#------------------------------------------------------------------------------ #$Date: 2019-06-01 03:26:27 +0300 (Sat, 01 Jun 2019) $ #$Revision: 215644 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/11/1551190.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_1551190 loop_ _publ_author_name 'Fataftah, Majed S.' 'Krzyaniak, Matthew D.' 'Vlaisavljevich, Bess' 'Wasielewski, Michael R.' 'Zadrozny, Joseph' 'Freedman, Danna' _publ_section_title ; Metal-Ligand Covalency Enables Room Temperature Molecular Qubit Candidates ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC00074G _journal_year 2019 _chemical_formula_moiety 'C18 H12 Se6 Ti, 2(C24 H20 P)' _chemical_formula_sum 'C66 H52 P2 Se6 Ti' _chemical_formula_weight 1428.67 _chemical_name_systematic 'tetraphenyl phosphonium titanium(IV) tris(diselenocatecholate)' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc210d8r _audit_creation_date 2018-03-07 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-11-05 deposited with the CCDC. 2019-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 114.114(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 25.191(3) _cell_length_b 13.8608(13) _cell_length_c 17.8294(18) _cell_measurement_reflns_used 9771 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.84 _cell_measurement_theta_min 2.40 _cell_volume 5682.2(11) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 99.95 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_unetI/netI 0.0219 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 80453 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.035 _diffrn_reflns_theta_min 1.715 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.092 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0783 before and 0.0479 after correction. The Ratio of minimum to maximum transmission is 0.8384. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'dull dark green' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.670 _exptl_crystal_description plate _exptl_crystal_F_000 2816 _exptl_crystal_preparation 'Synthesized by reaction of Ti(NMe2)4 with diseleno catechol in DMF with Ph4PBr' _exptl_crystal_recrystallization_method 'Crystallized from DMF at -35 C' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.647 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 339 _refine_ls_number_reflns 6847 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0248 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+12.7200P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.0604 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6009 _reflns_number_total 6847 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc00074g2.cif _cod_data_source_block msf5_123 _cod_original_cell_volume 5682.1(11) _cod_database_code 1551190 _shelx_shelxl_version_number 2016/6 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C008(H008), C00A(H00A), C00B(H00B), C00E(H00E), C00F(H00F), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012) ; _shelx_res_file ; TITL msf5_123_a.res in C2/c msf5_123.res created by SHELXL-2016/6 at 06:26:46 on 07-Mar-2018 REM Old TITL MSF5_123 in C2/c REM SHELXT solution in C2/c REM R1 0.063, Rweak 0.004, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C66 P2 Ti Se6 CELL 0.71073 25.1907 13.8608 17.8294 90 114.114 90 ZERR 4 0.0031 0.0013 0.0018 0 0.01 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H P Se Ti UNIT 264 208 8 24 4 L.S. 4 PLAN 20 TEMP -173.2 BOND $H list 4 fmap 2 acta OMIT -4 6 5 OMIT -7 1 5 OMIT -5 7 2 OMIT 1 1 5 OMIT -2 4 3 REM REM REM WGHT 0.025000 12.720000 FVAR 0.13493 SE01 4 0.453045 0.332635 0.819258 11.00000 0.01579 0.01591 = 0.01614 -0.00240 0.00542 0.00224 SE02 4 0.403020 0.236200 0.628574 11.00000 0.01572 0.01469 = 0.01569 -0.00179 0.00613 0.00018 SE03 4 0.511379 0.084712 0.662118 11.00000 0.01856 0.01559 = 0.02186 -0.00204 0.01245 0.00050 TI04 5 0.500000 0.220903 0.750000 10.50000 0.01338 0.01107 = 0.01637 0.00000 0.00709 0.00000 P005 3 0.317022 0.712296 0.669469 11.00000 0.01333 0.01289 = 0.01497 0.00116 0.00673 0.00043 C006 1 0.501237 -0.031980 0.711441 11.00000 0.01095 0.01484 = 0.02775 -0.00146 0.00719 0.00015 C007 1 0.247813 0.656624 0.646025 11.00000 0.01477 0.01122 = 0.01926 0.00297 0.00824 0.00133 C008 1 0.219939 0.605037 0.573162 11.00000 0.01720 0.01574 = 0.01849 0.00422 0.00979 0.00306 AFIX 43 H008 2 0.238548 0.595802 0.536877 11.00000 -1.20000 AFIX 0 C009 1 0.373738 0.348173 0.743508 11.00000 0.01576 0.01124 = 0.01909 0.00434 0.00699 0.00079 C00A 1 0.250922 0.879533 0.615315 11.00000 0.01479 0.01738 = 0.01574 -0.00096 0.00670 -0.00202 AFIX 43 H00A 2 0.217559 0.839585 0.600901 11.00000 -1.20000 AFIX 0 C00B 1 0.219978 0.670665 0.699233 11.00000 0.02117 0.01176 = 0.02281 0.00005 0.01178 0.00033 AFIX 43 H00B 2 0.239023 0.705153 0.749175 11.00000 -1.20000 AFIX 0 C00C 1 0.306439 0.839253 0.649518 11.00000 0.01674 0.01258 = 0.01417 -0.00111 0.00725 -0.00052 C00D 1 0.354318 0.311798 0.663542 11.00000 0.01585 0.00890 = 0.02238 0.00349 0.00916 0.00146 C00E 1 0.359740 0.559120 0.610408 11.00000 0.01819 0.01328 = 0.02090 0.00165 0.00826 0.00025 AFIX 43 H00E 2 0.345085 0.519106 0.640862 11.00000 -1.20000 AFIX 0 C00F 1 0.389650 0.518741 0.567901 11.00000 0.01859 0.01780 = 0.02585 -0.00231 0.00799 0.00218 AFIX 43 H00F 2 0.396569 0.451192 0.570555 11.00000 -1.20000 AFIX 0 C00G 1 0.351186 0.659265 0.608301 11.00000 0.01293 0.01492 = 0.01556 -0.00065 0.00572 0.00189 C00H 1 0.244724 0.978409 0.602463 11.00000 0.01785 0.01719 = 0.01797 0.00187 0.00577 0.00456 AFIX 43 H00H 2 0.207014 1.006403 0.580010 11.00000 -1.20000 AFIX 0 C00I 1 0.371329 0.717294 0.561610 11.00000 0.01418 0.01462 = 0.01622 0.00017 0.00453 -0.00048 AFIX 43 H00I 2 0.365498 0.785112 0.559945 11.00000 -1.20000 AFIX 0 C00J 1 0.409511 0.577159 0.521388 11.00000 0.01602 0.02328 = 0.02243 -0.00445 0.00961 0.00005 AFIX 43 H00J 2 0.429783 0.549158 0.492079 11.00000 -1.20000 AFIX 0 C00K 1 0.164890 0.567283 0.553958 11.00000 0.01831 0.01556 = 0.01914 0.00147 0.00644 0.00064 AFIX 43 H00K 2 0.145952 0.531466 0.504721 11.00000 -1.20000 AFIX 0 C00L 1 0.363671 0.698539 0.776836 11.00000 0.01514 0.02101 = 0.01725 0.00396 0.00805 0.00011 C00M 1 0.164720 0.634044 0.678562 11.00000 0.02265 0.01693 = 0.02657 0.00136 0.01638 0.00158 AFIX 43 H00M 2 0.145354 0.644678 0.713718 11.00000 -1.20000 AFIX 0 C00N 1 0.334852 0.398778 0.767060 11.00000 0.02113 0.01225 = 0.02212 0.00196 0.01152 0.00018 AFIX 43 H00N 2 0.347887 0.423842 0.821241 11.00000 -1.20000 AFIX 0 C00O 1 0.277537 0.412698 0.712167 11.00000 0.02049 0.01376 = 0.02927 0.00549 0.01443 0.00207 AFIX 43 H00O 2 0.251570 0.447480 0.728588 11.00000 -1.20000 AFIX 0 C00P 1 0.296330 0.325955 0.609143 11.00000 0.01914 0.01340 = 0.01996 0.00251 0.00597 -0.00089 AFIX 43 H00P 2 0.282994 0.301001 0.554894 11.00000 -1.20000 AFIX 0 C00Q 1 0.401148 0.619859 0.804870 11.00000 0.01641 0.01684 = 0.02365 0.00345 0.00793 -0.00319 AFIX 43 H00Q 2 0.402502 0.572391 0.767255 11.00000 -1.20000 AFIX 0 C00R 1 0.500696 -0.120145 0.672603 11.00000 0.01394 0.02015 = 0.03445 -0.00782 0.00766 -0.00025 AFIX 43 H00R 2 0.500854 -0.120539 0.619412 11.00000 -1.20000 AFIX 0 C00S 1 0.293380 1.036410 0.622285 11.00000 0.02215 0.01219 = 0.02096 -0.00083 0.00803 0.00062 AFIX 43 H00S 2 0.288799 1.103863 0.612274 11.00000 -1.20000 AFIX 0 C00T 1 0.355412 0.898539 0.671139 11.00000 0.01556 0.01621 = 0.02105 -0.00080 0.00671 0.00050 AFIX 43 H00T 2 0.393256 0.871269 0.695792 11.00000 -1.20000 AFIX 0 C00U 1 0.137502 0.581718 0.606432 11.00000 0.01530 0.01820 = 0.02791 0.00441 0.01055 0.00012 AFIX 43 H00U 2 0.099836 0.555646 0.592995 11.00000 -1.20000 AFIX 0 C00V 1 0.400013 0.675792 0.517394 11.00000 0.01787 0.02370 = 0.01847 -0.00118 0.00914 -0.00386 AFIX 43 H00V 2 0.413027 0.715049 0.484582 11.00000 -1.20000 AFIX 0 C00W 1 0.258175 0.375309 0.632589 11.00000 0.01677 0.01564 = 0.02834 0.00694 0.00798 0.00153 AFIX 43 H00W 2 0.218876 0.383919 0.594873 11.00000 -1.20000 AFIX 0 C00X 1 0.348847 0.996643 0.656711 11.00000 0.01920 0.01610 = 0.02453 -0.00172 0.00820 -0.00262 AFIX 43 H00X 2 0.382071 1.036735 0.670246 11.00000 -1.20000 AFIX 0 C00Y 1 0.499932 -0.206869 0.711077 11.00000 0.01394 0.01498 = 0.04923 -0.00722 0.00631 0.00050 AFIX 43 H00Y 2 0.499316 -0.266215 0.684077 11.00000 -1.20000 AFIX 0 C00Z 1 0.362190 0.768266 0.832567 11.00000 0.02441 0.03038 = 0.01955 0.00010 0.00952 0.00614 AFIX 43 H00Z 2 0.336759 0.822020 0.813742 11.00000 -1.20000 AFIX 0 C010 1 0.436386 0.611318 0.887872 11.00000 0.01730 0.02735 = 0.02581 0.00963 0.00712 0.00034 AFIX 43 H010 2 0.461801 0.557601 0.907126 11.00000 -1.20000 AFIX 0 C011 1 0.434851 0.680612 0.943110 11.00000 0.02355 0.04543 = 0.01680 0.00599 0.00662 0.00107 AFIX 43 H011 2 0.459154 0.674365 0.999955 11.00000 -1.20000 AFIX 0 C012 1 0.397825 0.758826 0.915163 11.00000 0.03432 0.04100 = 0.01974 -0.00214 0.01126 0.00564 AFIX 43 H012 2 0.396879 0.806367 0.952978 11.00000 -1.20000 AFIX 0 HKLF 4 REM msf5_123_a.res in C2/c REM R1 = 0.0248 for 6009 Fo > 4sig(Fo) and 0.0320 for all 6847 data REM 339 parameters refined using 0 restraints END WGHT 0.0253 12.7376 REM Highest difference peak 0.647, deepest hole -0.333, 1-sigma level 0.080 Q1 1 0.4897 0.0844 0.6070 11.00000 0.05 0.65 Q2 1 0.4281 0.2268 0.6842 11.00000 0.05 0.61 Q3 1 0.3405 0.7028 0.7276 11.00000 0.05 0.60 Q4 1 0.3823 0.2385 0.5737 11.00000 0.05 0.60 Q5 1 0.4741 0.3356 0.8786 11.00000 0.05 0.58 Q6 1 0.2820 0.6790 0.6587 11.00000 0.05 0.56 Q7 1 0.3747 0.2799 0.6459 11.00000 0.05 0.55 Q8 1 0.5363 0.0832 0.7204 11.00000 0.05 0.52 Q9 1 0.3669 0.2036 0.6221 11.00000 0.05 0.50 Q10 1 0.4230 0.3255 0.7607 11.00000 0.05 0.48 Q11 1 0.4844 0.3053 0.8192 11.00000 0.05 0.48 Q12 1 0.4017 0.3424 0.7711 11.00000 0.05 0.46 Q13 1 0.4383 0.2620 0.6272 11.00000 0.05 0.46 Q14 1 0.3257 0.3185 0.6401 11.00000 0.05 0.45 Q15 1 0.4165 0.3032 0.8095 11.00000 0.05 0.44 Q16 1 0.5537 0.0590 0.6877 11.00000 0.05 0.43 Q17 1 0.2259 0.6761 0.6598 11.00000 0.05 0.43 Q18 1 0.3676 0.3369 0.6995 11.00000 0.05 0.43 Q19 1 0.1968 0.6436 0.6876 11.00000 0.05 0.42 Q20 1 0.1575 0.5716 0.5887 11.00000 0.05 0.40 ; _shelx_res_checksum 94489 _olex2_exptl_crystal_mounting_method 'Mounted under paratone oil' _olex2_submission_original_sample_id 'compound 6' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 Se01 Se 0.45304(2) 0.33263(2) 0.81926(2) 0.01631(5) Uani 1 1 d . . . Se02 Se 0.40302(2) 0.23620(2) 0.62857(2) 0.01546(5) Uani 1 1 d . . . Se03 Se 0.51138(2) 0.08471(2) 0.66212(2) 0.01730(6) Uani 1 1 d . . . Ti04 Ti 0.500000 0.22090(4) 0.750000 0.01328(10) Uani 1 2 d S T P P005 P 0.31702(2) 0.71230(4) 0.66947(3) 0.01342(11) Uani 1 1 d . . . C006 C 0.50124(9) -0.03198(16) 0.71144(14) 0.0181(4) Uani 1 1 d . . . C007 C 0.24781(9) 0.65662(15) 0.64603(13) 0.0147(4) Uani 1 1 d . . . C008 C 0.21994(9) 0.60504(15) 0.57316(13) 0.0163(4) Uani 1 1 d . . . H008 H 0.238548 0.595802 0.536877 0.020 Uiso 1 1 calc R . . C009 C 0.37374(9) 0.34817(15) 0.74351(13) 0.0154(4) Uani 1 1 d . . . C00A C 0.25092(9) 0.87953(16) 0.61531(13) 0.0158(4) Uani 1 1 d . . . H00A H 0.217559 0.839585 0.600901 0.019 Uiso 1 1 calc R . . C00B C 0.21998(10) 0.67067(15) 0.69923(14) 0.0177(4) Uani 1 1 d . . . H00B H 0.239023 0.705153 0.749175 0.021 Uiso 1 1 calc R . . C00C C 0.30644(9) 0.83925(15) 0.64952(12) 0.0142(4) Uani 1 1 d . . . C00D C 0.35432(9) 0.31180(15) 0.66354(13) 0.0153(4) Uani 1 1 d . . . C00E C 0.35974(9) 0.55912(15) 0.61041(13) 0.0174(4) Uani 1 1 d . . . H00E H 0.345085 0.519106 0.640862 0.021 Uiso 1 1 calc R . . C00F C 0.38965(10) 0.51874(17) 0.56790(14) 0.0211(5) Uani 1 1 d . . . H00F H 0.396569 0.451192 0.570555 0.025 Uiso 1 1 calc R . . C00G C 0.35119(9) 0.65927(15) 0.60830(13) 0.0145(4) Uani 1 1 d . . . C00H C 0.24472(9) 0.97841(16) 0.60246(13) 0.0182(4) Uani 1 1 d . . . H00H H 0.207014 1.006403 0.580010 0.022 Uiso 1 1 calc R . . C00I C 0.37133(9) 0.71729(15) 0.56161(13) 0.0156(4) Uani 1 1 d . . . H00I H 0.365498 0.785112 0.559945 0.019 Uiso 1 1 calc R . . C00J C 0.40951(9) 0.57716(17) 0.52139(14) 0.0200(4) Uani 1 1 d . . . H00J H 0.429783 0.549158 0.492079 0.024 Uiso 1 1 calc R . . C00K C 0.16489(9) 0.56728(16) 0.55396(14) 0.0181(4) Uani 1 1 d . . . H00K H 0.145952 0.531466 0.504721 0.022 Uiso 1 1 calc R . . C00L C 0.36367(9) 0.69854(16) 0.77684(13) 0.0173(4) Uani 1 1 d . . . C00M C 0.16472(10) 0.63404(16) 0.67856(14) 0.0200(4) Uani 1 1 d . . . H00M H 0.145354 0.644678 0.713718 0.024 Uiso 1 1 calc R . . C00N C 0.33485(9) 0.39878(15) 0.76706(14) 0.0176(4) Uani 1 1 d . . . H00N H 0.347887 0.423842 0.821241 0.021 Uiso 1 1 calc R . . C00O C 0.27754(10) 0.41270(16) 0.71217(14) 0.0198(4) Uani 1 1 d . . . H00O H 0.251570 0.447480 0.728588 0.024 Uiso 1 1 calc R . . C00P C 0.29633(9) 0.32595(15) 0.60914(14) 0.0182(4) Uani 1 1 d . . . H00P H 0.282994 0.301001 0.554894 0.022 Uiso 1 1 calc R . . C00Q C 0.40115(9) 0.61986(16) 0.80487(14) 0.0190(4) Uani 1 1 d . . . H00Q H 0.402502 0.572391 0.767255 0.023 Uiso 1 1 calc R . . C00R C 0.50070(9) -0.12015(17) 0.67260(16) 0.0236(5) Uani 1 1 d . . . H00R H 0.500854 -0.120539 0.619412 0.028 Uiso 1 1 calc R . . C00S C 0.29338(10) 1.03641(16) 0.62229(13) 0.0187(4) Uani 1 1 d . . . H00S H 0.288799 1.103863 0.612274 0.022 Uiso 1 1 calc R . . C00T C 0.35541(9) 0.89854(16) 0.67114(13) 0.0179(4) Uani 1 1 d . . . H00T H 0.393256 0.871269 0.695792 0.021 Uiso 1 1 calc R . . C00U C 0.13750(9) 0.58172(16) 0.60643(14) 0.0199(4) Uani 1 1 d . . . H00U H 0.099836 0.555646 0.592995 0.024 Uiso 1 1 calc R . . C00V C 0.40001(9) 0.67579(17) 0.51739(14) 0.0195(4) Uani 1 1 d . . . H00V H 0.413027 0.715049 0.484582 0.023 Uiso 1 1 calc R . . C00W C 0.25817(10) 0.37531(16) 0.63259(14) 0.0207(5) Uani 1 1 d . . . H00W H 0.218876 0.383919 0.594873 0.025 Uiso 1 1 calc R . . C00X C 0.34885(10) 0.99664(16) 0.65671(14) 0.0202(4) Uani 1 1 d . . . H00X H 0.382071 1.036735 0.670246 0.024 Uiso 1 1 calc R . . C00Y C 0.49993(10) -0.20687(17) 0.71108(17) 0.0282(6) Uani 1 1 d . . . H00Y H 0.499316 -0.266215 0.684077 0.034 Uiso 1 1 calc R . . C00Z C 0.36219(10) 0.76827(19) 0.83257(14) 0.0246(5) Uani 1 1 d . . . H00Z H 0.336759 0.822020 0.813742 0.030 Uiso 1 1 calc R . . C010 C 0.43639(10) 0.61132(18) 0.88787(15) 0.0240(5) Uani 1 1 d . . . H010 H 0.461801 0.557601 0.907126 0.029 Uiso 1 1 calc R . . C011 C 0.43485(11) 0.6806(2) 0.94311(15) 0.0291(6) Uani 1 1 d . . . H011 H 0.459154 0.674365 0.999955 0.035 Uiso 1 1 calc R . . C012 C 0.39783(12) 0.7588(2) 0.91516(15) 0.0316(6) Uani 1 1 d . . . H012 H 0.396879 0.806367 0.952978 0.038 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 Se01 0.01579(10) 0.01591(11) 0.01614(10) -0.00240(8) 0.00542(8) 0.00224(8) Se02 0.01572(10) 0.01469(10) 0.01569(10) -0.00179(8) 0.00613(8) 0.00018(8) Se03 0.01856(11) 0.01559(11) 0.02186(11) -0.00204(8) 0.01245(9) 0.00050(8) Ti04 0.0134(2) 0.0111(2) 0.0164(2) 0.000 0.0071(2) 0.000 P005 0.0133(2) 0.0129(2) 0.0150(2) 0.00116(19) 0.0067(2) 0.0004(2) C006 0.0109(9) 0.0148(10) 0.0277(12) -0.0015(9) 0.0072(9) 0.0002(8) C007 0.0148(10) 0.0112(9) 0.0193(10) 0.0030(8) 0.0082(8) 0.0013(8) C008 0.0172(10) 0.0157(10) 0.0185(10) 0.0042(8) 0.0098(8) 0.0031(8) C009 0.0158(10) 0.0112(9) 0.0191(10) 0.0043(8) 0.0070(8) 0.0008(8) C00A 0.0148(10) 0.0174(10) 0.0157(10) -0.0010(8) 0.0067(8) -0.0020(8) C00B 0.0212(11) 0.0118(10) 0.0228(11) 0.0000(8) 0.0118(9) 0.0003(8) C00C 0.0167(10) 0.0126(10) 0.0142(9) -0.0011(7) 0.0072(8) -0.0005(8) C00D 0.0158(10) 0.0089(9) 0.0224(11) 0.0035(8) 0.0092(8) 0.0015(8) C00E 0.0182(10) 0.0133(10) 0.0209(11) 0.0016(8) 0.0083(9) 0.0003(8) C00F 0.0186(11) 0.0178(11) 0.0259(11) -0.0023(9) 0.0080(9) 0.0022(9) C00G 0.0129(9) 0.0149(10) 0.0156(10) -0.0007(8) 0.0057(8) 0.0019(8) C00H 0.0178(10) 0.0172(10) 0.0180(10) 0.0019(8) 0.0058(8) 0.0046(8) C00I 0.0142(9) 0.0146(10) 0.0162(10) 0.0002(8) 0.0045(8) -0.0005(8) C00J 0.0160(10) 0.0233(12) 0.0224(11) -0.0044(9) 0.0096(9) 0.0000(9) C00K 0.0183(10) 0.0156(10) 0.0191(10) 0.0015(8) 0.0064(9) 0.0006(8) C00L 0.0151(10) 0.0210(11) 0.0172(10) 0.0040(8) 0.0081(8) 0.0001(8) C00M 0.0227(11) 0.0169(11) 0.0266(11) 0.0014(9) 0.0164(10) 0.0016(9) C00N 0.0211(11) 0.0122(10) 0.0221(11) 0.0020(8) 0.0115(9) 0.0002(8) C00O 0.0205(11) 0.0138(10) 0.0293(12) 0.0055(9) 0.0144(9) 0.0021(8) C00P 0.0191(11) 0.0134(10) 0.0200(11) 0.0025(8) 0.0060(9) -0.0009(8) C00Q 0.0164(10) 0.0168(10) 0.0237(11) 0.0035(9) 0.0079(9) -0.0032(8) C00R 0.0139(10) 0.0202(11) 0.0345(13) -0.0078(10) 0.0077(9) -0.0003(9) C00S 0.0221(11) 0.0122(10) 0.0210(11) -0.0008(8) 0.0080(9) 0.0006(8) C00T 0.0156(10) 0.0162(10) 0.0210(11) -0.0008(8) 0.0067(8) 0.0005(8) C00U 0.0153(10) 0.0182(11) 0.0279(12) 0.0044(9) 0.0106(9) 0.0001(8) C00V 0.0179(10) 0.0237(11) 0.0185(10) -0.0012(9) 0.0091(9) -0.0039(9) C00W 0.0168(10) 0.0156(10) 0.0283(12) 0.0069(9) 0.0080(9) 0.0015(8) C00X 0.0192(11) 0.0161(10) 0.0245(11) -0.0017(9) 0.0082(9) -0.0026(9) C00Y 0.0139(10) 0.0150(11) 0.0492(15) -0.0072(10) 0.0063(11) 0.0005(9) C00Z 0.0244(12) 0.0304(13) 0.0196(11) 0.0001(10) 0.0095(9) 0.0061(10) C010 0.0173(11) 0.0274(12) 0.0258(12) 0.0096(10) 0.0071(9) 0.0003(9) C011 0.0235(12) 0.0454(16) 0.0168(11) 0.0060(11) 0.0066(10) 0.0011(11) C012 0.0343(14) 0.0410(15) 0.0197(12) -0.0021(11) 0.0113(11) 0.0056(12) 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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 C009 Se01 Ti04 106.47(7) . . C00D Se02 Ti04 107.03(7) . . C006 Se03 Ti04 105.98(7) . . Se01 Ti04 Se01 105.30(2) 2_656 . Se02 Ti04 Se01 83.491(13) 2_656 2_656 Se02 Ti04 Se01 90.659(14) 2_656 . Se02 Ti04 Se01 90.659(14) . 2_656 Se02 Ti04 Se01 83.490(12) . . Se02 Ti04 Se02 170.37(3) 2_656 . Se02 Ti04 Se03 81.212(12) 2_656 2_656 Se02 Ti04 Se03 106.105(14) . 2_656 Se02 Ti04 Se03 106.106(14) 2_656 . Se02 Ti04 Se03 81.212(12) . . Se03 Ti04 Se01 159.975(12) 2_656 2_656 Se03 Ti04 Se01 159.973(12) . . Se03 Ti04 Se01 87.772(10) 2_656 . Se03 Ti04 Se01 87.774(10) . 2_656 Se03 Ti04 Se03 84.15(2) . 2_656 C007 P005 C00C 108.93(10) . . C007 P005 C00G 110.07(10) . . C007 P005 C00L 110.63(10) . . C00C P005 C00G 110.47(10) . . C00C P005 C00L 107.11(10) . . C00G P005 C00L 109.58(10) . . C006 C006 Se03 121.35(7) 2_656 . C006 C006 C00R 119.29(14) 2_656 . C00R C006 Se03 119.18(18) . . C008 C007 P005 120.61(16) . . C008 C007 C00B 119.98(19) . . C00B C007 P005 119.28(16) . . C007 C008 H008 120.2 . . C00K C008 C007 119.7(2) . . C00K C008 H008 120.2 . . C00D C009 Se01 120.58(16) . . C00D C009 C00N 119.32(19) . . C00N C009 Se01 120.08(16) . . C00C C00A H00A 120.2 . . C00H C00A H00A 120.2 . . C00H C00A C00C 119.5(2) . . C007 C00B H00B 120.2 . . C00M C00B C007 119.7(2) . . C00M C00B H00B 120.2 . . C00A C00C P005 121.40(16) . . C00A C00C C00T 119.97(19) . . C00T C00C P005 118.61(16) . . C009 C00D Se02 121.94(15) . . C00P C00D Se02 118.75(16) . . C00P C00D C009 119.19(19) . . C00F C00E H00E 120.1 . . C00F C00E C00G 119.8(2) . . C00G C00E H00E 120.1 . . C00E C00F H00F 120.0 . . C00E C00F C00J 120.0(2) . . C00J C00F H00F 120.0 . . C00E C00G P005 119.62(16) . . C00I C00G P005 120.48(16) . . C00I C00G C00E 119.84(19) . . C00A C00H H00H 119.9 . . C00S C00H C00A 120.2(2) . . C00S C00H H00H 119.9 . . C00G C00I H00I 120.0 . . C00V C00I C00G 120.0(2) . . C00V C00I H00I 120.0 . . C00F C00J H00J 119.7 . . C00V C00J C00F 120.6(2) . . C00V C00J H00J 119.7 . . C008 C00K H00K 119.9 . . C00U C00K C008 120.1(2) . . C00U C00K H00K 119.9 . . C00Q C00L P005 121.06(17) . . C00Q C00L C00Z 119.8(2) . . C00Z C00L P005 119.15(17) . . C00B C00M H00M 120.0 . . C00B C00M C00U 120.1(2) . . C00U C00M H00M 120.0 . . C009 C00N H00N 119.6 . . C00O C00N C009 120.8(2) . . C00O C00N H00N 119.6 . . C00N C00O H00O 120.2 . . C00N C00O C00W 119.7(2) . . C00W C00O H00O 120.2 . . C00D C00P H00P 119.3 . . C00W C00P C00D 121.3(2) . . C00W C00P H00P 119.3 . . C00L C00Q H00Q 120.2 . . C010 C00Q C00L 119.6(2) . . C010 C00Q H00Q 120.2 . . C006 C00R H00R 119.7 . . C00Y C00R C006 120.7(2) . . C00Y C00R H00R 119.7 . . C00H C00S H00S 119.8 . . C00H C00S C00X 120.5(2) . . C00X C00S H00S 119.8 . . C00C C00T H00T 119.9 . . C00X C00T C00C 120.1(2) . . C00X C00T H00T 119.9 . . C00K C00U C00M 120.5(2) . . C00K C00U H00U 119.8 . . C00M C00U H00U 119.8 . . C00I C00V H00V 120.1 . . C00J C00V C00I 119.8(2) . . C00J C00V H00V 120.1 . . C00O C00W H00W 120.2 . . C00P C00W C00O 119.7(2) . . C00P C00W H00W 120.2 . . C00S C00X H00X 120.2 . . C00T C00X C00S 119.7(2) . . C00T C00X H00X 120.2 . . C00R C00Y H00Y 120.0 . . C00Y C00Y C00R 119.99(15) 2_656 . C00Y C00Y H00Y 120.0 2_656 . C00L C00Z H00Z 120.1 . . C012 C00Z C00L 119.8(2) . . C012 C00Z H00Z 120.1 . . C00Q C010 H010 119.7 . . C00Q C010 C011 120.5(2) . . C011 C010 H010 119.7 . . C010 C011 H011 120.1 . . C012 C011 C010 119.8(2) . . C012 C011 H011 120.1 . . C00Z C012 C011 120.4(2) . . C00Z C012 H012 119.8 . . C011 C012 H012 119.8 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Se01 Ti04 2.5526(4) . Se01 C009 1.912(2) . Se02 Ti04 2.5256(5) . Se02 C00D 1.902(2) . Se03 Ti04 2.5432(5) . Se03 C006 1.907(2) . P005 C007 1.793(2) . P005 C00C 1.794(2) . P005 C00G 1.799(2) . P005 C00L 1.801(2) . C006 C006 1.402(5) 2_656 C006 C00R 1.402(3) . C007 C008 1.395(3) . C007 C00B 1.405(3) . C008 H008 0.9500 . C008 C00K 1.388(3) . C009 C00D 1.399(3) . C009 C00N 1.401(3) . C00A H00A 0.9500 . C00A C00C 1.394(3) . C00A C00H 1.388(3) . C00B H00B 0.9500 . C00B C00M 1.383(3) . C00C C00T 1.399(3) . C00D C00P 1.398(3) . C00E H00E 0.9500 . C00E C00F 1.386(3) . C00E C00G 1.403(3) . C00F H00F 0.9500 . C00F C00J 1.390(3) . C00G C00I 1.394(3) . C00H H00H 0.9500 . C00H C00S 1.385(3) . C00I H00I 0.9500 . C00I C00V 1.393(3) . C00J H00J 0.9500 . C00J C00V 1.385(3) . C00K H00K 0.9500 . C00K C00U 1.385(3) . C00L C00Q 1.395(3) . C00L C00Z 1.398(3) . C00M H00M 0.9500 . C00M C00U 1.389(3) . C00N H00N 0.9500 . C00N C00O 1.387(3) . C00O H00O 0.9500 . C00O C00W 1.398(3) . C00P H00P 0.9500 . C00P C00W 1.377(3) . C00Q H00Q 0.9500 . C00Q C010 1.385(3) . C00R H00R 0.9500 . C00R C00Y 1.388(4) . C00S H00S 0.9500 . C00S C00X 1.390(3) . C00T H00T 0.9500 . C00T C00X 1.381(3) . C00U H00U 0.9500 . C00V H00V 0.9500 . C00W H00W 0.9500 . C00X H00X 0.9500 . C00Y C00Y 1.387(6) 2_656 C00Y H00Y 0.9500 . C00Z H00Z 0.9500 . C00Z C012 1.383(3) . C010 H010 0.9500 . C010 C011 1.387(4) . C011 H011 0.9500 . C011 C012 1.383(4) . C012 H012 0.9500 .