# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1218 #=============================================================================== data_global #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Christopher B. Gorman' _publ_contact_author_address ; Department of Chemistry Box 8204 North Carolina State University Raleigh, NC 27695-8204 ; _publ_contact_author_phone 1(919)5154252 _publ_contact_author_fax 1(919)5158920 _publ_contact_author_email chris_gorman@ncsu.edu _publ_requested_journal 'Chemical Communications' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; This is the CIF to accompany the manuscript entitled, "Hybrid Organic-Inorganic, Hexa-arm Dendrimers Based on a Mo~6~Cl~8~ Core" by Christopher B. Gorman, Wendy Y. Su, Hongwei Jiang, Christopher M. Watson, and Paul D. Boyle ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Hybrid Organic-Inorganic, Hexa-arm Dendrimers Based on a Mo~6~Cl~8~ Core ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Gorman, Christopher B.' #<--'Last name, first name ;Department of Chemistry Box 8204 North Carolina State University Raleigh, NC 27695-8204 ; 'Su, Wendy Y.' ;Department of Chemistry Box 8204 North Carolina State University Raleigh, NC 27695-8204 ; 'Jiang, Hongwei' ;Department of Chemistry Box 8204 North Carolina State University Raleigh, NC 27695-8204 ; 'Watson, Christopher M.' ;Department of Chemistry Box 8204 North Carolina State University Raleigh, NC 27695-8204 ; 'Boyle, Paul D.' ;Department of Chemistry Box 8204 North Carolina State University Raleigh, NC 27695-8204 ; #=============================================================================== _publ_section_exptl_refinement ; Hydrogen atoms were included in the model at calculated positions. The hydrogen atom positions and isotropic displacement parameters were allowed to ride on the parent carbon atom. Refinement of the structure was performed using full matrix least-squares based on F. All non-H atoms except those of the disordered ether were allowed to refine with anisotropic displacement parameters (ADP's). The structure contained several solvent molecules these included a disordered THF molecule and a disordered ether molecule. The disorder in the THF was not crystallographically imposed but was a conformational disorder in the molecule. This manifested as a two sites for atom C8s (C8s & C8s'). The occupancies for these two sites were refined to 0.602 and 0.398 respectively. C8s and C8s' were refined anisotropically, while the stability of the refinement dictated that atoms O3s, C9s, C9s', and C10s be refined isotropically. The ether molecule exhibited a number of problems which made a completely satisfactory refinement elusive. The ether molecule was both disordered across a crystallographic center and also displayed a conformational disorder. The conformational disorder was assumed to be 50/50 for C9s and C9s' sites while the overall occupancy of the molecule was assumed to be 0.5. As noted above, an attempt to refine the atoms anisotropically led to a non-convergent refinement. The isotropic refinement converged to an acceptable final shift/error (0.002). The largest peaks in the final difference map (1.17 e^-^/\%A^3^) were in the vicinity of the disordered ether molecule. The calculated structure factors included corrections for anomalous dispersion from the usual tabulation (International Tables for X-ray Crystallography, Vol. IV, (1974), Table 2.3.1, Kynoch Press, Birmingham, England). A secondary extinction correction was included in the final cycles of refinement. ; _publ_section_acknowledgements ; The authors gratefully acknowledge the National Science Foundation (NSF) for the award of an equipment grant (CHE9509532) used to purchase the X-ray diffractometer. ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_Na2G0 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; Disodium Hexakis(p-methoxyphenoxy) Octa-\m-3-chloro-Hexamolybdate ; _chemical_name_common ? _chemical_formula_moiety 'C60 H79 Cl8 Mo6 Na2 O16.50' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H79 Cl8 Mo6 Na2 O16.50' _chemical_formula_weight 1969.50 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo ? -1.683 .686 'International Tables Vol. IV Table 2.2B' Cl ? .148 .159 'International Tables Vol. IV Table 2.2B' C ? .003 .002 'International Tables Vol. IV Table 2.2B' H ? .000 .000 'International Tables Vol. IV Table 2.2B' O ? .011 .006 'International Tables Vol. IV Table 2.2B' Na ? .036 .025 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2+x,1/2+y,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 22.9666(19) _cell_length_b 18.1932(18) _cell_length_c 18.1761(19) _cell_angle_alpha 90.0 _cell_angle_beta 98.574(12) _cell_angle_gamma 90.0 _cell_volume 7509.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 148 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 15.50 _cell_measurement_theta_max 18.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max .48 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method ? _exptl_crystal_F_000 3890.30 _exptl_absorpt_coefficient_mu 1.33 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'NRCVAX ABSORP' _exptl_absorpt_correction_T_min .9353 _exptl_absorpt_correction_T_max .9941 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; The sample was mounted on the end of a glass fiber using a small amount of silicon grease and transferred to the diffractometer. The sample was maintained at a temperature of -125 deg C using a nitrogen cold stream. All X-ray measurements were made on an Enraf-Nonius CAD4-MACH diffractometer. The unit cell dimensions were determined by a fit of 24 well centered reflections and thier Friedel pairs with \q 31\% < 2\q < 36\%. A quadrant of unique data was collected using the omega scan mode in a non-bisecting geometry. The adoption of a non-bisecting scan mode was accomplished by offsetting psi by 20.00\% for each data point collected. This was done to minimize the interaction of the goniometer head with the cold stream. Three standard reflections were measured every 4800 seconds of X-ray exposure time. Scaling the data was accomplished using a 5 point smoothed curved routine fit to the intensity check reflections. The intensity data was corrected for Lorentz and polarization effects. The data was corrected for absorption empirically using psi scan data. ; _diffrn_ambient_temperature 148 _diffrn_radiation_wavelength .71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD4-MACH ' _diffrn_measurement_method 'Omega scan b/P/b ' _diffrn_standards_number 3 _diffrn_standards_interval_time 80 _diffrn_standards_decay_% 2.1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -10 3 2 -10 -3 -7 5 1 _diffrn_reflns_number 8106 _diffrn_reflns_av_R_equivalents .000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_reduction_process ? _reflns_number_total 8106 _reflns_number_observed 6108 _reflns_observed_criterion 'Inet > 1.0\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'SIR92' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details '1/(\s^2^(F)+ .00025F^2^) ' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method Larson _refine_ls_extinction_coef 0.017(3) _refine_ls_number_reflns 6094 _refine_ls_number_parameters 432 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all .037 _refine_ls_R_factor_obs .036 _refine_ls_wR_factor_all .042 _refine_ls_wR_factor_obs .041 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.42 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max .002 _refine_ls_shift/esd_mean ? _refine_diff_density_max 1.17 _refine_diff_density_min -.59 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Mo1 .002100(17) .09255(2) .54247(2) .01312(19) Uani ? . Mo Mo2 -.048312(17) .03600(2) .41772(2) .01270(18) Uani ? . Mo Mo3 -.065633(17) -.02261(2) .54359(2) .01306(18) Uani ? . Mo Cl1 .11050(5) .07533(6) .57838(6) .0166(5) Uani ? . Cl Cl2 -.01400(5) .03152(6) .66117(6) .0169(5) Uani ? . Cl Cl3 .01905(5) .14294(6) .42066(6) .0169(5) Uani ? . Cl Cl4 -.10619(5) .10084(6) .50411(6) .0180(5) Uani ? . Cl O1 .00619(15) .19158(17) .59532(18) .0218(17) Uani ? . O O2 -.10525(14) .07310(17) .32485(17) .0186(17) Uani ? . O O3 -.13570(14) -.04505(19) .60024(17) .0198(16) Uani ? . O O4 -.06598(20) .4812(2) .5517(2) .042(2) Uani ? . O O5 -.1095(2) .3662(2) .2376(2) .048(3) Uani ? . O O6 -.34720(16) -.1794(2) .4876(2) .0329(20) Uani ? . O C1 -.0139(2) .2603(3) .5808(3) .019(2) Uani ? . C C2 -.0411(2) .2846(3) .5112(3) .026(3) Uani ? . C C3 -.0588(2) .3575(3) .4992(3) .029(3) Uani ? . C C4 -.0500(2) .4076(3) .5578(3) .027(3) Uani ? . C C5 -.0243(3) .3835(3) .6275(3) .033(3) Uani ? . C C6 -.0061(2) .3118(3) .6390(3) .026(3) Uani ? . C C7 -.0839(3) .5090(3) .4788(4) .041(3) Uani ? . C C8 -.1068(2) .1451(3) .3027(3) .019(2) Uani ? . C C9 -.1402(2) .1977(3) .3333(3) .029(3) Uani ? . C C10 -.1406(3) .2706(3) .3094(3) .034(3) Uani ? . C C11 -.1075(3) .2923(3) .2556(3) .029(3) Uani ? . C C12 -.0752(2) .2407(3) .2238(3) .027(3) Uani ? . C C13 -.0748(2) .1677(3) .2474(3) .021(3) Uani ? . C C14 -.0772(3) .3888(3) .1798(4) .050(4) Uani ? . C C15 -.1864(2) -.0804(3) .5714(3) .019(2) Uani ? . C C16 -.2025(2) -.1460(3) .6021(3) .024(2) Uani ? . C C17 -.2555(2) -.1809(3) .5762(3) .028(3) Uani ? . C C18 -.2935(2) -.1499(3) .5171(3) .024(2) Uani ? . C C19 -.2779(2) -.0854(3) .4852(3) .026(3) Uani ? . C C20 -.2252(2) -.0508(3) .5121(3) .023(2) Uani ? . C C21 -.3683(3) -.2406(3) .5259(3) .039(3) Uani ? . C Na1 -.14649(9) .00863(11) .21938(10) .0230(10) Uani ? . Na O1s -.14741(18) -.1172(2) .2312(2) .038(2) Uani ? . O C1s -.1046(3) -.1724(3) .2227(4) .040(4) Uani ? . C C2s -.1304(3) -.2447(4) .2358(6) .071(6) Uani ? . C C3s -.1948(3) -.2323(4) .2313(5) .063(5) Uani ? . C C4s -.1991(3) -.1540(4) .2524(4) .053(4) Uani ? . C O2s -.24309(17) .0201(2) .2364(2) .034(2) Uani ? . O C5s -.2972(3) .0150(3) .1847(3) .037(3) Uani ? . C C6s -.3436(3) .0529(4) .2207(4) .056(4) Uani ? . C C7s -.3172(4) .0558(6) .3028(5) .079(6) Uani ? . C C8s -.2588(8) .0173(8) .3107(9) .043(8) Uani ? . C C8s' -.2598(11) .0521(12) .3032(13) .037(11) Uani ? . C O3s .2469(8) .2520(11) .0213(8) .038(4) Uiso ? . O C9s .2895(13) .2125(16) .0166(17) .050(7) Uiso ? . C C9s' .2561(16) .1941(20) -.0121(20) .064(9) Uiso ? . C C10s .2827(9) .1467(11) .0046(11) .079(5) Uiso ? . C H2 -.048 .250 .471 .0354 Uiso ? . H H3 -.077 .373 .451 .0387 Uiso ? . H H5 -.019 .417 .668 .0427 Uiso ? . H H6 .012 .296 .687 .0361 Uiso ? . H H7a -.094 .560 .481 .0507 Uiso ? . H H7b -.052 .504 .450 .0507 Uiso ? . H H7c -.118 .482 .456 .0507 Uiso ? . H H9 -.163 .183 .371 .0397 Uiso ? . H H10 -.165 .306 .330 .0446 Uiso ? . H H12 -.053 .255 .185 .0375 Uiso ? . H H13 -.052 .132 .226 .0313 Uiso ? . H H14a -.081 .441 .172 .0580 Uiso ? . H H14b -.036 .377 .194 .0580 Uiso ? . H H14c -.092 .363 .135 .0580 Uiso ? . H H16 -.176 -.168 .642 .0334 Uiso ? . H H17 -.266 -.226 .599 .0380 Uiso ? . H H19 -.304 -.064 .444 .0358 Uiso ? . H H20 -.215 -.006 .490 .0335 Uiso ? . H H21a -.406 -.256 .500 .0487 Uiso ? . H H21b -.341 -.281 .529 .0487 Uiso ? . H H21c -.373 -.225 .575 .0487 Uiso ? . H H1sa -.095 -.171 .173 .0510 Uiso ? . H H1sb -.069 -.164 .257 .0510 Uiso ? . H H2sa -.122 -.280 .200 .0826 Uiso ? . H H2sb -.115 -.262 .285 .0826 Uiso ? . H H3sa -.214 -.239 .181 .0743 Uiso ? . H H3sb -.212 -.265 .263 .0743 Uiso ? . H H4sa -.198 -.151 .305 .0627 Uiso ? . H H4sb -.235 -.132 .228 .0627 Uiso ? . H H5sa -.293 .039 .139 .0469 Uiso ? . H H5sb -.308 -.035 .174 .0469 Uiso ? . H H6sa -.352 .102 .201 .0657 Uiso ? . H H6sb -.379 .025 .215 .0657 Uiso ? . H H7sa -.312 .106 .318 .0900 Uiso ? . H H7sb -.343 .034 .334 .0900 Uiso ? . H H8sa -.259 -.031 .332 .0540 Uiso ? . H H8sb -.230 .043 .345 .0540 Uiso ? . H H8sa' -.242 .100 .311 .0460 Uiso ? . H H8sb' -.245 .020 .343 .0460 Uiso ? . H H9sa .310 .231 -.022 .0604 Uiso ? . H H9sb .316 .217 .062 .0604 Uiso ? . H H9sa' .236 .188 .030 .0737 Uiso ? . H H9sb' .232 .174 -.055 .0737 Uiso ? . H H10sa .313 .116 .031 .0892 Uiso ? . H H10sb .245 .129 .015 .0892 Uiso ? . H H10sc .284 .135 -.047 .0892 Uiso ? . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Mo1 .0167(2) .01311(19) .00903(19) -.00201(16) .00019(15) -.00026(15) Mo Mo2 .01538(20) .01392(19) .00818(18) -.00184(15) -.00025(15) .00060(15) Mo Mo3 .01480(20) .0155(2) .00867(19) -.00280(16) .00102(15) .00060(15) Mo Cl1 .0179(5) .0183(6) .0125(5) -.0046(4) -.0013(4) .0000(4) Cl Cl2 .0212(6) .0211(6) .0084(5) -.0019(4) .0023(4) -.0010(4) Cl Cl3 .0215(6) .0160(5) .0127(5) -.0042(4) .0010(4) .0028(4) Cl Cl4 .0189(6) .0193(6) .0152(5) .0016(5) .0006(5) -.0006(4) Cl O1 .0320(20) .0139(17) .0177(17) .0004(14) -.0026(15) -.0030(14) O O2 .0237(18) .0198(17) .0109(16) -.0007(14) -.0023(14) .0015(13) O O3 .0176(17) .0280(19) .0140(16) -.0073(14) .0031(14) -.0008(14) O O4 .063(3) .023(2) .038(2) .016(2) .006(2) -.0025(18) O O5 .085(4) .021(2) .037(2) .003(2) .005(2) .0067(18) O O6 .0229(19) .037(2) .037(2) -.0121(17) -.0033(17) -.0037(18) O C1 .018(2) .019(2) .020(2) -.0045(19) .0061(20) -.0027(19) C C2 .036(3) .024(3) .017(2) .001(2) -.002(2) -.006(2) C C3 .034(3) .028(3) .024(3) .007(2) .000(2) -.002(2) C C4 .033(3) .017(2) .030(3) .006(2) .004(2) -.003(2) C C5 .049(4) .022(3) .026(3) .005(3) .003(3) -.008(2) C C6 .038(3) .023(3) .017(3) .004(2) .002(2) -.002(2) C C7 .039(4) .029(3) .054(4) .011(3) .005(3) .008(3) C C8 .022(2) .022(2) .012(2) .000(2) -.0056(19) .0023(19) C C9 .032(3) .033(3) .024(3) .010(2) .007(2) .007(2) C C10 .048(4) .028(3) .027(3) .014(3) .007(3) .003(2) C C11 .045(3) .021(3) .021(3) .004(2) -.001(2) .007(2) C C12 .037(3) .026(3) .019(3) -.004(2) .004(2) .005(2) C C13 .029(3) .021(3) .015(2) .001(2) .002(2) .0004(19) C C14 .073(5) .029(3) .041(4) -.010(3) -.008(4) .012(3) C C15 .019(2) .021(3) .017(2) -.0017(19) .0069(20) -.0021(19) C C16 .022(3) .027(3) .022(3) -.001(2) -.001(2) .004(2) C C17 .024(3) .027(3) .033(3) -.007(2) .006(2) .004(2) C C18 .019(2) .028(3) .025(3) -.006(2) .006(2) -.009(2) C C19 .023(3) .033(3) .021(3) -.004(2) -.001(2) .004(2) C C20 .025(3) .025(3) .020(3) -.003(2) .005(2) .005(2) C C21 .032(3) .040(3) .044(4) -.018(3) .005(3) -.009(3) C Na1 .0272(11) .0260(10) .0153(10) -.0040(9) .0013(8) -.0018(8) Na O1s .039(2) .026(2) .048(3) -.0032(18) .005(2) -.0011(19) O C1s .041(4) .029(3) .052(4) .000(3) .016(3) -.001(3) C C2s .041(4) .034(4) .142(8) .002(3) .028(5) .008(5) C C3s .044(4) .042(4) .106(7) -.004(3) .020(4) .000(4) C C4s .041(4) .049(4) .068(5) -.007(3) .002(4) -.011(4) C O2s .026(2) .050(3) .026(2) .0017(18) .0052(17) .0019(18) O C5s .030(3) .043(4) .038(3) -.005(3) .001(3) .005(3) C C6s .044(4) .070(5) .054(5) .023(4) .006(4) .006(4) C C7s .058(5) .135(9) .047(5) .045(6) .015(4) .013(5) C C8s .050(8) .053(10) .029(7) .017(8) .019(6) .010(8) C C8s' .029(9) .057(14) .022(9) .013(12) -.004(7) -.002(11) C #=============================================================================== # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.5996(6) ? ? ? Mo1 Mo2 2.6251(6) ? 2_556 ? Mo1 Mo3 2.6115(6) ? ? ? Mo1 Mo3 2.6222(6) ? 2_556 ? Mo1 Cl1 2.4976(12) ? ? ? Mo1 Cl2 2.5024(11) ? ? ? Mo1 Cl3 2.4802(12) ? ? ? Mo1 Cl4 2.4855(12) ? ? ? Mo1 O1 2.037(3) ? ? ? Mo2 Mo1 2.6251(6) ? 2_556 ? Mo2 Mo3 2.6079(6) ? ? ? Mo2 Mo3 2.6179(6) ? 2_556 ? Mo2 Cl1 2.4855(11) ? 2_556 ? Mo2 Cl2 2.4950(12) ? 2_556 ? Mo2 Cl3 2.4813(11) ? ? ? Mo2 Cl4 2.4994(12) ? ? ? Mo2 O2 2.087(3) ? ? ? Mo3 Mo1 2.6222(6) ? 2_556 ? Mo3 Mo2 2.6179(6) ? 2_556 ? Mo3 Cl1 2.4932(12) ? 2_556 ? Mo3 Cl2 2.4876(12) ? ? ? Mo3 Cl3 2.4803(12) ? 2_556 ? Mo3 Cl4 2.4956(12) ? ? ? Mo3 O3 2.076(3) ? ? ? Cl1 Mo2 2.4855(11) ? 2_556 ? Cl1 Mo3 2.4932(12) ? 2_556 ? Cl2 Mo2 2.4950(12) ? 2_556 ? Cl3 Mo3 2.4803(12) ? 2_556 ? O1 C1 1.346(6) ? ? ? O2 C8 1.369(6) ? ? ? O2 Na1 2.325(4) ? ? ? O3 C15 1.364(6) ? ? ? O3 Na1 2.313(4) ? 6_555 ? O4 C4 1.388(6) ? ? ? O4 C7 1.422(8) ? ? ? O5 C11 1.383(6) ? ? ? O5 C14 1.432(9) ? ? ? O6 C18 1.378(6) ? ? ? O6 C21 1.437(7) ? ? ? C1 C2 1.397(7) ? ? ? C1 C6 1.403(7) ? ? ? C2 C3 1.396(7) ? ? ? C3 C4 1.394(7) ? ? ? C4 C5 1.386(8) ? ? ? C5 C6 1.377(8) ? ? ? C8 C9 1.393(7) ? ? ? C8 C13 1.393(7) ? ? ? C9 C10 1.394(8) ? ? ? C10 C11 1.383(8) ? ? ? C11 C12 1.374(8) ? ? ? C12 C13 1.396(7) ? ? ? C15 C16 1.391(7) ? ? ? C15 C20 1.401(7) ? ? ? C16 C17 1.391(7) ? ? ? C17 C18 1.397(8) ? ? ? C18 C19 1.380(7) ? ? ? C19 C20 1.387(7) ? ? ? Na1 O3c 2.313(4) ? ? ? Na1 O1s 2.300(4) ? ? ? Na1 O2s 2.295(4) ? ? ? O1s C1s 1.431(7) ? ? ? O1s C4s 1.464(8) ? ? ? C1s C2s 1.476(9) ? ? ? C2s C3s 1.486(10) ? ? ? C3s C4s 1.484(10) ? ? ? O2s C5s 1.446(7) ? ? ? O2s C8s 1.449(17) ? ? ? O2s C8s' 1.45(2) ? ? ? C5s C6s 1.500(9) ? ? ? C6s C7s 1.525(11) ? ? ? C7s C8s 1.502(18) ? ? ? C7s C8s' 1.32(3) ? ? ? C8s C8s' .65(2) ? ? ? O3s O3s .81(3) ? 4_555 ? O3s C9s 1.23(3) ? ? ? O3s C9s 1.19(4) ? 4_555 ? O3s C9s' 1.25(4) ? ? ? O3s C9s' 1.00(4) ? 4_555 ? C9s O3s 1.19(4) ? 4_555 ? C9s C9s' .92(5) ? ? ? C9s C10s 1.22(4) ? ? ? C9s' O3s 1.00(4) ? 4_555 ? C9s' C10s 1.08(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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mo2 Mo1 Mo2 89.827(18) ? ? 2_556 ? Mo2 Mo1 Mo3 60.060(15) ? ? ? ? Mo2 Mo1 Mo3 60.175(16) ? ? 2_556 ? Mo2 Mo1 Cl1 118.38(3) ? ? ? ? Mo2 Mo1 Cl2 118.20(3) ? ? ? ? Mo2 Mo1 Cl3 58.42(3) ? ? ? ? Mo2 Mo1 Cl4 58.83(3) ? ? ? ? Mo2 Mo1 O1 138.12(9) ? ? ? ? Mo2 Mo1 Mo3 59.990(16) 2_556 ? ? ? Mo2 Mo1 Mo3 59.604(15) 2_556 ? 2_556 ? Mo2 Mo1 Cl1 57.99(3) 2_556 ? ? ? Mo2 Mo1 Cl2 58.17(3) 2_556 ? ? ? Mo2 Mo1 Cl3 117.68(3) 2_556 ? ? ? Mo2 Mo1 Cl4 118.55(3) 2_556 ? ? ? Mo2 Mo1 O1 132.04(9) 2_556 ? ? ? Mo3 Mo1 Mo3 90.023(18) ? ? 2_556 ? Mo3 Mo1 Cl1 117.97(3) ? ? ? ? Mo3 Mo1 Cl2 58.17(3) ? ? ? ? Mo3 Mo1 Cl3 118.45(3) ? ? ? ? Mo3 Mo1 Cl4 58.57(3) ? ? ? ? Mo3 Mo1 O1 133.75(10) ? ? ? ? Mo3 Mo1 Cl1 58.22(3) 2_556 ? ? ? Mo3 Mo1 Cl2 117.77(3) 2_556 ? ? ? Mo3 Mo1 Cl3 58.09(3) 2_556 ? ? ? Mo3 Mo1 Cl4 118.99(3) 2_556 ? ? ? Mo3 Mo1 O1 136.04(10) 2_556 ? ? ? Cl1 Mo1 Cl2 89.35(4) ? ? ? ? Cl1 Mo1 Cl3 89.81(4) ? ? ? ? Cl1 Mo1 Cl4 176.13(4) ? ? ? ? Cl1 Mo1 O1 90.78(10) ? ? ? ? Cl2 Mo1 Cl3 175.34(4) ? ? ? ? Cl2 Mo1 Cl4 89.92(4) ? ? ? ? Cl2 Mo1 O1 89.32(10) ? ? ? ? Cl3 Mo1 Cl4 90.62(4) ? ? ? ? Cl3 Mo1 O1 95.27(10) ? ? ? ? Cl4 Mo1 O1 93.01(10) ? ? ? ? Mo1 Mo2 Mo1 90.173(18) ? ? 2_556 ? Mo1 Mo2 Mo3 60.196(16) ? ? ? ? Mo1 Mo2 Mo3 60.340(17) ? ? 2_556 ? Mo1 Mo2 Cl1 118.73(3) ? ? 2_556 ? Mo1 Mo2 Cl2 118.50(3) ? ? 2_556 ? Mo1 Mo2 Cl3 58.38(3) ? ? ? ? Mo1 Mo2 Cl4 58.31(3) ? ? ? ? Mo1 Mo2 O2 136.16(9) ? ? ? ? Mo1 Mo2 Mo3 60.143(15) 2_556 ? ? ? Mo1 Mo2 Mo3 59.747(15) 2_556 ? 2_556 ? Mo1 Mo2 Cl1 58.44(3) 2_556 ? 2_556 ? Mo1 Mo2 Cl2 58.45(3) 2_556 ? 2_556 ? Mo1 Mo2 Cl3 117.87(3) 2_556 ? ? ? Mo1 Mo2 Cl4 118.58(3) 2_556 ? ? ? Mo1 Mo2 O2 133.61(9) 2_556 ? ? ? Mo3 Mo2 Mo3 90.195(20) ? ? 2_556 ? Mo3 Mo2 Cl1 58.55(3) ? ? 2_556 ? Mo3 Mo2 Cl2 118.58(3) ? ? 2_556 ? Mo3 Mo2 Cl3 118.55(3) ? ? ? ? Mo3 Mo2 Cl4 58.46(3) ? ? ? ? Mo3 Mo2 O2 133.05(9) ? ? ? ? Mo3 Mo2 Cl1 118.18(3) 2_556 ? 2_556 ? Mo3 Mo2 Cl2 58.17(3) 2_556 ? 2_556 ? Mo3 Mo2 Cl3 58.14(3) 2_556 ? ? ? Mo3 Mo2 Cl4 118.63(3) 2_556 ? ? ? Mo3 Mo2 O2 136.71(9) 2_556 ? ? ? Cl1 Mo2 Cl2 89.79(4) 2_556 ? 2_556 ? Cl1 Mo2 Cl3 175.90(4) 2_556 ? ? ? Cl1 Mo2 Cl4 90.28(4) 2_556 ? ? ? Cl1 Mo2 O2 89.61(9) 2_556 ? ? ? Cl2 Mo2 Cl3 89.38(4) 2_556 ? ? ? Cl2 Mo2 Cl4 176.22(4) 2_556 ? ? ? Cl2 Mo2 O2 92.19(9) 2_556 ? ? ? Cl3 Mo2 Cl4 90.27(4) ? ? ? ? Cl3 Mo2 O2 94.43(9) ? ? ? ? Cl4 Mo2 O2 91.59(9) ? ? ? ? Mo1 Mo3 Mo1 89.977(18) ? ? 2_556 ? Mo1 Mo3 Mo2 59.745(16) ? ? ? ? Mo1 Mo3 Mo2 60.263(15) ? ? 2_556 ? Mo1 Mo3 Cl1 118.00(3) ? ? 2_556 ? Mo1 Mo3 Cl2 58.72(3) ? ? ? ? Mo1 Mo3 Cl3 118.42(3) ? ? 2_556 ? Mo1 Mo3 Cl4 58.19(3) ? ? ? ? Mo1 Mo3 O3 131.93(9) ? ? ? ? Mo1 Mo3 Mo2 60.253(16) 2_556 ? ? ? Mo1 Mo3 Mo2a 59.485(16) 2_556 ? ? ? Mo1 Mo3 Cl1a 58.39(3) 2_556 ? ? ? Mo1 Mo3 Cl2 117.92(3) 2_556 ? ? ? Mo1 Mo3 Cl3a 58.09(3) 2_556 ? ? ? Mo1 Mo3 Cl4 118.83(3) 2_556 ? ? ? Mo1 Mo3 O3 137.89(9) 2_556 ? ? ? Mo2 Mo3 Mo2 89.805(20) ? ? 2_556 ? Mo2 Mo3 Cl1 58.27(3) ? ? 2_556 ? Mo2 Mo3 Cl2 118.44(3) ? ? ? ? Mo2 Mo3 Cl3 118.33(3) ? ? 2_556 ? Mo2 Mo3 Cl4 58.60(3) ? ? ? ? Mo2 Mo3 O3 138.28(9) ? ? ? ? Mo2 Mo3 Cl1 117.85(3) 2_556 ? 2_556 ? Mo2 Mo3 Cl2 58.44(3) 2_556 ? ? ? Mo2 Mo3 Cl3 58.17(3) 2_556 ? 2_556 ? Mo2 Mo3 Cl4 118.45(3) 2_556 ? ? ? Mo2 Mo3 O3 131.77(9) 2_556 ? ? ? Cl1 Mo3 Cl2 175.70(4) 2_556 ? ? ? Cl1 Mo3 Cl3 89.91(4) 2_556 ? 2_556 ? Cl1 Mo3 Cl4 90.20(4) 2_556 ? ? ? Cl1 Mo3 O3 96.73(9) 2_556 ? ? ? Cl2 Mo3 Cl3 89.58(4) ? ? 2_556 ? Cl2 Mo3 Cl4 90.02(4) ? ? ? ? Cl2 Mo3 O3 87.55(9) ? ? ? ? Cl3 Mo3 Cl4 176.04(4) 2_556 ? ? ? Cl3 Mo3 O3 91.86(10) 2_556 ? ? ? Cl4 Mo3 O3 92.06(10) ? ? ? ? Mo1 Cl1 Mo2 63.58(3) ? ? 2_556 ? Mo1 Cl1 Mo3 63.39(3) ? ? 2_556 ? Mo2 Cl1 Mo3 63.18(3) 2_556 ? 2_556 ? Mo1 Cl2 Mo2 63.38(3) ? ? 2_556 ? Mo1 Cl2 Mo3 63.11(3) ? ? ? ? Mo2 Cl2 Mo3 63.39(3) 2_556 ? ? ? Mo1 Cl3 Mo2 63.20(3) ? ? ? ? Mo1 Cl3 Mo3 63.82(3) ? ? 2_556 ? Mo2 Cl3 Mo3 63.69(3) ? ? 2_556 ? Mo1 Cl4 Mo2 62.87(3) ? ? ? ? Mo1 Cl4 Mo3 63.24(3) ? ? ? ? Mo2 Cl4 Mo3 62.95(3) ? ? ? ? Mo1 O1 C1 137.7(3) ? ? ? ? Mo2 O2 C8 122.2(3) ? ? ? ? Mo2 O2 Na1 129.26(16) ? ? ? ? C8 O2 Na1 104.5(3) ? ? ? ? Mo3 O3 C15 125.6(3) ? ? ? ? Mo3 O3 Na1 127.38(16) ? ? 6_555 ? C15 O3 Na1 106.9(3) ? ? 6_555 ? C4 O4 C7 117.0(4) ? ? ? ? C11 O5 C14 116.7(5) ? ? ? ? C18 O6 C21 117.3(4) ? ? ? ? O1 C1 C2 124.4(4) ? ? ? ? O1 C1 C6 118.1(4) ? ? ? ? C2 C1 C6 117.5(4) ? ? ? ? C1 C2 C3 121.5(5) ? ? ? ? C2 C3 C4 119.8(5) ? ? ? ? O4 C4 C3 124.3(5) ? ? ? ? O4 C4 C5 116.7(5) ? ? ? ? C3 C4 C5 119.0(5) ? ? ? ? C4 C5 C6 121.1(5) ? ? ? ? C1 C6 C5 121.1(5) ? ? ? ? O2 C8 C9 122.2(4) ? ? ? ? O2 C8 C13 120.1(4) ? ? ? ? C9 C8 C13 117.7(4) ? ? ? ? C8 C9 C10 120.5(5) ? ? ? ? C9 C10 C11 120.9(5) ? ? ? ? O5 C11 C10 116.3(5) ? ? ? ? O5 C11 C12 124.4(5) ? ? ? ? C10 C11 C12 119.3(5) ? ? ? ? C11 C12 C13 120.0(5) ? ? ? ? C8 C13 C12 121.5(5) ? ? ? ? O3 C15 C16 120.9(4) ? ? ? ? O3 C15 C20 121.5(4) ? ? ? ? C16 C15 C20 117.5(4) ? ? ? ? C15 C16 C17 121.9(5) ? ? ? ? C16 C17 C18 119.4(5) ? ? ? ? O6 C18 C17 124.3(5) ? ? ? ? O6 C18 C19 116.1(5) ? ? ? ? C17 C18 C19 119.6(5) ? ? ? ? C18 C19 C20 120.4(5) ? ? ? ? C15 C20 C19 121.2(4) ? ? ? ? O2 Na1 O3 122.69(14) ? ? 6_554 ? O2 Na1 O1s 115.68(15) ? ? ? ? O2 Na1 O2s 97.25(15) ? ? ? ? O3 Na1 O1s 112.11(16) 6_554 ? ? ? O3 Na1 O2s 109.95(15) 6_554 ? ? ? O1s Na1 O2s 93.16(16) ? ? ? ? Na1 O1s C1s 132.3(3) ? ? ? ? Na1 O1s C4s 119.9(4) ? ? ? ? C1s O1s C4s 107.8(4) ? ? ? ? O1s C1s C2s 108.0(5) ? ? ? ? C1s C2s C3s 106.1(6) ? ? ? ? C2s C3s C4s 103.6(6) ? ? ? ? O1s C4s C3s 106.5(6) ? ? ? ? Na1 O2s C5s 131.4(3) ? ? ? ? Na1 O2s C8s 120.2(8) ? ? ? ? Na1 O2s C8s' 122.1(10) ? ? ? ? C5s O2s C8s 107.1(8) ? ? ? ? C5s O2s C8s' 105.1(10) ? ? ? ? C8s O2s C8s' 25.8(10) ? ? ? ? O2s C5s C6s 106.6(5) ? ? ? ? C5s C6s C7s 103.8(5) ? ? ? ? C6s C7s C8s 107.3(9) ? ? ? ? C6s C7s C8s' 104.8(12) ? ? ? ? C8s C7s C8s' 25.5(11) ? ? ? ? O2s C8s C7s 103.7(10) ? ? ? ? O2s C8s C8s' 77(3) ? ? ? ? C7s C8s C8s' 61(3) ? ? ? ? O2s C8s' C7s 113.9(17) ? ? ? ? O2s C8s' C8s 77(3) ? ? ? ? C7s C8s' C8s 93(3) ? ? ? ? O3s O3s C9s 67(2) 4_555 ? ? ? O3s O3s C9s 72(2) 4_555 ? 4_555 ? O3s O3s C9s' 52(2) 4_555 ? ? ? O3s O3s C9s' 86(3) 4_555 ? 4_555 ? C9s O3s C9s 140(2) ? ? 4_555 ? C9s O3s C9s' 43(2) ? ? ? ? C9s O3s C9s' 126(3) ? ? 4_555 ? C9sd O3s C9s' 109(3) ? ? ? ? C9sd O3s C9s' 48(3) ? ? 4_555 ? C9s' O3s C9s' 139(3) ? ? 4_555 ? O3s C9s O3s 39.2(14) ? ? 4_555 ? O3s C9s C9s' 69(3) ? ? ? ? O3s C9s C10s 120(3) ? ? ? ? O3s C9s C9s' 54(3) 4_555 ? ? ? O3s C9s C10s 111(3) 4_555 ? ? ? C9s' C9s C10s 58(3) ? ? ? ? O3s C9s' O3s 40.6(17) ? ? 4_555 ? O3s C9s' C9s 66(3) ? ? ? ? O3s C9s' C10s 132(4) ? ? ? ? O3s C9s' C9s 76(3) 4_555 ? ? ? O3s C9s' C10s 149(4) 4_555 ? ? ? C9s C9s' C10s 75(3) ? ? ? ? C9s C10s C9s' 46(3) ? ? ? ?