# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Simon Duckett' 'Cyril Godard' 'Simon Parsons' 'R. Perutz' _publ_contact_author_name 'Dr Simon Duckett' _publ_contact_author_address ; Chemistry University of York Heslington York York YO105DD UNITED KINGDOM ; _publ_contact_author_email SBD3@YORK.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Dipyridylketone binding and subsequent C-C bond insertion reactions at cyclopentadienylrhodium ; data_rhcg02 _database_code_CSD 213069 #Note to referee: see refine special details for xprep, shelx and #checkcif (Platon) output. _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [RhCp(Pyr2CH2CH2CO)] _chemical_formula_sum 'C18 H17 N2 O Rh' _chemical_formula_weight 380.25 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6828(13) _cell_length_b 11.9109(16) _cell_length_c 12.9438(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.842(2) _cell_angle_gamma 90.00 _cell_volume 1478.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6117 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9196 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.93 _reflns_number_total 3574 _reflns_number_gt 3263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution Dirdif _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + rhcg02 started at 14:11:35 on 20-Jun-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.683 11.911 12.944 90.00 97.84 90.00 9502 Reflections read from file rhcg02.hkl; mean (I/sigma) = 17.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4750 4742 4754 4745 7123 6337 6341 9502 N (int>3sigma) = 0 3902 3800 3868 3837 5785 5184 5199 7777 Mean intensity = 0.0 140.0 124.0 141.8 139.0 135.3 140.4 138.5 138.9 Mean int/sigma = 0.0 17.5 16.4 17.7 17.3 17.2 17.6 17.3 17.5 Lattice type: P chosen Volume: 1478.86 #------------------------------------------------------------------------------ DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 9.683 11.911 12.944 90.00 97.84 90.00 Niggli form: a.a = 93.76 b.b = 141.87 c.c = 167.54 b.c = 0.00 a.c = -17.10 a.b = 0.00 #------------------------------------------------------------------------------ Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) #----------------------------------------------------------------------------- Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.019 [ 3093] Cell: 9.683 11.911 12.944 90.00 97.84 90.00 Volume: 1478.86 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected #------------------------------------------------------------------------------ SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4750 4742 4754 4745 7123 6337 6341 9502 N (int>3sigma) = 0 3902 3800 3868 3837 5785 5184 5199 7777 Mean intensity = 0.0 140.0 124.0 141.8 139.0 135.3 140.4 138.5 138.9 Mean int/sigma = 0.0 17.5 16.4 17.7 17.3 17.2 17.6 17.3 17.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.888 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 9 296 299 297 N I>3s 1 143 144 11 0.8 234.2 231.8 0.6 1.5 21.2 21.0 1.0 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.019 3093 1.5 / 17.5 1.25 Option [A] chosen #------------------------------------------------------------------------------ INTENSITY STATISTICS FOR DATASET # 1 rhcg02.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 194 194 100.0 3.53 416.9 87.62 0.0166 0.0074 2.10 - 1.65 189 189 100.0 3.74 320.0 68.74 0.0173 0.0101 1.65 - 1.40 237 237 100.0 3.53 206.0 44.96 0.0247 0.0147 1.40 - 1.25 242 242 100.0 3.22 151.3 32.92 0.0249 0.0192 1.25 - 1.15 239 239 100.0 3.00 135.6 27.95 0.0238 0.0231 1.15 - 1.05 338 338 100.0 2.75 104.9 22.62 0.0245 0.0305 1.05 - 1.00 211 211 100.0 2.55 100.2 20.97 0.0261 0.0337 1.00 - 0.95 263 263 100.0 2.43 96.4 18.74 0.0269 0.0367 0.95 - 0.90 339 339 100.0 2.27 73.3 15.67 0.0284 0.0451 0.90 - 0.85 410 410 100.0 2.20 67.0 13.94 0.0313 0.0499 0.85 - 0.80 503 514 97.9 1.97 50.0 11.10 0.0353 0.0632 0.80 - 0.75 530 669 79.2 1.39 43.7 9.39 0.0484 0.0790 0.75 - 0.73 51 248 20.6 0.23 42.6 7.15 0.0235 0.1026 #----------------------------------------------------------------------------- 0.85 - 0.73 1084 1431 75.8 1.40 46.6 10.08 0.0405 0.0722 Inf - 0.73 3746 4093 91.5 2.32 118.5 25.16 0.0231 0.0276 Merged [A], lowest resolution = 12.82 Angstroms, 222 outliers downweighted final shelx res file.... #TITL rhcg02 in P21/n solved dirdif #CELL 0.71073 9.68280 11.91090 12.94380 90.0000 97.8420 90.0000 #ZERR 4.000 0.00130 0.00160 0.00170 0.0000 0.0020 0.0000 #LATT +1 #SYMM 1/2-X , 1/2+Y , 1/2-Z #SFAC C H N O RH #UNIT 72 68 8 4 4 #TEMP -123 #L.S. 4 #ACTA #MPLA C9 N10 C11 C12 C13 C14 #MPLA N1 C2 C3 C4 C5 C6 #MPLA C15 C16 C17 C18 C19 #MPLA N1 C2 C3 C4 C5 C6 #MPLA 3 RH1 C20 C21 C7 #FMAP 2 #PLAN 10 #WGHT 0.027000 0.862400 #EXTI 0.001102 #FVAR 0.27465 #RH1 5 0.145830 0.209597 0.104538 11.00000 0.01415 0.01521 = #0.01575 0.00027 0.00266 -0.00345 #N1 3 0.147331 0.188165 0.262212 11.00000 0.01504 0.01672 = #0.01748 -0.00134 0.00228 -0.00154 #C2 1 0.240158 0.230181 0.339161 11.00000 0.01714 0.02084 = #0.02401 -0.00266 0.00239 -0.00669 #AFIX 43 #H2 2 0.314524 0.274959 0.321224 11.00000 -1.20000 #AFIX 0 #C3 1 0.231676 0.210856 0.442987 11.00000 0.01820 0.02480 = #0.02017 -0.00573 -0.00006 -0.00069 #AFIX 43 #H3 2 0.299412 0.240653 0.495891 11.00000 -1.20000 #AFIX 0 #C4 1 0.121521 0.146691 0.468191 11.00000 0.02083 0.02217 = #0.01628 -0.00216 0.00288 0.00097 #AFIX 43 #H4 2 0.111806 0.132890 0.539127 11.00000 -1.20000 #AFIX 0 #C5 1 0.025656 0.102819 0.389128 11.00000 0.01442 0.01716 = #0.01889 0.00022 0.00364 0.00004 #AFIX 43 #H5 2 -0.050423 0.058993 0.405480 11.00000 -1.20000 #AFIX 0 #C6 1 0.041726 0.123429 0.285997 11.00000 0.01383 0.01136 = #0.01923 -0.00099 0.00125 0.00164 #C7 1 -0.044069 0.077880 0.187063 11.00000 0.01302 0.01393 = #0.01485 0.00171 0.00034 -0.00130 #O8 4 -0.055661 0.164361 0.113137 11.00000 0.01211 0.01554 = #0.01811 0.00491 0.00137 -0.00090 #C9 1 -0.186677 0.033708 0.203892 11.00000 0.01596 0.01632 = #0.01417 -0.00131 0.00185 -0.00246 #N10 3 -0.189680 -0.060133 0.261038 11.00000 0.01791 0.02135 = #0.02206 0.00578 0.00079 -0.00403 #C11 1 -0.314975 -0.103002 0.271819 11.00000 0.02346 0.02376 = #0.02325 0.00650 0.00218 -0.00659 #AFIX 43 #H11 2 -0.318051 -0.169279 0.312272 11.00000 -1.20000 #AFIX 0 #C12 1 -0.439087 -0.056734 0.227826 11.00000 0.01610 0.03331 = #0.03588 0.00606 0.00596 -0.00852 #AFIX 43 #H12 2 -0.525429 -0.090407 0.237247 11.00000 -1.20000 #AFIX 0 #C13 1 -0.435116 0.040078 0.169497 11.00000 0.01383 0.04118 = #0.05728 0.02127 0.00124 -0.00032 #AFIX 43 #H13 2 -0.518946 0.074693 0.138298 11.00000 -1.20000 #AFIX 0 #C14 1 -0.306731 0.085816 0.157287 11.00000 0.01564 0.02598 = #0.04208 0.01584 0.00193 -0.00155 #AFIX 43 #H14 2 -0.301336 0.152200 0.117352 11.00000 -1.20000 #AFIX 0 #C15 1 0.217860 0.387675 0.083224 11.00000 0.03776 0.01842 = #0.02940 -0.00257 0.01193 -0.01230 #AFIX 43 #H15 2 0.214246 0.447700 0.131111 11.00000 -1.20000 #AFIX 0 #C16 1 0.328857 0.307785 0.084025 11.00000 0.02192 0.03409 = #0.02333 0.00267 0.00581 -0.01288 #AFIX 43 #H16 2 0.410505 0.304187 0.133768 11.00000 -1.20000 #AFIX 0 #C17 1 0.295164 0.235043 -0.002635 11.00000 0.02775 0.02480 = #0.02762 0.00310 0.01433 -0.00523 #AFIX 43 #H17 2 0.352105 0.176379 -0.023128 11.00000 -1.20000 #AFIX 0 #C18 1 0.161244 0.265701 -0.053095 11.00000 0.03544 0.02505 = #0.01764 0.00221 0.00328 -0.01275 #AFIX 43 #H18 2 0.110479 0.229091 -0.111535 11.00000 -1.20000 #AFIX 0 #C19 1 0.116344 0.361619 -0.000212 11.00000 0.02971 0.02076 = #0.03284 0.00984 0.00553 -0.00435 #AFIX 43 #H19 2 0.031324 0.401053 -0.018900 11.00000 -1.20000 #AFIX 0 #C20 1 0.176771 0.035468 0.115922 11.00000 0.01659 0.01665 = #0.02017 -0.00008 0.00328 0.00011 #AFIX 23 #H20A 2 0.196413 0.004779 0.048353 11.00000 -1.20000 #H20B 2 0.256830 0.018165 0.169661 11.00000 -1.20000 #AFIX 0 #C21 1 0.044123 -0.016019 0.145676 11.00000 0.01663 0.01466 = #0.01592 -0.00125 -0.00017 0.00033 #AFIX 23 #H21A 2 0.067667 -0.073867 0.200154 11.00000 -1.20000 #H21B 2 -0.009545 -0.052318 0.084053 11.00000 -1.20000 #HKLF 4 #REM rhcg02 in P21/n solved dirdif #REM R1 = 0.0260 for 3263 Fo > 4sig(Fo) and 0.0292 for all 3574 data #REM 200 parameters refined using 0 restraints #END #WGHT 0.0270 0.8633 #REM Highest difference peak 0.544, deepest hole -0.581, 1-sigma level 0.088 #Q1 1 0.1224 0.1387 0.1093 11.00000 0.05 0.54 #Q2 1 -0.0121 0.1022 0.2328 11.00000 0.05 0.46 #Q3 1 0.2136 0.2092 0.1590 11.00000 0.05 0.45 #Q4 1 0.1647 0.2002 0.4530 11.00000 0.05 0.44 #Q5 1 0.0947 0.2040 0.0491 11.00000 0.05 0.44 #Q6 1 0.0435 0.1079 0.3411 11.00000 0.05 0.44 #Q7 1 0.2685 0.2007 0.4612 11.00000 0.05 0.42 #Q8 1 0.2074 0.1632 0.0818 11.00000 0.05 0.42 #Q9 1 -0.2449 0.0546 0.1804 11.00000 0.05 0.41 #Q10 1 -0.3649 0.0523 0.1424 11.00000 0.05 0.40 Checkcif output: #=============================================================================== # PLATON/CHECK-(191101) versus check.def version of 16/11/01 for entry: rhcg02 # Data From: rhcg02.cif - Data Type: CIF Bond Precision C-C = 0.0033 A # # CELL 0.71073 9.683 11.911 12.944 90.00 97.84 90.00 1478.90 # SpaceGroup from Symmetry P21/n Hall: -P 2yn # Reported P21/n ? # MoietyFormula C18 H17 N2 O Rh # Reported [RHCP(PYR2CH2CH2CO)] # SumFormula C18 H17 N2 O Rh # Reported C18 H17 N2 O Rh # Mr = 380.25[Calc], 380.25[Rep] # Dx,gcm-3 = 1.708[Calc], 1.708[Rep] # Z = 4[Calc], 4[Rep] # Mu (mm-1) = 1.157[Calc], 1.157[Rep] # F000 = 768.0[Calc], 768.0[Rep] # Reported T limits: Tmin=0.735 Tmax=0.862 'MULTISCAN' # Calculated T limits: Tmin=0.682 Tmin'=0.682 Tmax=0.699 # Reported Hmax= 13, Kmax= 15, Lmax= 16, Nref= 3574 , Th(max)= 28.93 # Calculated Hmax= 13, Kmax= 16, Lmax= 17, Nref= 3904( 3904), Ratio= 0.92( 0.92) # R= 0.0260( 3263), wR2= 0.0629( 3574), S = 1.070, Npar= 200 #=============================================================================== >>> The Following ALERTS were generated <<< 761_ALERT A CIF Contains no X-H Bonds .................... ? 762_ALERT A CIF Contains no X-Y-H or H-Y-H Angles ........ ? These were all calculated. #=============================================================================== Few problems with the C's.... 042_ALERT C Calc. and Rep. MoietyFormula Strings Differ .. ? 061_ALERT C Tmax/Tmin Range Test RR' too large ........... 0.87 062_ALERT C Rescale T(min) & T(max) by ................... 0.81 The crystal size includes mounting oil, and this should reduce mu*r a bit. 125_ALERT C No _symmetry_space_group_name_Hall given ..... ? 128_ALERT C Non-standard setting of space group P21/c .. P21/n 145_ALERT C su on beta Small or Missing (x 10000) ... 20 Deg. 220_ALERT C Large Non-Solvent C Ueq(max)/Ueq(min) . 2.68 Ratio C9-C14 have quite anisotropic Uij's - the ellipsoids look as though this group is librating about C8-C9. ALERT Level Summary 2 ALERT Level A = In General: Serious Problem 7 ALERT Level C = Check & Explain #=============================================================================== ; _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^)+(0.0270P)^2^+0.8624P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'Found in difference map, but idealised' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3574 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Rh1 Rh 0.145830(17) 0.209597(14) 0.104538(12) 0.01498(7) Uani 1 1 d . . . N1 N 0.14733(19) 0.18816(15) 0.26221(14) 0.0164(4) Uani 1 1 d . . . C2 C 0.2402(2) 0.23018(19) 0.33916(18) 0.0207(5) Uani 1 1 d . . . H2 H 0.3145 0.2750 0.3212 0.025 Uiso 1 1 calc R . . C3 C 0.2317(2) 0.21086(19) 0.44299(18) 0.0213(5) Uani 1 1 d . . . H3 H 0.2994 0.2407 0.4959 0.026 Uiso 1 1 calc R . . C4 C 0.1215(2) 0.14669(19) 0.46819(17) 0.0197(4) Uani 1 1 d . . . H4 H 0.1118 0.1329 0.5391 0.024 Uiso 1 1 calc R . . C5 C 0.0257(2) 0.10282(18) 0.38913(16) 0.0167(4) Uani 1 1 d . . . H5 H -0.0504 0.0590 0.4055 0.020 Uiso 1 1 calc R . . C6 C 0.0417(2) 0.12343(17) 0.28600(16) 0.0149(4) Uani 1 1 d . . . C7 C -0.0441(2) 0.07788(17) 0.18706(15) 0.0141(4) Uani 1 1 d . . . O8 O -0.05566(15) 0.16436(12) 0.11314(11) 0.0153(3) Uani 1 1 d . . . C9 C -0.1867(2) 0.03371(18) 0.20389(16) 0.0155(4) Uani 1 1 d . . . N10 N -0.18968(19) -0.06013(16) 0.26104(14) 0.0206(4) Uani 1 1 d . . . C11 C -0.3150(2) -0.1030(2) 0.27182(18) 0.0236(5) Uani 1 1 d . . . H11 H -0.3181 -0.1693 0.3123 0.028 Uiso 1 1 calc R . . C12 C -0.4391(2) -0.0567(2) 0.2278(2) 0.0282(5) Uani 1 1 d . . . H12 H -0.5254 -0.0904 0.2372 0.034 Uiso 1 1 calc R . . C13 C -0.4351(3) 0.0401(2) 0.1695(2) 0.0378(7) Uani 1 1 d . . . H13 H -0.5189 0.0747 0.1383 0.045 Uiso 1 1 calc R . . C14 C -0.3067(2) 0.0858(2) 0.1573(2) 0.0281(6) Uani 1 1 d . . . H14 H -0.3013 0.1522 0.1174 0.034 Uiso 1 1 calc R . . C15 C 0.2179(3) 0.3877(2) 0.08322(19) 0.0278(5) Uani 1 1 d . . . H15 H 0.2142 0.4477 0.1311 0.033 Uiso 1 1 calc R . . C16 C 0.3289(3) 0.3078(2) 0.08403(19) 0.0262(5) Uani 1 1 d . . . H16 H 0.4105 0.3042 0.1338 0.031 Uiso 1 1 calc R . . C17 C 0.2952(3) 0.2350(2) -0.00263(19) 0.0257(5) Uani 1 1 d . . . H17 H 0.3521 0.1764 -0.0231 0.031 Uiso 1 1 calc R . . C18 C 0.1612(3) 0.2657(2) -0.05309(18) 0.0261(5) Uani 1 1 d . . . H18 H 0.1105 0.2291 -0.1115 0.031 Uiso 1 1 calc R . . C19 C 0.1163(3) 0.3616(2) -0.0002(2) 0.0277(5) Uani 1 1 d . . . H19 H 0.0313 0.4011 -0.0189 0.033 Uiso 1 1 calc R . . C20 C 0.1768(2) 0.03547(18) 0.11592(17) 0.0177(4) Uani 1 1 d . . . H20A H 0.1964 0.0048 0.0484 0.021 Uiso 1 1 calc R . . H20B H 0.2568 0.0182 0.1697 0.021 Uiso 1 1 calc R . . C21 C 0.0441(2) -0.01602(18) 0.14568(16) 0.0160(4) Uani 1 1 d . . . H21A H 0.0677 -0.0739 0.2002 0.019 Uiso 1 1 calc R . . H21B H -0.0095 -0.0523 0.0841 0.019 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 Rh1 0.01415(10) 0.01521(10) 0.01575(10) 0.00027(6) 0.00266(6) -0.00345(6) N1 0.0150(9) 0.0167(9) 0.0175(9) -0.0013(7) 0.0023(7) -0.0015(7) C2 0.0171(11) 0.0208(11) 0.0240(11) -0.0027(9) 0.0024(9) -0.0067(9) C3 0.0182(11) 0.0248(12) 0.0202(11) -0.0057(9) -0.0001(9) -0.0007(9) C4 0.0208(11) 0.0222(11) 0.0163(10) -0.0022(9) 0.0029(9) 0.0010(9) C5 0.0144(10) 0.0172(10) 0.0189(10) 0.0002(8) 0.0036(8) 0.0000(8) C6 0.0138(10) 0.0114(9) 0.0192(10) -0.0010(8) 0.0013(8) 0.0016(8) C7 0.0130(10) 0.0139(10) 0.0149(9) 0.0017(8) 0.0003(8) -0.0013(8) O8 0.0121(7) 0.0155(7) 0.0181(7) 0.0049(6) 0.0014(6) -0.0009(6) C9 0.0160(10) 0.0163(10) 0.0142(9) -0.0013(8) 0.0018(8) -0.0025(8) N10 0.0179(9) 0.0214(10) 0.0221(9) 0.0058(8) 0.0008(7) -0.0040(8) C11 0.0235(12) 0.0238(12) 0.0232(11) 0.0065(9) 0.0022(9) -0.0066(10) C12 0.0161(11) 0.0333(14) 0.0359(13) 0.0061(11) 0.0060(10) -0.0085(10) C13 0.0138(11) 0.0412(16) 0.0573(18) 0.0213(14) 0.0012(12) -0.0003(11) C14 0.0156(11) 0.0260(13) 0.0421(14) 0.0158(11) 0.0019(10) -0.0015(10) C15 0.0378(14) 0.0184(12) 0.0294(12) -0.0026(10) 0.0119(11) -0.0123(10) C16 0.0219(12) 0.0341(14) 0.0233(12) 0.0027(10) 0.0058(10) -0.0129(10) C17 0.0278(13) 0.0248(12) 0.0276(12) 0.0031(10) 0.0143(10) -0.0052(10) C18 0.0354(14) 0.0250(12) 0.0176(11) 0.0022(9) 0.0033(10) -0.0127(11) C19 0.0297(13) 0.0208(12) 0.0328(13) 0.0098(10) 0.0055(11) -0.0043(10) C20 0.0166(10) 0.0166(10) 0.0202(10) -0.0001(8) 0.0033(8) 0.0001(8) C21 0.0166(10) 0.0147(10) 0.0159(10) -0.0012(8) -0.0002(8) 0.0003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O8 2.0417(14) . ? Rh1 N1 2.0549(18) . ? Rh1 C20 2.098(2) . ? Rh1 C17 2.157(2) . ? Rh1 C16 2.170(2) . ? Rh1 C18 2.171(2) . ? Rh1 C19 2.257(2) . ? Rh1 C15 2.261(2) . ? N1 C2 1.344(3) . ? N1 C6 1.349(3) . ? C2 C3 1.377(3) . ? C3 C4 1.387(3) . ? C4 C5 1.387(3) . ? C5 C6 1.387(3) . ? C6 C7 1.528(3) . ? C7 O8 1.400(2) . ? C7 C9 1.521(3) . ? C7 C21 1.547(3) . ? C9 N10 1.343(3) . ? C9 C14 1.382(3) . ? N10 C11 1.341(3) . ? C11 C12 1.373(3) . ? C12 C13 1.382(4) . ? C13 C14 1.386(3) . ? C15 C19 1.393(4) . ? C15 C16 1.434(4) . ? C16 C17 1.420(4) . ? C17 C18 1.418(4) . ? C18 C19 1.430(4) . ? C20 C21 1.520(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 O8 Rh1 N1 77.90(6) . . ? O8 Rh1 C20 82.16(7) . . ? N1 Rh1 C20 79.97(8) . . ? O8 Rh1 C17 143.27(8) . . ? N1 Rh1 C17 137.86(9) . . ? C20 Rh1 C17 94.72(9) . . ? O8 Rh1 C16 162.08(8) . . ? N1 Rh1 C16 107.06(8) . . ? C20 Rh1 C16 115.49(9) . . ? C17 Rh1 C16 38.30(9) . . ? O8 Rh1 C18 108.73(8) . . ? N1 Rh1 C18 168.35(8) . . ? C20 Rh1 C18 110.05(9) . . ? C17 Rh1 C18 38.24(10) . . ? C16 Rh1 C18 63.71(9) . . ? O8 Rh1 C19 101.60(8) . . ? N1 Rh1 C19 132.81(8) . . ? C20 Rh1 C19 147.20(9) . . ? C17 Rh1 C19 62.74(10) . . ? C16 Rh1 C19 62.13(10) . . ? C18 Rh1 C19 37.61(9) . . ? O8 Rh1 C15 124.55(8) . . ? N1 Rh1 C15 106.09(8) . . ? C20 Rh1 C15 153.17(9) . . ? C17 Rh1 C15 62.93(9) . . ? C16 Rh1 C15 37.70(10) . . ? C18 Rh1 C15 62.28(9) . . ? C19 Rh1 C15 35.90(9) . . ? C2 N1 C6 119.65(19) . . ? C2 N1 Rh1 127.10(15) . . ? C6 N1 Rh1 113.25(14) . . ? N1 C2 C3 122.6(2) . . ? C2 C3 C4 118.2(2) . . ? C5 C4 C3 119.5(2) . . ? C4 C5 C6 119.5(2) . . ? N1 C6 C5 120.59(19) . . ? N1 C6 C7 110.73(17) . . ? C5 C6 C7 128.64(19) . . ? O8 C7 C9 111.27(16) . . ? O8 C7 C6 107.18(16) . . ? C9 C7 C6 113.78(17) . . ? O8 C7 C21 106.97(16) . . ? C9 C7 C21 110.76(17) . . ? C6 C7 C21 106.52(17) . . ? C7 O8 Rh1 104.08(11) . . ? N10 C9 C14 122.3(2) . . ? N10 C9 C7 117.08(18) . . ? C14 C9 C7 120.55(19) . . ? C11 N10 C9 117.53(19) . . ? N10 C11 C12 123.9(2) . . ? C11 C12 C13 118.3(2) . . ? C12 C13 C14 118.9(2) . . ? C9 C14 C13 119.2(2) . . ? C19 C15 C16 107.9(2) . . ? C19 C15 Rh1 71.87(14) . . ? C16 C15 Rh1 67.68(13) . . ? C17 C16 C15 107.9(2) . . ? C17 C16 Rh1 70.38(13) . . ? C15 C16 Rh1 74.62(14) . . ? C18 C17 C16 107.7(2) . . ? C18 C17 Rh1 71.42(14) . . ? C16 C17 Rh1 71.31(13) . . ? C17 C18 C19 107.7(2) . . ? C17 C18 Rh1 70.35(13) . . ? C19 C18 Rh1 74.43(14) . . ? C15 C19 C18 108.7(2) . . ? C15 C19 Rh1 72.23(14) . . ? C18 C19 Rh1 67.96(13) . . ? C21 C20 Rh1 107.41(14) . . ? C20 C21 C7 108.76(17) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.93 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.544 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.088 data_rhcg01 _database_code_CSD 213070 #note to referee- please see refine special details for #reciprocal space exploration data, a shelx res file and #checkcif output (platon). _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [CpRh(PyrCOPry)] _chemical_formula_sum 'C16 H13 N2 O Rh' _chemical_formula_weight 352.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0676(12) _cell_length_b 5.5804(6) _cell_length_c 19.407(2) _cell_angle_alpha 90.0000(15) _cell_angle_beta 100.5909(15) _cell_angle_gamma 90.0000(13) _cell_volume 1284.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5422 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7664 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.89 _reflns_number_total 3087 _reflns_number_gt 2875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution Dirdif _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + rhcg01 started at 13:15:04 on 20-Jun-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.068 5.580 19.407 90.00 100.59 90.00 8147 Reflections read from file rhcg01.hkl; mean (I/sigma) = 17.95 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4073 4079 4076 4077 6114 5435 5426 8147 N (int>3sigma) = 0 3354 2981 3327 3215 4831 4420 4442 6630 Mean intensity = 0.0 280.1 272.5 287.5 267.3 280.0 275.1 279.5 277.9 Mean int/sigma = 0.0 18.0 17.0 18.2 17.3 17.7 17.8 18.1 18.0 Lattice type: P chosen Volume: 1284.66 #------------------------------------------------------------------------------ DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.580 12.068 19.407 100.59 90.00 90.00 Niggli form: a.a = 31.14 b.b = 145.63 c.c = 376.64 b.c = -43.04 a.c = 0.00 a.b = 0.00 #------------------------------------------------------------------------------ Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) #----------------------------------------------------------------------------- Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.018 [ 2486] Cell: 12.068 5.580 19.407 90.00 100.59 90.00 Volume: 1284.66 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected #------------------------------------------------------------------------------ SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4073 4079 4076 4077 6114 5435 5426 8147 N (int>3sigma) = 0 3354 2981 3327 3215 4831 4420 4442 6630 Mean intensity = 0.0 280.1 272.5 287.5 267.3 280.0 275.1 279.5 277.9 Mean int/sigma = 0.0 18.0 17.0 18.2 17.3 17.7 17.8 18.1 18.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.900 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 3 481 471 480 N I>3s 0 255 247 42 0.6 379.1 387.2 1.3 0.6 19.1 19.4 1.5 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.018 2486 1.5 / 18.0 1.40 [B] Pn # 7 non-cen 1 226 0.018 2486 1.5 / 18.0 3.75 [C] P2(1)/n # 14 centro 1 19410 0.018 2486 1.5 / 18.0 1.07 Option [C] chosen #------------------------------------------------------------------------------ INTENSITY STATISTICS FOR DATASET # 1 rhcg01.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 179 179 100.0 3.10 868.9 83.21 0.0131 0.0069 2.15 - 1.65 188 188 100.0 3.38 661.4 69.22 0.0150 0.0099 1.65 - 1.40 210 210 100.0 3.40 377.8 43.22 0.0207 0.0144 1.40 - 1.25 235 235 100.0 2.94 340.1 34.22 0.0248 0.0188 1.25 - 1.15 210 210 100.0 2.85 236.8 26.87 0.0246 0.0243 1.15 - 1.05 313 313 100.0 2.60 210.7 22.47 0.0261 0.0292 1.05 - 1.00 204 204 100.0 2.43 190.5 20.43 0.0249 0.0331 1.00 - 0.95 226 226 100.0 2.34 167.9 18.32 0.0264 0.0374 0.95 - 0.90 307 307 100.0 2.17 146.5 15.47 0.0280 0.0433 0.90 - 0.85 378 383 98.7 2.09 120.1 13.54 0.0306 0.0496 0.85 - 0.80 437 450 97.1 1.88 90.8 10.71 0.0373 0.0636 0.80 - 0.75 467 612 76.3 1.24 80.6 9.41 0.0433 0.0792 0.75 - 0.74 38 214 17.8 0.19 54.8 6.05 0.0303 0.1063 #----------------------------------------------------------------------------- 0.85 - 0.74 942 1276 73.8 1.29 84.3 9.88 0.0397 0.0721 Inf - 0.74 3392 3731 90.9 2.18 236.2 25.11 0.0211 0.0258 Merged [A], lowest resolution = 19.08 Angstroms, 153 outliers downweighted #TITL RHCG01 in P21/n solved dirdif #CELL 0.71073 12.0676 5.5804 19.4072 90.0000 100.5909 90.0000 #ZERR 4.000 0.0012 0.0006 0.0020 0.0015 0.0015 0.0013 #LATT +1 #SYMM 1/2-X , 1/2+Y , 1/2-Z #SFAC C H N O RH #UNIT 64 52 8 4 4 #TEMP -123 #L.S. 4 #ACTA #FMAP 2 #PLAN 10 #WGHT 0.026800 0.730800 #EXTI 0.000754 #FVAR 0.39906 #RH1 5 0.021108 0.085641 0.332340 11.00000 0.01522 0.01586 = #0.01906 0.00121 -0.00117 -0.00039 #N1 3 0.186833 0.127096 0.345828 11.00000 0.01662 0.01892 = #0.01911 -0.00154 0.00246 -0.00083 #C2 1 0.241480 0.297700 0.314757 11.00000 0.02769 0.02348 = #0.02295 0.00126 0.00532 -0.00281 #AFIX 43 #H2 2 0.198028 0.404147 0.282333 11.00000 -1.20000 #AFIX 0 #C3 1 0.355812 0.322732 0.328072 11.00000 0.02625 0.03118 = #0.02915 0.00048 0.01011 -0.00703 #AFIX 43 #H3 2 0.390781 0.443554 0.305006 11.00000 -1.20000 #AFIX 0 #C4 1 0.421477 0.167810 0.376320 11.00000 0.01796 0.03055 = #0.03275 -0.00583 0.00627 -0.00360 #AFIX 43 #H4 2 0.501160 0.184383 0.386622 11.00000 -1.20000 #AFIX 0 #C5 1 0.369687 -0.006268 0.408140 11.00000 0.01761 0.02433 = #0.02530 -0.00418 0.00277 0.00186 #AFIX 43 #H5 2 0.413461 -0.112199 0.440575 11.00000 -1.20000 #AFIX 0 #C6 1 0.251012 -0.029745 0.393039 11.00000 0.01811 0.01839 = #0.01864 -0.00338 0.00241 0.00085 #C7 1 0.183346 -0.195362 0.421345 11.00000 0.01622 0.01854 = #0.01914 -0.00281 0.00000 0.00121 #O9 4 0.074817 -0.173383 0.400127 11.00000 0.01546 0.01942 = #0.02229 0.00284 -0.00187 0.00054 #C9 1 0.219901 -0.391916 0.470457 11.00000 0.01990 0.01842 = #0.01859 -0.00256 0.00084 0.00365 #N10 3 0.329814 -0.409613 0.500560 11.00000 0.02114 0.02354 = #0.02767 0.00133 -0.00155 0.00300 #C11 1 0.359833 -0.595059 0.543654 11.00000 0.02328 0.02909 = #0.02613 0.00035 -0.00673 0.00760 #AFIX 43 #H11 2 0.437180 -0.610354 0.564403 11.00000 -1.20000 #AFIX 0 #C12 1 0.286246 -0.764956 0.559917 11.00000 0.03530 0.02355 = #0.01878 0.00203 -0.00019 0.00771 #AFIX 43 #H12 2 0.312254 -0.892835 0.591021 11.00000 -1.20000 #AFIX 0 #C13 1 0.173511 -0.745240 0.529925 11.00000 0.03144 0.02303 = #0.01871 -0.00036 0.00514 -0.00001 #AFIX 43 #H13 2 0.120177 -0.858631 0.540274 11.00000 -1.20000 #AFIX 0 #C14 1 0.140164 -0.557876 0.484754 11.00000 0.02068 0.02461 = #0.01788 -0.00193 0.00226 0.00276 #AFIX 43 #H14 2 0.063187 -0.541227 0.463324 11.00000 -1.20000 #AFIX 0 #C15 1 -0.076910 0.407859 0.305372 11.00000 0.03027 0.01625 = #0.05818 0.00414 -0.02054 0.00103 #AFIX 43 #H15 2 -0.050615 0.562565 0.320988 11.00000 -1.20000 #AFIX 0 #C16 1 -0.057839 0.291646 0.243369 11.00000 0.02158 0.04184 = #0.03787 0.02275 -0.00350 -0.00291 #AFIX 43 #H16 2 -0.014929 0.353644 0.210983 11.00000 -1.20000 #AFIX 0 #C17 1 -0.113519 0.068915 0.238275 11.00000 0.01865 0.03385 = #0.02113 -0.00202 -0.00318 0.00422 #AFIX 43 #H17 2 -0.118239 -0.042636 0.200870 11.00000 -1.20000 #AFIX 0 #C18 1 -0.161096 0.042126 0.299166 11.00000 0.01564 0.02258 = #0.02612 0.00404 -0.00096 0.00127 #AFIX 43 #H18 2 -0.199895 -0.095631 0.311003 11.00000 -1.20000 #AFIX 0 #C19 1 -0.141532 0.253533 0.339512 11.00000 0.02389 0.03339 = #0.02897 -0.00582 -0.00500 0.01187 #AFIX 43 #H19 2 -0.167309 0.285716 0.381979 11.00000 -1.20000 #HKLF 4 #REM RHCG01 in P21/n solved dirdif #REM R1 = 0.0270 for 2875 Fo > 4sig(Fo) and 0.0296 for all 3087 data #REM 182 parameters refined using 0 restraints #END #WGHT 0.0268 0.7338 #REM Highest difference peak 0.582, deepest hole -0.350, 1-sigma level 0.091 #Q1 1 0.0562 0.1042 0.2961 11.00000 0.05 0.58 #Q2 1 0.0614 0.1531 0.3044 11.00000 0.05 0.52 #Q3 1 -0.0209 0.1685 0.3571 11.00000 0.05 0.48 #Q4 1 0.0281 0.2479 0.3435 11.00000 0.05 0.47 #Q5 1 -0.0197 -0.0087 0.3537 11.00000 0.05 0.44 #Q6 1 -0.1718 0.1795 0.3157 11.00000 0.05 0.43 #Q7 1 0.2350 -0.7769 0.5341 11.00000 0.05 0.43 #Q8 1 0.3993 0.0583 0.3842 11.00000 0.05 0.40 #Q9 1 0.3249 -0.7267 0.5369 11.00000 0.05 0.39 #Q10 1 0.2214 -0.1380 0.4002 11.00000 0.05 0.37 #=============================================================================== # PLATON/CHECK-(191101) versus check.def version of 16/11/01 for entry: rhcg01 # Data From: rhcg01.cif - Data Type: CIF Bond Precision C-C = 0.0035 A # # CELL 0.71073 12.068 5.580 19.407 90.00 100.59 90.00 1284.60 # SpaceGroup from Symmetry P21/n Hall: -P 2yn # Reported P21/n ? # MoietyFormula C16 H13 N2 O Rh # Reported [CPRH(PYRCOPRY)] # SumFormula C16 H13 N2 O Rh # Reported C16 H13 N2 O Rh # Mr = 352.19[Calc], 352.19[Rep] # Dx,gcm-3 = 1.821[Calc], 1.821[Rep] # Z = 4[Calc], 4[Rep] # Mu (mm-1) = 1.325[Calc], 1.324[Rep] # F000 = 704.0[Calc], 704.0[Rep] # Reported T limits: Tmin=0.672 Tmax=0.862 'MULTISCAN' # Calculated T limits: Tmin=0.701 Tmin'=0.469 Tmax=0.842 # Reported Hmax= 15, Kmax= 7, Lmax= 25, Nref= 3087 , Th(max)= 28.89 # Calculated Hmax= 16, Kmax= 7, Lmax= 26, Nref= 3388( 3388), Ratio= 0.91( 0.91) # R= 0.0270( 2875), wR2= 0.0636( 3087), S = 1.115, Npar= 182 #=============================================================================== >>> The Following ALERTS were generated <<< 761_ALERT A CIF Contains no X-H Bonds .................... ? 762_ALERT A CIF Contains no X-Y-H or H-Y-H Angles ........ ? The H's were placed in calculated positions. #=============================================================================== 042_ALERT C Calc. and Rep. MoietyFormula Strings Differ .. ? 062_ALERT C Rescale T(min) & T(max) by ................... 0.98 125_ALERT C No _symmetry_space_group_name_Hall given ..... ? 128_ALERT C Non-standard setting of space group P21/c .. P21/n 145_ALERT C su on beta Small or Missing (x 10000) ... 15 Deg. No major problems here. ALERT Level Summary 2 ALERT Level A = In General: Serious Problem 5 ALERT Level C = Check & Explain #=============================================================================== ; _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^)+(0.0268P)^2^+0.7308P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3087 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Rh1 Rh 0.021108(13) 0.08564(3) 0.332340(9) 0.01726(7) Uani 1 1 d . . . N1 N 0.18683(16) 0.1271(3) 0.34583(10) 0.0183(4) Uani 1 1 d . . . C2 C 0.2415(2) 0.2977(5) 0.31476(13) 0.0246(5) Uani 1 1 d . . . H2 H 0.1980 0.4041 0.2823 0.030 Uiso 1 1 calc R . . C3 C 0.3558(2) 0.3227(5) 0.32807(14) 0.0282(6) Uani 1 1 d . . . H3 H 0.3908 0.4436 0.3050 0.034 Uiso 1 1 calc R . . C4 C 0.4215(2) 0.1678(5) 0.37632(14) 0.0269(5) Uani 1 1 d . . . H4 H 0.5012 0.1844 0.3866 0.032 Uiso 1 1 calc R . . C5 C 0.36969(19) -0.0063(5) 0.40814(13) 0.0226(5) Uani 1 1 d . . . H5 H 0.4135 -0.1122 0.4406 0.027 Uiso 1 1 calc R . . C6 C 0.25101(19) -0.0297(4) 0.39304(12) 0.0185(5) Uani 1 1 d . . . C7 C 0.18335(18) -0.1954(4) 0.42134(12) 0.0184(5) Uani 1 1 d . . . O9 O 0.07482(13) -0.1734(3) 0.40013(8) 0.0197(3) Uani 1 1 d . . . C9 C 0.21990(19) -0.3919(4) 0.47046(12) 0.0193(5) Uani 1 1 d . . . N10 N 0.32981(17) -0.4096(4) 0.50056(11) 0.0249(5) Uani 1 1 d . . . C11 C 0.3598(2) -0.5951(5) 0.54365(14) 0.0276(6) Uani 1 1 d . . . H11 H 0.4372 -0.6104 0.5644 0.033 Uiso 1 1 calc R . . C12 C 0.2862(2) -0.7650(5) 0.55992(13) 0.0265(5) Uani 1 1 d . . . H12 H 0.3123 -0.8928 0.5910 0.032 Uiso 1 1 calc R . . C13 C 0.1735(2) -0.7452(5) 0.52992(12) 0.0243(5) Uani 1 1 d . . . H13 H 0.1202 -0.8586 0.5403 0.029 Uiso 1 1 calc R . . C14 C 0.1402(2) -0.5579(4) 0.48475(12) 0.0212(5) Uani 1 1 d . . . H14 H 0.0632 -0.5412 0.4633 0.025 Uiso 1 1 calc R . . C15 C -0.0769(2) 0.4079(5) 0.30537(18) 0.0385(8) Uani 1 1 d . . . H15 H -0.0506 0.5626 0.3210 0.046 Uiso 1 1 calc R . . C16 C -0.0578(2) 0.2916(5) 0.24337(15) 0.0349(7) Uani 1 1 d . . . H16 H -0.0149 0.3536 0.2110 0.042 Uiso 1 1 calc R . . C17 C -0.1135(2) 0.0689(5) 0.23827(13) 0.0254(5) Uani 1 1 d . . . H17 H -0.1182 -0.0426 0.2009 0.030 Uiso 1 1 calc R . . C18 C -0.16110(19) 0.0421(4) 0.29917(13) 0.0221(5) Uani 1 1 d . . . H18 H -0.1999 -0.0956 0.3110 0.026 Uiso 1 1 calc R . . C19 C -0.1415(2) 0.2535(5) 0.33951(14) 0.0300(6) Uani 1 1 d . . . H19 H -0.1673 0.2857 0.3820 0.036 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 Rh1 0.01522(11) 0.01586(11) 0.01906(11) 0.00121(7) -0.00117(7) -0.00039(6) N1 0.0166(9) 0.0189(10) 0.0191(10) -0.0015(8) 0.0025(7) -0.0008(7) C2 0.0277(12) 0.0235(13) 0.0229(12) 0.0013(10) 0.0053(10) -0.0028(10) C3 0.0262(13) 0.0312(14) 0.0291(14) 0.0005(11) 0.0101(10) -0.0070(10) C4 0.0180(11) 0.0305(14) 0.0328(14) -0.0058(11) 0.0063(10) -0.0036(10) C5 0.0176(11) 0.0243(12) 0.0253(13) -0.0042(10) 0.0028(9) 0.0019(9) C6 0.0181(11) 0.0184(11) 0.0186(11) -0.0034(9) 0.0024(9) 0.0008(8) C7 0.0162(10) 0.0185(12) 0.0191(11) -0.0028(9) 0.0000(8) 0.0012(8) O9 0.0155(7) 0.0194(8) 0.0223(8) 0.0028(7) -0.0019(6) 0.0005(6) C9 0.0199(11) 0.0184(12) 0.0186(11) -0.0026(9) 0.0008(9) 0.0036(8) N10 0.0211(10) 0.0235(11) 0.0277(11) 0.0013(8) -0.0016(8) 0.0030(8) C11 0.0233(12) 0.0291(14) 0.0261(13) 0.0003(10) -0.0067(10) 0.0076(10) C12 0.0353(14) 0.0235(13) 0.0188(12) 0.0020(10) -0.0002(10) 0.0077(11) C13 0.0314(13) 0.0230(12) 0.0187(11) -0.0004(10) 0.0051(10) 0.0000(10) C14 0.0207(11) 0.0246(13) 0.0179(11) -0.0019(9) 0.0023(9) 0.0028(9) C15 0.0303(14) 0.0163(13) 0.058(2) 0.0041(12) -0.0205(14) 0.0010(10) C16 0.0216(12) 0.0418(17) 0.0379(16) 0.0227(13) -0.0035(11) -0.0029(11) C17 0.0187(11) 0.0339(15) 0.0211(12) -0.0020(10) -0.0032(9) 0.0042(10) C18 0.0156(11) 0.0226(12) 0.0261(13) 0.0040(10) -0.0010(9) 0.0013(9) C19 0.0239(12) 0.0334(15) 0.0290(13) -0.0058(11) -0.0050(10) 0.0119(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O9 1.9816(16) . ? Rh1 N1 1.9822(19) . ? Rh1 C16 2.146(3) . ? Rh1 C15 2.163(3) . ? Rh1 C18 2.188(2) . ? Rh1 C19 2.202(2) . ? Rh1 C17 2.211(2) . ? N1 C2 1.361(3) . ? N1 C6 1.394(3) . ? C2 C3 1.363(3) . ? C3 C4 1.407(4) . ? C4 C5 1.363(4) . ? C5 C6 1.414(3) . ? C6 C7 1.410(3) . ? C7 O9 1.304(3) . ? C7 C9 1.467(3) . ? C9 N10 1.351(3) . ? C9 C14 1.400(3) . ? N10 C11 1.338(3) . ? C11 C12 1.375(4) . ? C12 C13 1.382(3) . ? C13 C14 1.376(3) . ? C15 C19 1.407(4) . ? C15 C16 1.422(5) . ? C16 C17 1.408(4) . ? C17 C18 1.413(4) . ? C18 C19 1.412(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Rh1 N1 78.38(7) . . ? O9 Rh1 C16 165.36(10) . . ? N1 Rh1 C16 109.37(9) . . ? O9 Rh1 C15 149.84(11) . . ? N1 Rh1 C15 115.37(10) . . ? C16 Rh1 C15 38.55(12) . . ? O9 Rh1 C18 107.62(8) . . ? N1 Rh1 C18 170.65(9) . . ? C16 Rh1 C18 63.21(10) . . ? C15 Rh1 C18 62.99(10) . . ? O9 Rh1 C19 117.06(9) . . ? N1 Rh1 C19 146.23(9) . . ? C16 Rh1 C19 63.51(11) . . ? C15 Rh1 C19 37.58(12) . . ? C18 Rh1 C19 37.51(9) . . ? O9 Rh1 C17 128.19(8) . . ? N1 Rh1 C17 133.17(9) . . ? C16 Rh1 C17 37.66(10) . . ? C15 Rh1 C17 63.21(10) . . ? C18 Rh1 C17 37.48(9) . . ? C19 Rh1 C17 62.75(10) . . ? C2 N1 C6 118.3(2) . . ? C2 N1 Rh1 125.63(16) . . ? C6 N1 Rh1 116.01(15) . . ? N1 C2 C3 122.9(2) . . ? C2 C3 C4 119.3(2) . . ? C5 C4 C3 119.4(2) . . ? C4 C5 C6 120.2(2) . . ? N1 C6 C7 112.08(19) . . ? N1 C6 C5 119.8(2) . . ? C7 C6 C5 128.1(2) . . ? O9 C7 C6 115.8(2) . . ? O9 C7 C9 116.1(2) . . ? C6 C7 C9 128.1(2) . . ? C7 O9 Rh1 117.71(15) . . ? N10 C9 C14 121.5(2) . . ? N10 C9 C7 119.3(2) . . ? C14 C9 C7 119.2(2) . . ? C11 N10 C9 117.3(2) . . ? N10 C11 C12 124.4(2) . . ? C11 C12 C13 118.4(2) . . ? C14 C13 C12 118.6(2) . . ? C13 C14 C9 119.9(2) . . ? C19 C15 C16 108.0(2) . . ? C19 C15 Rh1 72.72(15) . . ? C16 C15 Rh1 70.09(15) . . ? C17 C16 C15 108.2(2) . . ? C17 C16 Rh1 73.69(15) . . ? C15 C16 Rh1 71.37(15) . . ? C16 C17 C18 107.3(2) . . ? C16 C17 Rh1 68.65(14) . . ? C18 C17 Rh1 70.36(14) . . ? C19 C18 C17 108.9(2) . . ? C19 C18 Rh1 71.79(14) . . ? C17 C18 Rh1 72.16(13) . . ? C15 C19 C18 107.5(3) . . ? C15 C19 Rh1 69.70(15) . . ? C18 C19 Rh1 70.70(14) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.89 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.582 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.091