# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'H Riesen' 'David Rae' _publ_contact_author_name 'Hans Riesen' _publ_contact_author_email H.RIESEN@ADFA.EDU.AU _publ_section_title ; Revisiting the crystal structure and thermal properties of NaMgAl(oxalate)3?9H2O/Cr(III): an extraordinary spectral hole-burning material. ; _publ_contact_author_address ; School of Physical, Environmental and Mathematical Sciences, UNSW@ADFA, Canberra ACT 2600, Australia ; _publ_contact_author_fax '+61 (0)2 6268 80 17' _publ_contact_author_phone '+61 (0)2 6268 86 79' _publ_requested_category 'FM ' # Attachment 'riesen01_2008B.cif' data_riesen01 _database_code_depnum_ccdc_archive 'CCDC 682927' # start Validation Reply Form _vrf_PLAT780_riesen01 ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: ... Encifer says it's fine, but platon seems to get confused. Maybe too many symmetry operations are being invoked by the program as the structure is a 3-dimensional polymer. ; # end Validation Reply Form # 2003 _audit_creation_method maXus _publ_section_abstract ; We present the crystal and molecular structure of NaMgAl(oxalate)3.9H2O ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. ; _publ_section_exptl_refinement ; ; _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS00 (Rae, 2000)' _computing_publication_material 'RAELS00 (Rae, 2000)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _publ_section_references ; Rae, A. D. (2000) RAELS00, The Australian National University, Canberra, ACT, Australia. 2000 Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435-435 Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; _publ_section_acknowledgements ; Dr A.C. Willis is acknowledged for his help with the X-ray data collection. ; _chemical_compound_source 'Local laboratory' _cell_measurement_temperature 200 _refine_ls_hydrogen_treatment noref ###################done # Submission details _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -15 _reflns_limit_l_max 16 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.04208 _diffrn_orient_matrix_UB_12 -0.03540 _diffrn_orient_matrix_UB_13 0.04168 _diffrn_orient_matrix_UB_21 0.00606 _diffrn_orient_matrix_UB_22 0.01805 _diffrn_orient_matrix_UB_23 0.06632 _diffrn_orient_matrix_UB_31 -0.05951 _diffrn_orient_matrix_UB_32 -0.04872 _diffrn_orient_matrix_UB_33 0.01870 _cell_formula_units_Z 6 _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _chemical_formula_weight 500.473 _diffrn_radiation_type ' MoK\a' #loop_ #_symmetry_equiv_pos_site_id #_symmetry_equiv_pos_as_xyz #1 x,y,z #2 -y,x-y,z #3 -x+y,-x,z #4 -y,-x,1/2+z #5 -x+y,y,1/2+z #6 x,x-y,1/2+z _symmetry_space_group_name_H-M 'P 3 c 1' _symmetry_cell_setting Trigonal _chemical_formula_moiety ; H12 Mg O6 2+, C6 Na Al O12 2-, 3(H2 O) ; _chemical_formula_sum 'C6 H18 Al Mg Na O21 ' _chemical_name_systematic ; Sodium magnesium aluminium tri oxalato nonahydrate ; loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C ' 0.0033 0.0016 International_Tables_Vol_IV_Table_2.2A 'H ' 0.0000 0.0000 International_Tables_Vol_IV_Table_2.2A 'AL ' .0645 -.0514 International_Tables_Vol_IV_Table_2.2A 'MG ' .0486 -.0363 International_Tables_Vol_IV_Table_2.2A 'NA ' .0362 -.0249 International_Tables_Vol_IV_Table_2.2A 'O ' 0.0106 0.0060 International_Tables_Vol_IV_Table_2.2A _cell_length_a 16.7348(4) _cell_length_b 16.7348(4) _cell_length_c 12.6333(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3064.00(13) _diffrn_reflns_number 45101 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _exptl_crystal_F_000 1548 ###################### done _cell_measurement_reflns_used 42432 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 27.485 _diffrn_measurement_method CCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_crystal_description prism ####done _exptl_crystal_colour colourless ###d _exptl_crystal_size_min 0.32 #### _exptl_crystal_size_mid 0.36 ### _exptl_crystal_size_max 0.36 #### _exptl_absorpt_coefficient_mu 0.249 #### d _exptl_absorpt_correction_type integration ############# done _exptl_absorpt_correction_T_min 0.917 ################d _exptl_absorpt_correction_T_max 0.943 ##############d _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; _diffrn_reflns_av_R_equivalents 0.034 ###################done _reflns_number_total 4580 _refine_diff_density_min -0.48 ############## done _refine_diff_density_max 0.50 ############## done _refine_ls_number_reflns 4039 ############# done #_refine_ls_number_restraints 1 ############# _refine_ls_number_parameters 187 ################# done #_refine_ls_R_factor_ref 0.038 _refine_ls_wR_factor_ref 0.064 ############# done _refine_ls_goodness_of_fit_ref 1.68 ############## done #_reflns_number_all 4580 _refine_ls_R_factor_all 0.043 ############## d _refine_ls_wR_factor_all 0.066 ############## d # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00\s(I) _reflns_number_gt 4039 ########## d _refine_ls_R_factor_gt 0.038 ############## d _refine_ls_wR_factor_gt 0.064 ######### d _refine_ls_shift/su_max 0.1 ########### d _refine_ls_abs_structure_Flack 0.6(3) ############## d _refine_ls_abs_structure_details 'Flack ' ############## d _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1/(\s^2^(F) + 0.0009F^2^) ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, 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_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_calc_attached_atom Al1 AL 0.33767(5) 0.33002(5) 0.25312(8) 0.0162(1) 1.000 1 d . . . Mg1 MG 0.00000 0.00000 0.25985(5) 0.0194(3) 1.000 3 d S . . Mg2 MG 0.66667 0.33333 0.24821(7) 0.0190(2) 1.000 3 d S . . Mg3 MG 0.33333 0.66667 0.24194(6) 0.0200(3) 1.000 3 d S . . Na1 NA 0.32924(6) 0.33678(6) 0.75217(12) 0.0227(2) 1.000 1 d . . . O11 O 0.44684(9) 0.39226(9) 0.17044(11) 0.0196(3) 1.000 1 d . . . O12 O 0.39638(9) 0.43609(9) 0.34125(11) 0.0211(3) 1.000 1 d . . . O13 O 0.57429(9) 0.53137(9) 0.15651(11) 0.0272(4) 1.000 1 d . . . O14 O 0.51896(9) 0.57941(9) 0.34126(11) 0.0236(4) 1.000 1 d . . . O21 O 0.28006(9) 0.38168(9) 0.16868(11) 0.0200(3) 1.000 1 d . . . O22 O 0.22797(9) 0.28056(9) 0.33577(12) 0.0216(2) 1.000 1 d . . . O23 O 0.14629(9) 0.38101(11) 0.15674(11) 0.0271(5) 1.000 1 d . . . O24 O 0.09747(9) 0.28672(11) 0.34676(12) 0.0264(4) 1.000 1 d . . . O31 O 0.29079(9) 0.22349(9) 0.16566(11) 0.0209(3) 1.000 1 d . . . O32 O 0.38346(10) 0.26733(9) 0.33708(11) 0.0219(2) 1.000 1 d . . . O33 O 0.27479(10) 0.08209(9) 0.16306(12) 0.0253(4) 1.000 1 d . . . O34 O 0.39099(9) 0.13768(9) 0.34009(12) 0.0258(3) 1.000 1 d . . . C11 C 0.50272(12) 0.47511(12) 0.20031(11) 0.0171(3) 1.000 1 d . . . C12 C 0.47223(12) 0.50215(12) 0.30372(11) 0.0164(3) 1.000 1 d . . . C21 C 0.19873(10) 0.36065(10) 0.20034(13) 0.0186(3) 1.000 1 d . . . C22 C 0.16962(10) 0.30418(10) 0.30411(13) 0.0189(2) 1.000 1 d . . . C31 C 0.30447(10) 0.15880(11) 0.20110(12) 0.0185(2) 1.000 1 d . . . C32 C 0.36516(9) 0.18762(11) 0.30188(12) 0.0189(2) 1.000 1 d . . . O1 O 0.03249(9) 0.11333(8) 0.16621(10) 0.0270(3) 1.000 1 d . . . O2 O 0.11334(9) 0.08095(8) 0.35442(10) 0.0269(2) 1.000 1 d . . . O3 O 0.55362(8) 0.30123(9) 0.15330(10) 0.0254(3) 1.000 1 d . . . O4 O 0.63533(9) 0.41551(9) 0.34175(10) 0.0279(3) 1.000 1 d . . . O5 O 0.36473(9) 0.58457(9) 0.14684(10) 0.0266(3) 1.000 1 d . . . O6 O 0.25242(9) 0.55341(9) 0.33585(10) 0.0285(4) 1.000 1 d . . . O7 O 0.15869(10) 0.16443(11) 0.00558(14) 0.0252(4) 1.000 1 d . . . O8 O 0.50921(10) 0.33837(12) 0.50077(13) 0.0245(3) 1.000 1 d . . . O9 O 0.32594(12) 0.50212(10) 0.49641(12) 0.0249(4) 1.000 1 d . . . H1O1 H -0.00614 0.14338 0.16124 0.031 1.000 1 c R . O1 H2O1 H 0.07717 0.13432 0.10591 0.034 1.000 1 c R . O1 H1O2 H 0.15550 0.14931 0.35240 0.032 1.000 1 c R . O2 H2O2 H 0.13385 0.05370 0.41136 0.033 1.000 1 c R . O2 H1O3 H 0.51339 0.32966 0.15419 0.030 1.000 1 c R . O3 H2O3 H 0.53308 0.25428 0.09543 0.030 1.000 1 c R . O3 H1O4 H 0.67260 0.48435 0.34570 0.032 1.000 1 c R . O4 H2O4 H 0.59061 0.39164 0.40199 0.034 1.000 1 c R . O4 H1O5 H 0.33956 0.51638 0.14934 0.031 1.000 1 c R . O5 H2O5 H 0.41277 0.61223 0.09023 0.032 1.000 1 c R . O5 H1O6 H 0.18402 0.52566 0.34183 0.033 1.000 1 c R . O6 H2O6 H 0.27554 0.53230 0.39659 0.035 1.000 1 c R . O6 H1O7 H 0.20830 0.18944 0.06060 0.025 1.000 1 c R . O7 H2O7 H 0.17361 0.21215 -0.05035 0.025 1.000 1 c R . O7 H1O8 H 0.46170 0.31388 0.44337 0.025 1.000 1 c R . O8 H2O8 H 0.49136 0.36960 0.55568 0.025 1.000 1 c R . O8 H1O9 H 0.35005 0.47569 0.44255 0.025 1.000 1 c R . O9 H2O9 H 0.29312 0.45565 0.55353 0.025 1.000 1 c R . O9 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_refinement_flags_adp Al1 0.0137(3) 0.0137(3) 0.0203(3) 0.0062(4) -0.0011(2) -0.0007(2) . Mg1 0.0195(5) 0.0195(5) 0.0193(8) 0.0097(2) 0.0000 0.0000 T Mg2 0.0185(3) 0.0185(3) 0.0201(5) 0.0092(1) 0.0000 0.0000 T Mg3 0.0195(4) 0.0195(4) 0.0211(7) 0.0097(2) 0.0000 0.0000 T Na1 0.0165(4) 0.0186(4) 0.0347(4) 0.0100(5) 0.0011(3) 0.0007(3) . O11 0.0174(3) 0.0195(4) 0.0221(5) 0.0094(3) 0.0005(3) -0.0033(3) U O12 0.0186(4) 0.0206(4) 0.0227(5) 0.0087(3) 0.0037(3) -0.0017(3) U O13 0.0221(4) 0.0229(5) 0.0307(7) 0.0068(4) 0.0091(4) -0.0002(4) U O14 0.0190(5) 0.0200(4) 0.0309(6) 0.0090(3) -0.0007(4) -0.0072(4) U O21 0.0204(3) 0.0202(4) 0.0208(4) 0.0112(3) 0.0021(3) 0.0039(3) U O22 0.0202(3) 0.0199(4) 0.0258(4) 0.0110(3) 0.0043(3) 0.0074(3) U O23 0.0229(4) 0.0330(9) 0.0294(6) 0.0168(6) 0.0050(4) 0.0122(6) U O24 0.0230(4) 0.0318(7) 0.0284(5) 0.0166(4) 0.0069(4) 0.0109(4) U O31 0.0198(5) 0.0182(3) 0.0240(3) 0.0090(3) -0.0058(3) -0.0039(3) U O32 0.0219(4) 0.0192(3) 0.0246(3) 0.0103(3) -0.0069(3) -0.0034(3) U O33 0.0257(8) 0.0186(3) 0.0311(7) 0.0106(4) -0.0065(5) -0.0060(4) U O34 0.0233(6) 0.0206(4) 0.0347(7) 0.0120(5) -0.0078(4) -0.0016(4) U C11 0.0151(3) 0.0174(3) 0.0200(5) 0.0091(3) 0.0008(3) 0.0003(2) U C12 0.0145(3) 0.0169(4) 0.0202(5) 0.0096(3) -0.0012(2) -0.0013(2) U C21 0.0193(3) 0.0160(5) 0.0211(4) 0.0093(3) 0.0011(3) 0.0018(3) U C22 0.0193(3) 0.0157(4) 0.0221(3) 0.0092(3) 0.0022(3) 0.0025(3) U C31 0.0141(5) 0.0165(3) 0.0233(4) 0.0065(3) -0.0009(3) -0.0022(3) U C32 0.0140(4) 0.0173(3) 0.0244(4) 0.0072(3) -0.0016(3) -0.0008(3) U O1 0.0264(5) 0.0255(4) 0.0290(6) 0.0130(2) 0.0020(1) 0.0070(3) U O2 0.0253(4) 0.0259(4) 0.0290(6) 0.0125(3) -0.0069(3) -0.0049(2) U O3 0.0232(4) 0.0248(5) 0.0281(5) 0.0120(2) -0.0044(3) -0.0012(1) U O4 0.0286(5) 0.0278(4) 0.0282(5) 0.0147(3) 0.0019(1) -0.0051(2) U O5 0.0261(6) 0.0254(4) 0.0289(6) 0.0134(4) 0.0014(1) -0.0037(2) U O6 0.0284(4) 0.0277(4) 0.0288(6) 0.0135(3) 0.0051(2) 0.0071(3) U O7 0.0244(9) 0.0259(9) 0.0212(8) 0.0096(7) -0.0007(7) 0.0047(7) . O8 0.0262(8) 0.0300(7) 0.0192(6) 0.0155(7) -0.0052(6) -0.0029(5) . O9 0.0299(8) 0.0267(8) 0.0192(8) 0.0150(7) 0.0039(6) -0.0010(6) . H1O1 0.028 0.027 0.040 0.014 0.000 0.009 U H2O1 0.035 0.034 0.032 0.017 0.008 0.014 U H1O2 0.026 0.026 0.042 0.012 -0.009 -0.009 U H2O2 0.033 0.034 0.032 0.017 -0.013 -0.005 U H1O3 0.024 0.027 0.038 0.014 -0.006 0.000 U H2O3 0.029 0.030 0.031 0.014 -0.009 -0.006 U H1O4 0.031 0.028 0.038 0.016 0.000 -0.010 U H2O4 0.037 0.037 0.031 0.019 0.007 -0.005 U H1O5 0.028 0.025 0.040 0.014 0.000 -0.007 U H2O5 0.032 0.032 0.032 0.017 0.006 -0.004 U H1O6 0.029 0.029 0.038 0.013 0.010 0.009 U H2O6 0.038 0.036 0.032 0.018 0.006 0.013 U H1O7 0.024 0.026 0.021 0.010 -0.001 0.005 U H2O7 0.024 0.026 0.021 0.010 -0.001 0.005 U H1O8 0.030 0.025 0.019 0.015 0.003 -0.002 U H2O8 0.030 0.025 0.019 0.015 0.003 -0.002 U H1O9 0.027 0.030 0.019 0.015 -0.005 -0.004 U H2O9 0.027 0.030 0.019 0.015 -0.005 -0.004 U 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 Al1 O11 1.900(1) . . . Al1 O12 1.900(1) . . . Al1 O21 1.910(1) . . . Al1 O22 1.904(1) . . . Al1 O31 1.902(1) . . . Al1 O32 1.902(1) . . . Mg1 O1 2.064(1) . . . Mg1 O1 2.064(1) . 2_555 . Mg1 O1 2.064(1) . 3_555 . Mg1 O2 2.071(1) . . . Mg1 O2 2.071(1) . 2_555 . Mg1 O2 2.071(1) . 3_555 . Mg2 O3 2.071(1) . . . Mg2 O3 2.071(1) . 2_655 . Mg2 O3 2.071(1) . 3_665 . Mg2 O4 2.070(1) . . . Mg2 O4 2.070(1) . 2_655 . Mg2 O4 2.070(1) . 3_665 . Mg3 O5 2.081(1) . . . Mg3 O5 2.081(1) . 2_665 . Mg3 O5 2.081(1) . 3_565 . Mg3 O6 2.066(1) . . . Mg3 O6 2.066(1) . 2_665 . Mg3 O6 2.066(1) . 3_565 . Na1 O13 2.376(2) . 4_665 . Na1 O14 2.396(1) . 4_665 . Na1 O23 2.382(1) . 5_555 . Na1 O24 2.378(1) . 5_555 . Na1 O33 2.391(2) . 6_555 . Na1 O34 2.387(1) . 6_555 . O11 C11 1.282(2) . . . O12 C12 1.286(2) . . . O13 C11 1.224(2) . . . O14 C12 1.224(2) . . . O21 C21 1.287(2) . . . O22 C22 1.287(2) . . . O23 C21 1.220(2) . . . O24 C22 1.217(2) . . . O31 C31 1.293(2) . . . O32 C32 1.289(2) . . . O33 C31 1.220(2) . . . O34 C32 1.216(2) . . . C11 C12 1.550(2) . . . C21 C22 1.546(2) . . . C31 C32 1.548(2) . . . O1 H1O1 1.000 . . . O1 H2O1 1.000 . . . O2 H1O2 1.000 . . . O2 H2O2 1.000 . . . O3 H1O3 1.000 . . . O3 H2O3 1.000 . . . O4 H1O4 1.000 . . . O4 H2O4 1.000 . . . O5 H1O5 1.000 . . . O5 H2O5 1.000 . . . O6 H1O6 1.000 . . . O6 H2O6 1.000 . . . O7 H1O7 1.000 . . . O7 H2O7 1.000 . . . O8 H1O8 1.000 . . . O8 H2O8 1.000 . . . O9 H1O9 1.000 . . . O9 H2O9 1.000 . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O11 O3 2.878(2) . . . O12 O9 2.785(2) . . . O13 O8 2.732(2) . 4_664 . O14 O6 2.811(2) . 2_665 . O23 O9 2.729(2) . 5_554 . O24 O7 2.726(2) . 5_555 . O31 O7 2.787(2) . . . O32 O8 2.760(2) . . . O33 O1 2.827(2) . 3_555 . O34 O4 2.815(2) . 2_655 . O1 O7 2.739(2) . . . O2 O7 2.726(2) . 6_555 . O3 O8 2.721(2) . 6_554 . O4 O8 2.726(2) . . . O5 O9 2.735(2) . 4_664 . O6 O9 2.724(2) . . . 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 O11 Al1 O12 84.5(1) . . . . O11 Al1 O21 90.5(1) . . . . O11 Al1 O22 173.4(1) . . . . O11 Al1 O31 91.6(1) . . . . O11 Al1 O32 93.8(1) . . . . O12 Al1 O21 92.7(1) . . . . O12 Al1 O22 91.2(1) . . . . O12 Al1 O31 173.9(1) . . . . O12 Al1 O32 91.5(1) . . . . O21 Al1 O22 84.7(1) . . . . O21 Al1 O31 92.0(1) . . . . O21 Al1 O32 174.2(1) . . . . O22 Al1 O31 93.1(1) . . . . O22 Al1 O32 91.2(1) . . . . O31 Al1 O32 84.2(1) . . . . O1 Mg1 O1 90.4(1) . . 2_555 . O1 Mg1 O1 90.4(1) . . 3_555 . O1 Mg1 O2 89.7(1) . . . . O1 Mg1 O2 89.8(1) . . 2_555 . O1 Mg1 O2 179.7(1) . . 3_555 . O1 Mg1 O1 90.4(1) 2_555 . 3_555 . O1 Mg1 O2 179.7(1) 2_555 . . . O1 Mg1 O2 89.7(1) 2_555 . 2_555 . O1 Mg1 O2 89.8(1) 2_555 . 3_555 . O1 Mg1 O2 89.8(1) 3_555 . . . O1 Mg1 O2 179.7(1) 3_555 . 2_555 . O1 Mg1 O2 89.7(1) 3_555 . 3_555 . O2 Mg1 O2 90.1(1) . . 2_555 . O2 Mg1 O2 90.1(1) . . 3_555 . O2 Mg1 O2 90.1(1) 2_555 . 3_555 . O3 Mg2 O3 89.8(1) . . 2_655 . O3 Mg2 O3 89.8(1) . . 3_665 . O3 Mg2 O4 90.0(1) . . . . O3 Mg2 O4 89.5(1) . . 2_655 . O3 Mg2 O4 179.3(1) . . 3_665 . O3 Mg2 O3 89.8(1) 2_655 . 3_665 . O3 Mg2 O4 179.3(1) 2_655 . . . O3 Mg2 O4 90.0(1) 2_655 . 2_655 . O3 Mg2 O4 89.5(1) 2_655 . 3_665 . O3 Mg2 O4 89.5(1) 3_665 . . . O3 Mg2 O4 179.3(1) 3_665 . 2_655 . O3 Mg2 O4 90.0(1) 3_665 . 3_665 . O4 Mg2 O4 90.6(1) . . 2_655 . O4 Mg2 O4 90.6(1) . . 3_665 . O4 Mg2 O4 90.6(1) 2_655 . 3_665 . O5 Mg3 O5 90.0(1) . . 2_665 . O5 Mg3 O5 90.0(1) . . 3_565 . O5 Mg3 O6 89.5(1) . . . . O5 Mg3 O6 90.2(1) . . 2_665 . O5 Mg3 O6 179.5(1) . . 3_565 . O5 Mg3 O5 90.0(1) 2_665 . 3_565 . O5 Mg3 O6 179.5(1) 2_665 . . . O5 Mg3 O6 89.5(1) 2_665 . 2_665 . O5 Mg3 O6 90.2(1) 2_665 . 3_565 . O5 Mg3 O6 90.2(1) 3_565 . . . O5 Mg3 O6 179.5(1) 3_565 . 2_665 . O5 Mg3 O6 89.5(1) 3_565 . 3_565 . O6 Mg3 O6 90.3(1) . . 2_665 . O6 Mg3 O6 90.3(1) . . 3_565 . O6 Mg3 O6 90.3(1) 2_665 . 3_565 . O13 Na1 O14 71.1(1) 4_665 . 4_665 . O13 Na1 O23 98.3(1) 4_665 . 5_555 . O13 Na1 O24 164.1(1) 4_665 . 5_555 . O13 Na1 O33 98.7(1) 4_665 . 6_555 . O13 Na1 O34 91.5(1) 4_665 . 6_555 . O14 Na1 O23 96.5(1) 4_665 . 5_555 . O14 Na1 O24 98.0(1) 4_665 . 5_555 . O14 Na1 O33 165.2(1) 4_665 . 6_555 . O14 Na1 O34 97.3(1) 4_665 . 6_555 . O23 Na1 O24 70.9(1) 5_555 . 5_555 . O23 Na1 O33 95.6(1) 5_555 . 6_555 . O23 Na1 O34 165.1(1) 5_555 . 6_555 . O24 Na1 O33 94.0(1) 5_555 . 6_555 . O24 Na1 O34 101.5(1) 5_555 . 6_555 . O33 Na1 O34 71.8(1) 6_555 . 6_555 . Al1 O11 C11 114.4(1) . . . . Al1 O12 C12 114.5(1) . . . . Na1 O13 C11 114.6(1) 4_664 . . . Na1 O14 C12 113.6(1) 4_664 . . . Al1 O21 C21 114.0(1) . . . . Al1 O22 C22 114.3(1) . . . . Na1 O23 C21 114.2(1) 5_554 . . . Na1 O24 C22 114.8(1) 5_554 . . . Al1 O31 C31 114.9(1) . . . . Al1 O32 C32 115.2(1) . . . . Na1 O33 C31 113.1(1) 6_554 . . . Na1 O34 C32 113.2(1) 6_554 . . . O11 C11 O13 127.1(1) . . . . O11 C11 C12 113.3(1) . . . . O13 C11 C12 119.6(1) . . . . O12 C12 O14 126.9(1) . . . . O12 C12 C11 112.8(1) . . . . O14 C12 C11 120.4(1) . . . . O21 C21 O23 126.4(2) . . . . O21 C21 C22 113.4(1) . . . . O23 C21 C22 120.2(1) . . . . O22 C22 O24 127.1(2) . . . . O22 C22 C21 113.3(1) . . . . O24 C22 C21 119.6(1) . . . . O31 C31 O33 126.5(2) . . . . O31 C31 C32 112.8(1) . . . . O33 C31 C32 120.7(1) . . . . O32 C32 O34 126.3(2) . . . . O32 C32 C31 112.7(1) . . . . O34 C32 C31 121.0(1) . . . . Mg1 O1 H1O1 124.0 . . . . Mg2 O4 H1O4 125.1 . . . . Mg3 O6 H1O6 122.8 . . . . H1O7 O7 H2O7 109.5 . . . . H1O8 O8 H2O8 109.5 . . . . H1O9 O9 H2O9 109.5 . . . . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H1O1 O33 1.00 1.83 2.827(2) 174.8 2_555 . O1 H2O1 O7 1.00 1.74 2.739(2) 174.7 . . O2 H2O2 O7 1.00 1.73 2.726(2) 173.3 6_555 . O3 H1O3 O11 1.00 1.88 2.878(2) 172.7 . . O3 H2O3 O8 1.00 1.73 2.721(2) 172.5 6_554 . O4 H1O4 O34 1.00 1.82 2.815(2) 173.8 3_665 . O4 H2O4 O8 1.00 1.73 2.726(2) 173.7 . . O5 H2O5 O9 1.00 1.74 2.735(2) 172.6 4_664 . O6 H1O6 O14 1.00 1.81 2.811(2) 174.6 3_565 . O6 H2O6 O9 1.00 1.73 2.724(2) 174.5 . . O7 H1O7 O31 1.00 1.79 2.787(2) 174.3 . . O7 H2O7 O24 1.00 1.73 2.726(2) 174.3 5_554 . O8 H1O8 O32 1.00 1.76 2.760(2) 175.3 . . O8 H2O8 O13 1.00 1.73 2.732(2) 175.3 4_665 . O9 H1O9 O12 1.00 1.79 2.785(2) 175.9 . . O9 H2O9 O23 1.00 1.73 2.729(2) 175.8 5_555 . #===END