# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global #=============================================================================== _audit_creation_date 08-09-02 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Carmichael, Duncan' 'Mathey, Francois' 'Ricard, Louis' 'Seeboth, Nicolas' _publ_contact_author 'Dr Duncan Carmichael' _publ_contact_author_address ; DCPH Ecole polytechnique 2 route de saclay Palaiseau 91128 FRANCE ; _publ_contact_author_email 'DUNCANC@MARS.POLYTECHNIQUE.FR' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Chem. Comm.. The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #============================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of 2-silyl substituted phospharuthenocenes and an elaboraton into the first phospharuthenocene-phosphine complex. ; _publ_section_exptl_prep ; All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; data_rumup_compound_4 _database_code_CSD 193091 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H54 P2 Ru2' _chemical_formula_weight 846.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.087(5) _cell_length_b 14.757(5) _cell_length_c 12.041(5) _cell_angle_alpha 90.000 _cell_angle_beta 96.340(5) _cell_angle_gamma 90.000 _cell_volume 1958.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'brownish red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type 'multiple scans' _exptl_absorpt_correction_T_min 0.8433 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15659 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5702 _reflns_number_gt 4346 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.3357P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5702 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.063174(15) -0.033786(12) -0.077393(16) 0.02123(8) Uani 1 1 d . . . P1 P 0.09086(5) 0.10242(4) 0.00550(5) 0.02293(15) Uani 1 1 d . . . C1 C 0.0850(2) 0.20657(18) -0.0723(2) 0.0286(5) Uani 1 1 d . . . H1 H 0.0203 0.2233 -0.1268 0.034 Uiso 1 1 calc R . . C2 C 0.1834(2) 0.25756(17) -0.0437(2) 0.0318(6) Uani 1 1 d . . . C3 C 0.2676(2) 0.21914(17) 0.0478(2) 0.0306(6) Uani 1 1 d . . . C4 C 0.2307(2) 0.13879(17) 0.0875(2) 0.0264(5) Uani 1 1 d . . . C5 C 0.2107(3) 0.3449(2) -0.1002(3) 0.0462(8) Uani 1 1 d . . . H5A H 0.1413 0.3618 -0.1538 0.069 Uiso 1 1 calc R . . H5B H 0.2827 0.3370 -0.1397 0.069 Uiso 1 1 calc R . . H5C H 0.2258 0.3927 -0.0440 0.069 Uiso 1 1 calc R . . C6 C 0.3851(3) 0.2673(2) 0.0857(3) 0.0494(8) Uani 1 1 d . . . H6A H 0.3684 0.3202 0.1308 0.074 Uiso 1 1 calc R . . H6B H 0.4234 0.2871 0.0202 0.074 Uiso 1 1 calc R . . H6C H 0.4397 0.2260 0.1306 0.074 Uiso 1 1 calc R . . C7 C 0.2878(2) 0.08719(18) 0.1838(2) 0.0287(5) Uani 1 1 d . . . C8 C 0.2874(2) -0.0078(2) 0.1835(3) 0.0334(6) Uani 1 1 d . . . H8 H 0.2521 -0.0394 0.1193 0.040 Uiso 1 1 calc R . . C9 C 0.3378(3) -0.0563(2) 0.2756(3) 0.0436(7) Uani 1 1 d . . . H9 H 0.3369 -0.1206 0.2740 0.052 Uiso 1 1 calc R . . C10 C 0.3892(3) -0.0115(3) 0.3697(3) 0.0511(9) Uani 1 1 d . . . H10 H 0.4251 -0.0449 0.4322 0.061 Uiso 1 1 calc R . . C11 C 0.3884(3) 0.0824(2) 0.3727(3) 0.0494(8) Uani 1 1 d . . . H11 H 0.4228 0.1134 0.4377 0.059 Uiso 1 1 calc R . . C12 C 0.3376(2) 0.1307(2) 0.2813(3) 0.0405(7) Uani 1 1 d . . . H12 H 0.3365 0.1950 0.2846 0.049 Uiso 1 1 calc R . . C13 C 0.1582(2) -0.0069(2) -0.2283(2) 0.0312(6) Uani 1 1 d . . . C14 C 0.0610(2) -0.06901(19) -0.2576(2) 0.0294(6) Uani 1 1 d . . . C15 C 0.0840(2) -0.14846(17) -0.1922(2) 0.0309(6) Uani 1 1 d . . . C16 C 0.1965(2) -0.13687(18) -0.1210(2) 0.0314(6) Uani 1 1 d . . . C17 C 0.2415(2) -0.04960(19) -0.1437(2) 0.0320(6) Uani 1 1 d . . . C18 C 0.1789(3) 0.0802(2) -0.2857(3) 0.0470(8) Uani 1 1 d . . . H18A H 0.2243 0.1217 -0.2330 0.070 Uiso 1 1 calc R . . H18B H 0.1005 0.1075 -0.3129 0.070 Uiso 1 1 calc R . . H18C H 0.2254 0.0688 -0.3489 0.070 Uiso 1 1 calc R . . C19 C -0.0381(3) -0.0550(2) -0.3514(3) 0.0439(7) Uani 1 1 d . . . H19A H -0.0082 -0.0711 -0.4224 0.066 Uiso 1 1 calc R . . H19B H -0.0633 0.0086 -0.3534 0.066 Uiso 1 1 calc R . . H19C H -0.1076 -0.0936 -0.3397 0.066 Uiso 1 1 calc R . . C20 C 0.0139(3) -0.23507(19) -0.2068(3) 0.0433(7) Uani 1 1 d . . . H20A H -0.0713 -0.2216 -0.2318 0.065 Uiso 1 1 calc R . . H20B H 0.0193 -0.2675 -0.1354 0.065 Uiso 1 1 calc R . . H20C H 0.0477 -0.2729 -0.2627 0.065 Uiso 1 1 calc R . . C21 C 0.2587(3) -0.2073(2) -0.0454(3) 0.0505(8) Uani 1 1 d . . . H21A H 0.3112 -0.2443 -0.0875 0.076 Uiso 1 1 calc R . . H21B H 0.1977 -0.2460 -0.0161 0.076 Uiso 1 1 calc R . . H21C H 0.3078 -0.1775 0.0168 0.076 Uiso 1 1 calc R . . C22 C 0.3638(2) -0.0122(2) -0.0990(3) 0.0485(8) Uani 1 1 d . . . H22A H 0.3896 -0.0393 -0.0259 0.073 Uiso 1 1 calc R . . H22B H 0.3582 0.0537 -0.0912 0.073 Uiso 1 1 calc R . . H22C H 0.4232 -0.0268 -0.1509 0.073 Uiso 1 1 calc R . . 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 0.02047(11) 0.01978(12) 0.02365(13) -0.00230(7) 0.00333(8) -0.00123(7) P1 0.0239(3) 0.0200(3) 0.0248(4) -0.0002(2) 0.0023(3) -0.0016(2) C1 0.0337(12) 0.0258(13) 0.0269(14) 0.0029(10) 0.0062(11) 0.0007(10) C2 0.0384(13) 0.0228(13) 0.0364(15) 0.0007(11) 0.0131(12) -0.0003(11) C3 0.0279(12) 0.0266(13) 0.0383(15) -0.0031(11) 0.0077(11) -0.0042(10) C4 0.0246(11) 0.0234(12) 0.0314(14) -0.0035(10) 0.0040(10) -0.0034(9) C5 0.0533(17) 0.0305(16) 0.059(2) 0.0113(14) 0.0238(16) -0.0020(13) C6 0.0372(15) 0.0399(17) 0.070(2) 0.0013(16) 0.0033(15) -0.0168(13) C7 0.0220(10) 0.0295(13) 0.0341(15) 0.0001(11) 0.0013(10) -0.0003(10) C8 0.0298(12) 0.0304(14) 0.0384(16) -0.0015(12) -0.0027(12) -0.0007(11) C9 0.0380(15) 0.0386(16) 0.052(2) 0.0083(15) -0.0049(15) 0.0052(13) C10 0.0457(18) 0.057(2) 0.046(2) 0.0113(17) -0.0158(16) 0.0030(16) C11 0.0445(17) 0.057(2) 0.043(2) -0.0020(16) -0.0134(15) 0.0004(15) C12 0.0349(14) 0.0390(16) 0.0452(18) -0.0052(14) -0.0062(13) -0.0025(12) C13 0.0365(14) 0.0334(14) 0.0253(14) -0.0041(11) 0.0106(11) 0.0067(12) C14 0.0275(12) 0.0344(14) 0.0273(14) -0.0078(11) 0.0070(11) 0.0017(11) C15 0.0325(12) 0.0274(13) 0.0348(15) -0.0092(11) 0.0130(11) -0.0034(10) C16 0.0298(12) 0.0309(14) 0.0341(15) -0.0075(12) 0.0067(11) 0.0085(11) C17 0.0231(12) 0.0418(16) 0.0326(15) -0.0098(12) 0.0096(11) -0.0020(10) C18 0.0630(19) 0.0345(17) 0.048(2) 0.0021(14) 0.0264(16) -0.0021(15) C19 0.0435(16) 0.0585(19) 0.0291(16) -0.0056(14) 0.0011(13) 0.0077(14) C20 0.0508(16) 0.0308(15) 0.0503(19) -0.0172(14) 0.0146(15) -0.0098(13) C21 0.0588(19) 0.0416(18) 0.051(2) 0.0013(15) 0.0044(16) 0.0238(15) C22 0.0255(13) 0.070(2) 0.052(2) -0.0247(18) 0.0103(13) -0.0128(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C15 2.213(3) . ? Ru1 C16 2.224(2) . ? Ru1 C17 2.225(2) . ? Ru1 C14 2.229(3) . ? Ru1 C13 2.234(3) . ? Ru1 P1 2.2401(9) 3 ? Ru1 P1 2.2501(9) . ? Ru1 Ru1 2.6471(8) 3 ? P1 C1 1.798(3) . ? P1 C4 1.825(3) . ? P1 Ru1 2.2401(9) 3 ? C1 C2 1.339(4) . ? C2 C3 1.476(4) . ? C2 C5 1.503(4) . ? C3 C4 1.359(3) . ? C3 C6 1.510(4) . ? C4 C7 1.470(4) . ? C7 C12 1.397(4) . ? C7 C8 1.402(4) . ? C8 C9 1.384(4) . ? C9 C10 1.379(5) . ? C10 C11 1.386(5) . ? C11 C12 1.378(4) . ? C13 C14 1.430(4) . ? C13 C17 1.442(4) . ? C13 C18 1.489(4) . ? C14 C15 1.420(4) . ? C14 C19 1.501(4) . ? C15 C16 1.443(4) . ? C15 C20 1.496(4) . ? C16 C17 1.419(4) . ? C16 C21 1.498(4) . ? C17 C22 1.508(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Ru1 C16 37.96(10) . . ? C15 Ru1 C17 62.43(9) . . ? C16 Ru1 C17 37.19(10) . . ? C15 Ru1 C14 37.27(10) . . ? C16 Ru1 C14 63.05(10) . . ? C17 Ru1 C14 62.65(10) . . ? C15 Ru1 C13 62.41(10) . . ? C16 Ru1 C13 62.89(10) . . ? C17 Ru1 C13 37.73(10) . . ? C14 Ru1 C13 37.36(10) . . ? C15 Ru1 P1 91.86(7) . 3 ? C16 Ru1 P1 109.69(8) . 3 ? C17 Ru1 P1 146.82(8) . 3 ? C14 Ru1 P1 110.12(7) . 3 ? C13 Ru1 P1 147.43(8) . 3 ? C15 Ru1 P1 160.30(7) . . ? C16 Ru1 P1 130.85(7) . . ? C17 Ru1 P1 99.78(7) . . ? C14 Ru1 P1 128.79(8) . . ? C13 Ru1 P1 98.54(8) . . ? P1 Ru1 P1 107.75(3) 3 . ? C15 Ru1 Ru1 145.87(6) . 3 ? C16 Ru1 Ru1 147.25(7) . 3 ? C17 Ru1 Ru1 148.50(7) . 3 ? C14 Ru1 Ru1 145.45(7) . 3 ? C13 Ru1 Ru1 147.07(8) . 3 ? P1 Ru1 Ru1 54.05(3) 3 3 ? P1 Ru1 Ru1 53.70(2) . 3 ? C1 P1 C4 90.59(12) . . ? C1 P1 Ru1 127.08(8) . 3 ? C4 P1 Ru1 124.22(9) . 3 ? C1 P1 Ru1 122.49(9) . . ? C4 P1 Ru1 124.68(8) . . ? Ru1 P1 Ru1 72.25(3) 3 . ? C2 C1 P1 111.4(2) . . ? C1 C2 C3 114.0(2) . . ? C1 C2 C5 124.4(3) . . ? C3 C2 C5 121.6(2) . . ? C4 C3 C2 114.1(2) . . ? C4 C3 C6 126.0(3) . . ? C2 C3 C6 119.9(2) . . ? C3 C4 C7 127.6(2) . . ? C3 C4 P1 109.7(2) . . ? C7 C4 P1 122.70(18) . . ? C12 C7 C8 117.5(3) . . ? C12 C7 C4 121.3(2) . . ? C8 C7 C4 121.0(2) . . ? C9 C8 C7 120.9(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 119.8(3) . . ? C12 C11 C10 120.0(3) . . ? C11 C12 C7 121.4(3) . . ? C14 C13 C17 107.5(3) . . ? C14 C13 C18 126.1(3) . . ? C17 C13 C18 125.9(3) . . ? C14 C13 Ru1 71.11(15) . . ? C17 C13 Ru1 70.77(14) . . ? C18 C13 Ru1 129.9(2) . . ? C15 C14 C13 107.9(2) . . ? C15 C14 C19 127.1(3) . . ? C13 C14 C19 124.6(3) . . ? C15 C14 Ru1 70.77(15) . . ? C13 C14 Ru1 71.53(15) . . ? C19 C14 Ru1 128.99(18) . . ? C14 C15 C16 108.8(2) . . ? C14 C15 C20 125.5(3) . . ? C16 C15 C20 125.1(3) . . ? C14 C15 Ru1 71.96(14) . . ? C16 C15 Ru1 71.42(14) . . ? C20 C15 Ru1 129.60(17) . . ? C17 C16 C15 107.0(2) . . ? C17 C16 C21 126.8(3) . . ? C15 C16 C21 126.0(3) . . ? C17 C16 Ru1 71.43(14) . . ? C15 C16 Ru1 70.62(13) . . ? C21 C16 Ru1 127.2(2) . . ? C16 C17 C13 108.8(2) . . ? C16 C17 C22 125.8(3) . . ? C13 C17 C22 125.0(3) . . ? C16 C17 Ru1 71.38(13) . . ? C13 C17 Ru1 71.50(14) . . ? C22 C17 Ru1 129.32(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.667 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.104 #============================================================ data_rupsi_compound_6a _database_code_CSD 193092 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H47 P Ru Si' _chemical_formula_weight 579.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9390(10) _cell_length_b 42.4640(10) _cell_length_c 8.1660(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.0700(10) _cell_angle_gamma 90.00 _cell_volume 2911.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'cube' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type 'multiple scans' _exptl_absorpt_correction_T_min 0.8807 _exptl_absorpt_correction_T_max 0.8807 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14078 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -53 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 30.02 _reflns_number_total 8165 _reflns_number_gt 6814 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.7198P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8165 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.714451(15) -0.148747(3) -0.203781(15) 0.01736(5) Uani 1 1 d . . . P1 P -0.57781(5) -0.132075(11) -0.39634(5) 0.01919(9) Uani 1 1 d . . . Si1 Si -0.65923(6) -0.061721(11) -0.34703(6) 0.01985(10) Uani 1 1 d . . . C1 C -0.4712(2) -0.15649(4) -0.2138(2) 0.0208(3) Uani 1 1 d . . . C2 C -0.4622(2) -0.14225(4) -0.0518(2) 0.0214(3) Uani 1 1 d . . . C3 C -0.5403(2) -0.11217(4) -0.0748(2) 0.0212(3) Uani 1 1 d . . . C4 C -0.6089(2) -0.10254(4) -0.2541(2) 0.0201(3) Uani 1 1 d . . . C5 C -0.3928(2) -0.18588(4) -0.2389(2) 0.0210(3) Uani 1 1 d . . . C6 C -0.4611(2) -0.20457(5) -0.3882(2) 0.0273(4) Uani 1 1 d . . . H6 H -0.5636 -0.1993 -0.4678 0.033 Uiso 1 1 calc R . . C7 C -0.3816(2) -0.23046(5) -0.4210(2) 0.0320(4) Uani 1 1 d . . . H7 H -0.4286 -0.2424 -0.5243 0.038 Uiso 1 1 calc R . . C8 C -0.2338(2) -0.23908(5) -0.3042(2) 0.0303(4) Uani 1 1 d . . . H8 H -0.1807 -0.2572 -0.3252 0.036 Uiso 1 1 calc R . . C9 C -0.1650(2) -0.22094(5) -0.1570(2) 0.0272(4) Uani 1 1 d . . . H9 H -0.0636 -0.2266 -0.0766 0.033 Uiso 1 1 calc R . . C10 C -0.2425(2) -0.19455(4) -0.1256(2) 0.0236(4) Uani 1 1 d . . . H10 H -0.1922 -0.1821 -0.0248 0.028 Uiso 1 1 calc R . . C11 C -0.3764(2) -0.15620(5) 0.1254(2) 0.0282(4) Uani 1 1 d . . . H11A H -0.3760 -0.1792 0.1164 0.042 Uiso 1 1 calc R . . H11B H -0.4310 -0.1500 0.2060 0.042 Uiso 1 1 calc R . . H11C H -0.2665 -0.1484 0.1690 0.042 Uiso 1 1 calc R . . C12 C -0.5422(2) -0.09244(5) 0.0787(2) 0.0288(4) Uani 1 1 d . . . H12A H -0.6358 -0.0787 0.0427 0.043 Uiso 1 1 calc R . . H12B H -0.4453 -0.0796 0.1199 0.043 Uiso 1 1 calc R . . H12C H -0.5465 -0.1063 0.1729 0.043 Uiso 1 1 calc R . . C13 C -0.4619(2) -0.04331(5) -0.3353(2) 0.0284(4) Uani 1 1 d . . . H13 H -0.4856 -0.0212 -0.3781 0.034 Uiso 1 1 calc R . . C14 C -0.3840(3) -0.05949(5) -0.4538(3) 0.0408(5) Uani 1 1 d . . . H14A H -0.2856 -0.0484 -0.4456 0.061 Uiso 1 1 calc R . . H14B H -0.4575 -0.0590 -0.5746 0.061 Uiso 1 1 calc R . . H14C H -0.3594 -0.0814 -0.4167 0.061 Uiso 1 1 calc R . . C15 C -0.3441(3) -0.04136(7) -0.1488(3) 0.0526(7) Uani 1 1 d . . . H15A H -0.3168 -0.0627 -0.1019 0.079 Uiso 1 1 calc R . . H15B H -0.3927 -0.0297 -0.0763 0.079 Uiso 1 1 calc R . . H15C H -0.2474 -0.0305 -0.1485 0.079 Uiso 1 1 calc R . . C16 C -0.7482(2) -0.03461(5) -0.2192(2) 0.0261(4) Uani 1 1 d . . . H16 H -0.6704 -0.0341 -0.0973 0.031 Uiso 1 1 calc R . . C17 C -0.9054(2) -0.04604(6) -0.2063(3) 0.0373(5) Uani 1 1 d . . . H17A H -0.9329 -0.0332 -0.1212 0.056 Uiso 1 1 calc R . . H17B H -0.8948 -0.0681 -0.1689 0.056 Uiso 1 1 calc R . . H17C H -0.9895 -0.0442 -0.3206 0.056 Uiso 1 1 calc R . . C18 C -0.7655(3) -0.00045(5) -0.2849(3) 0.0423(5) Uani 1 1 d . . . H18A H -0.8424 0.0004 -0.4040 0.063 Uiso 1 1 calc R . . H18B H -0.6620 0.0073 -0.2841 0.063 Uiso 1 1 calc R . . H18C H -0.8032 0.0127 -0.2085 0.063 Uiso 1 1 calc R . . C19 C -0.7842(2) -0.06545(4) -0.5869(2) 0.0240(4) Uani 1 1 d . . . H19 H -0.7274 -0.0811 -0.6361 0.029 Uiso 1 1 calc R . . C20 C -0.9501(2) -0.07905(6) -0.6217(2) 0.0350(5) Uani 1 1 d . . . H20A H -1.0121 -0.0646 -0.5762 0.052 Uiso 1 1 calc R . . H20B H -0.9412 -0.0995 -0.5636 0.052 Uiso 1 1 calc R . . H20C H -1.0037 -0.0817 -0.7475 0.052 Uiso 1 1 calc R . . C21 C -0.7930(3) -0.03503(5) -0.6920(2) 0.0411(5) Uani 1 1 d . . . H21A H -0.8404 -0.0397 -0.8168 0.062 Uiso 1 1 calc R . . H21B H -0.6855 -0.0265 -0.6670 0.062 Uiso 1 1 calc R . . H21C H -0.8589 -0.0195 -0.6593 0.062 Uiso 1 1 calc R . . C22 C -0.8993(2) -0.15099(4) -0.0839(3) 0.0281(4) Uani 1 1 d . . . C23 C -0.8047(2) -0.17877(5) -0.0417(2) 0.0260(4) Uani 1 1 d . . . C24 C -0.8223(2) -0.19491(4) -0.2013(2) 0.0235(3) Uani 1 1 d . . . C25 C -0.9279(2) -0.17700(5) -0.3411(2) 0.0244(4) Uani 1 1 d . . . C26 C -0.9769(2) -0.15008(4) -0.2691(3) 0.0270(4) Uani 1 1 d . . . C27 C -0.9286(3) -0.12856(6) 0.0442(3) 0.0485(6) Uani 1 1 d . . . H27A H -0.8362 -0.1285 0.1522 0.073 Uiso 1 1 calc R . . H27B H -1.0233 -0.1352 0.0695 0.073 Uiso 1 1 calc R . . H27C H -0.9454 -0.1073 -0.0056 0.073 Uiso 1 1 calc R . . C28 C -0.7176(3) -0.19085(6) 0.1385(3) 0.0460(6) Uani 1 1 d . . . H28A H -0.7906 -0.2033 0.1789 0.069 Uiso 1 1 calc R . . H28B H -0.6768 -0.1730 0.2176 0.069 Uiso 1 1 calc R . . H28C H -0.6285 -0.2041 0.1367 0.069 Uiso 1 1 calc R . . C29 C -0.7578(3) -0.22682(5) -0.2166(3) 0.0389(5) Uani 1 1 d . . . H29A H -0.6595 -0.2304 -0.1177 0.058 Uiso 1 1 calc R . . H29B H -0.7351 -0.2281 -0.3256 0.058 Uiso 1 1 calc R . . H29C H -0.8365 -0.2429 -0.2165 0.058 Uiso 1 1 calc R . . C30 C -0.9898(3) -0.18689(6) -0.5295(2) 0.0416(5) Uani 1 1 d . . . H30A H -1.0911 -0.1980 -0.5540 0.062 Uiso 1 1 calc R . . H30B H -0.9123 -0.2009 -0.5531 0.062 Uiso 1 1 calc R . . H30C H -1.0062 -0.1682 -0.6040 0.062 Uiso 1 1 calc R . . C31 C -1.1097(2) -0.12811(6) -0.3648(3) 0.0465(6) Uani 1 1 d . . . H31A H -1.2083 -0.1349 -0.3483 0.070 Uiso 1 1 calc R . . H31B H -1.1243 -0.1284 -0.4894 0.070 Uiso 1 1 calc R . . H31C H -1.0831 -0.1067 -0.3194 0.070 Uiso 1 1 calc R . . 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 0.01887(8) 0.01683(8) 0.01807(7) 0.00069(5) 0.00851(5) 0.00100(5) P1 0.0210(2) 0.0196(2) 0.01869(18) 0.00116(16) 0.00908(16) 0.00181(16) Si1 0.0211(2) 0.0172(2) 0.0218(2) -0.00008(17) 0.00802(17) 0.00035(17) C1 0.0191(8) 0.0218(9) 0.0222(8) 0.0024(6) 0.0080(6) 0.0016(6) C2 0.0197(8) 0.0242(9) 0.0205(7) 0.0020(6) 0.0071(6) 0.0011(7) C3 0.0214(8) 0.0223(9) 0.0203(7) -0.0008(6) 0.0076(6) -0.0020(7) C4 0.0207(8) 0.0188(9) 0.0220(7) -0.0014(6) 0.0089(6) -0.0013(6) C5 0.0225(8) 0.0196(9) 0.0240(7) 0.0040(6) 0.0117(6) 0.0013(6) C6 0.0231(9) 0.0312(11) 0.0274(8) -0.0023(7) 0.0086(7) 0.0033(7) C7 0.0322(10) 0.0324(12) 0.0341(9) -0.0088(8) 0.0147(8) 0.0003(8) C8 0.0308(10) 0.0240(10) 0.0440(10) -0.0003(8) 0.0232(8) 0.0038(8) C9 0.0210(8) 0.0284(11) 0.0346(9) 0.0062(8) 0.0127(7) 0.0045(7) C10 0.0220(8) 0.0218(9) 0.0282(8) 0.0012(7) 0.0104(7) 0.0007(7) C11 0.0276(9) 0.0329(11) 0.0223(8) 0.0041(7) 0.0061(7) 0.0060(8) C12 0.0366(10) 0.0281(11) 0.0218(8) -0.0027(7) 0.0101(7) 0.0003(8) C13 0.0259(9) 0.0246(10) 0.0343(9) 0.0035(8) 0.0097(7) -0.0044(7) C14 0.0321(11) 0.0368(13) 0.0617(13) 0.0014(10) 0.0268(10) -0.0014(9) C15 0.0328(12) 0.074(2) 0.0436(12) 0.0079(12) 0.0033(9) -0.0219(12) C16 0.0301(9) 0.0222(10) 0.0248(8) -0.0028(7) 0.0078(7) 0.0026(7) C17 0.0335(11) 0.0466(14) 0.0368(10) -0.0081(9) 0.0184(8) 0.0017(9) C18 0.0630(16) 0.0214(12) 0.0448(12) -0.0007(8) 0.0213(11) 0.0115(9) C19 0.0269(9) 0.0235(10) 0.0225(8) -0.0007(7) 0.0095(7) 0.0041(7) C20 0.0268(10) 0.0467(14) 0.0294(9) -0.0078(9) 0.0071(7) -0.0020(9) C21 0.0564(14) 0.0330(12) 0.0278(9) 0.0077(8) 0.0066(9) 0.0043(10) C22 0.0344(10) 0.0229(10) 0.0389(10) -0.0065(7) 0.0277(9) -0.0077(7) C23 0.0301(9) 0.0258(10) 0.0237(8) 0.0024(7) 0.0115(7) -0.0075(7) C24 0.0238(9) 0.0181(9) 0.0314(8) -0.0005(7) 0.0131(7) -0.0016(6) C25 0.0200(8) 0.0281(10) 0.0266(8) -0.0007(7) 0.0098(7) -0.0048(7) C26 0.0198(9) 0.0242(10) 0.0419(10) 0.0050(8) 0.0167(8) 0.0001(7) C27 0.0666(16) 0.0361(13) 0.0676(15) -0.0201(11) 0.0548(13) -0.0167(11) C28 0.0558(15) 0.0495(16) 0.0300(10) 0.0125(9) 0.0111(10) -0.0183(11) C29 0.0404(12) 0.0178(10) 0.0648(14) -0.0015(9) 0.0262(10) 0.0024(8) C30 0.0366(12) 0.0558(15) 0.0293(10) -0.0053(9) 0.0073(8) -0.0169(10) C31 0.0223(10) 0.0355(13) 0.0836(16) 0.0197(12) 0.0206(10) 0.0056(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C23 2.1817(17) . ? Ru1 C2 2.1862(17) . ? Ru1 C24 2.1879(18) . ? Ru1 C22 2.1927(17) . ? Ru1 C3 2.1955(17) . ? Ru1 C25 2.2065(17) . ? Ru1 C26 2.2211(18) . ? Ru1 C1 2.2284(17) . ? Ru1 C4 2.2750(17) . ? Ru1 P1 2.4050(5) . ? P1 C4 1.7949(17) . ? P1 C1 1.7975(17) . ? Si1 C4 1.8837(18) . ? Si1 C19 1.8995(17) . ? Si1 C13 1.9012(19) . ? Si1 C16 1.9017(18) . ? C1 C2 1.431(2) . ? C1 C5 1.480(2) . ? C2 C3 1.436(2) . ? C2 C11 1.507(2) . ? C3 C4 1.439(2) . ? C3 C12 1.513(2) . ? C5 C10 1.394(2) . ? C5 C6 1.406(2) . ? C6 C7 1.384(3) . ? C7 C8 1.387(3) . ? C8 C9 1.382(3) . ? C9 C10 1.387(3) . ? C13 C15 1.528(3) . ? C13 C14 1.535(3) . ? C16 C17 1.524(3) . ? C16 C18 1.536(3) . ? C19 C20 1.525(3) . ? C19 C21 1.538(3) . ? C22 C23 1.423(3) . ? C22 C26 1.431(3) . ? C22 C27 1.503(3) . ? C23 C24 1.433(2) . ? C23 C28 1.499(3) . ? C24 C25 1.426(3) . ? C24 C29 1.494(3) . ? C25 C26 1.422(3) . ? C25 C30 1.505(3) . ? C26 C31 1.501(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Ru1 C2 104.66(6) . . ? C23 Ru1 C24 38.28(6) . . ? C2 Ru1 C24 118.67(7) . . ? C23 Ru1 C22 37.97(7) . . ? C2 Ru1 C22 122.72(7) . . ? C24 Ru1 C22 63.57(7) . . ? C23 Ru1 C3 118.12(6) . . ? C2 Ru1 C3 38.27(6) . . ? C24 Ru1 C3 150.66(6) . . ? C22 Ru1 C3 109.62(6) . . ? C23 Ru1 C25 63.60(6) . . ? C2 Ru1 C25 154.23(7) . . ? C24 Ru1 C25 37.86(7) . . ? C22 Ru1 C25 63.29(7) . . ? C3 Ru1 C25 167.33(7) . . ? C23 Ru1 C26 63.31(7) . . ? C2 Ru1 C26 159.73(7) . . ? C24 Ru1 C26 63.05(7) . . ? C22 Ru1 C26 37.83(7) . . ? C3 Ru1 C26 130.54(7) . . ? C25 Ru1 C26 37.47(7) . . ? C23 Ru1 C1 120.30(7) . . ? C2 Ru1 C1 37.83(6) . . ? C24 Ru1 C1 107.87(7) . . ? C22 Ru1 C1 154.74(7) . . ? C3 Ru1 C1 65.26(6) . . ? C25 Ru1 C1 125.85(7) . . ? C26 Ru1 C1 162.03(7) . . ? C23 Ru1 C4 151.17(6) . . ? C2 Ru1 C4 65.34(6) . . ? C24 Ru1 C4 170.39(6) . . ? C22 Ru1 C4 122.75(6) . . ? C3 Ru1 C4 37.49(6) . . ? C25 Ru1 C4 135.82(6) . . ? C26 Ru1 C4 116.62(6) . . ? C1 Ru1 C4 69.53(6) . . ? C23 Ru1 P1 160.92(5) . . ? C2 Ru1 P1 71.21(4) . . ? C24 Ru1 P1 126.45(5) . . ? C22 Ru1 P1 159.11(6) . . ? C3 Ru1 P1 70.71(4) . . ? C25 Ru1 P1 111.86(5) . . ? C26 Ru1 P1 125.61(5) . . ? C1 Ru1 P1 45.46(4) . . ? C4 Ru1 P1 45.00(4) . . ? C4 P1 C1 91.26(8) . . ? C4 P1 Ru1 63.67(5) . . ? C1 P1 Ru1 62.07(5) . . ? C4 Si1 C19 108.28(8) . . ? C4 Si1 C13 105.59(8) . . ? C19 Si1 C13 107.06(8) . . ? C4 Si1 C16 115.02(8) . . ? C19 Si1 C16 114.06(8) . . ? C13 Si1 C16 106.18(9) . . ? C2 C1 C5 127.28(15) . . ? C2 C1 P1 111.62(13) . . ? C5 C1 P1 120.85(12) . . ? C2 C1 Ru1 69.49(9) . . ? C5 C1 Ru1 130.10(12) . . ? P1 C1 Ru1 72.47(6) . . ? C1 C2 C3 112.58(14) . . ? C1 C2 C11 124.74(16) . . ? C3 C2 C11 122.65(15) . . ? C1 C2 Ru1 72.69(10) . . ? C3 C2 Ru1 71.21(9) . . ? C11 C2 Ru1 125.56(13) . . ? C2 C3 C4 113.86(15) . . ? C2 C3 C12 121.80(15) . . ? C4 C3 C12 124.30(16) . . ? C2 C3 Ru1 70.51(10) . . ? C4 C3 Ru1 74.25(10) . . ? C12 C3 Ru1 125.56(12) . . ? C3 C4 P1 110.68(13) . . ? C3 C4 Si1 129.14(13) . . ? P1 C4 Si1 116.79(8) . . ? C3 C4 Ru1 68.25(10) . . ? P1 C4 Ru1 71.34(6) . . ? Si1 C4 Ru1 144.08(9) . . ? C10 C5 C6 117.35(16) . . ? C10 C5 C1 121.65(16) . . ? C6 C5 C1 120.73(15) . . ? C7 C6 C5 121.12(17) . . ? C6 C7 C8 120.52(18) . . ? C9 C8 C7 119.04(18) . . ? C8 C9 C10 120.67(17) . . ? C9 C10 C5 121.26(17) . . ? C15 C13 C14 110.26(19) . . ? C15 C13 Si1 112.50(14) . . ? C14 C13 Si1 113.44(14) . . ? C17 C16 C18 109.87(17) . . ? C17 C16 Si1 114.46(14) . . ? C18 C16 Si1 113.04(13) . . ? C20 C19 C21 110.74(17) . . ? C20 C19 Si1 114.44(12) . . ? C21 C19 Si1 113.89(13) . . ? C23 C22 C26 108.11(15) . . ? C23 C22 C27 125.99(19) . . ? C26 C22 C27 125.5(2) . . ? C23 C22 Ru1 70.59(10) . . ? C26 C22 Ru1 72.16(10) . . ? C27 C22 Ru1 128.39(13) . . ? C22 C23 C24 107.77(15) . . ? C22 C23 C28 125.93(18) . . ? C24 C23 C28 125.94(19) . . ? C22 C23 Ru1 71.43(10) . . ? C24 C23 Ru1 71.09(10) . . ? C28 C23 Ru1 128.31(14) . . ? C25 C24 C23 108.01(16) . . ? C25 C24 C29 125.81(17) . . ? C23 C24 C29 125.78(17) . . ? C25 C24 Ru1 71.78(10) . . ? C23 C24 Ru1 70.63(10) . . ? C29 C24 Ru1 128.88(13) . . ? C26 C25 C24 108.12(15) . . ? C26 C25 C30 126.14(18) . . ? C24 C25 C30 125.44(18) . . ? C26 C25 Ru1 71.82(10) . . ? C24 C25 Ru1 70.36(10) . . ? C30 C25 Ru1 128.43(13) . . ? C25 C26 C22 107.98(16) . . ? C25 C26 C31 125.79(19) . . ? C22 C26 C31 125.25(19) . . ? C25 C26 Ru1 70.71(10) . . ? C22 C26 Ru1 70.01(11) . . ? C31 C26 Ru1 133.67(14) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.865 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.071