# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vladimir Chernyshev' _publ_contact_author_email VLADIMIR@STRUCT.CHEM.MSU.RU _publ_section_title ; Ni(II), Co(II), Cu(II), Zn(II) and Na(I) complexes of a hybrid ligand 4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine ; loop_ _publ_author_name 'Vladimir Chernyshev' 'Vladimir E. Baulin' 'Irina S. Ivanova' 'Nadezhda M. Logacheva' 'Elena N. Pyatova' ; A.Yu.Tsivadze ; 'Yurii A. Velikodny' # Attachment 'new_cif.cif' # # Title: "Ni(II), Co(II), Cu(II), Zn(II) and Na(I) complexes of a hybrid # ligand 4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine" # Authors: Logacheva, Nadezhda; Baulin, Vladimir; Tsivadze, Aslan; Pyatova, # Elena; Ivanova, Irina; Velikodny, Yurii; Chernyshev, Vladimir # Manuscript ID: B819805E. # 7 Crystal structures (compounds 1-6 and 11), #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 692435' # start Validation Reply Form _vrf_PLAT341_1 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang ... 84 RESPONSE: This is a powder diffraction study. All structural parameters were refined with the laboratory powder diffraction data. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine]nickel(II) bis(hexafluorophosphate) ethanol disolvate monohydrate ; _chemical_name_common ; Bis(4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''- terpyridine)nickel(ii) bis(hexafluorophosphate) ethanol disolvate monohydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Ni N6 O12, 2(P F6), 2(C2 H6 O), H2 O' _chemical_formula_sum 'C64 H76 F12 N6 Ni O15 P2' _chemical_formula_weight 1517.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.801(2) _cell_length_b 20.582(2) _cell_length_c 25.813(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6801.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2072 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 39.99 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 1 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; ? ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology 'no specific habit' _pd_char_colour 'light brown' # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia ; _diffrn_ambient_temperature 295(2) _diffrn_source 'Fine focus X-ray tube' _diffrn_source_target Cu _diffrn_radiation_source 'line-focus sealed tube' _diffrn_radiation_monochromator 'Curved Germanium (111)' _diffrn_measurement_device 'Guinier camera G670' _diffrn_detector_type 'Imaging Plate' _diffrn_reflns_number ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_type CuK\a~1~ _diffrn_radiation_wavelength 1.5406 # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7501 _pd_meas_2theta_range_min 5.00 _pd_meas_2theta_range_max 80.00 _pd_meas_2theta_range_inc 0.01 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'local program' _computing_cell_refinement 'MRIA (Zlokazov & Chernyshev, 1992)' _computing_data_reduction 'local program' _computing_structure_solution MRIA _computing_structure_refinement MRIA _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ; MRIA, SHELXL97 (Sheldrick, 1997) ; #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function 'split-type pseudo-Voigt (Toraya, 1986)' _pd_proc_ls_pref_orient_corr ; March-Dollase (Dollase, 1986); direction of preferred orientation - 010, texture parameter r=0.87(1). ; _pd_proc_ls_background_function 'Chebyshev polynomial up to the 5th order' _pd_proc_ls_prof_R_factor 0.0165 _pd_proc_ls_prof_wR_factor 0.0219 _pd_proc_ls_prof_wR_expected 0.0121 _refine_special_details ; ? ; _refine_ls_R_I_factor ? _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 191 _refine_ls_number_restraints 202 _refine_ls_number_constraints 55 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.8083 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .005 _refine_ls_shift/su_mean .002 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.00 _pd_proc_2theta_range_max 80.00 _pd_proc_2theta_range_inc 0.01 _pd_proc_wavelength 1.5406 # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.7500 0.2500 0.4260(23) 0.043(7) Uiso 1 2 d S . . O1 O 1.1723(23) 0.1157(22) 0.4228(22) 0.067(6) Uiso 1 1 d . . . O2 O 1.4383(21) -0.0626(20) 0.3315(25) 0.067(6) Uiso 1 1 d . . . O3 O 1.3937(23) -0.1898(21) 0.3365(23) 0.067(6) Uiso 1 1 d . . . O4 O 1.4846(24) -0.2460(21) 0.4162(21) 0.067(6) Uiso 1 1 d . . . O5 O 1.6316(22) -0.1545(18) 0.4528(24) 0.067(6) Uiso 1 1 d . . . O6 O 1.5893(22) -0.0480(22) 0.3949(25) 0.067(6) Uiso 1 1 d . . . N1 N 0.8242(23) 0.3051(20) 0.3682(22) 0.067(6) Uiso 1 1 d . . . N2 N 0.8906(24) 0.2098(21) 0.4238(24) 0.067(6) Uiso 1 1 d . . . N3 N 0.7363(20) 0.1784(22) 0.4820(25) 0.067(6) Uiso 1 1 d . . . C1 C 0.7933(27) 0.3576(29) 0.3407(29) 0.067(6) Uiso 1 1 d . . . H1 H 0.7288 0.3750 0.3498 0.080 Uiso 1 1 calc . . . C2 C 0.8451(29) 0.3890(25) 0.3006(28) 0.067(6) Uiso 1 1 d . . . H2 H 0.8143 0.4223 0.2816 0.080 Uiso 1 1 calc . . . C3 C 0.9466(26) 0.3673(30) 0.2907(30) 0.067(6) Uiso 1 1 d . . . H3 H 0.9867 0.3877 0.2655 0.080 Uiso 1 1 calc . . . C4 C 0.9882(28) 0.3152(27) 0.3184(27) 0.067(6) Uiso 1 1 d . . . H4 H 1.0556 0.3003 0.3122 0.080 Uiso 1 1 calc . . . C5 C 0.9243(27) 0.2864(29) 0.3558(29) 0.067(6) Uiso 1 1 d . . . C6 C 0.9614(24) 0.2329(28) 0.3890(28) 0.067(6) Uiso 1 1 d . . . C7 C 1.0581(28) 0.2019(28) 0.3842(31) 0.067(6) Uiso 1 1 d . . . H7 H 1.1059 0.2159 0.3595 0.080 Uiso 1 1 calc . . . C8 C 1.0828(27) 0.1492(25) 0.4170(27) 0.067(6) Uiso 1 1 d . . . C9 C 1.0062(29) 0.1272(29) 0.4523(26) 0.067(6) Uiso 1 1 d . . . H9 H 1.0191 0.0913 0.4732 0.080 Uiso 1 1 calc . . . C10 C 0.9126(30) 0.1594(26) 0.4554(29) 0.067(6) Uiso 1 1 d . . . C11 C 0.8244(27) 0.1426(30) 0.4901(29) 0.067(6) Uiso 1 1 d . . . C12 C 0.8277(26) 0.0900(27) 0.5239(30) 0.067(6) Uiso 1 1 d . . . H12 H 0.8868 0.0638 0.5260 0.080 Uiso 1 1 calc . . . C13 C 0.7411(28) 0.0775(27) 0.5544(28) 0.067(6) Uiso 1 1 d . . . H13 H 0.7410 0.0425 0.5772 0.080 Uiso 1 1 calc . . . C14 C 0.6542(30) 0.1178(26) 0.5507(30) 0.067(6) Uiso 1 1 d . . . H14 H 0.5981 0.1131 0.5733 0.080 Uiso 1 1 calc . . . C15 C 0.6532(26) 0.1651(29) 0.5125(27) 0.067(6) Uiso 1 1 d . . . H15 H 0.5922 0.1889 0.5076 0.080 Uiso 1 1 calc . . . C16 C 1.2650(27) 0.1396(30) 0.3930(25) 0.067(6) Uiso 1 1 d . . . H16A H 1.2447 0.1481 0.3574 0.080 Uiso 1 1 calc . . . H16B H 1.2895 0.1800 0.4080 0.080 Uiso 1 1 calc . . . C17 C 1.3510(29) 0.0908(29) 0.3938(28) 0.067(6) Uiso 1 1 d . . . C18 C 1.3500(27) 0.0376(28) 0.3596(29) 0.067(6) Uiso 1 1 d . . . H18 H 1.2972 0.0339 0.3350 0.080 Uiso 1 1 calc . . . C19 C 1.4280(28) -0.0096(27) 0.3625(27) 0.067(6) Uiso 1 1 d . . . C20 C 1.5168(25) 0.0003(30) 0.3950(30) 0.067(6) Uiso 1 1 d . . . C21 C 1.5122(28) 0.0503(28) 0.4312(28) 0.067(6) Uiso 1 1 d . . . H21 H 1.5615 0.0522 0.4576 0.080 Uiso 1 1 calc . . . C22 C 1.4341(29) 0.0978(29) 0.4283(29) 0.067(6) Uiso 1 1 d . . . H22 H 1.4377 0.1343 0.4495 0.080 Uiso 1 1 calc . . . C23 C 1.3514(31) -0.0871(26) 0.3027(31) 0.067(6) Uiso 1 1 d . . . H23A H 1.3418 -0.0619 0.2713 0.080 Uiso 1 1 calc . . . H23B H 1.2881 -0.0841 0.3232 0.080 Uiso 1 1 calc . . . C24 C 1.3738(27) -0.1575(29) 0.2892(28) 0.067(6) Uiso 1 1 d . . . H24A H 1.3142 -0.1768 0.2718 0.080 Uiso 1 1 calc . . . H24B H 1.4340 -0.1605 0.2665 0.080 Uiso 1 1 calc . . . C25 C 1.4235(24) -0.2559(27) 0.3303(29) 0.067(6) Uiso 1 1 d . . . H25A H 1.4926 -0.2587 0.3151 0.080 Uiso 1 1 calc . . . H25B H 1.3746 -0.2782 0.3078 0.080 Uiso 1 1 calc . . . C26 C 1.4232(28) -0.2865(31) 0.3838(32) 0.067(6) Uiso 1 1 d . . . H26A H 1.3524 -0.2894 0.3970 0.080 Uiso 1 1 calc . . . H26B H 1.4526 -0.3299 0.3824 0.080 Uiso 1 1 calc . . . C27 C 1.5944(26) -0.2566(30) 0.4134(28) 0.067(6) Uiso 1 1 d . . . H27A H 1.6267 -0.2371 0.3832 0.080 Uiso 1 1 calc . . . H27B H 1.6139 -0.3020 0.4165 0.080 Uiso 1 1 calc . . . C28 C 1.6110(29) -0.2192(29) 0.4612(29) 0.067(6) Uiso 1 1 d . . . H28A H 1.5492 -0.2229 0.4827 0.080 Uiso 1 1 calc . . . H28B H 1.6689 -0.2382 0.4801 0.080 Uiso 1 1 calc . . . C29 C 1.7149(25) -0.1127(27) 0.4432(30) 0.067(6) Uiso 1 1 d . . . H29A H 1.7546 -0.1281 0.4136 0.080 Uiso 1 1 calc . . . H29B H 1.7610 -0.1115 0.4730 0.080 Uiso 1 1 calc . . . C30 C 1.6726(27) -0.0449(29) 0.4323(27) 0.067(6) Uiso 1 1 d . . . H30A H 1.6469 -0.0258 0.4642 0.080 Uiso 1 1 calc . . . H30B H 1.7283 -0.0175 0.4192 0.080 Uiso 1 1 calc . . . P1 P 0.9611(18) -0.0112(15) 0.3439(15) 0.057(9) Uiso 1 1 d . . . F11 F 0.8517(19) -0.0046(17) 0.3161(16) 0.128(12) Uiso 1 1 d . . . F12 F 1.0681(21) -0.0211(16) 0.3713(13) 0.128(12) Uiso 1 1 d . . . F13 F 0.9090(19) 0.0039(15) 0.3961(16) 0.128(12) Uiso 1 1 d . . . F14 F 0.9899(20) 0.0607(15) 0.3342(14) 0.128(12) Uiso 1 1 d . . . F15 F 1.0115(18) -0.0288(17) 0.2883(15) 0.128(12) Uiso 1 1 d . . . F16 F 0.9397(21) -0.0868(16) 0.3486(16) 0.128(12) Uiso 1 1 d . . . O7 O 0.2430(23) 0.1755(20) 0.2182(17) 0.106(15) Uiso 1 1 d . . . H71 H 0.2673 0.1871 0.1891 0.159 Uiso 1 1 d . . . C31 C 0.1592(26) 0.1308(26) 0.2137(25) 0.106(15) Uiso 1 1 d . . . H31A H 0.0938 0.1543 0.2163 0.127 Uiso 1 1 calc . . . H31B H 0.1618 0.1108 0.1797 0.127 Uiso 1 1 calc . . . C32 C 0.1612(27) 0.0779(25) 0.2546(23) 0.106(15) Uiso 1 1 d . . . H32A H 0.1029 0.0493 0.2496 0.159 Uiso 1 1 calc . . . H32B H 0.1570 0.0973 0.2884 0.159 Uiso 1 1 calc . . . H32C H 0.2250 0.0537 0.2517 0.159 Uiso 1 1 calc . . . O1W O 0.2500 0.2500 0.3175(19) 0.071(10) Uiso 1 2 d S . . H1W H 0.2231 0.2235 0.2959 0.107 Uiso 1 1 d . . . 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 Ni N1 2.10(6) . ? Ni N2 1.98(3) . ? Ni N3 2.08(6) . ? Ni N1 2.10(6) 2_655 ? Ni N2 1.98(3) 2_655 ? Ni N3 2.08(6) 2_655 ? P1 F14 1.55(4) . ? P1 F15 1.63(5) . ? P1 F16 1.59(5) . ? P1 F13 1.53(4) . ? P1 F11 1.58(5) . ? P1 F12 1.55(5) . ? O1 C8 1.34(5) . ? O1 C16 1.50(7) . ? O2 C23 1.42(6) . ? O2 C19 1.37(8) . ? O3 C25 1.42(9) . ? O3 C24 1.41(8) . ? O4 C26 1.42(7) . ? O4 C27 1.42(5) . ? O5 C29 1.38(6) . ? O5 C28 1.38(8) . ? O6 C30 1.44(9) . ? O6 C20 1.35(6) . ? O7 C31 1.42(6) . ? N1 C5 1.37(5) . ? N1 C1 1.35(8) . ? N2 C6 1.36(8) . ? N2 C10 1.35(8) . ? N3 C15 1.34(8) . ? N3 C11 1.35(6) . ? C1 C2 1.38(10) . ? C2 C3 1.41(6) . ? C3 C4 1.38(9) . ? C4 C5 1.41(8) . ? C5 C6 1.46(10) . ? C6 C7 1.40(6) . ? C7 C8 1.42(10) . ? C8 C9 1.41(9) . ? C9 C10 1.36(7) . ? C10 C11 1.49(8) . ? C11 C12 1.40(10) . ? C12 C13 1.38(8) . ? C13 C14 1.39(7) . ? C14 C15 1.40(10) . ? C16 C17 1.49(8) . ? C17 C22 1.39(8) . ? C17 C18 1.40(10) . ? C18 C19 1.41(7) . ? C19 C20 1.42(8) . ? C20 C21 1.39(10) . ? C21 C22 1.41(8) . ? C23 C24 1.51(9) . ? C25 C26 1.53(11) . ? C27 C28 1.48(10) . ? C29 C30 1.53(9) . ? C31 C32 1.52(8) . ? O7 H71 0.84 . ? O1W H1W 0.84 . ? C1 H1 0.93 . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 H4 0.93 . ? C7 H7 0.93 . ? C9 H9 0.93 . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 H16B 0.97 . ? C16 H16A 0.97 . ? C18 H18 0.93 . ? C21 H21 0.93 . ? C22 H22 0.93 . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24B 0.97 . ? C24 H24A 0.97 . ? C25 H25B 0.97 . ? C25 H25A 0.97 . ? C26 H26B 0.97 . ? C26 H26A 0.97 . ? C27 H27B 0.97 . ? C27 H27A 0.97 . ? C28 H28B 0.97 . ? C28 H28A 0.97 . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 H30B 0.97 . ? C30 H30A 0.97 . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? 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 N1 Ni N2 78(3) . . ? N1 Ni N3 156.7(15) . . ? N1 Ni N1 89(4) . 2_655 ? N1 Ni N2 100(3) . 2_655 ? N1 Ni N3 94(3) . 2_655 ? N2 Ni N3 79(3) . . ? N1 Ni N2 100(3) 2_655 . ? N2 Ni N2 177(6) . 2_655 ? N2 Ni N3 104(3) . 2_655 ? N1 Ni N3 94(3) 2_655 . ? N2 Ni N3 104(3) 2_655 . ? N3 Ni N3 92(5) . 2_655 ? N1 Ni N2 78(3) 2_655 2_655 ? N1 Ni N3 156.7(16) 2_655 2_655 ? N2 Ni N3 79(3) 2_655 2_655 ? F14 P1 F16 174(4) . . ? F15 P1 F16 85(3) . . ? F12 P1 F14 90(3) . . ? F11 P1 F12 177(4) . . ? F11 P1 F13 90(3) . . ? F11 P1 F14 93(3) . . ? F11 P1 F15 88(3) . . ? F11 P1 F16 88(3) . . ? F12 P1 F13 91(3) . . ? F13 P1 F14 93(3) . . ? F12 P1 F15 91(3) . . ? F13 P1 F15 177(3) . . ? F13 P1 F16 93(3) . . ? C8 O1 C16 117(7) . . ? C19 O2 C23 121(4) . . ? C24 O3 C25 114(8) . . ? C26 O4 C27 115(7) . . ? C28 O5 C29 140(5) . . ? C20 O6 C30 119(7) . . ? C31 O7 H71 113.11 . . ? Ni N1 C5 115(6) . . ? Ni N1 C1 132(4) . . ? C1 N1 C5 113(7) . . ? Ni N2 C10 120(5) . . ? C6 N2 C10 122(5) . . ? Ni N2 C6 118(6) . . ? Ni N3 C15 128(5) . . ? Ni N3 C11 114(5) . . ? C11 N3 C15 118(8) . . ? N1 C1 C2 128(6) . . ? C1 C2 C3 116(7) . . ? C2 C3 C4 121(7) . . ? C3 C4 C5 117(5) . . ? N1 C5 C4 125(8) . . ? N1 C5 C6 112(7) . . ? C4 C5 C6 122(5) . . ? C5 C6 C7 125(7) . . ? N2 C6 C7 119(8) . . ? F12 P1 F16 89(3) . . ? F14 P1 F15 89(3) . . ? N2 C6 C5 116(5) . . ? C6 C7 C8 120(7) . . ? O1 C8 C9 111(8) . . ? O1 C8 C7 131(7) . . ? C7 C8 C9 118(5) . . ? C8 C9 C10 119(8) . . ? C9 C10 C11 127(8) . . ? N2 C10 C11 112(5) . . ? N2 C10 C9 122(7) . . ? C10 C11 C12 122(5) . . ? N3 C11 C12 123(6) . . ? N3 C11 C10 115(8) . . ? C11 C12 C13 118(6) . . ? C12 C13 C14 121(8) . . ? C13 C14 C15 117(7) . . ? N3 C15 C14 123(5) . . ? O1 C16 C17 111(7) . . ? C16 C17 C22 120(8) . . ? C18 C17 C22 119(6) . . ? C16 C17 C18 121(7) . . ? C17 C18 C19 120(7) . . ? O2 C19 C20 113(5) . . ? C18 C19 C20 120(8) . . ? O2 C19 C18 126(7) . . ? O6 C20 C21 125(7) . . ? C19 C20 C21 117(5) . . ? O6 C20 C19 116(8) . . ? C20 C21 C22 121(7) . . ? C17 C22 C21 120(8) . . ? O2 C23 C24 107(5) . . ? O3 C24 C23 107(8) . . ? O3 C25 C26 107(8) . . ? O4 C26 C25 106(7) . . ? O4 C27 C28 91(6) . . ? O5 C28 C27 115(9) . . ? O5 C29 C30 109(4) . . ? O6 C30 C29 110(7) . . ? N1 C1 H1 116 . . ? C2 C1 H1 115 . . ? C3 C2 H2 121 . . ? C1 C2 H2 122 . . ? C2 C3 H3 119 . . ? C4 C3 H3 120 . . ? C5 C4 H4 121 . . ? C3 C4 H4 121 . . ? C8 C7 H7 119 . . ? C6 C7 H7 120 . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C13 C12 H12 121 . . ? C11 C12 H12 121 . . ? C14 C13 H13 119 . . ? C12 C13 H13 119 . . ? C15 C14 H14 121 . . ? C13 C14 H14 121 . . ? C14 C15 H15 117 . . ? N3 C15 H15 119 . . ? C17 C16 H16B 109 . . ? O1 C16 H16A 109 . . ? C17 C16 H16A 109 . . ? O1 C16 H16B 109 . . ? H16A C16 H16B 108 . . ? C19 C18 H18 119 . . ? C17 C18 H18 120 . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? C21 C22 H22 119 . . ? C17 C22 H22 119 . . ? H23A C23 H23B 108 . . ? O2 C23 H23A 109 . . ? C24 C23 H23A 109 . . ? C24 C23 H23B 110 . . ? O2 C23 H23B 111 . . ? O3 C24 H24B 109 . . ? C23 C24 H24B 111 . . ? H24A C24 H24B 108 . . ? C23 C24 H24A 110 . . ? O3 C24 H24A 109 . . ? O3 C25 H25B 110 . . ? C26 C25 H25B 110 . . ? H25A C25 H25B 109 . . ? C26 C25 H25A 109 . . ? O3 C25 H25A 109 . . ? C25 C26 H26A 109 . . ? C25 C26 H26B 110 . . ? O4 C26 H26B 110 . . ? H26A C26 H26B 109 . . ? O4 C26 H26A 110 . . ? O4 C27 H27B 114 . . ? O4 C27 H27A 113 . . ? C28 C27 H27B 112 . . ? H27A C27 H27B 111 . . ? C28 C27 H27A 112 . . ? O5 C28 H28B 108 . . ? C27 C28 H28A 108 . . ? C27 C28 H28B 108 . . ? H28A C28 H28B 107 . . ? O5 C28 H28A 108 . . ? O5 C29 H29B 109 . . ? C30 C29 H29A 109 . . ? O5 C29 H29A 110 . . ? H29A C29 H29B 108 . . ? C30 C29 H29B 109 . . ? O6 C30 H30A 109 . . ? O6 C30 H30B 110 . . ? H30A C30 H30B 107 . . ? C29 C30 H30A 109 . . ? C29 C30 H30B 110 . . ? O7 C31 H31A 109 . . ? C32 C31 H31A 109 . . ? C32 C31 H31B 108 . . ? O7 C31 H31B 108 . . ? H31A C31 H31B 107 . . ? C31 C32 H32B 109 . . ? C31 C32 H32C 108 . . ? C31 C32 H32A 109 . . ? H32A C32 H32C 109 . . ? H32B C32 H32C 110 . . ? H32A C32 H32B 110 . . ? _refine_diff_density_max 0.869 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.234 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 692436' _vrf_PLAT341_2 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang ... 89 RESPONSE: This is a powder diffraction study. All structural parameters were refined with the laboratory powder diffraction data. ; # end Validation Reply Form # start Validation Reply Form #_vrf_PLAT411_2 #; #PROBLEM: Short Inter H...H Contact H28B .. H28B .. 1.89 Ang. #RESPONSE: This crystal structure has been determined and refined #with the laboratory powder diffraction data, so all H-atoms were geometrically #positioned and not refined. #; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine]cobalt(II) bis(hexafluorophosphate) trihydrate ; _chemical_name_common ; Bis(4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''- terpyridine)cobalt(ii) bis(hexafluorophosphate) trihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Co N6 O12, 2(P F6), 3(H2 O)' _chemical_formula_sum 'C60 H68 Co F12 N6 O15 P2' _chemical_formula_weight 1462.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.636(2) _cell_length_b 20.828(2) _cell_length_c 25.056(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6594.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2014 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 40.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3020 _exptl_absorpt_coefficient_mu 3.407 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 1 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; ? ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology 'no specific habit' _pd_char_colour brown # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia ; _diffrn_ambient_temperature 295(2) _diffrn_source 'Fine focus X-ray tube' _diffrn_source_target Cu _diffrn_radiation_source 'line-focus sealed tube' _diffrn_radiation_monochromator 'Curved Germanium (111)' _diffrn_measurement_device 'Guinier camera G670' _diffrn_detector_type 'Imaging Plate' _diffrn_reflns_number ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_type CuK\a~1~ _diffrn_radiation_wavelength 1.5406 # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7501 _pd_meas_2theta_range_min 5.00 _pd_meas_2theta_range_max 80.00 _pd_meas_2theta_range_inc 0.01 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'local program' _computing_cell_refinement 'MRIA (Zlokazov & Chernyshev, 1992)' _computing_data_reduction 'local program' _computing_structure_solution MRIA _computing_structure_refinement MRIA _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ; MRIA, SHELXL97 (Sheldrick, 1997) ; #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function 'split-type pseudo-Voigt (Toraya, 1986)' _pd_proc_ls_pref_orient_corr ; March-Dollase (Dollase, 1986); direction of preferred orientation - 010, texture parameter r=0.89(1). ; _pd_proc_ls_background_function 'Chebyshev polynomial up to the 5th order' _pd_proc_ls_prof_R_factor 0.0092 _pd_proc_ls_prof_wR_factor 0.0119 _pd_proc_ls_prof_wR_expected 0.0091 _refine_special_details ; ? ; _refine_ls_R_I_factor ? _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 185 _refine_ls_number_restraints 199 _refine_ls_number_constraints 45 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.3163 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .006 _refine_ls_shift/su_mean .002 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.00 _pd_proc_2theta_range_max 80.00 _pd_proc_2theta_range_inc 0.01 _pd_proc_wavelength 1.5406 # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.7500 0.2500 0.4267(23) 0.044(8) Uiso 1 2 d S . . O1 O 1.1784(21) 0.1051(26) 0.4098(29) 0.057(6) Uiso 1 1 d . . . O2 O 1.4580(20) -0.0563(24) 0.3252(27) 0.057(6) Uiso 1 1 d . . . O3 O 1.3889(24) -0.1811(29) 0.3225(29) 0.057(6) Uiso 1 1 d . . . O4 O 1.4610(22) -0.2628(27) 0.4109(31) 0.057(6) Uiso 1 1 d . . . O5 O 1.6220(21) -0.1739(26) 0.4562(29) 0.057(6) Uiso 1 1 d . . . O6 O 1.5944(23) -0.0559(28) 0.3979(32) 0.057(6) Uiso 1 1 d . . . N1 N 0.8313(22) 0.2998(24) 0.3634(30) 0.057(6) Uiso 1 1 d . . . N2 N 0.8910(25) 0.2017(26) 0.4217(29) 0.057(6) Uiso 1 1 d . . . N3 N 0.7449(21) 0.1746(27) 0.4868(31) 0.057(6) Uiso 1 1 d . . . C1 C 0.7980(24) 0.3503(30) 0.3341(32) 0.057(6) Uiso 1 1 d . . . H1 H 0.7314 0.3674 0.3410 0.068 Uiso 1 1 calc . . . C2 C 0.8591(23) 0.3779(32) 0.2940(35) 0.057(6) Uiso 1 1 d . . . H2 H 0.8345 0.4127 0.2743 0.068 Uiso 1 1 calc . . . C3 C 0.9598(26) 0.3510(29) 0.2844(36) 0.057(6) Uiso 1 1 d . . . H3 H 1.0029 0.3683 0.2580 0.068 Uiso 1 1 calc . . . C4 C 0.9942(24) 0.3002(32) 0.3134(34) 0.057(6) Uiso 1 1 d . . . H4 H 1.0604 0.2823 0.3070 0.068 Uiso 1 1 calc . . . C5 C 0.9283(23) 0.2752(30) 0.3531(34) 0.057(6) Uiso 1 1 d . . . C6 C 0.9635(25) 0.2206(31) 0.3850(35) 0.057(6) Uiso 1 1 d . . . C7 C 1.0619(26) 0.1906(31) 0.3785(37) 0.057(6) Uiso 1 1 d . . . H7 H 1.1093 0.2051 0.3528 0.068 Uiso 1 1 calc . . . C8 C 1.0880(24) 0.1383(33) 0.4114(32) 0.057(6) Uiso 1 1 d . . . C9 C 1.0122(27) 0.1184(32) 0.4499(33) 0.057(6) Uiso 1 1 d . . . H9 H 1.0267 0.0840 0.4724 0.068 Uiso 1 1 calc . . . C10 C 0.9170(25) 0.1504(30) 0.4538(34) 0.057(6) Uiso 1 1 d . . . C11 C 0.8309(26) 0.1355(29) 0.4915(31) 0.057(6) Uiso 1 1 d . . . C12 C 0.8363(27) 0.0864(34) 0.5282(35) 0.057(6) Uiso 1 1 d . . . H12 H 0.8963 0.0606 0.5302 0.068 Uiso 1 1 calc . . . C13 C 0.7507(25) 0.0757(32) 0.5624(32) 0.057(6) Uiso 1 1 d . . . H13 H 0.7527 0.0428 0.5875 0.068 Uiso 1 1 calc . . . C14 C 0.6625(26) 0.1153(34) 0.5581(33) 0.057(6) Uiso 1 1 d . . . H14 H 0.6043 0.1095 0.5803 0.068 Uiso 1 1 calc . . . C15 C 0.6630(23) 0.1637(30) 0.5200(34) 0.057(6) Uiso 1 1 d . . . H15 H 0.6037 0.1900 0.5173 0.068 Uiso 1 1 calc . . . C16 C 1.2794(24) 0.1372(32) 0.3978(36) 0.057(6) Uiso 1 1 d . . . H16A H 1.2931 0.1706 0.4239 0.068 Uiso 1 1 calc . . . H16B H 1.2764 0.1568 0.3627 0.068 Uiso 1 1 calc . . . C17 C 1.3662(25) 0.0877(32) 0.3995(36) 0.057(6) Uiso 1 1 d . . . C18 C 1.3672(25) 0.0381(34) 0.3607(32) 0.057(6) Uiso 1 1 d . . . H18 H 1.3135 0.0362 0.3354 0.068 Uiso 1 1 calc . . . C19 C 1.4467(26) -0.0073(35) 0.3600(31) 0.057(6) Uiso 1 1 d . . . C20 C 1.5282(27) -0.0057(31) 0.4006(35) 0.057(6) Uiso 1 1 d . . . C21 C 1.5270(24) 0.0431(30) 0.4381(33) 0.057(6) Uiso 1 1 d . . . H21 H 1.5810 0.0457 0.4632 0.068 Uiso 1 1 calc . . . C22 C 1.4448(23) 0.0889(32) 0.4387(34) 0.057(6) Uiso 1 1 d . . . H22 H 1.4429 0.1200 0.4653 0.068 Uiso 1 1 calc . . . C23 C 1.3732(25) -0.0742(30) 0.2905(35) 0.057(6) Uiso 1 1 d . . . H23A H 1.3727 -0.0471 0.2590 0.068 Uiso 1 1 calc . . . H23B H 1.3058 -0.0697 0.3086 0.068 Uiso 1 1 calc . . . C24 C 1.3918(26) -0.1436(33) 0.2750(31) 0.057(6) Uiso 1 1 d . . . H24A H 1.3373 -0.1578 0.2504 0.068 Uiso 1 1 calc . . . H24B H 1.4600 -0.1481 0.2577 0.068 Uiso 1 1 calc . . . C25 C 1.4123(27) -0.2468(32) 0.3144(32) 0.057(6) Uiso 1 1 d . . . H25A H 1.4837 -0.2511 0.3006 0.068 Uiso 1 1 calc . . . H25B H 1.3638 -0.2646 0.2883 0.068 Uiso 1 1 calc . . . C26 C 1.4026(23) -0.2835(34) 0.3663(33) 0.057(6) Uiso 1 1 d . . . H26A H 1.3285 -0.2836 0.3763 0.068 Uiso 1 1 calc . . . H26B H 1.4223 -0.3277 0.3592 0.068 Uiso 1 1 calc . . . C27 C 1.5741(24) -0.2690(30) 0.4049(34) 0.057(6) Uiso 1 1 d . . . H27A H 1.5953 -0.3136 0.4014 0.068 Uiso 1 1 calc . . . H27B H 1.5999 -0.2448 0.3745 0.068 Uiso 1 1 calc . . . C28 C 1.6099(25) -0.2418(29) 0.4545(37) 0.057(6) Uiso 1 1 d . . . H28A H 1.5602 -0.2541 0.4822 0.068 Uiso 1 1 calc . . . H28B H 1.6775 -0.2611 0.4633 0.068 Uiso 1 1 calc . . . C29 C 1.7029(25) -0.1406(32) 0.4292(34) 0.057(6) Uiso 1 1 d . . . H29A H 1.7048 -0.1526 0.3918 0.068 Uiso 1 1 calc . . . H29B H 1.7713 -0.1497 0.4450 0.068 Uiso 1 1 calc . . . C30 C 1.6745(26) -0.0687(30) 0.4355(32) 0.057(6) Uiso 1 1 d . . . H30A H 1.6494 -0.0601 0.4714 0.068 Uiso 1 1 calc . . . H30B H 1.7360 -0.0421 0.4287 0.068 Uiso 1 1 calc . . . P1 P 0.9564(16) -0.0140(23) 0.3420(24) 0.046(7) Uiso 1 1 d . . . F11 F 0.8371(17) -0.0275(21) 0.3286(24) 0.106(12) Uiso 1 1 d . . . F12 F 1.0760(19) -0.0009(24) 0.3549(26) 0.106(12) Uiso 1 1 d . . . F13 F 0.9268(16) 0.0029(23) 0.4007(27) 0.106(12) Uiso 1 1 d . . . F14 F 0.9413(18) 0.0577(22) 0.3251(24) 0.106(12) Uiso 1 1 d . . . F15 F 0.9867(18) -0.0315(22) 0.2823(25) 0.106(12) Uiso 1 1 d . . . F16 F 0.9716(16) -0.0867(25) 0.3577(26) 0.106(12) Uiso 1 1 d . . . O1W O 0.2500 0.2500 0.2735(29) 0.082(9) Uiso 1 2 d S . . H1W H 0.2433 0.2170 0.2540 0.123 Uiso 1 1 d . . . O2W O 0.1721(21) 0.1151(28) 0.2275(30) 0.093(11) Uiso 1 1 d . . . H2W1 H 0.1131 0.0964 0.2227 0.123 Uiso 1 1 d . . . H2W2 H 0.2235 0.0901 0.2204 0.123 Uiso 1 1 d . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co N1 2.17(7) . ? Co N2 2.05(4) . ? Co N3 2.17(8) . ? Co N1 2.17(7) 2_655 ? Co N2 2.05(4) 2_655 ? Co N3 2.17(8) 2_655 ? P1 F15 1.60(7) . ? P1 F16 1.58(6) . ? P1 F12 1.57(4) . ? P1 F13 1.57(9) . ? P1 F11 1.57(3) . ? P1 F14 1.57(6) . ? O1 C16 1.47(6) . ? O1 C8 1.33(6) . ? O2 C23 1.44(8) . ? O2 C19 1.35(10) . ? O3 C24 1.41(10) . ? O3 C25 1.42(9) . ? O4 C26 1.41(9) . ? O4 C27 1.44(4) . ? O5 C29 1.41(7) . ? O5 C28 1.43(9) . ? O6 C20 1.34(8) . ? O6 C30 1.40(8) . ? O1W H1W 0.85 . ? O2W H2W2 0.85 . ? O2W H2W1 0.85 . ? N1 C5 1.36(5) . ? N1 C1 1.34(8) . ? N2 C6 1.37(9) . ? N2 C10 1.39(9) . ? N3 C15 1.35(7) . ? N3 C11 1.37(7) . ? C1 C2 1.39(10) . ? C2 C3 1.42(6) . ? C3 C4 1.36(10) . ? C4 C5 1.40(9) . ? C5 C6 1.45(10) . ? C6 C7 1.40(6) . ? C7 C8 1.40(10) . ? C8 C9 1.43(8) . ? C9 C10 1.38(6) . ? C10 C11 1.46(8) . ? C11 C12 1.38(11) . ? C12 C13 1.39(8) . ? C13 C14 1.38(6) . ? C14 C15 1.40(10) . ? C16 C17 1.50(7) . ? C17 C18 1.43(11) . ? C17 C22 1.40(9) . ? C18 C19 1.38(8) . ? C19 C20 1.45(10) . ? C20 C21 1.38(11) . ? C21 C22 1.41(7) . ? C23 C24 1.52(9) . ? C25 C26 1.51(10) . ? C27 C28 1.42(11) . ? C29 C30 1.55(9) . ? C1 H1 0.93 . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 H4 0.93 . ? C7 H7 0.93 . ? C9 H9 0.93 . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 H16B 0.97 . ? C16 H16A 0.97 . ? C18 H18 0.93 . ? C21 H21 0.93 . ? C22 H22 0.93 . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24B 0.97 . ? C24 H24A 0.97 . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 H27B 0.97 . ? C27 H27A 0.97 . ? C28 H28B 0.97 . ? C28 H28A 0.97 . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 H30B 0.97 . ? C30 H30A 0.97 . ? 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 N1 Co N2 77(2) . . ? N1 Co N3 150.7(13) . . ? N1 Co N1 85(3) . 2_655 ? N1 Co N2 98(2) . 2_655 ? N1 Co N3 99(2) . 2_655 ? N2 Co N3 74(2) . . ? N1 Co N2 98(2) 2_655 . ? N2 Co N2 173(4) . 2_655 ? N2 Co N3 112(2) . 2_655 ? N1 Co N3 99(2) 2_655 . ? N2 Co N3 112(2) 2_655 . ? N3 Co N3 92(3) . 2_655 ? N1 Co N2 77(2) 2_655 2_655 ? N1 Co N3 150.7(13) 2_655 2_655 ? N2 Co N3 74(2) 2_655 2_655 ? F13 P1 F15 179(3) . . ? F13 P1 F16 90(4) . . ? F14 P1 F15 90(3) . . ? F14 P1 F16 179(4) . . ? F15 P1 F16 89(4) . . ? F11 P1 F12 180(6) . . ? F11 P1 F13 90(3) . . ? F11 P1 F14 90(2) . . ? F11 P1 F15 90(3) . . ? F11 P1 F16 90(3) . . ? F12 P1 F13 90(4) . . ? F12 P1 F14 90(3) . . ? F12 P1 F15 90(3) . . ? F12 P1 F16 90(2) . . ? F13 P1 F14 91(3) . . ? C8 O1 C16 121(6) . . ? C19 O2 C23 121(4) . . ? C24 O3 C25 114(6) . . ? C26 O4 C27 114(6) . . ? C28 O5 C29 123(5) . . ? C20 O6 C30 124(7) . . ? H2W1 O2W H2W2 110.85 . . ? Co N1 C5 112(4) . . ? Co N1 C1 129(3) . . ? C1 N1 C5 119(6) . . ? C6 N2 C10 117(4) . . ? Co N2 C6 119(5) . . ? Co N2 C10 124(4) . . ? C11 N3 C15 117(6) . . ? Co N3 C11 118(4) . . ? Co N3 C15 125(4) . . ? N1 C1 C2 123(4) . . ? C1 C2 C3 117(6) . . ? C2 C3 C4 120(7) . . ? C3 C4 C5 119(4) . . ? C4 C5 C6 120(4) . . ? N1 C5 C4 122(6) . . ? N1 C5 C6 119(5) . . ? C5 C6 C7 124(7) . . ? N2 C6 C5 113(4) . . ? N2 C6 C7 123(7) . . ? C6 C7 C8 120(6) . . ? O1 C8 C9 116(6) . . ? O1 C8 C7 127(6) . . ? C7 C8 C9 117(4) . . ? C8 C9 C10 120(6) . . ? N2 C10 C9 123(5) . . ? C9 C10 C11 126(6) . . ? N2 C10 C11 111(4) . . ? N3 C11 C12 122(5) . . ? N3 C11 C10 114(6) . . ? C10 C11 C12 123(4) . . ? C11 C12 C13 119(5) . . ? C12 C13 C14 119(6) . . ? C13 C14 C15 119(5) . . ? N3 C15 C14 123(4) . . ? O1 C16 C17 109(5) . . ? C16 C17 C18 119(6) . . ? C16 C17 C22 122(7) . . ? C18 C17 C22 119(5) . . ? C17 C18 C19 121(5) . . ? O2 C19 C18 127(6) . . ? C18 C19 C20 120(7) . . ? O2 C19 C20 113(5) . . ? O6 C20 C19 113(7) . . ? O6 C20 C21 128(7) . . ? C19 C20 C21 119(5) . . ? C20 C21 C22 121(5) . . ? C17 C22 C21 120(6) . . ? O2 C23 C24 106(4) . . ? O3 C24 C23 108(6) . . ? O3 C25 C26 110(6) . . ? O4 C26 C25 120(5) . . ? O4 C27 C28 101(5) . . ? O5 C28 C27 117(7) . . ? O5 C29 C30 105(4) . . ? O6 C30 C29 107(5) . . ? N1 C1 H1 118 . . ? C2 C1 H1 118 . . ? C3 C2 H2 121 . . ? C1 C2 H2 121 . . ? C2 C3 H3 120 . . ? C4 C3 H3 119 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C6 C7 H7 120 . . ? C8 C7 H7 119 . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C11 C12 H12 119 . . ? C13 C12 H12 120 . . ? C12 C13 H13 120 . . ? C14 C13 H13 119 . . ? C13 C14 H14 121 . . ? C15 C14 H14 119 . . ? N3 C15 H15 118 . . ? C14 C15 H15 118 . . ? O1 C16 H16A 110 . . ? O1 C16 H16B 110 . . ? C17 C16 H16A 109 . . ? H16A C16 H16B 107 . . ? C17 C16 H16B 110 . . ? C17 C18 H18 119 . . ? C19 C18 H18 119 . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? C17 C22 H22 119 . . ? C21 C22 H22 120 . . ? O2 C23 H23B 112 . . ? O2 C23 H23A 110 . . ? H23A C23 H23B 109 . . ? C24 C23 H23A 111 . . ? C24 C23 H23B 110 . . ? O3 C24 H24A 110 . . ? C23 C24 H24B 109 . . ? O3 C24 H24B 110 . . ? C23 C24 H24A 109 . . ? H24A C24 H24B 108 . . ? O3 C25 H25B 109 . . ? C26 C25 H25A 109 . . ? C26 C25 H25B 110 . . ? H25A C25 H25B 109 . . ? O3 C25 H25A 108 . . ? O4 C26 H26A 107 . . ? O4 C26 H26B 106 . . ? C25 C26 H26B 107 . . ? H26A C26 H26B 108 . . ? C25 C26 H26A 107 . . ? O4 C27 H27A 111 . . ? C28 C27 H27A 111 . . ? C28 C27 H27B 111 . . ? O4 C27 H27B 111 . . ? H27A C27 H27B 109 . . ? C27 C28 H28A 108 . . ? C27 C28 H28B 109 . . ? H28A C28 H28B 109 . . ? O5 C28 H28B 107 . . ? O5 C28 H28A 107 . . ? C30 C29 H29A 109 . . ? O5 C29 H29A 111 . . ? O5 C29 H29B 110 . . ? H29A C29 H29B 109 . . ? C30 C29 H29B 110 . . ? O6 C30 H30B 111 . . ? O6 C30 H30A 110 . . ? H30A C30 H30B 107 . . ? C29 C30 H30A 110 . . ? C29 C30 H30B 110 . . ? _refine_diff_density_max 0.947 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.305 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 692437' #start Validation Reply Form _vrf_PLAT341_3 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang ... 89 RESPONSE: This is a powder diffraction study. All structural parameters were refined with the laboratory powder diffraction data. ; _vrf_PLAT411_3 ; PROBLEM: Short Inter H...H Contact H25C .. H30C .. 1.76 Ang. RESPONSE: This crystal structure has been determined and refined with the laboratory powder diffraction data, so all H-atoms were geometrically positioned and not refined. ; # end Validation Reply Form _audit_creation_method manual _chemical_name_systematic ; Bis[4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine] copper(II) bis(hexafluorophosphate) ; _chemical_name_common ; Bis(4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''- terpyridine) copper(ii) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Cu N6 O12, 2(P F6)' _chemical_formula_sum 'C60 H62 Cu F12 N6 O12 P2' _chemical_formula_weight 1412.65 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 12.618(2) _cell_length_b 12.557(2) _cell_length_c 39.689(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.969(17) _cell_angle_gamma 90.00 _cell_volume 6227.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1908 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 39.98 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2908 _exptl_absorpt_coefficient_mu 1.884 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 1 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; ? ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology 'no specific habit' _pd_char_colour 'light green' # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia ; _diffrn_ambient_temperature 295(2) _diffrn_source 'Fine focus X-ray tube' _diffrn_source_target Cu _diffrn_radiation_source 'line-focus sealed tube' _diffrn_radiation_monochromator 'Curved Germanium (111)' _diffrn_measurement_device 'Guinier camera G670' _diffrn_detector_type 'Imaging Plate' _diffrn_reflns_number ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_type CuK\a~1~ _diffrn_radiation_wavelength 1.5406 # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7631 _pd_meas_2theta_range_min 3.70 _pd_meas_2theta_range_max 80.00 _pd_meas_2theta_range_inc 0.01 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'local program' _computing_cell_refinement 'MRIA (Zlokazov & Chernyshev, 1992)' _computing_data_reduction 'local program' _computing_structure_solution 'FOX (Favre-Nicolin & Cerny, 2002) and MRIA' _computing_structure_refinement MRIA _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ; MRIA, SHELXL97 (Sheldrick, 1997) ; #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function 'split-type pseudo-Voigt (Toraya, 1986)' _pd_proc_ls_pref_orient_corr ; March-Dollase (Dollase, 1986); direction of preferred orientation - 010, texture parameter r=0.97(1). ; _pd_proc_ls_background_function 'Chebyshev polynomial up to the 5th order' _pd_proc_ls_prof_R_factor 0.0193 _pd_proc_ls_prof_wR_factor 0.0247 _pd_proc_ls_prof_wR_expected 0.0141 _refine_special_details ; ? ; _refine_ls_R_I_factor ? _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 306 _refine_ls_number_restraints 299 _refine_ls_number_constraints 85 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.7504 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .009 _refine_ls_shift/su_mean .004 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.00 _pd_proc_2theta_range_max 80.00 _pd_proc_2theta_range_inc 0.01 _pd_proc_wavelength 1.5406 # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.6619(21) 0.5000 0.058(6) Uiso 1 1 d . . . O1A O 0.5180(22) 0.6707(22) 0.6558(17) 0.071(7) Uiso 1 1 d . . . O2A O 0.6615(24) 0.9822(21) 0.7543(18) 0.071(7) Uiso 1 1 d . . . O3A O 0.7987(21) 1.1551(23) 0.7739(16) 0.071(7) Uiso 1 1 d . . . O4A O 0.8003(22) 1.1493(24) 0.8474(19) 0.071(7) Uiso 1 1 d . . . O5A O 0.6010(23) 0.9780(22) 0.8680(17) 0.071(7) Uiso 1 1 d . . . O6A O 0.5575(23) 0.8941(22) 0.7982(17) 0.071(7) Uiso 1 1 d . . . N1A N 0.3327(21) 0.7111(24) 0.5072(18) 0.071(7) Uiso 1 1 d . . . N2A N 0.5027(24) 0.6578(23) 0.5514(19) 0.071(7) Uiso 1 1 d . . . N3A N 0.6580(22) 0.5840(21) 0.5190(16) 0.071(7) Uiso 1 1 d . . . C1A C 0.2529(25) 0.7420(25) 0.4835(21) 0.071(7) Uiso 1 1 d . . . H1A H 0.2632 0.7382 0.4608 0.085 Uiso 1 1 calc . . . C2A C 0.1549(27) 0.7797(26) 0.4911(23) 0.071(7) Uiso 1 1 d . . . H2A H 0.0995 0.7961 0.4739 0.085 Uiso 1 1 calc . . . C3A C 0.1427(24) 0.7920(24) 0.5253(22) 0.071(7) Uiso 1 1 d . . . H3A H 0.0793 0.8188 0.5314 0.085 Uiso 1 1 calc . . . C4A C 0.2270(28) 0.7635(27) 0.5502(20) 0.071(7) Uiso 1 1 d . . . H4A H 0.2203 0.7710 0.5731 0.085 Uiso 1 1 calc . . . C5A C 0.3220(24) 0.7234(25) 0.5405(21) 0.071(7) Uiso 1 1 d . . . C6A C 0.4181(25) 0.6946(24) 0.5652(24) 0.071(7) Uiso 1 1 d . . . C7A C 0.4189(26) 0.7023(25) 0.6004(22) 0.071(7) Uiso 1 1 d . . . H7A H 0.3589 0.7261 0.6094 0.085 Uiso 1 1 calc . . . C8A C 0.5130(26) 0.6731(27) 0.6220(23) 0.071(7) Uiso 1 1 d . . . C9A C 0.5984(27) 0.6293(24) 0.6071(23) 0.071(7) Uiso 1 1 d . . . H9A H 0.6589 0.6040 0.6208 0.085 Uiso 1 1 calc . . . C10A C 0.5919(24) 0.6240(23) 0.5719(22) 0.071(7) Uiso 1 1 d . . . C11A C 0.6795(28) 0.5846(26) 0.5534(20) 0.071(7) Uiso 1 1 d . . . C12A C 0.7783(29) 0.5481(26) 0.5699(23) 0.071(7) Uiso 1 1 d . . . H12A H 0.7907 0.5434 0.5935 0.085 Uiso 1 1 calc . . . C13A C 0.8576(25) 0.5189(25) 0.5505(24) 0.071(7) Uiso 1 1 d . . . H13A H 0.9258 0.5011 0.5610 0.085 Uiso 1 1 calc . . . C14A C 0.8333(26) 0.5167(27) 0.5151(19) 0.071(7) Uiso 1 1 d . . . H14A H 0.8833 0.4929 0.5017 0.085 Uiso 1 1 calc . . . C15A C 0.7323(24) 0.5510(23) 0.5004(18) 0.071(7) Uiso 1 1 d . . . H15A H 0.7160 0.5509 0.4768 0.085 Uiso 1 1 calc . . . C16A C 0.6185(27) 0.6653(22) 0.6795(21) 0.071(7) Uiso 1 1 d . . . H16A H 0.6760 0.6988 0.6695 0.085 Uiso 1 1 calc . . . H16B H 0.6378 0.5917 0.6846 0.085 Uiso 1 1 calc . . . C17A C 0.6006(27) 0.7226(28) 0.7113(23) 0.071(7) Uiso 1 1 d . . . C18A C 0.6426(25) 0.8258(25) 0.7172(22) 0.071(7) Uiso 1 1 d . . . H18A H 0.6794 0.8577 0.7011 0.085 Uiso 1 1 calc . . . C19A C 0.6297(26) 0.8808(24) 0.7469(24) 0.071(7) Uiso 1 1 d . . . C20A C 0.5668(24) 0.8338(27) 0.7704(20) 0.071(7) Uiso 1 1 d . . . C21A C 0.5252(28) 0.7311(27) 0.7639(19) 0.071(7) Uiso 1 1 d . . . H21A H 0.4842 0.7003 0.7790 0.085 Uiso 1 1 calc . . . C22A C 0.5444(25) 0.6741(26) 0.7350(21) 0.071(7) Uiso 1 1 d . . . H22A H 0.5199 0.6045 0.7317 0.085 Uiso 1 1 calc . . . C23A C 0.7135(27) 1.0420(29) 0.7304(22) 0.071(7) Uiso 1 1 d . . . H23A H 0.6709 1.0404 0.7081 0.085 Uiso 1 1 calc . . . H23B H 0.7832 1.0118 0.7286 0.085 Uiso 1 1 calc . . . C24A C 0.7252(23) 1.1545(24) 0.7433(23) 0.071(7) Uiso 1 1 d . . . H24A H 0.7514 1.1997 0.7264 0.085 Uiso 1 1 calc . . . H24B H 0.6563 1.1816 0.7476 0.085 Uiso 1 1 calc . . . C25A C 0.7984(26) 1.2513(27) 0.7927(20) 0.071(7) Uiso 1 1 d . . . H25A H 0.7402 1.2951 0.7818 0.085 Uiso 1 1 calc . . . H25B H 0.8645 1.2888 0.7907 0.085 Uiso 1 1 calc . . . C26A C 0.7881(24) 1.2447(26) 0.8280(21) 0.071(7) Uiso 1 1 d . . . H26A H 0.8390 1.2951 0.8395 0.085 Uiso 1 1 calc . . . H26B H 0.7175 1.2720 0.8303 0.085 Uiso 1 1 calc . . . C27A C 0.7141(24) 1.1294(25) 0.8665(24) 0.071(7) Uiso 1 1 d . . . H27A H 0.6839 1.1967 0.8725 0.085 Uiso 1 1 calc . . . H27B H 0.7413 1.0925 0.8874 0.085 Uiso 1 1 calc . . . C28A C 0.6263(28) 1.0620(27) 0.8461(18) 0.071(7) Uiso 1 1 d . . . H28A H 0.5635 1.1052 0.8390 0.085 Uiso 1 1 calc . . . H28B H 0.6515 1.0329 0.8260 0.085 Uiso 1 1 calc . . . C29A C 0.6240(27) 0.8738(24) 0.8569(21) 0.071(7) Uiso 1 1 d . . . H29A H 0.6282 0.8242 0.8758 0.085 Uiso 1 1 calc . . . H29B H 0.6922 0.8735 0.8482 0.085 Uiso 1 1 calc . . . C30A C 0.5330(25) 0.8399(25) 0.8284(20) 0.071(7) Uiso 1 1 d . . . H30A H 0.5327 0.7633 0.8252 0.085 Uiso 1 1 calc . . . H30B H 0.4637 0.8619 0.8339 0.085 Uiso 1 1 calc . . . O1B O 0.4546(21) 0.6588(20) 0.3439(18) 0.071(7) Uiso 1 1 d . . . O2B O 0.7220(23) 0.5503(19) 0.2466(19) 0.071(7) Uiso 1 1 d . . . O3B O 0.8745(20) 0.4374(22) 0.2138(17) 0.071(7) Uiso 1 1 d . . . O4B O 0.8583(19) 0.4770(20) 0.1438(20) 0.071(7) Uiso 1 1 d . . . O5B O 0.6153(20) 0.6127(18) 0.1258(18) 0.071(7) Uiso 1 1 d . . . O6B O 0.5838(21) 0.6227(23) 0.1976(19) 0.071(7) Uiso 1 1 d . . . N1B N 0.4263(22) 0.5021(21) 0.4857(17) 0.071(7) Uiso 1 1 d . . . N2B N 0.4789(24) 0.6702(20) 0.4484(20) 0.071(7) Uiso 1 1 d . . . N3B N 0.5529(23) 0.8276(24) 0.4869(21) 0.071(7) Uiso 1 1 d . . . C1B C 0.3912(26) 0.4280(25) 0.5055(21) 0.071(7) Uiso 1 1 d . . . H1B H 0.3926 0.4417 0.5286 0.085 Uiso 1 1 calc . . . C2B C 0.3523(24) 0.3303(23) 0.4923(20) 0.071(7) Uiso 1 1 d . . . H2B H 0.3298 0.2784 0.5065 0.085 Uiso 1 1 calc . . . C3B C 0.3478(25) 0.3120(27) 0.4575(23) 0.071(7) Uiso 1 1 d . . . H3B H 0.3264 0.2461 0.4482 0.085 Uiso 1 1 calc . . . C4B C 0.3760(27) 0.3941(26) 0.4368(20) 0.071(7) Uiso 1 1 d . . . H4B H 0.3681 0.3856 0.4133 0.085 Uiso 1 1 calc . . . C5B C 0.4164(28) 0.4898(24) 0.4518(24) 0.071(7) Uiso 1 1 d . . . C6B C 0.4432(25) 0.5846(28) 0.4314(19) 0.071(7) Uiso 1 1 d . . . C7B C 0.4315(24) 0.5693(27) 0.3961(18) 0.071(7) Uiso 1 1 d . . . H7B H 0.4040 0.5070 0.3856 0.085 Uiso 1 1 calc . . . C8B C 0.4653(27) 0.6572(26) 0.3778(21) 0.071(7) Uiso 1 1 d . . . C9B C 0.5002(25) 0.7521(25) 0.3950(20) 0.071(7) Uiso 1 1 d . . . H9B H 0.5186 0.8112 0.3829 0.085 Uiso 1 1 calc . . . C10B C 0.5067(23) 0.7559(27) 0.4303(23) 0.071(7) Uiso 1 1 d . . . C11B C 0.5473(26) 0.8467(24) 0.4529(20) 0.071(7) Uiso 1 1 d . . . C12B C 0.5808(22) 0.9439(28) 0.4407(19) 0.071(7) Uiso 1 1 d . . . H12B H 0.5800 0.9545 0.4175 0.085 Uiso 1 1 calc . . . C13B C 0.6153(25) 1.0244(23) 0.4637(22) 0.071(7) Uiso 1 1 d . . . H13B H 0.6382 1.0893 0.4560 0.085 Uiso 1 1 calc . . . C14B C 0.6153(28) 1.0069(22) 0.4984(23) 0.071(7) Uiso 1 1 d . . . H14B H 0.6347 1.0606 0.5142 0.085 Uiso 1 1 calc . . . C15B C 0.5854(24) 0.9066(25) 0.5087(18) 0.071(7) Uiso 1 1 d . . . H15B H 0.5881 0.8937 0.5319 0.085 Uiso 1 1 calc . . . C16B C 0.4496(25) 0.5544(26) 0.3261(23) 0.071(7) Uiso 1 1 d . . . H16C H 0.3770 0.5270 0.3231 0.085 Uiso 1 1 calc . . . H16D H 0.4959 0.5031 0.3392 0.085 Uiso 1 1 calc . . . C17B C 0.4861(22) 0.5736(27) 0.2924(21) 0.071(7) Uiso 1 1 d . . . C18B C 0.5911(27) 0.5491(25) 0.2869(24) 0.071(7) Uiso 1 1 d . . . H18B H 0.6397 0.5226 0.3047 0.085 Uiso 1 1 calc . . . C19B C 0.6228(24) 0.5643(24) 0.2549(20) 0.071(7) Uiso 1 1 d . . . C20B C 0.5492(29) 0.6110(27) 0.2284(23) 0.071(7) Uiso 1 1 d . . . C21B C 0.4445(26) 0.6328(28) 0.2342(19) 0.071(7) Uiso 1 1 d . . . H21B H 0.3952 0.6591 0.2166 0.085 Uiso 1 1 calc . . . C22B C 0.4134(25) 0.6156(26) 0.2660(21) 0.071(7) Uiso 1 1 d . . . H22B H 0.3441 0.6321 0.2697 0.085 Uiso 1 1 calc . . . C23B C 0.7996(24) 0.4821(26) 0.2658(22) 0.071(7) Uiso 1 1 d . . . H23C H 0.7682 0.4125 0.2683 0.085 Uiso 1 1 calc . . . H23D H 0.8198 0.5117 0.2883 0.085 Uiso 1 1 calc . . . C24B C 0.8979(23) 0.4706(24) 0.2483(22) 0.071(7) Uiso 1 1 d . . . H24C H 0.9350 0.5384 0.2491 0.085 Uiso 1 1 calc . . . H24D H 0.9457 0.4192 0.2607 0.085(7) Uiso 1 1 calc . . . C25B C 0.9607(27) 0.4179(27) 0.1950(20) 0.071(7) Uiso 1 1 d . . . H25C H 0.9583 0.3438 0.1880 0.085 Uiso 1 1 calc . . . H25D H 1.0276 0.4290 0.2099 0.085 Uiso 1 1 calc . . . C26B C 0.9601(27) 0.4867(27) 0.1640(21) 0.071(7) Uiso 1 1 d . . . H26C H 0.9732 0.5603 0.1707 0.085 Uiso 1 1 calc . . . H26D H 1.0160 0.4640 0.1511 0.085 Uiso 1 1 calc . . . C27B C 0.7740(25) 0.5341(24) 0.1560(24) 0.071(7) Uiso 1 1 d . . . H27C H 0.8002 0.5606 0.1786 0.085 Uiso 1 1 calc . . . H27D H 0.7165 0.4845 0.1583 0.085 Uiso 1 1 calc . . . C28B C 0.7275(26) 0.6273(28) 0.1344(20) 0.071(7) Uiso 1 1 d . . . H28C H 0.7416 0.6933 0.1469 0.085 Uiso 1 1 calc . . . H28D H 0.7609 0.6316 0.1138 0.085 Uiso 1 1 calc . . . C29B C 0.5506(28) 0.6886(27) 0.1398(23) 0.071(7) Uiso 1 1 d . . . H29C H 0.4937 0.7103 0.1222 0.085 Uiso 1 1 calc . . . H29D H 0.5939 0.7510 0.1464 0.085 Uiso 1 1 calc . . . C30B C 0.5009(25) 0.6513(25) 0.1702(18) 0.071(7) Uiso 1 1 d . . . H30C H 0.4569 0.7076 0.1777 0.085 Uiso 1 1 calc . . . H30D H 0.4555 0.5901 0.1639 0.085 Uiso 1 1 calc . . . P1 P 0.7243(18) 0.9536(19) 0.6060(14) 0.079(9) Uiso 1 1 d . . . F11 F 0.6892(17) 0.9594(17) 0.6427(16) 0.149(12) Uiso 1 1 d . . . F12 F 0.7596(19) 0.9519(20) 0.5698(13) 0.149(12) Uiso 1 1 d . . . F13 F 0.8437(19) 0.9794(17) 0.6217(15) 0.149(12) Uiso 1 1 d . . . F14 F 0.7026(20) 1.0775(18) 0.6021(14) 0.149(12) Uiso 1 1 d . . . F15 F 0.6062(18) 0.9298(16) 0.5908(16) 0.149(12) Uiso 1 1 d . . . F16 F 0.7493(15) 0.8327(19) 0.6111(17) 0.149(12) Uiso 1 1 d . . . P2 P 0.7420(19) 0.4554(18) 0.3888(17) 0.068(8) Uiso 1 1 d . . . F21 F 0.8523(18) 0.5057(20) 0.3827(13) 0.118(11) Uiso 1 1 d . . . F22 F 0.6327(16) 0.4037(16) 0.3941(14) 0.118(11) Uiso 1 1 d . . . F23 F 0.6866(17) 0.5280(17) 0.3587(15) 0.118(11) Uiso 1 1 d . . . F24 F 0.7263(18) 0.5464(19) 0.4148(16) 0.118(11) Uiso 1 1 d . . . F25 F 0.7999(20) 0.3870(18) 0.4187(18) 0.118(11) Uiso 1 1 d . . . F26 F 0.7575(17) 0.3640(21) 0.3630(15) 0.118(11) Uiso 1 1 d . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 N1A 2.25(3) . ? Cu1 N1B 2.25(4) . ? Cu1 N2A 2.04(7) . ? Cu1 N2B 2.05(8) . ? Cu1 N3A 2.26(3) . ? Cu1 N3B 2.27(4) . ? P1 F12 1.56(7) . ? P1 F13 1.58(4) . ? P1 F14 1.58(3) . ? P1 F15 1.56(4) . ? P1 F16 1.56(4) . ? P1 F11 1.58(8) . ? P2 F21 1.58(4) . ? P2 F25 1.56(8) . ? P2 F26 1.57(6) . ? P2 F24 1.57(6) . ? P2 F22 1.56(3) . ? P2 F23 1.59(7) . ? O1A C16A 1.46(7) . ? O1A C8A 1.33(10) . ? O1B C8B 1.34(11) . ? O1B C16B 1.49(6) . ? O2A C23A 1.46(8) . ? O2A C19A 1.35(4) . ? O2B C19B 1.35(5) . ? O2B C23B 1.44(7) . ? O3A C24A 1.43(9) . ? O3A C25A 1.43(7) . ? O3B C25B 1.43(7) . ? O3B C24B 1.42(10) . ? O4A C26A 1.43(7) . ? O4A C27A 1.44(7) . ? O4B C26B 1.42(7) . ? O4B C27B 1.42(5) . ? O5A C29A 1.42(5) . ? O5A C28A 1.43(7) . ? O5B C29B 1.42(6) . ? O5B C28B 1.43(5) . ? O6A C20A 1.37(9) . ? O6A C30A 1.44(9) . ? O6B C30B 1.44(8) . ? O6B C20B 1.35(10) . ? N1A C1A 1.33(8) . ? N1A C5A 1.34(10) . ? N1B C1B 1.34(7) . ? N1B C5B 1.33(10) . ? N2A C10A 1.36(7) . ? N2A C6A 1.35(6) . ? N2B C6B 1.30(7) . ? N2B C10B 1.37(7) . ? N3A C15A 1.33(6) . ? N3A C11A 1.34(10) . ? N3B C11B 1.36(11) . ? N3B C15B 1.34(7) . ? C1A C2A 1.39(5) . ? C1B C2B 1.41(6) . ? C2A C3A 1.39(11) . ? C2B C3B 1.36(11) . ? C3A C4A 1.40(9) . ? C3B C4B 1.40(8) . ? C4A C5A 1.41(6) . ? C4B C5B 1.41(6) . ? C5A C6A 1.50(8) . ? C5B C6B 1.51(7) . ? C6A C7A 1.39(11) . ? C6B C7B 1.40(10) . ? C7A C8A 1.42(8) . ? C7B C8B 1.42(7) . ? C8A C9A 1.41(7) . ? C8B C9B 1.41(7) . ? C9A C10A 1.38(11) . ? C9B C10B 1.38(11) . ? C10A C11A 1.50(7) . ? C10B C11B 1.51(8) . ? C11A C12A 1.41(7) . ? C11B C12B 1.40(6) . ? C12A C13A 1.42(7) . ? C12B C13B 1.39(8) . ? C13A C14A 1.38(11) . ? C13B C14B 1.37(11) . ? C14A C15A 1.39(6) . ? C14B C15B 1.39(5) . ? C16A C17A 1.50(10) . ? C16B C17B 1.50(10) . ? C17A C18A 1.41(5) . ? C17A C22A 1.41(8) . ? C17B C22B 1.39(9) . ? C17B C18B 1.40(5) . ? C18A C19A 1.41(10) . ? C18B C19B 1.40(10) . ? C19A C20A 1.42(8) . ? C19B C20B 1.45(9) . ? C20A C21A 1.41(6) . ? C20B C21B 1.41(6) . ? C21A C22A 1.40(9) . ? C21B C22B 1.39(10) . ? C23A C24A 1.51(6) . ? C23B C24B 1.52(6) . ? C25A C26A 1.41(11) . ? C25B C26B 1.50(10) . ? C27A C28A 1.54(7) . ? C27B C28B 1.52(7) . ? C29A C30A 1.57(9) . ? C29B C30B 1.51(9) . ? C1A H1A 0.93 . ? C1B H1B 0.93 . ? C2A H2A 0.92 . ? C2B H2B 0.93 . ? C3A H3A 0.93 . ? C3B H3B 0.93 . ? C4A H4A 0.93 . ? C4B H4B 0.93 . ? C7A H7A 0.93 . ? C7B H7B 0.92 . ? C9A H9A 0.93 . ? C9B H9B 0.93 . ? C12A H12A 0.92 . ? C12B H12B 0.92 . ? C13A H13A 0.93 . ? C13B H13B 0.94 . ? C14A H14A 0.93 . ? C14B H14B 0.94 . ? C15A H15A 0.93 . ? C15B H15B 0.93 . ? C16A H16B 0.97 . ? C16A H16A 0.96 . ? C16B H16C 0.97 . ? C16B H16D 0.96 . ? C18A H18A 0.93 . ? C18B H18B 0.93 . ? C21A H21A 0.93 . ? C21B H21B 0.93 . ? C22A H22A 0.93 . ? C22B H22B 0.93 . ? C23A H23A 0.96 . ? C23A H23B 0.96 . ? C23B H23D 0.96 . ? C23B H23C 0.97 . ? C24A H24A 0.96 . ? C24A H24B 0.96 . ? C24B H24C 0.96 . ? C24B H24D 0.97 . ? C25A H25A 0.97 . ? C25A H25B 0.97 . ? C25B H25D 0.96 . ? C25B H25C 0.97 . ? C26A H26A 0.96 . ? C26A H26B 0.96 . ? C26B H26D 0.97 . ? C26B H26C 0.96 . ? C27A H27A 0.96 . ? C27A H27B 0.96 . ? C27B H27C 0.97 . ? C27B H27D 0.96 . ? C28A H28B 0.97 . ? C28A H28A 0.96 . ? C28B H28C 0.97 . ? C28B H28D 0.96 . ? C29A H29A 0.96 . ? C29A H29B 0.97 . ? C29B H29C 0.97 . ? C29B H29D 0.96 . ? C30A H30A 0.96 . ? C30A H30B 0.97 . ? C30B H30D 0.96 . ? C30B H30C 0.97 . ? _refine_diff_density_max 0.893 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.318 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 692438' # start Validation Reply Form _vrf_PLAT341_4 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang ... 87 RESPONSE: This is a powder diffraction study. All structural parameters were refined with the laboratory powder diffraction data. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine]zinc(II) bis(hexafluorophosphate) trihydrate ; _chemical_name_common ; Bis(4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''- terpyridine)zinc(ii) bis(hexafluorophosphate) trihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 N6 O12 Zn, 2(P F6), 3(H2 O)' _chemical_formula_sum 'C60 H68 F12 N6 O15 P2 Zn' _chemical_formula_weight 1468.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 12.679(2) _cell_length_b 20.891(2) _cell_length_c 25.303(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6702.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2047 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 40.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 1.854 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 1 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; ? ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology 'no specific habit' _pd_char_colour colourless # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia ; _diffrn_ambient_temperature 295(2) _diffrn_source 'Fine focus X-ray tube' _diffrn_source_target Cu _diffrn_radiation_source 'line-focus sealed tube' _diffrn_radiation_monochromator 'Curved Germanium (111)' _diffrn_measurement_device 'Guinier camera G670' _diffrn_detector_type 'Imaging Plate' _diffrn_reflns_number ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_type CuK\a~1~ _diffrn_radiation_wavelength 1.5406 # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7501 _pd_meas_2theta_range_min 5.00 _pd_meas_2theta_range_max 80.00 _pd_meas_2theta_range_inc 0.01 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'local program' _computing_cell_refinement 'MRIA (Zlokazov & Chernyshev, 1992)' _computing_data_reduction 'local program' _computing_structure_solution MRIA _computing_structure_refinement MRIA _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ; MRIA, SHELXL97 (Sheldrick, 1997) ; #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function 'split-type pseudo-Voigt (Toraya, 1986)' _pd_proc_ls_pref_orient_corr ; March-Dollase (Dollase, 1986); direction of preferred orientation - 010, texture parameter r=0.87(1). ; _pd_proc_ls_background_function 'Chebyshev polynomial up to the 5th order' _pd_proc_ls_prof_R_factor 0.0166 _pd_proc_ls_prof_wR_factor 0.0212 _pd_proc_ls_prof_wR_expected 0.0124 _refine_special_details ; ? ; _refine_ls_R_I_factor ? _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 185 _refine_ls_number_restraints 199 _refine_ls_number_constraints 45 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.7148 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .005 _refine_ls_shift/su_mean .001 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.00 _pd_proc_2theta_range_max 80.00 _pd_proc_2theta_range_inc 0.01 _pd_proc_wavelength 1.5406 # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.7500 0.2500 0.4257(23) 0.043(7) Uiso 1 2 d S . . O1 O 1.1883(21) 0.1101(25) 0.4134(29) 0.065(5) Uiso 1 1 d . . . O2 O 1.4728(23) -0.0645(24) 0.3246(27) 0.065(5) Uiso 1 1 d . . . O3 O 1.3836(20) -0.1902(25) 0.3293(29) 0.065(5) Uiso 1 1 d . . . O4 O 1.4519(21) -0.2677(26) 0.4151(30) 0.065(5) Uiso 1 1 d . . . O5 O 1.6214(19) -0.1799(23) 0.4396(26) 0.065(5) Uiso 1 1 d . . . O6 O 1.6126(21) -0.0534(22) 0.3996(31) 0.065(5) Uiso 1 1 d . . . N1 N 0.8383(22) 0.3014(25) 0.3615(29) 0.065(5) Uiso 1 1 d . . . N2 N 0.8994(22) 0.2020(27) 0.4219(28) 0.065(5) Uiso 1 1 d . . . N3 N 0.7461(21) 0.1720(24) 0.4877(30) 0.065(5) Uiso 1 1 d . . . C1 C 0.8074(24) 0.3522(31) 0.3305(33) 0.065(5) Uiso 1 1 d . . . H1 H 0.7404 0.3692 0.3358 0.078 Uiso 1 1 calc . . . C2 C 0.8704(22) 0.3793(30) 0.2920(34) 0.065(5) Uiso 1 1 d . . . H2 H 0.8478 0.4137 0.2716 0.078 Uiso 1 1 calc . . . C3 C 0.9733(25) 0.3511(33) 0.2853(31) 0.065(5) Uiso 1 1 d . . . H3 H 1.0186 0.3676 0.2598 0.078 Uiso 1 1 calc . . . C4 C 1.0046(21) 0.3026(30) 0.3145(33) 0.065(5) Uiso 1 1 d . . . H4 H 1.0714 0.2851 0.3097 0.078 Uiso 1 1 calc . . . C5 C 0.9360(24) 0.2772(32) 0.3533(32) 0.065(5) Uiso 1 1 d . . . C6 C 0.9706(24) 0.2219(32) 0.3868(30) 0.065(5) Uiso 1 1 d . . . C7 C 1.0706(26) 0.1932(34) 0.3814(33) 0.065(5) Uiso 1 1 d . . . H7 H 1.1187 0.2080 0.3565 0.078 Uiso 1 1 calc . . . C8 C 1.0956(23) 0.1415(31) 0.4148(35) 0.065(5) Uiso 1 1 d . . . C9 C 1.0184(24) 0.1209(31) 0.4522(31) 0.065(5) Uiso 1 1 d . . . H9 H 1.0328 0.0869 0.4748 0.078 Uiso 1 1 calc . . . C10 C 0.9219(25) 0.1519(29) 0.4547(32) 0.065(5) Uiso 1 1 d . . . C11 C 0.8333(22) 0.1357(33) 0.4918(35) 0.065(5) Uiso 1 1 d . . . C12 C 0.8386(27) 0.0864(32) 0.5287(34) 0.065(5) Uiso 1 1 d . . . H12 H 0.8990 0.0613 0.5315 0.078 Uiso 1 1 calc . . . C13 C 0.7514(23) 0.0751(34) 0.5616(33) 0.065(5) Uiso 1 1 d . . . H13 H 0.7536 0.0423 0.5865 0.078 Uiso 1 1 calc . . . C14 C 0.6616(24) 0.1131(31) 0.5569(31) 0.065(5) Uiso 1 1 d . . . H14 H 0.6030 0.1065 0.5783 0.078 Uiso 1 1 calc . . . C15 C 0.6629(25) 0.1611(30) 0.5192(36) 0.065(5) Uiso 1 1 d . . . H15 H 0.6036 0.1869 0.5155 0.078 Uiso 1 1 calc . . . C16 C 1.2816(27) 0.1304(32) 0.3832(32) 0.065(5) Uiso 1 1 d . . . H16A H 1.3044 0.1721 0.3955 0.078 Uiso 1 1 calc . . . H16B H 1.2631 0.1342 0.3461 0.078 Uiso 1 1 calc . . . C17 C 1.3705(24) 0.0834(33) 0.3892(34) 0.065(5) Uiso 1 1 d . . . C18 C 1.3784(23) 0.0313(31) 0.3530(33) 0.065(5) Uiso 1 1 d . . . H18 H 1.3274 0.0260 0.3270 0.078 Uiso 1 1 calc . . . C19 C 1.4621(22) -0.0117(35) 0.3564(35) 0.065(5) Uiso 1 1 d . . . C20 C 1.5349(24) -0.0073(32) 0.3996(35) 0.065(5) Uiso 1 1 d . . . C21 C 1.5258(26) 0.0423(30) 0.4349(32) 0.065(5) Uiso 1 1 d . . . H21 H 1.5724 0.0451 0.4632 0.078 Uiso 1 1 calc . . . C22 C 1.4451(26) 0.0899(30) 0.4286(31) 0.065(5) Uiso 1 1 d . . . H22 H 1.4431 0.1251 0.4511 0.078 Uiso 1 1 calc . . . C23 C 1.3765(27) -0.0836(34) 0.2946(33) 0.065(5) Uiso 1 1 d . . . H23A H 1.3140 -0.0768 0.3159 0.078 Uiso 1 1 calc . . . H23B H 1.3702 -0.0583 0.2626 0.078 Uiso 1 1 calc . . . C24 C 1.3876(22) -0.1516(32) 0.2815(32) 0.065(5) Uiso 1 1 d . . . H24A H 1.3312 -0.1644 0.2578 0.078 Uiso 1 1 calc . . . H24B H 1.4542 -0.1586 0.2636 0.078 Uiso 1 1 calc . . . C25 C 1.4415(28) -0.2508(31) 0.3190(34) 0.065(5) Uiso 1 1 d . . . H25A H 1.5172 -0.2440 0.3191 0.078 Uiso 1 1 calc . . . H25B H 1.4208 -0.2695 0.2855 0.078 Uiso 1 1 calc . . . C26 C 1.4064(23) -0.2942(33) 0.3668(30) 0.065(5) Uiso 1 1 d . . . H26A H 1.3301 -0.2949 0.3694 0.078 Uiso 1 1 calc . . . H26B H 1.4310 -0.3377 0.3615 0.078 Uiso 1 1 calc . . . C27 C 1.5690(26) -0.2857(33) 0.4143(33) 0.065(5) Uiso 1 1 d . . . H27A H 1.6017 -0.2767 0.3805 0.078 Uiso 1 1 calc . . . H27B H 1.5806 -0.3301 0.4238 0.078 Uiso 1 1 calc . . . C28 C 1.6060(24) -0.2390(31) 0.4580(36) 0.065(5) Uiso 1 1 d . . . H28A H 1.5534 -0.2377 0.4858 0.078 Uiso 1 1 calc . . . H28B H 1.6712 -0.2548 0.4732 0.078 Uiso 1 1 calc . . . C29 C 1.7037(25) -0.1401(35) 0.4441(37) 0.065(5) Uiso 1 1 d . . . H29A H 1.7497 -0.1450 0.4137 0.078 Uiso 1 1 calc . . . H29B H 1.7437 -0.1507 0.4756 0.078 Uiso 1 1 calc . . . C30 C 1.6648(27) -0.0697(34) 0.4476(35) 0.065(5) Uiso 1 1 d . . . H30A H 1.6167 -0.0650 0.4771 0.078 Uiso 1 1 calc . . . H30B H 1.7243 -0.0413 0.4532 0.078 Uiso 1 1 calc . . . P1 P 0.9518(17) -0.0108(20) 0.3457(21) 0.079(9) Uiso 1 1 d . . . F11 F 0.8740(18) 0.0446(22) 0.3561(23) 0.151(12) Uiso 1 1 d . . . F12 F 1.0262(19) -0.0699(21) 0.3329(20) 0.151(12) Uiso 1 1 d . . . F13 F 0.9880(18) -0.0114(20) 0.4036(21) 0.151(12) Uiso 1 1 d . . . F14 F 1.0399(20) 0.0361(22) 0.3290(23) 0.151(12) Uiso 1 1 d . . . F15 F 0.9142(17) -0.0156(22) 0.2856(22) 0.151(12) Uiso 1 1 d . . . F16 F 0.8596(18) -0.0605(20) 0.3599(21) 0.151(12) Uiso 1 1 d . . . O1W O 0.2500 0.2500 0.2749(24) 0.096(10) Uiso 1 2 d S . . H1W H 0.2448 0.2170 0.2553 0.096 Uiso 1 1 d . . . O2W O 0.1831(18) 0.1208(23) 0.2399(25) 0.120(12) Uiso 1 1 d . . . H2W1 H 0.1187 0.1113 0.2347 0.120 Uiso 1 1 d . . . H2W2 H 0.2233 0.0887 0.2361 0.120 Uiso 1 1 d . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Zn N1 2.25(4) . ? Zn N2 2.14(3) . ? Zn N3 2.26(5) . ? Zn N1 2.25(4) 2_655 ? Zn N2 2.14(3) 2_655 ? Zn N3 2.26(5) 2_655 ? P1 F15 1.59(7) . ? P1 F16 1.59(5) . ? P1 F12 1.59(5) . ? P1 F13 1.54(7) . ? P1 F11 1.55(5) . ? P1 F14 1.55(5) . ? O1 C16 1.47(7) . ? O1 C8 1.34(5) . ? O2 C23 1.49(7) . ? O2 C19 1.35(10) . ? O3 C24 1.43(10) . ? O3 C25 1.49(7) . ? O4 C26 1.45(9) . ? O4 C27 1.53(5) . ? O5 C29 1.34(6) . ? O5 C28 1.33(8) . ? O6 C20 1.38(6) . ? O6 C30 1.43(11) . ? O1W H1W 0.85 . ? O2W H2W2 0.85 . ? O2W H2W1 0.85 . ? N1 C5 1.36(4) . ? N1 C1 1.37(7) . ? N2 C6 1.34(6) . ? N2 C10 1.37(7) . ? N3 C15 1.34(7) . ? N3 C11 1.34(5) . ? C1 C2 1.39(9) . ? C2 C3 1.44(5) . ? C3 C4 1.32(9) . ? C4 C5 1.41(8) . ? C5 C6 1.50(9) . ? C6 C7 1.41(6) . ? C7 C8 1.42(10) . ? C8 C9 1.42(9) . ? C9 C10 1.38(5) . ? C10 C11 1.50(9) . ? C11 C12 1.40(11) . ? C12 C13 1.41(7) . ? C13 C14 1.39(6) . ? C14 C15 1.39(11) . ? C16 C17 1.49(7) . ? C17 C18 1.42(10) . ? C17 C22 1.40(8) . ? C18 C19 1.40(6) . ? C19 C20 1.45(11) . ? C20 C21 1.36(11) . ? C21 C22 1.44(7) . ? C23 C24 1.46(9) . ? C25 C26 1.57(10) . ? C27 C28 1.56(11) . ? C29 C30 1.55(9) . ? C1 H1 0.93 . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 H4 0.93 . ? C7 H7 0.93 . ? C9 H9 0.93 . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 H16B 0.97 . ? C16 H16A 0.97 . ? C18 H18 0.93 . ? C21 H21 0.93 . ? C22 H22 0.93 . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 H24B 0.97 . ? C24 H24A 0.97 . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 H27B 0.97 . ? C27 H27A 0.97 . ? C28 H28B 0.97 . ? C28 H28A 0.96 . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 H30B 0.97 . ? C30 H30A 0.97 . ? 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 N1 Zn N2 75.4(14) . . ? N1 Zn N3 148.9(11) . . ? N1 Zn N1 87(2) . 2_655 ? N1 Zn N2 100.4(16) . 2_655 ? N1 Zn N3 98.6(11) . 2_655 ? N2 Zn N3 73.5(12) . . ? N1 Zn N2 100.4(16) 2_655 . ? N2 Zn N2 174(3) . 2_655 ? N2 Zn N3 110.6(16) . 2_655 ? N1 Zn N3 98.6(11) 2_655 . ? N2 Zn N3 110.6(16) 2_655 . ? N3 Zn N3 92(2) . 2_655 ? N1 Zn N2 75.4(14) 2_655 2_655 ? N1 Zn N3 148.9(11) 2_655 2_655 ? N2 Zn N3 73.5(12) 2_655 2_655 ? F13 P1 F15 176(4) . . ? F13 P1 F16 90(3) . . ? F14 P1 F15 90(3) . . ? F14 P1 F16 177(5) . . ? F15 P1 F16 87(3) . . ? F11 P1 F12 176(4) . . ? F11 P1 F13 92(3) . . ? F11 P1 F14 92(3) . . ? F11 P1 F15 91(3) . . ? F11 P1 F16 89(2) . . ? F12 P1 F13 91(3) . . ? F12 P1 F14 90(2) . . ? F12 P1 F15 86(3) . . ? F12 P1 F16 89(3) . . ? F13 P1 F14 93(3) . . ? C8 O1 C16 126(6) . . ? C19 O2 C23 116(3) . . ? C24 O3 C25 108(6) . . ? C26 O4 C27 106(5) . . ? C28 O5 C29 132(5) . . ? C20 O6 C30 120(7) . . ? H2W1 O2W H2W2 111.53 . . ? Zn N1 C5 113(4) . . ? Zn N1 C1 129(2) . . ? C1 N1 C5 117(4) . . ? C6 N2 C10 120(4) . . ? Zn N2 C6 119(3) . . ? Zn N2 C10 121(2) . . ? C11 N3 C15 120(5) . . ? Zn N3 C11 116(4) . . ? Zn N3 C15 123(3) . . ? N1 C1 C2 123(4) . . ? C1 C2 C3 116(6) . . ? C2 C3 C4 121(5) . . ? C3 C4 C5 120(4) . . ? C4 C5 C6 120(4) . . ? N1 C5 C4 122(5) . . ? N1 C5 C6 118(5) . . ? C5 C6 C7 122(5) . . ? N2 C6 C5 115(3) . . ? N2 C6 C7 123(6) . . ? C6 C7 C8 118(5) . . ? O1 C8 C9 119(6) . . ? O1 C8 C7 123(6) . . ? C7 C8 C9 118(4) . . ? C8 C9 C10 121(6) . . ? N2 C10 C9 121(5) . . ? C9 C10 C11 126(6) . . ? N2 C10 C11 113(4) . . ? N3 C11 C12 121(5) . . ? N3 C11 C10 116(6) . . ? C10 C11 C12 123(4) . . ? C11 C12 C13 118(4) . . ? C12 C13 C14 120(6) . . ? C13 C14 C15 118(5) . . ? N3 C15 C14 123(4) . . ? O1 C16 C17 111(5) . . ? C16 C17 C18 119(5) . . ? C16 C17 C22 121(6) . . ? C18 C17 C22 120(4) . . ? C17 C18 C19 121(6) . . ? O2 C19 C18 125(6) . . ? C18 C19 C20 119(7) . . ? O2 C19 C20 116(5) . . ? O6 C20 C19 114(7) . . ? O6 C20 C21 126(6) . . ? C19 C20 C21 120(5) . . ? C20 C21 C22 121(6) . . ? C17 C22 C21 119(6) . . ? O2 C23 C24 108(4) . . ? O3 C24 C23 110(6) . . ? O3 C25 C26 103(5) . . ? O4 C26 C25 109(4) . . ? O4 C27 C28 97(4) . . ? O5 C28 C27 113(8) . . ? O5 C29 C30 110(3) . . ? O6 C30 C29 109(7) . . ? N1 C1 H1 119 . . ? C2 C1 H1 117 . . ? C3 C2 H2 121 . . ? C1 C2 H2 122 . . ? C2 C3 H3 119 . . ? C4 C3 H3 119 . . ? C5 C4 H4 120 . . ? C3 C4 H4 119 . . ? C6 C7 H7 121 . . ? C8 C7 H7 121 . . ? C8 C9 H9 119 . . ? C10 C9 H9 120 . . ? C11 C12 H12 120 . . ? C13 C12 H12 121 . . ? C12 C13 H13 119 . . ? C14 C13 H13 120 . . ? C13 C14 H14 121 . . ? C15 C14 H14 120 . . ? N3 C15 H15 118 . . ? C14 C15 H15 118 . . ? O1 C16 H16A 108 . . ? O1 C16 H16B 108 . . ? C17 C16 H16A 109 . . ? H16A C16 H16B 107 . . ? C17 C16 H16B 110 . . ? C17 C18 H18 119 . . ? C19 C18 H18 119 . . ? C22 C21 H21 118 . . ? C20 C21 H21 120 . . ? C17 C22 H22 120 . . ? C21 C22 H22 120 . . ? O2 C23 H23B 110 . . ? O2 C23 H23A 110 . . ? H23A C23 H23B 107 . . ? C24 C23 H23A 110 . . ? C24 C23 H23B 110 . . ? O3 C24 H24A 110 . . ? C23 C24 H24B 109 . . ? O3 C24 H24B 110 . . ? C23 C24 H24A 109 . . ? H24A C24 H24B 107 . . ? O3 C25 H25B 111 . . ? C26 C25 H25A 111 . . ? C26 C25 H25B 111 . . ? H25A C25 H25B 108 . . ? O3 C25 H25A 110 . . ? O4 C26 H26A 110 . . ? O4 C26 H26B 109 . . ? C25 C26 H26B 109 . . ? H26A C26 H26B 108 . . ? C25 C26 H26A 109 . . ? O4 C27 H27A 112 . . ? C28 C27 H27A 111 . . ? C28 C27 H27B 111 . . ? O4 C27 H27B 112 . . ? H27A C27 H27B 110 . . ? C27 C28 H28A 109 . . ? C27 C28 H28B 109 . . ? H28A C28 H28B 107 . . ? O5 C28 H28B 109 . . ? O5 C28 H28A 108 . . ? C30 C29 H29A 110 . . ? O5 C29 H29A 109 . . ? O5 C29 H29B 108 . . ? H29A C29 H29B 108 . . ? C30 C29 H29B 109 . . ? O6 C30 H30B 108 . . ? O6 C30 H30A 109 . . ? H30A C30 H30B 108 . . ? C29 C30 H30A 110 . . ? C29 C30 H30B 110 . . ? _refine_diff_density_max 0.744 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.220 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 692439' # start Validation Reply Form _vrf_PLAT341_5 ; PROBLEM: Low Bond Precision on C-C Bonds (x 1000) Ang ... 84 RESPONSE: This is a powder diffraction study. All structural parameters were refined with the laboratory powder diffraction data. ; _vrf_PLAT410_5 ; PROBLEM: Short Intra H...H Contact H21B .. H30D .. 1.76 Ang. RESPONSE: This crystal structure has been determined and refined with the laboratory powder diffraction data, so all H-atoms were geometrically positioned and not refined. ; # end Validation Reply Form _audit_creation_method manual _chemical_name_systematic ; Bis[4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''-terpyridine] cobalt(II) bis(thiocyanate) ; _chemical_name_common ; Bis(4'-(4'''-benzo-15-crown-5)-methyloxy-2,2':6',2''- terpyridine) cobalt(ii) bis(thiocyanate) ; _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Co N6 O12, 2 (C N S)' _chemical_formula_sum 'C62 H62 Co N8 O12 S2' _chemical_formula_weight 1234.25 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.654(2) _cell_length_b 16.644(4) _cell_length_c 8.9540(11) _cell_angle_alpha 94.66(2) _cell_angle_beta 101.42(2) _cell_angle_gamma 78.65(2) _cell_volume 1524.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1859 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 40.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 645 _exptl_absorpt_coefficient_mu 3.410 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 1 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; ? ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology prism _pd_char_colour brown # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia ; _diffrn_ambient_temperature 295(2) _diffrn_source 'Fine focus X-ray tube' _diffrn_source_target Cu _diffrn_radiation_source 'line-focus sealed tube' _diffrn_radiation_monochromator 'Curved Germanium (111)' _diffrn_measurement_device 'Guinier camera G670' _diffrn_detector_type 'Imaging Plate' _diffrn_reflns_number ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_type CuK\a~1~ _diffrn_radiation_wavelength 1.5406 # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7601 _pd_meas_2theta_range_min 4.00 _pd_meas_2theta_range_max 80.00 _pd_meas_2theta_range_inc 0.01 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'local program' _computing_cell_refinement 'MRIA (Zlokazov & Chernyshev, 1992)' _computing_data_reduction 'local program' _computing_structure_solution 'FOX (Favre-Nicolin & Cerny, 2002) and MRIA' _computing_structure_refinement MRIA _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ; MRIA, SHELXL97 (Sheldrick, 1997) ; #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function 'split-type pseudo-Voigt (Toraya, 1986)' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_background_function 'Chebyshev polynomial up to the 5th order' _pd_proc_ls_prof_R_factor 0.0072 _pd_proc_ls_prof_wR_factor 0.0095 _pd_proc_ls_prof_wR_expected 0.0071 _refine_special_details ; ? ; _refine_ls_R_I_factor ? _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 285 _refine_ls_number_restraints 290 _refine_ls_number_constraints 83 # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.3442 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .004 _refine_ls_shift/su_mean .001 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.00 _pd_proc_2theta_range_max 80.00 _pd_proc_2theta_range_inc 0.01 _pd_proc_wavelength 1.5406 # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.5000 0.5000 0.5000 0.044(9) Uiso 1 1 d . . . O1A O 0.9128(45) 0.7051(29) 0.5562(48) 0.061(11) Uiso 1 1 d . . . O2A O 1.1610(47) 0.9356(30) 0.4313(49) 0.061(11) Uiso 1 1 d . . . O3A O 1.1290(43) 0.9094(28) 0.1083(46) 0.061(11) Uiso 1 1 d . . . O4A O 1.4074(41) 0.9498(27) 0.1500(50) 0.061(11) Uiso 1 1 d . . . O5A O 1.6288(44) 0.8686(32) 0.4081(47) 0.061(11) Uiso 1 1 d . . . O6A O 1.3942(46) 0.8938(29) 0.5917(49) 0.061(11) Uiso 1 1 d . . . N1A N 0.6611(48) 0.4181(32) 0.6327(51) 0.061(11) Uiso 1 1 d . . . N2A N 0.6395(45) 0.5599(33) 0.5279(49) 0.061(11) Uiso 1 1 d . . . N3A N 0.3934(49) 0.6030(34) 0.3845(52) 0.061(11) Uiso 1 1 d . . . C1A C 0.6563(49) 0.3446(33) 0.6780(52) 0.061(11) Uiso 1 1 d . . . H1A H 0.5787 0.3248 0.6535 0.073 Uiso 1 1 calc . . . C2A C 0.7646(50) 0.2978(34) 0.7604(58) 0.061(11) Uiso 1 1 d . . . H2A H 0.7607 0.2464 0.7910 0.073 Uiso 1 1 calc . . . C3A C 0.8804(46) 0.3281(37) 0.7978(54) 0.061(11) Uiso 1 1 d . . . H3A H 0.9541 0.2971 0.8546 0.073 Uiso 1 1 calc . . . C4A C 0.8858(52) 0.4050(35) 0.7500(59) 0.061(11) Uiso 1 1 d . . . H4A H 0.9626 0.4258 0.7730 0.073 Uiso 1 1 calc . . . C5A C 0.7732(50) 0.4493(36) 0.6672(61) 0.061(11) Uiso 1 1 d . . . C6A C 0.7619(53) 0.5328(33) 0.6070(58) 0.061(11) Uiso 1 1 d . . . C7A C 0.8599(55) 0.5801(32) 0.6205(54) 0.061(11) Uiso 1 1 d . . . H7A H 0.9434 0.5615 0.6743 0.073 Uiso 1 1 calc . . . C8A C 0.8289(49) 0.6560(35) 0.5509(57) 0.061(11) Uiso 1 1 d . . . C9A C 0.6985(52) 0.6834(37) 0.4713(62) 0.061(11) Uiso 1 1 d . . . H9A H 0.6764 0.7334 0.4242 0.073 Uiso 1 1 calc . . . C10A C 0.6070(50) 0.6355(34) 0.4652(59) 0.061(11) Uiso 1 1 d . . . C11A C 0.4701(49) 0.6586(35) 0.3856(58) 0.061(11) Uiso 1 1 d . . . C12A C 0.4191(54) 0.7298(31) 0.3104(63) 0.061(11) Uiso 1 1 d . . . H12A H 0.4718 0.7677 0.3069 0.073 Uiso 1 1 calc . . . C13A C 0.2888(52) 0.7453(37) 0.2395(58) 0.061(11) Uiso 1 1 d . . . H13A H 0.2540 0.7936 0.1890 0.073 Uiso 1 1 calc . . . C14A C 0.2111(50) 0.6881(34) 0.2447(57) 0.061(11) Uiso 1 1 d . . . H14A H 0.1234 0.6974 0.1992 0.073 Uiso 1 1 calc . . . C15A C 0.2675(51) 0.6178(30) 0.3187(60) 0.061(11) Uiso 1 1 d . . . H15A H 0.2167 0.5789 0.3235 0.073 Uiso 1 1 calc . . . C16A C 1.0020(52) 0.7291(36) 0.6810(63) 0.061(11) Uiso 1 1 d . . . H16A H 1.0454 0.6804 0.7361 0.073 Uiso 1 1 calc . . . H16B H 0.9527 0.7648 0.7486 0.073 Uiso 1 1 calc . . . C17A C 1.1035(49) 0.7713(37) 0.6514(62) 0.061(11) Uiso 1 1 d . . . C18A C 1.0762(50) 0.8374(33) 0.5527(59) 0.061(11) Uiso 1 1 d . . . H18A H 0.9906 0.8582 0.5082 0.073 Uiso 1 1 calc . . . C19A C 1.1785(53) 0.8715(36) 0.5221(63) 0.061(11) Uiso 1 1 d . . . C20A C 1.3086(48) 0.8463(33) 0.6035(59) 0.061(11) Uiso 1 1 d . . . C21A C 1.3361(51) 0.7781(34) 0.6952(60) 0.061(11) Uiso 1 1 d . . . H21A H 1.4219 0.7541 0.7329 0.073 Uiso 1 1 calc . . . C22A C 1.2334(50) 0.7467(36) 0.7292(58) 0.061(11) Uiso 1 1 d . . . H22A H 1.2506 0.7087 0.8047 0.073 Uiso 1 1 calc . . . C23A C 1.0365(49) 0.9562(35) 0.3263(59) 0.061(11) Uiso 1 1 d . . . H23A H 0.9799 1.0017 0.3682 0.073 Uiso 1 1 calc . . . H23B H 0.9928 0.9095 0.3066 0.073 Uiso 1 1 calc . . . C24A C 1.0712(54) 0.9797(34) 0.1806(57) 0.061(11) Uiso 1 1 d . . . H24A H 0.9931 1.0058 0.1139 0.073 Uiso 1 1 calc . . . H24B H 1.1308 1.0181 0.2050 0.073 Uiso 1 1 calc . . . C25A C 1.2007(51) 0.9069(47) -0.0001(61) 0.061(11) Uiso 1 1 d . . . H25A H 1.1413 0.9235 -0.0939 0.073 Uiso 1 1 calc . . . H25B H 1.2407 0.8501 -0.0166 0.073 Uiso 1 1 calc . . . C26A C 1.3046(52) 0.9562(44) 0.0237(62) 0.061(11) Uiso 1 1 d . . . H26A H 1.3444 0.9459 -0.0662 0.073 Uiso 1 1 calc . . . H26B H 1.2613 1.0132 0.0227 0.073 Uiso 1 1 calc . . . C27A C 1.5178(48) 0.8915(43) 0.1492(58) 0.061(11) Uiso 1 1 d . . . H27A H 1.5432 0.8891 0.0505 0.073 Uiso 1 1 calc . . . H27B H 1.4995 0.8383 0.1647 0.073 Uiso 1 1 calc . . . C28A C 1.6318(54) 0.9104(47) 0.2751(59) 0.061(11) Uiso 1 1 d . . . H28A H 1.7142 0.8914 0.2414 0.073 Uiso 1 1 calc . . . H28B H 1.6221 0.9690 0.2980 0.073 Uiso 1 1 calc . . . C29A C 1.5896(51) 0.9064(54) 0.5273(57) 0.061(11) Uiso 1 1 d . . . H29A H 1.5244 0.9539 0.4929 0.073 Uiso 1 1 calc . . . H29B H 1.6630 0.9268 0.5898 0.073 Uiso 1 1 calc . . . C30A C 1.5333(53) 0.8613(45) 0.6289(62) 0.061(11) Uiso 1 1 d . . . H30A H 1.5516 0.8026 0.6068 0.073 Uiso 1 1 calc . . . H30B H 1.5677 0.8725 0.7356 0.073 Uiso 1 1 calc . . . O1B O 0.0407(46) 0.3222(37) 0.3626(49) 0.061(11) Uiso 1 1 d . . . O2B O -0.3579(44) 0.1053(37) 0.3546(52) 0.061(11) Uiso 1 1 d . . . O3B O -0.6152(47) 0.1299(39) 0.4062(48) 0.061(11) Uiso 1 1 d . . . O4B O -0.5865(48) 0.1031(40) 0.7350(50) 0.061(11) Uiso 1 1 d . . . O5B O -0.2745(44) 0.0691(39) 0.8813(54) 0.061(11) Uiso 1 1 d . . . O6B O -0.1931(46) 0.0345(42) 0.5935(51) 0.061(11) Uiso 1 1 d . . . N1B N 0.4031(44) 0.5314(38) 0.7067(55) 0.061(11) Uiso 1 1 d . . . N2B N 0.3516(48) 0.4427(43) 0.4598(53) 0.061(11) Uiso 1 1 d . . . N3B N 0.5182(49) 0.4384(42) 0.2838(52) 0.061(11) Uiso 1 1 d . . . C1B C 0.4362(50) 0.5792(48) 0.8294(59) 0.061(11) Uiso 1 1 d . . . H1B H 0.5077 0.6044 0.8356 0.073 Uiso 1 1 calc . . . C2B C 0.3674(53) 0.5925(49) 0.9479(57) 0.061(11) Uiso 1 1 d . . . H2B H 0.3945 0.6248 1.0334 0.073 Uiso 1 1 calc . . . C3B C 0.2570(49) 0.5573(45) 0.9387(62) 0.061(11) Uiso 1 1 d . . . H3B H 0.2103 0.5658 1.0178 0.073 Uiso 1 1 calc . . . C4B C 0.2185(52) 0.5100(47) 0.8112(58) 0.061(11) Uiso 1 1 d . . . H4B H 0.1436 0.4876 0.8001 0.073 Uiso 1 1 calc . . . C5B C 0.2963(55) 0.4965(51) 0.6975(62) 0.061(11) Uiso 1 1 d . . . C6B C 0.2666(56) 0.4454(49) 0.5565(58) 0.061(11) Uiso 1 1 d . . . C7B C 0.1605(51) 0.4073(48) 0.5303(64) 0.061(11) Uiso 1 1 d . . . H7B H 0.1076 0.4119 0.6029 0.073 Uiso 1 1 calc . . . C8B C 0.1322(48) 0.3611(53) 0.3927(57) 0.061(11) Uiso 1 1 d . . . C9B C 0.2232(54) 0.3573(49) 0.2922(61) 0.061(11) Uiso 1 1 d . . . H9B H 0.2115 0.3268 0.2004 0.073 Uiso 1 1 calc . . . C10B C 0.3259(52) 0.3970(47) 0.3274(58) 0.061(11) Uiso 1 1 d . . . C11B C 0.4254(54) 0.3936(49) 0.2297(55) 0.061(11) Uiso 1 1 d . . . C12B C 0.4219(49) 0.3502(50) 0.0880(58) 0.061(11) Uiso 1 1 d . . . H12B H 0.3581 0.3189 0.0514 0.073 Uiso 1 1 calc . . . C13B C 0.5161(51) 0.3554(48) 0.0044(54) 0.061(11) Uiso 1 1 d . . . H13B H 0.5143 0.3291 -0.0915 0.073 Uiso 1 1 calc . . . C14B C 0.6144(53) 0.4005(46) 0.0646(60) 0.061(11) Uiso 1 1 d . . . H14B H 0.6798 0.4031 0.0110 0.073 Uiso 1 1 calc . . . C15B C 0.6120(49) 0.4405(50) 0.2036(64) 0.061(11) Uiso 1 1 d . . . H15B H 0.6772 0.4702 0.2443 0.073 Uiso 1 1 calc . . . C16B C -0.0809(50) 0.3107(53) 0.3515(57) 0.061(11) Uiso 1 1 d . . . H16C H -0.1230 0.3156 0.2453 0.073 Uiso 1 1 calc . . . H16D H -0.1258 0.3554 0.4088 0.073 Uiso 1 1 calc . . . C17B C -0.1029(53) 0.2323(51) 0.4035(58) 0.061(11) Uiso 1 1 d . . . C18B C -0.2212(55) 0.2044(49) 0.3489(62) 0.061(11) Uiso 1 1 d . . . H18B H -0.2785 0.2283 0.2651 0.073 Uiso 1 1 calc . . . C19B C -0.2531(47) 0.1410(53) 0.4199(60) 0.061(11) Uiso 1 1 d . . . C20B C -0.1620(52) 0.0994(50) 0.5365(55) 0.061(11) Uiso 1 1 d . . . C21B C -0.0423(56) 0.1276(49) 0.5922(63) 0.061(11) Uiso 1 1 d . . . H21B H 0.0146 0.1047 0.6772 0.073 Uiso 1 1 calc . . . C22B C -0.0120(51) 0.1886(54) 0.5195(61) 0.061(11) Uiso 1 1 d . . . H22B H 0.0707 0.2016 0.5474 0.073 Uiso 1 1 calc . . . C23B C -0.4654(52) 0.1630(48) 0.2659(59) 0.061(11) Uiso 1 1 d . . . H23C H -0.4666 0.2183 0.3101 0.073 Uiso 1 1 calc . . . H23D H -0.4528 0.1626 0.1615 0.073 Uiso 1 1 calc . . . C24B C -0.5866(54) 0.1379(52) 0.2689(66) 0.061(11) Uiso 1 1 d . . . H24C H -0.6565 0.1774 0.2143 0.073 Uiso 1 1 calc . . . H24D H -0.5868 0.0856 0.2125 0.073 Uiso 1 1 calc . . . C25B C -0.6048(49) 0.1959(54) 0.5214(58) 0.061(11) Uiso 1 1 d . . . H25C H -0.6538 0.2473 0.4798 0.073 Uiso 1 1 calc . . . H25D H -0.5143 0.2014 0.5537 0.073 Uiso 1 1 calc . . . C26B C -0.6580(53) 0.1766(49) 0.6553(62) 0.061(11) Uiso 1 1 d . . . H26C H -0.6585 0.2232 0.7278 0.073 Uiso 1 1 calc . . . H26D H -0.7477 0.1700 0.6198 0.073 Uiso 1 1 calc . . . C27B C -0.4766(56) 0.1238(52) 0.8414(61) 0.061(11) Uiso 1 1 d . . . H27C H -0.5071 0.1632 0.9183 0.073 Uiso 1 1 calc . . . H27D H -0.4247 0.1492 0.7882 0.073 Uiso 1 1 calc . . . C28B C -0.3941(54) 0.0498(50) 0.9168(65) 0.061(11) Uiso 1 1 d . . . H28C H -0.3936 0.0507 1.0254 0.073 Uiso 1 1 calc . . . H28D H -0.4153 -0.0013 0.8679 0.073 Uiso 1 1 calc . . . C29B C -0.1909(51) -0.0066(48) 0.8447(62) 0.061(11) Uiso 1 1 d . . . H29C H -0.2441 -0.0463 0.7979 0.073 Uiso 1 1 calc . . . H29D H -0.1368 -0.0289 0.9378 0.073 Uiso 1 1 calc . . . C30B C -0.1075(55) 0.0066(49) 0.7405(63) 0.061(11) Uiso 1 1 d . . . H30C H -0.0482 -0.0440 0.7228 0.073 Uiso 1 1 calc . . . H30D H -0.0564 0.0478 0.7844 0.073 Uiso 1 1 calc . . . S1 S 0.7269(39) 0.6828(35) 0.0399(42) 0.055(10) Uiso 1 1 d . . . C1 C 0.8362(53) 0.6009(46) 0.0918(59) 0.055(10) Uiso 1 1 d . . . N1 N 0.9122(50) 0.5440(44) 0.1278(56) 0.055(10) Uiso 1 1 d . . . S2 S 0.1434(38) 0.1626(36) 1.0105(44) 0.087(12) Uiso 1 1 d . . . C2 C 0.1554(56) 0.2524(47) 0.9584(61) 0.087(12) Uiso 1 1 d . . . N2 N 0.1637(54) 0.3149(48) 0.9221(57) 0.087(12) Uiso 1 1 d . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Co N1A 2.18(5) . ? Co N1B 2.27(6) . ? Co N2A 1.92(5) . ? Co N2B 1.96(6) . ? Co N3A 2.09(5) . ? Co N3B 2.14(6) . ? S1 C1 1.64(10) . ? S2 C2 1.62(10) . ? O1A C16A 1.40(7) . ? O1A C8A 1.32(7) . ? O1B C8B 1.24(9) . ? O1B C16B 1.33(8) . ? O2A C19A 1.35(8) . ? O2A C23A 1.47(7) . ? O2B C23B 1.48(9) . ? O2B C19B 1.38(8) . ? O3A C25A 1.34(7) . ? O3A C24A 1.40(7) . ? O3B C24B 1.34(8) . ? O3B C25B 1.45(9) . ? O4A C26A 1.40(7) . ? O4A C27A 1.38(8) . ? O4B C27B 1.43(8) . ? O4B C26B 1.47(10) . ? O5A C29A 1.29(8) . ? O5A C28A 1.43(8) . ? O5B C29B 1.45(10) . ? O5B C28B 1.47(7) . ? O6A C30A 1.46(8) . ? O6A C20A 1.34(7) . ? O6B C30B 1.48(7) . ? O6B C20B 1.36(9) . ? N1A C1A 1.32(7) . ? N1A C5A 1.36(8) . ? N1B C5B 1.36(8) . ? N1B C1B 1.33(8) . ? N2A C6A 1.36(7) . ? N2A C10A 1.38(7) . ? N2B C6B 1.37(8) . ? N2B C10B 1.37(8) . ? N3A C15A 1.33(8) . ? N3A C11A 1.35(8) . ? N3B C15B 1.35(8) . ? N3B C11B 1.34(8) . ? N1 C1 1.14(10) . ? N2 C2 1.15(11) . ? C1A C2A 1.38(7) . ? C1B C2B 1.39(8) . ? C2A C3A 1.38(8) . ? C2B C3B 1.39(8) . ? C3A C4A 1.40(9) . ? C3B C4B 1.37(8) . ? C4A C5A 1.39(8) . ? C4B C5B 1.41(8) . ? C5A C6A 1.51(8) . ? C5B C6B 1.47(9) . ? C6A C7A 1.40(8) . ? C6B C7B 1.37(9) . ? C7A C8A 1.41(8) . ? C7B C8B 1.41(9) . ? C8A C9A 1.44(8) . ? C8B C9B 1.44(8) . ? C9A C10A 1.35(8) . ? C9B C10B 1.36(9) . ? C10A C11A 1.48(8) . ? C10B C11B 1.48(8) . ? C11A C12A 1.37(8) . ? C11B C12B 1.41(8) . ? C12A C13A 1.39(8) . ? C12B C13B 1.38(8) . ? C13A C14A 1.39(8) . ? C13B C14B 1.40(9) . ? C14A C15A 1.36(7) . ? C14B C15B 1.36(8) . ? C16A C17A 1.48(8) . ? C16B C17B 1.50(11) . ? C17A C22A 1.41(8) . ? C17A C18A 1.41(8) . ? C17B C18B 1.41(8) . ? C17B C22B 1.41(9) . ? C18A C19A 1.42(8) . ? C18B C19B 1.40(10) . ? C19A C20A 1.43(8) . ? C19B C20B 1.40(9) . ? C14A H14A 0.93 . ? C14B H14B 0.93 . ? C15A H15A 0.93 . ? C15B H15B 0.93 . ? C16A H16B 0.97 . ? C16A H16A 0.97 . ? C16B H16C 0.97 . ? C16B H16D 0.97 . ? C18A H18A 0.93 . ? C18B H18B 0.93 . ? C21A H21A 0.93 . ? C21B H21B 0.93 . ? C22A H22A 0.93 . ? C22B H22B 0.93 . ? C23A H23A 0.97 . ? C23A H23B 0.97 . ? C23B H23D 0.97 . ? C23B H23C 0.97 . ? C24A H24A 0.97 . ? C24A H24B 0.97 . ? C24B H24D 0.97 . ? C24B H24C 0.97 . ? C25A H25A 0.97 . ? C25A H25B 0.97 . ? C25B H25C 0.97 . ? C25B H25D 0.97 . ? C26A H26A 0.97 . ? C26A H26B 0.97 . ? C26B H26D 0.97 . ? C26B H26C 0.97 . ? C27A H27A 0.97 . ? C27A H27B 0.97 . ? C27B H27D 0.97 . ? C27B H27C 0.97 . ? C28A H28B 0.97 . ? C28A H28A 0.97 . ? C28B H28D 0.97 . ? C28B H28C 0.97 . ? C29A H29A 0.97 . ? C29A H29B 0.97 . ? C29B H29C 0.97 . ? C29B H29D 0.97 . ? C30A H30B 0.97 . ? C30A H30A 0.97 . ? C30B H30C 0.97 . ? C30B H30D 0.97 . ? 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 N1A Co N1B 91(2) . . ? N1A Co N2A 77(2) . . ? N1A Co N2B 106(3) . . ? N1A Co N3A 161(3) . . ? N1A Co N3B 96(2) . . ? N1B Co N2A 107(3) . . ? N1B Co N2B 75(2) . . ? N1B Co N3A 94(2) . . ? N1B Co N3B 152(3) . . ? N2A Co N2B 176(3) . . ? N2A Co N3A 84(2) . . ? N2A Co N3B 101(3) . . ? N2B Co N3A 93(2) . . ? N2B Co N3B 78(2) . . ? N3A Co N3B 89(2) . . ? C8A O1A C16A 129(5) . . ? C8B O1B C16B 156(7) . . ? C19A O2A C23A 118(5) . . ? C19B O2B C23B 112(6) . . ? C24A O3A C25A 125(5) . . ? C24B O3B C25B 119(6) . . ? C26A O4A C27A 120(5) . . ? C26B O4B C27B 109(6) . . ? C28A O5A C29A 124(6) . . ? C28B O5B C29B 109(6) . . ? C20A O6A C30A 119(5) . . ? C20B O6B C30B 114(5) . . ? Co N1A C1A 125.77 . . ? Co N1A C5A 112.94 . . ? C1A N1A C5A 121(5) . . ? Co N1B C1B 128.32 . . ? Co N1B C5B 112.90 . . ? C1B N1B C5B 119(5) . . ? Co N2A C6A 124.26 . . ? Co N2A C10A 114.63 . . ? C6A N2A C10A 121(5) . . ? Co N2B C6B 124.60 . . ? Co N2B C10B 120.76 . . ? C6B N2B C10B 115(6) . . ? Co N3A C11A 109.84 . . ? Co N3A C15A 128.92 . . ? C11A N3A C15A 121(5) . . ? Co N3B C11B 113.83 . . ? Co N3B C15B 125.98 . . ? C11B N3B C15B 120(5) . . ? N1A C1A C2A 121(5) . . ? N1B C1B C2B 122(6) . . ? C1A C2A C3A 120(5) . . ? C1B C2B C3B 120(6) . . ? C2A C3A C4A 120(5) . . ? C2B C3B C4B 119(5) . . ? C3A C4A C5A 117(5) . . ? C3B C4B C5B 119(5) . . ? N1A C5A C4A 121(6) . . ? N1A C5A C6A 115(5) . . ? C4A C5A C6A 124(5) . . ? N1B C5B C4B 122(6) . . ? N1B C5B C6B 114(5) . . ? C4B C5B C6B 124(6) . . ? N2A C6A C5A 111(5) . . ? N2A C6A C7A 121(5) . . ? C5A C6A C7A 128(5) . . ? N2B C6B C5B 113(6) . . ? N2B C6B C7B 126(6) . . ? C5B C6B C7B 121(5) . . ? C6A C7A C8A 118(5) . . ? C6B C7B C8B 120(5) . . ? O1A C8A C7A 124(5) . . ? O1A C8A C9A 117(6) . . ? C7A C8A C9A 119(5) . . ? O1B C8B C7B 124(5) . . ? O1B C8B C9B 121(6) . . ? C7B C8B C9B 114(5) . . ? C8A C9A C10A 120(6) . . ? C8B C9B C10B 122(5) . . ? N2A C10A C9A 121(5) . . ? N2A C10A C11A 116(5) . . ? C9A C10A C11A 124(5) . . ? N2B C10B C9B 123(5) . . ? N2B C10B C11B 112(5) . . ? C9B C10B C11B 125(6) . . ? N3A C11A C10A 116(5) . . ? N3A C11A C12A 119(5) . . ? C10A C11A C12A 125(5) . . ? N3B C11B C10B 115(5) . . ? N3B C11B C12B 121(5) . . ? C10B C11B C12B 124(6) . . ? C11A C12A C13A 120(5) . . ? C11B C12B C13B 118(6) . . ? C12A C13A C14A 120(5) . . ? C12B C13B C14B 119(5) . . ? C13A C14A C15A 117(5) . . ? C13B C14B C15B 119(5) . . ? N3A C15A C14A 123(5) . . ? N3B C15B C14B 122(6) . . ? O1A C16A C17A 118(5) . . ? O1B C16B C17B 119(6) . . ? C16A C17A C18A 122(5) . . ? C16A C17A C22A 119(5) . . ? C18A C17A C22A 119(5) . . ? C16B C17B C18B 121(6) . . ? C16B C17B C22B 120(5) . . ? C18B C17B C22B 118(7) . . ? C17A C18A C19A 120(5) . . ? C17B C18B C19B 121(6) . . ? O2A C19A C18A 124(5) . . ? O2A C19A C20A 116(5) . . ? C18A C19A C20A 119(5) . . ? O2B C19B C18B 121(5) . . ? O2B C19B C20B 117(7) . . ? C18B C19B C20B 120(5) . . ? O6A C20A C19A 115(5) . . ? O6A C20A C21A 125(5) . . ? C19A C20A C21A 119(5) . . ? O6B C20B C19B 118(5) . . ? O6B C20B C21B 123(5) . . ? C19B C20B C21B 119(6) . . ? C20A C21A C22A 119(5) . . ? C20B C21B C22B 120(6) . . ? C17A C22A C21A 122(5) . . ? C17B C22B C21B 122(6) . . ? O2A C23A C24A 105(4) . . ? O2B C23B C24B 108(6) . . ? O3A C24A C23A 108(4) . . ? O3B C24B C23B 117(5) . . ? O3A C25A C26A 120(5) . . ? O3B C25B C26B 109(6) . . ? O4A C26A C25A 124(5) . . ? O4B C26B C25B 115(5) . . ? O4A C27A C28A 111(5) . . ? O4B C27B C28B 111(6) . . ? O5A C28A C27A 108(5) . . ? O5B C28B C27B 93(5) . . ? O5A C29A C30A 120(6) . . ? O5B C29B C30B 111(6) . . ? O6A C30A C29A 103(5) . . ? O6B C30B C29B 108(5) . . ? S1 C1 N1 180(8) . . ? S2 C2 N2 180(8) . . ? N1A C1A H1A 120 . . ? C2A C1A H1A 119 . . ? N1B C1B H1B 119 . . ? C2B C1B H1B 118 . . ? C1A C2A H2A 120 . . ? C3A C2A H2A 120 . . ? C1B C2B H2B 119 . . ? C3B C2B H2B 120 . . ? C2A C3A H3A 120 . . ? C4A C3A H3A 119 . . ? C2B C3B H3B 120 . . ? C4B C3B H3B 120 . . ? C3A C4A H4A 121 . . ? C5A C4A H4A 121 . . ? C3B C4B H4B 120 . . ? C5B C4B H4B 120 . . ? C6A C7A H7A 121 . . ? C8A C7A H7A 120 . . ? C6B C7B H7B 119 . . ? C8B C7B H7B 119 . . ? C8A C9A H9A 119 . . ? C10A C9A H9A 120 . . ? C8B C9B H9B 119 . . ? C10B C9B H9B 118 . . ? C11A C12A H12A 119 . . ? C13A C12A H12A 120 . . ? C11B C12B H12B 120 . . ? C13B C12B H12B 120 . . ? C12A C13A H13A 119 . . ? C14A C13A H13A 120 . . ? C12B C13B H13B 120 . . ? C14B C13B H13B 120 . . ? C13A C14A H14A 121 . . ? C15A C14A H14A 121 . . ? C13B C14B H14B 120 . . ? C15B C14B H14B 120 . . ? N3A C15A H15A 118 . . ? C14A C15A H15A 118 . . ? N3B C15B H15B 119 . . ? C14B C15B H15B 118 . . ? O1A C16A H16A 107 . . ? O1A C16A H16B 107 . . ? C17A C16A H16A 107 . . ? C17A C16A H16B 107 . . ? H16A C16A H16B 107 . . ? O1B C16B H16C 107 . . ? O1B C16B H16D 108 . . ? C17B C16B H16C 107 . . ? C17B C16B H16D 107 . . ? H16C C16B H16D 107 . . ? C17A C18A H18A 120 . . ? C19A C18A H18A 119 . . ? C17B C18B H18B 119 . . ? C19B C18B H18B 119 . . ? C20A C21A H21A 120 . . ? C22A C21A H21A 120 . . ? C20B C21B H21B 119 . . ? C22B C21B H21B 120 . . ? C17A C22A H22A 119 . . ? C21A C22A H22A 118 . . ? C17B C22B H22B 119 . . ? C21B C22B H22B 118 . . ? O2A C23A H23A 110 . . ? O2A C23A H23B 110 . . ? C24A C23A H23A 110 . . ? C24A C23A H23B 111 . . ? H23A C23A H23B 109 . . ? O2B C23B H23C 110 . . ? O2B C23B H23D 110 . . ? C24B C23B H23C 109 . . ? C24B C23B H23D 109 . . ? H23C C23B H23D 108 . . ? O3A C24A H24A 109 . . ? O3A C24A H24B 109 . . ? C23A C24A H24A 109 . . ? C23A C24A H24B 110 . . ? H24A C24A H24B 108 . . ? O3B C24B H24C 108 . . ? O3B C24B H24D 108 . . ? C23B C24B H24C 107 . . ? C23B C24B H24D 107 . . ? H24C C24B H24D 107 . . ? O3A C25A H25A 107 . . ? O3A C25A H25B 107 . . ? C26A C25A H25A 107 . . ? C26A C25A H25B 107 . . ? H25A C25A H25B 106 . . ? O3B C25B H25C 110 . . ? O3B C25B H25D 109 . . ? C26B C25B H25C 109 . . ? C26B C25B H25D 109 . . ? H25C C25B H25D 108 . . ? O4A C26A H26A 106 . . ? O4A C26A H26B 106 . . ? C25A C26A H26A 106 . . ? C25A C26A H26B 106 . . ? H26A C26A H26B 106 . . ? O4B C26B H26C 108 . . ? O4B C26B H26D 108 . . ? C25B C26B H26C 108 . . ? C25B C26B H26D 108 . . ? H26C C26B H26D 107 . . ? O4A C27A H27A 108 . . ? O4A C27A H27B 109 . . ? C28A C27A H27A 109 . . ? C28A C27A H27B 109 . . ? H27A C27A H27B 108 . . ? O4B C27B H27C 109 . . ? O4B C27B H27D 109 . . ? C28B C27B H27C 108 . . ? C28B C27B H27D 108 . . ? H27C C27B H27D 108 . . ? O5A C28A H28A 110 . . ? O5A C28A H28B 109 . . ? C27A C28A H28A 110 . . ? C27A C28A H28B 110 . . ? H28A C28A H28B 108 . . ? O5B C28B H28C 113 . . ? O5B C28B H28D 113 . . ? C27B C28B H28C 113 . . ? C27B C28B H28D 113 . . ? H28C C28B H28D 110 . . ? O5A C29A H29A 107 . . ? O5A C29A H29B 107 . . ? C30A C29A H29A 107 . . ? C30A C29A H29B 107 . . ? H29A C29A H29B 106 . . ? O5B C29B H29C 109 . . ? O5B C29B H29D 109 . . ? C30B C29B H29C 109 . . ? C30B C29B H29D 109 . . ? H29C C29B H29D 108 . . ? O6A C30A H30A 111 . . ? O6A C30A H30B 111 . . ? C29A C30A H30A 110 . . ? C29A C30A H30B 110 . . ? H30A C30A H30B 109 . . ? O6B C30B H30C 110 . . ? O6B C30B H30D 110 . . ? C29B C30B H30C 109 . . ? C29B C30B H30D 110 . . ? H30C C30B H30D 107 . . ? _refine_diff_density_max 0.97 _refine_diff_density_min -0.70 _refine_diff_density_rms 0.37 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 692440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [4'-(4'''-Benzo-15-crown-5-sodium thiocyanate)-methyloxy-2,2':6',2''- terpyridine] ; _chemical_name_common ; (4'-(4'''-Benzo-15-crown-5-sodium thiocyanate)-methyloxy- 2,2':6',2''-terpyridine) ; _chemical_melting_point ? _chemical_formula_moiety 'C31 H31 N4 Na O6 S' _chemical_formula_sum 'C31 H31 N4 Na O6 S' _chemical_formula_weight 610.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.643(3) _cell_length_b 9.4581(11) _cell_length_c 18.524(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.351(14) _cell_angle_gamma 90.00 _cell_volume 3081.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 27.18 _cell_measurement_theta_max 35.33 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details ? _exptl_special_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.215 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 6188 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 66.92 _reflns_number_total 5377 _reflns_number_gt 2296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.19P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5377 _refine_ls_number_parameters 388 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1566 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.1435(3) 0.3523(6) 0.1474(3) 0.0678(15) Uani 1 1 d . . . O2 O 0.3336(4) 0.1499(7) 0.4556(3) 0.0866(19) Uani 1 1 d . . . O3 O 0.3365(6) 0.0359(11) 0.5881(6) 0.164(4) Uani 1 1 d . . . O4 O 0.4109(5) 0.1991(11) 0.7045(5) 0.141(3) Uani 1 1 d . . . O5 O 0.4112(5) 0.4498(10) 0.6315(4) 0.136(3) Uani 1 1 d . . . O6 O 0.3790(3) 0.4106(6) 0.4830(3) 0.0730(16) Uani 1 1 d . . . N1 N 0.0990(5) 0.5356(9) -0.1168(4) 0.086(2) Uani 1 1 d D . . N2 N -0.0206(4) 0.2885(7) -0.0644(3) 0.0603(17) Uani 1 1 d . . . N3 N -0.0867(4) 0.0353(7) 0.0435(3) 0.0645(18) Uani 1 1 d . . . C1 C 0.1022(6) 0.5940(12) -0.1821(6) 0.102(3) Uani 1 1 d . . . H1 H 0.1421 0.6554 -0.1786 0.123 Uiso 1 1 calc R . . C2 C 0.0502(6) 0.5690(11) -0.2540(6) 0.099(3) Uani 1 1 d . . . H2 H 0.0563 0.6107 -0.2970 0.119 Uiso 1 1 calc R . . C3 C -0.0102(6) 0.4821(11) -0.2608(6) 0.091(3) Uani 1 1 d . . . H3 H -0.0463 0.4631 -0.3083 0.110 Uiso 1 1 calc R . . C4 C -0.0158(6) 0.4233(10) -0.1943(5) 0.078(2) Uani 1 1 d . . . H4 H -0.0570 0.3661 -0.1964 0.093 Uiso 1 1 calc R . . C5 C 0.0397(6) 0.4496(10) -0.1253(5) 0.072(2) Uani 1 1 d . . . C6 C 0.0374(5) 0.3785(9) -0.0552(4) 0.061(2) Uani 1 1 d . . . C7 C 0.0910(5) 0.4021(9) 0.0162(5) 0.067(2) Uani 1 1 d . . . H7 H 0.1294 0.4679 0.0213 0.080 Uiso 1 1 calc R . . C8 C 0.0883(5) 0.3295(9) 0.0796(4) 0.062(2) Uani 1 1 d . . . C9 C 0.0294(4) 0.2344(9) 0.0705(4) 0.059(2) Uani 1 1 d . . . H9 H 0.0260 0.1825 0.1119 0.071 Uiso 1 1 calc R . . C10 C -0.0255(4) 0.2181(8) -0.0032(4) 0.0565(19) Uani 1 1 d . . . C11 C -0.0895(4) 0.1182(8) -0.0155(4) 0.059(2) Uani 1 1 d . . . C12 C -0.1478(5) 0.1151(11) -0.0850(5) 0.082(3) Uani 1 1 d . . . H12 H -0.1494 0.1769 -0.1246 0.098 Uiso 1 1 calc R . . C13 C -0.2044(5) 0.0138(12) -0.0923(5) 0.092(3) Uani 1 1 d . . . H13 H -0.2442 0.0070 -0.1384 0.110 Uiso 1 1 calc R . . C14 C -0.2031(5) -0.0756(10) -0.0338(5) 0.080(3) Uani 1 1 d . . . H14 H -0.2400 -0.1444 -0.0387 0.096 Uiso 1 1 calc R . . C15 C -0.1437(5) -0.0566(10) 0.0320(5) 0.078(3) Uani 1 1 d . . . H15 H -0.1427 -0.1136 0.0733 0.093 Uiso 1 1 calc R . . C16 C 0.1391(5) 0.2744(10) 0.2118(4) 0.069(2) Uani 1 1 d . . . H16A H 0.1421 0.1739 0.2028 0.082 Uiso 1 1 calc R . . H16B H 0.0909 0.2931 0.2194 0.082 Uiso 1 1 calc R . . C17 C 0.2033(5) 0.3173(9) 0.2817(4) 0.061(2) Uani 1 1 d . . . C18 C 0.2391(5) 0.2117(9) 0.3330(5) 0.070(2) Uani 1 1 d . . . H18 H 0.2242 0.1181 0.3222 0.083 Uiso 1 1 calc R . . C19 C 0.2979(5) 0.2456(9) 0.4015(5) 0.066(2) Uani 1 1 d . . . C20 C 0.3194(5) 0.3865(9) 0.4149(4) 0.062(2) Uani 1 1 d . . . C21 C 0.2844(5) 0.4877(9) 0.3634(4) 0.067(2) Uani 1 1 d . . . H21 H 0.3002 0.5812 0.3727 0.080 Uiso 1 1 calc R . . C22 C 0.2259(5) 0.4543(9) 0.2979(4) 0.064(2) Uani 1 1 d . . . H22 H 0.2015 0.5257 0.2641 0.077 Uiso 1 1 calc R . . C23 C 0.2919(6) 0.0236(10) 0.4554(7) 0.111(4) Uani 1 1 d . . . H23A H 0.2903 -0.0335 0.4114 0.134 Uiso 1 1 calc R . . H23B H 0.2401 0.0475 0.4512 0.134 Uiso 1 1 calc R . . C24 C 0.3278(9) -0.0599(14) 0.5273(7) 0.157(6) Uani 1 1 d . . . H24A H 0.2954 -0.1383 0.5305 0.188 Uiso 1 1 calc R . . H24B H 0.3767 -0.0970 0.5287 0.188 Uiso 1 1 calc R . . C25 C 0.3506(10) -0.0158(17) 0.6629(7) 0.172(6) Uani 1 1 d . . . H25A H 0.3976 -0.0695 0.6792 0.206 Uiso 1 1 calc R . . H25B H 0.3096 -0.0778 0.6642 0.206 Uiso 1 1 calc R . . C26 C 0.3564(8) 0.1065(15) 0.7151(9) 0.149(5) Uani 1 1 d . . . H26A H 0.3076 0.1537 0.7030 0.179 Uiso 1 1 calc R . . H26B H 0.3719 0.0748 0.7678 0.179 Uiso 1 1 calc R . . C27 C 0.4075(8) 0.3315(13) 0.7391(8) 0.135(5) Uani 1 1 d . . . H27A H 0.4297 0.3229 0.7942 0.162 Uiso 1 1 calc R . . H27B H 0.3548 0.3599 0.7271 0.162 Uiso 1 1 calc R . . C28 C 0.4490(8) 0.4405(15) 0.7113(5) 0.143(5) Uani 1 1 d . . . H28A H 0.4476 0.5306 0.7357 0.172 Uiso 1 1 calc R . . H28B H 0.5016 0.4130 0.7221 0.172 Uiso 1 1 calc R . . C29 C 0.4461(6) 0.5423(12) 0.5923(5) 0.116(4) Uani 1 1 d . . . H29A H 0.4937 0.5037 0.5907 0.139 Uiso 1 1 calc R . . H29B H 0.4553 0.6347 0.6164 0.139 Uiso 1 1 calc R . . C30 C 0.3878(5) 0.5506(8) 0.5131(5) 0.088(3) Uani 1 1 d . . . H30A H 0.3398 0.5857 0.5156 0.105 Uiso 1 1 calc R . . H30B H 0.4051 0.6135 0.4809 0.105 Uiso 1 1 calc R . . Na Na 0.4221(2) 0.2223(5) 0.5768(2) 0.0932(13) Uani 1 1 d . . . N4 N 0.5554(6) 0.1896(13) 0.6129(7) 0.099(4) Uani 1 1 d . . . C31 C 0.6130(4) 0.1904(12) 0.6608(5) 0.099(3) Uani 1 1 d . . . S1 S 0.6955(2) 0.1732(4) 0.72312(19) 0.1239(13) 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 O1 0.065(3) 0.083(4) 0.054(3) -0.001(3) 0.019(3) -0.016(3) O2 0.093(4) 0.074(4) 0.083(4) 0.017(3) 0.017(4) 0.003(4) O3 0.207(7) 0.146(6) 0.140(6) 0.027(5) 0.059(5) -0.026(5) O4 0.141(5) 0.166(6) 0.130(5) -0.016(5) 0.065(5) -0.017(5) O5 0.157(6) 0.145(6) 0.097(4) 0.006(4) 0.027(4) 0.015(5) O6 0.068(4) 0.085(4) 0.059(3) -0.003(3) 0.012(3) -0.004(3) N1 0.089(6) 0.095(6) 0.081(5) 0.019(5) 0.039(5) 0.005(5) N2 0.067(4) 0.062(4) 0.055(4) 0.000(3) 0.025(3) 0.013(3) N3 0.065(4) 0.073(5) 0.053(4) -0.001(3) 0.017(3) -0.005(4) C1 0.097(5) 0.106(5) 0.112(5) 0.010(4) 0.046(4) 0.001(4) C2 0.110(5) 0.101(5) 0.095(5) 0.006(4) 0.047(4) 0.013(4) C3 0.101(5) 0.091(5) 0.081(4) 0.001(4) 0.028(4) 0.012(4) C4 0.090(4) 0.079(4) 0.065(4) 0.008(4) 0.026(4) 0.009(4) C5 0.095(6) 0.066(6) 0.070(6) 0.011(4) 0.046(5) 0.023(5) C6 0.061(5) 0.065(5) 0.060(5) 0.005(4) 0.024(4) 0.018(4) C7 0.080(6) 0.058(5) 0.075(6) -0.003(4) 0.044(5) 0.000(4) C8 0.069(5) 0.068(5) 0.050(4) -0.008(4) 0.022(4) 0.001(4) C9 0.055(4) 0.071(5) 0.052(4) 0.001(4) 0.018(4) 0.003(4) C10 0.064(5) 0.057(5) 0.052(4) -0.001(4) 0.024(4) 0.012(4) C11 0.058(5) 0.069(5) 0.051(4) -0.008(4) 0.019(4) 0.004(4) C12 0.065(5) 0.115(8) 0.058(5) 0.005(5) 0.011(4) 0.001(5) C13 0.046(5) 0.142(10) 0.074(6) 0.000(6) 0.003(4) -0.012(6) C14 0.065(5) 0.104(8) 0.067(6) -0.015(5) 0.019(5) -0.020(5) C15 0.080(6) 0.095(7) 0.062(5) -0.006(5) 0.028(5) -0.010(5) C16 0.066(5) 0.083(6) 0.056(5) -0.005(4) 0.018(4) -0.010(5) C17 0.071(5) 0.068(5) 0.048(4) 0.002(4) 0.022(4) 0.003(4) C18 0.078(6) 0.067(6) 0.067(5) -0.010(4) 0.028(5) -0.012(5) C19 0.072(5) 0.058(5) 0.070(5) 0.010(4) 0.026(5) 0.006(4) C20 0.065(5) 0.071(6) 0.052(4) -0.006(4) 0.022(4) -0.004(4) C21 0.082(6) 0.058(5) 0.055(5) 0.005(4) 0.016(4) -0.011(4) C22 0.079(5) 0.057(5) 0.051(4) 0.000(4) 0.014(4) 0.001(4) C23 0.124(6) 0.090(6) 0.111(6) 0.015(5) 0.027(5) 0.001(5) C24 0.177(8) 0.140(8) 0.149(8) 0.008(6) 0.048(6) -0.006(6) C25 0.176(8) 0.176(9) 0.163(8) 0.017(7) 0.056(6) -0.019(6) C26 0.143(7) 0.162(8) 0.149(8) 0.007(6) 0.058(6) -0.004(6) C27 0.129(7) 0.148(8) 0.132(7) -0.012(6) 0.049(6) 0.016(6) C28 0.154(7) 0.145(7) 0.117(7) -0.022(6) 0.028(6) -0.008(6) C29 0.111(6) 0.111(6) 0.118(6) -0.029(5) 0.030(5) -0.013(5) C30 0.096(5) 0.082(5) 0.072(5) -0.001(4) 0.010(4) -0.012(5) Na 0.097(3) 0.111(3) 0.071(2) 0.009(2) 0.0281(19) 0.014(2) N4 0.095(5) 0.103(6) 0.100(5) 0.006(4) 0.035(4) 0.001(4) C31 0.099(5) 0.100(5) 0.101(5) 0.017(4) 0.039(4) 0.000(4) S1 0.144(3) 0.098(2) 0.113(2) 0.0241(18) 0.0204(19) -0.0012(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 C8 1.352(9) . ? O1 C16 1.427(9) . ? O2 C19 1.350(9) . ? O2 C23 1.424(8) . ? O2 Na 2.403(7) . ? O3 C25 1.409(12) . ? O3 C24 1.412(13) . ? O3 Na 2.433(11) . ? O4 C26 1.404(12) . ? O4 C27 1.418(11) . ? O4 Na 2.452(9) . ? O5 C28 1.414(7) . ? O5 C29 1.423(7) . ? O5 Na 2.415(10) . ? O6 C20 1.397(9) . ? O6 C30 1.425(7) . ? O6 Na 2.430(7) . ? N1 C5 1.340(12) . ? N1 C1 1.349(9) . ? N2 C6 1.341(10) . ? N2 C10 1.343(9) . ? N3 C11 1.332(6) . ? N3 C15 1.335(6) . ? C1 C2 1.383(14) . ? C1 H1 0.9297 . ? C2 C3 1.366(9) . ? C2 H2 0.9302 . ? C3 C4 1.386(12) . ? C3 H3 0.9300 . ? C4 C5 1.374(12) . ? C4 H4 0.9302 . ? C5 C6 1.475(11) . ? C6 C7 1.387(11) . ? C7 C8 1.375(11) . ? C7 H7 0.9300 . ? C8 C9 1.385(11) . ? C9 C10 1.418(10) . ? C9 H9 0.9298 . ? C10 C11 1.480(11) . ? C11 C12 1.383(11) . ? C12 C13 1.398(13) . ? C12 H12 0.9300 . ? C13 C14 1.369(8) . ? C13 H13 0.9301 . ? C14 C15 1.360(11) . ? C14 H14 0.9299 . ? C15 H15 0.9300 . ? C16 C17 1.499(11) . ? C16 H16A 0.9701 . ? C16 H16B 0.9700 . ? C17 C22 1.365(11) . ? C17 C18 1.387(11) . ? C18 C19 1.411(11) . ? C18 H18 0.9300 . ? C19 C20 1.390(11) . ? C20 C21 1.356(11) . ? C21 C22 1.373(11) . ? C21 H21 0.9299 . ? C22 H22 0.9300 . ? C23 C24 1.502(12) . ? C23 H23A 0.9702 . ? C23 H23B 0.9702 . ? C24 H24A 0.9699 . ? C24 H24B 0.9697 . ? C25 C26 1.489(14) . ? C25 H25A 0.9705 . ? C25 H25B 0.9704 . ? C26 H26A 0.9706 . ? C26 H26B 0.9689 . ? C27 C28 1.480(14) . ? C27 H27A 0.9694 . ? C27 H27B 0.9704 . ? C28 H28A 0.9699 . ? C28 H28B 0.9699 . ? C29 C30 1.512(7) . ? C29 Na 3.059(12) . ? C29 H29A 0.9698 . ? C29 H29B 0.9702 . ? C30 H30A 0.9699 . ? C30 H30B 0.9700 . ? Na N4 2.371(12) . ? N4 C31 1.144(12) . ? C31 S1 1.596(6) . ? 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 C8 O1 C16 117.2(6) . . ? C19 O2 C23 115.2(7) . . ? C19 O2 Na 121.3(6) . . ? C23 O2 Na 116.5(6) . . ? C25 O3 C24 119.7(11) . . ? C25 O3 Na 115.0(10) . . ? C24 O3 Na 107.6(9) . . ? C26 O4 C27 110.1(11) . . ? C26 O4 Na 119.2(8) . . ? C27 O4 Na 112.9(8) . . ? C28 O5 C29 114.7(10) . . ? C28 O5 Na 107.5(8) . . ? C29 O5 Na 102.6(7) . . ? C20 O6 C30 117.3(6) . . ? C20 O6 Na 120.1(5) . . ? C30 O6 Na 115.7(5) . . ? C5 N1 C1 115.0(9) . . ? C6 N2 C10 119.0(7) . . ? C11 N3 C15 116.1(7) . . ? C2 C1 N1 124.7(10) . . ? C2 C1 H1 117.6 . . ? N1 C1 H1 117.7 . . ? C3 C2 C1 119.1(10) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 117.4(10) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C5 C4 C3 120.0(9) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 123.9(8) . . ? N1 C5 C6 115.9(8) . . ? C4 C5 C6 120.2(9) . . ? N2 C6 C7 121.3(7) . . ? N2 C6 C5 115.8(8) . . ? C7 C6 C5 123.0(8) . . ? C8 C7 C6 121.0(8) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? O1 C8 C9 123.0(7) . . ? O1 C8 C7 118.8(8) . . ? C9 C8 C7 118.2(7) . . ? C8 C9 C10 118.5(7) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 122.0(7) . . ? N2 C10 C11 117.6(7) . . ? C9 C10 C11 120.4(7) . . ? N3 C11 C12 123.8(8) . . ? N3 C11 C10 116.1(6) . . ? C12 C11 C10 120.2(7) . . ? C11 C12 C13 116.1(8) . . ? C11 C12 H12 121.9 . . ? C13 C12 H12 121.9 . . ? C14 C13 C12 122.1(8) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 115.1(8) . . ? C13 C14 H14 122.4 . . ? C15 C14 H14 122.4 . . ? N3 C15 C14 126.7(8) . . ? N3 C15 H15 116.7 . . ? C14 C15 H15 116.7 . . ? O1 C16 C17 109.4(7) . . ? O1 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? O1 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? C22 C17 C18 119.3(7) . . ? C22 C17 C16 123.1(8) . . ? C18 C17 C16 117.5(8) . . ? C17 C18 C19 120.4(8) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? O2 C19 C20 117.9(8) . . ? O2 C19 C18 124.0(8) . . ? C20 C19 C18 118.1(8) . . ? C21 C20 C19 120.5(8) . . ? C21 C20 O6 125.0(8) . . ? C19 C20 O6 114.5(7) . . ? C20 C21 C22 121.0(8) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C17 C22 C21 120.6(7) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? O2 C23 C24 110.9(10) . . ? O2 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? O2 C23 H23B 109.4 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? O3 C24 C23 105.7(10) . . ? O3 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O3 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.8 . . ? O3 C25 C26 108.6(13) . . ? O3 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O3 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.3 . . ? O4 C26 C25 107.1(12) . . ? O4 C26 H26A 110.3 . . ? C25 C26 H26A 110.2 . . ? O4 C26 H26B 110.4 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? O4 C27 C28 110.5(11) . . ? O4 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? O4 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? O5 C28 C27 105.7(11) . . ? O5 C28 H28A 110.6 . . ? C27 C28 H28A 110.6 . . ? O5 C28 H28B 110.6 . . ? C27 C28 H28B 110.6 . . ? H28A C28 H28B 108.8 . . ? O5 C29 C30 102.9(8) . . ? O5 C29 Na 50.4(5) . . ? C30 C29 Na 85.6(5) . . ? O5 C29 H29A 111.2 . . ? C30 C29 H29A 111.2 . . ? Na C29 H29A 74.4 . . ? O5 C29 H29B 111.2 . . ? C30 C29 H29B 111.2 . . ? Na C29 H29B 158.8 . . ? H29A C29 H29B 109.1 . . ? O6 C30 C29 106.5(7) . . ? O6 C30 H30A 110.4 . . ? C29 C30 H30A 110.4 . . ? O6 C30 H30B 110.4 . . ? C29 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? N4 Na O2 123.9(4) . . ? N4 Na O5 102.9(4) . . ? O2 Na O5 121.3(3) . . ? N4 Na O3 122.5(4) . . ? O2 Na O3 66.9(3) . . ? O5 Na O3 117.4(4) . . ? N4 Na O6 111.4(4) . . ? O2 Na O6 65.1(2) . . ? O5 Na O6 66.0(3) . . ? O3 Na O6 121.5(3) . . ? N4 Na O4 97.6(4) . . ? O2 Na O4 128.6(3) . . ? O5 Na O4 68.2(3) . . ? O3 Na O4 65.4(4) . . ? O6 Na O4 129.9(3) . . ? N4 Na C29 89.7(4) . . ? O2 Na C29 113.8(3) . . ? O5 Na C29 27.0(2) . . ? O3 Na C29 142.0(4) . . ? O6 Na C29 49.1(2) . . ? O4 Na C29 93.1(3) . . ? C31 N4 Na 147.6(11) . . ? N4 C31 S1 172.7(13) . . ? _diffrn_measured_fraction_theta_max 0.98 _diffrn_reflns_theta_full 66.92 _diffrn_measured_fraction_theta_full 0.98 _refine_diff_density_max 0.654 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.082 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 692441' # start Validation Reply Form _vrf_PLAT201_11 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 90 RESPONSE: This crystal structure has been determined from extremely small and poorly diffracting single-crystal, so only isotropic displacement parameters were refined. ; _vrf_ATOM007_11 ; PROBLEM: _atom_site_aniso_label is missing RESPONSE: This crystal structure has been determined from extremely small and poorly diffracting single-crystal, so only isotropic displacement parameters were refined. ; # end Validation Reply Form _audit_creation_method manual _chemical_name_systematic ; {[4'-(4'''-Benzo-15-crown-5-sodium thiocyanate)- methyloxy-2,2':6',2''-terpyridine] [4'-(4'''-benzo-15-crown-5-sodium dithiocyanate)-methyloxy-2,2':6',2''- terpyridine]} copper(II) thiocyanate acetonitrile ; _chemical_name_common ; ((4'-(4'''-Benzo-15-crown-5-sodium thiocyanate)-methyloxy- 2,2':6',2''-terpyridine) (4'-(4'''-benzo-15-crown-5-sodium dithiocyanate)-methyloxy-2,2':6',2''-terpyridine)) copper(ii) thiocyanate acetonitrile ; _chemical_melting_point ? _chemical_formula_moiety 'C63 H62 Cu N9 Na2 O12 S3, C N S, C2 H3 N' _chemical_formula_sum 'C66 H65 Cu N11 Na2 O12 S4' _chemical_formula_weight 1442.10 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.674(2) _cell_length_b 12.833(2) _cell_length_c 13.256(3) _cell_angle_alpha 67.047(11) _cell_angle_beta 62.366(11) _cell_angle_gamma 87.686(12) _cell_volume 1732.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3832 _cell_measurement_theta_min 5.01 _cell_measurement_theta_max 18.25 _exptl_crystal_description prism? _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 749 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII area-detector diffractometer' _diffrn_measurement_method '\o and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17928 _diffrn_reflns_av_R_equivalents 0.1866 _diffrn_reflns_av_sigmaI/netI 0.4319 _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 -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.75 _reflns_number_total 5206 _reflns_number_gt 1543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT-Plus (Bruker, 1998)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'Fox (Favre-Nicolin & Cerny, 2002)' _computing_structure_refinement 'MRIA (Zlokazov & Chernyshev, 1992)' _computing_molecular_graphics 'PLATON (Spek, 2002)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)]' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5206 _refine_ls_number_parameters 386 _refine_ls_number_restraints 315 _refine_ls_R_factor_all 0.2783 _refine_ls_R_factor_gt 0.1571 _refine_ls_wR_factor_ref 0.4319 _refine_ls_wR_factor_gt 0.3578 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 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 _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.5000 0.5000 0.5000 0.0544(14) Uiso 1 1 d . . . O1A O 1.0463(25) 0.5645(22) 0.1830(29) 0.087(9) Uiso 1 1 d . . . O2A O 1.5067(26) 0.8549(20) -0.1533(32) 0.074(8) Uiso 1 1 d . . . O3A O 1.6123(26) 1.0521(24) -0.3783(27) 0.088(9) Uiso 1 1 d . . . O4A O 1.8313(27) 1.0101(21) -0.5258(31) 0.093(9) Uiso 1 1 d . . . O5A O 1.7897(23) 0.7704(23) -0.4370(24) 0.064(7) Uiso 1 1 d . . . O6A O 1.6064(24) 0.6801(19) -0.1950(23) 0.058(7) Uiso 1 1 d . . . N1A N 0.5535(30) 0.3955(24) 0.6429(33) 0.056(8) Uiso 1 1 d . . . N2A N 0.6779(29) 0.5250(23) 0.3967(30) 0.052(8) Uiso 1 1 d . . . N3A N 0.5297(31) 0.6161(24) 0.3078(32) 0.059(8) Uiso 1 1 d . . . C1A C 0.4889(39) 0.3349(31) 0.7694(38) 0.073(12) Uiso 1 1 d . . . H1A H 0.4058 0.3329 0.8083 0.087 Uiso 1 1 calc . . . C2A C 0.5386(40) 0.2766(28) 0.8426(39) 0.065(11) Uiso 1 1 d . . . H2A H 0.4896 0.2336 0.9283 0.078 Uiso 1 1 calc . . . C3A C 0.6627(42) 0.2823(37) 0.7880(40) 0.084(13) Uiso 1 1 d . . . H3A H 0.6990 0.2443 0.8360 0.101 Uiso 1 1 calc . . . C4A C 0.7322(38) 0.3471(33) 0.6578(38) 0.068(11) Uiso 1 1 d . . . H4A H 0.8155 0.3505 0.6171 0.082 Uiso 1 1 calc . . . C5A C 0.6748(34) 0.4058(27) 0.5911(36) 0.056(10) Uiso 1 1 d . . . C6A C 0.7409(31) 0.4731(32) 0.4513(33) 0.051(9) Uiso 1 1 d . . . C7A C 0.8678(33) 0.4816(28) 0.3862(38) 0.062(10) Uiso 1 1 d . . . H7A H 0.9108 0.4447 0.4270 0.075 Uiso 1 1 calc . . . C8A C 0.9252(37) 0.5494(33) 0.2559(41) 0.059(11) Uiso 1 1 d . . . C9A C 0.8570(36) 0.6062(30) 0.1986(37) 0.075(12) Uiso 1 1 d . . . H9A H 0.8951 0.6519 0.1127 0.090 Uiso 1 1 calc . . . C10A C 0.7322(33) 0.5934(29) 0.2711(34) 0.049(9) Uiso 1 1 d . . . C11A C 0.6511(28) 0.6448(28) 0.2219(31) 0.047(9) Uiso 1 1 d . . . C12A C 0.6890(31) 0.7202(30) 0.0998(38) 0.060(11) Uiso 1 1 d . . . H12A H 0.7712 0.7432 0.0425 0.072 Uiso 1 1 calc . . . C13A C 0.6032(29) 0.7630(32) 0.0609(36) 0.059(10) Uiso 1 1 d . . . H13A H 0.6281 0.8107 -0.0227 0.071 Uiso 1 1 calc . . . C14A C 0.4800(39) 0.7326(41) 0.1504(45) 0.084(14) Uiso 1 1 d . . . H14A H 0.4214 0.7611 0.1286 0.100 Uiso 1 1 calc . . . C15A C 0.4489(32) 0.6588(33) 0.2720(38) 0.052(10) Uiso 1 1 d . . . H15A H 0.3675 0.6377 0.3321 0.062 Uiso 1 1 calc . . . C16A C 1.0980(45) 0.6440(44) 0.0491(46) 0.113(17) Uiso 1 1 d . . . H16A H 1.0777 0.7197 0.0400 0.136 Uiso 1 1 calc . . . H16B H 1.0676 0.6156 0.0079 0.136 Uiso 1 1 calc . . . C17A C 1.2340(48) 0.6485(43) -0.0064(48) 0.094(15) Uiso 1 1 d . . . C18A C 1.3079(41) 0.7458(33) -0.0403(38) 0.070(12) Uiso 1 1 d . . . H18A H 1.2733 0.8062 -0.0227 0.084 Uiso 1 1 calc . . . C19A C 1.4318(43) 0.7554(32) -0.0997(43) 0.060(11) Uiso 1 1 d . . . C20A C 1.4828(42) 0.6632(31) -0.1288(39) 0.063(12) Uiso 1 1 d . . . C21A C 1.4104(38) 0.5606(28) -0.0873(37) 0.060(11) Uiso 1 1 d . . . H21A H 1.4443 0.4975 -0.0982 0.072 Uiso 1 1 calc . . . C22A C 1.2838(40) 0.5556(43) -0.0280(49) 0.085(14) Uiso 1 1 d . . . H22A H 1.2333 0.4897 -0.0031 0.102 Uiso 1 1 calc . . . C23A C 1.4528(47) 0.9591(40) -0.1681(50) 0.099(15) Uiso 1 1 d . . . H23A H 1.4068 0.9631 -0.0878 0.119 Uiso 1 1 calc . . . H23B H 1.3988 0.9593 -0.2014 0.119 Uiso 1 1 calc . . . C24A C 1.5553(48) 1.0605(41) -0.2580(47) 0.109(17) Uiso 1 1 d . . . H24A H 1.5246 1.1321 -0.2661 0.131 Uiso 1 1 calc . . . H24B H 1.6129 1.0572 -0.2284 0.131 Uiso 1 1 calc . . . C25A C 1.7102(42) 1.1460(39) -0.4748(48) 0.092(14) Uiso 1 1 d . . . H25A H 1.7550 1.1654 -0.4400 0.110 Uiso 1 1 calc . . . H25B H 1.6784 1.2131 -0.5084 0.110 Uiso 1 1 calc . . . C26A C 1.7911(47) 1.1113(40) -0.5758(51) 0.106(16) Uiso 1 1 d . . . H26A H 1.7479 1.0987 -0.6155 0.127 Uiso 1 1 calc . . . H26B H 1.8600 1.1722 -0.6391 0.127 Uiso 1 1 calc . . . C27A C 1.8885(41) 0.9549(44) -0.6092(42) 0.093(14) Uiso 1 1 d . . . H27A H 1.9662 1.0008 -0.6776 0.112 Uiso 1 1 calc . . . H27B H 1.8385 0.9476 -0.6444 0.112 Uiso 1 1 calc . . . C28A C 1.9059(49) 0.8368(40) -0.5362(51) 0.105(16) Uiso 1 1 d . . . H28A H 1.9453 0.7989 -0.5915 0.126 Uiso 1 1 calc . . . H28B H 1.9565 0.8440 -0.5017 0.126 Uiso 1 1 calc . . . C29A C 1.7962(40) 0.6668(34) -0.3478(41) 0.064(11) Uiso 1 1 d . . . H29A H 1.8348 0.6837 -0.3063 0.077 Uiso 1 1 calc . . . H29B H 1.8425 0.6195 -0.3888 0.077 Uiso 1 1 calc . . . C30A C 1.6661(32) 0.6046(29) -0.2527(33) 0.042(9) Uiso 1 1 d . . . H30A H 1.6265 0.5898 -0.2944 0.051 Uiso 1 1 calc . . . H30B H 1.6647 0.5320 -0.1903 0.051 Uiso 1 1 calc . . . O1B O -0.0394(26) 0.3957(24) 0.8577(29) 0.070(8) Uiso 1 1 d . . . O2B O -0.4715(22) 0.1788(23) 1.1420(24) 0.056(7) Uiso 1 1 d . . . O3B O -0.6043(24) -0.0250(22) 1.3238(27) 0.070(8) Uiso 1 1 d . . . O4B O -0.8423(23) 0.0001(24) 1.4327(28) 0.084(8) Uiso 1 1 d . . . O5B O -0.8238(21) 0.2306(21) 1.3904(23) 0.065(7) Uiso 1 1 d . . . O6B O -0.6061(23) 0.3288(19) 1.1995(22) 0.052(7) Uiso 1 1 d . . . N1B N 0.4771(27) 0.6526(23) 0.5447(30) 0.054(8) Uiso 1 1 d . . . N2B N 0.3246(23) 0.4703(20) 0.6121(28) 0.044(8) Uiso 1 1 d . . . N3B N 0.4418(26) 0.3386(21) 0.4989(31) 0.065(9) Uiso 1 1 d . . . C1B C 0.5578(38) 0.7411(41) 0.5048(43) 0.081(13) Uiso 1 1 d . . . H1B H 0.6376 0.7453 0.4472 0.098 Uiso 1 1 calc . . . C2B C 0.5282(39) 0.8284(33) 0.5452(39) 0.070(12) Uiso 1 1 d . . . H2B H 0.5866 0.8900 0.5159 0.079 Uiso 1 1 calc . . . C3B C 0.4084(33) 0.8205(28) 0.6308(33) 0.055(10) Uiso 1 1 d . . . H3B H 0.3858 0.8772 0.6603 0.066 Uiso 1 1 calc . . . C4B C 0.3231(31) 0.7297(31) 0.6723(39) 0.060(10) Uiso 1 1 d . . . H4B H 0.2428 0.7243 0.7295 0.072 Uiso 1 1 calc . . . C5B C 0.3593(29) 0.6448(28) 0.6270(33) 0.042(9) Uiso 1 1 d . . . C6B C 0.2767(31) 0.5445(33) 0.6673(34) 0.040(9) Uiso 1 1 d . . . C7B C 0.1532(32) 0.5229(30) 0.7502(37) 0.063(11) Uiso 1 1 d . . . H7B H 0.1195 0.5729 0.7874 0.075 Uiso 1 1 calc . . . C8B C 0.0783(36) 0.4252(32) 0.7784(41) 0.058(11) Uiso 1 1 d . . . C9B C 0.1334(32) 0.3491(34) 0.7241(39) 0.064(11) Uiso 1 1 d . . . H9B H 0.0874 0.2831 0.7422 0.077 Uiso 1 1 calc . . . C10B C 0.2582(38) 0.3743(33) 0.6424(40) 0.070(12) Uiso 1 1 d . . . C11B C 0.3220(31) 0.3000(34) 0.5776(31) 0.053(10) Uiso 1 1 d . . . C12B C 0.2666(33) 0.1987(32) 0.5993(39) 0.060(11) Uiso 1 1 d . . . H12B H 0.1847 0.1733 0.6567 0.073 Uiso 1 1 calc . . . C13B C 0.3317(39) 0.1323(31) 0.5362(37) 0.068(11) Uiso 1 1 d . . . H13B H 0.2948 0.0633 0.5500 0.082 Uiso 1 1 calc . . . C14B C 0.4528(38) 0.1742(37) 0.4528(41) 0.082(14) Uiso 1 1 d . . . H14B H 0.4991 0.1332 0.4081 0.098 Uiso 1 1 calc . . . C15B C 0.5052(40) 0.2737(39) 0.4351(46) 0.093(14) Uiso 1 1 d . . . H15B H 0.5871 0.2999 0.3777 0.111 Uiso 1 1 calc . . . C16B C -0.1017(37) 0.4802(38) 0.9014(48) 0.089(14) Uiso 1 1 d . . . H16C H -0.0904 0.5505 0.8306 0.107 Uiso 1 1 calc . . . H16D H -0.0698 0.4980 0.9478 0.107 Uiso 1 1 calc . . . C17B C -0.2309(31) 0.4301(29) 0.9829(33) 0.055(10) Uiso 1 1 d . . . C18B C -0.2869(28) 0.3168(30) 1.0314(36) 0.054(10) Uiso 1 1 d . . . H18B H -0.2392 0.2612 1.0191 0.065 Uiso 1 1 calc . . . C19B C -0.4125(32) 0.2855(30) 1.0978(33) 0.053(9) Uiso 1 1 d . . . C20B C -0.4849(30) 0.3698(33) 1.1236(30) 0.047(10) Uiso 1 1 d . . . C21B C -0.4304(36) 0.4803(31) 1.0810(37) 0.063(11) Uiso 1 1 d . . . H21B H -0.4776 0.5346 1.0993 0.075 Uiso 1 1 calc . . . C22B C -0.3043(31) 0.5113(32) 1.0103(34) 0.059(10) Uiso 1 1 d . . . H22B H -0.2686 0.5864 0.9810 0.071 Uiso 1 1 calc . . . C23B C -0.4080(39) 0.0826(33) 1.1660(40) 0.068(12) Uiso 1 1 d . . . H23C H -0.3811 0.0816 1.2239 0.082 Uiso 1 1 calc . . . H23D H -0.3376 0.0903 1.0884 0.082 Uiso 1 1 calc . . . C24B C -0.4929(30) -0.0272(28) 1.2213(39) 0.061(11) Uiso 1 1 d . . . H24C H -0.5082 -0.0329 1.1582 0.074 Uiso 1 1 calc . . . H24D H -0.4578 -0.0929 1.2514 0.074 Uiso 1 1 calc . . . C25B C -0.6988(32) -0.1207(30) 1.3768(31) 0.056(10) Uiso 1 1 d . . . H25C H -0.6729 -0.1933 1.4066 0.067 Uiso 1 1 calc . . . H25D H -0.7207 -0.1185 1.3150 0.067 Uiso 1 1 calc . . . C26B C -0.8063(37) -0.1050(40) 1.4866(38) 0.090(14) Uiso 1 1 d . . . H26C H -0.8725 -0.1688 1.5314 0.108 Uiso 1 1 calc . . . H26D H -0.7820 -0.1013 1.5448 0.108 Uiso 1 1 calc . . . C27B C -0.9287(31) 0.0403(30) 1.5218(42) 0.061(11) Uiso 1 1 d . . . H27C H -0.9011 0.0403 1.5789 0.073 Uiso 1 1 calc . . . H27D H -1.0063 -0.0103 1.5705 0.073 Uiso 1 1 calc . . . C28B C -0.9415(37) 0.1603(33) 1.4511(39) 0.071(12) Uiso 1 1 d . . . H28C H -0.9632 0.1624 1.3892 0.085 Uiso 1 1 calc . . . H28D H -1.0033 0.1875 1.5081 0.085 Uiso 1 1 calc . . . C29B C -0.8133(33) 0.3440(30) 1.3035(41) 0.058(10) Uiso 1 1 d . . . H29C H -0.8706 0.3848 1.3461 0.069 Uiso 1 1 calc . . . H29D H -0.8290 0.3417 1.2393 0.069 Uiso 1 1 calc . . . C30B C -0.6829(30) 0.4036(29) 1.2448(32) 0.054(10) Uiso 1 1 d . . . H30C H -0.6662 0.4780 1.1764 0.065 Uiso 1 1 calc . . . H30D H -0.6702 0.4146 1.3070 0.065 Uiso 1 1 calc . . . Na2 Na -0.6871(14) 0.1433(12) 1.2519(15) 0.071(5) Uiso 1 1 d . . . N3 N -0.7785(47) 0.1865(42) 1.1222(47) 0.095(23) Uiso 1 1 d . . . C3 C -0.8554(53) 0.2267(49) 1.1083(55) 0.104(24) Uiso 1 1 d . . . S3 S -0.9666(23) 0.2821(23) 1.0893(28) 0.110(9) Uiso 1 1 d . . . Na1 Na 1.7189(15) 0.8805(13) -0.3033(16) 0.080(5) Uiso 1 1 d . . . N1 N 1.8802(48) 0.7891(43) -0.2549(58) 0.103(20) Uiso 1 1 d . . . C1 C 1.9395(33) 0.7875(23) -0.2103(33) 0.096(15) Uiso 1 1 d . . . S1 S 2.0247(23) 0.7875(19) -0.1504(24) 0.099(10) Uiso 1 1 d . . . S2 S 1.8874(15) 1.1365(12) -0.1794(15) 0.116(9) Uiso 1 1 d . . . C2 C 1.8090(39) 1.0530(38) -0.1958(42) 0.085(13) Uiso 1 1 d . . . N2 N 1.7527(33) 0.9953(31) -0.2086(37) 0.103(12) Uiso 1 1 d . . . S4 S 0.1022(15) 0.5688(14) 0.4614(17) 0.089(9) Uiso 1 1 d . . . C4 C 0.1293(38) 0.6870(36) 0.3410(48) 0.096(15) Uiso 1 1 d . . . N4 N 0.1476(36) 0.7742(38) 0.2586(40) 0.114(13) Uiso 1 1 d . . . N5 N 0.8093(48) 0.8783(47) 0.2100(52) 0.101(23) Uiso 1 1 d . . . C5 C 0.8960(60) 0.9273(69) 0.1163(70) 0.129(33) Uiso 1 1 d . . . C6 C 1.0003(62) 0.9880(61) -0.0041(72) 0.119(34) Uiso 1 1 d . . . H6A H 1.0707 0.9580 -0.0032 0.179 Uiso 1 1 calc R . . H6B H 1.0104 1.0682 -0.0224 0.179 Uiso 1 1 calc R . . H6C H 0.9896 0.9783 -0.0672 0.179 Uiso 1 1 calc R . . 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 Cu N1A 2.23(3) . ? Cu N1B 2.24(3) . ? Cu N2A 1.98(3) . ? Cu N2B 1.96(3) . ? Cu N3A 2.24(3) . ? Cu N3B 2.23(3) . ? S1 C1 1.63(5) . ? S2 C2 1.63(6) . ? S3 C3 1.64(8) . ? S4 C4 1.62(6) . ? Na1 O2A 2.43(4) . ? Na1 O4A 2.44(4) . ? Na1 O5A 2.52(3) . ? Na1 O3A 2.64(4) . ? Na1 N1 2.53(7) . ? Na1 N2 2.43(5) . ? Na1 O6A 2.50(3) . ? Na2 O2B 2.38(3) . ? Na2 O4B 2.34(4) . ? Na2 O5B 2.48(3) . ? Na2 O3B 2.41(4) . ? Na2 N3 2.39(7) . ? Na2 O6B 2.33(3) . ? O1A C16A 1.48(6) . ? O1A C8A 1.35(6) . ? O1B C8B 1.32(6) . ? O1B C16B 1.45(7) . ? O2A C23A 1.46(7) . ? O2A C19A 1.35(6) . ? O2B C19B 1.35(5) . ? O2B C23B 1.46(6) . ? O3A C25A 1.44(7) . ? O3A C24A 1.46(6) . ? O3B C24B 1.44(5) . ? O3B C25B 1.46(5) . ? O4A C26A 1.40(7) . ? O4A C27A 1.43(6) . ? O4B C27B 1.45(5) . ? O4B C26B 1.43(6) . ? O5A C29A 1.42(5) . ? O5A C28A 1.43(7) . ? O5B C28B 1.46(6) . ? O5B C29B 1.41(5) . ? O6A C20A 1.36(6) . ? O6A C30A 1.44(5) . ? O6B C30B 1.44(5) . ? O6B C20B 1.36(5) . ? N1 C1 1.16(8) . ? N1A C1A 1.35(5) . ? N1A C5A 1.36(6) . ? N1B C1B 1.32(7) . ? N1B C5B 1.36(5) . ? N2 C2 1.16(7) . ? N2A C10A 1.37(5) . ? N2A C6A 1.31(6) . ? N2B C10B 1.34(6) . ? N2B C6B 1.37(5) . ? N3 C3 1.13(10) . ? N3A C11A 1.37(5) . ? N3A C15A 1.34(6) . ? N3B C15B 1.39(6) . ? N3B C11B 1.35(5) . ? N5 C5 1.16(10) . ? N4 C4 1.15(7) . ? C1A C2A 1.37(7) . ? C1B C2B 1.38(7) . ? C2A C3A 1.38(8) . ? C2B C3B 1.39(6) . ? C3A C4A 1.40(6) . ? C3B C4B 1.37(6) . ? C4A C5A 1.38(7) . ? C4B C5B 1.40(6) . ? C5A C6A 1.50(5) . ? C5B C6B 1.45(6) . ? C6A C7A 1.41(6) . ? C6B C7B 1.40(6) . ? C7A C8A 1.40(6) . ? C7B C8B 1.42(6) . ? C8A C9A 1.40(7) . ? C8B C9B 1.41(6) . ? C9A C10A 1.39(7) . ? C9B C10B 1.40(7) . ? C10A C11A 1.47(6) . ? C10B C11B 1.49(6) . ? C11A C12A 1.37(5) . ? C11B C12B 1.36(6) . ? C12A C13A 1.42(6) . ? C12B C13B 1.41(6) . ? C13A C14A 1.40(7) . ? C13B C14B 1.38(7) . ? C14A C15A 1.38(6) . ? C14B C15B 1.35(8) . ? C16A C17A 1.52(9) . ? C16B C17B 1.47(7) . ? C17A C18A 1.38(8) . ? C17A C22A 1.40(8) . ? C17B C18B 1.40(6) . ? C17B C22B 1.40(6) . ? C18A C19A 1.38(8) . ? C18B C19B 1.39(6) . ? C19A C20A 1.42(6) . ? C19B C20B 1.44(6) . ? C20A C21A 1.39(7) . ? C20B C21B 1.37(6) . ? C21A C22A 1.41(8) . ? C21B C22B 1.40(7) . ? C23A C24A 1.52(8) . ? C23B C24B 1.51(6) . ? C25A C26A 1.48(8) . ? C25B C26B 1.54(6) . ? C27A C28A 1.52(8) . ? C27B C28B 1.51(6) . ? C29A C30A 1.53(6) . ? C29B C30B 1.54(6) . ? C5 C6 1.43(11) . ? C1A H1A 0.93 . ? C1B H1B 0.93 . ? C2A H2A 0.93 . ? C2B H2B 0.93 . ? C3A H3A 0.93 . ? C3B H3B 0.93 . ? C4A H4A 0.93 . ? C4B H4B 0.93 . ? C7A H7A 0.93 . ? C7B H7B 0.93 . ? C9A H9A 0.93 . ? C9B H9B 0.93 . ? C12A H12A 0.93 . ? C12B H12B 0.93 . ? C13A H13A 0.93 . ? C13B H13B 0.93 . ? C14A H14A 0.93 . ? C14B H14B 0.93 . ? C15A H15A 0.93 . ? C15B H15B 0.93 . ? C16A H16A 0.97 . ? C16A H16B 0.97 . ? C16B H16D 0.97 . ? C16B H16C 0.97 . ? C18A H18A 0.93 . ? C18B H18B 0.93 . ? C21A H21A 0.93 . ? C21B H21B 0.93 . ? C22A H22A 0.93 . ? C22B H22B 0.93 . ? C23A H23B 0.97 . ? C23A H23A 0.97 . ? C23B H23D 0.97 . ? C23B H23C 0.97 . ? C24A H24B 0.97 . ? C24A H24A 0.97 . ? C24B H24D 0.97 . ? C24B H24C 0.97 . ? C25A H25B 0.97 . ? C25A H25A 0.97 . ? C25B H25D 0.97 . ? C25B H25C 0.97 . ? C26A H26A 0.97 . ? C26A H26B 0.97 . ? C26B H26C 0.97 . ? C26B H26D 0.97 . ? C27A H27B 0.97 . ? C27A H27A 0.97 . ? C27B H27D 0.97 . ? C27B H27C 0.97 . ? C28A H28B 0.97 . ? C28A H28A 0.97 . ? C28B H28D 0.97 . ? C28B H28C 0.97 . ? C29A H29B 0.97 . ? C29A H29A 0.97 . ? C29B H29C 0.97 . ? C29B H29D 0.97 . ? C30A H30A 0.97 . ? C30A H30B 0.97 . ? C30B H30C 0.97 . ? C30B H30D 0.97 . ? C6 H6C 0.96 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? 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 N1A Cu N1B 96.3(11) . . ? N1A Cu N2A 78.3(10) . . ? N1A Cu N2B 97.9(11) . . ? N1A Cu N3A 156.2(12) . . ? N1A Cu N3B 89.4(10) . . ? N1B Cu N2A 100.8(11) . . ? N1B Cu N2B 79.0(10) . . ? N1B Cu N3A 88.3(11) . . ? N1B Cu N3B 156.7(12) . . ? N2A Cu N2B 176.2(12) . . ? N2A Cu N3A 77.8(10) . . ? N2A Cu N3B 102.5(11) . . ? N2B Cu N3A 106.9(12) . . ? N2B Cu N3B 77.9(11) . . ? N3A Cu N3B 95.6(10) . . ? O2A Na1 O3A 66.6(12) . . ? O2A Na1 O4A 129.6(15) . . ? O2A Na1 O5A 121.4(13) . . ? O2A Na1 O6A 65.1(10) . . ? O2A Na1 N1 126.3(18) . . ? O2A Na1 N2 85.0(14) . . ? O3A Na1 O4A 65.1(12) . . ? O3A Na1 O5A 114.0(12) . . ? O3A Na1 O6A 118.6(13) . . ? O3A Na1 N1 155.6(18) . . ? O3A Na1 N2 82.0(14) . . ? O4A Na1 O5A 68.9(10) . . ? O4A Na1 O6A 130.9(12) . . ? O4A Na1 N1 103.8(19) . . ? O4A Na1 N2 101.4(14) . . ? O5A Na1 O6A 66.0(9) . . ? O5A Na1 N1 78.6(16) . . ? O5A Na1 N2 152.5(15) . . ? O6A Na1 N1 85.4(17) . . ? O6A Na1 N2 127.7(13) . . ? N1 Na1 N2 79.1(18) . . ? O2B Na2 O3B 67.8(11) . . ? O2B Na2 O4B 137.4(13) . . ? O2B Na2 O5B 127.9(12) . . ? O2B Na2 O6B 67.4(11) . . ? O2B Na2 N3 114.9(17) . . ? O3B Na2 O4B 70.5(12) . . ? O3B Na2 O5B 123.6(12) . . ? O3B Na2 O6B 123.7(13) . . ? O3B Na2 N3 129.1(17) . . ? O4B Na2 O5B 70.7(10) . . ? O4B Na2 O6B 134.6(12) . . ? O4B Na2 N3 98.2(18) . . ? O5B Na2 O6B 66.3(10) . . ? O5B Na2 N3 95.6(17) . . ? O6B Na2 N3 100.0(16) . . ? C8A O1A C16A 117(4) . . ? C8B O1B C16B 118(4) . . ? Na1 O2A C19A 121(3) . . ? Na1 O2A C23A 116(3) . . ? C19A O2A C23A 117(4) . . ? Na2 O2B C19B 119(2) . . ? Na2 O2B C23B 119(2) . . ? C19B O2B C23B 117(3) . . ? Na1 O3A C24A 94(3) . . ? Na1 O3A C25A 105(3) . . ? C24A O3A C25A 112(4) . . ? Na2 O3B C24B 110(2) . . ? Na2 O3B C25B 104(2) . . ? C24B O3B C25B 113(3) . . ? Na1 O4A C26A 121(3) . . ? Na1 O4A C27A 115(3) . . ? C26A O4A C27A 115(4) . . ? Na2 O4B C26B 116(3) . . ? Na2 O4B C27B 115(2) . . ? C26B O4B C27B 115(3) . . ? Na1 O5A C28A 102(3) . . ? Na1 O5A C29A 98(2) . . ? C28A O5A C29A 114(4) . . ? Na2 O5B C28B 103(2) . . ? Na2 O5B C29B 103(2) . . ? C28B O5B C29B 114(3) . . ? Na1 O6A C20A 118(2) . . ? Na1 O6A C30A 115(2) . . ? C20A O6A C30A 120(3) . . ? Na2 O6B C20B 121(2) . . ? Na2 O6B C30B 121(2) . . ? C20B O6B C30B 118(3) . . ? Na1 N1 C1 147(4) . . ? Cu N1A C1A 132.74 . . ? Cu N1A C5A 110.92 . . ? C1A N1A C5A 116(4) . . ? Cu N1B C1B 129.76 . . ? Cu N1B C5B 109.48 . . ? C1B N1B C5B 121(4) . . ? Na1 N2 C2 156(4) . . ? Cu N2A C6A 118.83 . . ? Cu N2A C10A 119.63 . . ? C6A N2A C10A 122(4) . . ? Cu N2B C6B 117.97 . . ? Cu N2B C10B 119.88 . . ? C6B N2B C10B 122(4) . . ? Na2 N3 C3 143(5) . . ? Cu N3A C11A 110.82 . . ? Cu N3A C15A 129.18 . . ? C11A N3A C15A 120(3) . . ? Cu N3B C11B 111.19 . . ? Cu N3B C15B 132.28 . . ? C11B N3B C15B 117(4) . . ? N1A C1A C2A 124(5) . . ? N1B C1B C2B 122(5) . . ? S1 C1 N1 178(4) . . ? S2 C2 N2 179(5) . . ? N5 C5 C6 177(11) . . ? S4 C4 N4 176(5) . . ? C1A C2A C3A 119(4) . . ? C1B C2B C3B 118(4) . . ? S3 C3 N3 178(7) . . ? C2A C3A C4A 118(5) . . ? C2B C3B C4B 120(4) . . ? C3A C4A C5A 119(5) . . ? C3B C4B C5B 119(4) . . ? N1A C5A C4A 123(4) . . ? N1A C5A C6A 114(4) . . ? C4A C5A C6A 123(4) . . ? N1B C5B C4B 120(4) . . ? N1B C5B C6B 117(3) . . ? C4B C5B C6B 123(4) . . ? N2A C6A C5A 118(4) . . ? N2A C6A C7A 124(3) . . ? C5A C6A C7A 118(4) . . ? N2B C6B C5B 117(3) . . ? N2B C6B C7B 119(4) . . ? C5B C6B C7B 124(4) . . ? C6A C7A C8A 116(4) . . ? C6B C7B C8B 120(4) . . ? O1A C8A C7A 122(5) . . ? O1A C8A C9A 118(4) . . ? C7A C8A C9A 120(5) . . ? O1B C8B C7B 124(4) . . ? O1B C8B C9B 117(4) . . ? C7B C8B C9B 118(4) . . ? C8A C9A C10A 120(4) . . ? C8B C9B C10B 119(4) . . ? N2A C10A C9A 119(4) . . ? N2A C10A C11A 116(3) . . ? C9A C10A C11A 125(3) . . ? N2B C10B C9B 121(4) . . ? N2B C10B C11B 116(4) . . ? C9B C10B C11B 122(4) . . ? N3A C11A C10A 116(3) . . ? N3A C11A C12A 120(4) . . ? C10A C11A C12A 124(4) . . ? N3B C11B C10B 114(4) . . ? N3B C11B C12B 122(4) . . ? C10B C11B C12B 124(4) . . ? C11A C12A C13A 120(4) . . ? C11B C12B C13B 121(4) . . ? C12A C13A C14A 119(4) . . ? C12B C13B C14B 116(4) . . ? C13A C14A C15A 117(5) . . ? C13B C14B C15B 121(5) . . ? N3A C15A C14A 123(4) . . ? N3B C15B C14B 123(5) . . ? O1A C16A C17A 105(4) . . ? O1B C16B C17B 108(4) . . ? C16A C17A C18A 121(5) . . ? C16A C17A C22A 119(5) . . ? C18A C17A C22A 120(6) . . ? C16B C17B C18B 129(4) . . ? C16B C17B C22B 113(4) . . ? C18B C17B C22B 118(4) . . ? C17A C18A C19A 121(5) . . ? C17B C18B C19B 122(4) . . ? O2A C19A C18A 122(4) . . ? O2A C19A C20A 118(4) . . ? C18A C19A C20A 119(4) . . ? O2B C19B C18B 125(4) . . ? O2B C19B C20B 116(3) . . ? C18B C19B C20B 119(4) . . ? O6A C20A C19A 116(4) . . ? O6A C20A C21A 123(4) . . ? C19A C20A C21A 121(5) . . ? O6B C20B C19B 115(3) . . ? O6B C20B C21B 126(4) . . ? C19B C20B C21B 120(4) . . ? C20A C21A C22A 118(4) . . ? C20B C21B C22B 121(4) . . ? C17A C22A C21A 121(5) . . ? C17B C22B C21B 121(4) . . ? O2A C23A C24A 108(5) . . ? O2B C23B C24B 108(4) . . ? O3A C24A C23A 106(4) . . ? O3B C24B C23B 107(3) . . ? O3A C25A C26A 109(4) . . ? O3B C25B C26B 104(3) . . ? O4A C26A C25A 110(4) . . ? O4B C26B C25B 106(3) . . ? O4A C27A C28A 109(4) . . ? O4B C27B C28B 109(3) . . ? O5A C28A C27A 109(5) . . ? O5B C28B C27B 106(4) . . ? O5A C29A C30A 107(4) . . ? O5B C29B C30B 107(3) . . ? O6A C30A C29A 106(3) . . ? O6B C30B C29B 106(3) . . ? N1A C1A H1A 117.97 . . ? C2A C1A H1A 117.71 . . ? N1B C1B H1B 118.91 . . ? C2B C1B H1B 119.00 . . ? C1A C2A H2A 120.02 . . ? C3A C2A H2A 120.86 . . ? C1B C2B H2B 121.17 . . ? C3B C2B H2B 120.40 . . ? C2A C3A H3A 120.76 . . ? C4A C3A H3A 121.38 . . ? C2B C3B H3B 120.20 . . ? C4B C3B H3B 120.12 . . ? C3A C4A H4A 120.41 . . ? C5A C4A H4A 120.20 . . ? C3B C4B H4B 120.45 . . ? C5B C4B H4B 120.41 . . ? C6A C7A H7A 121.86 . . ? C8A C7A H7A 122.30 . . ? C6B C7B H7B 119.92 . . ? C8B C7B H7B 120.00 . . ? C8A C9A H9A 120.25 . . ? C10A C9A H9A 119.82 . . ? C8B C9B H9B 120.57 . . ? C10B C9B H9B 120.20 . . ? C11A C12A H12A 120.23 . . ? C13A C12A H12A 119.78 . . ? C11B C12B H12B 119.52 . . ? C13B C12B H12B 119.23 . . ? C12A C13A H13A 120.38 . . ? C14A C13A H13A 120.44 . . ? C12B C13B H13B 121.44 . . ? C14B C13B H13B 122.10 . . ? C13A C14A H14A 121.70 . . ? C15A C14A H14A 121.01 . . ? C13B C14B H14B 119.34 . . ? C15B C14B H14B 119.81 . . ? N3A C15A H15A 118.25 . . ? C14A C15A H15A 118.30 . . ? N3B C15B H15B 118.68 . . ? C14B C15B H15B 118.39 . . ? O1A C16A H16A 110.78 . . ? O1A C16A H16B 110.37 . . ? C17A C16A H16A 110.41 . . ? C17A C16A H16B 111.16 . . ? H16A C16A H16B 108.88 . . ? O1B C16B H16C 110.68 . . ? O1B C16B H16D 109.60 . . ? C17B C16B H16C 110.59 . . ? C17B C16B H16D 109.87 . . ? H16C C16B H16D 108.03 . . ? C17A C18A H18A 119.05 . . ? C19A C18A H18A 119.91 . . ? C17B C18B H18B 119.16 . . ? C19B C18B H18B 118.97 . . ? C20A C21A H21A 120.61 . . ? C22A C21A H21A 121.21 . . ? C20B C21B H21B 119.40 . . ? C22B C21B H21B 119.94 . . ? C17A C22A H22A 119.77 . . ? C21A C22A H22A 119.64 . . ? C17B C22B H22B 119.99 . . ? C21B C22B H22B 119.22 . . ? O2A C23A H23A 110.34 . . ? O2A C23A H23B 110.54 . . ? C24A C23A H23A 110.11 . . ? C24A C23A H23B 109.97 . . ? H23A C23A H23B 108.26 . . ? O2B C23B H23C 110.44 . . ? O2B C23B H23D 110.24 . . ? C24B C23B H23C 109.89 . . ? C24B C23B H23D 109.53 . . ? H23C C23B H23D 108.36 . . ? O3A C24A H24A 110.71 . . ? O3A C24A H24B 110.21 . . ? C23A C24A H24A 110.94 . . ? C23A C24A H24B 110.07 . . ? H24A C24A H24B 109.14 . . ? O3B C24B H24C 110.58 . . ? O3B C24B H24D 109.85 . . ? C23B C24B H24C 110.43 . . ? C23B C24B H24D 110.14 . . ? H24C C24B H24D 108.45 . . ? O3A C25A H25A 109.66 . . ? O3A C25A H25B 110.02 . . ? C26A C25A H25A 109.88 . . ? C26A C25A H25B 110.20 . . ? H25A C25A H25B 108.17 . . ? O3B C25B H25C 110.57 . . ? O3B C25B H25D 110.70 . . ? C26B C25B H25C 110.89 . . ? C26B C25B H25D 111.12 . . ? H25C C25B H25D 109.06 . . ? O4A C26A H26A 109.90 . . ? O4A C26A H26B 109.75 . . ? C25A C26A H26A 109.48 . . ? C25A C26A H26B 109.27 . . ? H26A C26A H26B 108.35 . . ? O4B C26B H26C 110.12 . . ? O4B C26B H26D 110.50 . . ? C25B C26B H26C 109.93 . . ? C25B C26B H26D 110.74 . . ? H26C C26B H26D 109.07 . . ? O4A C27A H27A 110.01 . . ? O4A C27A H27B 110.15 . . ? C28A C27A H27A 109.37 . . ? C28A C27A H27B 110.10 . . ? H27A C27A H27B 108.22 . . ? O4B C27B H27C 109.53 . . ? O4B C27B H27D 110.22 . . ? C28B C27B H27C 109.97 . . ? C28B C27B H27D 109.76 . . ? H27C C27B H27D 108.62 . . ? O5A C28A H28A 109.42 . . ? O5A C28A H28B 110.13 . . ? C27A C28A H28A 109.82 . . ? C27A C28A H28B 110.43 . . ? H28A C28A H28B 108.37 . . ? O5B C28B H28C 110.27 . . ? O5B C28B H28D 110.03 . . ? C27B C28B H28C 111.06 . . ? C27B C28B H28D 110.58 . . ? H28C C28B H28D 109.24 . . ? O5A C29A H29A 110.53 . . ? O5A C29A H29B 110.47 . . ? C30A C29A H29A 110.32 . . ? C30A C29A H29B 110.49 . . ? H29A C29A H29B 108.23 . . ? O5B C29B H29C 110.80 . . ? O5B C29B H29D 110.03 . . ? C30B C29B H29C 110.67 . . ? C30B C29B H29D 110.43 . . ? H29C C29B H29D 108.00 . . ? O6A C30A H30A 110.69 . . ? O6A C30A H30B 110.46 . . ? C29A C30A H30A 110.58 . . ? C29A C30A H30B 110.41 . . ? H30A C30A H30B 108.40 . . ? O6B C30B H30C 110.09 . . ? O6B C30B H30D 110.59 . . ? C29B C30B H30C 110.82 . . ? C29B C30B H30D 110.44 . . ? H30C C30B H30D 109.19 . . ? C5 C6 H6A 109.40 . . ? C5 C6 H6B 109.88 . . ? C5 C6 H6C 109.46 . . ? H6A C6 H6B 109.27 . . ? H6A C6 H6C 109.27 . . ? H6B C6 H6C 109.55 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.824 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.237 #===END