#------------------------------------------------------------------------------ #$Date: 2024-12-24 03:06:49 +0200 (Tue, 24 Dec 2024) $ #$Revision: 296954 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/35/1573528.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_1573528 loop_ _publ_author_name 'Bouzid, Moad' 'Hierso, Jean-Cyrille' 'Mboyi, Cl\`eve D.' 'Poinsot, Didier' 'Domenichini, Bruno' 'Schreiner, Peter Richard' 'Ochmann, Lukas' _publ_section_title ; Sulfur functionalized diamondoid phosphines enable building nanocomposites interfacing sp3-carbon and gold nanolayer ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR03511A _journal_year 2025 _chemical_formula_moiety 'C14 H21 P S' _chemical_formula_sum 'C14 H21 P S' _chemical_formula_weight 252.34 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-08-06 _audit_creation_method ;FinalCif V139 by Daniel Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html ; _audit_update_record ; 2024-08-06 deposited with the CCDC. 2024-12-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.820(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.7405(4) _cell_length_b 13.6302(7) _cell_length_c 12.6387(6) _cell_measurement_reflns_used 5410 _cell_measurement_temperature 110.0(1) _cell_measurement_theta_max 27.33 _cell_measurement_theta_min 2.72 _cell_volume 1289.08(11) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2016)' _computing_data_collection 'APEX5 (Bruker, 2023)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 110.0(1) _diffrn_detector 'CCD Plate' _diffrn_detector_area_resol_mean 8.3 _diffrn_detector_type APEX2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Nonius Kappa Apex II' _diffrn_measurement_method '\f and \w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_collimation '0.6 mm' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a~1~' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 25147 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 2.239 _diffrn_source 'X-ray tube' _diffrn_source_current 5.0 _diffrn_source_power 0.1 _diffrn_source_target Mo _diffrn_source_type 'Siemens KFF Mo 2K-180' _diffrn_source_voltage 20.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.346 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_correction_T_min 0.8623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.0543 before and 0.0500 after correction. The Ratio of minimum to maximum transmission is 0.8998. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.300 _exptl_crystal_description needle _exptl_crystal_F_000 544 _exptl_crystal_recrystallization_method 'The material was recrystallised from DCM by slow evaporation' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.136 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.382 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 2954 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0375 _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^)+(0.0450P)^2^+1.0270P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.1051 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2209 _reflns_number_total 2954 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr03511a2.cif _cod_data_source_block Compound_3 _cod_database_code 1573528 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder oil' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All P(H,H) groups, All S(H) groups 2. Others Fixed Sof: S1A(0.54) H1A(0.54) P1A(0.54) H1AA(0.54) H1AB(0.54) S1(0.46) H1(0.46) P1(0.46) H1B(0.46) H1C(0.46) 3.a Everything fixed: H1AA, H1AB, H1B, H1C 3.b Ternary CH refined with riding coordinates: C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11) 3.c Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B) 3.d Idealised tetrahedral OH refined as rotating group: S1A(H1A), S1(H1) ; _olex2_submission_special_instructions 'No special instructions were received' _shelx_shelxl_version_number 2019/3 _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. ; _shelx_estimated_absorpt_t_min 0.891 _shelx_estimated_absorpt_t_max 0.976 _diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 600' _shelx_res_file ; TITL 20220512mblo02_0m_a.res in P2(1)/c 20220512mblo02_0m.res created by SHELXL-2019/3 at 13:19:08 on 06-Aug-2024 CELL 0.71073 7.7405 13.6302 12.6387 90 104.82 90 ZERR 4 0.0004 0.0007 0.0006 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H P S UNIT 56 84 4 4 L.S. 12 PLAN 20 SIZE 0.07 0.136 0.34 TEMP -163.15(10) CONF HTAB BOND LIST 4 MORE -1 BOND $H fmap 2 acta OMIT -2 55 REM REM REM WGHT 0.045000 1.027000 FVAR 0.66044 C1 1 0.371739 0.831584 0.577655 11.00000 0.01488 0.01900 = 0.01382 0.00153 0.00288 0.00273 C2 1 0.549606 0.887088 0.595352 11.00000 0.01931 0.01460 = 0.01849 0.00221 0.00364 -0.00144 AFIX 23 H2A 2 0.551545 0.924236 0.528355 11.00000 -1.20000 H2B 2 0.561544 0.934462 0.656176 11.00000 -1.20000 AFIX 0 C3 1 0.705936 0.814596 0.622330 11.00000 0.01431 0.01367 = 0.01615 -0.00042 0.00284 -0.00391 AFIX 13 H3 2 0.820559 0.851864 0.634014 11.00000 -1.20000 AFIX 0 C4 1 0.691395 0.742448 0.527255 11.00000 0.01751 0.01801 = 0.01133 0.00159 0.00555 -0.00173 AFIX 13 H4 2 0.693515 0.779928 0.459580 11.00000 -1.20000 AFIX 0 C5 1 0.512244 0.687615 0.508631 11.00000 0.01871 0.01805 = 0.00936 -0.00298 0.00267 -0.00368 AFIX 13 H5 2 0.500250 0.641074 0.446002 11.00000 -1.20000 AFIX 0 C6 1 0.354660 0.759446 0.482439 11.00000 0.01648 0.02333 = 0.01067 0.00026 0.00021 -0.00290 AFIX 23 H6A 2 0.240920 0.722757 0.470554 11.00000 -1.20000 H6B 2 0.353619 0.795949 0.414559 11.00000 -1.20000 AFIX 0 C7 1 0.371500 0.774112 0.682435 11.00000 0.01671 0.02271 = 0.01379 -0.00051 0.00572 -0.00001 AFIX 23 H7A 2 0.382967 0.820198 0.744393 11.00000 -1.20000 H7B 2 0.257277 0.738176 0.672297 11.00000 -1.20000 AFIX 0 C8 1 0.527661 0.701467 0.707843 11.00000 0.01671 0.01794 = 0.00954 0.00248 0.00449 -0.00074 AFIX 13 H8 2 0.525776 0.663980 0.775552 11.00000 -1.20000 AFIX 0 C9 1 0.707023 0.756353 0.726588 11.00000 0.01495 0.01473 = 0.01125 -0.00275 0.00075 -0.00142 AFIX 13 H9 2 0.719222 0.802952 0.789184 11.00000 -1.20000 AFIX 0 C10 1 0.846776 0.669658 0.552853 11.00000 0.01969 0.02111 = 0.01661 -0.00005 0.00751 0.00119 AFIX 23 H10A 2 0.961149 0.705463 0.563079 11.00000 -1.20000 H10B 2 0.835250 0.623679 0.490794 11.00000 -1.20000 AFIX 0 C11 1 0.512574 0.628982 0.612677 11.00000 0.01737 0.01516 = 0.01461 -0.00072 0.00387 -0.00540 AFIX 13 H11 2 0.397909 0.591744 0.600917 11.00000 -1.20000 AFIX 0 C12 1 0.669454 0.556619 0.638956 11.00000 0.02745 0.01306 = 0.01906 0.00032 0.00729 -0.00166 AFIX 23 H12A 2 0.667508 0.518803 0.705518 11.00000 -1.20000 H12B 2 0.657645 0.509801 0.577629 11.00000 -1.20000 AFIX 0 C13 1 0.846811 0.611925 0.657303 11.00000 0.01953 0.01651 = 0.01674 0.00223 0.00535 0.00446 C14 1 0.863540 0.683952 0.752754 11.00000 0.01602 0.02146 = 0.01378 0.00047 0.00100 0.00086 AFIX 23 H14A 2 0.863566 0.647293 0.820379 11.00000 -1.20000 H14B 2 0.977751 0.720264 0.765204 11.00000 -1.20000 AFIX 0 PART 1 S1A 4 0.174450 0.911606 0.549331 10.54000 0.01399 0.02116 = 0.03188 0.00612 0.00255 0.00851 AFIX 147 H1A 2 0.042236 0.863092 0.516382 10.54000 -1.20000 AFIX 0 P1A 3 1.051946 0.533577 0.690834 10.54000 0.01415 0.01673 = 0.03041 0.00467 0.00416 0.00761 AFIX 1 H1AA 2 1.010200 0.484700 0.764900 10.54000 -1.20000 AFIX 1 H1AB 2 0.993600 0.474400 0.612300 10.54000 -1.20000 AFIX 0 PART 2 S1 4 1.024273 0.519285 0.682140 10.46000 0.02761 AFIX 147 H1 2 1.166386 0.558397 0.716892 10.46000 -1.20000 AFIX 0 P1 3 0.194000 0.926958 0.553273 10.46000 0.02339 AFIX 1 H1B 2 0.156000 0.987200 0.605700 10.46000 -1.20000 AFIX 1 H1C 2 0.177500 0.945200 0.464200 10.46000 -1.20000 AFIX 0 HKLF 4 REM 20220512mblo02_0m_a.res in P2(1)/c REM wR2 = 0.1051, GooF = S = 1.021, Restrained GooF = 1.021 for all data REM R1 = 0.0375 for 2209 Fo > 4sig(Fo) and 0.0613 for all 2954 data REM 155 parameters refined using 0 restraints END WGHT 0.0450 1.0270 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.382, deepest hole -0.519, 1-sigma level 0.060 Q1 1 0.5077 0.6572 0.5559 11.00000 0.05 0.38 Q2 1 0.6102 0.7284 0.7219 11.00000 0.05 0.36 Q3 1 0.6058 0.7153 0.5194 11.00000 0.05 0.33 Q4 1 0.5322 0.6709 0.6591 11.00000 0.05 0.33 Q5 1 0.6892 0.7783 0.5711 11.00000 0.05 0.33 Q6 1 0.4342 0.7241 0.4985 11.00000 0.05 0.33 Q7 1 0.3725 0.7944 0.5373 11.00000 0.05 0.33 Q8 1 0.8620 0.6479 0.7011 11.00000 0.05 0.32 Q9 1 0.2448 0.9669 0.5690 11.00000 0.05 0.32 Q10 1 0.2004 0.9531 0.4460 11.00000 0.05 0.31 Q11 1 0.5835 0.5950 0.6233 11.00000 0.05 0.31 Q12 1 0.9571 0.4613 0.7540 11.00000 0.05 0.31 Q13 1 0.9179 0.5793 0.6738 11.00000 0.05 0.30 Q14 1 0.7075 0.7826 0.6760 11.00000 0.05 0.30 Q15 1 0.7746 0.5853 0.6560 11.00000 0.05 0.30 Q16 1 0.4574 0.7367 0.6983 11.00000 0.05 0.30 Q17 1 1.1738 0.5323 0.7126 11.00000 0.05 0.30 Q18 1 0.7816 0.7218 0.7395 11.00000 0.05 0.29 Q19 1 0.8335 0.6437 0.6081 11.00000 0.05 0.28 Q20 1 0.4525 0.8580 0.5797 11.00000 0.05 0.27 ; _shelx_res_checksum 49180 _shelx_hkl_file ; 1 0 0 980.70 20.60 1 0 0 928.41 21.20 -1 0 0 914.41 20.50 -1 0 0 912.31 21.10 -1 0 0 975.90 21.50 -1 0 0 1012.20 21.40 2 0 0 -0.70 4.20 2 0 0 4.30 4.60 -2 0 0 1.00 4.10 -2 0 0 5.00 3.20 -2 0 0 0.40 3.00 -2 0 0 3.60 3.00 2 0 0 -0.30 3.30 2 0 0 0.90 3.00 3 0 0 67.99 7.10 3 0 0 68.39 8.40 3 0 0 88.29 8.20 3 0 0 76.79 6.40 3 0 0 90.49 7.20 -3 0 0 72.79 7.50 -3 0 0 76.49 7.80 -3 0 0 84.09 7.00 -3 0 0 87.59 8.10 4 0 0 -4.60 4.10 4 0 0 2.40 4.90 4 0 0 -5.20 6.10 4 0 0 -5.30 3.90 4 0 0 -2.10 5.90 -4 0 0 -0.10 5.20 -4 0 0 -5.00 3.50 -4 0 0 9.30 5.60 -4 0 0 2.40 5.10 5 0 0 3.60 5.30 -5 0 0 6.40 4.80 5 0 0 0.90 5.00 5 0 0 7.00 7.50 -5 0 0 2.00 4.60 5 0 0 4.80 5.40 5 0 0 2.20 4.80 -6 0 0 1833.02 47.90 6 0 0 1840.92 53.99 6 0 0 1834.62 47.70 -6 0 0 1860.51 51.39 6 0 0 1873.41 52.39 6 0 0 1787.72 51.19 -7 0 0 2.50 5.80 7 0 0 14.00 10.00 7 0 0 -0.50 7.10 7 0 0 -15.00 6.90 7 0 0 5.90 9.90 -8 0 0 61.89 10.50 8 0 0 68.09 13.00 8 0 0 70.59 14.60 8 0 0 74.79 12.50 -9 0 0 314.97 20.00 9 0 0 258.37 26.20 0 -1 0 -0.60 0.70 0 -1 0 0.10 0.80 0 -1 0 -0.30 0.50 0 -1 0 -0.80 0.70 0 1 0 -0.10 0.60 0 1 0 -0.40 0.70 0 1 0 0.10 0.60 1 -1 0 940.11 21.50 1 -1 0 937.61 21.50 1 -1 0 987.20 21.70 1 -1 0 927.11 20.90 -1 -1 0 949.60 21.20 -1 -1 0 966.20 21.60 -1 -1 0 965.40 21.50 1 -1 0 944.11 21.80 -1 -1 0 921.51 21.40 -1 1 0 940.61 21.60 1 1 0 950.60 21.20 -1 1 0 947.01 20.10 1 1 0 975.40 21.70 1 1 0 968.90 20.30 1 1 0 925.51 21.40 -1 1 0 935.51 20.90 -1 1 0 957.50 21.90 -1 1 0 955.20 21.50 -2 -1 0 259.57 10.00 2 -1 0 270.87 10.40 -2 -1 0 278.37 10.20 2 -1 0 283.97 8.90 2 -1 0 262.67 10.40 -2 -1 0 261.47 10.10 -2 -1 0 254.47 10.60 2 -1 0 268.37 10.80 2 1 0 254.77 10.90 2 1 0 257.17 10.40 2 1 0 277.27 10.10 2 1 0 259.87 11.00 -2 1 0 269.27 9.00 -2 1 0 266.57 10.70 -2 1 0 274.77 10.60 -2 1 0 278.87 10.80 -3 -1 0 71.49 7.70 3 -1 0 62.89 8.10 -3 -1 0 72.99 7.10 3 -1 0 69.09 7.30 3 -1 0 64.49 5.80 -3 -1 0 74.59 7.10 3 -1 0 72.89 6.80 -3 -1 0 80.49 7.40 3 -1 0 64.69 7.30 3 1 0 72.79 8.20 -3 1 0 75.39 6.20 3 1 0 71.79 8.20 3 1 0 70.59 6.80 -3 1 0 68.09 7.70 3 1 0 70.49 8.20 3 1 0 84.09 7.10 -3 1 0 68.79 7.90 -3 1 0 72.69 7.60 -4 -1 0 10.40 5.70 4 -1 0 17.80 6.00 4 -1 0 7.60 5.10 -4 -1 0 13.50 5.10 4 -1 0 10.70 4.60 -4 -1 0 23.50 6.60 4 -1 0 9.60 6.50 -4 -1 0 16.00 6.00 4 -1 0 22.80 7.50 -4 1 0 17.60 6.00 -4 1 0 18.30 4.60 4 1 0 14.10 6.90 -4 1 0 18.70 5.50 4 1 0 22.60 7.30 4 1 0 15.10 7.10 4 1 0 10.60 5.00 4 1 0 3.60 4.60 -4 1 0 20.70 6.40 5 -1 0 165.48 13.00 -5 -1 0 152.58 11.00 5 -1 0 180.68 11.40 5 -1 0 158.08 13.90 -5 -1 0 171.78 11.80 5 -1 0 152.78 10.70 5 -1 0 152.38 13.90 5 1 0 150.58 12.10 5 1 0 163.58 13.00 5 1 0 150.88 14.40 -5 1 0 166.68 12.70 -5 1 0 169.78 10.50 5 1 0 176.48 11.30 5 1 0 180.38 14.00 6 -1 0 2144.29 57.29 6 -1 0 2057.89 52.19 6 -1 0 2083.29 58.89 -6 -1 0 2012.90 52.89 6 -1 0 2040.40 56.59 -6 -1 0 2068.19 55.59 6 -1 0 2042.70 51.59 6 1 0 2014.30 51.79 6 1 0 2032.90 55.99 -6 1 0 2088.19 50.49 -6 1 0 2050.89 51.59 -6 1 0 2180.98 56.79 6 1 0 2082.19 58.49 6 1 0 2020.20 56.59 7 -1 0 161.58 14.90 7 -1 0 140.89 17.20 -7 -1 0 127.79 13.10 7 -1 0 114.39 15.10 7 -1 0 153.28 18.30 -7 1 0 140.69 13.00 7 1 0 141.69 16.10 7 1 0 166.18 17.70 7 1 0 156.78 14.50 8 -1 0 38.90 12.60 -8 -1 0 14.50 7.90 8 -1 0 18.30 10.30 8 -1 0 33.90 11.30 8 1 0 38.70 10.20 8 1 0 13.70 14.10 -8 1 0 13.70 7.30 8 1 0 17.30 9.90 -9 -1 0 -1.80 7.30 9 -1 0 -5.60 13.50 -9 1 0 3.40 7.20 9 1 0 4.30 13.80 9 1 0 -0.70 10.70 0 -2 0 2220.48 44.80 0 -2 0 2118.89 45.20 0 -2 0 2266.77 45.50 0 -2 0 2036.40 45.00 0 2 0 2275.27 44.70 0 2 0 2176.28 45.40 0 2 0 2229.08 45.20 1 -2 0 5897.51 117.49 -1 -2 0 5910.91 116.29 1 -2 0 5780.62 117.39 -1 -2 0 5872.51 117.29 -1 -2 0 5962.20 117.39 1 -2 0 5858.01 117.79 -1 -2 0 5706.03 115.89 1 -2 0 5852.61 117.09 1 -2 0 5825.12 117.39 -1 -2 0 5879.21 117.19 1 2 0 5946.51 116.29 1 2 0 5906.81 117.19 -1 2 0 5870.41 117.39 1 2 0 5913.11 116.09 -1 2 0 5836.82 116.89 -1 2 0 5846.71 117.29 -1 2 0 5837.12 117.79 -1 2 0 5847.52 117.39 1 2 0 5756.82 117.29 1 2 0 5760.12 117.19 -2 -2 0 753.12 21.00 2 -2 0 779.82 20.90 2 -2 0 782.02 21.70 -2 -2 0 784.32 20.80 -2 -2 0 752.22 20.50 2 -2 0 773.12 22.00 -2 -2 0 764.02 20.70 2 -2 0 795.62 21.70 -2 -2 0 765.52 19.00 2 2 0 767.12 21.30 -2 2 0 770.42 19.90 -2 2 0 775.12 18.50 -2 2 0 808.52 21.10 2 2 0 763.72 20.30 -2 2 0 776.32 21.10 2 2 0 780.82 21.30 -2 2 0 771.02 21.20 2 2 0 778.12 18.70 2 2 0 790.62 19.90 3 -2 0 47.00 4.80 -3 -2 0 51.19 6.30 -3 -2 0 49.60 7.00 3 -2 0 47.50 6.10 -3 -2 0 37.50 6.70 3 -2 0 53.59 8.20 3 -2 0 50.29 6.80 -3 -2 0 57.19 6.90 3 -2 0 51.69 7.10 3 2 0 59.99 6.50 3 2 0 49.90 7.60 -3 2 0 46.90 6.50 -3 2 0 53.99 5.30 3 2 0 49.10 7.50 -3 2 0 52.79 5.70 -3 2 0 54.79 7.30 3 2 0 62.39 6.80 -3 2 0 47.90 6.70 -4 -2 0 171.98 10.70 4 -2 0 138.19 10.60 4 -2 0 146.49 12.40 -4 -2 0 166.18 9.90 4 -2 0 158.68 13.00 4 -2 0 161.38 10.20 4 -2 0 153.38 9.00 -4 -2 0 169.38 10.50 -4 -2 0 164.78 11.20 -4 2 0 140.29 11.50 4 2 0 144.49 10.10 4 2 0 153.78 10.30 -4 2 0 166.58 11.40 -4 2 0 150.88 8.90 -4 2 0 148.09 8.50 4 2 0 166.78 12.20 -4 2 0 131.49 10.60 4 2 0 150.08 12.10 -5 -2 0 823.82 27.40 5 -2 0 796.92 29.00 5 -2 0 786.52 28.30 -5 -2 0 802.02 26.30 5 -2 0 780.12 28.40 5 -2 0 812.12 24.10 5 -2 0 774.52 25.40 5 2 0 787.62 27.60 -5 2 0 803.92 23.90 -5 2 0 785.12 24.00 5 2 0 802.02 28.20 -5 2 0 825.42 28.00 5 2 0 794.62 25.00 6 -2 0 12.10 8.60 6 -2 0 2.20 7.00 -6 -2 0 10.60 7.50 -6 -2 0 7.40 6.50 6 -2 0 11.00 7.50 6 2 0 3.30 9.00 -6 2 0 9.80 5.70 6 2 0 10.00 8.10 6 2 0 1.80 6.50 -6 2 0 13.20 5.20 -7 -2 0 26.10 7.00 7 -2 0 22.90 11.30 7 -2 0 18.90 9.20 7 -2 0 18.70 10.30 7 2 0 1.50 7.40 7 2 0 16.00 9.80 -7 2 0 19.70 6.70 7 2 0 20.60 10.80 8 -2 0 218.68 22.30 8 -2 0 232.08 23.40 -8 -2 0 188.08 17.60 8 -2 0 210.38 21.60 8 2 0 186.18 14.80 -8 2 0 244.18 15.40 8 2 0 234.48 21.50 8 2 0 240.88 18.40 9 -2 0 12.40 13.80 -9 -2 0 0.10 7.70 9 -2 0 4.70 13.40 9 2 0 0.30 10.10 9 2 0 2.80 9.80 -9 2 0 -3.90 7.00 0 -3 0 -0.90 2.90 0 -3 0 -1.10 2.80 0 -3 0 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5 -6 0 61.29 11.70 -5 -6 0 80.39 10.30 -5 -6 0 61.69 10.60 5 6 0 78.79 11.60 5 6 0 68.39 7.60 5 6 0 77.39 10.90 -5 6 0 90.59 11.70 5 6 0 74.59 9.90 -5 6 0 60.69 6.50 -6 -6 0 33.80 8.70 -6 -6 0 23.20 6.30 6 -6 0 30.30 9.20 6 -6 0 16.40 8.70 -6 -6 0 22.40 8.60 6 -6 0 14.90 9.00 6 6 0 24.50 5.80 6 6 0 44.00 9.90 6 6 0 20.70 9.80 6 6 0 9.40 10.10 -6 6 0 28.70 5.80 7 -6 0 16.10 12.20 7 -6 0 9.70 8.40 -7 -6 0 -1.90 5.00 -7 -6 0 16.00 8.70 7 -6 0 10.20 9.30 7 6 0 10.20 9.40 7 6 0 -4.30 6.80 7 6 0 7.90 5.50 -7 6 0 8.70 4.80 7 6 0 -5.60 10.50 8 -6 0 302.37 27.00 -8 -6 0 322.77 22.80 8 -6 0 343.57 28.00 8 6 0 275.77 25.60 8 6 0 315.07 21.10 9 -6 0 7.00 10.90 -9 -6 0 -8.90 8.90 9 -6 0 3.40 14.70 9 6 0 -4.80 13.60 9 6 0 -8.80 11.20 0 -7 0 -0.40 4.60 0 -7 0 3.10 4.30 0 -7 0 0.70 4.70 0 -7 0 3.30 5.50 0 -7 0 -3.60 5.10 0 -7 0 -0.30 3.90 0 7 0 5.70 4.00 0 7 0 4.20 4.20 0 7 0 -7.30 4.40 -1 -7 0 52.39 7.80 -1 -7 0 48.30 7.10 1 -7 0 44.80 8.20 -1 -7 0 36.30 5.80 1 -7 0 54.39 7.50 1 -7 0 43.30 7.70 -1 -7 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4 537.15 16.70 -3 -2 4 499.35 18.30 -3 -2 4 503.25 11.00 3 -2 -4 499.85 16.90 3 -2 -4 518.15 16.10 3 2 -4 531.05 16.00 3 2 -4 532.85 16.50 -3 2 4 496.55 16.60 3 2 -4 532.55 18.50 -3 2 4 508.95 17.50 3 2 -4 539.45 17.90 -3 2 4 512.35 16.00 -3 2 4 538.45 17.20 2 -2 -4 34.80 5.20 -2 -2 4 45.00 4.40 2 -2 -4 53.59 6.50 2 -2 -4 43.90 5.00 -2 -2 4 41.50 4.40 2 -2 -4 56.49 5.70 -2 -2 4 39.80 6.00 2 2 -4 38.70 4.20 2 2 -4 42.40 6.20 -2 2 4 36.20 4.70 2 2 -4 41.50 3.80 -2 2 4 43.40 4.80 -2 2 4 44.00 5.20 2 2 -4 34.90 5.00 -2 2 4 36.50 5.00 1 -2 -4 1865.61 39.40 -1 -2 4 1808.42 37.70 1 -2 -4 1859.81 39.10 1 -2 -4 1849.42 38.90 -1 -2 4 1835.12 42.10 1 -2 -4 1796.82 39.30 1 -2 -4 1843.12 42.50 -1 2 4 1806.92 39.40 1 2 -4 1808.72 40.80 -1 2 4 1855.91 42.60 0 -2 4 1956.60 45.40 0 -2 -4 1982.50 42.00 0 -2 4 1891.11 43.10 0 -2 -4 2027.80 41.70 0 -2 4 1951.90 40.80 0 -2 4 1901.81 40.50 0 2 4 1948.31 42.20 0 2 4 1972.40 40.70 0 2 4 1947.21 45.70 0 2 -4 1964.40 40.30 0 2 4 1916.11 41.90 -1 -2 -4 34.40 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9 397.26 15.30 2 5 9 364.96 19.00 3 -5 9 -0.60 7.80 3 -5 9 6.40 6.80 3 -5 9 -1.70 4.80 3 -5 9 11.60 8.60 3 5 9 -2.20 9.70 3 5 9 -3.90 7.20 3 5 9 18.50 8.70 3 5 9 2.10 5.70 4 -5 9 33.00 11.10 4 -5 9 37.60 11.40 4 -5 9 40.30 10.50 4 5 9 54.49 9.60 4 5 9 56.99 11.60 4 5 9 34.90 10.90 4 5 9 48.60 13.50 5 -5 9 -7.70 8.80 5 -5 9 -6.00 12.70 5 -5 9 7.70 9.70 5 5 9 9.70 11.70 5 5 9 13.10 8.60 5 5 9 -12.20 9.00 5 5 9 -6.60 9.20 6 -5 9 25.00 12.50 6 -5 9 0.30 14.20 6 -5 9 4.80 11.30 6 5 9 14.00 12.10 6 5 9 2.60 11.40 6 5 9 2.60 11.20 -9 -6 9 70.59 19.00 -9 -6 9 79.69 15.40 9 6 -9 61.39 16.40 -9 6 9 74.79 15.10 -8 -6 9 45.60 13.10 -8 -6 9 40.00 13.50 8 6 -9 57.89 15.30 -8 6 9 62.99 13.70 -7 -6 9 28.60 9.80 -7 -6 9 13.50 10.00 -7 6 9 12.80 7.50 7 6 -9 17.70 10.40 -7 6 9 22.10 8.20 -6 -6 9 4.10 8.70 -6 -6 9 -13.60 7.80 -6 6 9 4.80 8.30 -6 6 9 13.40 8.10 6 6 -9 7.30 8.90 -5 -6 9 11.50 9.00 -5 -6 9 -7.10 5.50 5 -6 -9 -3.50 6.00 -5 -6 9 13.40 8.60 -5 6 9 -3.10 6.60 5 6 -9 -1.50 6.80 -4 -6 9 219.58 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9 79.49 13.60 6 7 -9 109.99 17.20 5 -7 -9 371.36 19.40 -5 -7 9 381.36 22.90 -5 -7 9 364.36 18.00 -5 -7 9 376.06 22.10 5 7 -9 346.67 22.60 -5 7 9 334.17 20.70 -4 -7 9 3.00 6.30 -4 -7 9 1.10 6.90 -4 -7 9 2.30 5.00 4 -7 -9 0.60 7.00 4 7 -9 8.30 9.00 -4 7 9 2.40 7.50 -3 -7 9 17.10 6.30 -3 -7 9 26.10 9.10 3 -7 -9 44.80 7.70 -3 -7 9 35.90 6.40 -3 -7 9 24.10 6.20 3 -7 -9 23.10 7.70 -3 -7 9 26.10 5.90 -3 -7 9 43.60 8.40 -3 7 9 30.40 4.60 -3 7 9 32.30 9.90 3 7 -9 40.50 8.50 -2 -7 9 10.20 4.50 -2 -7 9 18.60 6.60 -2 -7 9 16.80 9.70 -2 -7 9 8.00 4.90 2 -7 -9 11.40 6.70 2 -7 -9 12.80 5.80 -2 -7 9 6.80 7.60 -2 -7 9 9.00 5.10 2 7 -9 1.10 6.50 -2 7 9 3.60 7.70 -1 -7 9 -4.20 8.40 -1 -7 9 4.00 4.30 1 -7 -9 5.10 5.70 -1 -7 9 -2.30 4.20 1 -7 -9 -5.00 4.50 -1 -7 9 4.00 4.90 -1 -7 9 -1.60 6.70 -1 7 9 3.10 8.30 1 7 -9 0.30 5.40 0 -7 9 273.97 14.20 0 -7 -9 294.47 16.00 0 -7 9 272.67 11.70 0 -7 9 305.87 21.40 0 -7 9 284.27 14.10 0 -7 9 296.77 17.20 0 7 9 275.37 20.40 0 7 -9 263.67 13.90 1 -7 9 76.39 9.70 1 -7 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204.38 19.80 3 -8 9 108.79 14.30 3 -8 9 115.09 12.90 3 -8 9 94.49 13.70 3 -8 9 84.99 17.00 3 8 9 117.19 15.00 3 8 9 125.69 15.70 3 8 9 106.09 15.60 4 -8 9 -9.70 8.80 4 -8 9 12.80 11.30 4 -8 9 -12.80 12.10 4 8 9 -5.70 10.10 4 8 9 -7.90 9.20 4 8 9 -2.80 10.90 5 -8 9 -16.00 12.90 5 -8 9 19.00 11.90 5 -8 9 -7.60 10.60 5 8 9 15.50 12.00 5 8 9 -0.40 10.40 5 8 9 -3.50 11.10 -8 -9 9 -24.70 10.20 -8 -9 9 -0.90 10.70 -8 9 9 -1.30 6.40 -8 9 9 9.90 12.30 8 9 -9 -4.40 13.70 -7 -9 9 -14.20 9.60 -7 -9 9 -10.00 9.40 7 9 -9 -4.80 13.60 -7 9 9 -3.50 8.50 -7 9 9 5.00 8.80 -6 -9 9 24.40 11.00 -6 -9 9 12.00 8.10 -6 9 9 9.80 9.80 6 9 -9 6.40 11.70 -5 -9 9 61.99 12.10 -5 -9 9 59.49 11.60 5 9 -9 54.79 13.60 -5 9 9 51.69 12.40 -4 -9 9 -12.00 7.70 -4 -9 9 4.80 7.20 4 -9 -9 7.20 7.70 4 9 -9 0.40 9.90 -4 9 9 6.40 9.10 -3 -9 9 -3.90 5.80 -3 -9 9 1.60 6.20 -3 -9 9 7.60 6.70 -3 -9 9 -4.80 5.50 3 -9 -9 3.30 7.20 3 9 -9 7.00 9.00 -3 9 9 1.00 8.80 -2 -9 9 -7.00 7.70 -2 -9 9 0.30 7.10 -2 -9 9 1.60 5.80 2 -9 -9 3.30 7.20 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33.90 11.70 6 -4 10 5.10 15.30 -8 -5 10 -9.20 9.40 -8 -5 10 15.60 10.60 -8 5 10 10.40 10.20 8 5 -10 -2.50 10.40 -7 -5 10 11.10 11.00 -7 -5 10 32.80 11.70 -7 5 10 41.40 9.40 -7 5 10 30.20 11.40 7 5 -10 15.20 12.80 -6 -5 10 0.00 6.50 -6 -5 10 1.70 8.60 -6 5 10 -1.70 8.20 6 5 -10 -5.20 10.70 -6 5 10 5.20 7.40 -5 -5 10 324.07 20.80 -5 -5 10 310.67 20.60 -5 -5 10 311.57 15.40 -5 5 10 288.37 18.40 5 5 -10 287.67 20.40 -4 -5 10 422.66 15.20 -4 -5 10 427.06 16.30 -4 -5 10 461.05 22.60 -4 -5 10 419.16 22.90 4 -5 -10 413.36 17.10 -4 -5 10 434.56 16.80 -4 5 10 452.65 22.50 4 5 -10 472.85 22.90 -4 5 10 436.46 18.00 -3 -5 10 40.00 8.60 3 -5 -10 40.20 6.50 -3 -5 10 54.09 5.20 -3 -5 10 42.60 9.50 -3 -5 10 39.40 4.60 -3 -5 10 38.30 5.30 -3 5 10 44.70 9.70 3 5 -10 38.80 9.30 -3 5 10 37.50 6.20 -2 -5 10 1.10 5.70 -2 -5 10 6.30 2.30 2 -5 -10 -3.40 4.00 -2 -5 10 8.40 3.30 -2 -5 10 3.40 5.40 -2 -5 10 -9.80 7.40 -2 -5 10 4.30 2.50 -2 5 10 2.40 7.00 -2 5 10 -6.70 2.90 -2 5 10 6.60 3.50 2 5 -10 6.00 5.90 -1 -5 10 9.50 4.00 -1 -5 10 20.90 8.00 -1 -5 10 12.20 5.70 -1 -5 10 4.30 6.20 -1 -5 10 11.80 3.10 1 -5 -10 5.40 4.60 -1 -5 10 8.50 2.80 -1 5 10 8.70 3.00 1 5 -10 3.30 5.40 -1 5 10 6.10 6.40 0 -5 10 13.10 4.40 0 -5 10 8.90 6.90 0 -5 10 5.80 4.30 0 -5 10 10.70 4.90 0 -5 10 6.50 5.70 0 -5 -10 16.20 5.60 0 5 10 7.80 3.10 0 5 -10 8.10 5.00 0 5 10 10.60 5.30 0 5 10 8.90 6.10 0 5 10 1.30 8.70 -1 -5 -10 52.49 8.00 1 -5 10 56.09 7.60 1 -5 10 41.60 7.50 1 -5 10 69.99 6.30 1 -5 10 59.39 12.50 1 -5 10 56.59 8.80 1 5 10 47.90 5.60 1 5 10 57.79 9.30 1 5 10 57.49 9.50 1 5 10 59.89 12.80 2 -5 10 479.15 26.70 2 -5 10 437.66 20.00 2 -5 10 467.65 19.20 2 -5 10 472.05 19.00 2 5 10 484.25 21.50 2 5 10 439.26 27.00 2 5 10 424.76 20.90 3 -5 10 69.89 11.00 3 -5 10 73.79 15.20 3 -5 10 64.49 9.20 3 -5 10 76.79 11.50 3 5 10 67.79 12.10 3 5 10 52.59 13.80 3 5 10 69.69 9.70 3 5 10 62.49 11.40 4 -5 10 85.69 13.30 4 -5 10 85.39 13.50 4 -5 10 78.29 16.80 4 5 10 81.89 16.50 4 5 10 95.99 14.50 4 5 10 106.09 14.50 5 -5 10 4.60 9.30 5 -5 10 -7.50 10.50 5 -5 10 4.30 13.40 5 5 10 28.10 11.60 5 5 10 9.00 10.20 5 5 10 6.90 12.70 -8 -6 10 129.49 19.00 -8 -6 10 102.39 16.80 8 6 -10 122.09 20.90 -8 6 10 122.29 18.10 -7 -6 10 30.80 12.20 -7 -6 10 20.60 10.80 7 6 -10 1.80 12.70 -7 6 10 20.60 10.50 -7 6 10 19.60 8.90 -6 -6 10 14.60 10.10 -6 -6 10 24.40 8.60 -6 6 10 11.30 7.40 6 6 -10 7.80 9.60 -6 6 10 20.70 9.20 -5 -6 10 5.20 8.50 -5 -6 10 -4.00 5.30 -5 -6 10 15.20 9.00 5 6 -10 4.40 9.40 -5 6 10 16.50 8.30 -4 -6 10 112.09 13.50 -4 -6 10 139.29 10.20 4 -6 -10 109.09 14.00 -4 -6 10 134.29 14.40 4 6 -10 134.39 15.60 -4 6 10 138.09 14.50 -3 -6 10 114.89 7.70 -3 -6 10 107.89 13.60 -3 -6 10 140.89 13.20 -3 -6 10 133.09 8.90 3 -6 -10 136.89 11.30 -3 -6 10 124.19 8.50 -3 6 10 109.19 13.70 3 6 -10 111.39 13.20 -2 -6 10 122.69 13.60 -2 -6 10 109.99 10.80 -2 -6 10 112.49 6.90 -2 -6 10 127.59 8.40 2 -6 -10 114.29 10.10 -2 -6 10 116.39 7.50 -2 -6 10 100.89 13.50 2 6 -10 117.29 12.50 -2 6 10 117.89 5.30 -2 6 10 120.79 5.40 -2 6 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105.39 17.20 5 6 10 102.49 16.50 5 6 10 87.49 17.40 -8 -7 10 19.00 11.50 -8 -7 10 -1.50 11.40 8 7 -10 19.10 15.50 -8 7 10 11.90 10.10 -7 -7 10 84.79 14.60 -7 -7 10 74.39 14.50 7 7 -10 73.69 16.90 -7 7 10 93.39 15.40 -7 7 10 96.89 13.30 -6 -7 10 1.30 6.80 -6 -7 10 12.10 9.60 -6 7 10 -9.50 5.20 -6 7 10 2.50 7.90 6 7 -10 -4.80 11.10 -5 -7 10 6.70 8.80 -5 -7 10 -0.40 8.20 -5 -7 10 12.30 6.20 5 7 -10 -15.90 9.10 -5 7 10 13.80 8.80 -4 -7 10 17.20 7.70 -4 -7 10 9.30 5.60 -4 -7 10 11.30 7.70 4 7 -10 16.50 9.90 -4 7 10 6.00 8.00 -3 -7 10 200.18 17.70 3 -7 -10 175.68 15.70 -3 -7 10 193.08 14.50 -3 -7 10 191.08 11.10 -3 -7 10 218.48 11.90 3 7 -10 184.68 16.40 -3 7 10 187.28 15.60 -2 -7 10 224.68 14.30 -2 -7 10 240.58 11.90 2 -7 -10 216.18 13.90 -2 -7 10 195.48 17.10 -2 -7 10 235.38 11.40 -2 -7 10 247.18 20.30 2 7 -10 206.88 15.30 -2 7 10 240.48 19.10 -1 -7 10 284.87 19.70 -1 -7 10 259.47 12.30 1 -7 -10 296.87 15.30 -1 -7 10 258.27 13.40 -1 -7 10 243.78 12.90 -1 -7 10 247.48 17.20 -1 7 10 250.17 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14.40 -4 0 16 11.10 10.00 -3 0 16 0.60 8.20 -3 0 16 0.60 9.70 -3 0 16 0.80 7.40 -2 0 16 20.70 10.50 -2 0 16 27.70 10.10 -2 0 16 30.70 12.10 -1 0 16 -9.00 9.80 0 0 16 54.89 16.10 -5 -1 16 33.80 12.00 -5 -1 16 21.90 12.80 5 1 -16 6.60 10.30 -5 1 16 1.30 10.70 -4 -1 16 -9.50 12.70 -4 -1 16 6.50 9.60 -4 -1 16 7.90 10.50 -4 -1 16 1.80 9.00 4 1 -16 14.30 9.20 -4 1 16 24.10 12.60 -4 1 16 -9.40 8.40 -3 -1 16 -4.40 7.70 -3 -1 16 2.60 8.20 -3 -1 16 7.80 7.70 -3 -1 16 1.80 9.30 -3 1 16 -11.60 9.30 -3 1 16 0.30 7.30 -3 1 16 3.30 8.80 -2 -1 16 130.49 16.20 -2 -1 16 98.49 15.90 -2 -1 16 98.69 13.80 -2 -1 16 127.69 16.40 -2 1 16 153.58 19.00 -1 -1 16 33.60 13.30 -1 -1 16 48.40 11.50 -1 1 16 34.30 13.80 0 -1 16 2.90 10.90 0 1 16 27.80 13.20 -5 -2 16 4.40 10.50 -4 -2 16 55.09 12.80 -4 -2 16 47.80 12.80 -4 -2 16 37.20 12.90 4 2 -16 25.00 9.90 -4 2 16 38.70 11.10 -4 2 16 60.09 13.40 -3 -2 16 122.89 15.70 -3 -2 16 123.29 15.70 -3 -2 16 122.09 16.60 -3 -2 16 109.09 15.30 -3 2 16 121.69 17.00 -3 2 16 120.19 17.20 -2 -2 16 17.90 9.30 -2 -2 16 -2.70 8.80 -2 -2 16 17.30 9.40 -2 -2 16 7.10 7.80 -2 2 16 15.00 11.50 -1 -2 16 -6.30 9.60 -1 -2 16 -7.50 7.70 -1 2 16 -12.70 9.90 -4 -3 16 -11.40 8.40 -4 -3 16 4.70 10.30 -4 -3 16 10.20 9.50 -4 3 16 -23.00 9.40 -4 3 16 11.30 8.90 4 3 -16 6.70 8.50 -3 -3 16 116.99 15.40 -3 -3 16 75.09 13.40 -3 -3 16 132.29 17.50 -3 -3 16 107.29 15.10 -3 3 16 141.29 18.10 -2 -3 16 155.58 18.60 -2 -3 16 160.38 18.40 -2 -3 16 158.18 17.00 -2 -3 16 132.99 15.40 -2 3 16 161.98 21.00 -1 -3 16 -5.90 9.50 -1 -3 16 2.80 9.80 -1 3 16 24.50 13.70 -4 -4 16 13.50 10.80 -4 -4 16 0.50 9.40 -4 -4 16 15.00 10.90 -4 4 16 23.40 11.70 4 4 -16 3.90 8.20 -3 -4 16 28.80 11.40 -3 -4 16 15.30 8.80 -3 -4 16 22.90 9.90 -3 -4 16 27.70 10.00 -3 4 16 53.49 13.40 -2 -4 16 182.68 21.10 -2 -4 16 153.28 18.70 -2 -4 16 169.18 17.30 -2 4 16 199.88 22.40 -1 -4 16 20.50 11.50 -1 -4 16 -6.00 8.80 -1 4 16 5.60 12.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 62062 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 C1 C 0.3717(2) 0.83158(14) 0.57766(14) 0.0160(4) Uani 1 1 d . . . . . C2 C 0.5496(2) 0.88709(13) 0.59535(15) 0.0177(4) Uani 1 1 d . . . . . H2A H 0.551545 0.924236 0.528355 0.021 Uiso 1 1 calc R U . . . H2B H 0.561544 0.934462 0.656176 0.021 Uiso 1 1 calc R U . . . C3 C 0.7059(2) 0.81460(13) 0.62233(14) 0.0149(4) Uani 1 1 d . . . . . H3 H 0.820559 0.851864 0.634014 0.018 Uiso 1 1 calc R U . . . C4 C 0.6914(2) 0.74245(14) 0.52725(14) 0.0153(4) Uani 1 1 d . . . . . H4 H 0.693515 0.779928 0.459580 0.018 Uiso 1 1 calc R U . . . C5 C 0.5122(2) 0.68762(13) 0.50863(14) 0.0155(4) Uani 1 1 d . . . . . H5 H 0.500250 0.641074 0.446002 0.019 Uiso 1 1 calc R U . . . C6 C 0.3547(2) 0.75945(14) 0.48244(14) 0.0174(4) Uani 1 1 d . . . . . H6A H 0.240920 0.722757 0.470554 0.021 Uiso 1 1 calc R U . . . H6B H 0.353619 0.795949 0.414559 0.021 Uiso 1 1 calc R U . . . C7 C 0.3715(2) 0.77411(14) 0.68244(14) 0.0174(4) Uani 1 1 d . . . . . H7A H 0.382967 0.820198 0.744393 0.021 Uiso 1 1 calc R U . . . H7B H 0.257277 0.738176 0.672297 0.021 Uiso 1 1 calc R U . . . C8 C 0.5277(2) 0.70147(13) 0.70784(13) 0.0145(4) Uani 1 1 d . . . . . H8 H 0.525776 0.663980 0.775552 0.017 Uiso 1 1 calc R U . . . C9 C 0.7070(2) 0.75635(13) 0.72659(14) 0.0141(4) Uani 1 1 d . . . . . H9 H 0.719222 0.802952 0.789184 0.017 Uiso 1 1 calc R U . . . C10 C 0.8468(2) 0.66966(14) 0.55285(15) 0.0186(4) Uani 1 1 d . . . . . H10A H 0.961149 0.705463 0.563079 0.022 Uiso 1 1 calc R U . . . H10B H 0.835250 0.623679 0.490794 0.022 Uiso 1 1 calc R U . . . C11 C 0.5126(2) 0.62898(13) 0.61268(14) 0.0158(4) Uani 1 1 d . . . . . H11 H 0.397909 0.591744 0.600917 0.019 Uiso 1 1 calc R U . . . C12 C 0.6695(3) 0.55662(13) 0.63896(15) 0.0196(4) Uani 1 1 d . . . . . H12A H 0.667508 0.518803 0.705518 0.024 Uiso 1 1 calc R U . . . H12B H 0.657645 0.509801 0.577629 0.024 Uiso 1 1 calc R U . . . C13 C 0.8468(2) 0.61193(14) 0.65730(15) 0.0175(4) Uani 1 1 d . . . . . C14 C 0.8635(2) 0.68395(14) 0.75275(14) 0.0176(4) Uani 1 1 d . . . . . H14A H 0.863566 0.647293 0.820379 0.021 Uiso 1 1 calc R U . . . H14B H 0.977751 0.720264 0.765204 0.021 Uiso 1 1 calc R U . . . S1A S 0.1745(4) 0.9116(2) 0.5493(3) 0.0229(5) Uani 0.54 1 d . . P A 1 H1A H 0.042236 0.863092 0.516382 0.028 Uiso 0.54 1 calc R U P A 1 P1A P 1.0519(3) 0.53358(18) 0.6908(2) 0.0207(4) Uani 0.54 1 d . . P B 1 H1AA H 1.010200 0.484700 0.764900 0.025 Uiso 0.54 1 d . U P C 1 H1AB H 0.993600 0.474400 0.612300 0.025 Uiso 0.54 1 d . U P D 1 S1 S 1.0243(4) 0.5193(2) 0.6821(3) 0.0276(8) Uiso 0.46 1 d . . P B 2 H1 H 1.166386 0.558397 0.716892 0.033 Uiso 0.46 1 calc R U P B 2 P1 P 0.1940(6) 0.9270(3) 0.5533(4) 0.0234(9) Uiso 0.46 1 d . . P A 2 H1B H 0.156000 0.987200 0.605700 0.028 Uiso 0.46 1 d . U P E 2 H1C H 0.177500 0.945200 0.464200 0.028 Uiso 0.46 1 d . U P F 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 C1 0.0149(9) 0.0190(9) 0.0138(8) 0.0015(7) 0.0029(7) 0.0027(7) C2 0.0193(9) 0.0146(9) 0.0185(9) 0.0022(7) 0.0036(7) -0.0014(7) C3 0.0143(9) 0.0137(9) 0.0161(8) -0.0004(7) 0.0028(7) -0.0039(7) C4 0.0175(9) 0.0180(9) 0.0113(8) 0.0016(7) 0.0055(7) -0.0017(7) C5 0.0187(9) 0.0181(9) 0.0094(8) -0.0030(7) 0.0027(7) -0.0037(7) C6 0.0165(9) 0.0233(10) 0.0107(8) 0.0003(7) 0.0002(7) -0.0029(8) C7 0.0167(9) 0.0227(10) 0.0138(9) -0.0005(7) 0.0057(7) 0.0000(7) C8 0.0167(9) 0.0179(9) 0.0095(8) 0.0025(7) 0.0045(7) -0.0007(7) C9 0.0149(9) 0.0147(8) 0.0112(8) -0.0028(7) 0.0007(7) -0.0014(7) C10 0.0197(9) 0.0211(10) 0.0166(9) -0.0001(7) 0.0075(7) 0.0012(8) C11 0.0174(9) 0.0152(9) 0.0146(8) -0.0007(7) 0.0039(7) -0.0054(7) C12 0.0275(10) 0.0131(9) 0.0191(9) 0.0003(7) 0.0073(8) -0.0017(8) C13 0.0195(9) 0.0165(9) 0.0167(9) 0.0022(7) 0.0054(7) 0.0045(7) C14 0.0160(9) 0.0215(10) 0.0138(8) 0.0005(7) 0.0010(7) 0.0009(7) S1A 0.0140(9) 0.0212(11) 0.0319(9) 0.0061(8) 0.0026(6) 0.0085(8) P1A 0.0142(8) 0.0167(8) 0.0304(9) 0.0047(7) 0.0042(7) 0.0076(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 C1 C7 108.88(14) . . ? C2 C1 S1A 113.93(16) . . ? C2 C1 P1 106.10(17) . . ? C6 C1 C2 108.92(15) . . ? C6 C1 C7 109.27(15) . . ? C6 C1 S1A 109.12(16) . . ? C6 C1 P1 113.98(17) . . ? C7 C1 S1A 106.63(16) . . ? C7 C1 P1 109.55(18) . . ? C1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 C2 C1 110.02(15) . . ? C3 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C2 C3 H3 109.0 . . ? C2 C3 C4 110.10(14) . . ? C2 C3 C9 110.79(14) . . ? C4 C3 H3 109.0 . . ? C4 C3 C9 108.89(14) . . ? C9 C3 H3 109.0 . . ? C3 C4 H4 109.2 . . ? C3 C4 C5 108.28(14) . . ? C5 C4 H4 109.2 . . ? C10 C4 C3 110.74(14) . . ? C10 C4 H4 109.2 . . ? C10 C4 C5 110.27(15) . . ? C4 C5 H5 109.1 . . ? C6 C5 C4 111.03(15) . . ? C6 C5 H5 109.1 . . ? C6 C5 C11 110.10(14) . . ? C11 C5 C4 108.48(14) . . ? C11 C5 H5 109.1 . . ? C1 C6 H6A 109.7 . . ? C1 C6 H6B 109.7 . . ? C5 C6 C1 109.63(14) . . ? C5 C6 H6A 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C1 C7 H7A 109.8 . . ? C1 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C8 C7 C1 109.56(14) . . ? C8 C7 H7A 109.8 . . ? C8 C7 H7B 109.8 . . ? C7 C8 H8 109.0 . . ? C7 C8 C9 110.49(15) . . ? C7 C8 C11 110.69(14) . . ? C9 C8 H8 109.0 . . ? C11 C8 H8 109.0 . . ? C11 C8 C9 108.50(14) . . ? C3 C9 C8 108.17(13) . . ? C3 C9 H9 109.2 . . ? C8 C9 H9 109.2 . . ? C14 C9 C3 110.40(14) . . ? C14 C9 C8 110.62(15) . . ? C14 C9 H9 109.2 . . ? C4 C10 H10A 109.7 . . ? C4 C10 H10B 109.7 . . ? C4 C10 C13 109.96(14) . . ? H10A C10 H10B 108.2 . . ? C13 C10 H10A 109.7 . . ? C13 C10 H10B 109.7 . . ? C5 C11 H11 109.2 . . ? C8 C11 C5 108.55(14) . . ? C8 C11 H11 109.2 . . ? C12 C11 C5 110.33(15) . . ? C12 C11 C8 110.26(14) . . ? C12 C11 H11 109.2 . . ? C11 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C13 C12 C11 110.23(15) . . ? C13 C12 H12A 109.6 . . ? C13 C12 H12B 109.6 . . ? C10 C13 P1A 107.50(15) . . ? C10 C13 S1 109.59(17) . . ? C12 C13 C10 108.60(15) . . ? C12 C13 C14 109.03(15) . . ? C12 C13 P1A 115.45(15) . . ? C12 C13 S1 106.88(15) . . ? C14 C13 C10 109.21(15) . . ? C14 C13 P1A 106.92(15) . . ? C14 C13 S1 113.40(16) . . ? C9 C14 C13 109.84(14) . . ? C9 C14 H14A 109.7 . . ? C9 C14 H14B 109.7 . . ? C13 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C1 S1A H1A 109.5 . . ? C13 P1A H1AA 96.1 . . ? C13 P1A H1AB 94.2 . . ? H1AA P1A H1AB 97.9 . . ? C13 S1 H1 109.5 . . ? C1 P1 H1B 134.2 . . ? C1 P1 H1C 102.1 . . ? H1B P1 H1C 116.2 . . ? 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 C2 1.536(2) . ? C1 C6 1.533(2) . ? C1 C7 1.539(2) . ? C1 S1A 1.836(3) . ? C1 P1 1.860(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.532(2) . ? C3 H3 1.0000 . ? C3 C4 1.534(2) . ? C3 C9 1.537(2) . ? C4 H4 1.0000 . ? C4 C5 1.539(2) . ? C4 C10 1.529(2) . ? C5 H5 1.0000 . ? C5 C6 1.533(3) . ? C5 C11 1.538(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.532(2) . ? C8 H8 1.0000 . ? C8 C9 1.541(2) . ? C8 C11 1.538(2) . ? C9 H9 1.0000 . ? C9 C14 1.532(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C13 1.537(3) . ? C11 H11 1.0000 . ? C11 C12 1.533(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.531(3) . ? C13 C14 1.535(3) . ? C13 P1A 1.870(3) . ? C13 S1 1.833(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? S1A H1A 1.2000 . ? P1A H1AA 1.2567 . ? P1A H1AB 1.2690 . ? S1 H1 1.2000 . ? P1 H1B 1.1400 . ? P1 H1C 1.1278 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 60.78(18) . . . . ? C1 C2 C3 C9 -59.72(18) . . . . ? C1 C7 C8 C9 60.75(18) . . . . ? C1 C7 C8 C11 -59.47(19) . . . . ? C2 C1 C6 C5 58.93(18) . . . . ? C2 C1 C7 C8 -59.66(19) . . . . ? C2 C3 C4 C5 -59.09(18) . . . . ? C2 C3 C4 C10 179.90(14) . . . . ? C2 C3 C9 C8 58.73(18) . . . . ? C2 C3 C9 C14 179.89(14) . . . . ? C3 C4 C5 C6 58.89(18) . . . . ? C3 C4 C5 C11 -62.22(18) . . . . ? C3 C4 C10 C13 59.26(19) . . . . ? C3 C9 C14 C13 -59.86(19) . . . . ? C4 C3 C9 C8 -62.49(18) . . . . ? C4 C3 C9 C14 58.67(18) . . . . ? C4 C5 C6 C1 -59.56(18) . . . . ? C4 C5 C11 C8 62.33(18) . . . . ? C4 C5 C11 C12 -58.59(18) . . . . ? C4 C10 C13 C12 59.82(19) . . . . ? C4 C10 C13 C14 -58.97(19) . . . . ? C4 C10 C13 P1A -174.63(15) . . . . ? C4 C10 C13 S1 176.24(16) . . . . ? C5 C4 C10 C13 -60.56(18) . . . . ? C5 C11 C12 C13 59.91(19) . . . . ? C6 C1 C2 C3 -59.93(18) . . . . ? C6 C1 C7 C8 59.19(19) . . . . ? C6 C5 C11 C8 -59.36(18) . . . . ? C6 C5 C11 C12 179.72(14) . . . . ? C7 C1 C2 C3 59.15(19) . . . . ? C7 C1 C6 C5 -59.90(18) . . . . ? C7 C8 C9 C3 -59.34(17) . . . . ? C7 C8 C9 C14 179.63(13) . . . . ? C7 C8 C11 C5 59.05(18) . . . . ? C7 C8 C11 C12 -179.99(14) . . . . ? C8 C9 C14 C13 59.84(18) . . . . ? C8 C11 C12 C13 -59.98(19) . . . . ? C9 C3 C4 C5 62.55(18) . . . . ? C9 C3 C4 C10 -58.46(18) . . . . ? C9 C8 C11 C5 -62.35(18) . . . . ? C9 C8 C11 C12 58.61(18) . . . . ? C10 C4 C5 C6 -179.80(13) . . . . ? C10 C4 C5 C11 59.08(18) . . . . ? C10 C13 C14 C9 59.31(19) . . . . ? C11 C5 C6 C1 60.60(19) . . . . ? C11 C8 C9 C3 62.18(18) . . . . ? C11 C8 C9 C14 -58.84(17) . . . . ? C11 C12 C13 C10 -59.46(19) . . . . ? C11 C12 C13 C14 59.44(18) . . . . ? C11 C12 C13 P1A 179.78(15) . . . . ? C11 C12 C13 S1 -177.62(16) . . . . ? C12 C13 C14 C9 -59.21(19) . . . . ? S1A C1 C2 C3 178.01(16) . . . . ? S1A C1 C6 C5 -176.14(16) . . . . ? S1A C1 C7 C8 177.00(16) . . . . ? P1A C13 C14 C9 175.34(15) . . . . ? S1 C13 C14 C9 -178.16(16) . . . . ? P1 C1 C2 C3 176.97(18) . . . . ? P1 C1 C6 C5 177.17(18) . . . . ? P1 C1 C7 C8 -175.28(17) . . . . ?