#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515787.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4515787 loop_ _publ_author_name 'Messinis, Antonis M.' 'Wright, William R. H.' 'Batsanov, Andrei S.' 'Howard, Judith A. K.' 'Hanton, Martin J.' 'Dyer, Philip W.' _publ_section_title ; Exploration of Homogeneous Ethylene Dimerization Mediated by Tungsten Mono(imido) Complexes ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11235 _journal_paper_doi 10.1021/acscatal.8b02201 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C21 H45 Cl N P3 W' _chemical_formula_sum 'C21 H45 Cl N P3 W' _chemical_formula_weight 623.79 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_date 2016-11-30 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.7347(5) _cell_length_b 13.6973(4) _cell_length_c 12.7686(4) _cell_measurement_reflns_used 18327 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 32.3027 _cell_measurement_theta_min 2.5837 _cell_volume 2751.93(15) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction 'CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (2011)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2014/7 multi-CPU version (Sheldrick, 2015)' _computing_structure_solution 'SHELXS 2013/1 (Sheldrick, 2008)' _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 16.15 _diffrn_detector_type 'Sapphire3 CCD area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -98.00 -35.90 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 -38.0000 -60.0000 207 #__ type_ start__ end____ width___ exp.time_ 2 omega -43.00 42.20 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 38.0000 120.0000 284 #__ type_ start__ end____ width___ exp.time_ 3 omega -89.00 -62.00 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 -162.0000 -64.0000 90 #__ type_ start__ end____ width___ exp.time_ 4 omega 44.00 91.10 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - 26.1780 -138.0000 -170.0000 157 #__ type_ start__ end____ width___ exp.time_ 5 omega 63.00 91.80 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - 26.1780 -162.0000 -64.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega -38.00 19.00 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - 26.1780 -57.0000 -150.0000 190 #__ type_ start__ end____ width___ exp.time_ 7 omega -96.00 3.90 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 -77.0000 150.0000 333 #__ type_ start__ end____ width___ exp.time_ 8 omega -98.00 -1.10 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 -38.0000 0.0000 323 #__ type_ start__ end____ width___ exp.time_ 9 omega -94.00 -4.00 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 -57.0000 -150.0000 300 #__ type_ start__ end____ width___ exp.time_ 10 omega -47.00 43.00 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - -25.3968 57.0000 -60.0000 300 #__ type_ start__ end____ width___ exp.time_ 11 omega 53.00 101.90 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - 26.1780 -179.0000 60.0000 163 #__ type_ start__ end____ width___ exp.time_ 12 omega -43.00 35.00 0.3000 2.6700 omega____ theta____ kappa____ phi______ frames - 26.1780 -57.0000 0.0000 260 ; _diffrn_measurement_device_type 'Agilent Technologies, Gemini S Ultra kappa-diffractometer' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0054164000 _diffrn_orient_matrix_UB_12 -0.0287139000 _diffrn_orient_matrix_UB_13 -0.0395797000 _diffrn_orient_matrix_UB_21 0.0049671000 _diffrn_orient_matrix_UB_22 -0.0342011000 _diffrn_orient_matrix_UB_23 0.0333938000 _diffrn_orient_matrix_UB_31 -0.0550690000 _diffrn_orient_matrix_UB_32 -0.0060629000 _diffrn_orient_matrix_UB_33 -0.0008778000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_unetI/netI 0.0330 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.948 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 51754 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.948 _diffrn_reflns_theta_full 30.000 _diffrn_reflns_theta_max 32.376 _diffrn_reflns_theta_min 2.974 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.476 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'greenish black' _exptl_crystal_density_diffrn 1.506 _exptl_crystal_description brick _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.319 _exptl_crystal_size_min 0.313 _refine_diff_density_max 4.043 _refine_diff_density_min -5.494 _refine_diff_density_rms 0.252 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.386 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 184 _refine_ls_number_reflns 4846 _refine_ls_number_restraints 150 _refine_ls_restrained_S_all 1.368 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0545 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+41.7180P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1297 _refine_ls_wR_factor_ref 0.1311 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4561 _reflns_number_total 4846 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b02201_si_002.cif _cod_data_source_block 5 _cod_database_code 4515787 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 29.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All W(H) groups At 1.5 times of: All C(H,H) groups, All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C14A) = Uanis(C14B) 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Uiso(H8A)=Uiso(H8B)=Uiso(H8C)=FVAR(1) Uiso(H10A)=Uiso(H10B)=Uiso(H10C)=FVAR(2) Fixed Sof: P2B(0.25) C11B(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C12B(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C13B(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14B(0.25) H14A(0.5) H14B(0.25) C15B(0.5) H15A(0.5) H15B(0.5) H15C(0.5) P2A(0.25) C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5) C14A(0.25) H14C(0.5) H14D(0.25) C15A(0.5) H15D(0.5) H15E(0.5) H15F(0.5) 5.a Riding coordinates: W(H0), C11B(H11A,H11B,H11C), C12B(H12A,H12B,H12C), C13B(H13A,H13B,H13C), C14B(H14A,H14B), C15B(H15A,H15B,H15C), C11A(H11D,H11E,H11F), C12A(H12D,H12E, H12F), C13A(H13D,H13E,H13F), C14A(H14C,H14D), C15A(H15D,H15E,H15F) 5.b Ternary CH refined with riding coordinates: C7(H7), C9(H9) 5.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5) 5.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C10(H10A,H10B,H10C) ; _shelx_res_file ; 12srv061.res created by SHELXL-2014/7 TITL 12srv061 in Pnma #62 REM reset to Pnma #62 CELL 0.71073 15.7347 13.6973 12.7686 90 90 90 ZERR 4 0.0005 0.0004 0.0004 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM -X,0.5+Y,-Z SFAC C H Cl N P W UNIT 84 180 4 4 12 4 RIGU EADP C14A C14B L.S. 7 PLAN 20 TEMP -153.15 BOND fmap 2 acta 60 OMIT 7 4 1 OMIT 1 1 4 OMIT 1 0 5 OMIT 2 0 0 REM REM REM WGHT 0.000000 41.717999 FVAR 0.05721 0.04714 0.05024 W 6 0.262913 0.750000 0.818887 10.50000 0.01577 0.01114 = 0.01123 0.00000 0.00248 0.00000 AFIX 3 H0 2 0.364583 0.750000 0.820937 10.50000 -1.20000 AFIX 0 CL 3 0.318015 0.750000 0.632690 10.50000 0.02991 0.02323 = 0.01448 0.00000 0.00834 0.00000 P1 5 0.278687 0.929000 0.808466 11.00000 0.02922 0.01272 = 0.02447 0.00290 -0.00021 -0.00168 PART 2 P2B 5 0.113482 0.750000 0.733105 10.25000 0.01764 PART 0 N 4 0.234207 0.750000 0.953326 10.50000 0.01908 0.00841 = 0.01807 0.00000 0.00127 0.00000 C1 1 0.224014 0.750000 1.061692 10.50000 0.02996 0.00899 = 0.01505 0.00000 0.00471 0.00000 C2 1 0.144657 0.750000 1.106028 10.50000 0.02595 0.01373 = 0.01619 0.00000 0.00558 0.00000 C3 1 0.134194 0.750000 1.215159 10.50000 0.02970 0.01983 = 0.01848 0.00000 0.00618 0.00000 AFIX 43 H3 2 0.078645 0.750000 1.244308 10.50000 -1.20000 AFIX 0 C4 1 0.203887 0.750000 1.280184 10.50000 0.03919 0.01685 = 0.01762 0.00000 0.00249 0.00000 AFIX 43 H4 2 0.196013 0.750000 1.353949 10.50000 -1.20000 AFIX 0 C5 1 0.286906 0.750000 1.238553 10.50000 0.03059 0.02138 = 0.01529 0.00000 0.00654 0.00000 AFIX 43 H5 2 0.335119 0.750000 1.283338 10.50000 -1.20000 AFIX 0 C6 1 0.296405 0.750000 1.130112 10.50000 0.03592 0.01588 = 0.01410 0.00000 0.00589 0.00000 C7 1 0.062955 0.750000 1.039383 10.50000 0.02953 0.03688 = 0.01608 0.00000 0.00628 0.00000 AFIX 13 H7 2 0.081123 0.749999 0.964334 10.50000 -1.20000 AFIX 0 C8 1 0.009567 0.842175 1.056122 11.00000 0.03865 0.05091 = 0.03328 -0.00128 0.00393 0.01338 AFIX 137 H8A 2 -0.010472 0.844325 1.128755 11.00000 21.00000 H8B 2 -0.039350 0.841211 1.008626 11.00000 21.00000 H8C 2 0.044361 0.899973 1.041698 11.00000 21.00000 AFIX 0 C9 1 0.387226 0.750000 1.086222 10.50000 0.02704 0.03120 = 0.01548 0.00000 0.00039 0.00000 AFIX 13 H9 2 0.383911 0.749998 1.008011 10.50000 -1.20000 AFIX 0 C10 1 0.435058 0.841666 1.121059 11.00000 0.03390 0.03808 = 0.03447 0.00270 0.00140 -0.00789 AFIX 137 H10A 2 0.436534 0.844388 1.197732 11.00000 31.00000 H10B 2 0.406015 0.899685 1.093928 11.00000 31.00000 H10C 2 0.493263 0.839640 1.093830 11.00000 31.00000 AFIX 0 PART 2 C11B 1 0.218499 0.997792 0.895216 10.50000 0.05101 0.01768 = 0.03132 -0.00332 0.00514 0.00170 AFIX 3 H11A 2 0.159309 0.986691 0.881346 10.50000 -1.50000 H11B 2 0.231269 1.065742 0.885666 10.50000 -1.50000 H11C 2 0.231189 0.979141 0.965986 10.50000 -1.50000 AFIX 0 C12B 1 0.255723 0.986938 0.678356 10.50000 0.04697 0.01440 = 0.02431 0.00576 0.00430 0.00068 AFIX 3 H12A 2 0.291723 0.957608 0.626426 10.50000 -1.50000 H12B 2 0.267573 1.055568 0.682526 10.50000 -1.50000 H12C 2 0.197293 0.977398 0.659336 10.50000 -1.50000 AFIX 0 C13B 1 0.388516 0.971387 0.823212 10.50000 0.03992 0.03037 = 0.05408 0.01178 -0.00662 -0.00916 AFIX 3 H13A 2 0.407356 0.954237 0.892322 10.50000 -1.50000 H13B 2 0.390686 1.041017 0.814942 10.50000 -1.50000 H13C 2 0.424816 0.941107 0.772262 10.50000 -1.50000 AFIX 0 C14B 1 0.108054 0.750000 0.589107 10.25000 0.02953 0.05763 = 0.01202 0.00000 -0.01397 0.00000 AFIX 3 H14A 2 0.137264 0.808470 0.563407 10.50000 -1.50000 H14B 2 0.049264 0.750000 0.563737 10.25000 -1.50000 AFIX 0 C15B 1 0.043172 0.852117 0.760064 10.50000 0.01928 0.02381 = 0.03769 0.00370 -0.00342 0.00089 AFIX 3 H15A 2 0.043602 0.866197 0.833714 10.50000 -1.50000 H15B 2 -0.013678 0.836537 0.738404 10.50000 -1.50000 H15C 2 0.062952 0.908107 0.721964 10.50000 -1.50000 AFIX 0 PART 0 PART 1 P2A 5 0.132405 0.750000 0.711664 10.25000 0.02072 C11A 1 0.183441 0.998006 0.864172 10.50000 0.03206 0.02344 = 0.02150 0.00098 -0.00388 0.00776 AFIX 3 H11D 2 0.135431 0.989836 0.818632 10.50000 -1.50000 H11E 2 0.197891 1.065986 0.868392 10.50000 -1.50000 H11F 2 0.169511 0.974126 0.932752 10.50000 -1.50000 AFIX 0 C12A 1 0.306255 0.986993 0.693044 10.50000 0.04510 0.01637 = 0.02467 0.00352 0.00214 -0.00389 AFIX 3 H12D 2 0.361205 0.963743 0.672014 10.50000 -1.50000 H12E 2 0.308805 1.056183 0.704704 10.50000 -1.50000 H12F 2 0.265615 0.973213 0.638984 10.50000 -1.50000 AFIX 0 C13A 1 0.358139 0.983391 0.901403 10.50000 0.03394 0.02297 = 0.02883 -0.00278 -0.00046 0.00116 AFIX 3 H13D 2 0.336049 0.980671 0.971413 10.50000 -1.50000 H13E 2 0.369529 1.050081 0.882913 10.50000 -1.50000 H13F 2 0.409809 0.946261 0.897593 10.50000 -1.50000 AFIX 0 C14A 1 0.030876 0.750000 0.780989 10.25000 0.02953 0.05763 = 0.01202 0.00000 -0.01397 0.00000 AFIX 3 H14C 2 0.026536 0.808080 0.825489 10.50000 -1.50000 H14D 2 -0.014984 0.750000 0.729069 10.25000 -1.50000 AFIX 0 C15A 1 0.116906 0.851729 0.619126 10.50000 0.04407 0.04345 = 0.02821 0.00968 -0.01350 0.01060 AFIX 3 H15D 2 0.114386 0.911719 0.657857 10.50000 -1.50000 H15E 2 0.064736 0.842729 0.581366 10.50000 -1.50000 H15F 2 0.163486 0.854219 0.570626 10.50000 -1.50000 AFIX 0 HKLF 4 REM 12srv061 in Pnma #62 REM R1 = 0.0545 for 4561 Fo > 4sig(Fo) and 0.0577 for all 4846 data REM 184 parameters refined using 150 restraints END WGHT 0.0000 41.6805 REM Highest difference peak 4.043, deepest hole -5.494, 1-sigma level 0.252 Q1 1 0.3118 0.7500 0.8195 10.50000 0.05 4.04 Q2 1 0.2978 0.7500 0.5362 10.50000 0.05 4.04 Q3 1 0.2324 0.7500 0.5408 10.50000 0.05 3.69 Q4 1 0.2634 0.7500 1.0977 10.50000 0.05 3.31 Q5 1 0.2100 0.7500 0.7853 10.50000 0.05 2.56 Q6 1 0.2033 0.7500 0.8598 10.50000 0.05 2.15 Q7 1 0.1202 0.7500 1.0006 10.50000 0.05 1.89 Q8 1 0.2016 0.7500 1.1037 10.50000 0.05 1.85 Q9 1 0.2672 0.7500 1.3974 10.50000 0.05 1.84 Q10 1 0.3386 0.9304 0.8154 11.00000 0.05 1.62 Q11 1 0.3537 0.7500 0.7205 10.50000 0.05 1.57 Q12 1 0.1689 0.7500 0.7634 10.50000 0.05 1.53 Q13 1 0.2304 0.7500 1.2274 10.50000 0.05 1.46 Q14 1 0.3720 0.7500 0.6367 10.50000 0.05 1.39 Q15 1 0.1121 0.7500 1.2750 10.50000 0.05 1.38 Q16 1 0.1822 0.7500 0.6954 10.50000 0.05 1.35 Q17 1 0.1263 0.7500 0.9124 10.50000 0.05 1.35 Q18 1 0.0818 0.7500 0.6458 10.50000 0.05 1.26 Q19 1 0.2901 0.7885 0.8783 11.00000 0.05 1.21 Q20 1 0.1516 0.7500 1.3716 10.50000 0.05 1.19 ; _shelx_res_checksum 43519 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W W 0.26291(2) 0.7500 0.81889(3) 0.01272(9) Uani 1 2 d S TU P A . H0 H 0.3646 0.7500 0.8209 0.015 Uiso 1 2 d RS T P A . Cl Cl 0.31801(16) 0.7500 0.63269(17) 0.0225(4) Uani 1 2 d S TU P A . P1 P 0.27869(12) 0.92900(12) 0.80847(14) 0.0221(3) Uani 1 1 d . U . . . P2B P 0.1135(4) 0.7500 0.7331(5) 0.0176(11) Uiso 0.5 2 d S TU P A 2 N N 0.2342(5) 0.7500 0.9533(6) 0.0152(12) Uani 1 2 d S TU P A . C1 C 0.2240(6) 0.7500 1.0617(7) 0.0180(14) Uani 1 2 d S TU P . . C2 C 0.1447(6) 0.7500 1.1060(7) 0.0186(15) Uani 1 2 d S TU P A . C3 C 0.1342(7) 0.7500 1.2152(7) 0.0227(17) Uani 1 2 d S TU P . . H3 H 0.0786 0.7500 1.2443 0.027 Uiso 1 2 calc RS T P A . C4 C 0.2039(7) 0.7500 1.2802(8) 0.0246(17) Uani 1 2 d S TU P A . H4 H 0.1960 0.7500 1.3539 0.029 Uiso 1 2 calc RS T P . . C5 C 0.2869(7) 0.7500 1.2386(7) 0.0224(17) Uani 1 2 d S TU P . . H5 H 0.3351 0.7500 1.2833 0.027 Uiso 1 2 calc RS T P A . C6 C 0.2964(7) 0.7500 1.1301(7) 0.0220(16) Uani 1 2 d S TU P A . C7 C 0.0630(7) 0.7500 1.0394(8) 0.0275(19) Uani 1 2 d S TU P . . H7 H 0.0811 0.7500 0.9643 0.033 Uiso 1 2 calc RS T P A . C8 C 0.0096(6) 0.8422(7) 1.0561(7) 0.041(2) Uani 1 1 d . U . . . H8A H -0.0105 0.8443 1.1288 0.047(18) Uiso 1 1 calc GR . . . . H8B H -0.0393 0.8412 1.0086 0.047(18) Uiso 1 1 calc GR . . . . H8C H 0.0444 0.9000 1.0417 0.047(18) Uiso 1 1 calc GR . . . . C9 C 0.3872(7) 0.7500 1.0862(8) 0.0246(18) Uani 1 2 d S TU P . . H9 H 0.3839 0.7500 1.0080 0.029 Uiso 1 2 calc RS T P A . C10 C 0.4351(6) 0.8417(6) 1.1211(7) 0.0355(17) Uani 1 1 d . U . . . H10A H 0.4365 0.8444 1.1977 0.050(18) Uiso 1 1 calc GR . . . . H10B H 0.4060 0.8997 1.0939 0.050(18) Uiso 1 1 calc GR . . . . H10C H 0.4933 0.8396 1.0938 0.050(18) Uiso 1 1 calc GR . . . . C11B C 0.2185(13) 0.9978(12) 0.8952(14) 0.033(3) Uani 0.5 1 d . U . B 2 H11A H 0.1593 0.9867 0.8813 0.050 Uiso 0.5 1 d R . . B 2 H11B H 0.2313 1.0657 0.8857 0.050 Uiso 0.5 1 d R . . B 2 H11C H 0.2312 0.9791 0.9660 0.050 Uiso 0.5 1 d R . . B 2 C12B C 0.2557(12) 0.9869(10) 0.6784(12) 0.029(3) Uani 0.5 1 d . U . B 2 H12A H 0.2917 0.9576 0.6264 0.043 Uiso 0.5 1 d R . . B 2 H12B H 0.2676 1.0556 0.6825 0.043 Uiso 0.5 1 d R . . B 2 H12C H 0.1973 0.9774 0.6593 0.043 Uiso 0.5 1 d R . . B 2 C13B C 0.3885(11) 0.9714(13) 0.8232(17) 0.041(4) Uani 0.5 1 d . U . B 2 H13A H 0.4074 0.9542 0.8923 0.062 Uiso 0.5 1 d R . . B 2 H13B H 0.3907 1.0410 0.8149 0.062 Uiso 0.5 1 d R . . B 2 H13C H 0.4248 0.9411 0.7723 0.062 Uiso 0.5 1 d R . . B 2 C14B C 0.1081(15) 0.7500 0.5891(15) 0.033(4) Uani 0.5 2 d S TU P A 2 H14A H 0.1373 0.8085 0.5634 0.050 Uiso 0.5 1 d R . . A 2 H14B H 0.0493 0.7500 0.5637 0.050 Uiso 0.5 2 d RS T P A 2 C15B C 0.0432(9) 0.8521(10) 0.7601(13) 0.027(3) Uani 0.5 1 d . U . A 2 H15A H 0.0436 0.8662 0.8337 0.040 Uiso 0.5 1 d R . . A 2 H15B H -0.0137 0.8365 0.7384 0.040 Uiso 0.5 1 d R . . A 2 H15C H 0.0630 0.9081 0.7220 0.040 Uiso 0.5 1 d R . . A 2 P2A P 0.1324(4) 0.7500 0.7117(5) 0.0207(12) Uiso 0.5 2 d S TU P A 1 C11A C 0.1834(11) 0.9980(12) 0.8642(12) 0.026(3) Uani 0.5 1 d . U . B 1 H11D H 0.1354 0.9898 0.8186 0.039 Uiso 0.5 1 d R . . B 1 H11E H 0.1979 1.0660 0.8684 0.039 Uiso 0.5 1 d R . . B 1 H11F H 0.1695 0.9741 0.9328 0.039 Uiso 0.5 1 d R . . B 1 C12A C 0.3063(12) 0.9870(10) 0.6930(12) 0.029(3) Uani 0.5 1 d . U . B 1 H12D H 0.3612 0.9637 0.6720 0.043 Uiso 0.5 1 d R . . B 1 H12E H 0.3088 1.0562 0.7047 0.043 Uiso 0.5 1 d R . . B 1 H12F H 0.2656 0.9732 0.6390 0.043 Uiso 0.5 1 d R . . B 1 C13A C 0.3581(10) 0.9834(11) 0.9014(12) 0.029(3) Uani 0.5 1 d . U . B 1 H13D H 0.3360 0.9807 0.9714 0.043 Uiso 0.5 1 d R . . B 1 H13E H 0.3695 1.0501 0.8829 0.043 Uiso 0.5 1 d R . . B 1 H13F H 0.4098 0.9463 0.8976 0.043 Uiso 0.5 1 d R . . B 1 C14A C 0.0309(14) 0.7500 0.7810(16) 0.033(4) Uani 0.5 2 d S TU P A 1 H14C H 0.0265 0.8081 0.8255 0.050 Uiso 0.5 1 d R . . A 1 H14D H -0.0150 0.7500 0.7291 0.050 Uiso 0.5 2 d RS T P A 1 C15A C 0.1169(12) 0.8517(14) 0.6191(13) 0.039(4) Uani 0.5 1 d . U . A 1 H15D H 0.1144 0.9117 0.6579 0.058 Uiso 0.5 1 d R . . A 1 H15E H 0.0647 0.8427 0.5814 0.058 Uiso 0.5 1 d R . . A 1 H15F H 0.1635 0.8542 0.5706 0.058 Uiso 0.5 1 d R . . A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.01577(15) 0.01114(14) 0.01123(14) 0.000 0.00248(11) 0.000 Cl 0.0299(11) 0.0232(10) 0.0145(9) 0.000 0.0083(8) 0.000 P1 0.0292(9) 0.0127(7) 0.0245(8) 0.0029(6) -0.0002(7) -0.0017(6) N 0.019(3) 0.008(3) 0.018(3) 0.000 0.001(2) 0.000 C1 0.030(3) 0.009(3) 0.015(3) 0.000 0.005(2) 0.000 C2 0.026(3) 0.014(3) 0.016(3) 0.000 0.006(2) 0.000 C3 0.030(4) 0.020(4) 0.018(3) 0.000 0.006(3) 0.000 C4 0.039(4) 0.017(4) 0.018(3) 0.000 0.002(3) 0.000 C5 0.031(4) 0.021(4) 0.015(3) 0.000 0.007(3) 0.000 C6 0.036(4) 0.016(4) 0.014(3) 0.000 0.006(3) 0.000 C7 0.030(4) 0.037(5) 0.016(4) 0.000 0.006(3) 0.000 C8 0.039(4) 0.051(5) 0.033(4) -0.001(4) 0.004(4) 0.013(4) C9 0.027(4) 0.031(4) 0.015(4) 0.000 0.000(3) 0.000 C10 0.034(4) 0.038(4) 0.034(4) 0.003(3) 0.001(3) -0.008(3) C11B 0.051(8) 0.018(6) 0.031(7) -0.003(5) 0.005(6) 0.002(6) C12B 0.047(8) 0.014(5) 0.024(5) 0.006(4) 0.004(5) 0.001(6) C13B 0.040(6) 0.030(7) 0.054(9) 0.012(7) -0.007(6) -0.009(5) C14B 0.030(8) 0.058(10) 0.012(6) 0.000 -0.014(6) 0.000 C15B 0.019(6) 0.024(6) 0.038(8) 0.004(6) -0.003(6) 0.001(5) C11A 0.032(6) 0.023(6) 0.022(6) 0.001(5) -0.004(5) 0.008(5) C12A 0.045(8) 0.016(5) 0.025(5) 0.004(4) 0.002(5) -0.004(6) C13A 0.034(6) 0.023(6) 0.029(6) -0.003(5) 0.000(5) 0.001(5) C14A 0.030(8) 0.058(10) 0.012(6) 0.000 -0.014(6) 0.000 C15A 0.044(10) 0.043(10) 0.028(8) 0.010(7) -0.014(7) 0.011(8) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.162 0.00 0.00 -1.00 0.1620 1.00 -1.00 0.00 0.159 -1.00 1.00 0.00 0.159 1.00 1.00 0.00 0.182 -1.00 -1.00 0.00 0.182 -1.00 -1.00 -1.00 0.197 1.00 -1.00 -2.00 0.196 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 Cl W P2B 85.06(16) . . P1 W Cl 85.12(4) 8_575 . P1 W Cl 85.12(4) . . P1 W P1 166.90(9) . 8_575 P1 W P2B 93.92(5) . . P1 W P2B 93.92(5) 8_575 . P1 W P2A 93.08(5) . . P1 W P2A 93.08(5) 8_575 . N W Cl 174.7(3) . . N W P1 94.46(5) . 8_575 N W P1 94.46(5) . . N W P2B 100.2(3) . . N W P2A 108.9(3) . . P2A W Cl 76.34(17) . . C11B P1 W 116.8(6) . . C11B P1 C12B 103.3(8) . . C11B P1 C13B 106.1(10) . . C12B P1 W 116.7(5) . . C13B P1 W 113.8(6) . . C13B P1 C12B 98.0(8) . . C11A P1 W 113.1(5) . . C12A P1 W 121.8(5) . . C12A P1 C11A 106.7(8) . . C12A P1 C13A 100.9(8) . . C13A P1 W 115.3(5) . . C13A P1 C11A 95.2(7) . . C14B P2B W 117.6(8) . . C15B P2B W 118.2(5) 8_575 . C15B P2B W 118.2(5) . . C15B P2B C14B 99.3(7) 8_575 . C15B P2B C14B 99.3(7) . . C15B P2B C15B 100.7(10) 8_575 . C1 N W 171.9(7) . . N C1 C6 120.9(8) . . C2 C1 N 121.0(9) . . C2 C1 C6 118.1(8) . . C1 C2 C3 121.1(9) . . C1 C2 C7 122.1(8) . . C3 C2 C7 116.8(9) . . C4 C3 C2 120.4(10) . . C3 C4 C5 120.7(9) . . C6 C5 C4 118.3(10) . . C1 C6 C9 121.1(8) . . C5 C6 C1 121.3(10) . . C5 C6 C9 117.6(10) . . C8 C7 C2 112.4(6) 8_575 . C8 C7 C2 112.4(6) . . C8 C7 C8 111.1(10) . 8_575 C10 C9 C6 110.6(6) 8_575 . C10 C9 C6 110.6(6) . . C10 C9 C10 110.3(9) 8_575 . C14A P2A W 117.3(6) . . C14A P2A C15A 101.2(8) . . C14A P2A C15A 101.2(8) . 8_575 C15A P2A W 117.8(6) . . C15A P2A W 117.8(6) 8_575 . C15A P2A C15A 98.2(12) . 8_575 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W Cl 2.531(2) . W P1 2.4679(16) . W P1 2.4679(16) 8_575 W P2B 2.594(6) . W N 1.775(7) . W P2A 2.468(6) . P1 C11B 1.735(17) . P1 C12B 1.876(15) . P1 C13B 1.833(17) . P1 C11A 1.909(16) . P1 C12A 1.729(15) . P1 C13A 1.878(16) . P2B C14B 1.84(2) . P2B C15B 1.816(15) 8_575 P2B C15B 1.816(15) . N C1 1.393(11) . C1 C2 1.371(13) . C1 C6 1.435(14) . C2 C3 1.403(13) . C2 C7 1.542(15) . C3 C4 1.375(15) . C4 C5 1.410(14) . C5 C6 1.393(12) . C6 C9 1.535(15) . C7 C8 1.531(11) . C7 C8 1.532(11) 8_575 C9 C10 1.530(10) 8_575 C9 C10 1.530(10) . P2A C14A 1.83(2) . P2A C15A 1.843(17) 8_575 P2A C15A 1.843(17) .