#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:38:30 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257517 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705279.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_7705279 loop_ _publ_author_name 'Cha, Jeongmin' 'Kwon, Hyunchul' 'Song, Hayoung' 'Lee, Eunsung' _publ_section_title ; Dinitrogen activation by a penta-pyridyl molybdenum complex. ; _journal_issue 37 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12945 _journal_page_last 12949 _journal_paper_doi 10.1039/d0dt02692a _journal_volume 49 _journal_year 2020 _chemical_formula_moiety '0.5(C54 H74 N6 Na4 O8)' _chemical_formula_sum 'C27 H37 N3 Na2 O4' _chemical_formula_weight 513.57 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-07-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-07 deposited with the CCDC. 2020-08-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 113.285(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.427(5) _cell_length_b 18.077(10) _cell_length_c 11.027(4) _cell_measurement_reflns_used 281 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 23.50 _cell_measurement_theta_min 3.07 _cell_volume 2642(2) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.508 _diffrn_measured_fraction_theta_max 0.484 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_unetI/netI 0.0839 _diffrn_reflns_Laue_measured_fraction_full 0.508 _diffrn_reflns_Laue_measured_fraction_max 0.484 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 1939 _diffrn_reflns_point_group_measured_fraction_full 0.508 _diffrn_reflns_point_group_measured_fraction_max 0.484 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.300 _diffrn_reflns_theta_min 3.074 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.291 _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.263 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.052 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 167 _refine_ls_number_reflns 1595 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.960 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0617 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1477 _refine_ls_wR_factor_ref 0.1886 _reflns_Friedel_coverage 0.000 _reflns_number_gt 973 _reflns_number_total 1595 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02692a2.cif _cod_data_source_block c2c_a _cod_depositor_comments 'Adding full bibliography for 7705278--7705279.cif.' _cod_original_cell_volume 2641.5(19) _cod_database_code 7705279 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C00E(H00E,H00F), C00F(H00G,H00H) 2.b Aromatic/amide H refined with riding coordinates: C008(H008), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D), C00H(H00L) 2.c Idealised Me refined as rotating group: C00G(H00I,H00J,H00K), C00I(H00M,H00N,H00O), C00J(H00P,H00Q,H00R) ; _shelx_res_file ; TITL c2c_a_a.res in C2/c c2c_a.res created by SHELXL-2018/3 at 09:57:47 on 07-Jul-2020 REM Old TITL C2C_a.res in C2/c REM SHELXT solution in C2/c: R1 0.174, Rweak 0.002, Alpha 0.044 REM 0.392 for 56 systematic absences, Orientation as input REM Formula found by SHELXT: C27 N3 O4 Na2 CELL 0.71073 14.4268 18.0771 11.0267 90 113.285 90 ZERR 4 0.0046 0.0101 0.0039 0 0.008 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N Na O UNIT 108 148 12 8 16 L.S. 10 PLAN 20 TEMP 0 BOND list 4 fmap 2 ACTA REM REM REM WGHT 0.100000 FVAR 0.25733 NA01 4 0.617902 0.782559 0.359293 11.00000 0.01199 0.02310 = 0.01365 -0.00160 0.00256 -0.00083 O002 5 0.713395 0.777930 0.607016 11.00000 0.01933 0.03496 = 0.01911 -0.00356 0.00813 0.00288 O003 5 0.701651 0.901242 0.438922 11.00000 0.02254 0.02378 = 0.02883 -0.00286 -0.00109 -0.00321 N004 3 0.540782 0.816668 0.124958 11.00000 0.01385 0.01401 = 0.01608 0.00041 0.00704 0.00058 N005 3 0.500000 0.686181 0.250000 10.50000 0.01560 0.00974 = 0.01123 0.00000 -0.00024 0.00000 C006 1 0.565631 0.763530 0.051659 11.00000 0.00830 0.03916 = 0.01051 -0.00402 0.00132 0.00088 C007 1 0.527740 0.648316 0.160489 11.00000 0.01265 0.02199 = 0.01625 -0.00453 -0.00185 0.00205 C008 1 0.545452 0.887977 0.100265 11.00000 0.01853 0.02269 = 0.02051 0.00039 0.00791 -0.00238 AFIX 43 H008 2 0.527235 0.921239 0.151347 11.00000 -1.20000 AFIX 0 C009 1 0.558844 0.687646 0.068446 11.00000 0.02517 0.02252 = 0.01861 -0.00213 0.00827 0.00698 C00A 1 0.525375 0.570191 0.158798 11.00000 0.02540 0.01059 = 0.02672 -0.00697 0.00320 0.00287 AFIX 43 H00A 2 0.540886 0.544309 0.096353 11.00000 -1.20000 AFIX 0 C00B 1 0.500000 0.532366 0.250000 10.50000 0.02676 0.01594 = 0.03928 0.00000 -0.00187 0.00000 AFIX 43 H00B 2 0.500001 0.480920 0.250001 10.50000 -1.20000 AFIX 0 C00C 1 0.574797 0.917210 0.005947 11.00000 0.02644 0.04165 = 0.02510 0.00493 0.01343 -0.00606 AFIX 43 H00C 2 0.577243 0.967894 -0.006947 11.00000 -1.20000 AFIX 0 C00D 1 0.597881 0.792678 -0.047404 11.00000 0.04808 0.04047 = 0.03572 -0.01211 0.03527 -0.01208 AFIX 43 H00D 2 0.617391 0.759873 -0.097906 11.00000 -1.20000 AFIX 0 C00E 1 0.708188 0.853342 0.645086 11.00000 0.01832 0.04174 = 0.02280 -0.00905 0.00399 0.00494 AFIX 23 H00E 2 0.742864 0.858105 0.740097 11.00000 -1.20000 H00F 2 0.638219 0.867332 0.620795 11.00000 -1.20000 AFIX 0 C00F 1 0.755229 0.903075 0.579257 11.00000 0.01971 0.03041 = 0.03361 -0.01468 -0.00506 0.00901 AFIX 23 H00G 2 0.755635 0.953242 0.610679 11.00000 -1.20000 H00H 2 0.824639 0.888109 0.601805 11.00000 -1.20000 AFIX 0 C00G 1 0.741423 0.953133 0.378073 11.00000 0.03222 0.02284 = 0.04659 0.00538 0.00469 -0.00991 AFIX 137 H00I 2 0.812384 0.944421 0.404618 11.00000 -1.50000 H00J 2 0.731059 1.002107 0.403992 11.00000 -1.50000 H00K 2 0.708074 0.948419 0.283925 11.00000 -1.50000 AFIX 0 C00H 1 0.600566 0.865522 -0.068810 11.00000 0.05595 0.04705 = 0.03483 -0.00285 0.03702 -0.01835 AFIX 43 H00L 2 0.620108 0.881834 -0.135167 11.00000 -1.20000 AFIX 0 C00I 1 0.678249 0.727823 0.679629 11.00000 0.01890 0.07112 = 0.01990 0.01117 0.00718 0.00349 AFIX 137 H00M 2 0.614522 0.744700 0.677472 11.00000 -1.50000 H00N 2 0.726354 0.725598 0.769503 11.00000 -1.50000 H00O 2 0.670246 0.679490 0.640724 11.00000 -1.50000 AFIX 0 C00J 1 0.585347 0.639185 -0.025587 11.00000 0.12822 0.02140 = 0.05478 0.00748 0.06289 0.03279 AFIX 137 H00P 2 0.528250 0.635837 -0.108419 11.00000 -1.50000 H00Q 2 0.603201 0.590629 0.011624 11.00000 -1.50000 H00R 2 0.641359 0.660429 -0.039461 11.00000 -1.50000 AFIX 0 HKLF 4 REM c2c_a_a.res in C2/c REM wR2 = 0.1886, GooF = S = 0.960, Restrained GooF = 0.960 for all data REM R1 = 0.0617 for 973 Fo > 4sig(Fo) and 0.1064 for all 1595 data REM 167 parameters refined using 0 restraints END WGHT 0.0764 0.0000 REM Highest difference peak 0.263, deepest hole -0.240, 1-sigma level 0.052 Q1 1 0.7332 0.8885 0.3615 11.00000 0.05 0.26 Q2 1 0.5631 0.6534 -0.1148 11.00000 0.05 0.22 Q3 1 0.6715 0.6487 0.1109 11.00000 0.05 0.22 Q4 1 0.5378 0.7291 0.2815 11.00000 0.05 0.19 Q5 1 0.6124 0.6917 0.5948 11.00000 0.05 0.19 Q6 1 0.6997 0.8416 -0.1209 11.00000 0.05 0.19 Q7 1 0.5123 0.5152 0.0345 11.00000 0.05 0.18 Q8 1 0.5378 0.7791 0.2738 11.00000 0.05 0.18 Q9 1 0.6528 0.8081 -0.0155 11.00000 0.05 0.18 Q10 1 0.5887 0.9318 -0.1911 11.00000 0.05 0.18 Q11 1 0.5037 0.6000 -0.0603 11.00000 0.05 0.17 Q12 1 0.6191 0.7222 0.7956 11.00000 0.05 0.17 Q13 1 0.4720 0.5611 -0.0745 11.00000 0.05 0.17 Q14 1 0.6223 0.6525 0.0019 11.00000 0.05 0.17 Q15 1 0.5622 0.5708 -0.0610 11.00000 0.05 0.16 Q16 1 0.7659 0.8889 0.7343 11.00000 0.05 0.16 Q17 1 0.5571 0.7247 -0.1573 11.00000 0.05 0.16 Q18 1 0.7286 0.6715 0.8857 11.00000 0.05 0.16 Q19 1 0.6196 0.9582 0.1167 11.00000 0.05 0.16 Q20 1 0.5100 0.8538 -0.0792 11.00000 0.05 0.16 ; _shelx_res_checksum 10428 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Na01 Na 0.61790(9) 0.78256(12) 0.35929(11) 0.0170(6) Uani 1 1 d . . . . . O002 O 0.71339(18) 0.7779(2) 0.6070(2) 0.0243(10) Uani 1 1 d . . . . . O003 O 0.70165(19) 0.9012(3) 0.4389(2) 0.0286(11) Uani 1 1 d . . . . . N004 N 0.5408(2) 0.8167(3) 0.1250(3) 0.0143(10) Uani 1 1 d . . . . . N005 N 0.500000 0.6862(3) 0.250000 0.0139(13) Uani 1 2 d S T P . . C006 C 0.5656(3) 0.7635(3) 0.0517(3) 0.0201(14) Uani 1 1 d . . . . . C007 C 0.5277(3) 0.6483(3) 0.1605(3) 0.0193(12) Uani 1 1 d . . . . . C008 C 0.5455(3) 0.8880(3) 0.1003(3) 0.0205(13) Uani 1 1 d . . . . . H008 H 0.527235 0.921239 0.151347 0.025 Uiso 1 1 calc R . . . . C009 C 0.5588(3) 0.6876(3) 0.0684(3) 0.0222(13) Uani 1 1 d . . . . . C00A C 0.5254(3) 0.5702(3) 0.1588(4) 0.0231(12) Uani 1 1 d . . . . . H00A H 0.540886 0.544309 0.096353 0.028 Uiso 1 1 calc R . . . . C00B C 0.500000 0.5324(5) 0.250000 0.032(2) Uani 1 2 d S T P . . H00B H 0.500001 0.480920 0.250001 0.038 Uiso 1 2 calc RS T P . . C00C C 0.5748(3) 0.9172(4) 0.0059(3) 0.0300(16) Uani 1 1 d . . . . . H00C H 0.577243 0.967894 -0.006947 0.036 Uiso 1 1 calc R . . . . C00D C 0.5979(4) 0.7927(4) -0.0474(4) 0.0356(18) Uani 1 1 d . . . . . H00D H 0.617391 0.759873 -0.097906 0.043 Uiso 1 1 calc R . . . . C00E C 0.7082(3) 0.8533(4) 0.6451(3) 0.0289(16) Uani 1 1 d . . . . . H00E H 0.742864 0.858105 0.740097 0.035 Uiso 1 1 calc R . . . . H00F H 0.638219 0.867332 0.620795 0.035 Uiso 1 1 calc R . . . . C00F C 0.7552(3) 0.9031(4) 0.5793(4) 0.0328(15) Uani 1 1 d . . . . . H00G H 0.755635 0.953242 0.610679 0.039 Uiso 1 1 calc R . . . . H00H H 0.824639 0.888109 0.601805 0.039 Uiso 1 1 calc R . . . . C00G C 0.7414(3) 0.9531(4) 0.3781(4) 0.0373(16) Uani 1 1 d . . . . . H00I H 0.812384 0.944421 0.404618 0.056 Uiso 1 1 calc GR . . . . H00J H 0.731059 1.002107 0.403992 0.056 Uiso 1 1 calc GR . . . . H00K H 0.708074 0.948419 0.283925 0.056 Uiso 1 1 calc GR . . . . C00H C 0.6006(4) 0.8655(5) -0.0688(4) 0.040(2) Uani 1 1 d . . . . . H00L H 0.620108 0.881834 -0.135167 0.048 Uiso 1 1 calc R . . . . C00I C 0.6782(3) 0.7278(4) 0.6796(3) 0.037(2) Uani 1 1 d . . . . . H00M H 0.614522 0.744700 0.677472 0.055 Uiso 1 1 calc GR . . . . H00N H 0.726354 0.725598 0.769503 0.055 Uiso 1 1 calc GR . . . . H00O H 0.670246 0.679490 0.640724 0.055 Uiso 1 1 calc GR . . . . C00J C 0.5853(5) 0.6392(5) -0.0256(5) 0.060(2) Uani 1 1 d . . . . . H00P H 0.528250 0.635837 -0.108419 0.090 Uiso 1 1 calc GR . . . . H00Q H 0.603201 0.590629 0.011624 0.090 Uiso 1 1 calc GR . . . . H00R H 0.641359 0.660429 -0.039461 0.090 Uiso 1 1 calc GR . . . . 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 Na01 0.0120(7) 0.0231(16) 0.0136(6) -0.0016(6) 0.0026(5) -0.0008(7) O002 0.0193(14) 0.035(3) 0.0191(12) -0.0036(14) 0.0081(11) 0.0029(14) O003 0.0225(15) 0.024(4) 0.0288(14) -0.0029(15) -0.0011(11) -0.0032(14) N004 0.0139(15) 0.014(3) 0.0161(13) 0.0004(14) 0.0070(11) 0.0006(14) N005 0.016(2) 0.010(4) 0.0112(17) 0.000 -0.0002(15) 0.000 C006 0.0083(18) 0.039(5) 0.0105(14) -0.0040(17) 0.0013(13) 0.0009(17) C007 0.0126(18) 0.022(4) 0.0162(15) -0.0045(17) -0.0019(13) 0.0021(17) C008 0.019(2) 0.023(4) 0.0205(16) 0.0004(18) 0.0079(15) -0.0024(19) C009 0.025(2) 0.023(5) 0.0186(16) -0.0021(18) 0.0083(15) 0.007(2) C00A 0.025(2) 0.011(4) 0.0267(18) -0.0070(18) 0.0032(16) 0.0029(18) C00B 0.027(3) 0.016(6) 0.039(3) 0.000 -0.002(3) 0.000 C00C 0.026(2) 0.042(5) 0.0251(19) 0.005(2) 0.0134(17) -0.006(2) C00D 0.048(3) 0.040(7) 0.036(2) -0.012(2) 0.035(2) -0.012(3) C00E 0.018(2) 0.042(5) 0.0228(17) -0.009(2) 0.0040(16) 0.005(2) C00F 0.020(2) 0.030(5) 0.034(2) -0.015(2) -0.0051(16) 0.009(2) C00G 0.032(2) 0.023(5) 0.047(2) 0.005(3) 0.005(2) -0.010(2) C00H 0.056(3) 0.047(7) 0.035(2) -0.003(3) 0.037(2) -0.018(3) C00I 0.019(2) 0.071(7) 0.0199(17) 0.011(2) 0.0072(16) 0.003(2) C00J 0.128(5) 0.021(7) 0.055(3) 0.007(3) 0.063(3) 0.033(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' 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' O O 0.0106 0.0060 '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 Na01 Na01 Na01 162.09(6) 2_655 7_666 ? O002 Na01 Na01 138.85(9) . 2_655 ? O002 Na01 Na01 37.44(6) 7_666 7_666 ? O002 Na01 Na01 138.83(9) 7_666 2_655 ? O002 Na01 Na01 37.96(7) . 7_666 ? O002 Na01 O002 75.41(10) . 7_666 ? O003 Na01 Na01 78.29(9) . 7_666 ? O003 Na01 Na01 118.80(8) . 2_655 ? O003 Na01 O002 70.16(12) . . ? O003 Na01 O002 90.93(13) . 7_666 ? O003 Na01 N004 96.40(15) . . ? N004 Na01 Na01 47.45(8) . 2_655 ? N004 Na01 Na01 47.75(7) 2_655 2_655 ? N004 Na01 Na01 141.49(9) . 7_666 ? N004 Na01 Na01 130.37(8) 2_655 7_666 ? N004 Na01 O002 164.24(14) 2_655 7_666 ? N004 Na01 O002 105.64(10) . 7_666 ? N004 Na01 O002 93.28(9) 2_655 . ? N004 Na01 O002 166.56(17) . . ? N004 Na01 O003 95.55(15) 2_655 . ? N004 Na01 N004 87.93(12) 2_655 . ? N005 Na01 Na01 116.24(14) . 7_666 ? N005 Na01 Na01 46.55(11) . 2_655 ? N005 Na01 O002 119.59(13) . . ? N005 Na01 O002 101.97(15) . 7_666 ? N005 Na01 O003 165.34(15) . . ? N005 Na01 N004 73.79(13) . 2_655 ? N005 Na01 N004 73.58(13) . . ? Na01 O002 Na01 104.59(10) . 7_666 ? C00E O002 Na01 102.4(2) . . ? C00E O002 Na01 121.3(2) . 7_666 ? C00I O002 Na01 100.1(3) . 7_666 ? C00I O002 Na01 117.7(2) . . ? C00I O002 C00E 111.5(4) . . ? C00F O003 Na01 112.8(3) . . ? C00G O003 Na01 130.7(3) . . ? C00G O003 C00F 110.7(4) . . ? Na01 N004 Na01 84.79(11) 2_655 . ? C006 N004 Na01 108.9(3) . . ? C006 N004 Na01 109.3(3) . 2_655 ? C008 N004 Na01 112.7(3) . 2_655 ? C008 N004 Na01 115.0(3) . . ? C008 N004 C006 120.5(4) . . ? Na01 N005 Na01 86.9(2) . 2_655 ? C007 N005 Na01 110.4(2) . 2_655 ? C007 N005 Na01 110.4(2) 2_655 . ? C007 N005 Na01 111.7(2) 2_655 2_655 ? C007 N005 Na01 111.7(2) . . ? C007 N005 C007 120.7(6) 2_655 . ? N004 C006 C009 123.7(4) . . ? N004 C006 C00D 114.9(5) . . ? C009 C006 C00D 121.3(5) . . ? N005 C007 C009 120.9(5) . . ? N005 C007 C00A 119.4(4) . . ? C00A C007 C009 119.6(4) . . ? N004 C008 C00C 125.9(5) . . ? C006 C009 C007 129.4(4) . . ? C006 C009 C00J 115.3(4) . . ? C007 C009 C00J 115.3(5) . . ? C00B C00A C007 119.9(5) . . ? C00A C00B C00A 120.6(8) . 2_655 ? C008 C00C C00H 115.1(6) . . ? C00H C00D C006 122.1(5) . . ? O002 C00E C00F 110.3(4) . . ? O003 C00F C00E 111.1(4) . . ? C00D C00H C00C 121.5(4) . . ? 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 Na01 Na01 4.024(3) 7_666 ? Na01 Na01 3.301(2) 2_655 ? Na01 O002 2.558(3) 7_666 ? Na01 O002 2.528(3) . ? Na01 O003 2.448(5) . ? Na01 N004 2.454(3) . ? Na01 N004 2.442(3) 2_655 ? Na01 N005 2.400(5) . ? O002 C00E 1.437(7) . ? O002 C00I 1.428(6) . ? O003 C00F 1.431(4) . ? O003 C00G 1.401(7) . ? N004 C006 1.391(6) . ? N004 C008 1.325(7) . ? N005 C007 1.384(5) 2_655 ? N005 C007 1.384(5) . ? C006 C009 1.393(8) . ? C006 C00D 1.445(6) . ? C007 C009 1.448(6) . ? C007 C00A 1.413(8) . ? C008 C00C 1.374(6) . ? C009 C00J 1.517(7) . ? C00A C00B 1.380(7) . ? C00C C00H 1.390(9) . ? C00D C00H 1.341(10) . ? C00E C00F 1.478(8) . ?