#------------------------------------------------------------------------------ #$Date: 2014-03-15 13:45:36 +0200 (Sat, 15 Mar 2014) $ #$Revision: 106525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/18/7101894.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_7101894 loop_ _publ_author_name 'Yue, Yan-Feng' 'Wang, Bing-Wu' 'Gao, En-Qing' 'Fang, Chen-Jie' 'He, Cheng' 'Yan, Chun-Hua' _publ_section_title ; A novel three-dimensional heterometallic compound: templated assembly of the unprecedented planar "Na within [Cu4]" metalloporphyrin-like subunits. ; _journal_issue 20 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 2034 _journal_page_last 2036 _journal_year 2007 _chemical_formula_sum 'C16 H14 Cu4 N12 Na4 O23' _chemical_formula_weight 1088.52 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.6544(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.75580(10) _cell_length_b 16.6604(3) _cell_length_c 21.5919(4) _cell_measurement_reflns_used 30019 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 3.395 _cell_volume 3105.11(9) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0.76 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 29968 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.50 _exptl_absorpt_coefficient_mu 2.880 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_crystal_colour Deep-Bule _exptl_crystal_density_diffrn 2.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Rhombic _exptl_crystal_F_000 2152 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.912 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.127 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_matrix_type full _refine_ls_number_parameters 270 _refine_ls_number_reflns 3570 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.996 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0347 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.1054 _reflns_number_gt 2040 _reflns_number_total 3570 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b618296h.txt _[local]_cod_data_source_block 1 _[local]_cod_cif_authors_sg_H-M C2/c 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' loop_ _symmetry_equiv_pos_as_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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Cu1 Cu 0.43908(5) 0.07243(2) -0.10679(2) 0.01390(14) Uani 1 1 d . Cu2 Cu 0.42938(5) 0.43157(2) -0.10721(2) 0.01387(14) Uani 1 1 d . Na1 Na 0.2500 0.2500 0.0000 0.0197(5) Uani 1 2 d S Na2 Na 0.2500 0.7500 0.0000 0.0233(5) Uani 1 2 d S Na3 Na -0.00316(18) 0.66129(9) 0.15926(8) 0.0261(4) Uani 1 1 d . C1 C 0.6280(4) 0.1449(2) -0.18329(17) 0.0150(8) Uani 1 1 d . C2 C 0.5637(4) 0.2124(2) -0.14953(17) 0.0142(8) Uani 1 1 d . C3 C 0.5605(4) 0.2950(2) -0.14966(17) 0.0137(8) Uani 1 1 d . C4 C 0.6274(4) 0.3628(2) -0.18084(17) 0.0139(8) Uani 1 1 d . C5 C 0.3659(4) 0.5800(2) -0.05987(18) 0.0144(8) Uani 1 1 d . C6 C 0.2903(4) 0.5207(2) -0.02317(17) 0.0131(8) Uani 1 1 d . C7 C 0.2001(4) 0.5204(2) 0.02386(17) 0.0135(8) Uani 1 1 d . C8 C 0.1323(4) 0.5791(2) 0.06360(18) 0.0145(8) Uani 1 1 d . N1 N 0.4792(3) 0.18868(17) -0.10606(14) 0.0153(7) Uani 1 1 d . N2 N 0.4252(3) 0.25213(15) -0.07923(14) 0.0138(6) Uani 1 1 d . N3 N 0.4734(3) 0.31612(17) -0.10655(14) 0.0148(7) Uani 1 1 d . N4 N 0.3099(3) 0.44305(17) -0.03762(14) 0.0134(7) Uani 1 1 d . N5 N 0.2392(3) 0.39546(17) -0.00245(14) 0.0139(6) Uani 1 1 d . N6 N 0.1725(3) 0.44177(17) 0.03511(14) 0.0134(7) Uani 1 1 d . O1 O 0.5834(3) 0.07530(13) -0.16803(12) 0.0156(6) Uani 1 1 d . OW1 O 0.2156(3) 0.08458(15) -0.17553(12) 0.0209(6) Uani 1 1 d . O2 O 0.7165(3) 0.15849(15) -0.22097(12) 0.0226(6) Uani 1 1 d . OW2 O 0.2082(3) 0.42672(13) -0.18185(12) 0.0179(6) Uani 1 1 d . O3 O 0.7276(3) 0.35157(15) -0.21426(12) 0.0199(6) Uani 1 1 d . OW3 O 0.0842(3) 0.22128(16) -0.10380(13) 0.0253(7) Uani 1 1 d . O4 O 0.5747(3) 0.43194(13) -0.16762(12) 0.0168(6) Uani 1 1 d . OW4 O 0.0000 0.7442(2) 0.2500 0.0351(10) Uani 1 2 d S O5 O 0.4404(3) 0.54881(14) -0.09971(11) 0.0161(6) Uani 1 1 d . O6 O 0.3531(3) 0.65310(13) -0.05125(12) 0.0186(6) Uani 1 1 d . O7 O 0.1453(3) 0.65200(13) 0.05747(11) 0.0171(6) Uani 1 1 d . O8 O 0.0570(3) 0.54566(14) 0.10305(11) 0.0155(6) Uani 1 1 d . 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 Cu1 0.0176(3) 0.0088(2) 0.0173(3) 0.00044(19) 0.0089(2) 0.00017(18) Cu2 0.0171(3) 0.0090(2) 0.0175(3) -0.00057(19) 0.0089(2) -0.00013(18) Na1 0.0265(11) 0.0108(10) 0.0251(11) -0.0004(10) 0.0141(9) -0.0003(9) Na2 0.0325(12) 0.0123(10) 0.0288(12) 0.0001(10) 0.0159(10) 0.0012(10) Na3 0.0278(9) 0.0201(8) 0.0317(9) -0.0008(7) 0.0092(7) 0.0017(7) C1 0.016(2) 0.0163(19) 0.013(2) -0.0016(17) 0.0047(16) -0.0012(16) C2 0.0158(19) 0.0121(17) 0.016(2) 0.0013(17) 0.0059(16) 0.0014(16) C3 0.017(2) 0.0105(18) 0.014(2) -0.0004(16) 0.0055(16) 0.0001(16) C4 0.018(2) 0.0085(18) 0.015(2) -0.0007(15) 0.0030(16) -0.0016(15) C5 0.0133(18) 0.0146(19) 0.015(2) 0.0004(16) 0.0024(16) -0.0009(15) C6 0.0137(18) 0.0092(17) 0.016(2) -0.0009(15) 0.0021(16) 0.0003(15) C7 0.0159(18) 0.0113(18) 0.013(2) -0.0012(15) 0.0030(16) -0.0017(15) C8 0.0101(18) 0.017(2) 0.017(2) -0.0019(16) 0.0037(15) 0.0026(15) N1 0.0180(16) 0.0131(16) 0.0171(19) -0.0004(13) 0.0094(14) -0.0009(13) N2 0.0175(15) 0.0056(13) 0.0196(16) -0.0004(15) 0.0067(12) -0.0005(14) N3 0.0167(16) 0.0113(16) 0.0181(19) -0.0017(13) 0.0081(14) -0.0010(13) N4 0.0144(16) 0.0102(15) 0.0169(19) -0.0012(13) 0.0064(13) 0.0013(12) N5 0.0181(16) 0.0094(14) 0.0161(16) -0.0002(14) 0.0081(13) 0.0008(13) N6 0.0151(16) 0.0112(15) 0.0151(18) 0.0002(13) 0.0055(13) 0.0010(12) O1 0.0211(14) 0.0087(13) 0.0197(16) -0.0007(10) 0.0118(12) 0.0001(10) OW1 0.0206(14) 0.0237(14) 0.0185(16) 0.0020(12) 0.0040(12) -0.0003(12) O2 0.0307(16) 0.0154(14) 0.0258(16) -0.0036(12) 0.0167(13) -0.0018(12) OW2 0.0186(14) 0.0176(14) 0.0182(15) -0.0032(11) 0.0054(11) 0.0006(11) O3 0.0234(14) 0.0184(14) 0.0216(16) 0.0018(12) 0.0140(12) 0.0031(11) OW3 0.0258(16) 0.0247(14) 0.0263(16) 0.0070(13) 0.0070(13) -0.0008(12) O4 0.0207(14) 0.0116(13) 0.0205(16) 0.0008(11) 0.0108(12) 0.0010(11) OW4 0.056(3) 0.027(2) 0.022(2) 0.000 0.007(2) 0.000 O5 0.0204(15) 0.0100(12) 0.0206(17) -0.0025(11) 0.0115(12) -0.0006(10) O6 0.0243(15) 0.0085(13) 0.0261(16) -0.0005(12) 0.0133(12) 0.0005(11) O7 0.0245(14) 0.0077(13) 0.0208(15) 0.0006(11) 0.0093(12) -0.0021(11) O8 0.0181(14) 0.0123(12) 0.0184(16) -0.0005(11) 0.0096(12) 0.0011(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 N1 1.968(3) . Cu1 O8 1.969(2) 7 Cu1 O1 1.977(2) . Cu1 N6 1.978(3) 7 Cu1 OW1 2.258(3) . Cu2 O5 1.961(2) . Cu2 N3 1.961(3) . Cu2 O4 1.969(2) . Cu2 N4 1.979(3) . Cu2 OW2 2.304(3) . Na1 N5 2.426(3) . Na1 N5 2.426(3) 7 Na1 N2 2.482(3) . Na1 N2 2.482(3) 7 Na1 OW3 2.504(3) . Na1 OW3 2.504(3) 7 Na1 Na3 4.0234(16) 5_565 Na1 Na3 4.0234(16) 3_545 Na2 O6 2.232(2) 7_565 Na2 O6 2.232(2) . Na2 O7 2.330(2) 7_565 Na2 O7 2.330(2) . Na3 OW3 2.341(3) 5_565 Na3 O8 2.383(3) . Na3 OW4 2.394(3) . Na3 OW2 2.430(3) 5_565 Na3 O3 2.513(3) 5_665 Na3 O7 2.739(3) . Na3 C8 2.893(4) . Na3 Na3 3.909(3) 2 Na3 Na1 4.0234(16) 3_455 C1 O2 1.235(4) . C1 O1 1.284(4) . C1 C2 1.500(5) . C2 N1 1.349(4) . C2 C3 1.376(5) . C3 N3 1.345(4) . C3 C4 1.485(5) . C4 O3 1.241(4) . C4 O4 1.290(4) . C5 O6 1.240(4) . C5 O5 1.274(4) . C5 C6 1.489(5) . C6 N4 1.348(4) . C6 C7 1.387(5) . C7 N6 1.360(4) . C7 C8 1.489(5) . C8 O7 1.230(4) . C8 O8 1.287(4) . N1 N2 1.330(4) . N2 N3 1.321(4) . N4 N5 1.321(4) . N5 N6 1.324(4) . N6 Cu1 1.978(3) 7 OW2 Na3 2.430(3) 5_565 O3 Na3 2.513(3) 5_665 OW3 Na3 2.341(3) 5_565 OW4 Na3 2.394(3) 2 O8 Cu1 1.969(2) 7 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 N1 Cu1 O8 168.86(11) . 7 N1 Cu1 O1 81.28(10) . . O8 Cu1 O1 92.46(9) 7 . N1 Cu1 N6 102.85(12) . 7 O8 Cu1 N6 81.71(10) 7 7 O1 Cu1 N6 168.88(11) . 7 N1 Cu1 OW1 92.91(11) . . O8 Cu1 OW1 97.10(9) 7 . O1 Cu1 OW1 97.98(10) . . N6 Cu1 OW1 92.15(11) 7 . O5 Cu2 N3 165.78(11) . . O5 Cu2 O4 91.34(9) . . N3 Cu2 O4 81.94(10) . . O5 Cu2 N4 82.30(10) . . N3 Cu2 N4 102.56(12) . . O4 Cu2 N4 170.19(11) . . O5 Cu2 OW2 96.70(9) . . N3 Cu2 OW2 96.42(11) . . O4 Cu2 OW2 95.59(10) . . N4 Cu2 OW2 92.59(10) . . N5 Na1 N5 180.0 . 7 N5 Na1 N2 89.82(9) . . N5 Na1 N2 90.18(9) 7 . N5 Na1 N2 90.18(9) . 7 N5 Na1 N2 89.82(9) 7 7 N2 Na1 N2 180.0 . 7 N5 Na1 OW3 99.02(9) . . N5 Na1 OW3 80.98(9) 7 . N2 Na1 OW3 73.65(9) . . N2 Na1 OW3 106.35(9) 7 . N5 Na1 OW3 80.98(9) . 7 N5 Na1 OW3 99.02(9) 7 7 N2 Na1 OW3 106.35(9) . 7 N2 Na1 OW3 73.65(9) 7 7 OW3 Na1 OW3 180.00(8) . 7 N5 Na1 Na3 66.48(7) . 5_565 N5 Na1 Na3 113.52(8) 7 5_565 N2 Na1 Na3 73.21(7) . 5_565 N2 Na1 Na3 106.79(7) 7 5_565 OW3 Na1 Na3 32.58(6) . 5_565 OW3 Na1 Na3 147.42(6) 7 5_565 N5 Na1 Na3 113.52(7) . 3_545 N5 Na1 Na3 66.48(8) 7 3_545 N2 Na1 Na3 106.79(7) . 3_545 N2 Na1 Na3 73.21(7) 7 3_545 OW3 Na1 Na3 147.42(6) . 3_545 OW3 Na1 Na3 32.58(6) 7 3_545 Na3 Na1 Na3 180.00(6) 5_565 3_545 O6 Na2 O6 180.00(11) 7_565 . O6 Na2 O7 89.14(8) 7_565 7_565 O6 Na2 O7 90.86(8) . 7_565 O6 Na2 O7 90.86(8) 7_565 . O6 Na2 O7 89.14(8) . . O7 Na2 O7 180.00(10) 7_565 . OW3 Na3 O8 119.28(11) 5_565 . OW3 Na3 OW4 84.10(10) 5_565 . O8 Na3 OW4 155.57(11) . . OW3 Na3 OW2 115.87(11) 5_565 5_565 O8 Na3 OW2 81.28(9) . 5_565 OW4 Na3 OW2 95.25(9) . 5_565 OW3 Na3 O3 119.84(10) 5_565 5_665 O8 Na3 O3 83.97(9) . 5_665 OW4 Na3 O3 77.53(8) . 5_665 OW2 Na3 O3 122.46(10) 5_565 5_665 OW3 Na3 O7 77.33(9) 5_565 . O8 Na3 O7 50.97(8) . . OW4 Na3 O7 138.37(9) . . OW2 Na3 O7 126.37(10) 5_565 . O3 Na3 O7 80.04(9) 5_665 . OW3 Na3 C8 98.96(11) 5_565 . O8 Na3 C8 26.01(9) . . OW4 Na3 C8 155.20(10) . . OW2 Na3 C8 105.23(10) 5_565 . O3 Na3 C8 79.69(10) 5_665 . O7 Na3 C8 25.03(8) . . OW3 Na3 Na3 117.70(8) 5_565 2 O8 Na3 Na3 122.92(7) . 2 OW4 Na3 Na3 35.25(8) . 2 OW2 Na3 Na3 71.67(7) 5_565 2 O3 Na3 Na3 71.05(7) 5_665 2 O7 Na3 Na3 151.09(9) . 2 C8 Na3 Na3 140.98(9) . 2 OW3 Na3 Na1 35.17(7) 5_565 3_455 O8 Na3 Na1 89.69(8) . 3_455 OW4 Na3 Na1 114.73(7) . 3_455 OW2 Na3 Na1 94.83(8) 5_565 3_455 O3 Na3 Na1 140.42(8) 5_665 3_455 O7 Na3 Na1 66.06(6) . 3_455 C8 Na3 Na1 77.85(8) . 3_455 Na3 Na3 Na1 140.53(5) 2 3_455 O2 C1 O1 125.9(3) . . O2 C1 C2 120.7(3) . . O1 C1 C2 113.4(3) . . N1 C2 C3 106.3(3) . . N1 C2 C1 114.4(3) . . C3 C2 C1 139.3(3) . . N3 C3 C2 105.9(3) . . N3 C3 C4 115.3(3) . . C2 C3 C4 138.8(3) . . O3 C4 O4 125.3(3) . . O3 C4 C3 121.3(3) . . O4 C4 C3 113.3(3) . . O6 C5 O5 124.8(3) . . O6 C5 C6 120.8(3) . . O5 C5 C6 114.4(3) . . N4 C6 C7 106.0(3) . . N4 C6 C5 115.3(3) . . C7 C6 C5 138.6(3) . . N6 C7 C6 105.9(3) . . N6 C7 C8 115.4(3) . . C6 C7 C8 138.6(3) . . O7 C8 O8 124.5(3) . . O7 C8 C7 122.3(3) . . O8 C8 C7 113.3(3) . . O7 C8 Na3 70.48(19) . . O8 C8 Na3 54.26(17) . . C7 C8 Na3 166.8(3) . . N2 N1 C2 110.3(3) . . N2 N1 Cu1 135.2(2) . . C2 N1 Cu1 113.7(2) . . N3 N2 N1 106.5(3) . . N3 N2 Na1 126.8(2) . . N1 N2 Na1 126.5(2) . . N2 N3 C3 111.0(3) . . N2 N3 Cu2 135.9(2) . . C3 N3 Cu2 112.6(2) . . N5 N4 C6 110.6(3) . . N5 N4 Cu2 137.4(2) . . C6 N4 Cu2 111.9(2) . . N4 N5 N6 107.4(3) . . N4 N5 Na1 126.3(2) . . N6 N5 Na1 126.0(2) . . N5 N6 C7 110.0(3) . . N5 N6 Cu1 137.4(2) . 7 C7 N6 Cu1 112.4(2) . 7 C1 O1 Cu1 116.7(2) . . Cu2 OW2 Na3 116.32(11) . 5_565 C4 O3 Na3 117.1(2) . 5_665 Na3 OW3 Na1 112.25(11) 5_565 . C4 O4 Cu2 116.0(2) . . Na3 OW4 Na3 109.49(15) . 2 C5 O5 Cu2 116.0(2) . . C5 O6 Na2 147.1(2) . . C8 O7 Na2 143.3(2) . . C8 O7 Na3 84.5(2) . . Na2 O7 Na3 132.05(10) . . C8 O8 Cu1 116.9(2) . 7 C8 O8 Na3 99.7(2) . . Cu1 O8 Na3 142.26(12) 7 . _cod_database_code 7101894 _journal_paper_doi 10.1039/c1cc11296a