . H161 . 109.5 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Re1 . P2 . C17 . 116.9(3) yes Re1 . P2 . C23 . 120.6(3) yes C17 . P2 . C23 . 99.3(3) yes Re1 . P2 . C29 . 110.2(3) yes C17 . P2 . C29 . 104.3(4) yes C23 . P2 . C29 . 103.5(4) yes P2 . C17 . C18 . 124.4(6) yes P2 . C17 . C22 . 116.4(6) yes C18 . C17 . C22 . 119.1(7) yes C17 . C18 . C19 . 121.0(8) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 119.5 no C18 . C19 . C20 . 120.5(9) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 119.7 no C19 . C20 . C21 . 119.6(8) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.2 no C20 . C21 . C22 . 119.7(8) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 120.2 no C17 . C22 . C21 . 120.1(8) yes C17 . C22 . H221 . 119.9 no C21 . C22 . H221 . 119.9 no P2 . C23 . C24 . 117.6(7) yes P2 . C23 . C28 . 121.9(6) yes C24 . C23 . C28 . 120.4(8) yes C23 . C24 . C25 . 120.0(9) yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 120.0 no C24 . C25 . C26 . 119.8(9) yes C24 . C25 . H251 . 120.1 no C26 . C25 . H251 . 120.1 no C25 . C26 . C27 . 120.3(8) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 119.8 no C26 . C27 . C28 . 119.8(8) yes C26 . C27 . H271 . 120.1 no C28 . C27 . H271 . 120.1 no C23 . C28 . C27 . 119.5(8) yes C23 . C28 . H281 . 120.2 no C27 . C28 . H281 . 120.2 no P2 . C29 . C30 . 120.7(6) yes P2 . C29 . C34 . 118.9(6) yes C30 . C29 . C34 . 119.7(7) yes C29 . C30 . C31 . 120.9(8) yes C29 . C30 . H301 . 119.5 no C31 . C30 . H301 . 119.5 no C30 . C31 . C32 . 120.0(8) yes C30 . C31 . H311 . 120.0 no C32 . C31 . H311 . 120.0 no C31 . C32 . C33 . 119.5(8) yes C31 . C32 . H321 . 120.3 no C33 . C32 . H321 . 120.3 no C32 . C33 . C34 . 119.8(8) yes C32 . C33 . H331 . 120.1 no C34 . C33 . H331 . 120.1 no C29 . C34 . C33 . 120.1(8) yes C29 . C34 . H341 . 120.0 no C33 . C34 . H341 . 120.0 no Re1 . P3 . C35 . 113.8(3) yes Re1 . P3 . C41 . 120.5(3) yes C35 . P3 . C41 . 100.2(4) yes Re1 . P3 . C47 . 114.8(3) yes C35 . P3 . C47 . 104.3(4) yes C41 . P3 . C47 . 100.9(4) yes P3 . C35 . C36 . 117.2(6) yes P3 . C35 . C40 . 123.8(7) yes C36 . C35 . C40 . 118.8(8) yes C35 . C36 . C37 . 120.6(9) yes C35 . C36 . H361 . 119.7 no C37 . C36 . H361 . 119.7 no C36 . C37 . C38 . 120.4(9) yes C36 . C37 . H371 . 119.8 no C38 . C37 . H371 . 119.8 no C37 . C38 . C39 . 120.0(9) yes C37 . C38 . H381 . 120.0 no C39 . C38 . H381 . 120.0 no C38 . C39 . C40 . 120.2(9) yes C38 . C39 . H391 . 119.9 no C40 . C39 . H391 . 119.9 no C35 . C40 . C39 . 120.0(8) yes C35 . C40 . H401 . 120.0 no C39 . C40 . H401 . 120.0 no P3 . C41 . C42 . 120.6(7) yes P3 . C41 . C46 . 121.0(7) yes C42 . C41 . C46 . 118.3(8) yes C41 . C42 . C43 . 121.7(9) yes C41 . C42 . H421 . 119.2 no C43 . C42 . H421 . 119.2 no C42 . C43 . C44 . 120.9(9) yes C42 . C43 . H431 . 119.5 no C44 . C43 . H431 . 119.5 no C43 . C44 . C45 . 118.8(9) yes C43 . C44 . H441 . 120.6 no C45 . C44 . H441 . 120.6 no C44 . C45 . C46 . 121.1(10) yes C44 . C45 . H451 . 119.5 no C46 . C45 . H451 . 119.5 no C41 . C46 . C45 . 119.1(9) yes C41 . C46 . H461 . 120.4 no C45 . C46 . H461 . 120.4 no P3 . C47 . C48 . 121.4(7) yes P3 . C47 . C52 . 118.8(7) yes C48 . C47 . C52 . 119.5(8) yes C47 . C48 . C49 . 120.6(9) yes C47 . C48 . H481 . 119.7 no C49 . C48 . H481 . 119.7 no C48 . C49 . C50 . 119.8(9) yes C48 . C49 . H491 . 120.1 no C50 . C49 . H491 . 120.1 no C49 . C50 . C51 . 120.7(9) yes C49 . C50 . H501 . 119.7 no C51 . C50 . H501 . 119.7 no C50 . C51 . C52 . 119.1(10) yes C50 . C51 . H511 . 120.5 no C52 . C51 . H511 . 120.5 no C47 . C52 . C51 . 120.4(9) yes C47 . C52 . H521 . 119.8 no C51 . C52 . H521 . 119.8 no N3 . C53 . C54 . 177.4(16) yes C53 . C54 . H541 . 109.5 no C53 . C54 . H542 . 109.5 no H541 . C54 . H542 . 109.5 no C53 . C54 . H543 . 109.5 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no N4 . C55 . C56 . 179.2(1) yes C55 . C56 . H561 . 109.5 no C55 . C56 . H562 . 109.5 no H561 . C56 . H562 . 109.5 no C55 . C56 . H563 . 109.5 no H561 . C56 . H563 . 109.5 no H562 . C56 . H563 . 109.5 no N104 . C155 . C156 . 179.7(1) yes C155 . C156 . H1561 . 109.5 no C155 . C156 . H1562 . 109.5 no C155 . C156 . H1563 . 109.5 no H1561 . C156 . H1562 . 109.5 no H1561 . C156 . H1563 . 109.5 no H1562 . C156 . H1563 . 109.5 no N5 . C57 . C58 . 179.6(1) yes C57 . C58 . H581 . 109.5 no C57 . C58 . H582 . 109.5 no H581 . C58 . H582 . 109.5 no C57 . C58 . H583 . 109.5 no H581 . C58 . H583 . 109.5 no H582 . C58 . H583 . 109.5 no N105 . C157 . C158 . 179.2(1) yes C157 . C158 . H1581 . 109.5 no C157 . C158 . H1582 . 109.5 no C157 . C158 . H1583 . 109.5 no H1581 . C158 . H1582 . 109.5 no H1581 . C158 . H1583 . 109.5 no H1582 . C158 . H1583 . 109.5 no data_arc731 _database_code_depnum_ccdc_archive 'CCDC 255288' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_special_details ; All hydrogen atoms were positioned geometrically, the preferred orientations of the methyl groups having been previously determined by examination of a difference Fourier map Geometric restraints were applied to the disordered phenyl group C41-C46, C91-C96. C-C bond lengths were restrained to 1.39(2) \%A and C-C-C angles to 120(2)\% ; #============================================================= _cell_length_a 15.2069(2) _cell_angle_alpha 90 _cell_length_b 13.4521(2) _cell_angle_beta 105.5875(4) _cell_length_c 24.6870(3) _cell_angle_gamma 90 _cell_volume 4864.35(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C53.416 H48.124 Br2 N2.708 O1 P3 Re1 ' _chemical_formula_moiety ' C52 H46 Br2 N2 O1 P3 Re1, 0.708(C2 H3 N) ' _chemical_compound_source ; ? ; _chemical_formula_weight 1182.94 _cell_measurement_reflns_used 53221 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' tablet ' _exptl_crystal_colour ' green ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_max 0.08 _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2342.307 _exptl_absorpt_coefficient_mu 4.281 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.84 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 53221 _reflns_number_total 11075 #11541 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_theta_min 5.118 _diffrn_reflns_theta_max 27.481 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.481 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -19 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _refine_diff_density_min -1.43 _refine_diff_density_max 1.23 _refine_ls_number_reflns 6802 _refine_ls_number_restraints 36 _refine_ls_number_parameters 572 #_refine_ls_R_factor_ref 0.0325 _refine_ls_wR_factor_ref 0.0352 _refine_ls_goodness_of_fit_ref 1.0987 #_reflns_number_all 11075 _refine_ls_R_factor_all 0.0697 _refine_ls_wR_factor_all 0.0605 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6802 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_gt 0.0352 _refine_ls_shift/su_max 0.017660 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.354 0.131 0.166 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_disorder_group Re1 Re 0.50793(1) 0.32418(1) 0.25868(1) 0.0268 1.0000 Uani . Br1 Br 0.60518(4) 0.16207(4) 0.28175(3) 0.0471 1.0000 Uani . Br2 Br 0.35944(4) 0.22427(4) 0.24306(2) 0.0384 1.0000 Uani . N1 N 0.4580(3) 0.4463(3) 0.24255(17) 0.0304 1.0000 Uani . C1 C 0.4296(3) 0.5358(4) 0.2319(2) 0.0305 1.0000 Uani . C2 C 0.3282(4) 0.5566(4) 0.2079(2) 0.0378 1.0000 Uani . P1 P 0.51425(8) 0.6334(1) 0.24669(6) 0.0298 1.0000 Uani . O1 O 0.5997(2) 0.6054(3) 0.28936(16) 0.0356 1.0000 Uani . C3 C 0.5365(4) 0.6704(4) 0.1811(2) 0.0348 1.0000 Uani . C4 C 0.6241(4) 0.7014(4) 0.1822(3) 0.0391 1.0000 Uani . C5 C 0.6433(4) 0.7315(4) 0.1325(3) 0.0433 1.0000 Uani . C6 C 0.5774(5) 0.7302(4) 0.0826(3) 0.0461 1.0000 Uani . C7 C 0.4901(5) 0.6982(6) 0.0810(3) 0.0567 1.0000 Uani . C8 C 0.4691(4) 0.6682(5) 0.1300(3) 0.0472 1.0000 Uani . C9 C 0.4593(4) 0.7394(4) 0.2691(2) 0.0356 1.0000 Uani . C10 C 0.4711(4) 0.8347(4) 0.2504(3) 0.0401 1.0000 Uani . C11 C 0.4377(4) 0.9164(5) 0.2736(3) 0.0516 1.0000 Uani . C12 C 0.3918(4) 0.9024(6) 0.3137(3) 0.0612 1.0000 Uani . C13 C 0.3787(5) 0.8073(6) 0.3319(3) 0.0604 1.0000 Uani . C14 C 0.4140(5) 0.7255(5) 0.3102(3) 0.0511 1.0000 Uani . N2 N 0.6370(3) 0.3838(3) 0.27728(18) 0.0297 1.0000 Uani . C15 C 0.7048(4) 0.4244(4) 0.2866(2) 0.0372 1.0000 Uani . C16 C 0.7918(4) 0.4771(5) 0.2980(3) 0.0497 1.0000 Uani . P2 P 0.51822(8) 0.30294(9) 0.16247(6) 0.0276 1.0000 Uani . C17 C 0.4318(3) 0.3670(4) 0.1066(2) 0.0309 1.0000 Uani . C18 C 0.4483(4) 0.3994(4) 0.0567(2) 0.0366 1.0000 Uani . C19 C 0.3798(4) 0.4429(5) 0.0153(2) 0.0439 1.0000 Uani . C20 C 0.2930(4) 0.4515(5) 0.0218(3) 0.0494 1.0000 Uani . C21 C 0.2754(4) 0.4171(6) 0.0702(3) 0.0583 1.0000 Uani . C22 C 0.3448(4) 0.3745(5) 0.1127(3) 0.0443 1.0000 Uani . C23 C 0.5111(3) 0.1779(4) 0.1314(2) 0.0327 1.0000 Uani . C24 C 0.5471(4) 0.1599(4) 0.0860(3) 0.0419 1.0000 Uani . C25 C 0.5409(4) 0.0650(5) 0.0626(3) 0.0513 1.0000 Uani . C26 C 0.4973(4) -0.0101(4) 0.0830(3) 0.0499 1.0000 Uani . C27 C 0.4600(4) 0.0070(4) 0.1258(3) 0.0459 1.0000 Uani . C28 C 0.4666(4) 0.1020(4) 0.1511(2) 0.0378 1.0000 Uani . C29 C 0.6275(3) 0.3477(4) 0.1545(2) 0.0309 1.0000 Uani . C30 C 0.6408(3) 0.4465(4) 0.1423(2) 0.0324 1.0000 Uani . C31 C 0.7268(4) 0.4798(4) 0.1416(2) 0.0373 1.0000 Uani . C32 C 0.8006(4) 0.4165(5) 0.1535(3) 0.0467 1.0000 Uani . C33 C 0.7886(4) 0.3186(5) 0.1678(3) 0.0504 1.0000 Uani . C34 C 0.7040(4) 0.2844(4) 0.1683(3) 0.0419 1.0000 Uani . P3 P 0.50425(9) 0.33590(11) 0.35642(6) 0.0331 1.0000 Uani . C35 C 0.4268(4) 0.4319(5) 0.3700(2) 0.0385 1.0000 Uani . C36 C 0.3402(4) 0.4406(5) 0.3320(2) 0.0375 1.0000 Uani . C37 C 0.2770(4) 0.5068(5) 0.3425(2) 0.0457 1.0000 Uani . C38 C 0.2984(4) 0.5656(6) 0.3903(3) 0.0558 1.0000 Uani . C39 C 0.3838(4) 0.5570(6) 0.4283(3) 0.0585 1.0000 Uani . C40 C 0.4476(4) 0.4912(6) 0.4180(3) 0.0494 1.0000 Uani . C41 C 0.4687(6) 0.2222(6) 0.3862(4) 0.0385(19) 0.708(9) Uiso 1 C42 C 0.3939(6) 0.2220(7) 0.4085(4) 0.051(2) 0.708(9) Uiso 1 C43 C 0.3727(7) 0.1369(8) 0.4350(5) 0.063(2) 0.708(9) Uiso 1 C44 C 0.4271(7) 0.0546(7) 0.4411(5) 0.061(2) 0.708(9) Uiso 1 C45 C 0.5045(7) 0.0516(7) 0.4211(4) 0.055(2) 0.708(9) Uiso 1 C46 C 0.5245(6) 0.1347(6) 0.3926(4) 0.048(2) 0.708(9) Uiso 1 C91 C 0.464(2) 0.2473(17) 0.4012(11) 0.076(6) 0.292(9) Uiso 2 C92 C 0.447(2) 0.2734(16) 0.4524(11) 0.082(6) 0.292(9) Uiso 2 C93 C 0.429(2) 0.2018(19) 0.488(1) 0.087(6) 0.292(9) Uiso 2 C94 C 0.427(2) 0.1029(18) 0.4736(12) 0.086(6) 0.292(9) Uiso 2 C95 C 0.452(3) 0.0753(16) 0.4250(12) 0.083(6) 0.292(9) Uiso 2 C96 C 0.469(2) 0.1486(19) 0.389(1) 0.078(5) 0.292(9) Uiso 2 C47 C 0.6139(3) 0.3663(4) 0.4063(2) 0.0322 1.0000 Uani . C48 C 0.6615(4) 0.3026(4) 0.4478(2) 0.0391 1.0000 Uani . C49 C 0.7461(4) 0.3296(6) 0.4833(2) 0.0486 1.0000 Uani . C50 C 0.7812(4) 0.4207(6) 0.4778(3) 0.0506 1.0000 Uani . C51 C 0.7355(4) 0.4855(5) 0.4366(3) 0.0518 1.0000 Uani . C52 C 0.6525(4) 0.4585(5) 0.4005(3) 0.0443 1.0000 Uani . N3 N 0.2154(7) 0.246(1) 0.5179(6) 0.1010 0.708(9) Uani 1 C53 C 0.294(1) 0.260(1) 0.5412(6) 0.0823 0.708(9) Uani 1 C54 C 0.3923(9) 0.2781(11) 0.5697(7) 0.0943 0.708(9) Uani 1 H21 H 0.3184 0.6298 0.2022 0.0444 1.0000 Uiso . H22 H 0.2941 0.5321 0.2347 0.0444 1.0000 Uiso . H23 H 0.3055 0.5216 0.1711 0.0444 1.0000 Uiso . H41 H 0.6732 0.7021 0.2185 0.0478 1.0000 Uiso . H51 H 0.7063 0.7543 0.1335 0.0547 1.0000 Uiso . H61 H 0.5920 0.7523 0.0474 0.0589 1.0000 Uiso . H71 H 0.4418 0.6967 0.0444 0.0689 1.0000 Uiso . H81 H 0.4060 0.6452 0.1287 0.0562 1.0000 Uiso . H101 H 0.5034 0.8447 0.2205 0.0469 1.0000 Uiso . H111 H 0.4473 0.9851 0.2609 0.0590 1.0000 Uiso . H121 H 0.3675 0.9610 0.3299 0.0702 1.0000 Uiso . H131 H 0.3440 0.7976 0.3605 0.0744 1.0000 Uiso . H141 H 0.4066 0.6571 0.3244 0.0639 1.0000 Uiso . H161 H 0.8138 0.4776 0.2633 0.0573 1.0000 Uiso . H162 H 0.8377 0.4428 0.3290 0.0573 1.0000 Uiso . H163 H 0.7834 0.5471 0.3094 0.0573 1.0000 Uiso . H181 H 0.5104 0.3909 0.0507 0.0443 1.0000 Uiso . H191 H 0.3932 0.4684 -0.0197 0.0521 1.0000 Uiso . H201 H 0.2433 0.4825 -0.0084 0.0566 1.0000 Uiso . H211 H 0.2124 0.4227 0.0751 0.0689 1.0000 Uiso . H221 H 0.3312 0.3494 0.1477 0.0524 1.0000 Uiso . H241 H 0.5772 0.2148 0.0704 0.0501 1.0000 Uiso . H251 H 0.5683 0.0515 0.0308 0.0607 1.0000 Uiso . H261 H 0.4932 -0.0779 0.0658 0.0558 1.0000 Uiso . H271 H 0.4275 -0.0478 0.1398 0.0516 1.0000 Uiso . H281 H 0.4391 0.1143 0.1830 0.0435 1.0000 Uiso . H301 H 0.5881 0.4937 0.1340 0.0392 1.0000 Uiso . H311 H 0.7353 0.5509 0.1322 0.0438 1.0000 Uiso . H321 H 0.8621 0.4408 0.1520 0.0561 1.0000 Uiso . H331 H 0.8422 0.2726 0.1777 0.0590 1.0000 Uiso . H341 H 0.6965 0.2136 0.1785 0.0479 1.0000 Uiso . H361 H 0.3241 0.3990 0.2972 0.0453 1.0000 Uiso . H371 H 0.2152 0.5122 0.3153 0.0550 1.0000 Uiso . H381 H 0.2527 0.6139 0.3975 0.0692 1.0000 Uiso . H391 H 0.3994 0.5984 0.4632 0.0710 1.0000 Uiso . H401 H 0.5092 0.4862 0.4454 0.0597 1.0000 Uiso . H421 H 0.3552 0.2828 0.4056 0.0617 0.708 Uiso 1 H431 H 0.3175 0.1364 0.4497 0.0753 0.708 Uiso 1 H441 H 0.4109 -0.0053 0.4605 0.0737 0.708 Uiso 1 H451 H 0.5446 -0.0085 0.4270 0.0666 0.708 Uiso 1 H461 H 0.5784 0.1332 0.3766 0.0576 0.708 Uiso 1 H921 H 0.4484 0.3451 0.4633 0.0981 0.292 Uiso 2 H931 H 0.4167 0.2218 0.5248 0.1042 0.292 Uiso 2 H941 H 0.4094 0.0510 0.4976 0.1031 0.292 Uiso 2 H951 H 0.4579 0.0034 0.4161 0.0997 0.292 Uiso 2 H961 H 0.4842 0.1288 0.3534 0.0931 0.292 Uiso 2 H481 H 0.6350 0.2361 0.4525 0.0474 1.0000 Uiso . H491 H 0.7807 0.2822 0.5125 0.0577 1.0000 Uiso . H501 H 0.8409 0.4410 0.5039 0.0591 1.0000 Uiso . H511 H 0.7623 0.5521 0.4329 0.0621 1.0000 Uiso . H521 H 0.6202 0.5052 0.3701 0.0517 1.0000 Uiso . H541 H 0.3976 0.3205 0.6035 0.1118 0.708 Uiso 1 H542 H 0.4234 0.2128 0.5814 0.1118 0.708 Uiso 1 H543 H 0.4218 0.3122 0.5431 0.1118 0.708 Uiso 1 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 Re1 0.02274(9) 0.02231(9) 0.0330(1) 0.00199(9) 0.00334(7) -0.00218(8) Br1 0.0396(3) 0.0265(3) 0.0641(4) 0.0057(2) -0.0055(3) 0.0038(2) Br2 0.0319(3) 0.0371(3) 0.0441(3) 0.0010(2) 0.0066(2) -0.0119(2) N1 0.0234(19) 0.037(2) 0.031(2) -0.0034(18) 0.0074(17) -0.0111(17) C1 0.027(2) 0.025(2) 0.040(3) 0.004(2) 0.009(2) 0.0036(19) C2 0.031(3) 0.032(3) 0.048(3) 0.004(2) 0.006(2) 0.002(2) P1 0.0287(7) 0.0221(6) 0.0380(8) 0.0005(5) 0.0079(6) 0.0008(5) O1 0.0315(18) 0.0245(18) 0.046(2) 0.0008(15) 0.0031(16) 0.0005(14) C3 0.042(3) 0.022(2) 0.044(3) -0.004(2) 0.018(2) -0.001(2) C4 0.035(3) 0.033(3) 0.051(3) -0.001(2) 0.015(3) 0.002(2) C5 0.043(3) 0.034(3) 0.059(4) 0.004(3) 0.025(3) -0.003(2) C6 0.065(4) 0.034(3) 0.048(4) 0.005(3) 0.031(3) -0.001(3) C7 0.066(4) 0.066(5) 0.040(4) -0.002(3) 0.018(3) -0.013(4) C8 0.045(3) 0.054(4) 0.041(3) -0.006(3) 0.009(3) -0.011(3) C9 0.039(3) 0.032(3) 0.033(3) -0.004(2) 0.004(2) 0.003(2) C10 0.037(3) 0.029(3) 0.051(3) -0.001(2) 0.006(2) 0.005(2) C11 0.039(3) 0.037(3) 0.072(5) -0.012(3) 0.003(3) 0.011(3) C12 0.037(3) 0.058(4) 0.080(5) -0.034(4) 0.002(3) 0.014(3) C13 0.048(4) 0.069(5) 0.070(5) -0.029(4) 0.025(3) -0.001(3) C14 0.055(4) 0.041(3) 0.064(4) -0.014(3) 0.027(3) -0.007(3) N2 0.025(2) 0.024(2) 0.037(2) 0.0036(17) 0.0035(18) -0.0009(17) C15 0.033(3) 0.033(3) 0.041(3) -0.002(2) 0.002(2) -0.001(2) C16 0.027(3) 0.048(4) 0.069(4) -0.003(3) 0.003(3) -0.011(3) P2 0.0234(6) 0.0231(6) 0.0348(7) 0.0000(5) 0.0053(5) -0.0009(5) C17 0.022(2) 0.026(2) 0.041(3) -0.002(2) 0.002(2) 0.002(2) C18 0.038(3) 0.039(3) 0.033(3) -0.001(2) 0.011(2) -0.005(2) C19 0.048(3) 0.049(3) 0.034(3) 0.007(3) 0.009(3) 0.000(3) C20 0.047(3) 0.057(4) 0.038(3) 0.010(3) 0.000(3) 0.015(3) C21 0.033(3) 0.090(5) 0.050(4) 0.012(4) 0.007(3) 0.018(3) C22 0.035(3) 0.055(4) 0.041(3) 0.005(3) 0.007(2) 0.008(3) C23 0.026(2) 0.028(2) 0.042(3) -0.001(2) 0.006(2) 0.003(2) C24 0.037(3) 0.039(3) 0.049(3) -0.010(3) 0.011(3) 0.002(2) C25 0.037(3) 0.056(4) 0.060(4) -0.022(3) 0.009(3) 0.010(3) C26 0.045(3) 0.031(3) 0.063(4) -0.009(3) -0.003(3) 0.008(3) C27 0.050(4) 0.027(3) 0.052(4) 0.001(3) -0.002(3) -0.004(3) C28 0.041(3) 0.026(3) 0.042(3) -0.006(2) 0.003(2) -0.004(2) C29 0.025(2) 0.028(3) 0.038(3) 0.001(2) 0.005(2) -0.0016(19) C30 0.029(2) 0.025(3) 0.044(3) 0.001(2) 0.011(2) 0.001(2) C31 0.031(3) 0.029(3) 0.050(3) 0.003(2) 0.007(2) -0.005(2) C32 0.030(3) 0.041(3) 0.069(4) 0.001(3) 0.013(3) -0.006(2) C33 0.026(3) 0.040(3) 0.081(5) 0.002(3) 0.007(3) -0.001(3) C34 0.032(3) 0.032(3) 0.055(4) 0.008(3) 0.001(3) -0.003(2) P3 0.0260(6) 0.0383(8) 0.0339(7) 0.0080(6) 0.0059(5) -0.0037(6) C35 0.034(3) 0.054(3) 0.032(3) 0.006(3) 0.014(2) 0.002(3) C36 0.026(3) 0.057(4) 0.030(3) 0.002(3) 0.009(2) 0.000(2) C37 0.036(3) 0.067(4) 0.034(3) 0.004(3) 0.010(2) 0.013(3) C38 0.039(3) 0.090(5) 0.044(4) 0.000(4) 0.020(3) 0.018(3) C39 0.045(3) 0.092(6) 0.041(4) -0.009(3) 0.015(3) 0.017(4) C40 0.036(3) 0.078(5) 0.035(3) 0.003(3) 0.011(3) 0.004(3) C47 0.028(2) 0.038(3) 0.030(3) 0.004(2) 0.007(2) 0.002(2) C48 0.037(3) 0.045(3) 0.037(3) 0.004(2) 0.012(2) 0.009(2) C49 0.037(3) 0.078(5) 0.029(3) 0.009(3) 0.006(2) 0.018(3) C50 0.033(3) 0.077(5) 0.038(3) -0.004(3) 0.003(3) -0.001(3) C51 0.039(3) 0.054(4) 0.062(4) -0.012(3) 0.014(3) -0.006(3) C52 0.032(3) 0.046(3) 0.051(4) 0.004(3) 0.005(3) 0.000(2) N3 0.057(6) 0.129(11) 0.12(1) -0.046(8) 0.023(6) -0.016(6) C53 0.084(9) 0.066(8) 0.10(1) -0.018(7) 0.028(8) 0.006(7) C54 0.066(8) 0.089(9) 0.124(12) -0.036(9) 0.019(8) -0.019(7) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . Br1 . 2.6103(6) yes Re1 . Br2 . 2.5664(5) yes Re1 . N1 . 1.808(5) yes Re1 . N2 . 2.055(4) yes Re1 . P2 . 2.4386(14) yes Re1 . P3 . 2.4337(14) yes N1 . C1 . 1.282(7) yes C1 . C2 . 1.523(7) yes C1 . P1 . 1.806(5) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no P1 . O1 . 1.484(4) yes P1 . C3 . 1.811(5) yes P1 . C9 . 1.813(6) yes C3 . C4 . 1.389(8) yes C3 . C8 . 1.394(8) yes C4 . C5 . 1.395(8) yes C4 . H41 . 1.000 no C5 . C6 . 1.363(9) yes C5 . H51 . 1.000 no C6 . C7 . 1.386(9) yes C6 . H61 . 1.000 no C7 . C8 . 1.392(9) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.390(8) yes C9 . C14 . 1.384(9) yes C10 . C11 . 1.396(8) yes C10 . H101 . 1.000 no C11 . C12 . 1.368(11) yes C11 . H111 . 1.000 no C12 . C13 . 1.387(11) yes C12 . H121 . 1.000 no C13 . C14 . 1.392(9) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no N2 . C15 . 1.133(7) yes C15 . C16 . 1.460(8) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no P2 . C17 . 1.844(5) yes P2 . C23 . 1.840(5) yes P2 . C29 . 1.827(5) yes C17 . C18 . 1.391(8) yes C17 . C22 . 1.376(7) yes C18 . C19 . 1.378(8) yes C18 . H181 . 1.000 no C19 . C20 . 1.377(9) yes C19 . H191 . 1.000 no C20 . C21 . 1.373(9) yes C20 . H201 . 1.000 no C21 . C22 . 1.395(8) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C23 . C24 . 1.394(8) yes C23 . C28 . 1.382(8) yes C24 . C25 . 1.394(8) yes C24 . H241 . 1.000 no C25 . C26 . 1.38(1) yes C25 . H251 . 1.000 no C26 . C27 . 1.35(1) yes C26 . H261 . 1.000 no C27 . C28 . 1.414(8) yes C27 . H271 . 1.000 no C28 . H281 . 1.000 no C29 . C30 . 1.390(7) yes C29 . C34 . 1.408(7) yes C30 . C31 . 1.387(7) yes C30 . H301 . 1.000 no C31 . C32 . 1.376(8) yes C31 . H311 . 1.000 no C32 . C33 . 1.388(9) yes C32 . H321 . 1.000 no C33 . C34 . 1.370(8) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no P3 . C35 . 1.839(6) yes P3 . C41 . 1.840(8) yes P3 . C91 . 1.84(2) yes P3 . C47 . 1.833(5) yes C35 . C36 . 1.401(7) yes C35 . C40 . 1.392(9) yes C36 . C37 . 1.386(8) yes C36 . H361 . 1.000 no C37 . C38 . 1.385(9) yes C37 . H371 . 1.000 no C38 . C39 . 1.386(9) yes C38 . H381 . 1.000 no C39 . C40 . 1.386(9) yes C39 . H391 . 1.000 no C40 . H401 . 1.000 no C41 . C42 . 1.389(11) yes C41 . C46 . 1.435(11) yes C42 . C43 . 1.399(11) yes C42 . H421 . 1.000 no C43 . C44 . 1.366(12) yes C43 . H431 . 1.000 no C44 . C45 . 1.394(12) yes C44 . H441 . 1.000 no C45 . C46 . 1.397(11) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C91 . C92 . 1.399(18) yes C91 . C96 . 1.368(18) yes C92 . C93 . 1.390(18) yes C92 . H921 . 1.000 no C93 . C94 . 1.379(18) yes C93 . H931 . 1.000 no C94 . C95 . 1.402(18) yes C94 . H941 . 1.000 no C95 . C96 . 1.397(18) yes C95 . H951 . 1.000 no C96 . H961 . 1.000 no C47 . C48 . 1.383(7) yes C47 . C52 . 1.395(8) yes C48 . C49 . 1.396(8) yes C48 . H481 . 1.000 no C49 . C50 . 1.36(1) yes C49 . H491 . 1.000 no C50 . C51 . 1.38(1) yes C50 . H501 . 1.000 no C51 . C52 . 1.384(8) yes C51 . H511 . 1.000 no C52 . H521 . 1.000 no N3 . C53 . 1.198(16) yes C53 . C54 . 1.488(18) yes C54 . H541 . 0.998 no C54 . H542 . 1.002 no C54 . H543 . 0.999 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . Re1 . Br2 . 91.107(19) yes Br1 . Re1 . N1 . 170.57(13) yes Br2 . Re1 . N1 . 98.17(12) yes Br1 . Re1 . N2 . 79.98(11) yes Br2 . Re1 . N2 . 170.77(11) yes N1 . Re1 . N2 . 90.81(17) yes Br1 . Re1 . P2 . 86.20(3) yes Br2 . Re1 . P2 . 94.39(3) yes N1 . Re1 . P2 . 91.42(14) yes N2 . Re1 . P2 . 87.47(13) yes Br1 . Re1 . P3 . 90.03(4) yes Br2 . Re1 . P3 . 85.94(3) yes N1 . Re1 . P3 . 92.26(14) yes N2 . Re1 . P3 . 91.62(13) yes P2 . Re1 . P3 . 176.22(5) yes Re1 . N1 . C1 . 175.0(4) yes N1 . C1 . C2 . 120.2(5) yes N1 . C1 . P1 . 117.4(4) yes C2 . C1 . P1 . 122.4(4) yes C1 . C2 . H21 . 109.482 no C1 . C2 . H22 . 109.450 no H21 . C2 . H22 . 109.488 no C1 . C2 . H23 . 109.459 no H21 . C2 . H23 . 109.488 no H22 . C2 . H23 . 109.460 no C1 . P1 . O1 . 113.5(2) yes C1 . P1 . C3 . 108.2(2) yes O1 . P1 . C3 . 111.5(2) yes C1 . P1 . C9 . 105.8(2) yes O1 . P1 . C9 . 111.7(2) yes C3 . P1 . C9 . 105.6(3) yes P1 . C3 . C4 . 118.2(4) yes P1 . C3 . C8 . 122.3(4) yes C4 . C3 . C8 . 119.5(5) yes C3 . C4 . C5 . 119.7(5) yes C3 . C4 . H41 . 120.119 no C5 . C4 . H41 . 120.140 no C4 . C5 . C6 . 120.9(5) yes C4 . C5 . H51 . 119.579 no C6 . C5 . H51 . 119.542 no C5 . C6 . C7 . 119.8(6) yes C5 . C6 . H61 . 120.126 no C7 . C6 . H61 . 120.106 no C6 . C7 . C8 . 120.4(6) yes C6 . C7 . H71 . 119.792 no C8 . C7 . H71 . 119.795 no C3 . C8 . C7 . 119.7(6) yes C3 . C8 . H81 . 120.142 no C7 . C8 . H81 . 120.172 no P1 . C9 . C10 . 120.8(5) yes P1 . C9 . C14 . 118.6(4) yes C10 . C9 . C14 . 120.2(5) yes C9 . C10 . C11 . 119.7(6) yes C9 . C10 . H101 . 120.139 no C11 . C10 . H101 . 120.138 no C10 . C11 . C12 . 120.0(6) yes C10 . C11 . H111 . 119.970 no C12 . C11 . H111 . 119.996 no C11 . C12 . C13 . 120.4(6) yes C11 . C12 . H121 . 119.803 no C13 . C12 . H121 . 119.809 no C12 . C13 . C14 . 120.1(6) yes C12 . C13 . H131 . 119.950 no C14 . C13 . H131 . 119.928 no C9 . C14 . C13 . 119.5(6) yes C9 . C14 . H141 . 120.270 no C13 . C14 . H141 . 120.212 no Re1 . N2 . C15 . 174.1(4) yes N2 . C15 . C16 . 179.4(6) yes C15 . C16 . H161 . 109.446 no C15 . C16 . H162 . 109.487 no H161 . C16 . H162 . 109.467 no C15 . C16 . H163 . 109.476 no H161 . C16 . H163 . 109.454 no H162 . C16 . H163 . 109.498 no Re1 . P2 . C17 . 117.08(18) yes Re1 . P2 . C23 . 120.06(18) yes C17 . P2 . C23 . 99.5(2) yes Re1 . P2 . C29 . 111.35(18) yes C17 . P2 . C29 . 104.6(2) yes C23 . P2 . C29 . 102.1(2) yes P2 . C17 . C18 . 123.2(4) yes P2 . C17 . C22 . 117.7(4) yes C18 . C17 . C22 . 118.8(5) yes C17 . C18 . C19 . 120.6(5) yes C17 . C18 . H181 . 119.699 no C19 . C18 . H181 . 119.689 no C18 . C19 . C20 . 120.4(5) yes C18 . C19 . H191 . 119.806 no C20 . C19 . H191 . 119.791 no C19 . C20 . C21 . 119.4(5) yes C19 . C20 . H201 . 120.269 no C21 . C20 . H201 . 120.316 no C20 . C21 . C22 . 120.5(6) yes C20 . C21 . H211 . 119.785 no C22 . C21 . H211 . 119.742 no C17 . C22 . C21 . 120.2(6) yes C17 . C22 . H221 . 119.914 no C21 . C22 . H221 . 119.888 no P2 . C23 . C24 . 120.1(4) yes P2 . C23 . C28 . 120.6(4) yes C24 . C23 . C28 . 119.3(5) yes C23 . C24 . C25 . 119.7(6) yes C23 . C24 . H241 . 120.163 no C25 . C24 . H241 . 120.118 no C24 . C25 . C26 . 120.4(6) yes C24 . C25 . H251 . 119.804 no C26 . C25 . H251 . 119.831 no C25 . C26 . C27 . 120.5(6) yes C25 . C26 . H261 . 119.746 no C27 . C26 . H261 . 119.774 no C26 . C27 . C28 . 120.4(6) yes C26 . C27 . H271 . 119.802 no C28 . C27 . H271 . 119.776 no C23 . C28 . C27 . 119.7(6) yes C23 . C28 . H281 . 120.158 no C27 . C28 . H281 . 120.135 no P2 . C29 . C30 . 121.9(4) yes P2 . C29 . C34 . 119.5(4) yes C30 . C29 . C34 . 118.2(5) yes C29 . C30 . C31 . 120.3(5) yes C29 . C30 . H301 . 119.822 no C31 . C30 . H301 . 119.869 no C30 . C31 . C32 . 121.0(5) yes C30 . C31 . H311 . 119.527 no C32 . C31 . H311 . 119.492 no C31 . C32 . C33 . 119.1(5) yes C31 . C32 . H321 . 120.471 no C33 . C32 . H321 . 120.437 no C32 . C33 . C34 . 120.6(5) yes C32 . C33 . H331 . 119.722 no C34 . C33 . H331 . 119.669 no C29 . C34 . C33 . 120.8(5) yes C29 . C34 . H341 . 119.596 no C33 . C34 . H341 . 119.618 no Re1 . P3 . C35 . 114.41(18) yes Re1 . P3 . C41 . 115.4(3) yes C35 . P3 . C41 . 103.8(3) yes Re1 . P3 . C91 . 130.9(8) yes C35 . P3 . C91 . 90.6(9) yes Re1 . P3 . C47 . 114.89(17) yes C35 . P3 . C47 . 103.4(3) yes C41 . P3 . C47 . 103.3(3) yes C91 . P3 . C47 . 97.6(11) yes P3 . C35 . C36 . 118.0(4) yes P3 . C35 . C40 . 123.2(4) yes C36 . C35 . C40 . 118.7(5) yes C35 . C36 . C37 . 120.2(5) yes C35 . C36 . H361 . 119.917 no C37 . C36 . H361 . 119.915 no C36 . C37 . C38 . 120.7(5) yes C36 . C37 . H371 . 119.630 no C38 . C37 . H371 . 119.671 no C37 . C38 . C39 . 119.4(6) yes C37 . C38 . H381 . 120.324 no C39 . C38 . H381 . 120.284 no C38 . C39 . C40 . 120.3(6) yes C38 . C39 . H391 . 119.839 no C40 . C39 . H391 . 119.841 no C35 . C40 . C39 . 120.7(6) yes C35 . C40 . H401 . 119.625 no C39 . C40 . H401 . 119.653 no P3 . C41 . C42 . 121.3(6) yes P3 . C41 . C46 . 119.8(6) yes C42 . C41 . C46 . 118.5(7) yes C41 . C42 . C43 . 120.2(7) yes C41 . C42 . H421 . 119.919 no C43 . C42 . H421 . 119.857 no C42 . C43 . C44 . 120.4(8) yes C42 . C43 . H431 . 119.812 no C44 . C43 . H431 . 119.801 no C43 . C44 . C45 . 121.9(9) yes C43 . C44 . H441 . 119.033 no C45 . C44 . H441 . 119.107 no C44 . C45 . C46 . 118.4(8) yes C44 . C45 . H451 . 120.793 no C46 . C45 . H451 . 120.856 no C41 . C46 . C45 . 120.6(7) yes C41 . C46 . H461 . 119.732 no C45 . C46 . H461 . 119.676 no P3 . C91 . C92 . 123.4(16) yes P3 . C91 . C96 . 116.5(16) yes C92 . C91 . C96 . 118.7(13) yes C91 . C92 . C93 . 121.4(13) yes C91 . C92 . H921 . 119.327 no C93 . C92 . H921 . 119.270 no C92 . C93 . C94 . 119.3(13) yes C92 . C93 . H931 . 120.342 no C94 . C93 . H931 . 120.380 no C93 . C94 . C95 . 119.7(13) yes C93 . C94 . H941 . 120.142 no C95 . C94 . H941 . 120.156 no C94 . C95 . C96 . 119.7(13) yes C94 . C95 . H951 . 120.123 no C96 . C95 . H951 . 120.156 no C91 . C96 . C95 . 120.8(13) yes C91 . C96 . H961 . 119.630 no C95 . C96 . H961 . 119.608 no P3 . C47 . C48 . 124.0(4) yes P3 . C47 . C52 . 117.5(4) yes C48 . C47 . C52 . 118.4(5) yes C47 . C48 . C49 . 120.9(6) yes C47 . C48 . H481 . 119.552 no C49 . C48 . H481 . 119.521 no C48 . C49 . C50 . 119.5(6) yes C48 . C49 . H491 . 120.237 no C50 . C49 . H491 . 120.242 no C49 . C50 . C51 . 120.7(6) yes C49 . C50 . H501 . 119.626 no C51 . C50 . H501 . 119.656 no C50 . C51 . C52 . 120.2(6) yes C50 . C51 . H511 . 119.881 no C52 . C51 . H511 . 119.960 no C47 . C52 . C51 . 120.2(6) yes C47 . C52 . H521 . 119.905 no C51 . C52 . H521 . 119.890 no N3 . C53 . C54 . 179.4(14) yes C53 . C54 . H541 . 109.465 no C53 . C54 . H542 . 109.264 no H541 . C54 . H542 . 109.471 no C53 . C54 . H543 . 109.504 no H541 . C54 . H543 . 109.717 no H542 . C54 . H543 . 109.406 no data_ajr _database_code_depnum_ccdc_archive 'CCDC 255289' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 9.3008(2) _cell_angle_alpha 67.4001(7) _cell_length_b 9.5959(2) _cell_angle_beta 77.4316(7) _cell_length_c 12.3168(2) _cell_angle_gamma 87.2789(8) _cell_volume 989.74(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C19 H21 Cl2 N2 P Ti ' _chemical_formula_moiety ' C19 H21 Cl2 N2 P Ti ' _chemical_compound_source ; ? ; _chemical_formula_weight 427.17 _cell_measurement_reflns_used 4287 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.787 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.82 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 17856 _reflns_number_total 4484 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 5.102 _diffrn_reflns_theta_max 27.495 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.495 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -11 _reflns_limit_h_max 12 _reflns_limit_k_min -11 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_diff_density_min -0.32 _refine_diff_density_max 0.27 _refine_ls_number_reflns 3409 _refine_ls_number_restraints 0 _refine_ls_number_parameters 226 #_refine_ls_R_factor_ref 0.0293 _refine_ls_wR_factor_ref 0.0336 _refine_ls_goodness_of_fit_ref 1.0768 #_reflns_number_all 4484 _refine_ls_R_factor_all 0.0432 _refine_ls_wR_factor_all 0.0453 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3409 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_gt 0.0336 _refine_ls_shift/su_max 0.000561 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.499 0.149 0.219 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Ti1 Ti 0.32421(3) 0.15164(3) 0.29958(3) 0.0184 1.0000 Uani Cl1 Cl 0.34466(5) -0.08604(5) 0.44505(4) 0.0306 1.0000 Uani Cl2 Cl 0.11826(5) 0.11921(5) 0.23326(4) 0.0301 1.0000 Uani P1 P 0.27516(5) 0.49701(5) 0.34955(4) 0.0186 1.0000 Uani N1 N 0.28207(15) 0.31627(15) 0.34967(13) 0.0192 1.0000 Uani N2 N 0.18372(16) 0.20151(16) 0.44448(13) 0.0209 1.0000 Uani C1 C 0.2241(2) 0.1556(2) 0.56223(17) 0.0289 1.0000 Uani C2 C 0.0265(2) 0.2354(2) 0.45368(19) 0.0312 1.0000 Uani C3 C 0.47258(19) 0.55024(19) 0.30527(15) 0.0197 1.0000 Uani C4 C 0.5629(2) 0.4563(2) 0.37788(17) 0.0240 1.0000 Uani C5 C 0.7137(2) 0.4876(2) 0.35007(18) 0.0289 1.0000 Uani C6 C 0.7765(2) 0.6146(2) 0.25089(19) 0.0307 1.0000 Uani C7 C 0.6870(2) 0.7110(2) 0.18083(18) 0.0303 1.0000 Uani C8 C 0.5358(2) 0.6793(2) 0.20707(17) 0.0240 1.0000 Uani C9 C 0.21045(18) 0.60973(19) 0.21223(16) 0.0209 1.0000 Uani C10 C 0.1805(2) 0.5523(2) 0.13071(17) 0.0241 1.0000 Uani C11 C 0.1323(2) 0.6464(2) 0.02870(17) 0.0273 1.0000 Uani C12 C 0.1134(2) 0.7983(2) 0.00630(17) 0.0299 1.0000 Uani C13 C 0.1394(2) 0.8556(2) 0.08886(18) 0.0290 1.0000 Uani C14 C 0.1856(2) 0.7614(2) 0.19183(17) 0.0239 1.0000 Uani C15 C 0.5054(2) 0.3264(2) 0.15294(18) 0.0334 1.0000 Uani C16 C 0.4320(2) 0.2677(2) 0.09087(16) 0.0309 1.0000 Uani C17 C 0.4612(2) 0.1129(2) 0.12481(17) 0.0293 1.0000 Uani C18 C 0.5524(2) 0.0769(2) 0.20724(18) 0.0309 1.0000 Uani C19 C 0.5775(2) 0.2078(2) 0.22751(19) 0.0330 1.0000 Uani H11 H 0.3312 0.1333 0.5534 0.0327 1.0000 Uiso H12 H 0.2045 0.2392 0.5923 0.0327 1.0000 Uiso H13 H 0.1641 0.0631 0.6209 0.0327 1.0000 Uiso H21 H 0.0021 0.2662 0.3727 0.0369 1.0000 Uiso H22 H 0.0055 0.3196 0.4830 0.0369 1.0000 Uiso H23 H -0.0349 0.1435 0.5116 0.0369 1.0000 Uiso H41 H 0.5185 0.3658 0.4504 0.0292 1.0000 Uiso H51 H 0.7775 0.4184 0.4017 0.0366 1.0000 Uiso H61 H 0.8853 0.6363 0.2303 0.0390 1.0000 Uiso H71 H 0.7313 0.8041 0.1108 0.0355 1.0000 Uiso H81 H 0.4723 0.7491 0.1554 0.0289 1.0000 Uiso H101 H 0.1939 0.4429 0.1459 0.0290 1.0000 Uiso H111 H 0.1111 0.6041 -0.0290 0.0329 1.0000 Uiso H121 H 0.0813 0.8662 -0.0684 0.0328 1.0000 Uiso H131 H 0.1248 0.9649 0.0739 0.0332 1.0000 Uiso H141 H 0.2011 0.8026 0.2518 0.0287 1.0000 Uiso H151 H 0.5065 0.4339 0.1455 0.0369 1.0000 Uiso H161 H 0.3697 0.3255 0.0327 0.0344 1.0000 Uiso H171 H 0.4232 0.0416 0.0951 0.0354 1.0000 Uiso H181 H 0.5931 -0.0244 0.2454 0.0351 1.0000 Uiso H191 H 0.6359 0.2150 0.2845 0.0394 1.0000 Uiso 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 Ti1 0.02022(15) 0.01427(14) 0.01922(15) -0.00461(12) -0.00439(11) 0.00017(11) Cl1 0.0274(2) 0.0188(2) 0.0341(2) 0.00140(18) -0.00582(18) 0.00322(16) Cl2 0.0324(2) 0.0285(2) 0.0350(2) -0.01364(19) -0.01580(19) -0.00009(18) P1 0.0193(2) 0.0165(2) 0.0195(2) -0.00625(16) -0.00480(16) 0.00211(15) N1 0.0197(7) 0.0158(6) 0.0177(7) -0.0028(5) -0.0018(5) -0.0012(5) N2 0.0193(7) 0.0198(7) 0.0187(7) -0.0032(6) -0.0016(5) -0.0016(5) C1 0.0356(10) 0.0273(9) 0.0187(8) -0.0038(7) -0.0044(7) -0.0037(8) C2 0.0193(9) 0.0348(10) 0.0381(11) -0.0151(9) -0.0008(8) -0.0011(7) C3 0.0224(8) 0.0182(8) 0.0212(8) -0.0095(7) -0.0064(6) 0.0018(6) C4 0.0255(9) 0.0224(8) 0.0251(9) -0.0085(7) -0.0086(7) 0.0018(7) C5 0.0257(9) 0.0315(10) 0.0342(10) -0.0142(8) -0.0143(8) 0.0066(7) C6 0.0206(9) 0.0394(11) 0.0376(11) -0.0206(9) -0.0057(8) -0.0011(7) C7 0.0275(10) 0.0297(10) 0.0315(10) -0.0100(8) -0.0039(8) -0.0056(7) C8 0.0243(9) 0.0223(8) 0.0258(9) -0.0086(7) -0.0070(7) 0.0001(7) C9 0.0168(8) 0.0192(8) 0.0242(8) -0.0049(7) -0.0058(6) 0.0011(6) C10 0.0250(9) 0.0213(8) 0.0263(9) -0.0089(7) -0.0072(7) 0.0037(7) C11 0.0264(9) 0.0312(10) 0.0247(9) -0.0096(8) -0.0086(7) 0.0029(7) C12 0.0254(9) 0.0309(10) 0.0258(9) -0.0012(8) -0.0093(7) 0.0049(7) C13 0.0286(10) 0.0199(8) 0.0344(10) -0.0046(8) -0.0105(8) 0.0050(7) C14 0.0228(8) 0.0196(8) 0.0294(9) -0.0088(7) -0.0070(7) 0.0015(6) C15 0.0393(11) 0.0252(9) 0.0277(10) -0.0116(8) 0.0138(8) -0.0097(8) C16 0.0430(11) 0.0253(9) 0.0177(9) -0.0049(7) 0.0007(8) 0.0028(8) C17 0.0370(10) 0.0260(9) 0.0255(9) -0.0143(8) 0.0006(8) 0.0000(8) C18 0.0271(9) 0.0308(10) 0.0297(10) -0.0113(8) 0.0023(8) 0.0056(8) C19 0.0233(9) 0.0436(12) 0.0317(10) -0.0190(9) 0.0050(8) -0.0071(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3270(5) yes Ti1 . Cl2 . 2.3165(5) yes Ti1 . N1 . 1.9013(14) yes Ti1 . N2 . 2.1689(15) yes Ti1 . C15 . 2.3518(19) yes Ti1 . C16 . 2.3743(18) yes Ti1 . C17 . 2.4021(19) yes Ti1 . C18 . 2.3970(19) yes Ti1 . C19 . 2.3389(19) yes P1 . N1 . 1.7319(14) yes P1 . C3 . 1.8355(18) yes P1 . C9 . 1.8353(18) yes N1 . N2 . 1.4337(19) yes N2 . C1 . 1.473(2) yes N2 . C2 . 1.473(2) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . C4 . 1.398(2) yes C3 . C8 . 1.396(2) yes C4 . C5 . 1.388(3) yes C4 . H41 . 1.000 no C5 . C6 . 1.390(3) yes C5 . H51 . 1.000 no C6 . C7 . 1.385(3) yes C6 . H61 . 1.000 no C7 . C8 . 1.394(3) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.396(3) yes C9 . C14 . 1.396(2) yes C10 . C11 . 1.389(3) yes C10 . H101 . 1.000 no C11 . C12 . 1.386(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.395(3) yes C12 . H121 . 1.000 no C13 . C14 . 1.389(3) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.401(3) yes C15 . C19 . 1.407(3) yes C15 . H151 . 1.000 no C16 . C17 . 1.410(3) yes C16 . H161 . 1.000 no C17 . C18 . 1.396(3) yes C17 . H171 . 1.000 no C18 . C19 . 1.410(3) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl2 . 102.78(2) yes Cl1 . Ti1 . N1 . 118.27(5) yes Cl2 . Ti1 . N1 . 105.00(5) yes Cl1 . Ti1 . N2 . 86.21(4) yes Cl2 . Ti1 . N2 . 90.04(4) yes N1 . Ti1 . N2 . 40.58(5) yes Cl1 . Ti1 . C15 . 130.97(6) yes Cl2 . Ti1 . C15 . 115.08(6) yes N1 . Ti1 . C15 . 81.63(6) yes N2 . Ti1 . C15 . 122.00(6) yes Cl1 . Ti1 . C16 . 132.75(5) yes Cl2 . Ti1 . C16 . 84.07(6) yes N1 . Ti1 . C16 . 104.20(6) yes N2 . Ti1 . C16 . 140.95(6) yes C15 . Ti1 . C16 . 34.49(8) yes Cl1 . Ti1 . C17 . 98.96(5) yes Cl2 . Ti1 . C17 . 84.91(5) yes N1 . Ti1 . C17 . 137.21(6) yes N2 . Ti1 . C17 . 173.45(7) yes C15 . Ti1 . C17 . 57.16(7) yes Cl1 . Ti1 . C18 . 79.16(5) yes Cl2 . Ti1 . C18 . 115.87(5) yes N1 . Ti1 . C18 . 130.71(7) yes N2 . Ti1 . C18 . 152.40(7) yes C15 . Ti1 . C18 . 57.20(7) yes Cl1 . Ti1 . C19 . 96.23(6) yes Cl2 . Ti1 . C19 . 140.00(6) yes N1 . Ti1 . C19 . 96.10(7) yes N2 . Ti1 . C19 . 126.41(6) yes C15 . Ti1 . C19 . 34.92(8) yes C16 . Ti1 . C17 . 34.34(6) yes C16 . Ti1 . C18 . 56.80(7) yes C17 . Ti1 . C18 . 33.82(7) yes C16 . Ti1 . C19 . 57.68(8) yes C17 . Ti1 . C19 . 57.32(7) yes C18 . Ti1 . C19 . 34.61(7) yes N1 . P1 . C3 . 100.18(7) yes N1 . P1 . C9 . 103.84(7) yes C3 . P1 . C9 . 102.23(8) yes Ti1 . N1 . P1 . 161.83(9) yes Ti1 . N1 . N2 . 79.79(9) yes P1 . N1 . N2 . 117.90(11) yes Ti1 . N2 . N1 . 59.63(8) yes Ti1 . N2 . C1 . 120.49(12) yes N1 . N2 . C1 . 113.14(13) yes Ti1 . N2 . C2 . 125.60(12) yes N1 . N2 . C2 . 114.57(14) yes C1 . N2 . C2 . 111.14(15) yes N2 . C1 . H11 . 109.467 no N2 . C1 . H12 . 109.467 no H11 . C1 . H12 . 109.476 no N2 . C1 . H13 . 109.467 no H11 . C1 . H13 . 109.476 no H12 . C1 . H13 . 109.476 no N2 . C2 . H21 . 109.467 no N2 . C2 . H22 . 109.466 no H21 . C2 . H22 . 109.476 no N2 . C2 . H23 . 109.467 no H21 . C2 . H23 . 109.476 no H22 . C2 . H23 . 109.476 no P1 . C3 . C4 . 116.83(13) yes P1 . C3 . C8 . 124.27(13) yes C4 . C3 . C8 . 118.87(16) yes C3 . C4 . C5 . 120.51(17) yes C3 . C4 . H41 . 119.744 no C5 . C4 . H41 . 119.744 no C4 . C5 . C6 . 120.37(17) yes C4 . C5 . H51 . 119.816 no C6 . C5 . H51 . 119.816 no C5 . C6 . C7 . 119.44(18) yes C5 . C6 . H61 . 120.278 no C7 . C6 . H61 . 120.279 no C6 . C7 . C8 . 120.56(18) yes C6 . C7 . H71 . 119.718 no C8 . C7 . H71 . 119.718 no C3 . C8 . C7 . 120.19(17) yes C3 . C8 . H81 . 119.907 no C7 . C8 . H81 . 119.906 no P1 . C9 . C10 . 124.34(13) yes P1 . C9 . C14 . 116.75(14) yes C10 . C9 . C14 . 118.87(16) yes C9 . C10 . C11 . 120.37(17) yes C9 . C10 . H101 . 119.816 no C11 . C10 . H101 . 119.816 no C10 . C11 . C12 . 120.55(17) yes C10 . C11 . H111 . 119.724 no C12 . C11 . H111 . 119.724 no C11 . C12 . C13 . 119.40(17) yes C11 . C12 . H121 . 120.299 no C13 . C12 . H121 . 120.298 no C12 . C13 . C14 . 120.17(17) yes C12 . C13 . H131 . 119.913 no C14 . C13 . H131 . 119.914 no C9 . C14 . C13 . 120.54(17) yes C9 . C14 . H141 . 119.729 no C13 . C14 . H141 . 119.728 no Ti1 . C15 . C16 . 73.64(11) yes Ti1 . C15 . C19 . 72.04(11) yes C16 . C15 . C19 . 108.10(17) yes Ti1 . C15 . H151 . 120.170 no C16 . C15 . H151 . 125.951 no C19 . C15 . H151 . 125.951 no Ti1 . C16 . C15 . 71.88(11) yes Ti1 . C16 . C17 . 73.91(11) yes C15 . C16 . C17 . 108.01(18) yes Ti1 . C16 . H161 . 120.022 no C15 . C16 . H161 . 125.997 no C17 . C16 . H161 . 125.997 no Ti1 . C17 . C16 . 71.75(11) yes Ti1 . C17 . C18 . 72.89(11) yes C16 . C17 . C18 . 107.94(18) yes Ti1 . C17 . H171 . 121.089 no C16 . C17 . H171 . 126.028 no C18 . C17 . H171 . 126.028 no Ti1 . C18 . C17 . 73.29(11) yes Ti1 . C18 . C19 . 70.44(11) yes C17 . C18 . C19 . 108.31(18) yes Ti1 . C18 . H181 . 122.094 no C17 . C18 . H181 . 125.847 no C19 . C18 . H181 . 125.847 no Ti1 . C19 . C15 . 73.04(11) yes Ti1 . C19 . C18 . 74.95(11) yes C15 . C19 . C18 . 107.59(18) yes Ti1 . C19 . H191 . 117.823 no C15 . C19 . H191 . 126.203 no C18 . C19 . H191 . 126.203 no data_arc752 _database_code_depnum_ccdc_archive 'CCDC 255290' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; The NH hydrogen atom was located in a difference Fourier map and its coordinates and isotropic thermal parameters subsequently refined. Other H atoms were positioned geometrically, the preferred orientation of the methyl group H241-H243 having been determined by examination of the difference Fourier map ; #============================================================= _cell_length_a 18.7070(4) _cell_angle_alpha 90 _cell_length_b 13.7367(3) _cell_angle_beta 90 _cell_length_c 18.8545(5) _cell_angle_gamma 90 _cell_volume 4845.1(2) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C24 H31 Cl2 N2 P1 Ru1 ' _chemical_formula_moiety ' C24 H31 Cl2 N2 P1 Ru1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 550.47 _cell_measurement_reflns_used 31161 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.948 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.94 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 31161 _reflns_number_total 5494 #6061 unique data including absences _diffrn_reflns_av_R_equivalents 0.081 _diffrn_reflns_theta_min 5.246 _diffrn_reflns_theta_max 27.475 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.651 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _refine_diff_density_min -0.62 _refine_diff_density_max 0.47 _refine_ls_number_reflns 3207 _refine_ls_number_restraints 0 _refine_ls_number_parameters 275 #_refine_ls_R_factor_ref 0.0295 _refine_ls_wR_factor_ref 0.0306 _refine_ls_goodness_of_fit_ref 1.1166 #_reflns_number_all 5494 _refine_ls_R_factor_all 0.0732 _refine_ls_wR_factor_all 0.0722 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3207 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_gt 0.0306 _refine_ls_shift/su_max 0.006303 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.212 0.350E-01 0.390E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Ru1 Ru 0.461663(14) 0.233682(18) 0.272489(14) 0.0168 1.0000 Uani Cl1 Cl 0.49290(5) 0.37086(6) 0.34610(5) 0.0289 1.0000 Uani Cl2 Cl 0.44731(5) 0.34833(6) 0.17677(5) 0.0273 1.0000 Uani P1 P 0.58153(4) 0.22704(6) 0.24050(4) 0.0164 1.0000 Uani N1 N 0.61726(16) 0.3371(2) 0.22680(17) 0.0218 1.0000 Uani N2 N 0.68612(15) 0.3402(2) 0.19354(15) 0.0217 1.0000 Uani C1 C 0.7308(2) 0.4114(3) 0.2299(2) 0.0302 1.0000 Uani C2 C 0.6788(2) 0.3647(3) 0.1182(2) 0.0313 1.0000 Uani C3 C 0.60207(17) 0.1558(2) 0.16156(18) 0.0183 1.0000 Uani C4 C 0.55192(18) 0.1524(3) 0.10674(19) 0.0235 1.0000 Uani C5 C 0.5683(2) 0.1077(3) 0.0427(2) 0.0309 1.0000 Uani C6 C 0.6352(2) 0.0659(3) 0.0324(2) 0.0338 1.0000 Uani C7 C 0.6849(2) 0.0688(3) 0.0865(2) 0.0306 1.0000 Uani C8 C 0.6696(2) 0.1135(3) 0.15094(19) 0.0233 1.0000 Uani C9 C 0.63667(18) 0.1763(2) 0.31076(18) 0.0193 1.0000 Uani C10 C 0.64441(19) 0.0762(3) 0.31865(18) 0.0216 1.0000 Uani C11 C 0.6790(2) 0.0385(3) 0.3780(2) 0.0286 1.0000 Uani C12 C 0.7048(2) 0.1003(3) 0.4299(2) 0.0319 1.0000 Uani C13 C 0.6975(2) 0.2002(3) 0.42276(19) 0.0300 1.0000 Uani C14 C 0.66294(19) 0.2389(3) 0.36358(18) 0.0251 1.0000 Uani C15 C 0.41909(19) 0.1614(2) 0.36900(19) 0.0224 1.0000 Uani C16 C 0.46155(19) 0.0951(2) 0.33152(17) 0.0200 1.0000 Uani C17 C 0.44918(17) 0.0763(2) 0.25773(18) 0.0194 1.0000 Uani C18 C 0.39237(19) 0.1225(3) 0.2216(2) 0.0252 1.0000 Uani C19 C 0.34756(18) 0.1874(3) 0.2608(2) 0.0272 1.0000 Uani C20 C 0.3599(2) 0.2067(3) 0.3321(2) 0.0261 1.0000 Uani C21 C 0.4309(2) 0.1850(3) 0.44675(19) 0.0267 1.0000 Uani C22 C 0.5033(2) 0.1539(3) 0.4741(2) 0.0399 1.0000 Uani C23 C 0.3704(3) 0.1391(4) 0.4900(2) 0.0462 1.0000 Uani C24 C 0.3773(2) 0.1003(3) 0.1448(2) 0.0385 1.0000 Uani H1 H 0.591(2) 0.379(3) 0.212(2) 0.027(11) 1.0000 Uiso H11 H 0.7789 0.4137 0.2068 0.0362 1.0000 Uiso H12 H 0.7363 0.3923 0.2807 0.0362 1.0000 Uiso H13 H 0.7079 0.4770 0.2270 0.0362 1.0000 Uiso H21 H 0.7271 0.3666 0.0956 0.0376 1.0000 Uiso H22 H 0.6554 0.4298 0.1134 0.0376 1.0000 Uiso H23 H 0.6487 0.3143 0.0942 0.0376 1.0000 Uiso H41 H 0.5037 0.1825 0.1137 0.0282 1.0000 Uiso H51 H 0.5319 0.1056 0.0039 0.0370 1.0000 Uiso H61 H 0.6472 0.0341 -0.0138 0.0405 1.0000 Uiso H71 H 0.7328 0.0382 0.0792 0.0367 1.0000 Uiso H81 H 0.7064 0.1156 0.1894 0.0279 1.0000 Uiso H101 H 0.6251 0.0312 0.2816 0.0259 1.0000 Uiso H111 H 0.6851 -0.0335 0.3831 0.0343 1.0000 Uiso H121 H 0.7288 0.0728 0.4728 0.0382 1.0000 Uiso H131 H 0.7170 0.2446 0.4601 0.0361 1.0000 Uiso H141 H 0.6569 0.3109 0.3588 0.0302 1.0000 Uiso H161 H 0.5011 0.0604 0.3566 0.0240 1.0000 Uiso H171 H 0.4810 0.0300 0.2316 0.0233 1.0000 Uiso H191 H 0.3064 0.2196 0.2365 0.0326 1.0000 Uiso H201 H 0.3276 0.2523 0.3582 0.0313 1.0000 Uiso H211 H 0.4302 0.2575 0.4521 0.0321 1.0000 Uiso H221 H 0.5076 0.1714 0.5253 0.0479 1.0000 Uiso H222 H 0.5416 0.1877 0.4464 0.0479 1.0000 Uiso H223 H 0.5086 0.0818 0.4684 0.0479 1.0000 Uiso H231 H 0.3774 0.1541 0.5414 0.0554 1.0000 Uiso H232 H 0.3707 0.0669 0.4829 0.0554 1.0000 Uiso H233 H 0.3235 0.1662 0.4739 0.0554 1.0000 Uiso H241 H 0.4140 0.0539 0.1264 0.0462 1.0000 Uiso H242 H 0.3790 0.1619 0.1166 0.0462 1.0000 Uiso H243 H 0.3287 0.0704 0.1404 0.0462 1.0000 Uiso 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 0.01742(12) 0.01488(11) 0.01820(12) 0.00078(11) 0.00153(12) 0.00160(11) Cl1 0.0429(5) 0.0177(4) 0.0260(4) -0.0036(3) 0.0084(4) -0.0054(4) Cl2 0.0312(5) 0.0252(4) 0.0256(4) 0.0072(3) -0.0012(4) 0.0065(4) P1 0.0174(4) 0.0143(4) 0.0175(4) 0.0005(3) 0.0013(3) -0.0002(3) N1 0.0204(14) 0.0172(14) 0.0279(15) 0.0037(13) 0.0026(14) -0.0013(12) N2 0.0207(15) 0.0211(14) 0.0234(15) 0.0029(12) 0.0046(13) -0.0021(12) C1 0.0271(19) 0.0268(18) 0.037(2) 0.0009(18) 0.0037(17) -0.0091(15) C2 0.036(2) 0.032(2) 0.026(2) 0.0094(16) 0.0044(17) -0.0063(17) C3 0.0185(17) 0.0148(16) 0.0215(17) 0.0025(13) 0.0007(14) 0.0004(13) C4 0.0212(19) 0.0257(18) 0.0235(17) -0.0019(15) 0.0002(14) 0.0003(14) C5 0.038(2) 0.032(2) 0.0223(18) -0.0049(15) -0.0042(17) 0.0012(17) C6 0.049(3) 0.029(2) 0.0230(19) -0.0047(16) 0.0076(19) 0.0078(18) C7 0.035(2) 0.030(2) 0.027(2) -0.0017(16) 0.0046(17) 0.0103(17) C8 0.0229(18) 0.0228(18) 0.0241(18) 0.0005(14) -0.0003(15) 0.0020(14) C9 0.0175(17) 0.0198(17) 0.0204(17) 0.0019(14) 0.0005(14) 0.0016(13) C10 0.0206(17) 0.0233(18) 0.0208(17) 0.0037(14) 0.0031(15) 0.0015(14) C11 0.025(2) 0.033(2) 0.028(2) 0.0096(16) 0.0034(16) 0.0065(16) C12 0.027(2) 0.048(3) 0.0206(18) 0.0082(17) -0.0009(16) 0.0051(18) C13 0.027(2) 0.044(2) 0.0191(18) -0.0023(16) -0.0029(16) -0.0030(17) C14 0.0232(17) 0.0281(19) 0.0241(17) -0.0007(16) 0.0035(14) -0.0026(15) C15 0.0249(19) 0.0186(17) 0.0237(18) -0.0017(14) 0.0078(15) -0.0036(14) C16 0.0213(16) 0.0170(16) 0.0217(17) 0.0024(13) 0.0012(16) -0.0051(15) C17 0.0209(18) 0.0128(14) 0.0245(17) -0.0043(13) 0.0024(13) -0.0033(12) C18 0.0233(18) 0.0237(17) 0.0285(18) -0.0017(16) 0.0014(16) -0.0074(14) C19 0.0150(17) 0.031(2) 0.035(2) 0.0053(16) -0.0048(15) -0.0028(14) C20 0.0213(18) 0.0242(19) 0.033(2) 0.0027(15) 0.0073(16) 0.0039(14) C21 0.035(2) 0.0242(19) 0.0206(18) -0.0043(14) 0.0058(16) -0.0067(16) C22 0.046(3) 0.050(3) 0.0240(18) 0.0009(19) -0.004(2) -0.005(2) C23 0.054(3) 0.059(3) 0.026(2) -0.001(2) 0.012(2) -0.024(2) C24 0.033(2) 0.051(3) 0.032(2) 0.0020(19) -0.0075(18) -0.013(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . Cl1 . 2.4122(9) yes Ru1 . Cl2 . 2.4103(9) yes Ru1 . P1 . 2.3238(8) yes Ru1 . C15 . 2.220(3) yes Ru1 . C16 . 2.205(3) yes Ru1 . C17 . 2.193(3) yes Ru1 . C18 . 2.221(3) yes Ru1 . C19 . 2.238(3) yes Ru1 . C20 . 2.241(4) yes P1 . N1 . 1.673(3) yes P1 . C3 . 1.822(3) yes P1 . C9 . 1.818(3) yes N1 . N2 . 1.433(4) yes N1 . H1 . 0.80(4) yes N2 . C1 . 1.457(5) yes N2 . C2 . 1.466(5) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . C4 . 1.397(5) yes C3 . C8 . 1.406(5) yes C4 . C5 . 1.389(5) yes C4 . H41 . 1.000 no C5 . C6 . 1.392(6) yes C5 . H51 . 1.000 no C6 . C7 . 1.381(6) yes C6 . H61 . 1.000 no C7 . C8 . 1.392(5) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.390(5) yes C9 . C14 . 1.405(5) yes C10 . C11 . 1.392(5) yes C10 . H101 . 1.000 no C11 . C12 . 1.382(6) yes C11 . H111 . 1.000 no C12 . C13 . 1.386(6) yes C12 . H121 . 1.000 no C13 . C14 . 1.395(5) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.400(5) yes C15 . C20 . 1.448(5) yes C15 . C21 . 1.517(5) yes C16 . C17 . 1.434(5) yes C16 . H161 . 1.000 no C17 . C18 . 1.414(5) yes C17 . H171 . 1.000 no C18 . C19 . 1.430(5) yes C18 . C24 . 1.507(5) yes C19 . C20 . 1.388(5) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.511(6) yes C21 . C23 . 1.531(5) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ru1 . Cl2 . 86.98(3) yes Cl1 . Ru1 . P1 . 86.92(3) yes Cl2 . Ru1 . P1 . 86.49(3) yes Cl1 . Ru1 . C15 . 87.97(9) yes Cl2 . Ru1 . C15 . 149.97(10) yes P1 . Ru1 . C15 . 122.77(10) yes Cl1 . Ru1 . C16 . 112.59(9) yes Cl2 . Ru1 . C16 . 160.38(9) yes P1 . Ru1 . C16 . 95.62(10) yes C15 . Ru1 . C16 . 36.88(13) yes Cl1 . Ru1 . C17 . 150.37(9) yes Cl2 . Ru1 . C17 . 122.51(9) yes P1 . Ru1 . C17 . 91.78(9) yes C15 . Ru1 . C17 . 67.98(12) yes C16 . Ru1 . C17 . 38.06(12) yes Cl1 . Ru1 . C18 . 157.99(10) yes Cl2 . Ru1 . C18 . 93.46(10) yes P1 . Ru1 . C18 . 115.09(10) yes C15 . Ru1 . C18 . 80.66(13) yes C16 . Ru1 . C18 . 67.94(13) yes Cl1 . Ru1 . C19 . 120.63(10) yes Cl2 . Ru1 . C19 . 90.34(10) yes P1 . Ru1 . C19 . 152.09(10) yes C15 . Ru1 . C19 . 67.13(14) yes C16 . Ru1 . C19 . 78.66(13) yes Cl1 . Ru1 . C20 . 92.67(10) yes Cl2 . Ru1 . C20 . 112.89(10) yes P1 . Ru1 . C20 . 160.58(10) yes C15 . Ru1 . C20 . 37.87(13) yes C16 . Ru1 . C20 . 66.62(13) yes C17 . Ru1 . C18 . 37.36(13) yes C17 . Ru1 . C19 . 66.78(13) yes C18 . Ru1 . C19 . 37.40(13) yes C17 . Ru1 . C20 . 79.04(13) yes C18 . Ru1 . C20 . 66.88(14) yes C19 . Ru1 . C20 . 36.12(14) yes Ru1 . P1 . N1 . 112.96(11) yes Ru1 . P1 . C3 . 115.89(11) yes N1 . P1 . C3 . 105.95(15) yes Ru1 . P1 . C9 . 111.93(11) yes N1 . P1 . C9 . 103.44(16) yes C3 . P1 . C9 . 105.64(15) yes P1 . N1 . N2 . 116.9(2) yes P1 . N1 . H1 . 117(3) yes N2 . N1 . H1 . 112(3) yes N1 . N2 . C1 . 109.2(3) yes N1 . N2 . C2 . 110.3(3) yes C1 . N2 . C2 . 110.8(3) yes N2 . C1 . H11 . 109.467 no N2 . C1 . H12 . 109.467 no H11 . C1 . H12 . 109.476 no N2 . C1 . H13 . 109.467 no H11 . C1 . H13 . 109.476 no H12 . C1 . H13 . 109.476 no N2 . C2 . H21 . 109.467 no N2 . C2 . H22 . 109.466 no H21 . C2 . H22 . 109.476 no N2 . C2 . H23 . 109.467 no H21 . C2 . H23 . 109.476 no H22 . C2 . H23 . 109.476 no P1 . C3 . C4 . 118.7(2) yes P1 . C3 . C8 . 121.9(3) yes C4 . C3 . C8 . 119.0(3) yes C3 . C4 . C5 . 120.7(3) yes C3 . C4 . H41 . 119.670 no C5 . C4 . H41 . 119.670 no C4 . C5 . C6 . 120.2(4) yes C4 . C5 . H51 . 119.897 no C6 . C5 . H51 . 119.897 no C5 . C6 . C7 . 119.4(3) yes C5 . C6 . H61 . 120.324 no C7 . C6 . H61 . 120.324 no C6 . C7 . C8 . 121.3(4) yes C6 . C7 . H71 . 119.334 no C8 . C7 . H71 . 119.334 no C3 . C8 . C7 . 119.4(3) yes C3 . C8 . H81 . 120.281 no C7 . C8 . H81 . 120.281 no P1 . C9 . C10 . 121.1(3) yes P1 . C9 . C14 . 118.7(3) yes C10 . C9 . C14 . 119.6(3) yes C9 . C10 . C11 . 120.2(3) yes C9 . C10 . H101 . 119.918 no C11 . C10 . H101 . 119.918 no C10 . C11 . C12 . 120.1(4) yes C10 . C11 . H111 . 119.944 no C12 . C11 . H111 . 119.944 no C11 . C12 . C13 . 120.4(3) yes C11 . C12 . H121 . 119.794 no C13 . C12 . H121 . 119.794 no C12 . C13 . C14 . 120.0(4) yes C12 . C13 . H131 . 119.997 no C14 . C13 . H131 . 119.997 no C9 . C14 . C13 . 119.7(3) yes C9 . C14 . H141 . 120.140 no C13 . C14 . H141 . 120.140 no Ru1 . C15 . C16 . 70.96(19) yes Ru1 . C15 . C20 . 71.8(2) yes C16 . C15 . C20 . 118.1(3) yes Ru1 . C15 . C21 . 130.1(2) yes C16 . C15 . C21 . 123.0(3) yes C20 . C15 . C21 . 118.9(3) yes Ru1 . C16 . C15 . 72.2(2) yes Ru1 . C16 . C17 . 70.51(18) yes C15 . C16 . C17 . 121.0(3) yes Ru1 . C16 . H161 . 130.561 no C15 . C16 . H161 . 119.477 no C17 . C16 . H161 . 119.477 no Ru1 . C17 . C16 . 71.43(18) yes Ru1 . C17 . C18 . 72.40(19) yes C16 . C17 . C18 . 120.5(3) yes Ru1 . C17 . H171 . 128.743 no C16 . C17 . H171 . 119.735 no C18 . C17 . H171 . 119.735 no Ru1 . C18 . C17 . 70.24(18) yes Ru1 . C18 . C19 . 71.9(2) yes C17 . C18 . C19 . 118.1(3) yes Ru1 . C18 . C24 . 131.6(3) yes C17 . C18 . C24 . 120.9(3) yes C19 . C18 . C24 . 120.9(3) yes Ru1 . C19 . C18 . 70.66(19) yes Ru1 . C19 . C20 . 72.1(2) yes C18 . C19 . C20 . 121.5(3) yes Ru1 . C19 . H191 . 130.836 no C18 . C19 . H191 . 119.256 no C20 . C19 . H191 . 119.256 no Ru1 . C20 . C15 . 70.29(19) yes Ru1 . C20 . C19 . 71.8(2) yes C15 . C20 . C19 . 120.7(3) yes Ru1 . C20 . H201 . 131.015 no C15 . C20 . H201 . 119.650 no C19 . C20 . H201 . 119.650 no C15 . C21 . C22 . 113.5(3) yes C15 . C21 . C23 . 108.6(3) yes C22 . C21 . C23 . 111.4(3) yes C15 . C21 . H211 . 107.996 no C22 . C21 . H211 . 105.016 no C23 . C21 . H211 . 110.277 no C21 . C22 . H221 . 109.467 no C21 . C22 . H222 . 109.467 no H221 . C22 . H222 . 109.476 no C21 . C22 . H223 . 109.467 no H221 . C22 . H223 . 109.476 no H222 . C22 . H223 . 109.476 no C21 . C23 . H231 . 109.467 no C21 . C23 . H232 . 109.467 no H231 . C23 . H232 . 109.476 no C21 . C23 . H233 . 109.467 no H231 . C23 . H233 . 109.476 no H232 . C23 . H233 . 109.476 no C18 . C24 . H241 . 109.467 no C18 . C24 . H242 . 109.467 no H241 . C24 . H242 . 109.476 no C18 . C24 . H243 . 109.467 no H241 . C24 . H243 . 109.476 no H242 . C24 . H243 . 109.476 no data_arc863 _database_code_depnum_ccdc_archive 'CCDC 255291' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _chemical_absolute_configuration ad _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; Geometric restraints were applied to the disordered solvent. The C-Cl bond lengths were restrained to 1.78(2) \%A and the Cl-C-Cl angles to 112(2) \%. Vibrational simiarity restraints were applied to the pairs of nearly-overlapping atoms. The NH hydrogen atom was located in a difference Fourier map and its coordinates and isotropic thermal parameter subsequently refined. Other hydrogen atroms were positioned geometrically, the preferred orientation of the methyl group H271-H273 having been previously identified by examination of the Fourier map. ; #============================================================= _cell_length_a 7.4308(2) _cell_angle_alpha 90 _cell_length_b 13.7935(2) _cell_angle_beta 90 _cell_length_c 29.5131(4) _cell_angle_gamma 90 _cell_volume 3025.00(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C28 H38 Cl4 N3 P1 Ru1 ' _chemical_formula_moiety ' C27 H36 Cl2 N3 P Ru, C H2 Cl2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 690.48 _cell_measurement_reflns_used 23307 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' orange-brown ' _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.948 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 23307 _reflns_number_total 6723 #6749 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_min 5.186 _diffrn_reflns_theta_max 27.484 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.484 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 38 _refine_diff_density_min -1.07 _refine_diff_density_max 0.60 _refine_ls_number_reflns 5178 _refine_ls_number_restraints 9 _refine_ls_number_parameters 337 #_refine_ls_R_factor_ref 0.0398 _refine_ls_wR_factor_ref 0.0438 _refine_ls_goodness_of_fit_ref 1.0803 #_reflns_number_all 6723 _refine_ls_R_factor_all 0.0611 _refine_ls_wR_factor_all 0.0637 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5178 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_gt 0.0438 _refine_ls_shift/su_max 0.012345 _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_abs_structure_details 'Flack, 2825 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.509 0.0845 0.260 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_group Ru1 Ru 0.39843(5) 0.46384(2) 0.268450(12) 0.0173 1.0000 Uani . . . . Cl1 Cl 0.65705(14) 0.35726(8) 0.26378(4) 0.0264 1.0000 Uani . . . . Cl2 Cl 0.59338(18) 0.57401(8) 0.30852(4) 0.0268 1.0000 Uani . . . . P1 P 0.34470(14) 0.39342(8) 0.33863(4) 0.0173 1.0000 Uani . . . . N1 N 0.5369(5) 0.3746(3) 0.36798(13) 0.0200 1.0000 Uani . . . . N2 N 0.5299(5) 0.3054(3) 0.40414(13) 0.0199 1.0000 Uani . . . . C1 C 0.5979(7) 0.2122(3) 0.38901(15) 0.0241 1.0000 Uani . . . . C2 C 0.5901(8) 0.1394(3) 0.42771(17) 0.0289 1.0000 Uani . . . . C3 C 0.6425(6) 0.3403(3) 0.44212(15) 0.0215 1.0000 Uani . . . . C4 C 0.6336(6) 0.2688(3) 0.48079(15) 0.0237 1.0000 Uani . . . . N3 N 0.6980(6) 0.1722(3) 0.46589(13) 0.0268 1.0000 Uani . . . . C5 C 0.6881(8) 0.1029(5) 0.50295(19) 0.0395 1.0000 Uani . . . . C6 C 0.2272(6) 0.2772(3) 0.33853(17) 0.0214 1.0000 Uani . . . . C7 C 0.1370(6) 0.2430(4) 0.37697(16) 0.0244 1.0000 Uani . . . . C8 C 0.0733(6) 0.1498(3) 0.37916(17) 0.0260 1.0000 Uani . . . . C9 C 0.0988(7) 0.0866(3) 0.34242(18) 0.0303 1.0000 Uani . . . . C10 C 0.1876(6) 0.1193(3) 0.30383(17) 0.0238 1.0000 Uani . . . . C11 C 0.2516(6) 0.2143(3) 0.30206(16) 0.0208 1.0000 Uani . . . . C12 C 0.2131(6) 0.4710(4) 0.37560(15) 0.0218 1.0000 Uani . . . . C13 C 0.3018(6) 0.5390(4) 0.40158(16) 0.0262 1.0000 Uani . . . . C14 C 0.2023(8) 0.6073(4) 0.42663(19) 0.0348 1.0000 Uani . . . . C15 C 0.0156(8) 0.6071(4) 0.4245(2) 0.0343 1.0000 Uani . . . . C16 C -0.0726(6) 0.5398(4) 0.39833(17) 0.0301 1.0000 Uani . . . . C17 C 0.0254(6) 0.4712(4) 0.37430(16) 0.0231 1.0000 Uani . . . . C18 C 0.3151(7) 0.4200(3) 0.19850(16) 0.0250 1.0000 Uani . . . . C19 C 0.1717(6) 0.4024(3) 0.22953(18) 0.0268 1.0000 Uani . . . . C20 C 0.1085(6) 0.4776(3) 0.25847(14) 0.0244 1.0000 Uani . . . . C21 C 0.1833(6) 0.5721(3) 0.25707(16) 0.0251 1.0000 Uani . . . . C22 C 0.3233(6) 0.5877(3) 0.22476(16) 0.0230 1.0000 Uani . . . . C23 C 0.3890(7) 0.5165(3) 0.19620(14) 0.0252 1.0000 Uani . . . . C24 C 0.3800(10) 0.3369(3) 0.16873(17) 0.0394 1.0000 Uani . . . . C25 C 0.2321(12) 0.3141(6) 0.1337(2) 0.0605 1.0000 Uani . . . . C26 C 0.5601(10) 0.3557(5) 0.1458(2) 0.0472 1.0000 Uani . . . . C27 C 0.1211(7) 0.6504(4) 0.28827(18) 0.0333 1.0000 Uani . . . . C28 C 0.061(3) 0.8567(13) 0.4719(6) 0.107(5) 0.575(7) Uiso D U P 1 Cl3 Cl 0.1095(8) 0.7784(3) 0.51900(16) 0.0524(9) 0.575(7) Uiso D U P 1 Cl4 Cl 0.2051(9) 0.9596(5) 0.46852(19) 0.1033(14) 0.575(7) Uiso D U P 1 C38 C 0.186(4) 0.8511(14) 0.4648(7) 0.107(5) 0.425(7) Uiso D U P 2 Cl13 Cl 0.1139(11) 0.7967(5) 0.5157(2) 0.0536(12) 0.425(7) Uiso D U P 2 Cl14 Cl 0.0936(13) 0.9659(6) 0.4625(2) 0.1061(16) 0.425(7) Uiso D U P 2 H1 H 0.621(8) 0.365(4) 0.3488(18) 0.025(14) 1.0000 Uiso . . . . H11 H 0.7254 0.2196 0.3787 0.0289 1.0000 Uiso . . . . H12 H 0.5226 0.1882 0.3632 0.0289 1.0000 Uiso . . . . H21 H 0.4623 0.1317 0.4377 0.0346 1.0000 Uiso . . . . H22 H 0.6373 0.0756 0.4169 0.0346 1.0000 Uiso . . . . H31 H 0.5972 0.4048 0.4526 0.0258 1.0000 Uiso . . . . H32 H 0.7700 0.3469 0.4317 0.0258 1.0000 Uiso . . . . H41 H 0.7110 0.2923 0.5062 0.0284 1.0000 Uiso . . . . H42 H 0.5063 0.2631 0.4914 0.0284 1.0000 Uiso . . . . H51 H 0.7629 0.1264 0.5289 0.0474 1.0000 Uiso . . . . H52 H 0.5602 0.0959 0.5130 0.0474 1.0000 Uiso . . . . H53 H 0.7345 0.0386 0.4925 0.0474 1.0000 Uiso . . . . H71 H 0.1187 0.2874 0.4034 0.0293 1.0000 Uiso . . . . H81 H 0.0087 0.1268 0.4069 0.0312 1.0000 Uiso . . . . H91 H 0.0534 0.0185 0.3440 0.0363 1.0000 Uiso . . . . H101 H 0.2054 0.0748 0.2775 0.0285 1.0000 Uiso . . . . H111 H 0.3157 0.2375 0.2743 0.0250 1.0000 Uiso . . . . H131 H 0.4363 0.5399 0.4026 0.0314 1.0000 Uiso . . . . H141 H 0.2660 0.6559 0.4460 0.0417 1.0000 Uiso . . . . H151 H -0.0548 0.6562 0.4420 0.0412 1.0000 Uiso . . . . H161 H -0.2070 0.5402 0.3966 0.0361 1.0000 Uiso . . . . H171 H -0.0393 0.4214 0.3558 0.0278 1.0000 Uiso . . . . H191 H 0.1152 0.3367 0.2310 0.0321 1.0000 Uiso . . . . H201 H 0.0091 0.4634 0.2803 0.0292 1.0000 Uiso . . . . H221 H 0.3771 0.6540 0.2226 0.0277 1.0000 Uiso . . . . H231 H 0.4870 0.5318 0.1741 0.0302 1.0000 Uiso . . . . H241 H 0.4023 0.2797 0.1888 0.0473 1.0000 Uiso . . . . H251 H 0.2725 0.2596 0.1138 0.0725 1.0000 Uiso . . . . H252 H 0.2087 0.3729 0.1148 0.0725 1.0000 Uiso . . . . H253 H 0.1192 0.2951 0.1499 0.0725 1.0000 Uiso . . . . H261 H 0.5937 0.2983 0.1269 0.0566 1.0000 Uiso . . . . H262 H 0.6545 0.3668 0.1693 0.0566 1.0000 Uiso . . . . H263 H 0.5502 0.4143 0.1260 0.0566 1.0000 Uiso . . . . H271 H 0.0227 0.6249 0.3081 0.0400 1.0000 Uiso . . . . H272 H 0.2240 0.6724 0.3075 0.0400 1.0000 Uiso . . . . H273 H 0.0748 0.7063 0.2701 0.0400 1.0000 Uiso . . . . H281 H -0.0656 0.8799 0.4748 0.1278 0.575 Uiso . . . 1 H282 H 0.0744 0.8184 0.4434 0.1278 0.575 Uiso . . . 1 H381 H 0.3202 0.8554 0.4644 0.1283 0.425 Uiso . . . 2 H382 H 0.1438 0.8119 0.4384 0.1283 0.425 Uiso . . . 2 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 0.01731(15) 0.01582(14) 0.01881(14) 0.00237(15) -0.00169(15) -0.00223(15) Cl1 0.0233(5) 0.0288(5) 0.0271(5) 0.0002(5) 0.0031(5) 0.0047(4) Cl2 0.0284(5) 0.0234(5) 0.0285(5) 0.0018(4) -0.0061(5) -0.0081(5) P1 0.0149(5) 0.0176(5) 0.0194(5) 0.0019(4) -0.0009(4) -0.0012(4) N1 0.0154(17) 0.025(2) 0.0199(19) 0.0054(16) 0.0000(16) 0.0032(15) N2 0.0184(17) 0.023(2) 0.0181(18) 0.0041(15) -0.0036(15) 0.0024(15) C1 0.026(2) 0.025(2) 0.021(2) 0.0024(17) -0.002(2) 0.007(2) C2 0.031(2) 0.022(2) 0.034(2) 0.0038(19) -0.007(2) 0.003(2) C3 0.016(2) 0.027(2) 0.021(2) -0.0017(18) -0.0020(17) 0.0003(17) C4 0.025(3) 0.025(2) 0.020(2) 0.0043(17) -0.0036(19) 0.0012(19) N3 0.029(2) 0.030(2) 0.022(2) 0.0075(17) -0.0012(17) 0.0022(18) C5 0.037(3) 0.049(4) 0.033(3) 0.017(3) -0.007(2) 0.004(3) C6 0.0133(19) 0.023(2) 0.028(2) 0.0081(19) -0.0040(18) 0.0022(17) C7 0.020(2) 0.029(2) 0.024(2) 0.0059(19) 0.0010(18) 0.0000(18) C8 0.023(3) 0.020(2) 0.034(2) 0.0120(19) 0.001(2) 0.0015(19) C9 0.023(2) 0.024(2) 0.043(3) 0.001(2) -0.005(3) -0.008(2) C10 0.018(2) 0.023(2) 0.031(2) -0.001(2) -0.0069(19) -0.0013(18) C11 0.018(2) 0.023(2) 0.021(2) 0.0027(18) -0.0014(17) 0.0013(18) C12 0.019(2) 0.022(2) 0.024(2) 0.006(2) 0.0013(17) -0.001(2) C13 0.022(2) 0.029(2) 0.028(2) -0.002(2) 0.0007(18) -0.003(2) C14 0.036(3) 0.034(3) 0.035(3) -0.012(2) 0.000(2) 0.000(2) C15 0.037(3) 0.024(3) 0.041(3) -0.006(2) 0.006(2) 0.009(2) C16 0.022(2) 0.035(3) 0.034(2) -0.004(2) 0.0078(19) 0.007(2) C17 0.021(2) 0.024(2) 0.024(2) 0.004(2) -0.0011(17) -0.003(2) C18 0.035(3) 0.022(2) 0.018(2) 0.0004(19) -0.006(2) -0.003(2) C19 0.027(2) 0.026(2) 0.028(2) 0.008(2) -0.011(2) -0.0122(18) C20 0.0182(18) 0.027(2) 0.028(2) 0.0092(17) -0.0094(19) -0.001(2) C21 0.020(2) 0.025(2) 0.030(3) 0.0067(19) -0.0045(19) 0.0022(18) C22 0.024(2) 0.018(2) 0.026(2) 0.0073(18) -0.0050(19) -0.0044(17) C23 0.031(2) 0.027(2) 0.0174(19) 0.0063(17) -0.005(2) -0.003(2) C24 0.069(4) 0.018(2) 0.032(3) -0.0040(19) -0.004(3) -0.002(3) C25 0.087(6) 0.058(5) 0.036(3) -0.014(3) -0.015(4) -0.021(4) C26 0.074(5) 0.038(3) 0.029(3) -0.003(2) 0.012(3) 0.014(3) C27 0.030(3) 0.029(2) 0.041(3) 0.005(2) 0.000(2) 0.004(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . Cl1 . 2.4235(11) yes Ru1 . Cl2 . 2.4097(11) yes Ru1 . P1 . 2.3222(12) yes Ru1 . C18 . 2.238(5) yes Ru1 . C19 . 2.208(4) yes Ru1 . C20 . 2.182(5) yes Ru1 . C21 . 2.213(5) yes Ru1 . C22 . 2.212(4) yes Ru1 . C23 . 2.253(4) yes P1 . N1 . 1.691(4) yes P1 . C6 . 1.825(5) yes P1 . C12 . 1.814(5) yes N1 . N2 . 1.432(5) yes N1 . H1 . 0.86(6) no N2 . C1 . 1.453(6) yes N2 . C3 . 1.479(6) yes C1 . C2 . 1.521(6) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . N3 . 1.455(6) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.510(6) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . N3 . 1.482(6) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no N3 . C5 . 1.455(7) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.400(7) yes C6 . C11 . 1.395(7) yes C7 . C8 . 1.372(7) yes C7 . H71 . 1.000 no C8 . C9 . 1.404(7) yes C8 . H81 . 1.000 no C9 . C10 . 1.391(7) yes C9 . H91 . 1.000 no C10 . C11 . 1.395(7) yes C10 . H101 . 1.000 no C11 . H111 . 1.000 no C12 . C13 . 1.380(7) yes C12 . C17 . 1.395(6) yes C13 . C14 . 1.407(8) yes C13 . H131 . 1.000 no C14 . C15 . 1.388(7) yes C14 . H141 . 1.000 no C15 . C16 . 1.374(8) yes C15 . H151 . 1.000 no C16 . C17 . 1.389(7) yes C16 . H161 . 1.000 no C17 . H171 . 1.000 no C18 . C19 . 1.426(7) yes C18 . C23 . 1.441(6) yes C18 . C24 . 1.523(7) yes C19 . C20 . 1.423(7) yes C19 . H191 . 1.000 no C20 . C21 . 1.418(6) yes C20 . H201 . 1.000 no C21 . C22 . 1.428(7) yes C21 . C27 . 1.492(7) yes C22 . C23 . 1.383(7) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no C24 . C25 . 1.541(9) yes C24 . C26 . 1.522(10) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . Cl3 . 1.795(14) yes C28 . Cl4 . 1.780(15) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C38 . Cl13 . 1.762(16) yes C38 . Cl14 . 1.728(16) yes C38 . H381 . 1.000 no C38 . H382 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ru1 . Cl2 . 86.20(4) yes Cl1 . Ru1 . P1 . 86.18(4) yes Cl2 . Ru1 . P1 . 85.95(4) yes Cl1 . Ru1 . C18 . 90.18(14) yes Cl2 . Ru1 . C18 . 142.11(13) yes P1 . Ru1 . C18 . 131.46(13) yes Cl1 . Ru1 . C19 . 110.04(14) yes Cl2 . Ru1 . C19 . 162.94(13) yes P1 . Ru1 . C19 . 99.92(13) yes C18 . Ru1 . C19 . 37.40(19) yes Cl1 . Ru1 . C20 . 145.86(12) yes Cl2 . Ru1 . C20 . 127.22(12) yes P1 . Ru1 . C20 . 89.25(11) yes C18 . Ru1 . C20 . 68.03(18) yes C19 . Ru1 . C20 . 37.82(18) yes Cl1 . Ru1 . C21 . 166.76(13) yes Cl2 . Ru1 . C21 . 94.77(13) yes P1 . Ru1 . C21 . 107.06(13) yes C18 . Ru1 . C21 . 80.93(19) yes C19 . Ru1 . C21 . 68.22(18) yes Cl1 . Ru1 . C22 . 129.45(13) yes Cl2 . Ru1 . C22 . 87.17(12) yes P1 . Ru1 . C22 . 143.09(13) yes C18 . Ru1 . C22 . 66.49(17) yes C19 . Ru1 . C22 . 78.50(17) yes Cl1 . Ru1 . C23 . 99.57(13) yes Cl2 . Ru1 . C23 . 106.26(12) yes P1 . Ru1 . C23 . 166.73(13) yes C18 . Ru1 . C23 . 37.41(16) yes C19 . Ru1 . C23 . 66.90(18) yes C20 . Ru1 . C21 . 37.63(16) yes C20 . Ru1 . C22 . 66.75(16) yes C21 . Ru1 . C22 . 37.64(17) yes C20 . Ru1 . C23 . 79.26(18) yes C21 . Ru1 . C23 . 67.45(18) yes C22 . Ru1 . C23 . 36.08(17) yes Ru1 . P1 . N1 . 112.09(15) yes Ru1 . P1 . C6 . 116.63(17) yes N1 . P1 . C6 . 105.6(2) yes Ru1 . P1 . C12 . 112.49(16) yes N1 . P1 . C12 . 103.8(2) yes C6 . P1 . C12 . 105.1(2) yes P1 . N1 . N2 . 117.0(3) yes P1 . N1 . H1 . 108(4) no N2 . N1 . H1 . 114(4) no N1 . N2 . C1 . 110.4(4) yes N1 . N2 . C3 . 109.1(3) yes C1 . N2 . C3 . 108.9(4) yes N2 . C1 . C2 . 109.9(4) yes N2 . C1 . H11 . 109.373 no C2 . C1 . H11 . 109.373 no N2 . C1 . H12 . 109.373 no C2 . C1 . H12 . 109.373 no H11 . C1 . H12 . 109.467 no C1 . C2 . N3 . 110.8(4) yes C1 . C2 . H21 . 109.133 no N3 . C2 . H21 . 109.133 no C1 . C2 . H22 . 109.133 no N3 . C2 . H22 . 109.133 no H21 . C2 . H22 . 109.467 no N2 . C3 . C4 . 109.6(4) yes N2 . C3 . H31 . 109.446 no C4 . C3 . H31 . 109.446 no N2 . C3 . H32 . 109.446 no C4 . C3 . H32 . 109.446 no H31 . C3 . H32 . 109.466 no C3 . C4 . N3 . 110.4(4) yes C3 . C4 . H41 . 109.233 no N3 . C4 . H41 . 109.233 no C3 . C4 . H42 . 109.233 no N3 . C4 . H42 . 109.233 no H41 . C4 . H42 . 109.467 no C2 . N3 . C4 . 109.3(4) yes C2 . N3 . C5 . 110.5(4) yes C4 . N3 . C5 . 110.6(4) yes N3 . C5 . H51 . 109.466 no N3 . C5 . H52 . 109.467 no H51 . C5 . H52 . 109.475 no N3 . C5 . H53 . 109.467 no H51 . C5 . H53 . 109.476 no H52 . C5 . H53 . 109.476 no P1 . C6 . C7 . 121.6(4) yes P1 . C6 . C11 . 119.1(4) yes C7 . C6 . C11 . 118.5(4) yes C6 . C7 . C8 . 121.3(5) yes C6 . C7 . H71 . 119.345 no C8 . C7 . H71 . 119.345 no C7 . C8 . C9 . 119.9(4) yes C7 . C8 . H81 . 120.045 no C9 . C8 . H81 . 120.045 no C8 . C9 . C10 . 119.7(4) yes C8 . C9 . H91 . 120.147 no C10 . C9 . H91 . 120.146 no C9 . C10 . C11 . 119.8(4) yes C9 . C10 . H101 . 120.110 no C11 . C10 . H101 . 120.110 no C6 . C11 . C10 . 120.8(4) yes C6 . C11 . H111 . 119.617 no C10 . C11 . H111 . 119.617 no P1 . C12 . C13 . 118.5(3) yes P1 . C12 . C17 . 121.6(4) yes C13 . C12 . C17 . 119.4(5) yes C12 . C13 . C14 . 119.8(4) yes C12 . C13 . H131 . 120.120 no C14 . C13 . H131 . 120.120 no C13 . C14 . C15 . 120.0(5) yes C13 . C14 . H141 . 119.998 no C15 . C14 . H141 . 119.998 no C14 . C15 . C16 . 120.2(5) yes C14 . C15 . H151 . 119.896 no C16 . C15 . H151 . 119.896 no C15 . C16 . C17 . 119.8(4) yes C15 . C16 . H161 . 120.087 no C17 . C16 . H161 . 120.087 no C12 . C17 . C16 . 120.8(5) yes C12 . C17 . H171 . 119.615 no C16 . C17 . H171 . 119.615 no Ru1 . C18 . C19 . 70.1(3) yes Ru1 . C18 . C23 . 71.9(3) yes C19 . C18 . C23 . 118.2(4) yes Ru1 . C18 . C24 . 130.4(4) yes C19 . C18 . C24 . 118.6(5) yes C23 . C18 . C24 . 123.2(5) yes Ru1 . C19 . C18 . 72.5(3) yes Ru1 . C19 . C20 . 70.1(3) yes C18 . C19 . C20 . 120.5(4) yes Ru1 . C19 . H191 . 130.277 no C18 . C19 . H191 . 119.735 no C20 . C19 . H191 . 119.735 no Ru1 . C20 . C19 . 72.1(3) yes Ru1 . C20 . C21 . 72.4(2) yes C19 . C20 . C21 . 121.5(4) yes Ru1 . C20 . H201 . 128.726 no C19 . C20 . H201 . 119.229 no C21 . C20 . H201 . 119.228 no Ru1 . C21 . C20 . 70.0(3) yes Ru1 . C21 . C22 . 71.1(3) yes C20 . C21 . C22 . 116.3(4) yes Ru1 . C21 . C27 . 128.2(3) yes C20 . C21 . C27 . 121.7(4) yes C22 . C21 . C27 . 121.9(4) yes Ru1 . C22 . C21 . 71.2(3) yes Ru1 . C22 . C23 . 73.6(3) yes C21 . C22 . C23 . 123.8(4) yes Ru1 . C22 . H221 . 129.944 no C21 . C22 . H221 . 118.079 no C23 . C22 . H221 . 118.079 no Ru1 . C23 . C18 . 70.7(2) yes Ru1 . C23 . C22 . 70.3(3) yes C18 . C23 . C22 . 119.5(4) yes Ru1 . C23 . H231 . 131.441 no C18 . C23 . H231 . 120.239 no C22 . C23 . H231 . 120.239 no C18 . C24 . C25 . 108.3(6) yes C18 . C24 . C26 . 114.0(5) yes C25 . C24 . C26 . 111.3(5) yes C18 . C24 . H241 . 107.775 no C25 . C24 . H241 . 110.703 no C26 . C24 . H241 . 104.582 no C24 . C25 . H251 . 109.466 no C24 . C25 . H252 . 109.467 no H251 . C25 . H252 . 109.476 no C24 . C25 . H253 . 109.466 no H251 . C25 . H253 . 109.476 no H252 . C25 . H253 . 109.476 no C24 . C26 . H261 . 109.467 no C24 . C26 . H262 . 109.467 no H261 . C26 . H262 . 109.476 no C24 . C26 . H263 . 109.467 no H261 . C26 . H263 . 109.476 no H262 . C26 . H263 . 109.476 no C21 . C27 . H271 . 109.467 no C21 . C27 . H272 . 109.467 no H271 . C27 . H272 . 109.476 no C21 . C27 . H273 . 109.467 no H271 . C27 . H273 . 109.476 no H272 . C27 . H273 . 109.476 no Cl3 . C28 . Cl4 . 113.8(9) yes Cl3 . C28 . H281 . 108.360 no Cl4 . C28 . H281 . 108.361 no Cl3 . C28 . H282 . 108.380 no Cl4 . C28 . H282 . 108.382 no H281 . C28 . H282 . 109.467 no Cl13 . C38 . Cl14 . 107.7(10) yes Cl13 . C38 . H381 . 109.931 no Cl14 . C38 . H381 . 109.930 no Cl13 . C38 . H382 . 109.892 no Cl14 . C38 . H382 . 109.889 no H381 . C38 . H382 . 109.468 no loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N1 H1 Cl1 0.86(6) 2.52(6) 3.211(4) 138(5) yes data_ARC941 _database_code_depnum_ccdc_archive 'CCDC 255292' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; The NH hydrogen atom was located in a difference Fourier map and its coordinates and isotropic displacement parameter subsequently refined. All other hydrogen atoms were positioned geometrically, the preferred orientation of the methyl group H271-H273 having been previously identified by examination of the Fourier map ; #============================================================= _cell_length_a 10.0630(2) _cell_angle_alpha 90 _cell_length_b 14.6827(3) _cell_angle_beta 91.8167(9) _cell_length_c 20.0092(5) _cell_angle_gamma 90 _cell_volume 2954.91(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C28 H37 Cl4 N2 P Ru ' _chemical_formula_moiety ' C27 H35 Cl2 N2 P Ru, C H2 Cl2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 675.47 _cell_measurement_reflns_used 22074 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange-red ' _exptl_crystal_size_min 0.22 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.967 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.81 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 22074 _reflns_number_total 6690 # 6947 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_min 5.168 _diffrn_reflns_theta_max 27.469 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.469 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.73 _refine_diff_density_max 0.43 _refine_ls_number_reflns 4303 _refine_ls_number_restraints 0 _refine_ls_number_parameters 329 #_refine_ls_R_factor_ref 0.0308 _refine_ls_wR_factor_ref 0.0340 _refine_ls_goodness_of_fit_ref 1.1084 #_reflns_number_all 6690 _refine_ls_R_factor_all 0.0643 _refine_ls_wR_factor_all 0.0669 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4303 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_gt 0.0340 _refine_ls_shift/su_max 0.002290 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.291 0.0737 0.0890 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Ru1 Ru 0.51146(2) 0.133601(16) 0.397497(12) 0.0149 1.0000 Uani Cl1 Cl 0.45137(7) 0.20372(5) 0.50155(4) 0.0212 1.0000 Uani Cl2 Cl 0.73271(7) 0.11528(5) 0.44554(4) 0.0218 1.0000 Uani P1 P 0.58506(8) 0.27711(5) 0.36335(4) 0.0154 1.0000 Uani N1 N 0.6878(3) 0.32354(19) 0.42054(15) 0.0202 1.0000 Uani N2 N 0.7210(3) 0.41791(17) 0.41298(13) 0.0174 1.0000 Uani C1 C 0.6480(3) 0.4735(2) 0.46041(17) 0.0249 1.0000 Uani C2 C 0.6786(4) 0.5731(2) 0.4495(2) 0.0317 1.0000 Uani C3 C 0.8270(4) 0.5911(2) 0.45742(18) 0.0281 1.0000 Uani C4 C 0.9034(3) 0.5286(2) 0.41226(17) 0.0265 1.0000 Uani C5 C 0.8657(3) 0.4288(2) 0.42336(18) 0.0245 1.0000 Uani C6 C 0.4593(3) 0.3631(2) 0.34221(15) 0.0193 1.0000 Uani C7 C 0.4900(3) 0.4438(2) 0.30907(17) 0.0260 1.0000 Uani C8 C 0.3947(4) 0.5108(3) 0.29955(19) 0.0337 1.0000 Uani C9 C 0.2670(4) 0.4984(3) 0.32240(19) 0.0346 1.0000 Uani C10 C 0.2356(4) 0.4191(3) 0.35513(18) 0.0317 1.0000 Uani C11 C 0.3312(3) 0.3512(2) 0.36570(16) 0.0230 1.0000 Uani C12 C 0.6847(3) 0.2736(2) 0.28896(16) 0.0199 1.0000 Uani C13 C 0.8189(4) 0.2497(2) 0.29726(18) 0.0267 1.0000 Uani C14 C 0.8989(4) 0.2441(3) 0.2414(2) 0.0351 1.0000 Uani C15 C 0.8456(4) 0.2614(3) 0.17854(19) 0.0358 1.0000 Uani C16 C 0.7124(4) 0.2829(3) 0.16936(18) 0.0348 1.0000 Uani C17 C 0.6320(3) 0.2892(2) 0.22470(17) 0.0262 1.0000 Uani C18 C 0.3084(3) 0.0671(2) 0.39007(16) 0.0206 1.0000 Uani C19 C 0.3331(3) 0.1161(2) 0.33095(16) 0.0219 1.0000 Uani C20 C 0.4530(3) 0.1005(2) 0.29585(16) 0.0222 1.0000 Uani C21 C 0.5470(3) 0.0349(2) 0.31744(16) 0.0215 1.0000 Uani C22 C 0.5196(3) -0.0147(2) 0.37702(17) 0.0222 1.0000 Uani C23 C 0.4039(3) 0.0008(2) 0.41253(16) 0.0197 1.0000 Uani C24 C 0.1824(3) 0.0776(2) 0.42906(18) 0.0269 1.0000 Uani C25 C 0.0862(4) 0.0019(3) 0.4057(2) 0.0381 1.0000 Uani C26 C 0.1158(4) 0.1700(3) 0.4253(2) 0.0403 1.0000 Uani C27 C 0.6744(4) 0.0189(3) 0.28175(19) 0.0300 1.0000 Uani C28 C 0.2772(4) 0.7616(3) 0.3851(2) 0.0398 1.0000 Uani Cl3 Cl 0.12383(12) 0.71763(8) 0.40954(6) 0.0511 1.0000 Uani Cl4 Cl 0.26555(10) 0.80779(8) 0.30405(5) 0.0440 1.0000 Uani H1 H 0.685(5) 0.303(3) 0.461(3) 0.053(15) 1.0000 Uiso H11 H 0.6755 0.4560 0.5071 0.0299 1.0000 Uiso H12 H 0.5504 0.4630 0.4534 0.0299 1.0000 Uiso H21 H 0.6307 0.6103 0.4829 0.0379 1.0000 Uiso H22 H 0.6476 0.5908 0.4033 0.0379 1.0000 Uiso H31 H 0.8562 0.5801 0.5050 0.0338 1.0000 Uiso H32 H 0.8455 0.6559 0.4453 0.0338 1.0000 Uiso H41 H 1.0008 0.5363 0.4221 0.0318 1.0000 Uiso H42 H 0.8827 0.5452 0.3646 0.0318 1.0000 Uiso H51 H 0.8920 0.4105 0.4701 0.0294 1.0000 Uiso H52 H 0.9129 0.3895 0.3909 0.0294 1.0000 Uiso H71 H 0.5814 0.4532 0.2922 0.0312 1.0000 Uiso H81 H 0.4178 0.5685 0.2761 0.0403 1.0000 Uiso H91 H 0.1982 0.5468 0.3151 0.0414 1.0000 Uiso H101 H 0.1436 0.4100 0.3714 0.0381 1.0000 Uiso H111 H 0.3080 0.2942 0.3900 0.0276 1.0000 Uiso H131 H 0.8576 0.2368 0.3429 0.0321 1.0000 Uiso H141 H 0.9949 0.2275 0.2473 0.0425 1.0000 Uiso H151 H 0.9038 0.2584 0.1390 0.0435 1.0000 Uiso H161 H 0.6740 0.2939 0.1234 0.0420 1.0000 Uiso H171 H 0.5358 0.3051 0.2182 0.0315 1.0000 Uiso H191 H 0.2669 0.1618 0.3136 0.0261 1.0000 Uiso H201 H 0.4703 0.1372 0.2549 0.0266 1.0000 Uiso H221 H 0.5846 -0.0616 0.3937 0.0266 1.0000 Uiso H231 H 0.3879 -0.0350 0.4540 0.0236 1.0000 Uiso H241 H 0.2088 0.0722 0.4775 0.0324 1.0000 Uiso H251 H 0.0017 0.0069 0.4305 0.0458 1.0000 Uiso H252 H 0.1278 -0.0589 0.4148 0.0458 1.0000 Uiso H253 H 0.0663 0.0084 0.3567 0.0458 1.0000 Uiso H261 H 0.0343 0.1693 0.4526 0.0486 1.0000 Uiso H262 H 0.1787 0.2175 0.4431 0.0486 1.0000 Uiso H263 H 0.0904 0.1842 0.3777 0.0486 1.0000 Uiso H271 H 0.6605 -0.0304 0.2477 0.0362 1.0000 Uiso H272 H 0.7457 0.0001 0.3148 0.0362 1.0000 Uiso H273 H 0.7015 0.0763 0.2590 0.0362 1.0000 Uiso H281 H 0.3061 0.8105 0.4172 0.0473 1.0000 Uiso H282 H 0.3445 0.7116 0.3860 0.0473 1.0000 Uiso 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 0.01473(11) 0.01503(11) 0.01480(11) -0.00010(10) 0.00042(8) -0.00105(10) Cl1 0.0229(4) 0.0234(4) 0.0175(3) -0.0026(3) 0.0026(3) 0.0002(3) Cl2 0.0160(3) 0.0237(4) 0.0256(4) 0.0035(3) -0.0016(3) 0.0007(3) P1 0.0157(4) 0.0151(4) 0.0154(4) -0.0001(3) 0.0010(3) -0.0013(3) N1 0.0213(14) 0.0188(13) 0.0203(14) 0.0000(11) -0.0019(11) -0.0051(11) N2 0.0182(13) 0.0133(12) 0.0207(13) -0.0005(10) 0.0006(10) -0.0038(10) C1 0.0229(16) 0.0253(17) 0.0266(17) -0.0086(14) 0.0026(13) -0.0025(14) C2 0.034(2) 0.0202(17) 0.040(2) -0.0069(15) -0.0022(16) 0.0039(15) C3 0.0331(19) 0.0196(16) 0.0319(19) 0.0001(14) 0.0047(15) -0.0059(14) C4 0.0277(18) 0.0257(17) 0.0262(17) -0.0014(14) 0.0035(14) -0.0113(14) C5 0.0180(16) 0.0241(17) 0.0314(18) -0.0031(14) -0.0005(13) -0.0025(13) C6 0.0205(14) 0.0192(15) 0.0182(14) -0.0035(13) -0.0010(11) -0.0019(13) C7 0.0265(18) 0.0266(17) 0.0250(17) 0.0023(14) -0.0005(14) 0.0029(14) C8 0.043(2) 0.0274(18) 0.0306(19) 0.0090(16) -0.0062(16) 0.0079(17) C9 0.040(2) 0.033(2) 0.0312(19) 0.0008(16) -0.0053(16) 0.0180(17) C10 0.0238(18) 0.043(2) 0.0280(18) -0.0013(17) 0.0020(14) 0.0105(16) C11 0.0194(15) 0.0283(18) 0.0213(16) 0.0003(14) 0.0004(12) 0.0034(13) C12 0.0229(16) 0.0161(15) 0.0210(15) -0.0034(12) 0.0036(12) -0.0024(12) C13 0.0265(18) 0.0227(16) 0.0311(18) -0.0002(14) 0.0064(14) 0.0000(14) C14 0.0281(19) 0.0317(19) 0.047(2) -0.0024(18) 0.0196(17) 0.0012(16) C15 0.045(2) 0.032(2) 0.032(2) -0.0060(16) 0.0216(18) -0.0044(17) C16 0.049(2) 0.032(2) 0.0242(18) -0.0043(16) 0.0080(16) -0.0104(18) C17 0.0296(18) 0.0267(17) 0.0224(16) -0.0027(14) 0.0021(14) -0.0080(15) C18 0.0187(15) 0.0188(15) 0.0241(16) -0.0019(13) -0.0028(13) -0.0064(12) C19 0.0214(15) 0.0225(17) 0.0213(15) -0.0012(13) -0.0062(12) -0.0023(13) C20 0.0270(17) 0.0225(16) 0.0169(15) -0.0023(13) -0.0024(13) -0.0075(13) C21 0.0281(17) 0.0199(15) 0.0164(15) -0.0062(13) 0.0015(12) -0.0024(13) C22 0.0265(17) 0.0142(14) 0.0257(16) -0.0027(12) -0.0002(14) -0.0010(13) C23 0.0217(16) 0.0141(14) 0.0232(16) -0.0009(12) 0.0014(12) -0.0045(12) C24 0.0168(16) 0.0297(18) 0.0345(19) 0.0019(15) 0.0029(14) -0.0011(14) C25 0.028(2) 0.040(2) 0.046(2) -0.0012(19) 0.0054(17) -0.0094(17) C26 0.0265(19) 0.036(2) 0.059(3) 0.000(2) 0.0126(18) 0.0015(17) C27 0.0325(19) 0.0257(18) 0.0323(19) -0.0060(15) 0.0087(15) 0.0003(15) C28 0.036(2) 0.045(2) 0.038(2) -0.0016(19) -0.0143(17) -0.0033(18) Cl3 0.0517(7) 0.0491(6) 0.0521(6) 0.0151(5) -0.0039(5) -0.0203(5) Cl4 0.0358(5) 0.0632(7) 0.0330(5) 0.0027(5) 0.0041(4) 0.0033(5) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . Cl1 . 2.4167(8) yes Ru1 . Cl2 . 2.4120(8) yes Ru1 . P1 . 2.3425(8) yes Ru1 . C18 . 2.265(3) yes Ru1 . C19 . 2.215(3) yes Ru1 . C20 . 2.155(3) yes Ru1 . C21 . 2.198(3) yes Ru1 . C22 . 2.218(3) yes Ru1 . C23 . 2.256(3) yes P1 . N1 . 1.664(3) yes P1 . C6 . 1.827(3) yes P1 . C12 . 1.822(3) yes N1 . N2 . 1.434(4) yes N1 . H1 . 0.86(5) yes N2 . C1 . 1.467(4) yes N2 . C5 . 1.473(4) yes C1 . C2 . 1.511(5) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C3 . 1.521(5) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.515(5) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . C5 . 1.531(5) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C6 . C7 . 1.398(5) yes C6 . C11 . 1.397(4) yes C7 . C8 . 1.382(5) yes C7 . H71 . 1.000 no C8 . C9 . 1.389(6) yes C8 . H81 . 1.000 no C9 . C10 . 1.377(6) yes C9 . H91 . 1.000 no C10 . C11 . 1.397(5) yes C10 . H101 . 1.000 no C11 . H111 . 1.000 no C12 . C13 . 1.400(5) yes C12 . C17 . 1.394(5) yes C13 . C14 . 1.400(5) yes C13 . H131 . 1.000 no C14 . C15 . 1.376(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.384(6) yes C15 . H151 . 1.000 no C16 . C17 . 1.395(5) yes C16 . H161 . 1.000 no C17 . H171 . 1.000 no C18 . C19 . 1.414(5) yes C18 . C23 . 1.430(5) yes C18 . C24 . 1.518(5) yes C19 . C20 . 1.433(5) yes C19 . H191 . 1.000 no C20 . C21 . 1.409(5) yes C20 . H201 . 1.000 no C21 . C22 . 1.431(5) yes C21 . C27 . 1.505(5) yes C22 . C23 . 1.401(4) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no C24 . C25 . 1.537(5) yes C24 . C26 . 1.514(5) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C25 . H253 . 1.000 no C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . Cl3 . 1.757(4) yes C28 . Cl4 . 1.758(4) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ru1 . Cl2 . 87.54(3) yes Cl1 . Ru1 . P1 . 87.60(3) yes Cl2 . Ru1 . P1 . 85.42(3) yes Cl1 . Ru1 . C18 . 89.46(8) yes Cl2 . Ru1 . C18 . 142.87(9) yes P1 . Ru1 . C18 . 131.43(9) yes Cl1 . Ru1 . C19 . 110.31(9) yes Cl2 . Ru1 . C19 . 161.19(9) yes P1 . Ru1 . C19 . 100.74(9) yes C18 . Ru1 . C19 . 36.77(12) yes Cl1 . Ru1 . C20 . 147.24(9) yes Cl2 . Ru1 . C20 . 124.89(9) yes P1 . Ru1 . C20 . 90.39(9) yes C18 . Ru1 . C20 . 67.80(12) yes C19 . Ru1 . C20 . 38.26(12) yes Cl1 . Ru1 . C21 . 163.69(9) yes Cl2 . Ru1 . C21 . 92.71(9) yes P1 . Ru1 . C21 . 108.68(9) yes C18 . Ru1 . C21 . 80.51(12) yes C19 . Ru1 . C21 . 68.48(12) yes Cl1 . Ru1 . C22 . 126.10(9) yes Cl2 . Ru1 . C22 . 85.72(9) yes P1 . Ru1 . C22 . 144.63(9) yes C18 . Ru1 . C22 . 66.59(12) yes C19 . Ru1 . C22 . 79.00(12) yes Cl1 . Ru1 . C23 . 96.85(8) yes Cl2 . Ru1 . C23 . 106.94(9) yes P1 . Ru1 . C23 . 166.97(9) yes C18 . Ru1 . C23 . 36.88(12) yes C19 . Ru1 . C23 . 66.24(12) yes C20 . Ru1 . C21 . 37.76(13) yes C20 . Ru1 . C22 . 67.35(12) yes C21 . Ru1 . C22 . 37.82(12) yes C20 . Ru1 . C23 . 79.23(12) yes C21 . Ru1 . C23 . 67.47(12) yes C22 . Ru1 . C23 . 36.50(12) yes Ru1 . P1 . N1 . 111.30(11) yes Ru1 . P1 . C6 . 117.77(10) yes N1 . P1 . C6 . 106.66(14) yes Ru1 . P1 . C12 . 113.58(11) yes N1 . P1 . C12 . 103.14(15) yes C6 . P1 . C12 . 103.04(15) yes P1 . N1 . N2 . 117.7(2) yes P1 . N1 . H1 . 118(3) yes N2 . N1 . H1 . 117(3) yes N1 . N2 . C1 . 110.3(2) yes N1 . N2 . C5 . 108.8(2) yes C1 . N2 . C5 . 111.2(2) yes N2 . C1 . C2 . 109.7(3) yes N2 . C1 . H11 . 109.427 no C2 . C1 . H11 . 109.426 no N2 . C1 . H12 . 109.427 no C2 . C1 . H12 . 109.426 no H11 . C1 . H12 . 109.467 no C1 . C2 . C3 . 110.9(3) yes C1 . C2 . H21 . 109.108 no C3 . C2 . H21 . 109.108 no C1 . C2 . H22 . 109.108 no C3 . C2 . H22 . 109.108 no H21 . C2 . H22 . 109.467 no C2 . C3 . C4 . 110.3(3) yes C2 . C3 . H31 . 109.262 no C4 . C3 . H31 . 109.263 no C2 . C3 . H32 . 109.262 no C4 . C3 . H32 . 109.263 no H31 . C3 . H32 . 109.467 no C3 . C4 . C5 . 111.1(3) yes C3 . C4 . H41 . 109.055 no C5 . C4 . H41 . 109.055 no C3 . C4 . H42 . 109.055 no C5 . C4 . H42 . 109.055 no H41 . C4 . H42 . 109.467 no N2 . C5 . C4 . 109.4(3) yes N2 . C5 . H51 . 109.485 no C4 . C5 . H51 . 109.485 no N2 . C5 . H52 . 109.485 no C4 . C5 . H52 . 109.485 no H51 . C5 . H52 . 109.467 no P1 . C6 . C7 . 122.3(2) yes P1 . C6 . C11 . 118.4(2) yes C7 . C6 . C11 . 119.1(3) yes C6 . C7 . C8 . 120.4(3) yes C6 . C7 . H71 . 119.798 no C8 . C7 . H71 . 119.798 no C7 . C8 . C9 . 120.4(3) yes C7 . C8 . H81 . 119.812 no C9 . C8 . H81 . 119.811 no C8 . C9 . C10 . 119.8(3) yes C8 . C9 . H91 . 120.110 no C10 . C9 . H91 . 120.110 no C9 . C10 . C11 . 120.5(3) yes C9 . C10 . H101 . 119.763 no C11 . C10 . H101 . 119.763 no C6 . C11 . C10 . 119.9(3) yes C6 . C11 . H111 . 120.052 no C10 . C11 . H111 . 120.052 no P1 . C12 . C13 . 117.7(3) yes P1 . C12 . C17 . 123.0(3) yes C13 . C12 . C17 . 119.2(3) yes C12 . C13 . C14 . 119.8(3) yes C12 . C13 . H131 . 120.109 no C14 . C13 . H131 . 120.109 no C13 . C14 . C15 . 120.2(4) yes C13 . C14 . H141 . 119.921 no C15 . C14 . H141 . 119.921 no C14 . C15 . C16 . 120.7(3) yes C14 . C15 . H151 . 119.636 no C16 . C15 . H151 . 119.636 no C15 . C16 . C17 . 119.6(4) yes C15 . C16 . H161 . 120.215 no C17 . C16 . H161 . 120.215 no C12 . C17 . C16 . 120.5(3) yes C12 . C17 . H171 . 119.747 no C16 . C17 . H171 . 119.747 no Ru1 . C18 . C19 . 69.70(17) yes Ru1 . C18 . C23 . 71.20(17) yes C19 . C18 . C23 . 118.4(3) yes Ru1 . C18 . C24 . 133.5(2) yes C19 . C18 . C24 . 123.4(3) yes C23 . C18 . C24 . 118.1(3) yes Ru1 . C19 . C18 . 73.53(18) yes Ru1 . C19 . C20 . 68.59(17) yes C18 . C19 . C20 . 120.1(3) yes Ru1 . C19 . H191 . 130.496 no C18 . C19 . H191 . 119.955 no C20 . C19 . H191 . 119.955 no Ru1 . C20 . C19 . 73.15(18) yes Ru1 . C20 . C21 . 72.78(18) yes C19 . C20 . C21 . 121.8(3) yes Ru1 . C20 . H201 . 127.017 no C19 . C20 . H201 . 119.112 no C21 . C20 . H201 . 119.112 no Ru1 . C21 . C20 . 69.46(18) yes Ru1 . C21 . C22 . 71.83(18) yes C20 . C21 . C22 . 117.2(3) yes Ru1 . C21 . C27 . 127.6(2) yes C20 . C21 . C27 . 122.3(3) yes C22 . C21 . C27 . 120.4(3) yes Ru1 . C22 . C21 . 70.35(17) yes Ru1 . C22 . C23 . 73.23(18) yes C21 . C22 . C23 . 121.7(3) yes Ru1 . C22 . H221 . 129.898 no C21 . C22 . H221 . 119.149 no C23 . C22 . H221 . 119.149 no Ru1 . C23 . C18 . 71.92(17) yes Ru1 . C23 . C22 . 70.27(18) yes C18 . C23 . C22 . 120.7(3) yes Ru1 . C23 . H231 . 130.942 no C18 . C23 . H231 . 119.626 no C22 . C23 . H231 . 119.626 no C18 . C24 . C25 . 107.4(3) yes C18 . C24 . C26 . 116.2(3) yes C25 . C24 . C26 . 111.0(3) yes C18 . C24 . H241 . 106.848 no C25 . C24 . H241 . 112.471 no C26 . C24 . H241 . 102.876 no C24 . C25 . H251 . 109.467 no C24 . C25 . H252 . 109.467 no H251 . C25 . H252 . 109.476 no C24 . C25 . H253 . 109.467 no H251 . C25 . H253 . 109.476 no H252 . C25 . H253 . 109.476 no C24 . C26 . H261 . 109.467 no C24 . C26 . H262 . 109.467 no H261 . C26 . H262 . 109.476 no C24 . C26 . H263 . 109.467 no H261 . C26 . H263 . 109.476 no H262 . C26 . H263 . 109.476 no C21 . C27 . H271 . 109.467 no C21 . C27 . H272 . 109.467 no H271 . C27 . H272 . 109.476 no C21 . C27 . H273 . 109.467 no H271 . C27 . H273 . 109.476 no H272 . C27 . H273 . 109.476 no Cl3 . C28 . Cl4 . 111.4(2) yes Cl3 . C28 . H281 . 108.986 no Cl4 . C28 . H281 . 108.986 no Cl3 . C28 . H282 . 108.986 no Cl4 . C28 . H282 . 108.986 no H281 . C28 . H282 . 109.467 no data_arc730 _database_code_depnum_ccdc_archive 'CCDC 255293' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_special_details ; The refined thermal parameters of some of the phenyl C atoms are realtively large and highly anisotropic, suggesting that there may be some disorder of the groups C9-C14 and C21-C26. Attempts to include this disorder in the model did not lead to improvement in the agreement with the diffraction data and were consequently abandoned. ; #============================================================= _cell_length_a 10.2052(2) _cell_angle_alpha 90 _cell_length_b 15.3009(3) _cell_angle_beta 91.8367(7) _cell_length_c 23.1420(4) _cell_angle_gamma 90 _cell_volume 3611.74(12) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C38 H33 Br3 N1 P2 Re1 ' _chemical_formula_moiety ' C38 H33 Br3 N1 P2 Re1 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 991.55 _cell_measurement_reflns_used 44163 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1912.000 _exptl_absorpt_coefficient_mu 6.800 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.22 _exptl_absorpt_correction_T_max 0.58 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 44163 _reflns_number_total 8188 #8493 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_theta_min 5.150 _diffrn_reflns_theta_max 27.468 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.468 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _refine_diff_density_min -1.08 _refine_diff_density_max 0.80 _refine_ls_number_reflns 5069 _refine_ls_number_restraints 0 _refine_ls_number_parameters 406 #_refine_ls_R_factor_ref 0.0318 _refine_ls_wR_factor_ref 0.0350 _refine_ls_goodness_of_fit_ref 1.1000 #_reflns_number_all 8188 _refine_ls_R_factor_all 0.0671 _refine_ls_wR_factor_all 0.0685 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5069 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_gt 0.0350 _refine_ls_shift/su_max 0.008233 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.264 0.111 0.910E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Re1 Re 0.45261(2) 0.22621(2) 0.65055(2) 0.0240 1.0000 Uani Br1 Br 0.29768(6) 0.35411(4) 0.63337(2) 0.0312 1.0000 Uani Br2 Br 0.63305(6) 0.31545(4) 0.69672(3) 0.0325 1.0000 Uani Br3 Br 0.29951(6) 0.11514(4) 0.60846(3) 0.0356 1.0000 Uani N1 N 0.5794(5) 0.1226(3) 0.6647(2) 0.0300 1.0000 Uani C1 C 0.6487(6) 0.0652(4) 0.6723(3) 0.0328 1.0000 Uani C2 C 0.7348(7) -0.0093(5) 0.6824(3) 0.0464 1.0000 Uani P1 P 0.54829(15) 0.2494(1) 0.55473(6) 0.0267 1.0000 Uani C3 C 0.6795(7) 0.1689(5) 0.5459(3) 0.0404 1.0000 Uani C4 C 0.6437(8) 0.0839(5) 0.5273(3) 0.0507 1.0000 Uani C5 C 0.731(1) 0.0162(6) 0.5261(3) 0.0623 1.0000 Uani C6 C 0.853(1) 0.0321(8) 0.5443(4) 0.0693 1.0000 Uani C7 C 0.8996(9) 0.1123(8) 0.5630(4) 0.0735 1.0000 Uani C8 C 0.8061(7) 0.1838(7) 0.5653(3) 0.0635 1.0000 Uani C9 C 0.6234(8) 0.3544(5) 0.5378(3) 0.0422 1.0000 Uani C10 C 0.5876(7) 0.4307(5) 0.5642(3) 0.0408 1.0000 Uani C11 C 0.6374(8) 0.5111(5) 0.5471(3) 0.0491 1.0000 Uani C12 C 0.7285(11) 0.5139(6) 0.5033(4) 0.0698 1.0000 Uani C13 C 0.7666(16) 0.4403(7) 0.4776(5) 0.1135 1.0000 Uani C14 C 0.7123(13) 0.3608(7) 0.4937(4) 0.0866 1.0000 Uani C15 C 0.4448(6) 0.2333(4) 0.4890(2) 0.0322 1.0000 Uani C16 C 0.3101(7) 0.2485(4) 0.4899(3) 0.0357 1.0000 Uani C17 C 0.2338(8) 0.2416(5) 0.4392(3) 0.0461 1.0000 Uani C18 C 0.2900(9) 0.2212(5) 0.3881(3) 0.0505 1.0000 Uani C19 C 0.422(1) 0.2067(6) 0.3860(3) 0.0607 1.0000 Uani C20 C 0.5006(8) 0.2125(6) 0.4367(3) 0.0493 1.0000 Uani P2 P 0.36200(14) 0.1954(1) 0.74627(6) 0.0244 1.0000 Uani C21 C 0.4445(6) 0.1020(4) 0.7793(3) 0.0328 1.0000 Uani C22 C 0.4103(7) 0.0185(5) 0.7612(3) 0.0473 1.0000 Uani C23 C 0.475(1) -0.0549(6) 0.7833(5) 0.0772 1.0000 Uani C24 C 0.5775(11) -0.043(1) 0.8242(6) 0.0937 1.0000 Uani C25 C 0.6162(9) 0.039(1) 0.8400(4) 0.0860 1.0000 Uani C26 C 0.5506(7) 0.1119(6) 0.8180(3) 0.0528 1.0000 Uani C27 C 0.3737(6) 0.2812(4) 0.8015(3) 0.0314 1.0000 Uani C28 C 0.3875(6) 0.3685(4) 0.7858(3) 0.0343 1.0000 Uani C29 C 0.3877(7) 0.4350(5) 0.8275(3) 0.0394 1.0000 Uani C30 C 0.3749(6) 0.4145(5) 0.8842(3) 0.0409 1.0000 Uani C31 C 0.3619(7) 0.3282(5) 0.9007(3) 0.0424 1.0000 Uani C32 C 0.3600(7) 0.2616(5) 0.8600(3) 0.0435 1.0000 Uani C33 C 0.1879(6) 0.1658(4) 0.7514(2) 0.0297 1.0000 Uani C34 C 0.0941(6) 0.2053(4) 0.7147(3) 0.0323 1.0000 Uani C35 C -0.0371(6) 0.1905(5) 0.7223(3) 0.0389 1.0000 Uani C36 C -0.0791(6) 0.1370(5) 0.7653(3) 0.0428 1.0000 Uani C37 C 0.0102(7) 0.0960(5) 0.8007(3) 0.0428 1.0000 Uani C38 C 0.1451(6) 0.1107(5) 0.7948(3) 0.0363 1.0000 Uani H21 H 0.7200 -0.0340 0.7216 0.0556 1.0000 Uiso H22 H 0.8282 0.0099 0.6800 0.0556 1.0000 Uiso H23 H 0.7156 -0.0550 0.6524 0.0556 1.0000 Uiso H41 H 0.5506 0.0730 0.5144 0.0611 1.0000 Uiso H51 H 0.7031 -0.0431 0.5122 0.0747 1.0000 Uiso H61 H 0.9165 -0.0178 0.5444 0.0833 1.0000 Uiso H71 H 0.9940 0.1209 0.5746 0.0879 1.0000 Uiso H81 H 0.8334 0.2423 0.5806 0.0762 1.0000 Uiso H101 H 0.5245 0.4286 0.5964 0.0488 1.0000 Uiso H111 H 0.6083 0.5663 0.5660 0.0586 1.0000 Uiso H121 H 0.7654 0.5713 0.4910 0.0840 1.0000 Uiso H131 H 0.8338 0.4423 0.4471 0.1385 1.0000 Uiso H141 H 0.7380 0.3065 0.4729 0.1054 1.0000 Uiso H161 H 0.2683 0.2643 0.5269 0.0427 1.0000 Uiso H171 H 0.1371 0.2517 0.4401 0.0548 1.0000 Uiso H181 H 0.2341 0.2167 0.3519 0.0602 1.0000 Uiso H191 H 0.4630 0.1922 0.3484 0.0727 1.0000 Uiso H201 H 0.5971 0.2016 0.4353 0.0589 1.0000 Uiso H221 H 0.3379 0.0109 0.7315 0.0571 1.0000 Uiso H231 H 0.4481 -0.1149 0.7704 0.0939 1.0000 Uiso H241 H 0.6227 -0.0947 0.8420 0.1133 1.0000 Uiso H251 H 0.6926 0.0471 0.8676 0.1032 1.0000 Uiso H261 H 0.5797 0.1718 0.8300 0.0633 1.0000 Uiso H281 H 0.3974 0.3840 0.7441 0.0412 1.0000 Uiso H291 H 0.3972 0.4975 0.8156 0.0473 1.0000 Uiso H301 H 0.3749 0.4619 0.9140 0.0491 1.0000 Uiso H311 H 0.3536 0.3136 0.9426 0.0510 1.0000 Uiso H321 H 0.3489 0.1996 0.8726 0.0523 1.0000 Uiso H341 H 0.1225 0.2443 0.6828 0.0388 1.0000 Uiso H351 H -0.1032 0.2196 0.6959 0.0468 1.0000 Uiso H361 H -0.1750 0.1280 0.7706 0.0515 1.0000 Uiso H371 H -0.0203 0.0550 0.8311 0.0517 1.0000 Uiso H381 H 0.2102 0.0817 0.8217 0.0436 1.0000 Uiso 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 Re1 0.02448(11) 0.02639(12) 0.02111(11) 0.0006(1) 0.00236(7) 0.0014(1) Br1 0.0337(3) 0.0327(3) 0.0273(3) 0.0032(2) 0.0030(2) 0.0071(3) Br2 0.0258(3) 0.0404(4) 0.0314(3) -0.0044(3) 0.0003(2) -0.0023(3) Br3 0.0388(3) 0.0372(3) 0.0307(3) -0.0015(3) 0.0014(3) -0.0089(3) N1 0.033(3) 0.032(3) 0.026(2) 0.002(2) 0.008(2) 0.001(2) C1 0.039(3) 0.029(3) 0.030(3) -0.004(3) 0.002(3) 0.007(3) C2 0.045(4) 0.038(4) 0.056(4) 0.003(3) 0.001(3) 0.015(3) P1 0.0296(8) 0.0287(8) 0.0220(7) -0.0011(6) 0.0044(6) 0.0007(6) C3 0.048(4) 0.053(5) 0.021(3) 0.006(3) 0.008(3) 0.014(3) C4 0.070(5) 0.045(4) 0.038(4) 0.009(3) 0.015(4) 0.027(4) C5 0.081(6) 0.067(6) 0.038(4) 0.004(4) -0.001(4) 0.027(5) C6 0.071(6) 0.100(8) 0.037(4) -0.007(5) 0.009(4) 0.017(6) C7 0.052(5) 0.12(1) 0.043(5) 0.015(6) -0.007(4) 0.023(6) C8 0.036(4) 0.125(8) 0.030(4) -0.015(4) 0.002(3) 0.016(5) C9 0.056(4) 0.038(4) 0.032(3) 0.002(3) 0.003(3) -0.010(3) C10 0.044(4) 0.039(4) 0.039(4) 0.000(3) -0.004(3) -0.002(3) C11 0.055(5) 0.038(4) 0.053(4) 0.007(4) -0.009(4) -0.005(4) C12 0.112(8) 0.060(6) 0.038(4) 0.005(4) 0.010(5) -0.032(6) C13 0.199(15) 0.055(6) 0.093(8) -0.010(6) 0.094(9) -0.050(8) C14 0.14(1) 0.064(6) 0.064(6) -0.019(5) 0.064(6) -0.030(6) C15 0.043(3) 0.033(3) 0.020(3) 0.002(3) -0.005(2) 0.000(3) C16 0.042(4) 0.028(3) 0.036(3) -0.003(3) -0.003(3) -0.001(3) C17 0.056(4) 0.038(4) 0.044(4) 0.000(3) -0.018(3) 0.011(3) C18 0.070(5) 0.045(4) 0.035(4) -0.006(3) -0.015(3) 0.010(4) C19 0.084(6) 0.075(6) 0.023(3) -0.006(4) -0.005(4) 0.013(5) C20 0.054(4) 0.065(5) 0.028(3) 0.000(3) -0.007(3) 0.005(4) P2 0.0226(7) 0.0297(8) 0.0208(7) 0.0022(6) 0.0021(5) -0.0004(6) C21 0.027(3) 0.041(4) 0.031(3) 0.012(3) 0.005(2) -0.002(3) C22 0.037(4) 0.045(4) 0.060(5) 0.013(4) 0.014(3) 0.005(3) C23 0.066(6) 0.047(5) 0.122(9) 0.045(5) 0.053(6) 0.029(4) C24 0.061(6) 0.12(1) 0.105(9) 0.082(8) 0.039(6) 0.055(7) C25 0.045(5) 0.147(12) 0.066(6) 0.054(7) 0.001(4) 0.029(6) C26 0.036(4) 0.079(6) 0.043(4) 0.021(4) -0.002(3) 0.014(4) C27 0.024(3) 0.042(4) 0.028(3) 0.001(3) 0.006(2) 0.000(3) C28 0.033(3) 0.037(4) 0.032(3) -0.006(3) 0.001(3) 0.000(3) C29 0.039(4) 0.048(4) 0.031(3) -0.010(3) -0.001(3) 0.007(3) C30 0.032(3) 0.054(4) 0.036(3) -0.017(3) 0.002(3) 0.000(3) C31 0.040(4) 0.068(5) 0.020(3) -0.002(3) 0.007(3) -0.006(4) C32 0.052(4) 0.053(4) 0.026(3) -0.001(3) 0.005(3) -0.012(4) C33 0.025(3) 0.041(4) 0.023(3) -0.005(3) 0.000(2) 0.001(3) C34 0.029(3) 0.038(4) 0.030(3) 0.005(3) 0.001(2) 0.001(3) C35 0.028(3) 0.051(4) 0.038(4) 0.001(3) 0.003(3) 0.004(3) C36 0.028(3) 0.061(5) 0.040(4) -0.014(3) 0.004(3) -0.009(3) C37 0.034(3) 0.059(5) 0.036(3) 0.003(3) 0.017(3) -0.011(3) C38 0.032(3) 0.044(4) 0.033(3) 0.005(3) 0.002(3) -0.003(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . Br1 . 2.5391(6) yes Re1 . Br2 . 2.5042(6) yes Re1 . Br3 . 2.4861(7) yes Re1 . N1 . 2.065(5) yes Re1 . P1 . 2.4769(14) yes Re1 . P2 . 2.4730(14) yes N1 . C1 . 1.138(8) yes C1 . C2 . 1.454(9) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no P1 . C3 . 1.835(7) yes P1 . C9 . 1.828(7) yes P1 . C15 . 1.840(6) yes C3 . C4 . 1.415(11) yes C3 . C8 . 1.37(1) yes C4 . C5 . 1.365(11) yes C4 . H41 . 1.000 no C5 . C6 . 1.330(14) yes C5 . H51 . 1.000 no C6 . C7 . 1.380(15) yes C6 . H61 . 1.000 no C7 . C8 . 1.453(13) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.37(1) yes C9 . C14 . 1.390(11) yes C10 . C11 . 1.39(1) yes C10 . H101 . 1.000 no C11 . C12 . 1.398(12) yes C11 . H111 . 1.000 no C12 . C13 . 1.337(14) yes C12 . H121 . 1.000 no C13 . C14 . 1.393(13) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.395(9) yes C15 . C20 . 1.391(9) yes C16 . C17 . 1.391(9) yes C16 . H161 . 1.000 no C17 . C18 . 1.367(11) yes C17 . H171 . 1.000 no C18 . C19 . 1.371(12) yes C18 . H181 . 1.000 no P2 . C21 . 1.815(7) yes P2 . C27 . 1.833(7) yes P2 . C33 . 1.841(6) yes C19 . C20 . 1.40(1) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.39(1) yes C21 . C26 . 1.39(1) yes C22 . C23 . 1.391(11) yes C22 . H221 . 1.000 no C23 . C24 . 1.404(18) yes C23 . H231 . 1.000 no C24 . C25 . 1.361(18) yes C24 . H241 . 1.000 no C25 . C26 . 1.386(14) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C27 . C28 . 1.393(9) yes C27 . C32 . 1.399(9) yes C28 . C29 . 1.404(9) yes C28 . H281 . 1.000 no C29 . C30 . 1.36(1) yes C29 . H291 . 1.000 no C30 . C31 . 1.383(11) yes C30 . H301 . 1.000 no C31 . C32 . 1.39(1) yes C31 . H311 . 1.000 no C32 . H321 . 1.000 no C33 . C34 . 1.397(8) yes C33 . C38 . 1.392(9) yes C34 . C35 . 1.375(9) yes C34 . H341 . 1.000 no C35 . C36 . 1.37(1) yes C35 . H351 . 1.000 no C36 . C37 . 1.36(1) yes C36 . H361 . 1.000 no C37 . C38 . 1.406(9) yes C37 . H371 . 1.000 no C38 . H381 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . Re1 . Br2 . 95.29(2) yes Br1 . Re1 . Br3 . 94.88(2) yes Br2 . Re1 . Br3 . 169.81(2) yes Br1 . Re1 . N1 . 179.69(15) yes Br2 . Re1 . N1 . 84.40(15) yes Br3 . Re1 . N1 . 85.42(15) yes Br1 . Re1 . P1 . 90.62(4) yes Br2 . Re1 . P1 . 89.91(4) yes Br3 . Re1 . P1 . 90.46(4) yes N1 . Re1 . P1 . 89.37(13) yes Br1 . Re1 . P2 . 92.20(4) yes Br2 . Re1 . P2 . 90.73(4) yes Br3 . Re1 . P2 . 88.40(4) yes N1 . Re1 . P2 . 87.81(13) yes P1 . Re1 . P2 . 177.03(5) yes Re1 . N1 . C1 . 179.6(5) yes N1 . C1 . C2 . 178.7(7) yes C1 . C2 . H21 . 109.466 no C1 . C2 . H22 . 109.465 no H21 . C2 . H22 . 109.475 no C1 . C2 . H23 . 109.467 no H21 . C2 . H23 . 109.478 no H22 . C2 . H23 . 109.477 no Re1 . P1 . C3 . 108.3(2) yes Re1 . P1 . C9 . 119.8(2) yes C3 . P1 . C9 . 104.7(4) yes Re1 . P1 . C15 . 119.2(2) yes C3 . P1 . C15 . 102.7(3) yes C9 . P1 . C15 . 100.0(3) yes P1 . C3 . C4 . 117.9(6) yes P1 . C3 . C8 . 122.4(7) yes C4 . C3 . C8 . 118.9(8) yes C3 . C4 . C5 . 122.8(9) yes C3 . C4 . H41 . 118.580 no C5 . C4 . H41 . 118.579 no C4 . C5 . C6 . 117.4(10) yes C4 . C5 . H51 . 121.301 no C6 . C5 . H51 . 121.300 no C5 . C6 . C7 . 124.9(10) yes C5 . C6 . H61 . 117.548 no C7 . C6 . H61 . 117.544 no C6 . C7 . C8 . 117.4(8) yes C6 . C7 . H71 . 121.284 no C8 . C7 . H71 . 121.280 no C3 . C8 . C7 . 118.5(9) yes C3 . C8 . H81 . 120.773 no C7 . C8 . H81 . 120.774 no P1 . C9 . C10 . 122.2(5) yes P1 . C9 . C14 . 120.4(6) yes C10 . C9 . C14 . 117.2(7) yes C9 . C10 . C11 . 121.3(7) yes C9 . C10 . H101 . 119.373 no C11 . C10 . H101 . 119.371 no C10 . C11 . C12 . 119.4(8) yes C10 . C11 . H111 . 120.301 no C12 . C11 . H111 . 120.300 no C11 . C12 . C13 . 120.4(8) yes C11 . C12 . H121 . 119.815 no C13 . C12 . H121 . 119.813 no C12 . C13 . C14 . 119.6(9) yes C12 . C13 . H131 . 120.204 no C14 . C13 . H131 . 120.204 no C9 . C14 . C13 . 122.1(9) yes C9 . C14 . H141 . 118.939 no C13 . C14 . H141 . 118.939 no P1 . C15 . C16 . 120.4(5) yes P1 . C15 . C20 . 120.6(5) yes C16 . C15 . C20 . 118.8(6) yes C15 . C16 . C17 . 120.0(6) yes C15 . C16 . H161 . 119.990 no C17 . C16 . H161 . 119.990 no C16 . C17 . C18 . 120.6(7) yes C16 . C17 . H171 . 119.719 no C18 . C17 . H171 . 119.719 no C17 . C18 . C19 . 120.5(7) yes C17 . C18 . H181 . 119.744 no C19 . C18 . H181 . 119.743 no Re1 . P2 . C21 . 110.2(2) yes Re1 . P2 . C27 . 118.0(2) yes C21 . P2 . C27 . 104.5(3) yes Re1 . P2 . C33 . 119.63(19) yes C21 . P2 . C33 . 102.4(3) yes C27 . P2 . C33 . 99.9(3) yes C18 . C19 . C20 . 119.8(7) yes C18 . C19 . H191 . 120.117 no C20 . C19 . H191 . 120.116 no C15 . C20 . C19 . 120.3(7) yes C15 . C20 . H201 . 119.840 no C19 . C20 . H201 . 119.841 no P2 . C21 . C22 . 119.2(5) yes P2 . C21 . C26 . 121.8(6) yes C22 . C21 . C26 . 118.6(7) yes C21 . C22 . C23 . 121.4(8) yes C21 . C22 . H221 . 119.277 no C23 . C22 . H221 . 119.279 no C22 . C23 . C24 . 118.4(10) yes C22 . C23 . H231 . 120.808 no C24 . C23 . H231 . 120.809 no C23 . C24 . C25 . 120.4(8) yes C23 . C24 . H241 . 119.784 no C25 . C24 . H241 . 119.774 no C24 . C25 . C26 . 120.6(10) yes C24 . C25 . H251 . 119.715 no C26 . C25 . H251 . 119.710 no C21 . C26 . C25 . 120.4(10) yes C21 . C26 . H261 . 119.804 no C25 . C26 . H261 . 119.802 no P2 . C27 . C28 . 120.6(5) yes P2 . C27 . C32 . 121.0(5) yes C28 . C27 . C32 . 118.2(6) yes C27 . C28 . C29 . 120.9(6) yes C27 . C28 . H281 . 119.542 no C29 . C28 . H281 . 119.541 no C28 . C29 . C30 . 119.9(7) yes C28 . C29 . H291 . 120.039 no C30 . C29 . H291 . 120.038 no C29 . C30 . C31 . 120.1(6) yes C29 . C30 . H301 . 119.974 no C31 . C30 . H301 . 119.974 no C30 . C31 . C32 . 120.9(6) yes C30 . C31 . H311 . 119.560 no C32 . C31 . H311 . 119.562 no C27 . C32 . C31 . 120.0(7) yes C27 . C32 . H321 . 119.981 no C31 . C32 . H321 . 119.981 no P2 . C33 . C34 . 119.9(5) yes P2 . C33 . C38 . 121.5(5) yes C34 . C33 . C38 . 118.4(6) yes C33 . C34 . C35 . 120.2(6) yes C33 . C34 . H341 . 119.908 no C35 . C34 . H341 . 119.908 no C34 . C35 . C36 . 121.4(6) yes C34 . C35 . H351 . 119.315 no C36 . C35 . H351 . 119.313 no C35 . C36 . C37 . 119.7(6) yes C35 . C36 . H361 . 120.163 no C37 . C36 . H361 . 120.163 no C36 . C37 . C38 . 120.5(6) yes C36 . C37 . H371 . 119.764 no C38 . C37 . H371 . 119.764 no C33 . C38 . C37 . 119.9(6) yes C33 . C38 . H381 . 120.067 no C37 . C38 . H381 . 120.068 no data_arc944 _database_code_depnum_ccdc_archive 'CCDC 255294' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; The NH hydrogen atoms were located in a difference Fourier map and their coordinates and isotropic displacement parameters subsequently refined. Other hydrogen atoms were positioned geometrically, the preferred orientation of the methyl group H241-H243 having been previously identified by examination of the Fourier map ; #============================================================= _cell_length_a 9.5016(2) _cell_angle_alpha 90 _cell_length_b 20.4988(3) _cell_angle_beta 95.2880(7) _cell_length_c 15.5874(2) _cell_angle_gamma 90 _cell_volume 3023.06(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C28 H40 Cl3 N2 O P Ru ' _chemical_formula_moiety ' C24 H32 Cl2 N2 P Ru, C4 H8 O, Cl' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 659.04 _cell_measurement_reflns_used 34547 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange-red ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.26 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.860 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 34647 _reflns_number_total 6887 #7081 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_min 5.131 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.478 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.67 _refine_diff_density_max 0.56 _refine_ls_number_reflns 5434 _refine_ls_number_restraints 0 _refine_ls_number_parameters 333 #_refine_ls_R_factor_ref 0.0282 _refine_ls_wR_factor_ref 0.0321 _refine_ls_goodness_of_fit_ref 1.0780 #_reflns_number_all 6887 _refine_ls_R_factor_all 0.0400 _refine_ls_wR_factor_all 0.0431 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5434 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_gt 0.0321 _refine_ls_shift/su_max 0.003380 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.440 0.157 0.192 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type Ru1 Ru 0.406801(17) 0.608801(8) 0.104610(10) 0.0168 1.0000 Uani Cl1 Cl 0.29664(6) 0.50844(3) 0.14577(4) 0.0272 1.0000 Uani Cl2 Cl 0.62946(6) 0.56085(3) 0.15941(3) 0.0254 1.0000 Uani P1 P 0.38973(6) 0.64917(2) 0.24355(3) 0.0168 1.0000 Uani N1 N 0.4851(2) 0.60692(8) 0.32295(12) 0.0196 1.0000 Uani N2 N 0.4741(2) 0.53677(9) 0.32573(13) 0.0236 1.0000 Uani C1 C 0.3484(3) 0.51311(12) 0.36768(16) 0.0307 1.0000 Uani C2 C 0.6088(3) 0.51049(12) 0.36945(17) 0.0313 1.0000 Uani C3 C 0.2154(2) 0.65935(10) 0.28162(14) 0.0210 1.0000 Uani C4 C 0.2033(3) 0.68847(12) 0.36207(15) 0.0279 1.0000 Uani C5 C 0.0745(3) 0.68841(14) 0.39694(16) 0.0352 1.0000 Uani C6 C -0.0430(3) 0.65983(15) 0.35231(18) 0.0378 1.0000 Uani C7 C -0.0324(3) 0.63138(16) 0.27254(18) 0.0385 1.0000 Uani C8 C 0.0968(3) 0.63129(12) 0.23699(15) 0.0278 1.0000 Uani C9 C 0.4770(2) 0.72703(10) 0.26457(13) 0.0204 1.0000 Uani C10 C 0.6234(3) 0.72782(11) 0.28088(16) 0.0279 1.0000 Uani C11 C 0.6949(3) 0.78651(13) 0.29347(18) 0.0355 1.0000 Uani C12 C 0.6205(3) 0.84468(12) 0.28869(17) 0.0366 1.0000 Uani C13 C 0.4759(3) 0.84413(12) 0.27056(17) 0.0348 1.0000 Uani C14 C 0.4022(3) 0.78583(11) 0.25859(15) 0.0269 1.0000 Uani C15 C 0.2467(2) 0.61652(11) -0.01077(14) 0.0230 1.0000 Uani C16 C 0.2571(2) 0.67658(10) 0.03277(14) 0.0216 1.0000 Uani C17 C 0.3911(2) 0.70764(10) 0.05139(14) 0.0221 1.0000 Uani C18 C 0.5161(2) 0.67921(11) 0.02641(14) 0.0235 1.0000 Uani C19 C 0.5036(3) 0.61837(12) -0.01872(14) 0.0259 1.0000 Uani C20 C 0.3736(3) 0.58735(11) -0.03660(13) 0.0241 1.0000 Uani C21 C 0.1073(3) 0.58188(13) -0.03636(17) 0.0329 1.0000 Uani C22 C 0.0869(3) 0.57733(19) -0.1349(2) 0.0522 1.0000 Uani C23 C -0.0218(3) 0.61349(18) -0.0033(2) 0.0484 1.0000 Uani C24 C 0.6578(3) 0.71081(13) 0.04728(17) 0.0339 1.0000 Uani Cl3 Cl 0.50527(7) 0.63229(3) 0.52002(4) 0.0303 1.0000 Uani O1 O 0.1038(2) 0.80570(10) 0.11537(13) 0.0389 1.0000 Uani C25 C 0.1405(3) 0.87319(15) 0.1117(2) 0.0432 1.0000 Uani C26 C 0.0020(4) 0.90891(16) 0.0926(2) 0.0529 1.0000 Uani C27 C -0.1013(3) 0.86686(18) 0.1371(2) 0.0516 1.0000 Uani C28 C -0.0278(4) 0.80164(18) 0.1483(3) 0.0662 1.0000 Uani H1 H 0.486(3) 0.6222(14) 0.3772(19) 0.028(7) 1.0000 Uiso H2 H 0.467(3) 0.5245(14) 0.270(2) 0.029(7) 1.0000 Uiso H11 H 0.3471 0.4643 0.3675 0.0365 1.0000 Uiso H12 H 0.3538 0.5293 0.4284 0.0365 1.0000 Uiso H13 H 0.2601 0.5299 0.3352 0.0365 1.0000 Uiso H21 H 0.6033 0.4618 0.3721 0.0372 1.0000 Uiso H22 H 0.6236 0.5285 0.4292 0.0372 1.0000 Uiso H23 H 0.6895 0.5236 0.3363 0.0372 1.0000 Uiso H41 H 0.2876 0.7092 0.3942 0.0334 1.0000 Uiso H51 H 0.0659 0.7090 0.4544 0.0425 1.0000 Uiso H61 H -0.1358 0.6598 0.3779 0.0456 1.0000 Uiso H71 H -0.1173 0.6110 0.2406 0.0460 1.0000 Uiso H81 H 0.1044 0.6110 0.1793 0.0331 1.0000 Uiso H101 H 0.6773 0.6859 0.2835 0.0335 1.0000 Uiso H111 H 0.8000 0.7868 0.3060 0.0428 1.0000 Uiso H121 H 0.6717 0.8870 0.2984 0.0445 1.0000 Uiso H131 H 0.4231 0.8864 0.2659 0.0420 1.0000 Uiso H141 H 0.2971 0.7859 0.2459 0.0322 1.0000 Uiso H161 H 0.1698 0.6978 0.0509 0.0257 1.0000 Uiso H171 H 0.3963 0.7503 0.0827 0.0264 1.0000 Uiso H191 H 0.5905 0.5975 -0.0380 0.0315 1.0000 Uiso H201 H 0.3687 0.5446 -0.0676 0.0287 1.0000 Uiso H211 H 0.1146 0.5379 -0.0085 0.0385 1.0000 Uiso H221 H -0.0043 0.5547 -0.1528 0.0612 1.0000 Uiso H222 H 0.0849 0.6222 -0.1601 0.0612 1.0000 Uiso H223 H 0.1669 0.5521 -0.1561 0.0612 1.0000 Uiso H231 H -0.1079 0.5876 -0.0231 0.0576 1.0000 Uiso H232 H -0.0321 0.6590 -0.0262 0.0576 1.0000 Uiso H233 H -0.0102 0.6147 0.0611 0.0576 1.0000 Uiso H241 H 0.7327 0.6833 0.0243 0.0407 1.0000 Uiso H242 H 0.6576 0.7551 0.0203 0.0407 1.0000 Uiso H243 H 0.6773 0.7150 0.1112 0.0407 1.0000 Uiso H251 H 0.1889 0.8878 0.1681 0.0522 1.0000 Uiso H252 H 0.2038 0.8810 0.0649 0.0522 1.0000 Uiso H261 H 0.0072 0.9540 0.1172 0.0637 1.0000 Uiso H262 H -0.0253 0.9113 0.0292 0.0637 1.0000 Uiso H271 H -0.1191 0.8858 0.1943 0.0618 1.0000 Uiso H272 H -0.1930 0.8625 0.1006 0.0618 1.0000 Uiso H281 H -0.0145 0.7902 0.2109 0.0813 1.0000 Uiso H282 H -0.0863 0.7673 0.1164 0.0813 1.0000 Uiso 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 0.02122(9) 0.01229(8) 0.01653(8) -0.00123(6) -0.00015(6) 0.00036(6) Cl1 0.0376(3) 0.0161(2) 0.0264(3) 0.00162(19) -0.0043(2) -0.0070(2) Cl2 0.0254(3) 0.0254(3) 0.0249(3) -0.0041(2) -0.00127(19) 0.0066(2) P1 0.0202(2) 0.0135(2) 0.0164(2) -0.00031(18) -0.00056(19) 0.00069(19) N1 0.0277(9) 0.0129(8) 0.0176(8) 0.0001(7) -0.0016(7) 0.0019(7) N2 0.0340(10) 0.0151(8) 0.0209(9) 0.0018(7) -0.0011(8) 0.0022(7) C1 0.0371(13) 0.0224(11) 0.0318(13) 0.0066(9) -0.0015(10) -0.0069(10) C2 0.0361(13) 0.0253(11) 0.0317(12) 0.0050(10) -0.0020(10) 0.0121(10) C3 0.0223(10) 0.0205(10) 0.0196(10) 0.0012(8) -0.0008(8) 0.0023(8) C4 0.0285(11) 0.0304(12) 0.0248(11) -0.0022(9) 0.0024(9) 0.0023(9) C5 0.0324(13) 0.0453(15) 0.0285(12) -0.0025(11) 0.0064(10) 0.0069(11) C6 0.0229(12) 0.0556(17) 0.0355(14) 0.0051(12) 0.0063(10) 0.0047(11) C7 0.0240(12) 0.0570(17) 0.0339(14) -0.0008(12) -0.0009(10) -0.0020(11) C8 0.0255(11) 0.0331(12) 0.0241(11) -0.0010(9) -0.0019(9) 0.0002(9) C9 0.0303(11) 0.0156(9) 0.0154(9) -0.0019(7) 0.0022(8) -0.0009(8) C10 0.0288(12) 0.0225(11) 0.0325(12) -0.0039(9) 0.0037(9) -0.0038(9) C11 0.0371(14) 0.0316(13) 0.0383(14) -0.0070(10) 0.0063(11) -0.0136(11) C12 0.0565(17) 0.0237(12) 0.0310(13) -0.0062(10) 0.0119(12) -0.0165(11) C13 0.0565(17) 0.0180(11) 0.0307(13) -0.0014(9) 0.0083(11) 0.0019(11) C14 0.0378(13) 0.0179(10) 0.0249(11) 0.0002(8) 0.0029(9) 0.0030(9) C15 0.0296(11) 0.0196(10) 0.0183(10) 0.0030(8) -0.0063(8) 0.0011(9) C16 0.0256(11) 0.0190(10) 0.0196(10) 0.0054(8) -0.0008(8) 0.0047(8) C17 0.0310(11) 0.0159(9) 0.0193(10) 0.0031(7) 0.0011(8) 0.0005(8) C18 0.0302(11) 0.0201(10) 0.0205(10) 0.0036(8) 0.0044(8) -0.0036(9) C19 0.0316(11) 0.0285(12) 0.0186(10) 0.0031(9) 0.0075(9) 0.0041(9) C20 0.0360(12) 0.0205(10) 0.0151(9) -0.0033(8) -0.0015(8) 0.0025(9) C21 0.0343(13) 0.0279(12) 0.0341(13) 0.0021(10) -0.0094(10) -0.0064(10) C22 0.0431(17) 0.072(2) 0.0374(15) -0.0169(15) -0.0155(13) -0.0003(15) C23 0.0297(13) 0.075(2) 0.0389(15) -0.0064(15) -0.0025(11) -0.0098(14) C24 0.0304(13) 0.0350(13) 0.0364(14) 0.0056(10) 0.0045(10) -0.0082(10) Cl3 0.0456(3) 0.0219(3) 0.0225(3) -0.0004(2) -0.0021(2) 0.0038(2) O1 0.0358(10) 0.0374(10) 0.0441(11) -0.0019(8) 0.0076(8) 0.0026(8) C25 0.0431(16) 0.0399(15) 0.0476(16) -0.0012(12) 0.0097(13) -0.0085(12) C26 0.065(2) 0.0370(15) 0.057(2) 0.0009(14) 0.0081(16) 0.0080(15) C27 0.0372(16) 0.0534(19) 0.064(2) -0.0016(16) 0.0033(14) 0.0026(14) C28 0.0427(18) 0.0452(19) 0.115(3) 0.006(2) 0.033(2) -0.0015(15) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . Cl1 . 2.4215(5) yes Ru1 . Cl2 . 2.4163(5) yes Ru1 . P1 . 2.3379(5) yes Ru1 . C15 . 2.252(2) yes Ru1 . C16 . 2.217(2) yes Ru1 . C17 . 2.189(2) yes Ru1 . C18 . 2.209(2) yes Ru1 . C19 . 2.215(2) yes Ru1 . C20 . 2.238(2) yes P1 . N1 . 1.7017(18) yes P1 . C3 . 1.822(2) yes P1 . C9 . 1.814(2) yes N1 . N2 . 1.443(2) yes N1 . H1 . 0.90(3) no N2 . C1 . 1.495(3) yes N2 . C2 . 1.494(3) yes N2 . H2 . 0.90(3) no C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C2 . H23 . 1.000 no C3 . C4 . 1.403(3) yes C3 . C8 . 1.393(3) yes C4 . C5 . 1.384(3) yes C4 . H41 . 1.000 no C5 . C6 . 1.389(4) yes C5 . H51 . 1.000 no C6 . C7 . 1.385(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.392(4) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.391(3) yes C9 . C14 . 1.398(3) yes C10 . C11 . 1.387(3) yes C10 . H101 . 1.000 no C11 . C12 . 1.385(4) yes C11 . H111 . 1.000 no C12 . C13 . 1.377(4) yes C12 . H121 . 1.000 no C13 . C14 . 1.389(3) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.405(3) yes C15 . C20 . 1.437(3) yes C15 . C21 . 1.523(3) yes C16 . C17 . 1.430(3) yes C16 . H161 . 1.000 no C17 . C18 . 1.410(3) yes C17 . H171 . 1.000 no C18 . C19 . 1.432(3) yes C18 . C24 . 1.502(3) yes C19 . C20 . 1.395(3) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.533(4) yes C21 . C23 . 1.518(4) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C22 . H222 . 1.000 no C22 . H223 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C23 . H233 . 1.000 no C24 . H241 . 1.000 no C24 . H242 . 1.000 no C24 . H243 . 1.000 no O1 . C25 . 1.429(3) yes O1 . C28 . 1.396(4) yes C25 . C26 . 1.512(5) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . C27 . 1.521(5) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . C28 . 1.511(5) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ru1 . Cl2 . 86.93(2) yes Cl1 . Ru1 . P1 . 89.238(19) yes Cl2 . Ru1 . P1 . 87.117(18) yes Cl1 . Ru1 . C15 . 89.69(6) yes Cl2 . Ru1 . C15 . 144.70(6) yes P1 . Ru1 . C15 . 127.99(6) yes Cl1 . Ru1 . C16 . 113.16(6) yes Cl2 . Ru1 . C16 . 159.02(6) yes P1 . Ru1 . C16 . 98.63(6) yes C15 . Ru1 . C16 . 36.64(8) yes Cl1 . Ru1 . C17 . 150.54(6) yes Cl2 . Ru1 . C17 . 122.50(6) yes P1 . Ru1 . C17 . 90.88(6) yes C15 . Ru1 . C17 . 67.35(8) yes C16 . Ru1 . C17 . 37.86(8) yes Cl1 . Ru1 . C18 . 159.70(6) yes Cl2 . Ru1 . C18 . 91.14(6) yes P1 . Ru1 . C18 . 110.86(6) yes C15 . Ru1 . C18 . 80.27(8) yes C16 . Ru1 . C18 . 67.94(8) yes Cl1 . Ru1 . C19 . 121.97(6) yes Cl2 . Ru1 . C19 . 85.57(6) yes P1 . Ru1 . C19 . 147.40(7) yes C15 . Ru1 . C19 . 66.72(9) yes C16 . Ru1 . C19 . 78.74(8) yes Cl1 . Ru1 . C20 . 93.92(6) yes Cl2 . Ru1 . C20 . 107.89(6) yes P1 . Ru1 . C20 . 164.79(6) yes C15 . Ru1 . C20 . 37.32(8) yes C16 . Ru1 . C20 . 66.46(8) yes C17 . Ru1 . C18 . 37.38(8) yes C17 . Ru1 . C19 . 66.95(8) yes C18 . Ru1 . C19 . 37.76(8) yes C17 . Ru1 . C20 . 79.09(8) yes C18 . Ru1 . C20 . 67.46(8) yes C19 . Ru1 . C20 . 36.50(9) yes Ru1 . P1 . N1 . 114.58(7) yes Ru1 . P1 . C3 . 119.01(7) yes N1 . P1 . C3 . 105.09(9) yes Ru1 . P1 . C9 . 114.15(7) yes N1 . P1 . C9 . 96.46(9) yes C3 . P1 . C9 . 104.73(10) yes P1 . N1 . N2 . 119.60(14) yes P1 . N1 . H1 . 117.7(18) no N2 . N1 . H1 . 108.2(18) no N1 . N2 . C1 . 113.54(18) yes N1 . N2 . C2 . 108.18(18) yes C1 . N2 . C2 . 111.64(18) yes N1 . N2 . H2 . 104.4(18) no C1 . N2 . H2 . 109.9(18) no C2 . N2 . H2 . 108.9(18) no N2 . C1 . H11 . 109.467 no N2 . C1 . H12 . 109.467 no H11 . C1 . H12 . 109.476 no N2 . C1 . H13 . 109.467 no H11 . C1 . H13 . 109.476 no H12 . C1 . H13 . 109.476 no N2 . C2 . H21 . 109.467 no N2 . C2 . H22 . 109.466 no H21 . C2 . H22 . 109.476 no N2 . C2 . H23 . 109.467 no H21 . C2 . H23 . 109.476 no H22 . C2 . H23 . 109.476 no P1 . C3 . C4 . 119.46(17) yes P1 . C3 . C8 . 120.52(17) yes C4 . C3 . C8 . 119.5(2) yes C3 . C4 . C5 . 119.9(2) yes C3 . C4 . H41 . 120.030 no C5 . C4 . H41 . 120.030 no C4 . C5 . C6 . 120.2(2) yes C4 . C5 . H51 . 119.921 no C6 . C5 . H51 . 119.921 no C5 . C6 . C7 . 120.3(2) yes C5 . C6 . H61 . 119.831 no C7 . C6 . H61 . 119.831 no C6 . C7 . C8 . 119.8(2) yes C6 . C7 . H71 . 120.076 no C8 . C7 . H71 . 120.076 no C3 . C8 . C7 . 120.2(2) yes C3 . C8 . H81 . 119.904 no C7 . C8 . H81 . 119.904 no P1 . C9 . C10 . 118.41(16) yes P1 . C9 . C14 . 121.70(18) yes C10 . C9 . C14 . 119.7(2) yes C9 . C10 . C11 . 120.3(2) yes C9 . C10 . H101 . 119.844 no C11 . C10 . H101 . 119.844 no C10 . C11 . C12 . 119.9(2) yes C10 . C11 . H111 . 120.053 no C12 . C11 . H111 . 120.052 no C11 . C12 . C13 . 119.9(2) yes C11 . C12 . H121 . 120.039 no C13 . C12 . H121 . 120.039 no C12 . C13 . C14 . 121.0(2) yes C12 . C13 . H131 . 119.484 no C14 . C13 . H131 . 119.484 no C9 . C14 . C13 . 119.1(2) yes C9 . C14 . H141 . 120.453 no C13 . C14 . H141 . 120.453 no Ru1 . C15 . C16 . 70.34(12) yes Ru1 . C15 . C20 . 70.83(12) yes C16 . C15 . C20 . 118.5(2) yes Ru1 . C15 . C21 . 133.13(16) yes C16 . C15 . C21 . 123.8(2) yes C20 . C15 . C21 . 117.7(2) yes Ru1 . C16 . C15 . 73.03(12) yes Ru1 . C16 . C17 . 70.02(12) yes C15 . C16 . C17 . 120.7(2) yes Ru1 . C16 . H161 . 129.803 no C15 . C16 . H161 . 119.666 no C17 . C16 . H161 . 119.666 no Ru1 . C17 . C16 . 72.13(12) yes Ru1 . C17 . C18 . 72.09(12) yes C16 . C17 . C18 . 121.2(2) yes Ru1 . C17 . H171 . 128.721 no C16 . C17 . H171 . 119.415 no C18 . C17 . H171 . 119.415 no Ru1 . C18 . C17 . 70.53(12) yes Ru1 . C18 . C19 . 71.34(12) yes C17 . C18 . C19 . 117.5(2) yes Ru1 . C18 . C24 . 128.30(16) yes C17 . C18 . C24 . 121.5(2) yes C19 . C18 . C24 . 121.0(2) yes Ru1 . C19 . C18 . 70.91(12) yes Ru1 . C19 . C20 . 72.65(13) yes C18 . C19 . C20 . 121.8(2) yes Ru1 . C19 . H191 . 130.020 no C18 . C19 . H191 . 119.088 no C20 . C19 . H191 . 119.087 no Ru1 . C20 . C15 . 71.85(12) yes Ru1 . C20 . C19 . 70.85(12) yes C15 . C20 . C19 . 120.4(2) yes Ru1 . C20 . H201 . 130.020 no C15 . C20 . H201 . 119.822 no C19 . C20 . H201 . 119.822 no C15 . C21 . C22 . 108.5(2) yes C15 . C21 . C23 . 115.0(2) yes C22 . C21 . C23 . 109.5(2) yes C15 . C21 . H211 . 106.411 no C22 . C21 . H211 . 112.174 no C23 . C21 . H211 . 105.279 no C21 . C22 . H221 . 109.466 no C21 . C22 . H222 . 109.467 no H221 . C22 . H222 . 109.476 no C21 . C22 . H223 . 109.466 no H221 . C22 . H223 . 109.475 no H222 . C22 . H223 . 109.477 no C21 . C23 . H231 . 109.466 no C21 . C23 . H232 . 109.466 no H231 . C23 . H232 . 109.476 no C21 . C23 . H233 . 109.467 no H231 . C23 . H233 . 109.476 no H232 . C23 . H233 . 109.476 no C18 . C24 . H241 . 109.467 no C18 . C24 . H242 . 109.466 no H241 . C24 . H242 . 109.476 no C18 . C24 . H243 . 109.467 no H241 . C24 . H243 . 109.476 no H242 . C24 . H243 . 109.476 no C25 . O1 . C28 . 107.6(2) yes O1 . C25 . C26 . 105.4(2) yes O1 . C25 . H251 . 110.480 no C26 . C25 . H251 . 110.479 no O1 . C25 . H252 . 110.479 no C26 . C25 . H252 . 110.479 no H251 . C25 . H252 . 109.467 no C25 . C26 . C27 . 102.8(3) yes C25 . C26 . H261 . 111.106 no C27 . C26 . H261 . 111.106 no C25 . C26 . H262 . 111.105 no C27 . C26 . H262 . 111.105 no H261 . C26 . H262 . 109.466 no C26 . C27 . C28 . 104.0(3) yes C26 . C27 . H271 . 110.810 no C28 . C27 . H271 . 110.811 no C26 . C27 . H272 . 110.811 no C28 . C27 . H272 . 110.811 no H271 . C27 . H272 . 109.466 no O1 . C28 . C27 . 109.0(3) yes O1 . C28 . H281 . 109.594 no C27 . C28 . H281 . 109.593 no O1 . C28 . H282 . 109.595 no C27 . C28 . H282 . 109.594 no H281 . C28 . H282 . 109.467 no loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N1 H1 Cl3 0.90(3) 2.23(3) 3.1039(19) 164(3) yes N2 H2 Cl1 0.90(3) 2.43(3) 3.190(2) 142(2) yes N2 H2 Cl2 0.90(3) 2.53(3) 3.138(2) 125(2) yes # The N2...Cl1 and N2...Cl2 interactions are a possible bifurcated #hydrogen bond