# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pb2006-sr _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _chemical_name_systematic ; ? ; _chemical_compound_source 'Nicola Bell' _exptl_crystal_recrystallization_method 'diffusion of Et2O into MeOH/MeCN solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H57 B2 F18 N17 P3 Ru S6' _chemical_formula_weight 1525.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_cell_setting monoclinic 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 21.6714(7) _cell_length_b 18.3557(6) _cell_length_c 17.4348(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.030(2) _cell_angle_gamma 90.00 _cell_volume 6908.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120.00(10) _cell_measurement_reflns_used 6342 _cell_measurement_theta_min 3.1202 _cell_measurement_theta_max 58.8555 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.1769 _exptl_crystal_size_mid 0.0378 _exptl_crystal_size_min 0.0330 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3092 _exptl_absorpt_coefficient_mu 5.013 _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.877 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.00(10) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9923 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 58.93 _reflns_number_total 9923 _reflns_number_gt 6441 _reflns_threshold_expression >2\s(I) _reflns_odcompleteness_completeness 99.96 _reflns_odcompleteness_theta 58.86 _reflns_odcompleteness_iscentric 1 _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. #=================================================================== The following checkCIF ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-level. #============================================================= THETM01_ALERT_3_B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5555 RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25 Weighted R factor given 0.270 PLAT084_ALERT_2_C High wR2 Value ................................. 0.27 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.14 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.9 Ratio PLAT234_ALERT_4_C Large Hirshfeld Difference N9 -- B1A .. 0.16 Ang. PLAT234_ALERT_4_C Large Hirshfeld Difference N52 -- B1A .. 0.16 Ang. PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.6 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.5 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.4 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.0180 Ang PLAT072_ALERT_2_G SHELXL First Parameter in WGHT Unusually Large. 0.14 PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large. 27.13 Weak data, diffracting at 0.9 A PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 4 PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C2 PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C4 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C27 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for B1A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT242_ALERT_2_G Check Low Ueq as Compared to Neighbors for N52 PLAT213_ALERT_2_C Atom N11 has ADP max/min Ratio ..... 3.5 prola PLAT213_ALERT_2_C Atom N12 has ADP max/min Ratio ..... 3.6 prola PLAT213_ALERT_2_C Atom N14 has ADP max/min Ratio ..... 3.3 prola PLAT213_ALERT_2_C Atom C24 has ADP max/min Ratio ..... 3.3 prola PLAT213_ALERT_2_C Atom C26 has ADP max/min Ratio ..... 3.2 prola PLAT213_ALERT_2_C Atom C27 has ADP max/min Ratio ..... 3.2 prola PLAT410_ALERT_2_C Short Intra H...H Contact H31 .. H57 .. 1.96 Ang. PLAT413_ALERT_2_C Short Inter XH3 .. XHn H1C .. H54D .. 2.12 Ang. PLAT413_ALERT_2_C Short Inter XH3 .. XHn H13A .. H51D .. 2.12 Ang. PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 27 PLAT003_ALERT_2_G Number of Uiso or Uij Restrained Atom Sites .... 5 PLAT301_ALERT_3_G Note: Main Residue Disorder ................... 14 Perc. Due to significant disorder in one half of the main fragment. Restraints were applied to minimise this. PLAT244_ALERT_4_C Low Solvent Ueq as Compared to Neighbors of P4 PLAT244_ALERT_4_G Low Solvent Ueq as Compared to Neighbors of P1 PLAT244_ALERT_4_G Low Solvent Ueq as Compared to Neighbors of P1 PLAT244_ALERT_4_G Low Solvent Ueq as Compared to Neighbors of P2 PLAT244_ALERT_4_G Low Solvent Ueq as Compared to Neighbors of P2 PLAT244_ALERT_4_C Low Solvent Ueq as Compared to Neighbors of C201 PLAT302_ALERT_4_G Note: Anion/Solvent Disorder ................... 58 Perc. Disorder is common in PF6 counter ions. PLAT605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of . 158 A**3 PLAT869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed ! Platon SQUEEZE used to remove 8 molecules of MeOH and 3 molecules of MeCN per unit cell. PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C38 H54 B2 N16 Ru S6 PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 8 PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... # 107 N52 -B1A -N52 1.555 1.555 1.555 27.20 Deg. PLAT811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms .... ! PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 87 No Action Taken ; _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^)+(0.1380P)^2^+27.1268P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9923 _refine_ls_number_parameters 926 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2696 _refine_ls_wR_factor_gt 0.2466 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 C8 C 0.1660(4) 0.6856(5) -0.2669(5) 0.030(2) Uani 1 1 d . . . C9 C 0.2025(5) 0.6199(6) -0.3824(5) 0.048(3) Uani 1 1 d . . . H9A H 0.2420 0.6153 -0.3533 0.072 Uiso 1 1 calc R . . H9B H 0.2082 0.6376 -0.4331 0.072 Uiso 1 1 calc R . . H9C H 0.1825 0.5732 -0.3861 0.072 Uiso 1 1 calc R . . C10 C 0.1170(4) 0.7141(5) -0.3798(5) 0.038(2) Uani 1 1 d . . . H10 H 0.1058 0.7160 -0.4325 0.046 Uiso 1 1 calc R . . C11 C 0.0915(4) 0.7513(5) -0.3267(5) 0.033(2) Uani 1 1 d . . . H11 H 0.0591 0.7843 -0.3354 0.039 Uiso 1 1 calc R . . C12 C 0.1783(5) 0.8737(5) -0.1779(5) 0.041(2) Uani 1 1 d . . . C13 C 0.2325(6) 0.9927(6) -0.1504(7) 0.063(3) Uani 1 1 d . . . H13A H 0.2618 0.9750 -0.1843 0.095 Uiso 1 1 calc R . . H13B H 0.2539 1.0065 -0.1021 0.095 Uiso 1 1 calc R . . H13C H 0.2112 1.0342 -0.1732 0.095 Uiso 1 1 calc R . . C14 C 0.1431(5) 0.9385(5) -0.0848(6) 0.045(3) Uani 1 1 d . . . H14 H 0.1388 0.9758 -0.0495 0.054 Uiso 1 1 calc R . . C15 C 0.1078(4) 0.8789(5) -0.0937(5) 0.037(2) Uani 1 1 d . . . H15 H 0.0752 0.8665 -0.0650 0.044 Uiso 1 1 calc R . . C16 C 0.1672(4) 0.7082(5) -0.0591(5) 0.0281(19) Uani 1 1 d . . . C17 C 0.2062(5) 0.6333(6) 0.0518(6) 0.051(3) Uani 1 1 d . . . H17A H 0.2424 0.6141 0.0307 0.076 Uiso 1 1 calc R . . H17B H 0.1884 0.5965 0.0821 0.076 Uiso 1 1 calc R . . H17C H 0.2177 0.6747 0.0836 0.076 Uiso 1 1 calc R . . C18 C 0.1050(4) 0.6197(5) -0.0273(6) 0.042(2) Uani 1 1 d . . . H18 H 0.0894 0.5805 -0.0014 0.050 Uiso 1 1 calc R . . C19 C 0.0786(4) 0.6545(5) -0.0893(6) 0.040(2) Uani 1 1 d . . . H19 H 0.0407 0.6420 -0.1149 0.048 Uiso 1 1 calc R . . C20 C 0.3963(5) 0.6299(8) -0.1450(6) 0.058(3) Uani 1 1 d . . . C21 C 0.3444(6) 0.5134(7) -0.1823(8) 0.077(4) Uani 1 1 d . . . H21A H 0.3327 0.4936 -0.2325 0.115 Uiso 1 1 calc R . . H21B H 0.3088 0.5351 -0.1623 0.115 Uiso 1 1 calc R . . H21C H 0.3601 0.4751 -0.1485 0.115 Uiso 1 1 calc R . . C22 C 0.4351(5) 0.5629(9) -0.2379(7) 0.070(4) Uani 1 1 d . . . H22 H 0.4403 0.5264 -0.2738 0.084 Uiso 1 1 calc R . . C23 C 0.4709(5) 0.6246(9) -0.2239(6) 0.069(4) Uani 1 1 d . . . H23 H 0.5051 0.6377 -0.2494 0.082 Uiso 1 1 calc R . . C25 C 0.3660(6) 0.8850(7) 0.0559(7) 0.069(4) Uani 1 1 d . . . H25A H 0.3573 0.8672 0.1056 0.103 Uiso 1 1 calc R . . H25B H 0.3279 0.8898 0.0237 0.103 Uiso 1 1 calc R . . H25C H 0.3860 0.9316 0.0615 0.103 Uiso 1 1 calc R . . C26 C 0.4537(5) 0.7964(10) 0.0602(7) 0.086(5) Uani 1 1 d . . . H26 H 0.4651 0.7981 0.1129 0.104 Uiso 1 1 calc R . . C27 C 0.4813(6) 0.7547(11) 0.0046(7) 0.098(6) Uani 1 1 d . . . H27 H 0.5138 0.7218 0.0136 0.118 Uiso 1 1 calc R . . C29 C 0.3679(6) 0.8600(7) -0.3809(6) 0.064(4) Uani 1 1 d . . . H29A H 0.3624 0.8183 -0.4141 0.096 Uiso 1 1 calc R . . H29B H 0.3818 0.9006 -0.4095 0.096 Uiso 1 1 calc R . . H29C H 0.3292 0.8720 -0.3611 0.096 Uiso 1 1 calc R . . C30 C 0.4691(6) 0.8791(8) -0.2990(8) 0.079(5) Uani 1 1 d . . . H30 H 0.4852 0.9171 -0.3263 0.095 Uiso 1 1 calc R . . C31 C 0.4955(6) 0.8478(9) -0.2333(7) 0.076(4) Uani 1 1 d . . . H31 H 0.5324 0.8624 -0.2064 0.091 Uiso 1 1 calc R . . C201 C 0.9737(9) 0.4496(11) 0.4089(9) 0.085(5) Uani 1 1 d . . . C301 C 1.0307(9) 0.4135(10) 0.3986(9) 0.115(8) Uani 1 1 d . . . H30A H 1.0392 0.4167 0.3456 0.173 Uiso 1 1 calc R . . H30B H 1.0276 0.3632 0.4130 0.173 Uiso 1 1 calc R . . H30C H 1.0636 0.4362 0.4304 0.173 Uiso 1 1 calc R . . N001 N 0.9295(10) 0.4792(10) 0.4191(11) 0.138(7) Uani 1 1 d . . . N3 N 0.1210(3) 0.7331(4) -0.2547(4) 0.0289(16) Uani 1 1 d . . . N4 N 0.1637(3) 0.6715(4) -0.3435(4) 0.0342(18) Uani 1 1 d . . . N5 N 0.1289(4) 0.8390(4) -0.1537(4) 0.0351(18) Uani 1 1 d . . . N6 N 0.1874(4) 0.9349(4) -0.1376(5) 0.045(2) Uani 1 1 d . . . N7 N 0.1159(3) 0.7120(4) -0.1101(4) 0.0291(16) Uani 1 1 d . . . N8 N 0.1612(4) 0.6555(4) -0.0106(4) 0.0390(19) Uani 1 1 d . . . N9 N 0.4465(4) 0.6641(6) -0.1644(5) 0.062(3) Uani 1 1 d . D . N10 N 0.3909(4) 0.5671(6) -0.1878(5) 0.061(3) Uani 1 1 d . . . N11 N 0.4503(5) 0.7724(7) -0.0668(5) 0.076(3) Uani 1 1 d U D . N12 N 0.4066(4) 0.8337(7) 0.0207(5) 0.077(4) Uani 1 1 d . D . N14 N 0.4139(4) 0.8434(6) -0.3171(5) 0.057(3) Uani 1 1 d . D . F19 F 0.9634(5) 0.4207(5) 0.8476(5) 0.113(3) Uani 1 1 d . . . F20 F 0.9196(5) 0.4775(4) 0.7458(5) 0.101(3) Uani 1 1 d . . . F21 F 0.8778(5) 0.4835(6) 0.8608(8) 0.153(5) Uani 1 1 d . . . F22 F 1.0067(5) 0.5210(6) 0.7993(6) 0.124(4) Uani 1 1 d . . . F23 F 0.9661(9) 0.5204(6) 0.9136(5) 0.196(7) Uani 1 1 d . . . F24 F 0.9217(6) 0.5818(4) 0.8116(5) 0.125(4) Uani 1 1 d . . . P4 P 0.94100(19) 0.50109(18) 0.83026(17) 0.0680(10) Uani 1 1 d . . . S002 S 0.22286(10) 0.64884(12) -0.20249(12) 0.0333(5) Uani 1 1 d . . . S003 S 0.23210(10) 0.76610(14) -0.05074(12) 0.0369(6) Uani 1 1 d . . . S004 S 0.34253(11) 0.73394(15) -0.27232(13) 0.0431(6) Uani 1 1 d . D . S005 S 0.23002(11) 0.84165(13) -0.24126(13) 0.0372(6) Uani 1 1 d . . . S006 S 0.34917(13) 0.85436(18) -0.12262(15) 0.0574(8) Uani 1 1 d . D . S007 S 0.34327(12) 0.65917(19) -0.08379(14) 0.0574(8) Uani 1 1 d . . . Ru01 Ru 0.28670(3) 0.75090(4) -0.16228(4) 0.0363(3) Uani 1 1 d . . . B1 B 0.1015(5) 0.7639(5) -0.1778(6) 0.028(2) Uani 1 1 d . . . B1A B 0.4729(7) 0.7400(11) -0.1414(8) 0.073(5) Uani 1 1 d U . . N13 N 0.4591(4) 0.7918(6) -0.2136(5) 0.059(3) Uani 1 1 d . D . C28 C 0.4076(5) 0.7901(7) -0.2657(6) 0.052(3) Uani 1 1 d . . . C24 C 0.4037(5) 0.8214(8) -0.0565(6) 0.064(4) Uani 1 1 d U . . N2 N 0.0297(3) 0.7751(4) -0.1955(4) 0.0386(19) Uani 1 1 d D . . C5 C -0.0012(5) 0.8380(5) -0.1988(6) 0.046(3) Uani 1 1 d D . . H5 H 0.0158 0.8831 -0.1847 0.055 Uiso 1 1 calc R . . N1 N -0.0599(4) 0.8267(5) -0.2252(5) 0.060(3) Uani 1 1 d D . . C7 C -0.0129(4) 0.7226(6) -0.2220(6) 0.046(3) Uani 1 1 d D . . H7 H -0.0040 0.6734 -0.2276 0.055 Uiso 1 1 calc R . . C6 C -0.0691(5) 0.7530(7) -0.2384(7) 0.061(3) Uani 1 1 d D . . H6 H -0.1060 0.7296 -0.2549 0.073 Uiso 1 1 calc R . . C4 C -0.1064(7) 0.8845(8) -0.2384(7) 0.096(6) Uani 1 1 d D . . H4A H -0.0899 0.9296 -0.2160 0.115 Uiso 1 1 calc R . . H4B H -0.1428 0.8717 -0.2127 0.115 Uiso 1 1 calc R . . C3 C -0.1250(6) 0.8963(7) -0.3230(6) 0.067(4) Uani 1 1 d D . . H3A H -0.0882 0.9065 -0.3490 0.080 Uiso 1 1 calc R . . H3B H -0.1431 0.8517 -0.3446 0.080 Uiso 1 1 calc R . . C2 C -0.1695(8) 0.9561(9) -0.3387(8) 0.107(7) Uani 1 1 d D . . H2A H -0.1493 1.0015 -0.3227 0.129 Uiso 1 1 calc R . . H2B H -0.2037 0.9490 -0.3072 0.129 Uiso 1 1 calc R . . C1 C -0.1952(6) 0.9635(8) -0.4213(7) 0.074(4) Uani 1 1 d D . . H1A H -0.1633 0.9529 -0.4545 0.112 Uiso 1 1 calc R . . H1B H -0.2098 1.0124 -0.4305 0.112 Uiso 1 1 calc R . . H1C H -0.2289 0.9300 -0.4317 0.112 Uiso 1 1 calc R . . P2 P 0.7983(2) 0.6869(3) 0.5765(3) 0.0529(16) Uani 0.532(5) 1 d P A 1 F7 F 0.7729(6) 0.7654(7) 0.5941(8) 0.076(4) Uani 0.532(5) 1 d P A 1 F8 F 0.8657(6) 0.7167(7) 0.5871(7) 0.059(3) Uani 0.532(5) 1 d P A 1 F9 F 0.7935(7) 0.7093(8) 0.4861(8) 0.075(4) Uani 0.532(5) 1 d P A 1 F11 F 0.8035(6) 0.6754(10) 0.6583(8) 0.099(6) Uani 0.532(5) 1 d P A 1 F12 F 0.8242(6) 0.6096(7) 0.5554(8) 0.071(4) Uani 0.532(5) 1 d P A 1 F18 F 0.7294(6) 0.6550(9) 0.5632(11) 0.087(5) Uani 0.532(5) 1 d P A 1 P2' P 0.7506(3) 0.5984(3) 0.4235(4) 0.0551(18) Uani 0.468(5) 1 d P A 2 F7' F 0.6828(8) 0.5897(14) 0.3921(11) 0.121(9) Uani 0.468(5) 1 d P A 2 F8' F 0.7644(6) 0.5680(6) 0.3477(6) 0.046(3) Uani 0.468(5) 1 d P A 2 F9' F 0.7615(8) 0.6764(9) 0.3867(10) 0.084(5) Uani 0.468(5) 1 d P A 2 F11' F 0.7404(7) 0.5214(8) 0.4607(9) 0.067(4) Uani 0.468(5) 1 d P A 2 F12' F 0.8211(8) 0.5953(11) 0.4540(13) 0.106(7) Uani 0.468(5) 1 d P A 2 F18' F 0.7328(13) 0.6373(10) 0.4992(12) 0.126(9) Uani 0.468(5) 1 d P A 2 P1 P 0.6538(3) 0.6991(3) 0.1761(3) 0.0496(13) Uani 0.50 1 d P B 1 F1 F 0.7034(6) 0.6475(9) 0.1456(8) 0.076(4) Uani 0.50 1 d P B 1 F2 F 0.6357(6) 0.6404(7) 0.2388(8) 0.064(3) Uani 0.50 1 d P B 1 F3 F 0.6021(7) 0.6665(9) 0.1134(8) 0.073(4) Uani 0.50 1 d P B 1 F4 F 0.7012(7) 0.7298(7) 0.2353(7) 0.070(4) Uani 0.50 1 d P B 1 F5 F 0.6700(8) 0.7592(9) 0.1181(9) 0.087(5) Uani 0.50 1 d P B 1 F6 F 0.6063(6) 0.7592(6) 0.2016(7) 0.057(3) Uani 0.50 1 d P B 1 P1' P 0.5137(3) 0.5206(3) 0.0043(3) 0.0348(12) Uani 0.50 1 d P C -2 F1' F 0.5233(7) 0.5340(8) -0.0851(6) 0.054(3) Uani 0.50 1 d P C -2 F3' F 0.5067(7) 0.5066(7) 0.0936(6) 0.049(3) Uani 0.50 1 d P C -2 F4' F 0.5114(9) 0.6067(8) 0.0170(8) 0.077(5) Uani 0.50 1 d P C -2 F5' F 0.5863(7) 0.5230(9) 0.0215(9) 0.070(4) Uani 0.50 1 d P C -2 F2' F 0.5186(8) 0.4351(8) -0.0077(8) 0.058(4) Uani 0.50 1 d P C -2 F6' F 0.4429(7) 0.5178(11) -0.0153(8) 0.071(5) Uani 0.50 1 d P C -2 N52 N 0.5429(5) 0.7502(9) -0.1235(7) 0.033(4) Uani 0.542(9) 1 d PDU D 1 C55 C 0.5765(7) 0.6903(10) -0.1116(9) 0.039(5) Uani 0.542(9) 1 d PDU D 1 H55 H 0.5622 0.6434 -0.1231 0.047 Uiso 0.542(9) 1 calc PR D 1 N51 N 0.6337(6) 0.7061(8) -0.0810(11) 0.047(5) Uani 0.542(9) 1 d PD D 1 C57 C 0.5818(7) 0.8067(9) -0.0989(9) 0.038(4) Uani 0.542(9) 1 d PD D 1 H57 H 0.5707 0.8556 -0.1003 0.046 Uiso 0.542(9) 1 calc PR D 1 C56 C 0.6382(7) 0.7812(9) -0.0724(10) 0.046(5) Uani 0.542(9) 1 d PD D 1 H56 H 0.6724 0.8080 -0.0528 0.055 Uiso 0.542(9) 1 calc PR D 1 C54 C 0.6833(7) 0.6539(10) -0.0612(10) 0.050 Uiso 0.542(9) 1 d PD D 1 H54A H 0.6651 0.6070 -0.0507 0.060 Uiso 0.542(9) 1 calc PR D 1 H54B H 0.7070 0.6699 -0.0144 0.060 Uiso 0.542(9) 1 calc PR D 1 C53 C 0.7268(8) 0.6446(10) -0.1242(10) 0.050 Uiso 0.542(9) 1 d PD D 1 H53A H 0.7438 0.6918 -0.1359 0.060 Uiso 0.542(9) 1 calc PR D 1 H53B H 0.7610 0.6135 -0.1052 0.060 Uiso 0.542(9) 1 calc PR D 1 C52 C 0.6969(10) 0.6129(10) -0.1953(10) 0.050 Uiso 0.542(9) 1 d PD D 1 H52A H 0.7247 0.6165 -0.2358 0.060 Uiso 0.542(9) 1 calc PR D 1 H52B H 0.6597 0.6403 -0.2113 0.060 Uiso 0.542(9) 1 calc PR D 1 C51 C 0.6798(10) 0.5324(9) -0.1840(12) 0.050 Uiso 0.542(9) 1 d PD D 1 H51A H 0.7123 0.5089 -0.1523 0.075 Uiso 0.542(9) 1 calc PR D 1 H51B H 0.6745 0.5087 -0.2332 0.075 Uiso 0.542(9) 1 calc PR D 1 H51C H 0.6419 0.5296 -0.1595 0.075 Uiso 0.542(9) 1 calc PR D 1 N52' N 0.5446(9) 0.7087(11) -0.1232(14) 0.050 Uiso 0.458(9) 1 d PD D 2 C55' C 0.5706(8) 0.6445(11) -0.1070(14) 0.050 Uiso 0.458(9) 1 d PD D 2 H55' H 0.5516 0.5996 -0.1172 0.060 Uiso 0.458(9) 1 calc PR D 2 N51' N 0.6279(7) 0.6538(10) -0.0739(11) 0.050 Uiso 0.458(9) 1 d PD D 2 C57' C 0.5861(10) 0.7604(12) -0.0934(15) 0.050 Uiso 0.458(9) 1 d PD D 2 H57' H 0.5789 0.8104 -0.0931 0.060 Uiso 0.458(9) 1 calc PR D 2 C56' C 0.6391(12) 0.7276(13) -0.065(2) 0.050 Uiso 0.458(9) 1 d PD D 2 H56' H 0.6752 0.7499 -0.0435 0.060 Uiso 0.458(9) 1 calc PR D 2 C54' C 0.6710(9) 0.5952(11) -0.0504(11) 0.050 Uiso 0.458(9) 1 d PD D 2 H54C H 0.6480 0.5502 -0.0464 0.060 Uiso 0.458(9) 1 calc PR D 2 H54D H 0.6912 0.6062 0.0001 0.060 Uiso 0.458(9) 1 calc PR D 2 C53' C 0.7193(8) 0.5851(13) -0.1064(10) 0.050 Uiso 0.458(9) 1 d PD D 2 H53C H 0.7490 0.6244 -0.0988 0.060 Uiso 0.458(9) 1 calc PR D 2 H53D H 0.7412 0.5400 -0.0936 0.060 Uiso 0.458(9) 1 calc PR D 2 C52' C 0.6976(11) 0.5827(13) -0.1868(11) 0.050 Uiso 0.458(9) 1 d PD D 2 H52C H 0.7338 0.5789 -0.2156 0.060 Uiso 0.458(9) 1 calc PR D 2 H52D H 0.6785 0.6294 -0.1999 0.060 Uiso 0.458(9) 1 calc PR D 2 C51' C 0.6526(11) 0.5243(11) -0.2166(15) 0.050 Uiso 0.458(9) 1 d PD D 2 H51D H 0.6752 0.4815 -0.2292 0.075 Uiso 0.458(9) 1 calc PR D 2 H51E H 0.6286 0.5416 -0.2618 0.075 Uiso 0.458(9) 1 calc PR D 2 H51F H 0.6255 0.5125 -0.1777 0.075 Uiso 0.458(9) 1 calc PR D 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 C8 0.045(5) 0.027(5) 0.021(5) -0.002(4) 0.010(4) -0.011(4) C9 0.055(6) 0.067(7) 0.025(5) -0.005(5) 0.020(5) 0.025(5) C10 0.052(6) 0.041(5) 0.022(5) 0.007(4) 0.002(4) -0.001(5) C11 0.032(5) 0.040(5) 0.025(5) 0.009(4) -0.002(4) 0.001(4) C12 0.066(7) 0.030(5) 0.027(5) -0.003(4) 0.013(5) -0.012(5) C13 0.108(10) 0.041(6) 0.044(7) -0.010(5) 0.025(7) -0.022(6) C14 0.067(7) 0.032(5) 0.037(6) -0.002(4) 0.007(5) -0.001(5) C15 0.049(6) 0.038(5) 0.023(5) -0.003(4) 0.007(4) 0.002(4) C16 0.034(5) 0.035(5) 0.017(4) 0.005(4) 0.013(4) 0.003(4) C17 0.047(6) 0.071(7) 0.035(6) 0.016(5) 0.009(5) 0.009(5) C18 0.041(6) 0.044(6) 0.042(6) 0.016(5) 0.015(5) 0.003(4) C19 0.036(5) 0.044(6) 0.039(6) -0.003(5) 0.003(4) -0.001(4) C20 0.034(6) 0.115(11) 0.026(6) 0.025(7) 0.011(5) 0.024(6) C21 0.092(10) 0.080(9) 0.064(9) 0.039(7) 0.038(7) 0.032(8) C22 0.043(7) 0.134(13) 0.034(6) 0.035(7) 0.010(5) 0.030(8) C23 0.035(6) 0.147(13) 0.023(6) 0.023(7) 0.000(5) 0.019(7) C25 0.084(9) 0.088(9) 0.035(6) -0.017(6) 0.015(6) -0.038(7) C26 0.044(7) 0.194(17) 0.021(6) -0.013(8) 0.006(5) -0.040(9) C27 0.043(7) 0.22(2) 0.028(7) -0.007(9) -0.006(5) -0.031(9) C29 0.086(9) 0.082(9) 0.022(6) 0.010(6) -0.004(6) -0.035(7) C30 0.062(8) 0.112(11) 0.066(9) -0.040(8) 0.023(7) -0.050(8) C31 0.055(7) 0.139(13) 0.035(7) -0.035(8) 0.015(6) -0.046(8) C201 0.079(11) 0.111(14) 0.066(10) 0.011(9) 0.012(9) -0.012(10) C301 0.156(18) 0.112(14) 0.070(11) 0.037(10) -0.028(11) -0.086(14) N001 0.182(19) 0.115(14) 0.119(15) 0.022(11) 0.016(14) 0.016(13) N3 0.036(4) 0.026(4) 0.025(4) -0.003(3) 0.004(3) 0.001(3) N4 0.048(5) 0.030(4) 0.025(4) 0.007(3) 0.009(3) 0.006(3) N5 0.052(5) 0.033(4) 0.020(4) -0.001(3) 0.006(3) 0.001(4) N6 0.076(6) 0.033(4) 0.027(4) -0.006(4) 0.005(4) -0.017(4) N7 0.037(4) 0.024(4) 0.027(4) 0.000(3) 0.005(3) -0.005(3) N8 0.041(5) 0.053(5) 0.023(4) 0.004(4) 0.002(3) 0.011(4) N9 0.047(6) 0.119(9) 0.021(5) 0.009(5) 0.008(4) 0.003(6) N10 0.055(6) 0.092(8) 0.039(6) 0.035(6) 0.021(5) 0.027(5) N11 0.053(6) 0.160(10) 0.014(4) -0.004(5) 0.003(4) -0.025(6) N12 0.045(6) 0.164(12) 0.021(5) -0.033(6) 0.011(4) -0.034(6) N14 0.055(5) 0.097(7) 0.022(4) -0.004(5) 0.019(4) -0.040(5) F19 0.167(9) 0.077(6) 0.091(7) 0.040(5) -0.021(6) -0.018(6) F20 0.160(8) 0.069(5) 0.069(5) -0.009(4) -0.026(5) -0.018(5) F21 0.147(9) 0.115(8) 0.214(13) 0.063(9) 0.111(9) -0.002(7) F22 0.127(8) 0.141(9) 0.105(8) 0.028(7) 0.015(6) -0.061(7) F23 0.42(2) 0.114(8) 0.042(5) 0.004(5) -0.024(9) -0.074(12) F24 0.269(13) 0.041(4) 0.074(6) 0.001(4) 0.067(7) -0.009(6) P4 0.117(3) 0.0511(17) 0.0358(16) 0.0016(14) 0.0090(17) -0.0390(18) S002 0.0388(13) 0.0385(12) 0.0228(11) 0.0048(9) 0.0042(9) 0.0005(9) S003 0.0354(12) 0.0588(15) 0.0168(11) 0.0009(10) 0.0047(9) -0.0071(10) S004 0.0394(13) 0.0707(17) 0.0190(11) 0.0052(11) 0.0019(10) -0.0112(11) S005 0.0532(14) 0.0379(13) 0.0212(11) 0.0032(9) 0.0067(10) -0.0122(10) S006 0.0500(16) 0.096(2) 0.0270(13) -0.0156(14) 0.0055(11) -0.0308(15) S007 0.0406(14) 0.109(2) 0.0232(13) 0.0228(14) 0.0072(11) 0.0189(14) Ru01 0.0354(4) 0.0574(5) 0.0163(4) 0.0036(3) 0.0029(3) -0.0068(3) B1 0.035(6) 0.022(5) 0.028(5) 0.004(4) 0.001(4) -0.003(4) B1A 0.046(7) 0.152(14) 0.024(6) -0.003(8) 0.016(5) 0.006(8) N13 0.045(5) 0.114(8) 0.020(4) -0.016(5) 0.005(4) -0.021(5) C28 0.047(6) 0.091(9) 0.021(5) -0.009(5) 0.014(4) -0.020(6) C24 0.035(6) 0.134(10) 0.026(6) -0.009(6) 0.017(5) -0.027(6) N2 0.046(5) 0.043(5) 0.024(4) -0.005(3) -0.007(3) 0.007(4) C5 0.062(7) 0.038(6) 0.035(6) -0.013(4) -0.007(5) 0.021(5) N1 0.044(5) 0.084(7) 0.050(6) -0.015(5) -0.008(4) 0.030(5) C7 0.045(6) 0.042(6) 0.050(7) 0.001(5) 0.000(5) -0.005(5) C6 0.040(6) 0.080(9) 0.059(8) -0.025(7) -0.012(5) 0.009(6) C4 0.112(12) 0.118(12) 0.051(8) -0.024(8) -0.030(8) 0.075(10) C3 0.063(8) 0.081(9) 0.053(8) -0.020(7) -0.014(6) 0.018(6) C2 0.114(13) 0.141(15) 0.062(9) -0.020(9) -0.023(9) 0.085(12) C1 0.071(9) 0.087(10) 0.063(9) 0.005(7) -0.008(7) 0.018(7) P2 0.049(3) 0.049(3) 0.060(4) 0.009(3) 0.000(3) 0.005(2) F7 0.084(10) 0.063(8) 0.086(11) 0.002(7) 0.029(8) 0.002(7) F8 0.069(8) 0.061(7) 0.048(7) 0.010(6) 0.006(6) -0.005(6) F9 0.093(10) 0.079(9) 0.051(8) 0.000(7) -0.003(7) 0.008(8) F11 0.049(8) 0.187(17) 0.055(9) -0.071(10) -0.031(6) 0.041(9) F12 0.090(10) 0.057(8) 0.070(9) -0.001(7) 0.022(7) 0.000(7) F18 0.054(8) 0.089(11) 0.115(14) 0.028(10) -0.001(8) 0.002(7) P2' 0.068(4) 0.052(4) 0.048(4) 0.013(3) 0.018(3) 0.008(3) F7' 0.055(10) 0.23(3) 0.079(13) 0.019(14) -0.013(9) -0.059(13) F8' 0.060(8) 0.049(7) 0.030(6) 0.008(5) 0.012(5) -0.009(6) F9' 0.086(11) 0.078(11) 0.093(13) 0.014(9) 0.034(10) 0.009(9) F11' 0.077(10) 0.058(9) 0.068(10) 0.012(7) 0.023(8) -0.010(7) F12' 0.072(11) 0.119(15) 0.123(17) 0.029(13) -0.014(11) -0.016(10) F18' 0.25(3) 0.075(12) 0.064(12) -0.004(10) 0.071(15) 0.031(14) P1 0.054(3) 0.049(3) 0.047(3) 0.003(3) 0.014(3) -0.002(3) F1 0.065(9) 0.100(11) 0.065(9) -0.009(8) 0.022(7) 0.001(8) F2 0.072(9) 0.061(8) 0.061(8) 0.012(7) 0.016(7) -0.003(7) F3 0.077(9) 0.096(11) 0.048(8) 0.003(7) 0.007(7) 0.003(8) F4 0.120(12) 0.057(8) 0.037(7) 0.002(6) 0.024(7) 0.025(8) F5 0.103(12) 0.095(12) 0.068(10) 0.031(9) 0.026(9) -0.008(9) F6 0.086(9) 0.049(7) 0.037(7) -0.009(5) 0.011(6) 0.006(6) P1' 0.042(5) 0.044(5) 0.018(2) 0.003(3) 0.005(2) 0.006(3) F1' 0.087(10) 0.060(9) 0.016(6) 0.001(6) 0.008(6) -0.003(7) F3' 0.080(10) 0.043(7) 0.025(6) 0.008(6) 0.014(6) 0.011(7) F4' 0.150(16) 0.043(9) 0.044(8) 0.014(7) 0.050(9) 0.005(9) F5' 0.051(9) 0.083(11) 0.075(11) 0.012(8) -0.008(8) -0.004(8) F2' 0.093(14) 0.035(10) 0.050(8) 0.009(7) 0.033(8) 0.006(9) F6' 0.045(10) 0.108(15) 0.058(9) 0.039(9) -0.003(7) -0.009(10) N52 0.025(7) 0.065(9) 0.008(6) -0.006(7) -0.001(5) -0.003(7) C55 0.049(11) 0.056(11) 0.013(8) -0.011(8) 0.007(8) -0.004(9) N51 0.032(9) 0.068(16) 0.040(12) -0.008(9) 0.001(7) -0.001(9) C57 0.043(10) 0.060(12) 0.011(8) -0.011(8) -0.006(7) 0.007(9) C56 0.058(13) 0.051(12) 0.027(10) -0.001(9) -0.005(9) -0.008(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C8 N3 1.340(11) . ? C8 N4 1.356(11) . ? C8 S002 1.730(9) . ? C9 N4 1.470(11) . ? C10 C11 1.312(13) . ? C10 N4 1.388(12) . ? C11 N3 1.397(11) . ? C12 N6 1.331(12) . ? C12 N5 1.344(12) . ? C12 S005 1.744(10) . ? C13 N6 1.472(13) . ? C14 C15 1.335(14) . ? C14 N6 1.389(13) . ? C15 N5 1.389(12) . ? C16 N8 1.300(11) . ? C16 N7 1.363(11) . ? C16 S003 1.759(9) . ? C17 N8 1.453(12) . ? C18 C19 1.340(13) . ? C18 N8 1.392(12) . ? C19 N7 1.396(12) . ? C20 N9 1.326(15) . ? C20 N10 1.373(17) . ? C20 S007 1.721(11) . ? C21 N10 1.420(16) . ? C22 N10 1.353(14) . ? C22 C23 1.38(2) . ? C23 N9 1.406(16) . ? C25 N12 1.460(16) . ? C26 N12 1.364(18) . ? C26 C27 1.41(2) . ? C27 N11 1.400(16) . ? C29 N14 1.460(14) . ? C30 C31 1.36(2) . ? C30 N14 1.377(14) . ? C31 N13 1.359(16) . ? C201 N001 1.13(2) . ? C201 C301 1.43(2) . ? N3 B1 1.548(12) . ? N5 B1 1.544(12) . ? N7 B1 1.527(12) . ? N9 B1A 1.55(2) . ? N11 C24 1.374(17) . ? N11 B1A 1.549(17) . ? N12 C24 1.362(13) . ? N14 C28 1.342(15) . ? F19 P4 1.575(9) . ? F20 P4 1.566(8) . ? F21 P4 1.547(10) . ? F22 P4 1.608(10) . ? F23 P4 1.547(10) . ? F24 P4 1.565(9) . ? S002 Ru01 2.397(2) . ? S003 Ru01 2.380(2) . ? S004 C28 1.741(10) . ? S004 Ru01 2.377(3) . ? S005 Ru01 2.426(2) . ? S006 C24 1.689(13) . ? S006 Ru01 2.399(3) . ? S007 Ru01 2.432(3) . ? B1 N2 1.574(12) . ? B1A N52 1.534(18) . ? B1A N13 1.584(19) . ? B1A N52' 1.66(2) . ? N13 C28 1.377(13) . ? N2 C5 1.332(11) . ? N2 C7 1.386(12) . ? C5 N1 1.331(12) . ? N1 C6 1.385(14) . ? N1 C4 1.468(13) . ? C7 C6 1.348(14) . ? C4 C3 1.510(14) . ? C3 C2 1.470(14) . ? C2 C1 1.505(14) . ? P2 F11 1.436(16) . ? P2 F8 1.555(13) . ? P2 F12 1.581(14) . ? P2 F7 1.583(14) . ? P2 F18 1.602(14) . ? P2 F9 1.622(14) . ? P2' F8' 1.488(13) . ? P2' F7' 1.531(17) . ? P2' F12' 1.573(18) . ? P2' F18' 1.578(19) . ? P2' F11' 1.580(15) . ? P2' F9' 1.594(17) . ? P1 F4 1.499(16) . ? P1 F5 1.557(15) . ? P1 F1 1.561(15) . ? P1 F6 1.598(13) . ? P1 F2 1.607(14) . ? P1 F3 1.611(15) . ? P1' F6' 1.543(18) . ? P1' F5' 1.575(15) . ? P1' F2' 1.588(17) . ? P1' F4' 1.597(16) . ? P1' F3' 1.597(12) . ? P1' F1' 1.610(12) . ? N52 C55 1.325(17) . ? N52 C57 1.380(17) . ? C55 N51 1.338(16) . ? N51 C56 1.389(19) . ? N51 C54 1.459(16) . ? C57 C56 1.350(18) . ? C54 C53 1.519(18) . ? C53 C52 1.469(17) . ? C52 C51 1.539(17) . ? N52' C55' 1.326(18) . ? N52' C57' 1.378(18) . ? C55' N51' 1.336(17) . ? N51' C56' 1.38(2) . ? N51' C54' 1.458(17) . ? C57' C56' 1.35(2) . ? C54' C53' 1.505(18) . ? C53' C52' 1.439(17) . ? C52' C51' 1.510(18) . ? 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 N3 C8 N4 108.4(8) . . ? N3 C8 S002 129.7(7) . . ? N4 C8 S002 121.9(7) . . ? C11 C10 N4 107.8(8) . . ? C10 C11 N3 108.8(8) . . ? N6 C12 N5 108.7(8) . . ? N6 C12 S005 123.0(8) . . ? N5 C12 S005 127.7(7) . . ? C15 C14 N6 107.9(9) . . ? C14 C15 N5 107.2(9) . . ? N8 C16 N7 109.9(8) . . ? N8 C16 S003 121.4(7) . . ? N7 C16 S003 128.6(6) . . ? C19 C18 N8 104.4(8) . . ? C18 C19 N7 110.7(8) . . ? N9 C20 N10 106.9(10) . . ? N9 C20 S007 128.2(12) . . ? N10 C20 S007 124.8(9) . . ? N10 C22 C23 104.9(13) . . ? C22 C23 N9 108.1(11) . . ? N12 C26 C27 105.6(10) . . ? N11 C27 C26 106.6(14) . . ? C31 C30 N14 106.6(12) . . ? N13 C31 C30 108.8(10) . . ? N001 C201 C301 178(2) . . ? C8 N3 C11 107.2(7) . . ? C8 N3 B1 129.2(7) . . ? C11 N3 B1 123.6(7) . . ? C8 N4 C10 107.8(8) . . ? C8 N4 C9 127.1(8) . . ? C10 N4 C9 125.1(8) . . ? C12 N5 C15 108.0(8) . . ? C12 N5 B1 129.5(8) . . ? C15 N5 B1 122.1(8) . . ? C12 N6 C14 108.1(8) . . ? C12 N6 C13 126.7(9) . . ? C14 N6 C13 125.0(8) . . ? C16 N7 C19 104.4(7) . . ? C16 N7 B1 129.4(7) . . ? C19 N7 B1 126.1(7) . . ? C16 N8 C18 110.5(8) . . ? C16 N8 C17 126.6(8) . . ? C18 N8 C17 122.8(8) . . ? C20 N9 C23 108.4(12) . . ? C20 N9 B1A 130.8(11) . . ? C23 N9 B1A 120.1(10) . . ? C22 N10 C20 111.6(12) . . ? C22 N10 C21 123.4(13) . . ? C20 N10 C21 125.0(10) . . ? C24 N11 C27 109.7(11) . . ? C24 N11 B1A 130.5(10) . . ? C27 N11 B1A 119.6(13) . . ? C24 N12 C26 112.5(11) . . ? C24 N12 C25 123.1(12) . . ? C26 N12 C25 124.3(10) . . ? C28 N14 C30 109.4(11) . . ? C28 N14 C29 123.9(9) . . ? C30 N14 C29 126.7(11) . . ? F21 P4 F23 88.4(9) . . ? F21 P4 F24 92.3(6) . . ? F23 P4 F24 92.5(6) . . ? F21 P4 F20 93.9(7) . . ? F23 P4 F20 175.8(8) . . ? F24 P4 F20 90.9(5) . . ? F21 P4 F19 90.3(6) . . ? F23 P4 F19 87.6(6) . . ? F24 P4 F19 177.3(6) . . ? F20 P4 F19 89.0(5) . . ? F21 P4 F22 178.8(7) . . ? F23 P4 F22 90.9(8) . . ? F24 P4 F22 86.7(6) . . ? F20 P4 F22 86.8(6) . . ? F19 P4 F22 90.6(6) . . ? C8 S002 Ru01 104.2(3) . . ? C16 S003 Ru01 108.2(3) . . ? C28 S004 Ru01 109.6(3) . . ? C12 S005 Ru01 101.2(3) . . ? C24 S006 Ru01 104.9(5) . . ? C20 S007 Ru01 101.4(4) . . ? S004 Ru01 S003 178.84(10) . . ? S004 Ru01 S002 89.04(8) . . ? S003 Ru01 S002 90.86(8) . . ? S004 Ru01 S006 91.26(9) . . ? S003 Ru01 S006 88.86(9) . . ? S002 Ru01 S006 179.05(10) . . ? S004 Ru01 S005 84.26(9) . . ? S003 Ru01 S005 96.89(9) . . ? S002 Ru01 S005 96.90(8) . . ? S006 Ru01 S005 82.23(10) . . ? S004 Ru01 S007 95.53(9) . . ? S003 Ru01 S007 83.31(9) . . ? S002 Ru01 S007 82.71(10) . . ? S006 Ru01 S007 98.16(12) . . ? S005 Ru01 S007 179.56(11) . . ? N7 B1 N5 107.5(7) . . ? N7 B1 N3 112.9(7) . . ? N5 B1 N3 115.7(7) . . ? N7 B1 N2 111.4(7) . . ? N5 B1 N2 106.7(7) . . ? N3 B1 N2 102.5(7) . . ? N52 B1A N9 120.0(13) . . ? N52 B1A N11 99.4(11) . . ? N9 B1A N11 115.2(11) . . ? N52 B1A N13 101.8(11) . . ? N9 B1A N13 107.2(10) . . ? N11 B1A N13 112.6(13) . . ? N52 B1A N52' 27.2(7) . . ? N9 B1A N52' 93.2(13) . . ? N11 B1A N52' 109.4(13) . . ? N13 B1A N52' 117.9(13) . . ? C31 N13 C28 107.8(10) . . ? C31 N13 B1A 125.6(10) . . ? C28 N13 B1A 126.6(10) . . ? N14 C28 N13 107.4(9) . . ? N14 C28 S004 121.1(8) . . ? N13 C28 S004 131.5(9) . . ? N12 C24 N11 105.4(11) . . ? N12 C24 S006 125.7(11) . . ? N11 C24 S006 128.6(8) . . ? C5 N2 C7 105.8(8) . . ? C5 N2 B1 127.3(8) . . ? C7 N2 B1 126.4(8) . . ? N1 C5 N2 110.0(9) . . ? C5 N1 C6 109.2(8) . . ? C5 N1 C4 124.4(11) . . ? C6 N1 C4 126.3(10) . . ? C6 C7 N2 110.2(9) . . ? C7 C6 N1 104.8(9) . . ? N1 C4 C3 112.2(9) . . ? C2 C3 C4 113.7(10) . . ? C3 C2 C1 115.3(11) . . ? F11 P2 F8 86.7(8) . . ? F11 P2 F12 95.8(9) . . ? F8 P2 F12 89.7(7) . . ? F11 P2 F7 86.5(9) . . ? F8 P2 F7 89.7(7) . . ? F12 P2 F7 177.6(9) . . ? F11 P2 F18 94.6(10) . . ? F8 P2 F18 178.3(10) . . ? F12 P2 F18 89.1(8) . . ? F7 P2 F18 91.4(8) . . ? F11 P2 F9 173.7(10) . . ? F8 P2 F9 90.4(7) . . ? F12 P2 F9 89.7(8) . . ? F7 P2 F9 87.9(8) . . ? F18 P2 F9 88.4(8) . . ? F8' P2' F7' 84.6(10) . . ? F8' P2' F12' 91.3(10) . . ? F7' P2' F12' 171.8(14) . . ? F8' P2' F18' 174.2(10) . . ? F7' P2' F18' 92.7(14) . . ? F12' P2' F18' 92.0(14) . . ? F8' P2' F11' 94.3(8) . . ? F7' P2' F11' 83.5(11) . . ? F12' P2' F11' 89.8(10) . . ? F18' P2' F11' 90.4(10) . . ? F8' P2' F9' 86.1(8) . . ? F7' P2' F9' 97.0(12) . . ? F12' P2' F9' 89.7(10) . . ? F18' P2' F9' 89.2(10) . . ? F11' P2' F9' 179.4(11) . . ? F4 P1 F5 90.1(9) . . ? F4 P1 F1 90.7(8) . . ? F5 P1 F1 90.4(9) . . ? F4 P1 F6 88.2(7) . . ? F5 P1 F6 83.1(8) . . ? F1 P1 F6 173.4(8) . . ? F4 P1 F2 88.7(8) . . ? F5 P1 F2 177.0(9) . . ? F1 P1 F2 92.3(8) . . ? F6 P1 F2 94.1(7) . . ? F4 P1 F3 179.1(9) . . ? F5 P1 F3 90.2(9) . . ? F1 P1 F3 90.0(8) . . ? F6 P1 F3 91.0(8) . . ? F2 P1 F3 90.9(8) . . ? F6' P1' F5' 178.1(10) . . ? F6' P1' F2' 90.8(9) . . ? F5' P1' F2' 88.6(10) . . ? F6' P1' F4' 91.2(11) . . ? F5' P1' F4' 89.4(10) . . ? F2' P1' F4' 178.1(11) . . ? F6' P1' F3' 91.8(8) . . ? F5' P1' F3' 89.9(8) . . ? F2' P1' F3' 89.1(7) . . ? F4' P1' F3' 91.0(7) . . ? F6' P1' F1' 90.0(8) . . ? F5' P1' F1' 88.2(8) . . ? F2' P1' F1' 90.4(7) . . ? F4' P1' F1' 89.5(8) . . ? F3' P1' F1' 178.1(9) . . ? C55 N52 C57 105.3(11) . . ? C55 N52 B1A 116.8(14) . . ? C57 N52 B1A 136.1(14) . . ? N52 C55 N51 111.0(14) . . ? C55 N51 C56 108.2(13) . . ? C55 N51 C54 126.1(15) . . ? C56 N51 C54 125.8(14) . . ? C56 C57 N52 110.8(14) . . ? C57 C56 N51 104.7(13) . . ? N51 C54 C53 113.2(15) . . ? C52 C53 C54 113.5(14) . . ? C53 C52 C51 111.5(16) . . ? C55' N52' C57' 106.4(15) . . ? C55' N52' B1A 136.1(18) . . ? C57' N52' B1A 113.7(17) . . ? N52' C55' N51' 109.8(16) . . ? C55' N51' C56' 108.8(15) . . ? C55' N51' C54' 125.1(17) . . ? C56' N51' C54' 126.1(17) . . ? C56' C57' N52' 109.7(17) . . ? C57' C56' N51' 105.0(16) . . ? N51' C54' C53' 111.9(15) . . ? C52' C53' C54' 116.8(16) . . ? C53' C52' C51' 120.1(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 58.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.235 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.134 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 172 53 ' ' 2 0.068 0.284 0.026 82 26 ' ' 3 0.932 0.716 -0.026 82 26 ' ' 4 0.500 0.500 0.500 172 53 ' ' 5 0.932 0.784 0.474 82 26 ' ' 6 0.068 0.216 0.526 82 26 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 936860' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pb1015-sr _audit_creation_method ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H78 B2 F18 N16 P3 Ru S6' _chemical_formula_weight 1941.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_cell_setting monoclinic 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 10.4293(2) _cell_length_b 25.9269(4) _cell_length_c 17.5308(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.999(2) _cell_angle_gamma 90.00 _cell_volume 4618.84(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14945 _cell_measurement_theta_min 4.2779 _cell_measurement_theta_max 74.9827 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.1654 _exptl_crystal_size_mid 0.1201 _exptl_crystal_size_min 0.1117 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1982 _exptl_absorpt_coefficient_mu 3.875 _exptl_absorpt_correction_T_min 0.57369 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44704 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 75.16 _reflns_number_total 9297 _reflns_number_gt 7697 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. #================================================================= The following ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-level. #================================================================= PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.977 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.85 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.1 Ratio PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.1 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds ...............0.0081 Ang PLAT072_ALERT_2_G SHELXL First Parameter in WGHT Unusually Large. 0.16 No Action taken PLAT128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n Yes indeed, this minimised correlation effects by reducing beta. PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of P2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of P4 Some rotational motion is common in PF6, the central atom thus usually has lower ADPs. PLAT231_ALERT_4_G Hirshfeld Test (Solvent) P2 -- F1 .. 5.3 su PLAT231_ALERT_4_G Hirshfeld Test (Solvent) P2 -- F2 .. 8.3 su PLAT231_ALERT_4_G Hirshfeld Test (Solvent) P2 -- F3 .. 8.2 su PLAT231_ALERT_4_G Hirshfeld Test (Solvent) P2 -- F4 .. 5.4 su PLAT231_ALERT_4_G Hirshfeld Test (Solvent) P2 -- F5 .. 13.8 su PLAT231_ALERT_4_G Hirshfeld Test (Solvent) P2 -- F6 .. 10.4 su Common for disordered PF6 anions. This is common for atom pairs which are very different in mass. PLAT605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of . 322 A**3 PLAT869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed ! Platon SQUEEZE used to eliminate 42 e/A**3, equal to one DCM molecule. PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? No Action taken ; _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^)+(0.1567P)^2^+3.2942P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9297 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.2246 _refine_ls_wR_factor_gt 0.2125 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _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 0.0000 0.5000 0.0000 0.03067(16) Uani 1 2 d S . . S2 S -0.16669(10) 0.44954(4) -0.07710(6) 0.0345(2) Uani 1 1 d . . . S3 S -0.15218(10) 0.56195(4) 0.03318(6) 0.0335(2) Uani 1 1 d . . . P4 P 0.5000 0.5000 0.5000 0.0472(4) Uani 1 2 d S . . S5 S 0.04640(10) 0.54452(4) -0.11435(6) 0.0362(2) Uani 1 1 d . . . F7 F 0.4538(5) 0.51299(17) 0.5789(2) 0.0749(10) Uani 1 1 d . . . N8 N -0.4238(3) 0.45536(14) -0.0703(2) 0.0366(7) Uani 1 1 d . . . N9 N -0.0452(4) 0.49024(15) -0.2481(2) 0.0398(8) Uani 1 1 d . . . N10 N -0.3893(4) 0.59580(14) -0.2264(2) 0.0405(8) Uani 1 1 d . . . F11 F 0.3930(5) 0.5384(2) 0.4526(2) 0.0995(17) Uani 1 1 d . . . N12 N -0.2030(4) 0.60520(13) -0.1149(2) 0.0369(7) Uani 1 1 d . . . F13 F 0.3980(5) 0.4543(2) 0.4799(4) 0.1039(17) Uani 1 1 d . . . N14 N -0.2013(4) 0.53081(13) -0.2104(2) 0.0366(7) Uani 1 1 d . . . N15 N -0.3626(4) 0.52474(14) -0.1239(2) 0.0365(7) Uani 1 1 d . . . N16 N -0.0871(4) 0.65414(14) -0.0236(2) 0.0387(8) Uani 1 1 d . . . C17 C -0.2584(5) 0.49975(16) -0.2737(3) 0.0407(10) Uani 1 1 d . . . H17 H -0.3501 0.4962 -0.2953 0.049 Uiso 1 1 calc R . . N18 N -0.4911(5) 0.63774(19) -0.3298(3) 0.0575(11) Uani 1 1 d . . . C19 C -0.0143(4) 0.67355(15) 0.0503(3) 0.0377(9) Uani 1 1 d . . . C20 C -0.0922(5) 0.67848(18) -0.0949(3) 0.0470(10) Uani 1 1 d . . . H20 H -0.0527 0.7105 -0.1026 0.056 Uiso 1 1 calc R . . C21 C -0.0770(5) 0.68257(18) 0.1104(3) 0.0453(10) Uani 1 1 d . . . H21 H -0.1689 0.6770 0.1035 0.054 Uiso 1 1 calc R . . C22 C -0.1515(4) 0.60858(15) -0.0365(2) 0.0355(8) Uani 1 1 d . . . C23 C -0.4965(5) 0.52858(18) -0.1260(3) 0.0413(9) Uani 1 1 d . . . H23 H -0.5520 0.5565 -0.1473 0.050 Uiso 1 1 calc R . . C25 C -0.4053(5) 0.6004(2) -0.3045(3) 0.0460(10) Uani 1 1 d . . . H25 H -0.3620 0.5802 -0.3363 0.055 Uiso 1 1 calc R . . C26 C -0.4660(5) 0.63287(19) -0.2027(3) 0.0459(10) Uani 1 1 d . . . H26 H -0.4716 0.6393 -0.1502 0.055 Uiso 1 1 calc R . . C27 C 0.1719(5) 0.50427(19) -0.2767(3) 0.0463(11) Uani 1 1 d . . . H27 H 0.1549 0.5402 -0.2830 0.056 Uiso 1 1 calc R . . C28 C -0.3185(4) 0.47898(16) -0.0900(2) 0.0364(8) Uani 1 1 d . . . C29 C -0.4264(4) 0.40522(16) -0.0350(3) 0.0385(9) Uani 1 1 d . . . C32 C -0.0013(6) 0.70020(19) 0.1817(3) 0.0515(12) Uani 1 1 d . . . H32 H -0.0429 0.7063 0.2238 0.062 Uiso 1 1 calc R . . C33 C -0.5312(6) 0.3233(2) -0.0359(4) 0.0590(14) Uani 1 1 d . . . H33 H -0.5982 0.2999 -0.0599 0.071 Uiso 1 1 calc R . . C35 C -0.0703(4) 0.52322(16) -0.1936(2) 0.0358(8) Uani 1 1 d . . . C36 C -0.1628(5) 0.64846(17) -0.1504(3) 0.0451(10) Uani 1 1 d . . . H36 H -0.1824 0.6554 -0.2051 0.054 Uiso 1 1 calc R . . C37 C -0.1623(5) 0.47571(19) -0.2990(3) 0.0447(10) Uani 1 1 d . . . H37 H -0.1720 0.4533 -0.3427 0.054 Uiso 1 1 calc R . . C38 C 0.1054(5) 0.4190(2) -0.2466(3) 0.0456(10) Uani 1 1 d . . . H38 H 0.0424 0.3967 -0.2323 0.055 Uiso 1 1 calc R . . C39 C 0.1906(5) 0.7006(2) 0.1305(3) 0.0532(12) Uani 1 1 d . . . H39 H 0.2820 0.7071 0.1368 0.064 Uiso 1 1 calc R . . C40 C -0.5223(5) 0.3707(2) -0.0709(3) 0.0504(11) Uani 1 1 d . . . H40 H -0.5812 0.3794 -0.1188 0.061 Uiso 1 1 calc R . . C41 C 0.1307(5) 0.70891(19) 0.1927(3) 0.0492(11) Uani 1 1 d . . . C42 C 0.2227(5) 0.3997(2) -0.2582(3) 0.0489(11) Uani 1 1 d . . . H42 H 0.2403 0.3638 -0.2515 0.059 Uiso 1 1 calc R . . C44 C 0.2877(6) 0.4836(2) -0.2875(3) 0.0537(12) Uani 1 1 d . . . H44 H 0.3512 0.5060 -0.3012 0.064 Uiso 1 1 calc R . . C46 C -0.5338(5) 0.48608(19) -0.0929(3) 0.0427(9) Uani 1 1 d . . . H46 H -0.6198 0.4786 -0.0864 0.051 Uiso 1 1 calc R . . C47 C -0.6784(9) 0.6388(3) -0.4402(4) 0.082(2) Uani 1 1 d . . . H47A H -0.7311 0.6553 -0.4066 0.099 Uiso 1 1 calc R . . H47B H -0.6871 0.6010 -0.4354 0.099 Uiso 1 1 calc R . . C48 C -0.3398(5) 0.39275(18) 0.0343(3) 0.0424(9) Uani 1 1 d . . . H48 H -0.2755 0.4169 0.0592 0.051 Uiso 1 1 calc R . . C49 C -0.4446(6) 0.3093(2) 0.0331(3) 0.0547(12) Uani 1 1 d . . . C50 C -0.3476(5) 0.34461(19) 0.0671(3) 0.0482(10) Uani 1 1 d . . . H50 H -0.2856 0.3355 0.1136 0.058 Uiso 1 1 calc R . . C51 C 0.1174(5) 0.68299(19) 0.0593(3) 0.0480(11) Uani 1 1 d . . . H51 H 0.1585 0.6774 0.0169 0.058 Uiso 1 1 calc R . . C53 C -0.4545(10) 0.2576(3) 0.0706(5) 0.087(2) Uani 1 1 d . . . H53A H -0.5385 0.2553 0.0866 0.130 Uiso 1 1 calc R . . H53B H -0.3818 0.2537 0.1166 0.130 Uiso 1 1 calc R . . H53C H -0.4498 0.2301 0.0329 0.130 Uiso 1 1 calc R . . C54 C 0.0806(5) 0.47133(18) -0.2562(3) 0.0411(9) Uani 1 1 d . . . B55 B -0.2849(5) 0.56275(19) -0.1661(3) 0.0370(9) Uani 1 1 d . . . C56 C -0.5400(7) 0.6531(3) -0.4120(3) 0.0723(19) Uani 1 1 d . . . H56A H -0.5305 0.6909 -0.4168 0.087 Uiso 1 1 calc R . . H56B H -0.4864 0.6362 -0.4448 0.087 Uiso 1 1 calc R . . C57 C 0.3153(5) 0.4316(2) -0.2794(3) 0.0516(11) Uani 1 1 d . . . C58 C 0.4453(6) 0.4100(3) -0.2911(4) 0.0650(15) Uani 1 1 d . . . H58A H 0.5172 0.4219 -0.2486 0.097 Uiso 1 1 calc R . . H58B H 0.4605 0.4219 -0.3414 0.097 Uiso 1 1 calc R . . H58C H 0.4420 0.3722 -0.2907 0.097 Uiso 1 1 calc R . . C59 C -0.5328(6) 0.6589(2) -0.2669(3) 0.0538(12) Uani 1 1 d . . . H59 H -0.5949 0.6859 -0.2683 0.065 Uiso 1 1 calc R . . C60 C 0.2130(8) 0.7257(3) 0.2719(4) 0.0728(18) Uani 1 1 d . . . H60A H 0.1547 0.7347 0.3066 0.109 Uiso 1 1 calc R . . H60B H 0.2661 0.7558 0.2650 0.109 Uiso 1 1 calc R . . H60C H 0.2711 0.6974 0.2951 0.109 Uiso 1 1 calc R . . C62 C -0.7343(10) 0.6546(4) -0.5258(5) 0.100(3) Uani 1 1 d . . . H62A H -0.7349 0.6927 -0.5297 0.119 Uiso 1 1 calc R . . H62B H -0.6764 0.6411 -0.5588 0.119 Uiso 1 1 calc R . . C64 C -0.8740(12) 0.6343(4) -0.5566(6) 0.112(4) Uani 1 1 d . . . H64A H -0.8738 0.5966 -0.5531 0.168 Uiso 1 1 calc R . . H64B H -0.9055 0.6447 -0.6114 0.168 Uiso 1 1 calc R . . H64C H -0.9323 0.6485 -0.5252 0.168 Uiso 1 1 calc R . . P2 P 0.3955(2) 0.22950(8) 0.77339(13) 0.0361(5) Uani 1 1 d P . . F2 F 0.4428(7) 0.2861(2) 0.7912(3) 0.113(2) Uani 1 1 d . . . F1 F 0.4028(12) 0.2181(2) 0.8619(4) 0.182(5) Uani 1 1 d . . . F3 F 0.3515(6) 0.1707(2) 0.7577(4) 0.126(2) Uani 1 1 d . . . F6 F 0.3946(7) 0.2393(3) 0.6838(4) 0.130(2) Uani 1 1 d . . . F5 F 0.5403(7) 0.2108(3) 0.7816(6) 0.146(3) Uani 1 1 d . . . F4 F 0.2538(6) 0.2466(3) 0.7582(7) 0.175(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0351(2) 0.0291(2) 0.0225(2) 0.00054(13) -0.00485(16) -0.00111(14) S2 0.0370(5) 0.0314(5) 0.0295(5) -0.0012(3) -0.0042(4) -0.0023(3) S3 0.0392(5) 0.0307(5) 0.0263(5) -0.0003(3) -0.0020(4) -0.0004(3) P4 0.0573(10) 0.0500(10) 0.0289(8) -0.0030(6) -0.0014(7) 0.0007(7) S5 0.0403(5) 0.0378(5) 0.0250(5) 0.0015(3) -0.0042(4) -0.0047(4) F7 0.104(3) 0.080(2) 0.0421(18) -0.0022(17) 0.0203(19) 0.015(2) N8 0.0374(17) 0.0336(17) 0.0337(18) -0.0020(13) -0.0029(14) -0.0026(13) N9 0.046(2) 0.0390(18) 0.0278(18) -0.0027(14) -0.0050(15) 0.0026(15) N10 0.050(2) 0.0364(18) 0.0292(18) 0.0014(14) -0.0044(15) 0.0051(15) F11 0.124(4) 0.111(3) 0.046(2) -0.013(2) -0.018(2) 0.061(3) N12 0.0447(18) 0.0323(16) 0.0277(17) 0.0019(13) -0.0040(14) 0.0009(14) F13 0.105(3) 0.096(3) 0.118(4) -0.042(3) 0.041(3) -0.044(3) N14 0.0407(18) 0.0333(16) 0.0303(17) 0.0001(13) -0.0035(14) 0.0013(13) N15 0.0391(18) 0.0351(17) 0.0287(17) -0.0019(13) -0.0063(14) 0.0010(13) N16 0.050(2) 0.0304(16) 0.0309(18) 0.0004(13) -0.0005(15) -0.0035(14) C17 0.042(2) 0.040(2) 0.032(2) -0.0057(15) -0.0077(18) -0.0028(16) N18 0.073(3) 0.060(3) 0.033(2) 0.0089(18) -0.0026(19) 0.023(2) C19 0.046(2) 0.0267(18) 0.037(2) -0.0033(15) 0.0010(17) -0.0020(15) C20 0.064(3) 0.034(2) 0.039(2) 0.0054(17) 0.002(2) -0.0031(19) C21 0.050(2) 0.041(2) 0.043(3) -0.0084(18) 0.006(2) -0.0069(18) C22 0.041(2) 0.0315(19) 0.031(2) -0.0004(15) 0.0008(16) -0.0011(15) C23 0.043(2) 0.040(2) 0.035(2) -0.0002(17) -0.0028(18) 0.0027(17) C25 0.053(3) 0.053(3) 0.027(2) 0.0033(18) -0.0023(18) 0.015(2) C26 0.054(3) 0.046(2) 0.034(2) 0.0020(18) 0.0010(19) 0.006(2) C27 0.054(3) 0.045(2) 0.036(2) 0.0026(17) 0.000(2) 0.0001(19) C28 0.041(2) 0.033(2) 0.0288(19) -0.0040(15) -0.0051(16) -0.0007(16) C29 0.044(2) 0.034(2) 0.035(2) -0.0040(16) 0.0045(17) -0.0033(16) C32 0.074(3) 0.041(2) 0.038(2) -0.0111(19) 0.010(2) -0.011(2) C33 0.075(4) 0.045(3) 0.055(3) -0.009(2) 0.009(3) -0.023(2) C35 0.044(2) 0.034(2) 0.0254(18) 0.0003(14) -0.0014(16) -0.0015(16) C36 0.064(3) 0.035(2) 0.031(2) 0.0081(16) 0.0000(19) -0.0020(19) C37 0.048(2) 0.046(2) 0.033(2) -0.0067(17) -0.0067(18) -0.0017(19) C38 0.047(2) 0.048(3) 0.038(2) 0.0000(19) 0.0022(19) 0.0006(19) C39 0.049(3) 0.049(3) 0.057(3) -0.013(2) 0.002(2) -0.008(2) C40 0.057(3) 0.047(3) 0.041(3) -0.004(2) -0.002(2) -0.012(2) C41 0.061(3) 0.037(2) 0.044(3) -0.0087(19) 0.000(2) -0.008(2) C42 0.053(3) 0.043(2) 0.045(3) 0.0024(19) 0.000(2) 0.005(2) C44 0.055(3) 0.060(3) 0.046(3) 0.005(2) 0.010(2) -0.004(2) C46 0.039(2) 0.048(2) 0.038(2) 0.0003(19) 0.0015(18) 0.0010(18) C47 0.102(5) 0.086(5) 0.049(4) 0.004(3) -0.004(3) 0.038(4) C48 0.044(2) 0.041(2) 0.039(2) 0.0004(17) 0.0021(18) -0.0034(17) C49 0.073(3) 0.039(2) 0.055(3) 0.000(2) 0.021(3) -0.006(2) C50 0.054(3) 0.043(2) 0.046(3) 0.0050(19) 0.009(2) 0.004(2) C51 0.049(2) 0.044(2) 0.049(3) -0.014(2) 0.007(2) -0.0066(19) C53 0.127(7) 0.049(3) 0.082(5) 0.007(3) 0.020(5) -0.020(4) C54 0.044(2) 0.045(2) 0.028(2) -0.0010(16) -0.0035(17) 0.0031(18) B55 0.042(2) 0.038(2) 0.025(2) 0.0013(17) -0.0047(18) 0.0016(18) C56 0.088(4) 0.082(4) 0.037(3) 0.013(3) -0.007(3) 0.039(4) C57 0.050(3) 0.060(3) 0.041(3) 0.003(2) 0.002(2) 0.000(2) C58 0.055(3) 0.073(4) 0.068(4) 0.012(3) 0.017(3) 0.009(3) C59 0.066(3) 0.051(3) 0.040(3) 0.005(2) 0.001(2) 0.022(2) C60 0.097(5) 0.064(4) 0.049(3) -0.014(3) -0.003(3) -0.021(3) C62 0.125(7) 0.098(6) 0.054(4) -0.008(4) -0.026(4) 0.043(5) C64 0.149(9) 0.086(6) 0.074(5) -0.016(4) -0.031(5) 0.042(6) P2 0.0352(9) 0.0345(10) 0.0394(11) -0.0271(8) 0.0102(8) -0.0169(8) F2 0.181(6) 0.075(3) 0.083(3) -0.025(2) 0.027(3) -0.049(3) F1 0.386(14) 0.083(4) 0.099(4) -0.025(3) 0.098(7) -0.066(6) F3 0.125(4) 0.091(4) 0.154(6) -0.064(4) 0.017(4) -0.038(3) F6 0.154(6) 0.149(6) 0.089(4) -0.044(4) 0.035(4) -0.040(4) F5 0.111(5) 0.131(5) 0.197(8) -0.001(5) 0.036(5) -0.024(4) F4 0.091(4) 0.133(6) 0.321(14) 0.033(7) 0.089(7) 0.006(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S2 2.3460(9) 3_565 ? Ru1 S2 2.3460(9) . ? Ru1 S3 2.4191(10) 3_565 ? Ru1 S3 2.4191(10) . ? Ru1 S5 2.4539(10) . ? Ru1 S5 2.4539(10) 3_565 ? S2 C28 1.726(4) . ? S3 C22 1.720(4) . ? P4 F13 1.578(4) 3_666 ? P4 F13 1.578(4) . ? P4 F11 1.583(4) 3_666 ? P4 F11 1.583(4) . ? P4 F7 1.600(3) 3_666 ? P4 F7 1.600(3) . ? S5 C35 1.719(4) . ? N8 C28 1.367(6) . ? N8 C46 1.379(6) . ? N8 C29 1.443(6) . ? N9 C35 1.351(6) . ? N9 C37 1.393(6) . ? N9 C54 1.437(6) . ? N10 C25 1.348(6) . ? N10 C26 1.373(6) . ? N10 B55 1.587(6) . ? N12 C22 1.360(6) . ? N12 C36 1.393(6) . ? N12 B55 1.549(6) . ? N14 C35 1.346(6) . ? N14 C17 1.392(6) . ? N14 B55 1.534(6) . ? N15 C28 1.360(6) . ? N15 C23 1.392(6) . ? N15 B55 1.564(6) . ? N16 C22 1.353(5) . ? N16 C20 1.391(6) . ? N16 C19 1.436(6) . ? C17 C37 1.338(7) . ? N18 C25 1.325(6) . ? N18 C59 1.386(7) . ? N18 C56 1.471(7) . ? C19 C51 1.369(7) . ? C19 C21 1.378(7) . ? C20 C36 1.332(7) . ? C21 C32 1.397(7) . ? C23 C46 1.343(7) . ? C26 C59 1.362(7) . ? C27 C44 1.373(8) . ? C27 C54 1.385(7) . ? C29 C48 1.378(7) . ? C29 C40 1.383(6) . ? C32 C41 1.364(8) . ? C33 C40 1.385(8) . ? C33 C49 1.386(9) . ? C38 C42 1.378(7) . ? C38 C54 1.385(7) . ? C39 C51 1.386(7) . ? C39 C41 1.390(8) . ? C41 C60 1.523(8) . ? C42 C57 1.385(8) . ? C44 C57 1.379(8) . ? C47 C56 1.465(12) . ? C47 C62 1.538(10) . ? C48 C50 1.384(7) . ? C49 C50 1.395(8) . ? C49 C53 1.507(8) . ? C57 C58 1.524(8) . ? C62 C64 1.529(15) . ? P2 F4 1.508(7) . ? P2 F5 1.562(8) . ? P2 F2 1.557(5) . ? P2 F1 1.565(7) . ? P2 F6 1.588(7) . ? P2 F3 1.598(5) . ? 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 S2 Ru1 S2 180.0 3_565 . ? S2 Ru1 S3 93.87(3) 3_565 3_565 ? S2 Ru1 S3 86.13(3) . 3_565 ? S2 Ru1 S3 86.13(3) 3_565 . ? S2 Ru1 S3 93.87(3) . . ? S3 Ru1 S3 180.0 3_565 . ? S2 Ru1 S5 87.22(3) 3_565 . ? S2 Ru1 S5 92.78(3) . . ? S3 Ru1 S5 81.68(3) 3_565 . ? S3 Ru1 S5 98.32(3) . . ? S2 Ru1 S5 92.78(3) 3_565 3_565 ? S2 Ru1 S5 87.22(3) . 3_565 ? S3 Ru1 S5 98.32(3) 3_565 3_565 ? S3 Ru1 S5 81.68(3) . 3_565 ? S5 Ru1 S5 180.00(5) . 3_565 ? C28 S2 Ru1 111.57(14) . . ? C22 S3 Ru1 100.85(15) . . ? F13 P4 F13 180.000(1) 3_666 . ? F13 P4 F11 89.6(4) 3_666 3_666 ? F13 P4 F11 90.4(4) . 3_666 ? F13 P4 F11 90.4(4) 3_666 . ? F13 P4 F11 89.6(4) . . ? F11 P4 F11 180.000(2) 3_666 . ? F13 P4 F7 91.8(3) 3_666 3_666 ? F13 P4 F7 88.2(2) . 3_666 ? F11 P4 F7 90.4(2) 3_666 3_666 ? F11 P4 F7 89.6(2) . 3_666 ? F13 P4 F7 88.2(2) 3_666 . ? F13 P4 F7 91.8(3) . . ? F11 P4 F7 89.6(2) 3_666 . ? F11 P4 F7 90.4(2) . . ? F7 P4 F7 180.000(2) 3_666 . ? C35 S5 Ru1 105.99(14) . . ? C28 N8 C46 109.4(4) . . ? C28 N8 C29 127.3(4) . . ? C46 N8 C29 123.3(4) . . ? C35 N9 C37 110.0(4) . . ? C35 N9 C54 127.8(4) . . ? C37 N9 C54 122.2(4) . . ? C25 N10 C26 107.3(4) . . ? C25 N10 B55 129.4(4) . . ? C26 N10 B55 122.4(4) . . ? C22 N12 C36 108.1(4) . . ? C22 N12 B55 132.2(4) . . ? C36 N12 B55 119.7(4) . . ? C35 N14 C17 108.7(4) . . ? C35 N14 B55 129.3(4) . . ? C17 N14 B55 121.7(4) . . ? C28 N15 C23 108.2(4) . . ? C28 N15 B55 126.6(4) . . ? C23 N15 B55 124.5(4) . . ? C22 N16 C20 109.1(4) . . ? C22 N16 C19 126.8(4) . . ? C20 N16 C19 123.9(4) . . ? C37 C17 N14 108.4(4) . . ? C25 N18 C59 109.4(4) . . ? C25 N18 C56 125.8(5) . . ? C59 N18 C56 124.8(5) . . ? C51 C19 C21 121.1(4) . . ? C51 C19 N16 118.7(4) . . ? C21 C19 N16 120.2(4) . . ? C36 C20 N16 107.2(4) . . ? C19 C21 C32 118.0(5) . . ? N16 C22 N12 107.1(4) . . ? N16 C22 S3 125.1(3) . . ? N12 C22 S3 127.5(3) . . ? C46 C23 N15 108.4(4) . . ? N18 C25 N10 109.0(4) . . ? C59 C26 N10 108.7(4) . . ? C44 C27 C54 118.3(5) . . ? N15 C28 N8 106.8(4) . . ? N15 C28 S2 130.8(3) . . ? N8 C28 S2 122.3(3) . . ? C48 C29 C40 120.8(4) . . ? C48 C29 N8 121.2(4) . . ? C40 C29 N8 117.9(4) . . ? C41 C32 C21 122.0(5) . . ? C40 C33 C49 121.6(5) . . ? N14 C35 N9 106.7(4) . . ? N14 C35 S5 128.9(3) . . ? N9 C35 S5 124.1(3) . . ? C20 C36 N12 108.4(4) . . ? C17 C37 N9 106.1(4) . . ? C42 C38 C54 119.0(5) . . ? C51 C39 C41 120.2(5) . . ? C33 C40 C29 119.0(5) . . ? C32 C41 C39 118.7(5) . . ? C32 C41 C60 121.3(5) . . ? C39 C41 C60 119.9(5) . . ? C38 C42 C57 121.2(5) . . ? C27 C44 C57 122.4(5) . . ? C23 C46 N8 107.2(4) . . ? C56 C47 C62 113.0(8) . . ? C29 C48 C50 119.3(4) . . ? C33 C49 C50 117.9(5) . . ? C33 C49 C53 121.3(6) . . ? C50 C49 C53 120.8(6) . . ? C48 C50 C49 121.3(5) . . ? C19 C51 C39 119.9(5) . . ? C27 C54 C38 121.0(5) . . ? C27 C54 N9 120.8(4) . . ? C38 C54 N9 118.2(4) . . ? N14 B55 N12 112.0(4) . . ? N14 B55 N15 108.3(3) . . ? N12 B55 N15 116.8(4) . . ? N14 B55 N10 109.7(3) . . ? N12 B55 N10 102.0(3) . . ? N15 B55 N10 107.7(4) . . ? C47 C56 N18 111.1(6) . . ? C44 C57 C42 118.1(5) . . ? C44 C57 C58 121.1(5) . . ? C42 C57 C58 120.7(5) . . ? C26 C59 N18 105.6(4) . . ? C64 C62 C47 112.0(9) . . ? F4 P2 F5 175.2(6) . . ? F4 P2 F2 90.7(4) . . ? F5 P2 F2 91.1(4) . . ? F4 P2 F1 93.3(6) . . ? F5 P2 F1 91.1(6) . . ? F2 P2 F1 92.1(3) . . ? F4 P2 F6 89.5(5) . . ? F5 P2 F6 86.1(4) . . ? F2 P2 F6 88.8(3) . . ? F1 P2 F6 177.1(6) . . ? F4 P2 F3 91.0(4) . . ? F5 P2 F3 87.3(4) . . ? F2 P2 F3 177.8(4) . . ? F1 P2 F3 86.5(4) . . ? F6 P2 F3 92.6(4) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 75.16 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.823 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.131 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.087 0.397 0.317 12 7 ' ' 2 0.413 0.897 0.183 12 7 ' ' 3 0.587 0.103 0.817 12 7 ' ' 4 0.913 0.603 0.683 12 7 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 936861' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pb2005-sr _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H56 B2 F18 N18 P3 Rh S6' _chemical_formula_weight 1564.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1' _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7354(3) _cell_length_b 9.9613(3) _cell_length_c 16.6355(7) _cell_angle_alpha 99.986(3) _cell_angle_beta 91.995(3) _cell_angle_gamma 90.774(3) _cell_volume 1587.55(10) _cell_formula_units_Z 1 _cell_measurement_temperature 120.00(10) _cell_measurement_reflns_used 18977 _cell_measurement_theta_min 4.5042 _cell_measurement_theta_max 73.7583 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3363 _exptl_crystal_size_mid 0.1325 _exptl_crystal_size_min 0.0883 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 5.652 _exptl_absorpt_correction_T_min 0.139 _exptl_absorpt_correction_T_max 0.601 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.00(10) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6297 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0188 _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 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.51 _diffrn_reflns_theta_max 73.92 _reflns_number_total 6297 _reflns_number_gt 6197 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. #=========================================================================== The following ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-level. #============================================================================ PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of P2 Some rotational motion is common in PF6, the central atom thus usually has lower ADPs. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Rh01 -- S001 .. 7.0 su PLAT230_ALERT_2_C Hirshfeld Test Diff for S002 -- C12 .. 5.4 su Common for atom pair with large difference in mass. PLAT605_ALERT_4_G Structure Contains Solvent Accessible VOIDS of . 104 A**3 PLAT869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed ! Platon SQUEEZE was used to remove 26 e/A***3, equivalent to one molecule of EtOH. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.976 PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT154_ALERT_1_G The su's on the Cell Angles are Equal ..........0.00300 Deg. PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 5 No Action Taken ; _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^)+(0.0426P)^2^+1.2688P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6297 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Rh01 Rh 0.0000 0.0000 0.0000 0.01260(6) Uani 1 2 d S . . S002 S -0.20089(4) 0.12464(4) 0.04084(3) 0.01530(10) Uani 1 1 d . . . S003 S 0.16345(4) 0.18555(4) 0.03496(3) 0.01551(10) Uani 1 1 d . . . P1 P 0.49853(5) 0.48884(5) 0.20030(3) 0.02251(12) Uani 1 1 d . . . S001 S 0.02330(4) -0.07996(4) 0.12611(3) 0.01570(10) Uani 1 1 d . . . P2 P 0.5000 0.0000 0.5000 0.0716(4) Uani 1 2 d S . . N007 N 0.0460(2) 0.9153(2) 0.35319(12) 0.0344(4) Uani 1 1 d . . . F12 F 0.45711(14) 0.40155(14) 0.11311(8) 0.0353(3) Uani 1 1 d . . . F16 F 0.45317(13) 0.62588(13) 0.16961(8) 0.0304(3) Uani 1 1 d . . . F14 F 0.34590(14) 0.46735(15) 0.22969(10) 0.0399(3) Uani 1 1 d . . . N3 N 0.14204(16) 0.20287(16) 0.20336(9) 0.0150(3) Uani 1 1 d . . . F15 F 0.54588(14) 0.35277(14) 0.23214(9) 0.0352(3) Uani 1 1 d . . . F11 F 0.65128(13) 0.50945(13) 0.17106(9) 0.0321(3) Uani 1 1 d . . . F13 F 0.54043(15) 0.57679(14) 0.28813(8) 0.0365(3) Uani 1 1 d . . . N8 N -0.19667(16) -0.06384(16) 0.22116(10) 0.0177(3) Uani 1 1 d . . . N7 N -0.10064(15) 0.13792(16) 0.22759(9) 0.0152(3) Uani 1 1 d . . . N4 N 0.33568(16) 0.12312(17) 0.15487(10) 0.0189(3) Uani 1 1 d . . . C10 C 0.3376(2) 0.1118(2) 0.23611(12) 0.0211(4) Uani 1 1 d . . . H10 H 0.4091 0.0786 0.2651 0.025 Uiso 1 1 calc R . . N1 N -0.00753(16) 0.37669(16) 0.29121(9) 0.0163(3) Uani 1 1 d . . . N5 N -0.05312(15) 0.33037(16) 0.14330(9) 0.0150(3) Uani 1 1 d . . . F22 F 0.4257(3) 0.0590(4) 0.42697(15) 0.1091(10) Uani 1 1 d . . . C17 C -0.2284(2) -0.2096(2) 0.19923(14) 0.0262(4) Uani 1 1 d . . . H17A H -0.2434 -0.2333 0.1411 0.039 Uiso 1 1 calc R . . H17B H -0.3097 -0.2309 0.2259 0.039 Uiso 1 1 calc R . . H17C H -0.1528 -0.2603 0.2163 0.039 Uiso 1 1 calc R . . N6 N -0.15996(16) 0.39404(16) 0.03910(10) 0.0171(3) Uani 1 1 d . . . C13 C -0.2558(2) 0.3946(2) -0.03044(13) 0.0240(4) Uani 1 1 d . . . H13A H -0.2392 0.3177 -0.0721 0.036 Uiso 1 1 calc R . . H13B H -0.2428 0.4772 -0.0519 0.036 Uiso 1 1 calc R . . H13C H -0.3484 0.3895 -0.0130 0.036 Uiso 1 1 calc R . . C7 C -0.1660(3) 0.7958(2) 0.48201(15) 0.0359(5) Uani 1 1 d . . . H7A H -0.1882 0.8254 0.4312 0.054 Uiso 1 1 calc R . . H7B H -0.1529 0.8739 0.5245 0.054 Uiso 1 1 calc R . . H7C H -0.2398 0.7396 0.4953 0.054 Uiso 1 1 calc R . . N2 N -0.0398(2) 0.71760(18) 0.47440(11) 0.0262(4) Uani 1 1 d . . . C5 C -0.0289(2) 0.6089(2) 0.41584(12) 0.0219(4) Uani 1 1 d . . . C12 C -0.13822(18) 0.28684(19) 0.07726(11) 0.0155(3) Uani 1 1 d . . . C15 C -0.0170(2) 0.46602(19) 0.14217(12) 0.0181(4) Uani 1 1 d . . . H15 H 0.0437 0.5199 0.1790 0.022 Uiso 1 1 calc R . . C1 C 0.1023(2) 0.4274(2) 0.34060(12) 0.0192(4) Uani 1 1 d . . . H1 H 0.1864 0.3849 0.3323 0.023 Uiso 1 1 calc R . . C3 C 0.0953(2) 0.5377(2) 0.40180(12) 0.0222(4) Uani 1 1 d . . . H3 H 0.1731 0.5664 0.4347 0.027 Uiso 1 1 calc R . . C16 C -0.09419(18) 0.00344(19) 0.19204(11) 0.0159(4) Uani 1 1 d . . . C18 C -0.26897(19) 0.0250(2) 0.27580(12) 0.0199(4) Uani 1 1 d . . . H18 H -0.3435 0.0032 0.3049 0.024 Uiso 1 1 calc R . . C11 C 0.21719(19) 0.1576(2) 0.26582(12) 0.0185(4) Uani 1 1 d . . . H11 H 0.1890 0.1588 0.3188 0.022 Uiso 1 1 calc R . . F21 F 0.5324(2) -0.1353(3) 0.43861(17) 0.1126(11) Uani 1 1 d . . . C4 C -0.1418(2) 0.5588(2) 0.36203(12) 0.0215(4) Uani 1 1 d . . . H4 H -0.2260 0.6019 0.3674 0.026 Uiso 1 1 calc R . . C9 C 0.4480(2) 0.0810(2) 0.10052(13) 0.0245(4) Uani 1 1 d . . . H9A H 0.4436 -0.0161 0.0833 0.037 Uiso 1 1 calc R . . H9B H 0.5344 0.1067 0.1290 0.037 Uiso 1 1 calc R . . H9C H 0.4398 0.1248 0.0536 0.037 Uiso 1 1 calc R . . C20 C 0.1387(2) 0.8596(2) 0.32557(14) 0.0286(5) Uani 1 1 d . . . C14 C -0.0846(2) 0.50549(19) 0.07891(12) 0.0195(4) Uani 1 1 d . . . H14 H -0.0813 0.5917 0.0646 0.023 Uiso 1 1 calc R . . C2 C -0.12695(19) 0.4480(2) 0.30262(12) 0.0188(4) Uani 1 1 d . . . H2 H -0.2022 0.4189 0.2677 0.023 Uiso 1 1 calc R . . C6 C 0.0792(3) 0.7703(2) 0.52669(14) 0.0349(5) Uani 1 1 d . . . H6A H 0.1177 0.6984 0.5514 0.052 Uiso 1 1 calc R . . H6B H 0.0512 0.8425 0.5685 0.052 Uiso 1 1 calc R . . H6C H 0.1470 0.8046 0.4945 0.052 Uiso 1 1 calc R . . B1 B -0.0041(2) 0.2577(2) 0.21385(12) 0.0151(4) Uani 1 1 d . . . C8 C 0.21527(18) 0.17527(19) 0.13433(11) 0.0159(4) Uani 1 1 d . . . F23 F 0.3598(3) -0.0607(4) 0.5193(2) 0.1194(11) Uani 1 1 d . . . C19 C -0.21165(19) 0.1492(2) 0.27917(12) 0.0182(4) Uani 1 1 d . . . H19 H -0.2409 0.2294 0.3106 0.022 Uiso 1 1 calc R . . C21 C 0.2579(3) 0.7889(3) 0.29000(18) 0.0405(6) Uani 1 1 d . . . H21A H 0.2747 0.8160 0.2385 0.061 Uiso 1 1 calc R . . H21B H 0.2408 0.6923 0.2818 0.061 Uiso 1 1 calc R . . H21C H 0.3368 0.8120 0.3262 0.061 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 Rh01 0.01296(10) 0.01009(10) 0.01432(10) 0.00103(7) 0.00020(6) -0.00037(7) S002 0.0135(2) 0.0129(2) 0.0184(2) -0.00012(16) -0.00057(15) 0.00063(15) S003 0.0164(2) 0.0129(2) 0.0167(2) 0.00142(16) 0.00078(15) -0.00265(16) P1 0.0183(2) 0.0188(3) 0.0301(3) 0.0043(2) -0.00211(19) -0.00195(18) S001 0.0182(2) 0.0123(2) 0.0165(2) 0.00228(16) 0.00112(15) 0.00145(16) P2 0.0310(5) 0.1185(12) 0.0523(7) -0.0208(7) 0.0002(5) 0.0034(6) N007 0.0393(11) 0.0339(11) 0.0317(10) 0.0100(9) 0.0036(8) 0.0029(9) F12 0.0400(7) 0.0262(7) 0.0366(7) -0.0011(6) -0.0097(6) -0.0005(6) F16 0.0286(6) 0.0228(6) 0.0402(7) 0.0074(5) -0.0042(5) 0.0028(5) F14 0.0237(7) 0.0359(8) 0.0609(9) 0.0094(7) 0.0093(6) -0.0054(6) N3 0.0161(7) 0.0125(7) 0.0156(7) 0.0007(6) -0.0002(6) -0.0006(6) F15 0.0356(7) 0.0239(7) 0.0481(8) 0.0134(6) -0.0071(6) -0.0020(5) F11 0.0213(6) 0.0285(7) 0.0472(8) 0.0085(6) 0.0043(5) -0.0001(5) F13 0.0434(8) 0.0331(7) 0.0310(7) 0.0013(6) -0.0054(6) -0.0045(6) N8 0.0187(8) 0.0141(8) 0.0204(8) 0.0028(6) 0.0016(6) -0.0014(6) N7 0.0155(7) 0.0146(8) 0.0152(7) 0.0018(6) 0.0002(6) 0.0005(6) N4 0.0150(7) 0.0182(8) 0.0227(8) 0.0018(6) 0.0003(6) 0.0000(6) C10 0.0185(9) 0.0191(10) 0.0254(10) 0.0041(8) -0.0040(7) 0.0010(7) N1 0.0173(7) 0.0141(8) 0.0166(7) 0.0005(6) -0.0003(6) -0.0003(6) N5 0.0170(7) 0.0114(7) 0.0160(7) 0.0001(6) 0.0011(6) -0.0001(6) F22 0.104(2) 0.152(3) 0.0606(14) -0.0077(16) -0.0131(13) 0.0201(19) C17 0.0271(10) 0.0156(10) 0.0357(12) 0.0035(8) 0.0066(8) -0.0057(8) N6 0.0187(7) 0.0150(8) 0.0176(7) 0.0032(6) -0.0001(6) 0.0023(6) C13 0.0248(10) 0.0241(11) 0.0243(10) 0.0084(8) -0.0056(8) 0.0035(8) C7 0.0441(14) 0.0256(12) 0.0335(12) -0.0088(10) 0.0074(10) 0.0038(10) N2 0.0405(10) 0.0174(9) 0.0189(8) -0.0016(7) 0.0016(7) -0.0003(7) C5 0.0330(11) 0.0157(10) 0.0169(9) 0.0028(7) 0.0026(8) -0.0021(8) C12 0.0128(8) 0.0168(9) 0.0165(8) 0.0016(7) 0.0016(6) 0.0026(7) C15 0.0221(9) 0.0117(9) 0.0195(9) 0.0000(7) 0.0027(7) -0.0019(7) C1 0.0207(9) 0.0163(9) 0.0199(9) 0.0022(7) -0.0016(7) -0.0016(7) C3 0.0265(10) 0.0187(10) 0.0201(9) 0.0017(8) -0.0051(8) -0.0038(8) C16 0.0166(8) 0.0144(9) 0.0168(8) 0.0039(7) -0.0022(7) 0.0000(7) C18 0.0165(9) 0.0206(10) 0.0230(9) 0.0041(8) 0.0033(7) 0.0000(7) C11 0.0206(9) 0.0166(9) 0.0185(9) 0.0042(7) -0.0026(7) -0.0003(7) F21 0.0629(14) 0.159(3) 0.0878(17) -0.0559(18) -0.0193(12) 0.0266(16) C4 0.0244(10) 0.0176(10) 0.0221(9) 0.0017(8) 0.0041(7) 0.0022(7) C9 0.0161(9) 0.0269(11) 0.0289(10) -0.0007(8) 0.0042(8) 0.0036(8) C20 0.0361(12) 0.0223(11) 0.0283(11) 0.0074(9) -0.0011(9) -0.0017(9) C14 0.0242(9) 0.0112(9) 0.0231(9) 0.0026(7) 0.0031(7) 0.0005(7) C2 0.0181(9) 0.0170(9) 0.0212(9) 0.0028(7) -0.0003(7) 0.0004(7) C6 0.0543(15) 0.0241(12) 0.0227(11) -0.0041(9) -0.0076(10) -0.0045(10) B1 0.0160(9) 0.0137(10) 0.0151(9) 0.0012(8) 0.0007(7) -0.0004(7) C8 0.0146(8) 0.0118(9) 0.0204(9) 0.0010(7) -0.0006(7) -0.0027(6) F23 0.0492(13) 0.149(3) 0.152(3) 0.002(2) 0.0232(15) -0.0055(15) C19 0.0160(8) 0.0187(10) 0.0193(9) 0.0017(7) 0.0014(7) 0.0006(7) C21 0.0419(14) 0.0287(13) 0.0516(16) 0.0073(11) 0.0086(11) 0.0059(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Rh01 S001 2.3746(4) 2 ? Rh01 S001 2.3746(4) . ? Rh01 S002 2.3862(4) 2 ? Rh01 S002 2.3862(4) . ? Rh01 S003 2.4021(4) 2 ? Rh01 S003 2.4021(4) . ? S002 C12 1.7199(19) . ? S003 C8 1.7320(19) . ? P1 F12 1.5920(14) . ? P1 F16 1.6004(13) . ? P1 F11 1.6021(13) . ? P1 F14 1.6035(14) . ? P1 F13 1.6044(14) . ? P1 F15 1.6060(14) . ? S001 C16 1.7316(19) . ? P2 F23 1.551(3) . ? P2 F23 1.551(3) 2_656 ? P2 F21 1.586(3) 2_656 ? P2 F21 1.586(3) . ? P2 F22 1.594(3) . ? P2 F22 1.594(3) 2_656 ? N007 C20 1.135(3) . ? N3 C8 1.362(2) . ? N3 C11 1.392(2) . ? N3 B1 1.535(2) . ? N8 C16 1.344(2) . ? N8 C18 1.374(3) . ? N8 C17 1.460(3) . ? N7 C16 1.370(2) . ? N7 C19 1.397(2) . ? N7 B1 1.562(3) . ? N4 C8 1.346(2) . ? N4 C10 1.375(3) . ? N4 C9 1.463(2) . ? C10 C11 1.343(3) . ? N1 C1 1.362(2) . ? N1 C2 1.372(2) . ? N1 B1 1.593(2) . ? N5 C12 1.358(2) . ? N5 C15 1.395(2) . ? N5 B1 1.547(2) . ? N6 C12 1.349(2) . ? N6 C14 1.378(3) . ? N6 C13 1.462(2) . ? C7 N2 1.461(3) . ? N2 C5 1.333(3) . ? N2 C6 1.459(3) . ? C5 C3 1.416(3) . ? C5 C4 1.421(3) . ? C15 C14 1.341(3) . ? C1 C3 1.366(3) . ? C18 C19 1.342(3) . ? C4 C2 1.361(3) . ? C20 C21 1.455(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 S001 Rh01 S001 180.00(3) 2 . ? S001 Rh01 S002 92.554(15) 2 2 ? S001 Rh01 S002 87.446(15) . 2 ? S001 Rh01 S002 87.446(15) 2 . ? S001 Rh01 S002 92.554(15) . . ? S002 Rh01 S002 180.000(11) 2 . ? S001 Rh01 S003 95.963(15) 2 2 ? S001 Rh01 S003 84.037(15) . 2 ? S002 Rh01 S003 97.428(15) 2 2 ? S002 Rh01 S003 82.572(15) . 2 ? S001 Rh01 S003 84.038(15) 2 . ? S001 Rh01 S003 95.962(15) . . ? S002 Rh01 S003 82.572(15) 2 . ? S002 Rh01 S003 97.428(15) . . ? S003 Rh01 S003 180.000(14) 2 . ? C12 S002 Rh01 103.57(6) . . ? C8 S003 Rh01 103.10(6) . . ? F12 P1 F16 90.66(7) . . ? F12 P1 F11 90.17(8) . . ? F16 P1 F11 90.05(7) . . ? F12 P1 F14 89.79(8) . . ? F16 P1 F14 90.29(8) . . ? F11 P1 F14 179.66(8) . . ? F12 P1 F13 179.94(10) . . ? F16 P1 F13 89.35(7) . . ? F11 P1 F13 89.77(8) . . ? F14 P1 F13 90.26(8) . . ? F12 P1 F15 90.18(8) . . ? F16 P1 F15 179.05(8) . . ? F11 P1 F15 89.49(7) . . ? F14 P1 F15 90.17(8) . . ? F13 P1 F15 89.81(8) . . ? C16 S001 Rh01 108.27(6) . . ? F23 P2 F23 180.00(9) . 2_656 ? F23 P2 F21 88.84(17) . 2_656 ? F23 P2 F21 91.16(17) 2_656 2_656 ? F23 P2 F21 91.16(17) . . ? F23 P2 F21 88.84(17) 2_656 . ? F21 P2 F21 180.000(1) 2_656 . ? F23 P2 F22 89.15(18) . . ? F23 P2 F22 90.85(18) 2_656 . ? F21 P2 F22 90.30(15) 2_656 . ? F21 P2 F22 89.70(15) . . ? F23 P2 F22 90.85(18) . 2_656 ? F23 P2 F22 89.15(18) 2_656 2_656 ? F21 P2 F22 89.70(15) 2_656 2_656 ? F21 P2 F22 90.30(15) . 2_656 ? F22 P2 F22 180.00(11) . 2_656 ? C8 N3 C11 107.73(15) . . ? C8 N3 B1 129.11(15) . . ? C11 N3 B1 122.81(15) . . ? C16 N8 C18 109.92(16) . . ? C16 N8 C17 126.00(17) . . ? C18 N8 C17 124.08(17) . . ? C16 N7 C19 106.97(15) . . ? C16 N7 B1 127.36(15) . . ? C19 N7 B1 125.67(15) . . ? C8 N4 C10 109.50(16) . . ? C8 N4 C9 126.57(17) . . ? C10 N4 C9 123.91(16) . . ? C11 C10 N4 107.32(17) . . ? C1 N1 C2 116.10(16) . . ? C1 N1 B1 125.99(16) . . ? C2 N1 B1 117.21(15) . . ? C12 N5 C15 107.53(15) . . ? C12 N5 B1 130.85(16) . . ? C15 N5 B1 121.53(15) . . ? C12 N6 C14 109.59(15) . . ? C12 N6 C13 125.23(17) . . ? C14 N6 C13 125.07(16) . . ? C5 N2 C6 120.6(2) . . ? C5 N2 C7 120.99(19) . . ? C6 N2 C7 118.10(18) . . ? N2 C5 C3 122.72(19) . . ? N2 C5 C4 121.6(2) . . ? C3 C5 C4 115.63(18) . . ? N6 C12 N5 107.47(16) . . ? N6 C12 S002 123.81(14) . . ? N5 C12 S002 128.57(14) . . ? C14 C15 N5 108.38(17) . . ? N1 C1 C3 123.29(18) . . ? C1 C3 C5 120.85(18) . . ? N8 C16 N7 107.48(16) . . ? N8 C16 S001 121.94(14) . . ? N7 C16 S001 130.48(14) . . ? C19 C18 N8 106.99(17) . . ? C10 C11 N3 107.93(17) . . ? C2 C4 C5 120.09(19) . . ? N007 C20 C21 179.6(3) . . ? C15 C14 N6 106.93(17) . . ? C4 C2 N1 123.92(18) . . ? N3 B1 N5 112.83(15) . . ? N3 B1 N7 108.01(15) . . ? N5 B1 N7 114.12(15) . . ? N3 B1 N1 110.32(14) . . ? N5 B1 N1 102.37(14) . . ? N7 B1 N1 109.05(14) . . ? N4 C8 N3 107.35(16) . . ? N4 C8 S003 123.79(15) . . ? N3 C8 S003 128.55(14) . . ? C18 C19 N7 108.62(17) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 73.92 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.680 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.070 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.500 103 26 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 936862' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pb2004 _audit_creation_method ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 B2 Cl18 N14 Pd S6' _chemical_formula_weight 1575.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_cell_setting monoclinic 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 15.2678(5) _cell_length_b 11.8506(4) _cell_length_c 17.0134(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.756(4) _cell_angle_gamma 90.00 _cell_volume 3074.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120.00(10) _cell_measurement_reflns_used 4554 _cell_measurement_theta_min 2.8691 _cell_measurement_theta_max 25.2953 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2279 _exptl_crystal_size_mid 0.0501 _exptl_crystal_size_min 0.0362 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.329 _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_T_max 1.136 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.00(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24308 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5626 _reflns_number_gt 3863 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. #=============================================================================== The following checkCIF ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-level. #=============================================================================== PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C100 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C030 PLAT431_ALERT_2_C Short Inter HL..A Contact Cl11 .. S2 . 3.29 Ang. PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n PLAT434_ALERT_2_G Short Inter HL..HL Contact Cl13 .. Cl13 . 3.16 Ang. PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 4 No Action Taken ; _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^)+(0.0355P)^2^+1.0167P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5626 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _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 C1 C -0.0053(3) -0.2729(3) -0.0004(3) 0.0172(10) Uani 1 1 d . . . C2 C 0.0840(3) -0.4165(4) 0.0327(3) 0.0261(12) Uani 1 1 d . . . H2 H 0.1133 -0.4723 0.0620 0.031 Uiso 1 1 calc R . . C3 C 0.0932(3) -0.3926(3) -0.0434(3) 0.0230(11) Uani 1 1 d . . . H3 H 0.1310 -0.4292 -0.0763 0.028 Uiso 1 1 calc R . . C4 C -0.0040(3) -0.3334(4) 0.1404(3) 0.0308(12) Uani 1 1 d . . . H4A H 0.0253 -0.2705 0.1657 0.046 Uiso 1 1 calc R . . H4B H 0.0118 -0.4016 0.1681 0.046 Uiso 1 1 calc R . . H4C H -0.0663 -0.3225 0.1409 0.046 Uiso 1 1 calc R . . C5 C -0.1569(3) 0.0993(3) 0.0955(3) 0.0185(10) Uani 1 1 d . . . C6 C -0.2199(3) 0.0646(4) 0.2087(3) 0.0253(12) Uani 1 1 d . . . H6 H -0.2566 0.0343 0.2453 0.030 Uiso 1 1 calc R . . C7 C -0.1558(3) 0.1412(4) 0.2229(3) 0.0230(11) Uani 1 1 d . . . H7 H -0.1400 0.1728 0.2716 0.028 Uiso 1 1 calc R . . C8 C -0.2793(3) -0.0407(4) 0.0894(3) 0.0308(13) Uani 1 1 d . . . H8A H -0.3082 -0.0048 0.0447 0.046 Uiso 1 1 calc R . . H8B H -0.3223 -0.0662 0.1248 0.046 Uiso 1 1 calc R . . H8C H -0.2461 -0.1040 0.0721 0.046 Uiso 1 1 calc R . . C9 C 0.1262(3) 0.2312(4) 0.1881(3) 0.0216(11) Uani 1 1 d . . . C10 C 0.1350(3) 0.0444(4) 0.2067(3) 0.0239(11) Uani 1 1 d . . . H10 H 0.1577 -0.0269 0.2182 0.029 Uiso 1 1 calc R . . C11 C 0.0520(3) 0.0687(3) 0.1852(3) 0.0218(11) Uani 1 1 d . . . H11 H 0.0064 0.0171 0.1791 0.026 Uiso 1 1 calc R . . C12 C 0.2743(3) 0.1567(4) 0.2309(4) 0.0380(14) Uani 1 1 d . . . H12A H 0.2960 0.2263 0.2106 0.057 Uiso 1 1 calc R . . H12B H 0.3060 0.0947 0.2096 0.057 Uiso 1 1 calc R . . H12C H 0.2822 0.1564 0.2872 0.057 Uiso 1 1 calc R . . C13 C -0.0587(3) 0.3495(4) 0.2084(3) 0.0217(11) Uani 1 1 d . . . C020 C 0.7175(3) 0.6427(4) 0.9832(3) 0.0299(12) Uani 1 1 d . . . H020 H 0.7709 0.6594 0.9557 0.036 Uiso 1 1 calc R . . C030 C 0.4161(3) 0.6993(4) 0.8790(3) 0.0348(13) Uani 1 1 d . . . H030 H 0.4346 0.6962 0.9349 0.042 Uiso 1 1 calc R . . C100 C 0.4184(3) 0.8128(4) 1.1216(3) 0.0303(12) Uani 1 1 d . . . H100 H 0.4179 0.8382 1.1764 0.036 Uiso 1 1 calc R . . N1 N 0.0375(2) -0.3043(3) -0.0654(2) 0.0190(9) Uani 1 1 d . . . N2 N 0.0223(2) -0.3417(3) 0.0590(2) 0.0243(9) Uani 1 1 d . . . N3 N -0.1174(2) 0.1649(3) 0.1521(2) 0.0203(9) Uani 1 1 d . . . N4 N -0.2204(2) 0.0400(3) 0.1301(2) 0.0218(9) Uani 1 1 d . . . N5 N 0.0454(2) 0.1849(3) 0.1735(2) 0.0193(9) Uani 1 1 d . . . N6 N 0.1811(2) 0.1454(3) 0.2085(2) 0.0255(10) Uani 1 1 d . . . N7 N -0.0801(3) 0.4192(3) 0.2497(3) 0.0299(10) Uani 1 1 d . . . S1 S -0.08078(8) -0.16631(9) 0.00839(8) 0.0223(3) Uani 1 1 d . . . S2 S -0.13667(7) 0.08946(9) -0.00312(7) 0.0207(3) Uani 1 1 d . . . S6 S 0.15365(8) 0.36985(9) 0.18337(8) 0.0247(3) Uani 1 1 d . . . Cl11 Cl 0.31108(9) 0.78974(14) 1.08680(11) 0.0590(5) Uani 1 1 d . . . Cl12 Cl 0.47911(9) 0.68740(11) 1.11818(9) 0.0410(4) Uani 1 1 d . . . Cl13 Cl 0.46823(11) 0.91756(12) 1.06569(10) 0.0594(5) Uani 1 1 d . . . Cl21 Cl 0.67706(9) 0.51187(11) 0.94980(9) 0.0449(4) Uani 1 1 d . . . Cl22 Cl 0.74512(9) 0.63621(11) 1.08517(8) 0.0383(3) Uani 1 1 d . . . Cl23 Cl 0.64178(9) 0.75083(11) 0.96247(9) 0.0423(4) Uani 1 1 d . . . Cl31 Cl 0.44150(9) 0.83349(10) 0.84264(9) 0.0392(4) Uani 1 1 d . . . Cl32 Cl 0.47265(10) 0.59411(11) 0.82903(10) 0.0519(4) Uani 1 1 d . . . Cl33 Cl 0.30346(10) 0.67550(11) 0.86998(12) 0.0603(5) Uani 1 1 d . . . Pd Pd 0.0000 0.0000 0.0000 0.01735(14) Uani 1 2 d S . . B B -0.0380(3) 0.2486(4) 0.1477(3) 0.0208(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(2) 0.015(2) 0.018(3) -0.001(2) -0.003(2) -0.0049(19) C2 0.028(3) 0.021(2) 0.030(3) 0.007(2) 0.000(2) 0.005(2) C3 0.024(3) 0.016(2) 0.029(3) -0.003(2) 0.003(2) 0.001(2) C4 0.041(3) 0.033(3) 0.019(3) 0.005(2) 0.005(2) 0.002(2) C5 0.018(2) 0.013(2) 0.023(3) 0.000(2) 0.001(2) 0.0022(19) C6 0.027(3) 0.027(3) 0.023(3) 0.004(2) 0.009(2) 0.000(2) C7 0.026(3) 0.030(3) 0.013(3) 0.000(2) 0.003(2) 0.001(2) C8 0.035(3) 0.024(3) 0.034(3) -0.007(2) 0.006(3) -0.004(2) C9 0.023(3) 0.022(2) 0.020(3) 0.007(2) 0.000(2) 0.000(2) C10 0.033(3) 0.016(2) 0.022(3) 0.006(2) 0.003(2) 0.004(2) C11 0.029(3) 0.011(2) 0.026(3) 0.004(2) 0.005(2) 0.001(2) C12 0.022(3) 0.038(3) 0.053(4) 0.015(3) -0.004(3) 0.005(2) C13 0.021(3) 0.024(3) 0.020(3) 0.003(2) 0.004(2) -0.001(2) C020 0.032(3) 0.023(3) 0.035(3) 0.003(2) 0.004(3) -0.002(2) C030 0.044(3) 0.028(3) 0.032(3) -0.003(2) -0.001(3) 0.008(2) C100 0.039(3) 0.031(3) 0.020(3) 0.003(2) -0.007(2) 0.001(2) N1 0.020(2) 0.0149(18) 0.022(2) 0.0007(17) 0.0014(18) 0.0020(16) N2 0.028(2) 0.022(2) 0.023(3) 0.0054(18) 0.0026(19) -0.0003(18) N3 0.024(2) 0.0187(19) 0.018(2) 0.0005(17) 0.0036(18) 0.0037(16) N4 0.020(2) 0.0184(19) 0.027(3) -0.0018(18) 0.0023(19) -0.0052(16) N5 0.026(2) 0.0146(18) 0.017(2) -0.0010(16) 0.0022(18) 0.0007(16) N6 0.025(2) 0.023(2) 0.028(3) 0.0037(18) -0.0014(19) 0.0065(18) N7 0.035(2) 0.031(2) 0.025(3) -0.003(2) 0.007(2) 0.0031(19) S1 0.0223(6) 0.0187(6) 0.0264(7) -0.0010(5) 0.0063(5) 0.0006(5) S2 0.0209(6) 0.0196(6) 0.0216(7) -0.0023(5) 0.0008(5) 0.0009(5) S6 0.0263(7) 0.0193(6) 0.0284(8) 0.0041(5) -0.0003(6) -0.0018(5) Cl11 0.0333(8) 0.0809(11) 0.0612(12) -0.0021(9) -0.0155(8) 0.0069(8) Cl12 0.0456(8) 0.0362(7) 0.0401(9) -0.0051(6) -0.0082(7) 0.0088(6) Cl13 0.0853(12) 0.0449(9) 0.0475(11) 0.0163(8) -0.0024(9) -0.0150(8) Cl21 0.0558(9) 0.0306(7) 0.0482(10) -0.0074(7) 0.0012(8) -0.0112(6) Cl22 0.0464(8) 0.0367(7) 0.0320(8) 0.0018(6) 0.0039(7) -0.0034(6) Cl23 0.0414(8) 0.0340(7) 0.0507(10) -0.0057(6) -0.0062(7) 0.0056(6) Cl31 0.0434(8) 0.0267(7) 0.0481(10) -0.0045(6) 0.0078(7) -0.0003(6) Cl32 0.0516(9) 0.0335(7) 0.0702(12) -0.0208(8) -0.0011(8) 0.0127(7) Cl33 0.0418(9) 0.0349(8) 0.1057(16) 0.0226(9) 0.0180(9) 0.0039(7) Pd 0.0187(3) 0.0152(2) 0.0183(3) -0.0013(2) 0.0024(2) 0.0011(2) B 0.024(3) 0.016(3) 0.022(3) -0.003(2) 0.001(3) 0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N2 1.350(6) . ? C1 N1 1.362(5) . ? C1 S1 1.721(4) . ? C2 C3 1.339(7) . ? C2 N2 1.383(6) . ? C2 H2 0.9300 . ? C3 N1 1.389(6) . ? C3 H3 0.9300 . ? C4 N2 1.465(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N4 1.355(5) . ? C5 N3 1.356(6) . ? C5 S2 1.725(5) . ? C6 C7 1.348(6) . ? C6 N4 1.368(6) . ? C6 H6 0.9300 . ? C7 N3 1.393(6) . ? C7 H7 0.9300 . ? C8 N4 1.464(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N6 1.352(6) . ? C9 N5 1.362(6) . ? C9 S6 1.698(4) . ? C10 C11 1.333(6) . ? C10 N6 1.389(6) . ? C10 H10 0.9300 . ? C11 N5 1.394(5) . ? C11 H11 0.9300 . ? C12 N6 1.462(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N7 1.143(5) . ? C13 B 1.622(7) . ? C020 Cl23 1.750(5) . ? C020 Cl21 1.753(5) . ? C020 Cl22 1.768(6) . ? C020 H020 0.9800 . ? C030 Cl33 1.742(5) . ? C030 Cl31 1.757(5) . ? C030 Cl32 1.759(5) . ? C030 H030 0.9800 . ? C100 Cl11 1.738(5) . ? C100 Cl12 1.753(5) . ? C100 Cl13 1.759(5) . ? C100 H100 0.9800 . ? N1 B 1.548(7) 3 ? N3 B 1.571(6) . ? N5 B 1.526(6) . ? S1 Pd 2.3330(11) . ? S2 Pd 2.3389(11) . ? Pd S1 2.3330(11) 3 ? Pd S2 2.3389(11) 3 ? B N1 1.548(7) 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 N2 C1 N1 107.3(4) . . ? N2 C1 S1 124.4(3) . . ? N1 C1 S1 128.3(4) . . ? C3 C2 N2 106.4(4) . . ? C3 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? C2 C3 N1 109.1(4) . . ? C2 C3 H3 125.4 . . ? N1 C3 H3 125.4 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 N3 107.0(4) . . ? N4 C5 S2 123.5(4) . . ? N3 C5 S2 129.5(3) . . ? C7 C6 N4 106.8(4) . . ? C7 C6 H6 126.6 . . ? N4 C6 H6 126.6 . . ? C6 C7 N3 108.3(4) . . ? C6 C7 H7 125.9 . . ? N3 C7 H7 125.9 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 N5 106.8(4) . . ? N6 C9 S6 126.0(4) . . ? N5 C9 S6 127.2(3) . . ? C11 C10 N6 107.1(4) . . ? C11 C10 H10 126.5 . . ? N6 C10 H10 126.5 . . ? C10 C11 N5 108.3(4) . . ? C10 C11 H11 125.8 . . ? N5 C11 H11 125.8 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 B 174.6(5) . . ? Cl23 C020 Cl21 111.3(3) . . ? Cl23 C020 Cl22 110.7(3) . . ? Cl21 C020 Cl22 110.1(3) . . ? Cl23 C020 H020 108.2 . . ? Cl21 C020 H020 108.2 . . ? Cl22 C020 H020 108.2 . . ? Cl33 C030 Cl31 110.4(3) . . ? Cl33 C030 Cl32 110.4(3) . . ? Cl31 C030 Cl32 110.4(3) . . ? Cl33 C030 H030 108.5 . . ? Cl31 C030 H030 108.5 . . ? Cl32 C030 H030 108.5 . . ? Cl11 C100 Cl12 110.3(3) . . ? Cl11 C100 Cl13 110.6(3) . . ? Cl12 C100 Cl13 109.7(3) . . ? Cl11 C100 H100 108.7 . . ? Cl12 C100 H100 108.7 . . ? Cl13 C100 H100 108.7 . . ? C1 N1 C3 107.4(4) . . ? C1 N1 B 129.8(4) . 3 ? C3 N1 B 122.3(4) . 3 ? C1 N2 C2 109.8(4) . . ? C1 N2 C4 125.2(4) . . ? C2 N2 C4 124.9(4) . . ? C5 N3 C7 107.9(4) . . ? C5 N3 B 130.2(4) . . ? C7 N3 B 121.8(4) . . ? C5 N4 C6 110.1(4) . . ? C5 N4 C8 124.8(4) . . ? C6 N4 C8 125.2(4) . . ? C9 N5 C11 108.2(4) . . ? C9 N5 B 126.1(3) . . ? C11 N5 B 125.7(4) . . ? C9 N6 C10 109.6(4) . . ? C9 N6 C12 125.6(4) . . ? C10 N6 C12 124.8(4) . . ? C1 S1 Pd 104.84(14) . . ? C5 S2 Pd 102.10(15) . . ? S1 Pd S1 180.00(6) . 3 ? S1 Pd S2 84.87(4) . . ? S1 Pd S2 95.13(4) 3 . ? S1 Pd S2 95.13(4) . 3 ? S1 Pd S2 84.87(4) 3 3 ? S2 Pd S2 180.00(5) . 3 ? N5 B N1 115.5(4) . 3 ? N5 B N3 108.0(3) . . ? N1 B N3 110.5(4) 3 . ? N5 B C13 111.5(4) . . ? N1 B C13 105.8(3) 3 . ? N3 B C13 105.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.865 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 936863'