#------------------------------------------------------------------------------ #$Date: 2026-06-27 23:13:28 +0100 (Sat, 27 Jun 2026) $ #$Revision: 306669 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/74/1577455.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_1577455 loop_ _publ_author_name 'Sutcliffe, Erica' 'Aalto, Jonathan P.' 'Hadt, Ryan G.' _publ_section_title ; Excited-state orbital angular momentum enables all-optical molecular spin coherence ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC04497B _journal_year 2026 _chemical_formula_sum 'C12 H17 Na0.25 O2.25 W0.25' _chemical_formula_weight 248.96 _chemical_name_common '[Na(THF)4][WO(2,6-dimethylphenoxide)4]' _chemical_name_systematic '[Na(THF)4][WO(ODmp)4]' _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system tetragonal _space_group_IT_number 130 _space_group_name_Hall '-P 4a 2ac' _space_group_name_H-M_alt 'P 4/n c c :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2026-04-30 deposited with the CCDC. 2026-06-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 13.4381(4) _cell_length_b 13.4381(4) _cell_length_c 25.9450(13) _cell_measurement_reflns_used 9888 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.45 _cell_measurement_theta_min 2.66 _cell_volume 4685.2(3) _computing_cell_refinement 'SAINT v8.40A (Bruker-AXS, 2013)' _computing_data_collection 'APEX3 v2019.11-0 (Bruker Nano, 2020)' _computing_data_reduction 'SAINT v8.40A (Bruker-AXS, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.69 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0074 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 98370 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.657 _diffrn_source 'I\mS HB micro-focus sealed tube' _exptl_absorpt_coefficient_mu 2.527 _exptl_absorpt_correction_T_max 0.0998 _exptl_absorpt_correction_T_min 0.0680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Sheldrick, 2014)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 2052 _exptl_crystal_recrystallization_method 'Vapour deposition' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 2.423 _refine_diff_density_min -2.045 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 222 _refine_ls_number_reflns 2083 _refine_ls_number_restraints 507 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0364 _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^)+34.4048P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.0819 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1557 _reflns_number_total 2083 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc04497b2.cif _cod_data_source_block V26039 _cod_original_cell_volume 4685.2(4) _cod_original_sg_symbol_H-M 'P 4/n c c' _cod_database_code 1577455 _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 0.786 _shelx_estimated_absorpt_t_max 0.786 _shelx_res_file ; TITL V26039 in P4/ncc V26039.res created by SHELXL-2019/3 at 09:31:28 on 27-Jan-2026 CELL 0.71073 13.43810 13.43810 25.94500 90.0000 90.0000 90.0000 ZERR 16.00 0.00042 0.00042 0.00130 0.0000 0.0000 0.0000 LATT 1 SYMM 0.5-X, 0.5-Y, Z SYMM 0.5-Y, X, Z SYMM Y, 0.5-X, Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, -Y, 0.5-Z SYMM 0.5+Y, 0.5+X, 0.5-Z SYMM -Y, -X, 0.5-Z SFAC C H O NA W UNIT 192 272 36 4 4 TEMP -173 SIZE 0.10 0.10 0.10 OMIT 1 1 0 OMIT 0 1 2 ACTA WPDB -2 CONF L.S. 10 BOND $H FMAP 2 PLAN 20 simu w1 > c12 simu 0.01 c7 c7a c2 c2a rigu w1 > c12 WGHT 0.000000 34.404804 FVAR 0.04641 0.60467 O1 3 0.250000 0.250000 0.282352 10.25000 0.02840 0.02840 = 0.03265 0.00000 0.00000 0.00000 same w1 o2 c1 c6 c8 c5 c4 c3 c2 c7 same w1 o2a > c8a W1 5 0.250000 0.250000 0.349067 10.25000 0.02160 0.02160 = 0.02290 0.00000 0.00000 0.00000 PART 1 21 O2 3 0.349400 0.348351 0.371322 21.00000 0.02391 0.03015 = 0.03247 0.00206 -0.00055 -0.00293 C1 1 0.446033 0.339252 0.388625 21.00000 0.03405 0.03598 = 0.04824 0.00008 -0.00833 -0.00476 C2 1 0.524827 0.312227 0.356138 21.00000 0.03854 0.04037 = 0.05569 0.00253 0.00147 0.00019 C7 1 0.506179 0.300349 0.299311 21.00000 0.04276 0.04466 = 0.05732 0.00273 0.01224 -0.00321 AFIX 137 H7A 2 0.565570 0.320717 0.280097 21.00000 -1.50000 H7B 2 0.449707 0.342068 0.289099 21.00000 -1.50000 H7C 2 0.491110 0.230521 0.291710 21.00000 -1.50000 AFIX 0 C3 1 0.620485 0.311079 0.376549 21.00000 0.03805 0.04188 = 0.07510 0.01060 0.00070 0.00308 AFIX 43 H3 2 0.675072 0.296079 0.354618 21.00000 -1.20000 AFIX 0 C4 1 0.637985 0.331173 0.427810 21.00000 0.04195 0.04835 = 0.08158 0.00929 -0.01517 -0.00386 AFIX 43 H4 2 0.703520 0.326305 0.441309 21.00000 -1.20000 AFIX 0 C5 1 0.560910 0.358132 0.459235 21.00000 0.05016 0.04238 = 0.07036 0.00260 -0.01870 -0.00215 AFIX 43 H5 2 0.573429 0.373030 0.494436 21.00000 -1.20000 AFIX 0 C6 1 0.464634 0.363948 0.440239 21.00000 0.04444 0.03327 = 0.04900 0.00137 -0.00943 -0.00155 C8 1 0.381472 0.396766 0.473940 21.00000 0.04929 0.04572 = 0.04135 -0.01086 -0.00961 -0.01417 AFIX 137 H8A 2 0.346193 0.452153 0.457513 21.00000 -1.50000 H8B 2 0.408067 0.418530 0.507255 21.00000 -1.50000 H8C 2 0.335310 0.341258 0.479279 21.00000 -1.50000 AFIX 0 PART 2 -21 O2A 3 0.380331 0.201757 0.371778 -21.00000 0.03923 0.02924 = 0.04261 0.00518 -0.00699 0.00019 C1A 1 0.465941 0.249597 0.386971 -21.00000 0.02881 0.02132 = 0.03461 -0.00120 -0.00539 0.00458 C2A 1 0.524885 0.299304 0.350529 -21.00000 0.03746 0.03625 = 0.05149 0.00029 0.00492 -0.00030 C7A 1 0.494835 0.294166 0.294714 -21.00000 0.04377 0.04552 = 0.04661 0.00088 0.01043 0.00431 AFIX 137 H7A1 2 0.462748 0.356746 0.284717 -21.00000 -1.50000 H7A2 2 0.448179 0.238948 0.289731 -21.00000 -1.50000 H7A3 2 0.554011 0.283457 0.273347 -21.00000 -1.50000 AFIX 0 C3A 1 0.615174 0.338102 0.366787 -21.00000 0.04244 0.03390 = 0.07032 0.02133 -0.00485 -0.00477 AFIX 43 H3A 2 0.658067 0.369302 0.342579 -21.00000 -1.20000 AFIX 0 C4A 1 0.643156 0.331801 0.417647 -21.00000 0.04265 0.03607 = 0.07693 0.00684 -0.01362 -0.00537 AFIX 43 H4A 2 0.704306 0.360923 0.428138 -21.00000 -1.20000 AFIX 0 C5A 1 0.584957 0.284413 0.453823 -21.00000 0.04079 0.04233 = 0.05331 0.00182 -0.01822 0.00231 AFIX 43 H5A 2 0.606273 0.280343 0.488671 -21.00000 -1.20000 AFIX 0 C6A 1 0.494917 0.242653 0.438961 -21.00000 0.03900 0.03497 = 0.03499 -0.00181 -0.00720 0.00068 C8A 1 0.434016 0.180973 0.475385 -21.00000 0.03948 0.05004 = 0.04117 0.00347 -0.00213 0.00630 AFIX 137 H8A1 2 0.462546 0.185185 0.510079 -21.00000 -1.50000 H8A2 2 0.434210 0.111502 0.463897 -21.00000 -1.50000 H8A3 2 0.365504 0.205935 0.475978 -21.00000 -1.50000 AFIX 0 PART 0 same na1 o3 c12 < c9 NA1 4 0.250000 0.250000 0.194674 10.25000 0.02788 0.02788 = 0.03051 0.00000 0.00000 0.00000 O3 3 0.182135 0.098875 0.165579 11.00000 0.04280 0.04492 = 0.06129 -0.01138 0.00313 -0.00606 C9 1 0.098210 0.051713 0.188661 11.00000 0.05090 0.06285 = 0.06011 0.00084 0.00711 -0.00446 AFIX 23 H9A 2 0.037529 0.092549 0.184096 11.00000 -1.20000 H9B 2 0.109432 0.040972 0.225961 11.00000 -1.20000 AFIX 0 C10 1 0.088541 -0.045389 0.161024 11.00000 0.05286 0.05595 = 0.10786 -0.00460 0.00152 -0.00871 AFIX 23 H10A 2 0.134298 -0.095967 0.175447 11.00000 -1.20000 H10B 2 0.019485 -0.070878 0.162575 11.00000 -1.20000 AFIX 0 C11 1 0.116726 -0.018142 0.107829 11.00000 0.05808 0.08317 = 0.08692 -0.04049 0.00233 -0.01894 AFIX 23 H11A 2 0.060117 0.012305 0.089184 11.00000 -1.20000 H11B 2 0.140483 -0.076871 0.088354 11.00000 -1.20000 AFIX 0 C12 1 0.199951 0.056573 0.116119 11.00000 0.05477 0.06854 = 0.05848 -0.01834 0.00577 -0.01576 AFIX 23 H12A 2 0.265564 0.023117 0.115217 11.00000 -1.20000 H12B 2 0.198500 0.108613 0.089120 11.00000 -1.20000 AFIX 0 HKLF 4 REM V26039 in P4/ncc REM wR2 = 0.0819, GooF = S = 1.214, Restrained GooF = 1.092 for all data REM R1 = 0.0364 for 1557 Fo > 4sig(Fo) and 0.0511 for all 2083 data REM 222 parameters refined using 507 restraints END WGHT 0.0000 34.4043 REM Highest difference peak 2.423, deepest hole -2.045, 1-sigma level 0.118 Q1 1 0.2500 0.2500 0.4526 10.25000 0.05 2.42 Q2 1 0.2500 0.2500 0.0570 10.25000 0.05 1.40 Q3 1 0.0961 0.1758 0.1638 11.00000 0.05 1.05 Q4 1 0.2500 0.2500 0.3120 10.25000 0.05 0.85 Q5 1 0.3018 0.0585 0.1175 11.00000 0.05 0.73 Q6 1 0.2500 0.2500 0.1132 10.25000 0.05 0.70 Q7 1 0.1180 -0.1750 0.1286 11.00000 0.05 0.69 Q8 1 0.4476 0.1593 0.3899 11.00000 0.05 0.67 Q9 1 0.2500 0.2500 0.2191 10.25000 0.05 0.66 Q10 1 0.5221 0.1915 0.3530 11.00000 0.05 0.65 Q11 1 0.1423 -0.1662 0.0758 11.00000 0.05 0.64 Q12 1 0.5042 0.1989 0.2991 11.00000 0.05 0.60 Q13 1 0.3614 0.5632 0.4589 11.00000 0.05 0.59 Q14 1 0.2500 0.2500 0.5100 10.25000 0.05 0.58 Q15 1 0.3613 0.4591 0.4427 11.00000 0.05 0.58 Q16 1 0.3838 -0.0054 0.1083 11.00000 0.05 0.58 Q17 1 0.1866 0.2505 0.2462 11.00000 0.05 0.57 Q18 1 0.2520 0.2135 0.2334 11.00000 0.05 0.54 Q19 1 0.3131 0.2617 0.4844 11.00000 0.05 0.53 Q20 1 -0.0433 0.0887 0.1616 11.00000 0.05 0.52 ; _shelx_res_checksum 85111 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, 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 O1 O 0.250000 0.250000 0.2824(3) 0.0298(15) Uani 1 4 d S T P A . W1 W 0.250000 0.250000 0.34907(2) 0.02204(13) Uani 1 4 d DS TU P . . O2 O 0.3494(5) 0.3484(5) 0.3713(2) 0.0288(14) Uani 0.605(6) 1 d D U P A 1 C1 C 0.4460(6) 0.3393(7) 0.3886(3) 0.039(2) Uani 0.605(6) 1 d D U P A 1 C2 C 0.5248(10) 0.312(2) 0.3561(5) 0.045(3) Uani 0.605(6) 1 d D U P A 1 C7 C 0.506(2) 0.300(3) 0.2993(5) 0.048(3) Uani 0.605(6) 1 d D U P A 1 H7A H 0.565570 0.320717 0.280097 0.072 Uiso 0.605(6) 1 calc R U P A 1 H7B H 0.449707 0.342068 0.289099 0.072 Uiso 0.605(6) 1 calc R U P A 1 H7C H 0.491110 0.230521 0.291710 0.072 Uiso 0.605(6) 1 calc R U P A 1 C3 C 0.6205(9) 0.3111(12) 0.3765(6) 0.052(4) Uani 0.605(6) 1 d D U P A 1 H3 H 0.675072 0.296079 0.354618 0.062 Uiso 0.605(6) 1 calc R U P A 1 C4 C 0.6380(11) 0.331(2) 0.4278(6) 0.057(4) Uani 0.605(6) 1 d D U P A 1 H4 H 0.703520 0.326305 0.441309 0.069 Uiso 0.605(6) 1 calc R U P A 1 C5 C 0.5609(7) 0.3581(8) 0.4592(4) 0.054(3) Uani 0.605(6) 1 d D U P A 1 H5 H 0.573429 0.373030 0.494436 0.065 Uiso 0.605(6) 1 calc R U P A 1 C6 C 0.4646(7) 0.3639(7) 0.4402(3) 0.042(2) Uani 0.605(6) 1 d D U P A 1 C8 C 0.3815(7) 0.3968(8) 0.4739(3) 0.045(2) Uani 0.605(6) 1 d D U P A 1 H8A H 0.346193 0.452153 0.457513 0.068 Uiso 0.605(6) 1 calc R U P A 1 H8B H 0.408067 0.418530 0.507255 0.068 Uiso 0.605(6) 1 calc R U P A 1 H8C H 0.335310 0.341258 0.479279 0.068 Uiso 0.605(6) 1 calc R U P A 1 O2A O 0.3803(7) 0.2018(8) 0.3718(4) 0.037(2) Uani 0.395(6) 1 d D U P A 2 C1A C 0.4659(8) 0.2496(9) 0.3870(4) 0.028(2) Uani 0.395(6) 1 d D U P A 2 C2A C 0.5249(16) 0.299(3) 0.3505(7) 0.042(3) Uani 0.395(6) 1 d D U P A 2 C7A C 0.495(3) 0.294(5) 0.2947(7) 0.045(5) Uani 0.395(6) 1 d D U P A 2 H7A1 H 0.462748 0.356746 0.284717 0.068 Uiso 0.395(6) 1 calc R U P A 2 H7A2 H 0.448179 0.238948 0.289731 0.068 Uiso 0.395(6) 1 calc R U P A 2 H7A3 H 0.554011 0.283457 0.273347 0.068 Uiso 0.395(6) 1 calc R U P A 2 C3A C 0.6152(14) 0.3381(19) 0.3668(8) 0.049(5) Uani 0.395(6) 1 d D U P A 2 H3A H 0.658067 0.369302 0.342579 0.059 Uiso 0.395(6) 1 calc R U P A 2 C4A C 0.6432(16) 0.332(3) 0.4176(8) 0.052(5) Uani 0.395(6) 1 d D U P A 2 H4A H 0.704306 0.360923 0.428138 0.062 Uiso 0.395(6) 1 calc R U P A 2 C5A C 0.5850(10) 0.2844(11) 0.4538(6) 0.045(3) Uani 0.395(6) 1 d D U P A 2 H5A H 0.606273 0.280343 0.488671 0.055 Uiso 0.395(6) 1 calc R U P A 2 C6A C 0.4949(9) 0.2427(10) 0.4390(4) 0.036(3) Uani 0.395(6) 1 d D U P A 2 C8A C 0.4340(11) 0.1810(12) 0.4754(5) 0.044(3) Uani 0.395(6) 1 d D U P A 2 H8A1 H 0.462546 0.185185 0.510079 0.065 Uiso 0.395(6) 1 calc R U P A 2 H8A2 H 0.434210 0.111502 0.463897 0.065 Uiso 0.395(6) 1 calc R U P A 2 H8A3 H 0.365504 0.205935 0.475978 0.065 Uiso 0.395(6) 1 calc R U P A 2 Na1 Na 0.250000 0.250000 0.19467(14) 0.0288(8) Uani 1 4 d DS T P . . O3 O 0.1821(3) 0.0989(3) 0.16558(16) 0.0497(10) Uani 1 1 d D U . . . C9 C 0.0982(5) 0.0517(5) 0.1887(3) 0.0580(16) Uani 1 1 d D U . . . H9A H 0.037529 0.092549 0.184096 0.070 Uiso 1 1 calc R U . . . H9B H 0.109432 0.040972 0.225961 0.070 Uiso 1 1 calc R U . . . C10 C 0.0885(6) -0.0454(5) 0.1610(3) 0.072(2) Uani 1 1 d D U . . . H10A H 0.134298 -0.095967 0.175447 0.087 Uiso 1 1 calc R U . . . H10B H 0.019485 -0.070878 0.162575 0.087 Uiso 1 1 calc R U . . . C11 C 0.1167(6) -0.0181(6) 0.1078(3) 0.076(2) Uani 1 1 d D U . . . H11A H 0.060117 0.012305 0.089184 0.091 Uiso 1 1 calc R U . . . H11B H 0.140483 -0.076871 0.088354 0.091 Uiso 1 1 calc R U . . . C12 C 0.2000(5) 0.0566(6) 0.1161(3) 0.0606(18) Uani 1 1 d D U . . . H12A H 0.265564 0.023117 0.115217 0.073 Uiso 1 1 calc R U . . . H12B H 0.198500 0.108613 0.089120 0.073 Uiso 1 1 calc R U . . . 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 O1 0.028(2) 0.028(2) 0.033(4) 0.000 0.000 0.000 W1 0.02160(15) 0.02160(15) 0.0229(2) 0.000 0.000 0.000 O2 0.024(3) 0.030(3) 0.032(3) 0.002(3) -0.001(3) -0.003(3) C1 0.034(4) 0.036(5) 0.048(4) 0.000(4) -0.008(3) -0.005(4) C2 0.039(4) 0.040(7) 0.056(4) 0.003(5) 0.001(4) 0.000(4) C7 0.043(7) 0.045(8) 0.057(5) 0.003(6) 0.012(5) -0.003(6) C3 0.038(5) 0.042(9) 0.075(7) 0.011(6) 0.001(5) 0.003(5) C4 0.042(6) 0.048(9) 0.082(7) 0.009(7) -0.015(5) -0.004(6) C5 0.050(5) 0.042(6) 0.070(6) 0.003(5) -0.019(4) -0.002(5) C6 0.044(4) 0.033(5) 0.049(4) 0.001(4) -0.009(3) -0.002(4) C8 0.049(6) 0.046(6) 0.041(5) -0.011(4) -0.010(4) -0.014(5) O2A 0.039(5) 0.029(6) 0.043(5) 0.005(5) -0.007(4) 0.000(4) C1A 0.029(5) 0.021(6) 0.035(5) -0.001(4) -0.005(4) 0.005(4) C2A 0.037(5) 0.036(8) 0.051(5) 0.000(5) 0.005(5) 0.000(5) C7A 0.044(9) 0.046(10) 0.047(6) 0.001(8) 0.010(6) 0.004(9) C3A 0.042(7) 0.034(11) 0.070(8) 0.021(7) -0.005(6) -0.005(7) C4A 0.043(9) 0.036(11) 0.077(9) 0.007(8) -0.014(6) -0.005(8) C5A 0.041(7) 0.042(8) 0.053(7) 0.002(6) -0.018(5) 0.002(6) C6A 0.039(6) 0.035(6) 0.035(5) -0.002(5) -0.007(4) 0.001(5) C8A 0.039(8) 0.050(9) 0.041(7) 0.003(7) -0.002(6) 0.006(7) Na1 0.0279(12) 0.0279(12) 0.0305(19) 0.000 0.000 0.000 O3 0.043(2) 0.045(2) 0.061(2) -0.011(2) 0.003(2) -0.0061(19) C9 0.051(4) 0.063(4) 0.060(4) 0.001(3) 0.007(3) -0.004(3) C10 0.053(4) 0.056(4) 0.108(5) -0.005(4) 0.002(4) -0.009(3) C11 0.058(4) 0.083(5) 0.087(5) -0.040(4) 0.002(4) -0.019(4) C12 0.055(4) 0.069(5) 0.058(4) -0.018(3) 0.006(3) -0.016(3) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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_ _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 W1 O1 Na1 180.0 . . ? O1 W1 O2A 107.5(3) . . ? O1 W1 O2A 107.5(3) . 3 ? O2A W1 O2A 84.81(17) . 3 ? O1 W1 O2A 107.5(3) . 4 ? O1 W1 O2A 107.5(3) . 2 ? O2A W1 O2A 145.0(6) . 2 ? O2A W1 O2A 84.80(17) 3 2 ? O2A W1 O2A 84.80(17) 4 2 ? O1 W1 O2 107.08(16) . . ? O1 W1 O2 107.08(16) . 2 ? O2A W1 O2 107.3(3) . 2 ? O2A W1 O2 137.5(3) 3 2 ? O2A W1 O2 23.9(3) 4 2 ? O2A W1 O2 61.7(3) 2 2 ? O2 W1 O2 145.8(3) . 2 ? O1 W1 O2 107.08(16) . 3 ? O2A W1 O2 137.5(3) . 3 ? O2A W1 O2 61.7(3) 3 3 ? O2A W1 O2 107.3(3) 4 3 ? O2A W1 O2 23.9(3) 2 3 ? O2 W1 O2 85.05(9) . 3 ? O2 W1 O2 85.05(9) 2 3 ? O1 W1 O2 107.08(16) . 4 ? O2 W1 O2 85.05(9) . 4 ? O2 W1 O2 85.05(9) 2 4 ? O2 W1 O2 145.8(3) 3 4 ? C1 O2 W1 132.5(6) . . ? O2 C1 C2 122.6(8) . . ? O2 C1 C6 117.2(7) . . ? C2 C1 C6 120.1(9) . . ? C3 C2 C1 118.2(10) . . ? C3 C2 C7 121.8(13) . . ? C1 C2 C7 119.4(14) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C3 C2 121.6(12) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.9(13) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.5(9) . . ? C5 C6 C8 120.6(8) . . ? C1 C6 C8 119.9(8) . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1A O2A W1 132.8(8) . . ? O2A C1A C2A 120.1(11) . . ? O2A C1A C6A 118.4(9) . . ? C2A C1A C6A 121.4(12) . . ? C3A C2A C1A 117.9(14) . . ? C3A C2A C7A 123.0(17) . . ? C1A C2A C7A 118.4(18) . . ? C2A C7A H7A1 109.5 . . ? C2A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C2A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C4A C3A C2A 120.6(15) . . ? C4A C3A H3A 119.7 . . ? C2A C3A H3A 119.7 . . ? C3A C4A C5A 121.8(16) . . ? C3A C4A H4A 119.1 . . ? C5A C4A H4A 119.1 . . ? C4A C5A C6A 119.5(13) . . ? C4A C5A H5A 120.3 . . ? C6A C5A H5A 120.3 . . ? C5A C6A C1A 118.7(10) . . ? C5A C6A C8A 121.6(11) . . ? C1A C6A C8A 119.3(10) . . ? C6A C8A H8A1 109.5 . . ? C6A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C6A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? O1 Na1 O3 108.73(13) . 2 ? O1 Na1 O3 108.73(13) . 4 ? O3 Na1 O3 84.08(8) 2 4 ? O1 Na1 O3 108.73(13) . 3 ? O3 Na1 O3 84.08(8) 2 3 ? O3 Na1 O3 142.5(3) 4 3 ? O1 Na1 O3 108.73(13) . . ? O3 Na1 O3 142.5(3) 2 . ? O3 Na1 O3 84.08(8) 4 . ? O3 Na1 O3 84.08(8) 3 . ? C12 O3 C9 109.5(5) . . ? C12 O3 Na1 124.7(4) . . ? C9 O3 Na1 123.8(4) . . ? O3 C9 C10 104.8(5) . . ? O3 C9 H9A 110.8 . . ? C10 C9 H9A 110.8 . . ? O3 C9 H9B 110.8 . . ? C10 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C11 C10 C9 102.1(6) . . ? C11 C10 H10A 111.3 . . ? C9 C10 H10A 111.3 . . ? C11 C10 H10B 111.3 . . ? C9 C10 H10B 111.3 . . ? H10A C10 H10B 109.2 . . ? C10 C11 C12 102.7(6) . . ? C10 C11 H11A 111.2 . . ? C12 C11 H11A 111.2 . . ? C10 C11 H11B 111.2 . . ? C12 C11 H11B 111.2 . . ? H11A C11 H11B 109.1 . . ? O3 C12 C11 105.5(5) . . ? O3 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? O3 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.8 . . ? 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 O1 W1 1.731(7) . ? O1 Na1 2.275(8) . ? W1 O2A 1.958(8) . ? W1 O2A 1.958(8) 3 ? W1 O2A 1.958(8) 4 ? W1 O2A 1.958(8) 2 ? W1 O2 1.966(5) . ? W1 O2 1.966(5) 2 ? W1 O2 1.966(5) 3 ? W1 O2 1.966(5) 4 ? O2 C1 1.379(10) . ? C1 C2 1.401(14) . ? C1 C6 1.402(10) . ? C2 C3 1.390(13) . ? C2 C7 1.504(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C3 C4 1.377(12) . ? C3 H3 0.9500 . ? C4 C5 1.367(14) . ? C4 H4 0.9500 . ? C5 C6 1.387(11) . ? C5 H5 0.9500 . ? C6 C8 1.486(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O2A C1A 1.376(12) . ? C1A C2A 1.403(15) . ? C1A C6A 1.407(12) . ? C2A C3A 1.386(14) . ? C2A C7A 1.505(13) . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C3A C4A 1.375(14) . ? C3A H3A 0.9500 . ? C4A C5A 1.378(15) . ? C4A H4A 0.9500 . ? C5A C6A 1.388(13) . ? C5A H5A 0.9500 . ? C6A C8A 1.500(13) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? Na1 O3 2.351(4) 2 ? Na1 O3 2.351(4) 4 ? Na1 O3 2.351(4) 3 ? Na1 O3 2.351(4) . ? O3 C12 1.424(7) . ? O3 C9 1.426(7) . ? C9 C10 1.495(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.477(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.518(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 W1 O2 C1 C2 71.1(16) . . . . ? W1 O2 C1 C6 -112.6(8) . . . . ? O2 C1 C2 C3 176.1(15) . . . . ? C6 C1 C2 C3 0(3) . . . . ? O2 C1 C2 C7 5(3) . . . . ? C6 C1 C2 C7 -171.2(19) . . . . ? C1 C2 C3 C4 3(3) . . . . ? C7 C2 C3 C4 174(2) . . . . ? C2 C3 C4 C5 -4(3) . . . . ? C3 C4 C5 C6 1(3) . . . . ? C4 C5 C6 C1 2(2) . . . . ? C4 C5 C6 C8 -177.8(16) . . . . ? O2 C1 C6 C5 -178.6(9) . . . . ? C2 C1 C6 C5 -2.2(18) . . . . ? O2 C1 C6 C8 0.9(13) . . . . ? C2 C1 C6 C8 177.4(14) . . . . ? W1 O2A C1A C2A -72(2) . . . . ? W1 O2A C1A C6A 111.4(12) . . . . ? O2A C1A C2A C3A -174(2) . . . . ? C6A C1A C2A C3A 3(4) . . . . ? O2A C1A C2A C7A -3(4) . . . . ? C6A C1A C2A C7A 173(3) . . . . ? C1A C2A C3A C4A -3(5) . . . . ? C7A C2A C3A C4A -173(4) . . . . ? C2A C3A C4A C5A 2(5) . . . . ? C3A C4A C5A C6A -1(4) . . . . ? C4A C5A C6A C1A 0(3) . . . . ? C4A C5A C6A C8A 173(2) . . . . ? O2A C1A C6A C5A 175.3(12) . . . . ? C2A C1A C6A C5A -1(3) . . . . ? O2A C1A C6A C8A 2.1(19) . . . . ? C2A C1A C6A C8A -175(2) . . . . ? C12 O3 C9 C10 20.8(7) . . . . ? Na1 O3 C9 C10 -174.6(4) . . . . ? O3 C9 C10 C11 -36.6(7) . . . . ? C9 C10 C11 C12 37.6(8) . . . . ? C9 O3 C12 C11 3.1(8) . . . . ? Na1 O3 C12 C11 -161.2(5) . . . . ? C10 C11 C12 O3 -25.9(8) . . . . ?