# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 182/1079 data_ARDO _audit_creation_date 1998-09-04 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 1998-09-09 _audit_conform_dict_name 'cif_core.dic' _audit_conform_dict_version '2.0.1' _publ_requested_journal 'J. C. S. Chem. Commun.' _publ_contact_author_name 'Bernardinelli, G\'erald' _publ_contact_author_address ; Laboratoire de Cristallographie Universit\'e de Gen\`eve 24, quai E. Ansermet CH - 1211 Gen\`eve 4 Switzerland ; _publ_contact_author_email gerald.bernardinelli@cryst.unige.ch _publ_contact_author_phone '(+[41] 22) 702 62 02' _publ_contact_author_fax '(+[41] 22) 781 21 92' _chemical_formula_moiety ; Fe(C11H7N5)2 [Na(H2O)4]0.5 [Na(CH3CN)4(C4H8O)2]0.5 ; _chemical_formula_sum 'C30 H32 N12 O3 Na Fe' _chemical_formula_weight 343.7 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P-421c No 114' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2+x,1/2-y,1/2-z -x,-y,+z 1/2-x,1/2+y,1/2-z 1/2-y,1/2-x,1/2+z -y,+x,-z +y,-x,-z 1/2+y,1/2+x,1/2+z _cell_length_a 13.3185(5) _cell_length_b 13.3185(5) _cell_length_c 19.4550(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3451.0(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_meas 'not measured' _diffrn_radiation_type 'X-ray tube CuK\a' _diffrn_radiation_wavelength 1.54183 _cell_measurement_reflns_used 34 _cell_measurement_theta_min 26.5 _cell_measurement_theta_max 36.5 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu 4.039 _exptl_crystal_description 'prism' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_colour black _diffrn_measurement_device_type Stoe_Stadi-4_4-circle_diffractometer _diffrn_measurement_method \w-1.0_\q_scans _exptl_absorpt_correction_type Analytical_integration _exptl_absorpt_correction_T_min .281061 _exptl_absorpt_correction_T_max .490068 _diffrn_reflns_number 4966 _reflns_number_total 2446 _reflns_number_gt 1661 _reflns_threshold_expression refl_observed_if_F____>_4.00_sigma(F___) _diffrn_reflns_theta_max 54.6 _diffrn_reflns_av_R_equivalents .078 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 2 _diffrn_standards_interval_time 45 _diffrn_standards_decay_% 8 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .051 _refine_ls_wR_factor_ref .046 _refine_ls_goodness_of_fit_ref 1.615 _refine_ls_number_reflns 1661 _refine_ls_number_parameters 250 _refine_ls_weighting_scheme calc _refine_ls_weighting_details '\w=1/[\s^2(Fo)+0.0002(Fo^2)]' _refine_ls_hydrogen_treatment ; THF : Calculated H2O : Observed and refined with restraints on bond lengths Ligand : Observed and refined with restraints on bond lengths and angles ; _refine_ls_shift/su_max .185 _refine_diff_density_max .362 _refine_diff_density_min -.565 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1495(301) _refine_ls_abs_structure_Flack '0.02(2)' _computing_data_collection Stoe_Stadi-4 _computing_cell_refinement 'xtal_latcon' _computing_structure_solution 'Multan 87' _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics 'xtal_GX3_ORTEP' _computing_publication_material xtal_BONDLA_CIFIO loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .017 .009 H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0 N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .029 .018 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .047 .032 Fe Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 -1.179 3.204 Na Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .129 .124 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Fe .50000 .00000 .74570(10) .0295(12) 1.00000 Uani Na1 .50000 .50000 .00000 .038(3) 1.00000 Uani Na2 .50000 .50000 .50000 .073(5) 1.00000 Uani N1 .5841(5) .1168(5) .7505(4) .028(4) 1.00000 Uani N2 .5963(6) -.0362(5) .6755(4) .029(5) 1.00000 Uani N3 .7395(5) .0073(7) .6198(4) .042(5) 1.00000 Uani N4 .4268(6) .0718(6) .8162(4) .032(5) 1.00000 Uani N5 .4258(7) .2045(6) .8879(5) .047(6) 1.00000 Uani C1 .6686(7) .1184(7) .7115(5) .035(6) 1.00000 Uani C2 .7312(8) .1995(8) .7185(5) .042(7) 1.00000 Uani C3 .7111(9) .2733(8) .7647(7) .055(8) 1.00000 Uani C4 .6262(8) .2686(7) .8059(5) .049(7) 1.00000 Uani C5 .5616(7) .1874(8) .7984(5) .038(7) 1.00000 Uani C6 .6713(7) .0313(7) .6684(5) .031(6) 1.00000 Uani C7 .6158(8) -.1083(8) .6270(5) .039(7) 1.00000 Uani C8 .7022(8) -.0812(7) .5939(5) .040(7) 1.00000 Uani C9 .4712(7) .1603(8) .8353(6) .038(7) 1.00000 Uani C10 .3474(8) .0607(8) .8582(5) .041(7) 1.00000 Uani C11 .3455(8) .1424(8) .9021(5) .047(7) 1.00000 Uani O1a .50000 .50000 .6221(6) .106(10) 1.00000 Uani C1a .4533(14) .4289(14) .6646(10) .150(16) 1.00000 Uani C2a .4545(10) .4645(15) .7338(7) .115(14) 1.00000 Uani N1b .4353(8) .6798(8) .5012(8) .099(9) 1.00000 Uani C1b .4099(10) .7570(10) .4984(8) .089(10) 1.00000 Uani C2b .3767(10) .8595(9) .4944(7) .101(11) 1.00000 Uani O1c .6013(7) .6069(6) -.0539(5) .097(7) 1.00000 Uani H2 .798(3) .204(3) .6891(15) .05000 1.00000 Uiso H3 .759(4) .335(3) .7695(17) .05000 1.00000 Uiso H4 .612(3) .322(3) .8395(19) .05000 1.00000 Uiso H7 .573(3) -.172(3) .6180(12) .05000 1.00000 Uiso H8 .734(3) -.119(3) .5564(18) .05000 1.00000 Uiso H10 .296(3) -.002(3) .8572(13) .05000 1.00000 Uiso H11 .289(3) .155(2) .9424(17) .05000 1.00000 Uiso H1a1 .37812 .41602 .65057 .05000 1.00000 Uiso H1a2 .49736 .35909 .66429 .05000 1.00000 Uiso H2a1 .38619 .50478 .74751 .05000 1.00000 Uiso H2a2 .46590 .40367 .77203 .05000 1.00000 Uiso H2b1 .359(4) .877(3) .444(3) .05000 1.00000 Uiso H2b2 .311(4) .868(3) .525(3) .05000 1.00000 Uiso H2b3 .432(4) .906(3) .511(3) .05000 1.00000 Uiso H1c1 .585(6) .680(4) -.078(4) .05000 1.00000 Uiso H1c2 .668(5) .577(6) -.074(4) .05000 1.00000 Uiso 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 Fe .0300(14) .0307(14) .0278(10) -.0031(11) .00000 .00000 Na1 .036(3) .036(3) .041(4) .00000 .00000 .00000 Na2 .072(5) .072(5) .075(6) .00000 .00000 .00000 N1 .025(4) .033(4) .025(4) -.004(4) -.007(5) .002(5) N2 .024(5) .026(5) .036(5) -.007(4) -.002(5) -.003(4) N3 .034(5) .052(6) .040(5) -.000(5) .004(4) .013(6) N4 .031(6) .023(5) .043(5) .003(4) .002(5) -.001(4) N5 .057(6) .048(6) .035(6) .007(6) .010(5) -.005(5) C1 .030(6) .048(6) .028(6) -.005(6) -.008(5) .010(5) C2 .044(7) .043(7) .041(7) -.019(6) .003(6) -.007(6) C3 .055(7) .046(8) .064(9) -.030(6) -.003(7) .008(7) C4 .071(8) .041(7) .036(7) -.005(7) -.005(6) .004(6) C5 .032(7) .039(6) .044(7) -.001(6) -.006(6) -.001(6) C6 .026(6) .042(7) .026(6) .007(6) .005(5) .006(5) C7 .044(7) .034(7) .038(6) .006(5) -.004(6) .000(6) C8 .052(7) .032(6) .038(6) .014(6) .002(6) -.005(6) C9 .041(8) .038(7) .036(7) .009(6) -.012(6) .000(6) C10 .030(7) .053(8) .041(7) .017(6) .002(6) -.003(6) C11 .055(8) .052(8) .034(6) .002(6) .011(6) -.006(6) O1a .166(14) .084(10) .068(8) -.050(12) .00000 .00000 C1a .187(19) .162(17) .099(12) -.075(14) -.013(15) .021(14) C2a .067(9) .18(3) .098(11) -.011(8) .018(9) .020(13) N1b .109(9) .072(7) .114(10) .036(7) .006(9) .028(9) C1b .096(10) .093(10) .077(10) .047(9) .027(9) .021(12) C2b .132(14) .107(12) .064(9) .031(9) .042(11) .008(10) O1c .095(7) .063(6) .133(8) .036(5) .082(7) .055(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance Fe N1 . . 1.920(6) Fe N2 . . 1.935(8) Fe N4 . . 1.935(8) Fe N1 . 3_655 1.920(6) Fe N2 . 3_655 1.935(8) Fe N4 . 3_655 1.935(8) Na1 O1c . . 2.224(9) Na1 O1c . 3_665 2.224(9) Na1 O1c . 6_655 2.224(9) Na1 O1c . 7_565 2.224(9) Na2 O1a . . 2.375(11) Na2 O1a . 6_656 2.375(11) N1 C1 . . 1.357(11) N1 C5 . . 1.358(12) N2 C6 . . 1.351(11) N2 C7 . . 1.371(12) N3 C6 . . 1.350(12) N3 C8 . . 1.374(13) N4 C9 . . 1.371(12) N4 C10 . . 1.345(12) N5 C9 . . 1.328(13) N5 C11 . . 1.380(13) C1 C2 . . 1.372(13) C1 C6 . . 1.431(13) C2 C3 . . 1.358(15) C2 H2 . . 1.06(4) C3 C4 . . 1.387(16) C3 H3 . . 1.04(4) C4 C5 . . 1.389(14) C4 H4 . . .99(4) C5 C9 . . 1.447(13) C7 C8 . . 1.367(14) C7 H7 . . 1.03(4) C8 H8 . . .98(4) C10 C11 . . 1.383(14) C10 H10 . . 1.08(4) C11 H11 . . 1.10(4) O1a C1a . . 1.40(2) O1a C1a . 3_665 1.40(2) C1a C2a . . 1.43(3) C1a H1a1 . . 1.052(18) C1a H1a2 . . 1.100(18) C2a H2a1 . . 1.089(15) C2a H2a2 . . 1.110(17) C2a C2a . 3_665 1.54(3) N1b C1b . . 1.084(17) C1b C2b . . 1.437(18) C2b H2b1 . . 1.03(5) C2b H2b2 . . 1.07(6) C2b H2b3 . . 1.01(5) O1c H1c1 . . 1.10(6) O1c H1c2 . . 1.05(7) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle N1 Fe N2 . . . 81.3(3) N1 Fe N4 . . . 81.9(3) N1 Fe N1 . . 3_655 174.5(4) N1 Fe N2 . . 3_655 102.7(3) N1 Fe N4 . . 3_655 94.1(3) N2 Fe N4 . . . 163.2(3) N2 Fe N1 . . 3_655 102.7(3) N2 Fe N2 . . 3_655 90.2(4) N2 Fe N4 . . 3_655 92.5(4) N4 Fe N1 . . 3_655 94.1(3) N4 Fe N2 . . 3_655 92.5(4) N4 Fe N4 . . 3_655 89.7(4) N1 Fe N2 3_655 . 3_655 81.3(3) N1 Fe N4 3_655 . 3_655 81.9(3) N2 Fe N4 3_655 . 3_655 163.2(3) O1c Na1 O1c . . 3_665 123.8(4) O1c Na1 O1c . . 6_655 102.8(3) O1c Na1 O1c . . 7_565 102.8(3) O1c Na1 O1c 3_665 . 6_655 102.8(3) O1c Na1 O1c 3_665 . 7_565 102.8(3) O1c Na1 O1c 6_655 . 7_565 123.8(4) O1a Na2 O1a . . 6_656 180.0000 Fe N1 C1 . . . 118.0(6) Fe N1 C5 . . . 117.8(6) C1 N1 C5 . . . 123.8(7) Fe N2 C6 . . . 113.3(6) Fe N2 C7 . . . 141.8(7) C6 N2 C7 . . . 104.9(8) C6 N3 C8 . . . 102.5(8) Fe N4 C9 . . . 113.5(6) Fe N4 C10 . . . 140.6(7) C9 N4 C10 . . . 105.6(8) C9 N5 C11 . . . 104.0(8) N1 C1 C2 . . . 117.4(8) N1 C1 C6 . . . 109.7(8) C2 C1 C6 . . . 133.0(9) C1 C2 C3 . . . 121.1(10) C1 C2 H2 . . . 120(3) C3 C2 H2 . . . 118(3) C2 C3 C4 . . . 120.7(10) C2 C3 H3 . . . 120(3) C4 C3 H3 . . . 119(3) C3 C4 C5 . . . 118.6(9) C3 C4 H4 . . . 121(3) C5 C4 H4 . . . 121(3) N1 C5 C4 . . . 118.3(8) N1 C5 C9 . . . 110.5(8) C4 C5 C9 . . . 131.1(9) N2 C6 N3 . . . 114.2(8) N2 C6 C1 . . . 117.4(8) N3 C6 C1 . . . 128.3(8) N2 C7 C8 . . . 107.4(9) N2 C7 H7 . . . 125.9(18) C8 C7 H7 . . . 126.7(19) N3 C8 C7 . . . 111.0(8) N3 C8 H8 . . . 124(2) C7 C8 H8 . . . 125(2) N4 C9 N5 . . . 113.2(9) N4 C9 C5 . . . 116.1(9) N5 C9 C5 . . . 130.6(9) N4 C10 C11 . . . 107.7(9) N4 C10 H10 . . . 125.0(19) C11 C10 H10 . . . 127.4(19) N5 C11 C10 . . . 109.5(9) N5 C11 H11 . . . 125.9(18) C10 C11 H11 . . . 124.6(18) Na2 O1a C1a . . . 126.2(9) Na2 O1a C1a . . 3_665 126.2(9) C1a O1a C1a . . 3_665 107.7(13) O1a C1a C2a . . . 109.1(15) O1a C1a H1a1 . . . 112.3(15) O1a C1a H1a2 . . . 109.3(14) C2a C1a H1a1 . . . 108.1(15) C2a C1a H1a2 . . . 106.2(16) H1a1 C1a H1a2 . . . 111.6(16) C1a C2a H2a1 . . . 112.6(13) C1a C2a H2a2 . . . 113.1(16) C1a C2a C2a . . 3_665 102.3(12) H2a1 C2a H2a2 . . . 108.1(12) H2a1 C2a C2a . . 3_665 110.8(16) H2a2 C2a C2a . . 3_665 109.9(11) N1b C1b C2b . . . 179.7(16) C1b C2b H2b1 . . . 110(3) C1b C2b H2b2 . . . 109(3) C1b C2b H2b3 . . . 110(3) H2b1 C2b H2b2 . . . 109(4) H2b1 C2b H2b3 . . . 110(4) H2b2 C2b H2b3 . . . 110(4) Na1 O1c H1c1 . . . 130(4) Na1 O1c H1c2 . . . 117(5) H1c1 O1c H1c2 . . . 110(6) #END-------------------------------------------------------------------