#------------------------------------------------------------------------------ #$Date: 2019-11-07 23:07:13 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223937 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/83/7048316.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_7048316 loop_ _publ_author_name 'Ptak, Maciej' 'Zarychta, Bartosz' 'Stefa\'nska, Dagmara' 'Ciupa, Aneta' 'Paraguassu, Waldeci' _publ_section_title ; Novel bimetallic MOF phosphors with an imidazolium cation: structure, phonons, high- pressure phase transitions and optical response. ; _journal_issue 1 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 242 _journal_page_last 252 _journal_paper_doi 10.1039/c8dt04246b _journal_volume 48 _journal_year 2018 _chemical_formula_sum 'C12 H16 Al N4 Na O12' _chemical_formula_weight 458.26 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2017-11-07 deposited with the CCDC. 2018-11-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.455(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.1711(2) _cell_length_b 12.3854(2) _cell_length_c 12.6588(2) _cell_measurement_reflns_used 3724 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 25.999 _cell_measurement_theta_min 3.219 _cell_volume 1908.18(5) _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2007)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2007)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2007)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100.0(1) _diffrn_detector_area_resol_mean 10.4508 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device '4-circle kappa geometry goniometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur System' _diffrn_measurement_method \w--scan _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 12728 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 3.219 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.306 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 3724 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.953 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.0629 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3029 _reflns_number_total 3724 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt04246b2.cif _cod_data_source_block 100K_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7048313--7048316.cif.' _cod_database_code 7048316 _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. ; _shelxl_version_number 2013-4 _shelx_res_file ; TITL mp_a.res in P2(1)/n REM Old TITL mP in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.177, Rweak 0.006, Alpha 0.024, Orientation as input REM Formula found by SHELXT: C16 O12 S2 CELL 0.71073 12.1711 12.3854 12.6588 90.000 90.455 90.000 ZERR 4.000 0.0002 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H O N Na Al UNIT 48 64 48 16 4 4 L.S. 10 BOND $H OMIT 0 52 OMIT 0 4 2 OMIT 4 4 4 OMIT -4 0 2 OMIT 0 4 4 OMIT 2 2 8 OMIT -5 3 2 OMIT 3 1 3 OMIT 2 2 4 OMIT 4 0 2 OMIT 2 4 2 OMIT -7 1 4 OMIT 5 1 3 OMIT 3 5 2 OMIT -4 0 4 OMIT -1 1 4 OMIT 4 2 1 OMIT 1 6 2 HTAB N11 O3 HTAB N11 O4 EQIV $1 x+1/2, -y+3/2, z-1/2 HTAB N14 O8_$1 HTAB N21 O11 HTAB N21 O12 EQIV $2 -x, -y+1, -z+1 HTAB N24 O6_$2 EQIV $3 -x+1/2, y-1/2, -z+3/2 HTAB N24 O10_$3 HTAB C5 O3 EQIV $4 -x+1, -y+1, -z+1 HTAB C15 O1_$4 HTAB C23 O9_$3 HTAB C25 O3_$2 HTAB C25 O5_$2 ACTA LIST 6 FMAP 2 PLAN 20 WGHT 0.039000 FVAR 0.34698 NA1 5 0.246480 0.760664 0.989101 11.00000 0.01114 0.01165 = 0.01071 -0.00068 0.00008 -0.00010 AL1 6 0.247425 0.757222 0.494077 11.00000 0.01062 0.01081 = 0.00886 0.00002 0.00005 0.00111 O1 3 0.295202 0.742841 0.634837 11.00000 0.01752 0.01632 = 0.01026 -0.00127 -0.00105 0.00454 O2 3 0.290399 0.751607 0.809232 11.00000 0.03246 0.03022 = 0.01048 0.00152 0.00123 0.00759 O3 3 0.293688 0.611625 0.469007 11.00000 0.01600 0.01212 = 0.01341 -0.00043 0.00221 0.00113 O4 3 0.326982 0.439797 0.505615 11.00000 0.02171 0.01108 = 0.02269 -0.00017 0.00519 0.00046 O5 3 0.199007 0.757779 0.351040 11.00000 0.01482 0.01999 = 0.01045 0.00138 -0.00035 -0.00274 O6 3 0.210126 0.760818 0.176626 11.00000 0.02169 0.02177 = 0.01030 0.00020 0.00094 0.00003 O7 3 0.194297 0.898489 0.518286 11.00000 0.01281 0.01114 = 0.01539 0.00122 0.00092 0.00084 O8 3 0.193723 1.077663 0.523666 11.00000 0.01858 0.01192 = 0.01788 -0.00080 0.00287 -0.00006 O9 3 0.386681 0.809478 0.458786 11.00000 0.01034 0.01488 = 0.01617 0.00157 0.00023 0.00114 O10 3 0.567632 0.808467 0.482806 11.00000 0.01243 0.02206 = 0.02482 -0.00258 -0.00289 0.00136 O11 3 0.107958 0.702663 0.533408 11.00000 0.01220 0.01437 = 0.01308 0.00226 0.00013 0.00075 O12 3 -0.071657 0.679675 0.527203 11.00000 0.01308 0.02314 = 0.02378 0.00803 0.00116 0.00072 N11 4 0.442369 0.467944 0.320218 11.00000 0.01663 0.01682 = 0.01542 0.00030 0.00336 0.00080 N14 4 0.550429 0.457630 0.187742 11.00000 0.01558 0.02307 = 0.01771 -0.00539 0.00406 -0.00257 N21 4 -0.020122 0.540947 0.687615 11.00000 0.03285 0.01626 = 0.01622 0.00296 0.00251 0.00052 N24 4 -0.060231 0.408745 0.788942 11.00000 0.01988 0.01538 = 0.01759 0.00217 0.00112 -0.00121 H11 2 0.410045 0.456682 0.378295 11.00000 -1.20000 H14 2 0.598661 0.439101 0.141861 11.00000 -1.20000 H21 2 -0.025419 0.586752 0.635461 11.00000 -1.20000 H24 2 -0.097690 0.352778 0.811972 11.00000 -1.20000 C1 1 0.256012 0.776991 0.722010 11.00000 0.01779 0.01669 = 0.01408 0.00055 0.00151 0.00340 AFIX 43 H1 2 0.197022 0.824630 0.718674 11.00000 -1.20000 AFIX 0 C2 1 0.285533 0.527799 0.527216 11.00000 0.01385 0.01497 = 0.01408 -0.00109 0.00152 -0.00123 AFIX 43 H2 2 0.246009 0.533502 0.589542 11.00000 -1.20000 AFIX 0 C3 1 0.241184 0.788934 0.265225 11.00000 0.01443 0.01481 = 0.01359 0.00209 0.00066 -0.00055 AFIX 43 H3 2 0.300059 0.836647 0.269408 11.00000 -1.20000 AFIX 0 C4 1 0.231359 0.990801 0.492671 11.00000 0.01360 0.01539 = 0.01327 0.00133 0.00177 0.00028 AFIX 43 H4 2 0.291083 0.993013 0.447350 11.00000 -1.20000 AFIX 0 C5 1 0.480496 0.763161 0.466955 11.00000 0.01487 0.01486 = 0.01460 -0.00074 0.00069 0.00158 AFIX 43 H5 2 0.482032 0.688410 0.460166 11.00000 -1.20000 AFIX 0 C6 1 0.013775 0.721023 0.494234 11.00000 0.01623 0.01428 = 0.01488 0.00431 0.00234 0.00409 AFIX 43 H6 2 0.008641 0.768357 0.437377 11.00000 -1.20000 AFIX 0 C12 1 0.416691 0.551459 0.253999 11.00000 0.02104 0.01961 = 0.02693 0.00388 0.00083 0.00517 AFIX 43 H12 2 0.362508 0.603207 0.264549 11.00000 -1.20000 AFIX 0 C13 1 0.484041 0.544989 0.171035 11.00000 0.02627 0.02508 = 0.02250 0.00677 0.00006 0.00000 AFIX 43 H13 2 0.485342 0.591166 0.113126 11.00000 -1.20000 AFIX 0 C15 1 0.523637 0.411886 0.278368 11.00000 0.01748 0.01726 = 0.02121 -0.00259 -0.00135 0.00233 AFIX 43 H15 2 0.556312 0.350826 0.307624 11.00000 -1.20000 AFIX 0 C22 1 0.049738 0.546492 0.773352 11.00000 0.02386 0.01894 = 0.02450 -0.00146 0.00259 -0.00437 AFIX 43 H22 2 0.104393 0.597721 0.784899 11.00000 -1.20000 AFIX 0 C23 1 0.023886 0.463415 0.837575 11.00000 0.02096 0.02252 = 0.01632 -0.00009 -0.00278 -0.00060 AFIX 43 H23 2 0.056718 0.446626 0.902100 11.00000 -1.20000 AFIX 0 C25 1 -0.085506 0.456775 0.698909 11.00000 0.02547 0.01720 = 0.01812 -0.00148 -0.00171 0.00105 AFIX 43 H25 2 -0.139997 0.435057 0.651577 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM mp_a.res in P2(1)/n REM R1 = 0.0250 for 3029 Fo > 4sig(Fo) and 0.0341 for all 3724 data REM 283 parameters refined using 0 restraints END WGHT 0.0390 0.0000 REM Highest difference peak 0.306, deepest hole -0.222, 1-sigma level 0.042 Q1 1 0.0521 0.5393 0.6940 11.00000 0.05 0.31 Q2 1 0.1564 0.7354 0.5118 11.00000 0.05 0.22 Q3 1 0.3302 0.7771 0.4740 11.00000 0.05 0.22 Q4 1 -0.0285 0.4787 0.6764 11.00000 0.05 0.22 Q5 1 0.3618 0.6058 0.3196 11.00000 0.05 0.19 Q6 1 0.1515 0.7992 0.7172 11.00000 0.05 0.16 Q7 1 0.0197 0.5288 0.8172 11.00000 0.05 0.14 Q8 1 0.2704 0.7526 0.5748 11.00000 0.05 0.14 Q9 1 0.1367 0.7312 0.3347 11.00000 0.05 0.14 Q10 1 0.3941 0.7973 0.4378 11.00000 0.05 0.14 Q11 1 0.3711 0.8664 0.4464 11.00000 0.05 0.14 Q12 1 0.2851 0.8829 0.3036 11.00000 0.05 0.13 Q13 1 0.1182 0.6932 0.5589 11.00000 0.05 0.13 Q14 1 0.2423 0.8544 0.5128 11.00000 0.05 0.13 Q15 1 0.1876 0.8851 0.4453 11.00000 0.05 0.13 Q16 1 0.4192 0.5294 0.1959 11.00000 0.05 0.13 Q17 1 0.2137 0.8795 0.6981 11.00000 0.05 0.13 Q18 1 0.3517 0.7187 0.6259 11.00000 0.05 0.12 Q19 1 0.3374 0.7947 0.2616 11.00000 0.05 0.12 Q20 1 0.4797 0.5829 0.2338 11.00000 0.05 0.12 ; _shelx_res_checksum 58447 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Na1 Na 0.24648(3) 0.76066(3) 0.98910(3) 0.01116(11) Uani 1 1 d . . Al1 Al 0.24742(3) 0.75722(3) 0.49408(2) 0.01010(9) Uani 1 1 d . . O1 O 0.29520(7) 0.74284(6) 0.63484(6) 0.01471(19) Uani 1 1 d . . O2 O 0.29040(8) 0.75161(7) 0.80923(6) 0.0244(2) Uani 1 1 d . . O3 O 0.29369(6) 0.61163(6) 0.46901(6) 0.01383(18) Uani 1 1 d . . O4 O 0.32698(7) 0.43980(6) 0.50562(6) 0.0185(2) Uani 1 1 d . . O5 O 0.19901(7) 0.75778(6) 0.35104(6) 0.01509(19) Uani 1 1 d . . O6 O 0.21013(7) 0.76082(7) 0.17663(6) 0.0179(2) Uani 1 1 d . . O7 O 0.19430(6) 0.89849(6) 0.51829(6) 0.01311(18) Uani 1 1 d . . O8 O 0.19372(7) 1.07766(6) 0.52367(6) 0.01611(19) Uani 1 1 d . . O9 O 0.38668(6) 0.80948(6) 0.45879(6) 0.01380(18) Uani 1 1 d . . O10 O 0.56763(7) 0.80847(7) 0.48281(7) 0.0198(2) Uani 1 1 d . . O11 O 0.10796(6) 0.70266(6) 0.53341(6) 0.01322(18) Uani 1 1 d . . O12 O -0.07166(7) 0.67967(7) 0.52720(7) 0.0200(2) Uani 1 1 d . . N11 N 0.44237(9) 0.46794(8) 0.32022(8) 0.0163(2) Uani 1 1 d . . N14 N 0.55043(9) 0.45763(9) 0.18774(8) 0.0188(2) Uani 1 1 d . . N21 N -0.02012(9) 0.54095(9) 0.68761(8) 0.0218(3) Uani 1 1 d . . N24 N -0.06023(9) 0.40874(8) 0.78894(8) 0.0176(2) Uani 1 1 d . . H11 H 0.4100(11) 0.4567(11) 0.3783(10) 0.021 Uiso 1 1 d . U H14 H 0.5987(11) 0.4391(11) 0.1419(11) 0.021 Uiso 1 1 d . U H21 H -0.0254(11) 0.5868(11) 0.6355(10) 0.021 Uiso 1 1 d . U H24 H -0.0977(11) 0.3528(11) 0.8120(10) 0.021 Uiso 1 1 d . U C1 C 0.25601(10) 0.77699(10) 0.72201(9) 0.0162(3) Uani 1 1 d . . H1 H 0.1970 0.8246 0.7187 0.019 Uiso 1 1 calc R U C2 C 0.28553(10) 0.52780(9) 0.52722(9) 0.0143(3) Uani 1 1 d . . H2 H 0.2460 0.5335 0.5895 0.017 Uiso 1 1 calc R U C3 C 0.24118(10) 0.78893(9) 0.26523(9) 0.0143(3) Uani 1 1 d . . H3 H 0.3001 0.8366 0.2694 0.017 Uiso 1 1 calc R U C4 C 0.23136(10) 0.99080(9) 0.49267(9) 0.0141(3) Uani 1 1 d . . H4 H 0.2911 0.9930 0.4474 0.017 Uiso 1 1 calc R U C5 C 0.48050(9) 0.76316(10) 0.46695(9) 0.0148(3) Uani 1 1 d . . H5 H 0.4820 0.6884 0.4602 0.018 Uiso 1 1 calc R U C6 C 0.01378(10) 0.72102(9) 0.49423(9) 0.0151(3) Uani 1 1 d . . H6 H 0.0086 0.7684 0.4374 0.018 Uiso 1 1 calc R U C12 C 0.41669(11) 0.55146(10) 0.25400(10) 0.0225(3) Uani 1 1 d . . H12 H 0.3625 0.6032 0.2645 0.027 Uiso 1 1 calc R U C13 C 0.48404(11) 0.54499(11) 0.17104(10) 0.0246(3) Uani 1 1 d . . H13 H 0.4853 0.5912 0.1131 0.030 Uiso 1 1 calc R U C15 C 0.52364(10) 0.41189(10) 0.27837(10) 0.0187(3) Uani 1 1 d . . H15 H 0.5563 0.3508 0.3076 0.022 Uiso 1 1 calc R U C22 C 0.04974(11) 0.54649(10) 0.77335(10) 0.0224(3) Uani 1 1 d . . H22 H 0.1044 0.5977 0.7849 0.027 Uiso 1 1 calc R U C23 C 0.02389(11) 0.46341(10) 0.83757(10) 0.0200(3) Uani 1 1 d . . H23 H 0.0567 0.4466 0.9021 0.024 Uiso 1 1 calc R U C25 C -0.08551(11) 0.45678(10) 0.69891(10) 0.0203(3) Uani 1 1 d . . H25 H -0.1400 0.4351 0.6516 0.024 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 Na1 0.0111(2) 0.0116(2) 0.0107(2) -0.00068(17) 0.00008(18) -0.00010(18) Al1 0.01062(18) 0.01081(18) 0.00886(18) 0.00002(13) 0.00005(13) 0.00111(13) O1 0.0175(5) 0.0163(4) 0.0103(4) -0.0013(3) -0.0010(3) 0.0045(3) O2 0.0325(6) 0.0302(5) 0.0105(5) 0.0015(4) 0.0012(4) 0.0076(4) O3 0.0160(4) 0.0121(4) 0.0134(4) -0.0004(3) 0.0022(3) 0.0011(3) O4 0.0217(5) 0.0111(4) 0.0227(5) -0.0002(3) 0.0052(4) 0.0005(3) O5 0.0148(4) 0.0200(5) 0.0105(4) 0.0014(3) -0.0004(3) -0.0027(3) O6 0.0217(5) 0.0218(5) 0.0103(4) 0.0002(3) 0.0009(4) 0.0000(4) O7 0.0128(4) 0.0111(4) 0.0154(4) 0.0012(3) 0.0009(3) 0.0008(3) O8 0.0186(5) 0.0119(4) 0.0179(4) -0.0008(3) 0.0029(3) -0.0001(3) O9 0.0103(4) 0.0149(4) 0.0162(4) 0.0016(3) 0.0002(3) 0.0011(3) O10 0.0124(5) 0.0221(5) 0.0248(5) -0.0026(4) -0.0029(4) 0.0014(4) O11 0.0122(4) 0.0144(4) 0.0131(4) 0.0023(3) 0.0001(3) 0.0007(3) O12 0.0131(5) 0.0231(5) 0.0238(5) 0.0080(4) 0.0012(4) 0.0007(4) N11 0.0166(6) 0.0168(5) 0.0154(6) 0.0003(4) 0.0034(4) 0.0008(4) N14 0.0156(6) 0.0231(6) 0.0177(6) -0.0054(4) 0.0041(4) -0.0026(5) N21 0.0329(7) 0.0163(6) 0.0162(6) 0.0030(4) 0.0025(5) 0.0005(5) N24 0.0199(6) 0.0154(5) 0.0176(5) 0.0022(4) 0.0011(4) -0.0012(4) C1 0.0178(7) 0.0167(6) 0.0141(6) 0.0006(5) 0.0015(5) 0.0034(5) C2 0.0138(6) 0.0150(6) 0.0141(6) -0.0011(5) 0.0015(5) -0.0012(5) C3 0.0144(6) 0.0148(6) 0.0136(6) 0.0021(5) 0.0007(5) -0.0006(5) C4 0.0136(7) 0.0154(6) 0.0133(6) 0.0013(5) 0.0018(5) 0.0003(5) C5 0.0149(6) 0.0149(6) 0.0146(6) -0.0007(5) 0.0007(5) 0.0016(5) C6 0.0162(7) 0.0143(6) 0.0149(6) 0.0043(5) 0.0023(5) 0.0041(5) C12 0.0210(7) 0.0196(7) 0.0269(7) 0.0039(5) 0.0008(6) 0.0052(5) C13 0.0263(8) 0.0251(7) 0.0225(7) 0.0068(6) 0.0001(6) 0.0000(6) C15 0.0175(7) 0.0173(6) 0.0212(7) -0.0026(5) -0.0013(5) 0.0023(5) C22 0.0239(7) 0.0189(7) 0.0245(7) -0.0015(5) 0.0026(6) -0.0044(5) C23 0.0210(7) 0.0225(7) 0.0163(6) -0.0001(5) -0.0028(5) -0.0006(5) C25 0.0255(7) 0.0172(7) 0.0181(7) -0.0015(5) -0.0017(5) 0.0011(5) 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' N N 0.0061 0.0033 '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' Al Al 0.0645 0.0514 '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 O10 Na1 O2 99.70(3) 4_576 . O10 Na1 O12 169.82(3) 4_576 4_676 O2 Na1 O12 89.59(3) . 4_676 O10 Na1 O8 86.23(3) 4_576 2_546 O2 Na1 O8 79.45(3) . 2_546 O12 Na1 O8 91.43(3) 4_676 2_546 O10 Na1 O4 89.57(3) 4_576 2_556 O2 Na1 O4 99.18(3) . 2_556 O12 Na1 O4 93.07(3) 4_676 2_556 O8 Na1 O4 175.29(3) 2_546 2_556 O10 Na1 O6 81.74(3) 4_576 1_556 O2 Na1 O6 176.22(3) . 1_556 O12 Na1 O6 88.73(3) 4_676 1_556 O8 Na1 O6 97.21(3) 2_546 1_556 O4 Na1 O6 84.29(3) 2_556 1_556 O9 Al1 O1 89.15(4) . . O9 Al1 O7 91.73(4) . . O1 Al1 O7 92.16(3) . . O9 Al1 O11 178.39(4) . . O1 Al1 O11 89.32(4) . . O7 Al1 O11 88.81(4) . . O9 Al1 O5 92.63(4) . . O1 Al1 O5 174.77(4) . . O7 Al1 O5 92.71(4) . . O11 Al1 O5 88.85(4) . . O9 Al1 O3 91.03(4) . . O1 Al1 O3 88.78(3) . . O7 Al1 O3 177.09(4) . . O11 Al1 O3 88.45(4) . . O5 Al1 O3 86.27(3) . . C1 O1 Al1 132.30(8) . . C1 O2 Na1 141.97(9) . . C2 O3 Al1 130.16(8) . . C2 O4 Na1 131.29(8) . 2_546 C3 O5 Al1 133.98(8) . . C3 O6 Na1 146.86(8) . 1_554 C4 O7 Al1 131.90(8) . . C4 O8 Na1 133.79(8) . 2_556 C5 O9 Al1 129.35(8) . . C5 O10 Na1 130.33(8) . 4_675 C6 O11 Al1 129.98(7) . . C6 O12 Na1 125.96(8) . 4_575 C15 N11 C12 108.65(11) . . C15 N11 H11 127.9(9) . . C12 N11 H11 123.4(9) . . C15 N14 C13 108.91(11) . . C15 N14 H14 130.2(9) . . C13 N14 H14 120.9(9) . . C25 N21 C22 108.87(10) . . C25 N21 H21 123.7(9) . . C22 N21 H21 127.3(9) . . C25 N24 C23 109.49(11) . . C25 N24 H24 121.5(9) . . C23 N24 H24 128.9(9) . . O2 C1 O1 124.69(11) . . O2 C1 H1 117.7 . . O1 C1 H1 117.7 . . O4 C2 O3 123.84(11) . . O4 C2 H2 118.1 . . O3 C2 H2 118.1 . . O6 C3 O5 124.90(11) . . O6 C3 H3 117.5 . . O5 C3 H3 117.5 . . O8 C4 O7 124.68(11) . . O8 C4 H4 117.7 . . O7 C4 H4 117.7 . . O10 C5 O9 125.64(11) . . O10 C5 H5 117.2 . . O9 C5 H5 117.2 . . O12 C6 O11 123.74(11) . . O12 C6 H6 118.1 . . O11 C6 H6 118.1 . . C13 C12 N11 107.30(11) . . C13 C12 H12 126.4 . . N11 C12 H12 126.4 . . C12 C13 N14 106.91(11) . . C12 C13 H13 126.5 . . N14 C13 H13 126.5 . . N14 C15 N11 108.23(11) . . N14 C15 H15 125.9 . . N11 C15 H15 125.9 . . C23 C22 N21 106.95(11) . . C23 C22 H22 126.5 . . N21 C22 H22 126.5 . . C22 C23 N24 106.44(11) . . C22 C23 H23 126.8 . . N24 C23 H23 126.8 . . N24 C25 N21 108.24(11) . . N24 C25 H25 125.9 . . N21 C25 H25 125.9 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Na1 O10 2.3398(9) 4_576 Na1 O2 2.3456(9) . Na1 O12 2.3794(9) 4_676 Na1 O8 2.3864(9) 2_546 Na1 O4 2.3931(9) 2_556 Na1 O6 2.4182(9) 1_556 Al1 O9 1.8717(8) . Al1 O1 1.8784(8) . Al1 O7 1.8911(8) . Al1 O11 1.8972(8) . Al1 O5 1.8997(8) . Al1 O3 1.9164(8) . O1 C1 1.2777(14) . O2 C1 1.2189(14) . O3 C2 1.2774(14) . O4 C2 1.2327(14) . O4 Na1 2.3931(9) 2_546 O5 C3 1.2654(14) . O6 C3 1.2310(14) . O6 Na1 2.4182(9) 1_554 O7 C4 1.2721(14) . O8 C4 1.2345(14) . O8 Na1 2.3864(9) 2_556 O9 C5 1.2813(13) . O10 C5 1.2151(14) . O10 Na1 2.3399(9) 4_675 O11 C6 1.2659(14) . O12 C6 1.2347(14) . O12 Na1 2.3793(9) 4_575 N11 C15 1.3226(15) . N11 C12 1.3661(16) . N11 H11 0.848(14) . N14 C15 1.3226(15) . N14 C13 1.3659(17) . N14 H14 0.860(14) . N21 C25 1.3200(16) . N21 C22 1.3751(17) . N21 H21 0.872(13) . N24 C25 1.3198(15) . N24 C23 1.3695(16) . N24 H24 0.881(13) . C1 H1 0.9300 . C2 H2 0.9300 . C3 H3 0.9300 . C4 H4 0.9300 . C5 H5 0.9300 . C6 H6 0.9300 . C12 C13 1.3398(18) . C12 H12 0.9300 . C13 H13 0.9300 . C15 H15 0.9300 . C22 C23 1.3501(18) . C22 H22 0.9300 . C23 H23 0.9300 . C25 H25 0.9300 . 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 N11 H11 O3 0.848(14) 2.652(14) 3.1691(13) 120.6(11) . N11 H11 O4 0.848(14) 1.921(14) 2.7666(13) 175.0(13) . N14 H14 O8 0.860(14) 1.910(14) 2.7576(13) 168.2(13) 4_675 N21 H21 O11 0.872(13) 2.530(13) 3.2095(13) 135.4(11) . N21 H21 O12 0.872(13) 1.873(13) 2.7293(13) 166.7(13) . N24 H24 O6 0.881(13) 1.969(13) 2.8181(13) 161.6(12) 3_566 N24 H24 O10 0.881(13) 2.677(13) 3.1470(13) 114.5(10) 2_546 C5 H5 O3 0.93 2.49 2.9485(14) 111.0 . C15 H15 O1 0.93 2.26 3.1149(15) 152.0 3_666 C23 H23 O9 0.93 2.54 3.3794(15) 150.6 2_546 C25 H25 O3 0.93 2.47 3.4016(15) 175.7 3_566 C25 H25 O5 0.93 2.49 3.0587(15) 119.3 3_566