Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_method 'RAELSPUB and manual entry' _journal_coden_Cambridge 186 loop_ _publ_author_name 'Stephen Colbran' 'Donald C. Craig' 'Zhicong He' _publ_contact_author_name 'Dr. Stephen. B. Colbran' _publ_contact_author_address ; School of Chemical Sciences, The University of New South Wales, UNSW, Sydney, NSW, 2052, Australia ; _publ_contact_author_email 'S.Colbran@unsw.edu.au' _publ_contact_letter ? _publ_requested_journal 'J. Chem. Soc. Dalton Transactions' _publ_requested_category 'Article' # TITLE AND AUTHOR LIST _publ_section_title ; Structures and properties of 6-aryl substituted [tris(2-pyridylmethyl)amine] transition metal complexes ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' data_L _database_code_CSD 190789 _audit_creation_method 'RAELSPUB and manual entry' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 N4 O2' _chemical_formula_sum 'C26 H26 N4 O2' _chemical_formula_iupac ? _chemical_formula_weight 426.5 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 6.301(2) _cell_length_b 29.064(4) _cell_length_c 12.661(4) _cell_angle_alpha 90 _cell_angle_beta 92.57(1) _cell_angle_gamma 90 _cell_volume 2316.3(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 20 _cell_measurement_theta_max 23 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904.0 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3773 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 60 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ; Thermal motion was refined using four 15-parameter TLX rigid body thermal parameters, one for each ring, and individual anisotropic parameters for the methyl carbons, the ternary nitrogen and its attached methylene carbons. ; _reflns_number_total 3424 _reflns_number_gt 1924 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.054 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1924 _refine_ls_number_parameters 192 _refine_ls_goodness_of_fit_ref 1.60 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.29 _refine_diff_density_min -0.31 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy O1 0.18652(34) 0.69914(7) 0.30689(15) 0.073(2) Uani O 1.0 O2 0.88273(33) 0.79382(7) 0.47266(15) 0.070(1) Uani O 1.0 N1 0.44561(32) 0.65920(7) 0.58413(16) 0.041(1) Uani N 1.0 N2 0.6010(5) 0.5781(1) 0.9893(2) 0.090(1) Uani N 1.0 N3 0.4526(5) 0.4455(1) 0.6331(2) 0.086(3) Uani N 1.0 N4 0.42640(36) 0.55567(8) 0.73690(18) 0.0530(6) Uani N 1.0 C1 0.5009(5) 0.6029(1) 0.7240(2) 0.0588(9) Uani C 1.0 C2 0.35302(44) 0.63056(9) 0.65082(21) 0.045(1) Uani C 1.0 C3 0.1343(5) 0.6269(1) 0.6576(2) 0.052(2) Uani C 1.0 C4 0.0077(4) 0.6545(1) 0.5931(2) 0.055(2) Uani C 1.0 C5 0.09942(43) 0.68426(9) 0.52356(22) 0.050(2) Uani C 1.0 C6 0.31894(42) 0.68539(9) 0.52044(20) 0.043(1) Uani C 1.0 C7 0.42746(42) 0.71748(9) 0.44843(20) 0.044(1) Uani C 1.0 C8 0.3572(5) 0.7250(1) 0.3437(2) 0.054(1) Uani C 1.0 C9 0.4589(5) 0.7561(1) 0.2823(2) 0.058(2) Uani C 1.0 C10 0.6362(5) 0.7804(1) 0.3222(2) 0.055(2) Uani C 1.0 C11 0.70894(46) 0.77285(9) 0.42461(23) 0.052(1) Uani C 1.0 C12 0.60532(42) 0.74158(9) 0.48715(20) 0.0452(8) Uani C 1.0 C13 0.0995(6) 0.7079(1) 0.2037(3) 0.087(1) Uani C 1.0 C14 0.9984(6) 0.8256(1) 0.4122(3) 0.079(1) Uani C 1.0 C15 0.5346(5) 0.5343(1) 0.8293(2) 0.0643(9) Uani C 1.0 C16 0.4585(5) 0.5550(1) 0.9300(3) 0.063(2) Uani C 1.0 C17 0.2511(6) 0.5498(1) 0.9578(3) 0.083(2) Uani C 1.0 C18 0.1868(7) 0.5694(2) 1.0504(3) 0.102(3) Uani C 1.0 C19 0.3309(9) 0.5935(2) 1.1127(3) 0.111(3) Uani C 1.0 C20 0.5342(8) 0.5969(2) 1.0790(4) 0.116(2) Uani C 1.0 C21 0.4609(5) 0.5288(1) 0.6409(3) 0.068(1) Uani C 1.0 C22 0.3387(6) 0.4838(1) 0.6408(2) 0.067(3) Uani C 1.0 C23 0.1205(7) 0.4837(2) 0.6472(3) 0.101(4) Uani C 1.0 C24 0.0131(8) 0.4427(2) 0.6475(4) 0.128(5) Uani C 1.0 C25 0.1245(9) 0.4031(2) 0.6424(3) 0.113(5) Uani C 1.0 C26 0.3415(9) 0.4052(1) 0.6331(3) 0.104(5) Uani C 1.0 H1C1 0.6449 0.6022 0.6940 0.059 Uani H 1.0 H2C1 0.5102 0.6182 0.7948 0.059 Uani H 1.0 HC3 0.0709 0.6049 0.7080 0.057 Uani H 1.0 HC4 -0.1503 0.6529 0.5965 0.063 Uani H 1.0 HC5 0.0093 0.7046 0.4763 0.053 Uani H 1.0 HC9 0.4054 0.7615 0.2077 0.074 Uani H 1.0 HC10 0.7094 0.8030 0.2767 0.065 Uani H 1.0 HC12 0.6595 0.7362 0.5616 0.051 Uani H 1.0 H1C13 -0.0225 0.6866 0.1880 0.087 Uani H 1.0 H2C13 0.0487 0.7405 0.1991 0.087 Uani H 1.0 H3C13 0.2109 0.7028 0.1511 0.087 Uani H 1.0 H1C14 1.1201 0.8382 0.4567 0.079 Uani H 1.0 H2C14 1.0538 0.8097 0.3491 0.079 Uani H 1.0 H3C14 0.9027 0.8514 0.3883 0.079 Uani H 1.0 H1C15 0.6911 0.5394 0.8260 0.064 Uani H 1.0 H2C15 0.5043 0.5005 0.8288 0.064 Uani H 1.0 HC17 0.1480 0.5320 0.9114 0.112 Uani H 1.0 HC18 0.0367 0.5661 1.0717 0.139 Uani H 1.0 HC19 0.2895 0.6081 1.1802 0.144 Uani H 1.0 HC20 0.6398 0.6146 1.1242 0.171 Uani H 1.0 H1C21 0.6160 0.5220 0.6372 0.068 Uani H 1.0 H2C21 0.4124 0.5473 0.5777 0.068 Uani H 1.0 HC23 0.0412 0.5134 0.6517 0.135 Uani H 1.0 HC24 -0.1451 0.4421 0.6513 0.187 Uani H 1.0 HC25 0.0507 0.3727 0.6452 0.139 Uani H 1.0 HC26 0.4214 0.3757 0.6261 0.142 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol O1 0.079(2) 0.084(3) 0.055(2) -0.024(2) -0.016(1) 0.014(1) O O2 0.068(2) 0.072(2) 0.070(2) -0.023(1) -0.0044(8) 0.015(1) O N1 0.043(1) 0.037(2) 0.044(2) -0.0001(8) 0.0006(6) 0.0031(7) N N2 0.093(2) 0.095(3) 0.080(1) -0.007(2) -0.009(1) -0.002(1) N N3 0.117(8) 0.058(2) 0.084(2) 0.006(3) 0.020(1) -0.010(1) N N4 0.059(2) 0.045(1) 0.055(2) -0.002(1) 0.001(1) 0.014(1) N C1 0.056(2) 0.051(2) 0.069(2) -0.005(2) -0.004(2) 0.022(2) C C2 0.046(1) 0.040(2) 0.047(2) -0.0018(9) 0.0037(6) 0.0042(6) C C3 0.047(1) 0.052(3) 0.057(3) -0.004(1) 0.0072(9) 0.0056(8) C C4 0.043(1) 0.060(3) 0.062(3) -0.001(1) 0.0048(9) 0.005(1) C C5 0.043(1) 0.052(3) 0.054(2) 0.0034(9) 0.0003(7) 0.0030(8) C C6 0.043(1) 0.040(2) 0.046(2) 0.0020(9) -0.0005(6) 0.0027(6) C C7 0.047(1) 0.040(1) 0.0442(9) 0.0035(7) 0.0016(8) 0.0036(9) C C8 0.059(1) 0.056(2) 0.047(1) -0.004(1) -0.0037(8) 0.008(1) C C9 0.067(2) 0.060(3) 0.048(1) -0.003(1) -0.0008(9) 0.013(1) C C10 0.061(2) 0.052(2) 0.053(1) -0.001(1) 0.0059(8) 0.012(1) C C11 0.054(2) 0.049(1) 0.0540(9) -0.0035(7) 0.0029(7) 0.008(1) C C12 0.048(2) 0.042(1) 0.0464(7) 0.0016(7) 0.0015(7) 0.0043(9) C C13 0.103(3) 0.096(3) 0.059(2) -0.011(2) -0.029(2) 0.003(2) C C14 0.084(3) 0.067(2) 0.087(3) -0.028(2) 0.010(2) 0.015(2) C C15 0.072(2) 0.057(2) 0.064(2) 0.006(2) 0.001(2) 0.020(2) C C16 0.070(3) 0.054(2) 0.064(2) 0.004(2) -0.003(1) 0.022(1) C C17 0.077(3) 0.088(3) 0.084(2) 0.005(2) 0.011(2) 0.023(2) C C18 0.111(4) 0.109(4) 0.088(2) 0.031(3) 0.027(2) 0.031(2) C C19 0.156(5) 0.104(4) 0.074(1) 0.039(3) 0.014(2) 0.014(1) C C20 0.142(4) 0.121(3) 0.085(2) 0.003(2) -0.007(2) -0.016(2) C C21 0.073(3) 0.062(2) 0.069(2) 0.002(2) 0.013(2) 0.008(2) C C22 0.083(7) 0.063(2) 0.056(4) 0.002(3) 0.001(1) -0.005(1) C C23 0.081(7) 0.090(2) 0.131(6) -0.011(3) -0.004(2) 0.005(2) C C24 0.113(8) 0.113(3) 0.157(9) -0.040(4) -0.008(2) 0.007(3) C C25 0.164(9) 0.090(2) 0.083(5) -0.046(5) 0.000(2) -0.004(2) C C26 0.167(9) 0.063(2) 0.084(3) -0.013(4) 0.022(2) -0.012(1) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C8 1.377(3) 1_555 1_555 no O1 C13 1.418(3) 1_555 1_555 no O2 C11 1.371(3) 1_555 1_555 no O2 C14 1.422(3) 1_555 1_555 no N1 C2 1.338(3) 1_555 1_555 no N1 C6 1.345(3) 1_555 1_555 no N2 C16 1.327(4) 1_555 1_555 no N2 C20 1.346(5) 1_555 1_555 no N3 C22 1.330(4) 1_555 1_555 no N3 C26 1.366(5) 1_555 1_555 no N4 C1 1.464(3) 1_555 1_555 no N4 C15 1.465(3) 1_555 1_555 no N4 C21 1.469(4) 1_555 1_555 no C1 C2 1.514(4) 1_555 1_555 no C2 C3 1.388(4) 1_555 1_555 no C3 C4 1.373(4) 1_555 1_555 no C4 C5 1.380(4) 1_555 1_555 no C5 C6 1.386(3) 1_555 1_555 no C6 C7 1.491(3) 1_555 1_555 no C7 C8 1.396(3) 1_555 1_555 no C7 C12 1.392(3) 1_555 1_555 no C8 C9 1.370(4) 1_555 1_555 no C9 C10 1.396(4) 1_555 1_555 no C10 C11 1.373(4) 1_555 1_555 no C11 C12 1.388(3) 1_555 1_555 no C15 C16 1.506(4) 1_555 1_555 no C16 C17 1.377(4) 1_555 1_555 no C17 C18 1.381(5) 1_555 1_555 no C18 C19 1.368(6) 1_555 1_555 no C19 C20 1.371(6) 1_555 1_555 no C21 C22 1.517(4) 1_555 1_555 no C22 C23 1.381(5) 1_555 1_555 no C23 C24 1.370(6) 1_555 1_555 no C24 C25 1.350(6) 1_555 1_555 no C25 C26 1.379(6) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 O1 C13 118.6(2) 1_555 1_555 1_555 no C11 O2 C14 117.9(2) 1_555 1_555 1_555 no C2 N1 C6 117.8(2) 1_555 1_555 1_555 no C16 N2 C20 117.0(4) 1_555 1_555 1_555 no C22 N3 C26 116.1(4) 1_555 1_555 1_555 no C1 N4 C15 110.3(2) 1_555 1_555 1_555 no C1 N4 C21 110.3(2) 1_555 1_555 1_555 no C15 N4 C21 110.8(2) 1_555 1_555 1_555 no N4 C1 C2 112.0(2) 1_555 1_555 1_555 no N1 C2 C1 116.2(3) 1_555 1_555 1_555 no N1 C2 C3 123.2(3) 1_555 1_555 1_555 no C1 C2 C3 120.5(3) 1_555 1_555 1_555 no C2 C3 C4 118.1(3) 1_555 1_555 1_555 no C3 C4 C5 119.8(3) 1_555 1_555 1_555 no C4 C5 C6 118.7(3) 1_555 1_555 1_555 no N1 C6 C5 122.4(3) 1_555 1_555 1_555 no N1 C6 C7 116.4(2) 1_555 1_555 1_555 no C5 C6 C7 121.2(3) 1_555 1_555 1_555 no C6 C7 C8 122.9(3) 1_555 1_555 1_555 no C6 C7 C12 118.9(2) 1_555 1_555 1_555 no C8 C7 C12 118.1(3) 1_555 1_555 1_555 no O1 C8 C7 116.5(3) 1_555 1_555 1_555 no O1 C8 C9 123.1(3) 1_555 1_555 1_555 no C7 C8 C9 120.4(3) 1_555 1_555 1_555 no C8 C9 C10 120.9(3) 1_555 1_555 1_555 no C9 C10 C11 119.3(3) 1_555 1_555 1_555 no O2 C11 C10 125.1(3) 1_555 1_555 1_555 no O2 C11 C12 115.1(3) 1_555 1_555 1_555 no C10 C11 C12 119.8(3) 1_555 1_555 1_555 no C7 C12 C11 121.4(3) 1_555 1_555 1_555 no N4 C15 C16 110.7(2) 1_555 1_555 1_555 no N2 C16 C15 116.6(3) 1_555 1_555 1_555 no N2 C16 C17 122.4(3) 1_555 1_555 1_555 no C15 C16 C17 121.0(3) 1_555 1_555 1_555 no C16 C17 C18 119.3(4) 1_555 1_555 1_555 no C17 C18 C19 119.3(4) 1_555 1_555 1_555 no C18 C19 C20 117.6(4) 1_555 1_555 1_555 no N2 C20 C19 124.4(4) 1_555 1_555 1_555 no N4 C21 C22 111.4(3) 1_555 1_555 1_555 no N3 C22 C21 116.4(3) 1_555 1_555 1_555 no N3 C22 C23 122.9(4) 1_555 1_555 1_555 no C21 C22 C23 120.6(4) 1_555 1_555 1_555 no C22 C23 C24 119.8(4) 1_555 1_555 1_555 no C23 C24 C25 118.8(5) 1_555 1_555 1_555 no C24 C25 C26 119.1(5) 1_555 1_555 1_555 no N3 C26 C25 123.3(4) 1_555 1_555 1_555 no #===END data_[MnCl2(L)].MeOH _database_code_CSD 190790 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 Cl2 Mn N4 O2,C H4 O' _chemical_formula_sum 'C27 H30 Cl2 Mn N4 O3' _chemical_formula_iupac ? _chemical_formula_weight 584.4 # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2-x,1/2+y,1/2+z 4 1/2+x,1/2-y,z _cell_length_a 26.142(8) _cell_length_b 10.442(3) _cell_length_c 10.284(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2807(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.38 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212.0 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.92 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 2624 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ; Thermal motion was refined using two 15-parameter TLX rigid body thermal parameters, one for the hydroquinone, and the other with all remaining ligand atoms except the methyls. Individual anisotropic parameters were used for the metal, chlorines, methyl carbons and solvent atoms. ; _reflns_number_total 2624 _reflns_number_gt 1771 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.038 _refine_ls_abs_structure_details ; The polarity is confirmed, with the alternative giving R factor 0.034 ; _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1771 _refine_ls_number_parameters 183 _refine_ls_goodness_of_fit_ref 1.22 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.53 _refine_diff_density_min -0.83 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Mn 0.40091(3) 0.69755(6) 0.40000 0.0342(2) Uani Mn 1.0 Cl1 0.48125(5) 0.67949(12) 0.52810(17) 0.0500(4) Uani Cl 1.0 Cl2 0.35698(6) 0.87606(12) 0.49351(18) 0.0550(4) Uani Cl 1.0 O1 0.2396(2) 0.4758(5) 0.5986(5) 0.076(4) Uani O 1.0 O2 0.3716(2) 0.7815(4) 0.8804(5) 0.077(3) Uani O 1.0 N1 0.3802(2) 0.4826(4) 0.4683(4) 0.0369(7) Uani N 1.0 N2 0.3329(2) 0.6383(4) 0.2710(5) 0.050(1) Uani N 1.0 N3 0.4446(2) 0.8218(4) 0.2526(5) 0.0428(6) Uani N 1.0 N4 0.4353(2) 0.5647(4) 0.2413(4) 0.0425(7) Uani N 1.0 C1 0.4433(2) 0.4361(5) 0.3016(6) 0.0461(8) Uani C 1.0 C2 0.4001(2) 0.3962(4) 0.3852(6) 0.0407(7) Uani C 1.0 C3 0.3832(2) 0.2689(4) 0.3849(7) 0.051(1) Uani C 1.0 C4 0.3476(2) 0.2301(5) 0.4728(7) 0.053(1) Uani C 1.0 C5 0.3272(2) 0.3180(5) 0.5584(6) 0.0519(9) Uani C 1.0 C6 0.3444(2) 0.4446(5) 0.5529(6) 0.0451(9) Uani C 1.0 C7 0.3244(2) 0.5404(5) 0.6466(5) 0.042(2) Uani C 1.0 C8 0.2713(2) 0.5509(6) 0.6724(6) 0.058(3) Uani C 1.0 C9 0.2543(3) 0.6370(7) 0.7627(8) 0.072(4) Uani C 1.0 C10 0.2889(3) 0.7137(6) 0.8311(7) 0.068(3) Uani C 1.0 C11 0.3403(2) 0.7029(6) 0.8087(6) 0.058(2) Uani C 1.0 C12 0.3580(2) 0.6177(5) 0.7149(5) 0.047(2) Uani C 1.0 C13 0.1866(3) 0.4751(8) 0.6286(8) 0.086(3) Uani C 1.0 C14 0.4205(4) 0.8079(8) 0.8323(8) 0.100(3) Uani C 1.0 C15 0.3996(3) 0.5591(6) 0.1295(6) 0.056(1) Uani C 1.0 C16 0.3449(2) 0.5596(6) 0.1732(6) 0.057(1) Uani C 1.0 C17 0.3084(3) 0.4865(7) 0.1101(7) 0.078(2) Uani C 1.0 C18 0.2579(3) 0.4920(8) 0.1535(10) 0.091(2) Uani C 1.0 C19 0.2463(2) 0.5725(7) 0.2537(9) 0.085(2) Uani C 1.0 C20 0.2842(2) 0.6452(6) 0.3110(8) 0.066(1) Uani C 1.0 C21 0.4847(2) 0.6192(5) 0.1982(6) 0.0518(7) Uani C 1.0 C22 0.4808(2) 0.7627(5) 0.1832(6) 0.0498(7) Uani C 1.0 C23 0.5153(3) 0.8304(6) 0.1069(7) 0.066(1) Uani C 1.0 C24 0.5128(3) 0.9620(6) 0.1042(7) 0.069(1) Uani C 1.0 C25 0.4758(3) 1.0235(6) 0.1734(7) 0.063(1) Uani C 1.0 C26 0.4416(2) 0.9507(5) 0.2455(6) 0.0517(9) Uani C 1.0 O1Me 0.5988(3) 0.7499(9) 0.4872(11) 0.175(4) Uani O 1.0 C1Me 0.6118(8) 0.7908(19) 0.3779(15) 0.234(9) Uani C 1.0 H1C1 0.4750 0.4390 0.3557 0.050 Uani H 1.0 H2C1 0.4476 0.3715 0.2307 0.059 Uani H 1.0 HC3 0.3973 0.2067 0.3202 0.063 Uani H 1.0 HC4 0.3362 0.1386 0.4753 0.063 Uani H 1.0 HC5 0.3006 0.2917 0.6231 0.063 Uani H 1.0 HC9 0.2167 0.6452 0.7800 0.097 Uani H 1.0 HC10 0.2760 0.7768 0.8966 0.083 Uani H 1.0 HC12 0.3955 0.6122 0.6966 0.054 Uani H 1.0 H1C13 0.1682 0.4166 0.5674 0.086 Uani H 1.0 H2C13 0.1816 0.4445 0.7199 0.086 Uani H 1.0 H3C13 0.1726 0.5638 0.6198 0.086 Uani H 1.0 H1C14 0.4389 0.8658 0.8941 0.100 Uani H 1.0 H2C14 0.4401 0.7261 0.8228 0.100 Uani H 1.0 H3C14 0.4176 0.8507 0.7457 0.100 Uani H 1.0 H1C15 0.4063 0.4788 0.0792 0.069 Uani H 1.0 H2C15 0.4057 0.6350 0.0724 0.064 Uani H 1.0 HC17 0.3180 0.4308 0.0348 0.093 Uani H 1.0 HC18 0.2307 0.4382 0.1120 0.112 Uani H 1.0 HC19 0.2103 0.5789 0.2858 0.105 Uani H 1.0 HC20 0.2752 0.7043 0.3840 0.072 Uani H 1.0 H1C21 0.4943 0.5804 0.1127 0.068 Uani H 1.0 H2C21 0.5116 0.5987 0.2642 0.054 Uani H 1.0 HC23 0.5417 0.7840 0.0544 0.081 Uani H 1.0 HC24 0.5380 1.0122 0.0517 0.084 Uani H 1.0 HC25 0.4734 1.1190 0.1724 0.073 Uani H 1.0 HC26 0.4137 0.9954 0.2941 0.057 Uani H 1.0 HO1Me 0.5661 0.7084 0.4594 0.175 Uani H 1.0 H1C1Me 0.6451 0.8373 0.3855 0.234 Uani H 1.0 H2C1Me 0.6158 0.7172 0.3165 0.234 Uani H 1.0 H3C1Me 0.5850 0.8506 0.3443 0.234 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Mn 0.0336(3) 0.0275(3) 0.0414(4) 0.0020(3) 0.0025(5) -0.0006(5) Mn Cl1 0.0444(7) 0.0457(7) 0.0598(9) 0.0001(6) -0.0119(7) 0.0019(8) Cl Cl2 0.0596(8) 0.0395(7) 0.0657(9) 0.0136(7) 0.0172(8) -0.0002(8) Cl O1 0.046(3) 0.100(5) 0.081(4) -0.011(3) 0.017(3) -0.026(4) O O2 0.088(4) 0.078(3) 0.065(3) -0.019(2) 0.015(2) -0.023(3) O N1 0.035(1) 0.0310(8) 0.045(1) 0.0025(8) 0.0026(9) -0.0012(7) N N2 0.040(1) 0.044(1) 0.068(1) -0.0013(9) -0.013(1) 0.010(1) N N3 0.0440(9) 0.0350(8) 0.0493(9) -0.0007(7) 0.001(1) 0.0033(7) N N4 0.0474(9) 0.0356(8) 0.045(1) 0.0001(7) 0.0092(9) -0.0066(8) N C1 0.047(1) 0.0319(8) 0.060(2) 0.0053(8) 0.0134(8) -0.0082(9) C C2 0.041(1) 0.0291(9) 0.052(1) 0.0030(8) 0.0037(8) -0.0038(8) C C3 0.056(2) 0.0301(9) 0.066(2) -0.0009(8) 0.005(1) -0.0044(8) C C4 0.056(2) 0.0347(8) 0.069(2) -0.0064(9) 0.001(1) 0.0031(9) C C5 0.051(1) 0.0423(9) 0.063(1) -0.0075(8) 0.0063(9) 0.0056(9) C C6 0.044(1) 0.0392(8) 0.052(1) -0.0021(8) 0.0088(8) 0.0008(7) C C7 0.046(2) 0.041(3) 0.040(2) -0.002(2) 0.009(2) 0.008(2) C C8 0.048(3) 0.068(3) 0.059(3) -0.003(3) 0.015(2) -0.007(2) C C9 0.058(3) 0.085(5) 0.074(4) 0.002(3) 0.022(3) -0.019(4) C C10 0.072(3) 0.068(4) 0.063(3) 0.001(2) 0.021(2) -0.013(3) C C11 0.069(3) 0.056(2) 0.050(2) -0.006(2) 0.013(2) -0.005(2) C C12 0.053(2) 0.047(2) 0.042(2) -0.004(2) 0.008(2) 0.004(2) C C13 0.045(4) 0.119(6) 0.093(6) -0.008(4) 0.014(4) -0.031(5) C C14 0.110(6) 0.111(7) 0.080(5) -0.047(5) -0.003(5) -0.028(5) C C15 0.076(2) 0.050(2) 0.042(1) -0.015(1) 0.000(1) -0.0046(9) C C16 0.063(2) 0.053(2) 0.055(1) -0.015(1) -0.019(2) 0.007(1) C C17 0.091(3) 0.073(3) 0.070(2) -0.033(2) -0.037(2) 0.013(2) C C18 0.076(3) 0.085(3) 0.111(3) -0.033(2) -0.051(3) 0.030(3) C C19 0.045(2) 0.075(3) 0.136(4) -0.012(1) -0.034(2) 0.032(3) C C20 0.035(2) 0.055(2) 0.108(2) 0.002(1) -0.013(1) 0.019(2) C C21 0.0534(9) 0.0432(8) 0.059(2) -0.0004(8) 0.0220(9) -0.007(1) C C22 0.053(1) 0.0443(9) 0.052(1) -0.0052(8) 0.0128(9) 0.0003(8) C C23 0.072(2) 0.059(1) 0.065(2) -0.014(1) 0.024(1) 0.004(1) C C24 0.078(2) 0.059(1) 0.070(2) -0.019(1) 0.014(2) 0.013(1) C C25 0.070(2) 0.045(1) 0.073(2) -0.011(1) -0.001(2) 0.016(1) C C26 0.054(1) 0.0354(9) 0.066(1) -0.0018(8) -0.002(1) 0.0090(9) C O1Me 0.093(5) 0.193(7) 0.240(9) 0.004(5) -0.004(6) 0.097(8) O C1Me 0.240(9) 0.333(9) 0.128(9) -0.151(9) -0.005(9) 0.048(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn Cl1 2.486(1) 1_555 1_555 no Mn Cl2 2.391(1) 1_555 1_555 no Mn N1 2.413(4) 1_555 1_555 no Mn N2 2.303(5) 1_555 1_555 no Mn N3 2.300(4) 1_555 1_555 no Mn N4 2.322(4) 1_555 1_555 no O1 C8 1.371(7) 1_555 1_555 no O1 C13 1.420(7) 1_555 1_555 no O2 C11 1.374(7) 1_555 1_555 no O2 C14 1.398(9) 1_555 1_555 no N1 C2 1.347(6) 1_555 1_555 no N1 C6 1.339(6) 1_555 1_555 no N2 C16 1.336(8) 1_555 1_555 no N2 C20 1.339(7) 1_555 1_555 no N3 C22 1.336(7) 1_555 1_555 no N3 C26 1.350(6) 1_555 1_555 no N4 C1 1.494(6) 1_555 1_555 no N4 C15 1.482(7) 1_555 1_555 no N4 C21 1.479(7) 1_555 1_555 no C1 C2 1.479(7) 1_555 1_555 no C2 C3 1.400(6) 1_555 1_555 no C3 C4 1.359(8) 1_555 1_555 no C4 C5 1.379(8) 1_555 1_555 no C5 C6 1.398(7) 1_555 1_555 no C6 C7 1.484(7) 1_555 1_555 no C7 C8 1.417(8) 1_555 1_555 no C7 C12 1.384(7) 1_555 1_555 no C8 C9 1.368(9) 1_555 1_555 no C9 C10 1.399(9) 1_555 1_555 no C10 C11 1.368(9) 1_555 1_555 no C11 C12 1.391(8) 1_555 1_555 no C15 C16 1.500(9) 1_555 1_555 no C16 C17 1.384(8) 1_555 1_555 no C17 C18 1.395(11) 1_555 1_555 no C18 C19 1.364(12) 1_555 1_555 no C19 C20 1.381(9) 1_555 1_555 no C21 C22 1.510(8) 1_555 1_555 no C22 C23 1.389(8) 1_555 1_555 no C23 C24 1.377(9) 1_555 1_555 no C24 C25 1.361(8) 1_555 1_555 no C25 C26 1.388(8) 1_555 1_555 no O1Me C1Me 1.250(15) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Mn Cl2 104.58(6) 1_555 1_555 1_555 no Cl1 Mn N1 87.9(1) 1_555 1_555 1_555 no Cl1 Mn N2 159.5(1) 1_555 1_555 1_555 no Cl1 Mn N3 88.4(1) 1_555 1_555 1_555 no Cl1 Mn N4 90.0(1) 1_555 1_555 1_555 no Cl2 Mn N1 120.0(1) 1_555 1_555 1_555 no Cl2 Mn N2 94.0(1) 1_555 1_555 1_555 no Cl2 Mn N3 93.7(1) 1_555 1_555 1_555 no Cl2 Mn N4 159.1(1) 1_555 1_555 1_555 no N1 Mn N2 75.2(2) 1_555 1_555 1_555 no N1 Mn N3 145.9(1) 1_555 1_555 1_555 no N1 Mn N4 74.7(1) 1_555 1_555 1_555 no N2 Mn N3 99.0(2) 1_555 1_555 1_555 no N2 Mn N4 74.5(2) 1_555 1_555 1_555 no N3 Mn N4 71.4(2) 1_555 1_555 1_555 no C8 O1 C13 118.2(5) 1_555 1_555 1_555 no C11 O2 C14 118.2(5) 1_555 1_555 1_555 no Mn N1 C2 110.6(3) 1_555 1_555 1_555 no Mn N1 C6 128.4(3) 1_555 1_555 1_555 no C2 N1 C6 118.9(4) 1_555 1_555 1_555 no Mn N2 C16 114.7(4) 1_555 1_555 1_555 no Mn N2 C20 122.8(5) 1_555 1_555 1_555 no C16 N2 C20 119.2(6) 1_555 1_555 1_555 no Mn N3 C22 116.3(3) 1_555 1_555 1_555 no Mn N3 C26 124.7(4) 1_555 1_555 1_555 no C22 N3 C26 118.3(5) 1_555 1_555 1_555 no Mn N4 C1 107.4(3) 1_555 1_555 1_555 no Mn N4 C15 109.0(3) 1_555 1_555 1_555 no Mn N4 C21 108.6(3) 1_555 1_555 1_555 no C1 N4 C15 112.0(4) 1_555 1_555 1_555 no C1 N4 C21 110.3(4) 1_555 1_555 1_555 no C15 N4 C21 109.4(4) 1_555 1_555 1_555 no N4 C1 C2 112.8(4) 1_555 1_555 1_555 no N1 C2 C1 118.3(4) 1_555 1_555 1_555 no N1 C2 C3 121.1(5) 1_555 1_555 1_555 no C1 C2 C3 120.5(5) 1_555 1_555 1_555 no C2 C3 C4 119.8(5) 1_555 1_555 1_555 no C3 C4 C5 119.4(5) 1_555 1_555 1_555 no C4 C5 C6 118.6(5) 1_555 1_555 1_555 no N1 C6 C5 122.2(5) 1_555 1_555 1_555 no N1 C6 C7 117.9(4) 1_555 1_555 1_555 no C5 C6 C7 119.8(5) 1_555 1_555 1_555 no C6 C7 C8 121.2(5) 1_555 1_555 1_555 no C6 C7 C12 120.0(5) 1_555 1_555 1_555 no C8 C7 C12 118.7(5) 1_555 1_555 1_555 no O1 C8 C7 116.4(5) 1_555 1_555 1_555 no O1 C8 C9 123.7(6) 1_555 1_555 1_555 no C7 C8 C9 119.8(6) 1_555 1_555 1_555 no C8 C9 C10 120.4(6) 1_555 1_555 1_555 no C9 C10 C11 120.3(6) 1_555 1_555 1_555 no O2 C11 C10 116.5(6) 1_555 1_555 1_555 no O2 C11 C12 123.8(6) 1_555 1_555 1_555 no C10 C11 C12 119.8(6) 1_555 1_555 1_555 no C7 C12 C11 120.9(5) 1_555 1_555 1_555 no N4 C15 C16 111.6(5) 1_555 1_555 1_555 no N2 C16 C15 116.8(5) 1_555 1_555 1_555 no N2 C16 C17 122.1(7) 1_555 1_555 1_555 no C15 C16 C17 121.0(6) 1_555 1_555 1_555 no C16 C17 C18 118.7(8) 1_555 1_555 1_555 no C17 C18 C19 118.5(7) 1_555 1_555 1_555 no C18 C19 C20 120.1(7) 1_555 1_555 1_555 no N2 C20 C19 121.4(7) 1_555 1_555 1_555 no N4 C21 C22 110.7(5) 1_555 1_555 1_555 no N3 C22 C21 116.9(5) 1_555 1_555 1_555 no N3 C22 C23 121.7(5) 1_555 1_555 1_555 no C21 C22 C23 121.3(5) 1_555 1_555 1_555 no C22 C23 C24 119.2(6) 1_555 1_555 1_555 no C23 C24 C25 119.6(6) 1_555 1_555 1_555 no C24 C25 C26 118.6(5) 1_555 1_555 1_555 no N3 C26 C25 122.5(5) 1_555 1_555 1_555 no #===END data_[FeCl2(L)].MeOH _database_code_CSD 190791 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 Cl2 Fe N4 O2,C H4 O' _chemical_formula_sum 'C27 H30 Cl2 Fe1 N4 O3' _chemical_formula_iupac ? _chemical_formula_weight 585.3 # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2-x,1/2+y,1/2+z 4 1/2+x,1/2-y,z _cell_length_a 26.009(15) _cell_length_b 10.354(3) _cell_length_c 10.268(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2765(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216.0 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.90 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 2583 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ; Thermal motion was refined using two 15-parameter TLX rigid body thermal parameters, one for the hydroquinone, and the other with all remaining ligand atoms except the methyls. Individual anisotropic parameters were used for the metal, chlorines, methyl carbons and solvent atoms. ; _reflns_number_total 2583 _reflns_number_gt 2069 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.041 _refine_ls_abs_structure_details ; The polarity is confirmed, with the alternative giving R_factor 0.037 ; _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2069 _refine_ls_number_parameters 183 _refine_ls_goodness_of_fit_ref 1.22 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 0.45 _refine_diff_density_min -0.72 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Fe 0.40103(2) 0.69412(6) 0.40000 0.0317(2) Uani Fe 1.0 Cl1 0.48052(5) 0.67858(12) 0.53177(15) 0.0455(3) Uani Cl 1.0 Cl2 0.35793(5) 0.86594(12) 0.49735(16) 0.0505(4) Uani Cl 1.0 O1 0.2396(2) 0.4818(4) 0.6026(5) 0.068(3) Uani O 1.0 O2 0.3730(2) 0.7848(4) 0.8883(5) 0.072(3) Uani O 1.0 N1 0.3805(1) 0.4846(4) 0.4741(4) 0.0343(7) Uani N 1.0 N2 0.3345(2) 0.6370(4) 0.2770(5) 0.0447(9) Uani N 1.0 N3 0.4445(2) 0.8210(4) 0.2632(4) 0.0381(6) Uani N 1.0 N4 0.4362(2) 0.5646(4) 0.2505(4) 0.0375(7) Uani N 1.0 C1 0.4442(2) 0.4355(5) 0.3087(5) 0.0414(7) Uani C 1.0 C2 0.4005(2) 0.3952(4) 0.3935(7) 0.0371(7) Uani C 1.0 C3 0.3835(2) 0.2674(4) 0.3943(7) 0.046(1) Uani C 1.0 C4 0.3473(2) 0.2297(5) 0.4822(6) 0.0486(9) Uani C 1.0 C5 0.3267(2) 0.3201(5) 0.5674(6) 0.0479(9) Uani C 1.0 C6 0.3441(2) 0.4473(5) 0.5591(5) 0.0420(8) Uani C 1.0 C7 0.3246(2) 0.5438(5) 0.6533(5) 0.040(2) Uani C 1.0 C8 0.2713(2) 0.5563(6) 0.6779(6) 0.054(3) Uani C 1.0 C9 0.2543(2) 0.6434(7) 0.7677(7) 0.066(3) Uani C 1.0 C10 0.2893(3) 0.7188(6) 0.8395(6) 0.063(3) Uani C 1.0 C11 0.3410(2) 0.7077(6) 0.8154(6) 0.055(2) Uani C 1.0 C12 0.3585(2) 0.6207(5) 0.7218(5) 0.044(2) Uani C 1.0 C13 0.1869(2) 0.4800(8) 0.6358(8) 0.082(2) Uani C 1.0 C14 0.4217(3) 0.8108(8) 0.8409(7) 0.087(2) Uani C 1.0 C15 0.4017(2) 0.5585(5) 0.1367(5) 0.048(1) Uani C 1.0 C16 0.3456(2) 0.5607(6) 0.1769(6) 0.050(1) Uani C 1.0 C17 0.3096(3) 0.4881(6) 0.1120(7) 0.069(2) Uani C 1.0 C18 0.2587(3) 0.4947(7) 0.1545(9) 0.081(2) Uani C 1.0 C19 0.2469(2) 0.5742(7) 0.2581(9) 0.077(2) Uani C 1.0 C20 0.2856(2) 0.6441(6) 0.3152(7) 0.059(1) Uani C 1.0 C21 0.4861(2) 0.6191(5) 0.2084(6) 0.0455(7) Uani C 1.0 C22 0.4814(2) 0.7638(5) 0.1944(6) 0.0434(6) Uani C 1.0 C23 0.5161(2) 0.8335(5) 0.1175(7) 0.0566(9) Uani C 1.0 C24 0.5118(3) 0.9665(6) 0.1129(7) 0.060(1) Uani C 1.0 C25 0.4740(2) 1.0256(6) 0.1826(7) 0.055(1) Uani C 1.0 C26 0.4406(2) 0.9504(5) 0.2570(6) 0.0460(8) Uani C 1.0 O1Me 0.5975(2) 0.7500(8) 0.4939(10) 0.148(3) Uani O 1.0 C1Me 0.6139(6) 0.7847(18) 0.3827(14) 0.211(8) Uani C 1.0 H1C1 0.4763 0.4374 0.3622 0.046 Uani H 1.0 H2C1 0.4481 0.3709 0.2369 0.052 Uani H 1.0 HC3 0.3979 0.2038 0.3307 0.056 Uani H 1.0 HC4 0.3356 0.1378 0.4853 0.058 Uani H 1.0 HC5 0.3002 0.2947 0.6330 0.058 Uani H 1.0 HC9 0.2165 0.6538 0.7828 0.086 Uani H 1.0 HC10 0.2766 0.7801 0.9076 0.076 Uani H 1.0 HC12 0.3962 0.6140 0.7039 0.048 Uani H 1.0 H1C13 0.1679 0.4226 0.5741 0.082 Uani H 1.0 H2C13 0.1828 0.4467 0.7266 0.082 Uani H 1.0 H3C13 0.1727 0.5696 0.6303 0.082 Uani H 1.0 H1C14 0.4405 0.8676 0.9037 0.087 Uani H 1.0 H2C14 0.4410 0.7280 0.8297 0.087 Uani H 1.0 H3C14 0.4189 0.8555 0.7549 0.087 Uani H 1.0 H1C15 0.4086 0.4769 0.0877 0.059 Uani H 1.0 H2C15 0.4087 0.6344 0.0791 0.054 Uani H 1.0 HC17 0.3196 0.4322 0.0367 0.082 Uani H 1.0 HC18 0.2313 0.4429 0.1106 0.101 Uani H 1.0 HC19 0.2108 0.5806 0.2909 0.094 Uani H 1.0 HC20 0.2767 0.7032 0.3889 0.064 Uani H 1.0 H1C21 0.4962 0.5805 0.1228 0.058 Uani H 1.0 H2C21 0.5130 0.5985 0.2749 0.049 Uani H 1.0 HC23 0.5434 0.7879 0.0668 0.070 Uani H 1.0 HC24 0.5362 1.0186 0.0590 0.072 Uani H 1.0 HC25 0.4702 1.1217 0.1805 0.064 Uani H 1.0 HC26 0.4127 0.9942 0.3075 0.052 Uani H 1.0 HO1Me 0.5604 0.7274 0.5059 0.148 Uani H 1.0 H1C1Me 0.6515 0.8036 0.3882 0.211 Uani H 1.0 H2C1Me 0.6079 0.7138 0.3184 0.211 Uani H 1.0 H3C1Me 0.5951 0.8641 0.3541 0.211 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Fe 0.0314(3) 0.0270(3) 0.0368(3) 0.0021(3) 0.0026(4) -0.0010(4) Fe Cl1 0.0408(7) 0.0447(7) 0.0511(8) -0.0006(6) -0.0091(6) 0.0026(7) Cl Cl2 0.0559(8) 0.0383(7) 0.0573(8) 0.0129(6) 0.0157(7) -0.0007(7) Cl O1 0.042(4) 0.095(4) 0.069(4) -0.009(3) 0.013(3) -0.022(3) O O2 0.084(4) 0.075(3) 0.056(2) -0.015(2) 0.011(2) -0.023(2) O N1 0.033(1) 0.0317(8) 0.038(1) 0.0015(7) 0.0020(7) -0.0012(6) N N2 0.034(1) 0.042(1) 0.058(1) -0.0006(9) -0.010(1) 0.0080(8) N N3 0.0387(9) 0.0332(8) 0.0423(7) -0.0003(7) 0.0008(8) 0.0016(6) N N4 0.0405(9) 0.0336(8) 0.0385(9) 0.0010(7) 0.0069(8) -0.0052(7) N C1 0.0418(9) 0.0313(8) 0.051(1) 0.0051(7) 0.0105(8) -0.0058(9) C C2 0.0378(9) 0.0295(8) 0.0440(9) 0.0023(7) 0.0024(7) -0.0027(7) C C3 0.052(2) 0.0303(9) 0.056(1) -0.0013(7) 0.0035(9) -0.0028(8) C C4 0.052(2) 0.0352(8) 0.058(1) -0.0068(8) 0.001(1) 0.0031(8) C C5 0.048(1) 0.0423(8) 0.054(1) -0.0076(7) 0.0061(8) 0.0048(8) C C6 0.041(1) 0.0391(8) 0.045(1) -0.0026(7) 0.0081(6) 0.0004(6) C C7 0.043(2) 0.041(3) 0.036(2) 0.000(2) 0.005(2) 0.004(2) C C8 0.045(3) 0.065(3) 0.052(2) -0.001(2) 0.012(2) -0.008(2) C C9 0.055(3) 0.079(4) 0.063(3) 0.005(3) 0.017(2) -0.016(3) C C10 0.069(3) 0.064(3) 0.055(2) 0.003(2) 0.017(2) -0.012(2) C C11 0.065(3) 0.054(2) 0.045(2) -0.004(2) 0.010(1) -0.007(2) C C12 0.050(2) 0.045(2) 0.037(2) -0.002(2) 0.004(1) 0.001(1) C C13 0.045(4) 0.122(6) 0.079(5) -0.012(4) 0.013(4) -0.026(5) C C14 0.088(5) 0.100(6) 0.072(5) -0.040(5) 0.005(4) -0.018(5) C C15 0.064(2) 0.045(1) 0.0357(9) -0.011(1) 0.000(1) -0.0042(8) C C16 0.054(2) 0.049(2) 0.0471(8) -0.012(1) -0.016(1) 0.0056(9) C C17 0.079(3) 0.068(3) 0.060(1) -0.029(2) -0.032(2) 0.011(1) C C18 0.066(3) 0.081(3) 0.097(2) -0.030(2) -0.044(2) 0.027(2) C C19 0.039(2) 0.073(3) 0.118(3) -0.010(1) -0.027(1) 0.030(2) C C20 0.031(2) 0.053(2) 0.092(2) 0.002(1) -0.0096(9) 0.017(1) C C21 0.0447(8) 0.0402(8) 0.052(1) 0.0011(8) 0.0172(9) -0.0046(9) C C22 0.0446(9) 0.0406(8) 0.045(1) -0.0034(7) 0.0095(9) 0.0002(7) C C23 0.060(1) 0.053(1) 0.057(2) -0.010(1) 0.019(1) 0.003(1) C C24 0.066(2) 0.052(1) 0.061(2) -0.015(1) 0.010(1) 0.010(1) C C25 0.062(2) 0.0407(9) 0.063(2) -0.0091(9) 0.000(1) 0.011(1) C C26 0.049(1) 0.0334(8) 0.056(1) -0.0011(7) -0.0006(8) 0.0055(8) C O1Me 0.075(4) 0.177(7) 0.193(9) 0.000(4) 0.011(5) 0.071(7) O C1Me 0.180(9) 0.343(9) 0.111(9) -0.108(9) 0.001(9) 0.037(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe Cl1 2.476(1) 1_555 1_555 no Fe Cl2 2.328(1) 1_555 1_555 no Fe N1 2.360(4) 1_555 1_555 no Fe N2 2.223(4) 1_555 1_555 no Fe N3 2.231(4) 1_555 1_555 no Fe N4 2.235(4) 1_555 1_555 no O1 C8 1.369(7) 1_555 1_555 no O1 C13 1.411(7) 1_555 1_555 no O2 C11 1.375(7) 1_555 1_555 no O2 C14 1.384(8) 1_555 1_555 no N1 C2 1.347(6) 1_555 1_555 no N1 C6 1.343(6) 1_555 1_555 no N2 C16 1.328(7) 1_555 1_555 no N2 C20 1.334(7) 1_555 1_555 no N3 C22 1.330(6) 1_555 1_555 no N3 C26 1.346(6) 1_555 1_555 no N4 C1 1.479(6) 1_555 1_555 no N4 C15 1.476(7) 1_555 1_555 no N4 C21 1.479(6) 1_555 1_555 no C1 C2 1.492(7) 1_555 1_555 no C2 C3 1.395(6) 1_555 1_555 no C3 C4 1.363(8) 1_555 1_555 no C4 C5 1.388(8) 1_555 1_555 no C5 C6 1.395(7) 1_555 1_555 no C6 C7 1.481(7) 1_555 1_555 no C7 C8 1.415(7) 1_555 1_555 no C7 C12 1.381(7) 1_555 1_555 no C8 C9 1.364(9) 1_555 1_555 no C9 C10 1.409(9) 1_555 1_555 no C10 C11 1.371(9) 1_555 1_555 no C11 C12 1.394(7) 1_555 1_555 no C15 C16 1.517(8) 1_555 1_555 no C16 C17 1.372(8) 1_555 1_555 no C17 C18 1.397(10) 1_555 1_555 no C18 C19 1.379(11) 1_555 1_555 no C19 C20 1.371(9) 1_555 1_555 no C21 C22 1.511(7) 1_555 1_555 no C22 C23 1.398(7) 1_555 1_555 no C23 C24 1.382(8) 1_555 1_555 no C24 C25 1.362(7) 1_555 1_555 no C25 C26 1.394(7) 1_555 1_555 no O1Me C1Me 1.270(14) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Fe Cl2 102.53(5) 1_555 1_555 1_555 no Cl1 Fe N1 87.3(1) 1_555 1_555 1_555 no Cl1 Fe N2 160.6(1) 1_555 1_555 1_555 no Cl1 Fe N3 87.7(1) 1_555 1_555 1_555 no Cl1 Fe N4 89.7(1) 1_555 1_555 1_555 no Cl2 Fe N1 117.1(1) 1_555 1_555 1_555 no Cl2 Fe N2 94.2(1) 1_555 1_555 1_555 no Cl2 Fe N3 93.7(1) 1_555 1_555 1_555 no Cl2 Fe N4 161.9(1) 1_555 1_555 1_555 no N1 Fe N2 76.2(2) 1_555 1_555 1_555 no N1 Fe N3 149.2(1) 1_555 1_555 1_555 no N1 Fe N4 76.3(1) 1_555 1_555 1_555 no N2 Fe N3 101.2(2) 1_555 1_555 1_555 no N2 Fe N4 76.6(2) 1_555 1_555 1_555 no N3 Fe N4 73.3(2) 1_555 1_555 1_555 no C8 O1 C13 117.1(5) 1_555 1_555 1_555 no C11 O2 C14 118.4(5) 1_555 1_555 1_555 no Fe N1 C2 110.3(3) 1_555 1_555 1_555 no Fe N1 C6 129.3(3) 1_555 1_555 1_555 no C2 N1 C6 118.3(4) 1_555 1_555 1_555 no Fe N2 C16 115.4(4) 1_555 1_555 1_555 no Fe N2 C20 124.1(4) 1_555 1_555 1_555 no C16 N2 C20 117.9(5) 1_555 1_555 1_555 no Fe N3 C22 116.0(3) 1_555 1_555 1_555 no Fe N3 C26 125.3(4) 1_555 1_555 1_555 no C22 N3 C26 118.2(5) 1_555 1_555 1_555 no Fe N4 C1 108.8(3) 1_555 1_555 1_555 no Fe N4 C15 108.7(3) 1_555 1_555 1_555 no Fe N4 C21 109.3(3) 1_555 1_555 1_555 no C1 N4 C15 111.5(4) 1_555 1_555 1_555 no C1 N4 C21 109.9(4) 1_555 1_555 1_555 no C15 N4 C21 108.7(4) 1_555 1_555 1_555 no N4 C1 C2 112.5(4) 1_555 1_555 1_555 no N1 C2 C1 117.5(4) 1_555 1_555 1_555 no N1 C2 C3 121.8(5) 1_555 1_555 1_555 no C1 C2 C3 120.6(5) 1_555 1_555 1_555 no C2 C3 C4 119.6(5) 1_555 1_555 1_555 no C3 C4 C5 119.4(5) 1_555 1_555 1_555 no C4 C5 C6 118.2(5) 1_555 1_555 1_555 no N1 C6 C5 122.7(5) 1_555 1_555 1_555 no N1 C6 C7 118.1(4) 1_555 1_555 1_555 no C5 C6 C7 119.1(5) 1_555 1_555 1_555 no C6 C7 C8 120.9(5) 1_555 1_555 1_555 no C6 C7 C12 120.2(5) 1_555 1_555 1_555 no C8 C7 C12 118.8(5) 1_555 1_555 1_555 no O1 C8 C7 116.0(5) 1_555 1_555 1_555 no O1 C8 C9 124.0(6) 1_555 1_555 1_555 no C7 C8 C9 119.9(6) 1_555 1_555 1_555 no C8 C9 C10 120.7(6) 1_555 1_555 1_555 no C9 C10 C11 119.6(6) 1_555 1_555 1_555 no O2 C11 C10 116.5(5) 1_555 1_555 1_555 no O2 C11 C12 123.6(5) 1_555 1_555 1_555 no C10 C11 C12 119.9(6) 1_555 1_555 1_555 no C7 C12 C11 121.0(5) 1_555 1_555 1_555 no N4 C15 C16 111.7(4) 1_555 1_555 1_555 no N2 C16 C15 115.3(5) 1_555 1_555 1_555 no N2 C16 C17 123.7(6) 1_555 1_555 1_555 no C15 C16 C17 121.0(6) 1_555 1_555 1_555 no C16 C17 C18 117.9(7) 1_555 1_555 1_555 no C17 C18 C19 118.7(6) 1_555 1_555 1_555 no C18 C19 C20 118.9(7) 1_555 1_555 1_555 no N2 C20 C19 122.9(7) 1_555 1_555 1_555 no N4 C21 C22 109.6(4) 1_555 1_555 1_555 no N3 C22 C21 116.7(5) 1_555 1_555 1_555 no N3 C22 C23 122.3(5) 1_555 1_555 1_555 no C21 C22 C23 120.9(5) 1_555 1_555 1_555 no C22 C23 C24 118.8(6) 1_555 1_555 1_555 no C23 C24 C25 119.2(5) 1_555 1_555 1_555 no C24 C25 C26 119.1(5) 1_555 1_555 1_555 no N3 C26 C25 122.3(5) 1_555 1_555 1_555 no #===END data_[CoCl(L)][BPh4] _database_code_CSD 190792 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 Cl Co N4 O2 1+, C24 H20 B 1-' _chemical_formula_sum 'C50 H46 B Cl Co N4 O2' _chemical_formula_iupac ? _chemical_formula_weight 840.1 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 9.759(5) _cell_length_b 15.821(4) _cell_length_c 28.626(19) _cell_angle_alpha 90 _cell_angle_beta 103.95(3) _cell_angle_gamma 90 _cell_volume 4289(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.15 _exptl_crystal_density_diffrn 1.30 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756.0 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 7683 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ; Anion phenyls were described as identical planar groups with refineable mm2 symmetry. Thermal motion of the cation was refined using two 15-parameter TLX rigid body thermal parameters, one for the hydroquinone, and the other with all remaining ligand atoms except the methyls. Individual anisotropic parameters were used for the metal, chlorine, and methyl carbons. Each phenyl of the anion was refined using a 12 parameter TL rigid group thermal parameter, with the centre of libration at the central boron atom, which had a single atom anisotropic thermal parameter. ; _reflns_number_total 7520 _reflns_number_gt 3699 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.057 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3699 _refine_ls_number_parameters 243 _refine_ls_goodness_of_fit_ref 1.43 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.005 _refine_diff_density_max 0.55 _refine_diff_density_min -0.48 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Co 0.92705(7) 0.18379(4) 0.13124(2) 0.0457(2) Uani Co 1.0 Cl 1.08261(14) 0.08897(9) 0.11485(5) 0.0741(4) Uani Cl 1.0 O1 0.6712(5) 0.1182(3) 0.0359(1) 0.108(6) Uani O 1.0 O2 0.9381(7) -0.1881(3) 0.0697(2) 0.148(7) Uani O 1.0 N1 0.7390(4) 0.1249(3) 0.1404(1) 0.0501(7) Uani N 1.0 N2 0.9003(4) 0.2683(3) 0.0742(1) 0.0535(6) Uani N 1.0 N3 1.0600(4) 0.2280(2) 0.1959(1) 0.0456(5) Uani N 1.0 N4 0.8084(4) 0.2878(2) 0.1530(1) 0.0460(6) Uani N 1.0 C1 0.7255(5) 0.2536(3) 0.1856(2) 0.0483(7) Uani C 1.0 C2 0.6693(5) 0.1679(3) 0.1681(2) 0.0509(7) Uani C 1.0 C3 0.5521(5) 0.1364(4) 0.1813(2) 0.0630(8) Uani C 1.0 C4 0.5054(6) 0.0568(4) 0.1659(2) 0.075(1) Uani C 1.0 C5 0.5750(6) 0.0120(4) 0.1369(2) 0.076(1) Uani C 1.0 C6 0.6893(6) 0.0486(3) 0.1236(2) 0.0629(9) Uani C 1.0 C7 0.7523(5) 0.0056(3) 0.0877(2) 0.058(4) Uani C 1.0 C8 0.7358(7) 0.0419(4) 0.0421(2) 0.078(5) Uani C 1.0 C9 0.7875(8) 0.0006(4) 0.0078(2) 0.105(8) Uani C 1.0 C10 0.8543(8) -0.0757(4) 0.0182(2) 0.107(8) Uani C 1.0 C11 0.8706(8) -0.1108(4) 0.0625(2) 0.096(5) Uani C 1.0 C12 0.8193(6) -0.0717(3) 0.0982(2) 0.075(4) Uani C 1.0 C13 0.6337(10) 0.1523(5) -0.0106(3) 0.151(4) Uani C 1.0 C14 1.0014(8) -0.2147(5) 0.1147(3) 0.137(3) Uani C 1.0 C15 0.7170(5) 0.3223(3) 0.1086(2) 0.0544(7) Uani C 1.0 C16 0.7974(5) 0.3267(3) 0.0703(2) 0.0580(7) Uani C 1.0 C17 0.7689(6) 0.3838(4) 0.0333(2) 0.073(1) Uani C 1.0 C18 0.8463(6) 0.3828(4) -0.0011(2) 0.084(1) Uani C 1.0 C19 0.9531(6) 0.3241(4) 0.0032(2) 0.079(1) Uani C 1.0 C20 0.9768(6) 0.2681(4) 0.0408(2) 0.0641(8) Uani C 1.0 C21 0.9121(5) 0.3499(3) 0.1779(2) 0.0510(6) Uani C 1.0 C22 1.0307(5) 0.3049(3) 0.2115(2) 0.0501(5) Uani C 1.0 C23 1.1064(5) 0.3390(3) 0.2538(2) 0.0628(6) Uani C 1.0 C24 1.2161(6) 0.2938(4) 0.2815(2) 0.0698(7) Uani C 1.0 C25 1.2500(5) 0.2162(4) 0.2663(2) 0.0643(6) Uani C 1.0 C26 1.1702(5) 0.1851(3) 0.2230(2) 0.0526(5) Uani C 1.0 B1T 0.4000(5) 0.4937(4) 0.1515(2) 0.043(1) Uani B 1.0 C1T 0.3829(3) 0.4217(2) 0.1085(1) 0.045(1) Uani C 1.0 C2T 0.3559(3) 0.3365(2) 0.1161(1) 0.056(1) Uani C 1.0 C3T 0.3384(4) 0.2758(2) 0.0801(1) 0.072(2) Uani C 1.0 C4T 0.3470(4) 0.2978(2) 0.0343(1) 0.078(2) Uani C 1.0 C5T 0.3734(4) 0.3810(3) 0.0252(1) 0.072(1) Uani C 1.0 C6T 0.3907(3) 0.4411(2) 0.0614(1) 0.056(1) Uani C 1.0 C7T 0.2440(3) 0.5126(2) 0.1609(1) 0.045(1) Uani C 1.0 C8T 0.1211(3) 0.5120(2) 0.1236(1) 0.049(1) Uani C 1.0 C9T -0.0081(3) 0.5410(2) 0.1292(1) 0.056(1) Uani C 1.0 C10T -0.0206(3) 0.5723(2) 0.1729(1) 0.062(2) Uani C 1.0 C11T 0.0976(4) 0.5740(2) 0.2107(1) 0.067(2) Uani C 1.0 C12T 0.2262(3) 0.5449(2) 0.2046(1) 0.056(1) Uani C 1.0 C13T 0.4611(3) 0.5827(2) 0.1346(1) 0.042(1) Uani C 1.0 C14T 0.3942(3) 0.6611(2) 0.1343(1) 0.049(1) Uani C 1.0 C15T 0.4454(4) 0.7350(2) 0.1189(1) 0.057(1) Uani C 1.0 C16T 0.5675(4) 0.7341(2) 0.1027(1) 0.056(1) Uani C 1.0 C17T 0.6371(3) 0.6584(2) 0.1023(1) 0.054(1) Uani C 1.0 C18T 0.5847(3) 0.5849(2) 0.1178(1) 0.048(1) Uani C 1.0 C19T 0.5060(3) 0.4583(2) 0.2016(1) 0.043(1) Uani C 1.0 C20T 0.6453(3) 0.4856(2) 0.2197(1) 0.049(1) Uani C 1.0 C21T 0.7331(3) 0.4526(2) 0.2612(1) 0.058(1) Uani C 1.0 C22T 0.6853(4) 0.3900(2) 0.2867(1) 0.065(2) Uani C 1.0 C23T 0.5489(4) 0.3612(2) 0.2703(1) 0.067(2) Uani C 1.0 C24T 0.4621(3) 0.3946(2) 0.2288(1) 0.054(1) Uani C 1.0 H1C1 0.6450 0.2925 0.1860 0.056 Uani H 1.0 H2C1 0.7874 0.2486 0.2189 0.049 Uani H 1.0 HC3 0.5024 0.1707 0.2015 0.069 Uani H 1.0 HC4 0.4225 0.0314 0.1755 0.090 Uani H 1.0 HC5 0.5431 -0.0461 0.1256 0.092 Uani H 1.0 HC9 0.7763 0.0262 -0.0248 0.151 Uani H 1.0 HC10 0.8912 -0.1058 -0.0070 0.145 Uani H 1.0 HC12 0.8303 -0.0985 0.1305 0.098 Uani H 1.0 H1C13 0.5873 0.2084 -0.0096 0.151 Uani H 1.0 H2C13 0.7203 0.1597 -0.0230 0.151 Uani H 1.0 H3C13 0.5667 0.1132 -0.0323 0.151 Uani H 1.0 H1C14 1.0445 -0.2715 0.1130 0.137 Uani H 1.0 H2C14 1.0767 -0.1735 0.1300 0.137 Uani H 1.0 H3C14 0.9296 -0.2185 0.1343 0.137 Uani H 1.0 H1C15 0.6851 0.3803 0.1149 0.062 Uani H 1.0 H2C15 0.6328 0.2849 0.0975 0.058 Uani H 1.0 HC17 0.6917 0.4262 0.0312 0.082 Uani H 1.0 HC18 0.8255 0.4238 -0.0285 0.100 Uani H 1.0 HC19 1.0124 0.3224 -0.0208 0.091 Uani H 1.0 HC20 1.0539 0.2255 0.0436 0.066 Uani H 1.0 H1C21 0.8658 0.3896 0.1966 0.058 Uani H 1.0 H2C21 0.9496 0.3824 0.1538 0.056 Uani H 1.0 HC23 1.0819 0.3961 0.2645 0.073 Uani H 1.0 HC24 1.2714 0.3175 0.3128 0.085 Uani H 1.0 HC25 1.3304 0.1828 0.2860 0.075 Uani H 1.0 HC26 1.1952 0.1289 0.2115 0.056 Uani H 1.0 HC2T 0.3491 0.3185 0.1489 0.062 Uani H 1.0 HC3T 0.3193 0.2158 0.0875 0.090 Uani H 1.0 HC4T 0.3344 0.2543 0.0083 0.097 Uani H 1.0 HC5T 0.3800 0.3982 -0.0078 0.091 Uani H 1.0 HC6T 0.4098 0.5009 0.0536 0.063 Uani H 1.0 HC8T 0.1268 0.4897 0.0914 0.057 Uani H 1.0 HC9T -0.0926 0.5392 0.1013 0.066 Uani H 1.0 HC10T -0.1135 0.5932 0.1771 0.072 Uani H 1.0 HC11T 0.0906 0.5965 0.2427 0.087 Uani H 1.0 HC12T 0.3100 0.5470 0.2327 0.067 Uani H 1.0 HC14T 0.3053 0.6638 0.1459 0.056 Uani H 1.0 HC15T 0.3935 0.7894 0.1195 0.069 Uani H 1.0 HC16T 0.6049 0.7873 0.0915 0.064 Uani H 1.0 HC17T 0.7258 0.6565 0.0907 0.065 Uani H 1.0 HC18T 0.6376 0.5309 0.1171 0.054 Uani H 1.0 HC20T 0.6831 0.5310 0.2020 0.054 Uani H 1.0 HC21T 0.8317 0.4744 0.2725 0.068 Uani H 1.0 HC22T 0.7482 0.3661 0.3166 0.078 Uani H 1.0 HC23T 0.5123 0.3158 0.2884 0.085 Uani H 1.0 HC24T 0.3637 0.3724 0.2178 0.062 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Co 0.0443(4) 0.0439(4) 0.0500(4) 0.0088(3) 0.0136(3) -0.0012(4) Co Cl 0.0676(9) 0.069(1) 0.087(1) 0.0224(8) 0.0226(8) -0.0135(8) Cl O1 0.176(9) 0.075(3) 0.062(5) 0.024(3) 0.011(4) 0.008(2) O O2 0.223(9) 0.088(5) 0.136(7) 0.056(4) 0.046(5) -0.018(3) O N1 0.0493(9) 0.0501(9) 0.0520(9) 0.0007(8) 0.0143(6) -0.0001(7) N N2 0.0566(9) 0.061(1) 0.0464(9) 0.0100(7) 0.0189(6) 0.0093(7) N N3 0.0440(8) 0.048(1) 0.0466(9) 0.0057(7) 0.0143(6) 0.0025(6) N N4 0.0475(8) 0.045(1) 0.0487(8) 0.0106(7) 0.0170(6) 0.0048(7) N C1 0.0468(8) 0.051(1) 0.0510(9) 0.0116(8) 0.0195(7) 0.0044(7) C C2 0.0445(9) 0.056(1) 0.0545(8) 0.0041(7) 0.0168(6) 0.0052(7) C C3 0.0476(9) 0.074(2) 0.071(1) -0.0003(9) 0.0214(7) 0.010(1) C C4 0.058(1) 0.082(2) 0.088(2) -0.015(1) 0.021(1) 0.008(1) C C5 0.071(2) 0.070(2) 0.087(2) -0.020(1) 0.017(1) -0.003(1) C C6 0.065(1) 0.057(1) 0.067(1) -0.009(1) 0.0153(8) -0.0061(8) C C7 0.072(8) 0.045(3) 0.054(3) -0.016(2) 0.011(3) -0.006(2) C C8 0.118(9) 0.060(3) 0.053(4) -0.004(3) 0.015(3) -0.002(2) C C9 0.178(9) 0.082(5) 0.062(4) -0.001(5) 0.042(4) -0.007(2) C C10 0.163(9) 0.084(5) 0.085(5) 0.002(4) 0.051(5) -0.021(3) C C11 0.137(9) 0.065(4) 0.089(4) 0.010(2) 0.032(3) -0.015(3) C C12 0.108(8) 0.047(4) 0.068(3) -0.004(2) 0.019(2) -0.004(2) C C13 0.226(9) 0.128(7) 0.068(5) 0.039(7) -0.022(5) 0.024(5) C C14 0.113(6) 0.112(6) 0.153(7) 0.044(5) -0.033(5) -0.027(6) C C15 0.0527(9) 0.057(1) 0.055(1) 0.0160(9) 0.0166(6) 0.0126(8) C C16 0.060(1) 0.064(1) 0.0528(9) 0.0142(8) 0.0176(6) 0.0164(8) C C17 0.076(2) 0.082(2) 0.064(1) 0.021(1) 0.0214(9) 0.031(1) C C18 0.090(2) 0.101(3) 0.064(1) 0.020(2) 0.028(1) 0.037(2) C C19 0.086(2) 0.101(3) 0.057(1) 0.015(2) 0.032(1) 0.026(1) C C20 0.069(1) 0.079(2) 0.0503(9) 0.012(1) 0.0266(9) 0.0130(8) C C21 0.058(1) 0.042(1) 0.0566(9) 0.0071(6) 0.0201(7) 0.0012(7) C C22 0.0528(8) 0.048(1) 0.0512(9) 0.0016(7) 0.0151(6) -0.0023(7) C C23 0.067(1) 0.062(1) 0.0584(9) -0.006(1) 0.0126(8) -0.010(1) C C24 0.063(1) 0.083(2) 0.058(1) -0.007(1) 0.0050(9) -0.007(1) C C25 0.0504(8) 0.083(2) 0.056(1) 0.0031(9) 0.0058(9) 0.005(1) C C26 0.0447(8) 0.061(1) 0.052(1) 0.0086(8) 0.0125(7) 0.0066(8) C B1T 0.039(3) 0.052(4) 0.038(3) 0.007(3) 0.012(3) 0.002(3) B C1T 0.029(2) 0.055(2) 0.047(2) 0.002(2) 0.004(2) -0.002(1) C C2T 0.047(2) 0.054(2) 0.063(2) -0.002(2) 0.008(2) -0.005(1) C C3T 0.067(3) 0.062(2) 0.081(2) -0.002(2) 0.009(2) -0.019(2) C C4T 0.073(3) 0.083(2) 0.072(2) 0.004(2) 0.007(2) -0.028(2) C C5T 0.072(3) 0.090(2) 0.053(2) 0.006(2) 0.010(2) -0.016(2) C C6T 0.049(2) 0.071(2) 0.046(2) 0.003(2) 0.009(2) -0.004(1) C C7T 0.041(1) 0.045(2) 0.049(2) 0.003(1) 0.013(1) 0.001(2) C C8T 0.040(1) 0.051(2) 0.057(2) 0.003(1) 0.011(1) 0.003(2) C C9T 0.041(1) 0.053(3) 0.076(2) 0.005(1) 0.015(1) 0.008(2) C C10T 0.048(1) 0.057(3) 0.087(3) 0.007(2) 0.029(1) 0.002(2) C C11T 0.056(2) 0.078(3) 0.075(2) 0.008(2) 0.030(2) -0.010(2) C C12T 0.050(1) 0.068(2) 0.056(2) 0.005(1) 0.020(1) -0.007(2) C C13T 0.040(2) 0.050(1) 0.034(2) 0.007(1) 0.005(2) 0.001(1) C C14T 0.052(2) 0.049(1) 0.045(2) 0.009(1) 0.009(1) 0.003(1) C C15T 0.067(2) 0.051(1) 0.050(2) 0.004(1) 0.009(2) 0.004(1) C C16T 0.066(2) 0.059(1) 0.041(2) -0.007(1) 0.006(2) 0.004(2) C C17T 0.054(2) 0.065(2) 0.044(2) -0.006(1) 0.010(2) 0.002(2) C C18T 0.043(2) 0.058(1) 0.041(2) 0.003(1) 0.009(1) 0.002(1) C C19T 0.040(2) 0.052(2) 0.039(1) 0.007(1) 0.012(1) -0.003(1) C C20T 0.041(2) 0.058(2) 0.046(2) 0.007(1) 0.006(1) -0.006(1) C C21T 0.048(1) 0.073(3) 0.047(2) 0.014(1) 0.002(1) -0.007(2) C C22T 0.059(2) 0.089(3) 0.045(2) 0.023(2) 0.009(1) 0.007(2) C C23T 0.059(2) 0.089(3) 0.054(2) 0.018(2) 0.017(1) 0.022(2) C C24T 0.047(1) 0.068(2) 0.049(2) 0.010(1) 0.016(1) 0.012(1) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co Cl 2.262(1) 1_555 1_555 no Co N1 2.131(4) 1_555 1_555 no Co N2 2.077(4) 1_555 1_555 no Co N3 2.108(4) 1_555 1_555 no Co N4 2.187(3) 1_555 1_555 no O1 C8 1.354(6) 1_555 1_555 no O1 C13 1.400(7) 1_555 1_555 no O2 C11 1.381(7) 1_555 1_555 no O2 C14 1.354(8) 1_555 1_555 no N1 C2 1.347(5) 1_555 1_555 no N1 C6 1.345(6) 1_555 1_555 no N2 C16 1.349(5) 1_555 1_555 no N2 C20 1.347(5) 1_555 1_555 no N3 C22 1.350(5) 1_555 1_555 no N3 C26 1.347(5) 1_555 1_555 no N4 C1 1.478(5) 1_555 1_555 no N4 C15 1.471(5) 1_555 1_555 no N4 C21 1.466(6) 1_555 1_555 no C1 C2 1.503(6) 1_555 1_555 no C2 C3 1.381(6) 1_555 1_555 no C3 C4 1.376(7) 1_555 1_555 no C4 C5 1.388(7) 1_555 1_555 no C5 C6 1.388(7) 1_555 1_555 no C6 C7 1.483(7) 1_555 1_555 no C7 C8 1.401(7) 1_555 1_555 no C7 C12 1.385(7) 1_555 1_555 no C8 C9 1.371(8) 1_555 1_555 no C9 C10 1.370(8) 1_555 1_555 no C10 C11 1.359(8) 1_555 1_555 no C11 C12 1.386(8) 1_555 1_555 no C15 C16 1.494(6) 1_555 1_555 no C16 C17 1.370(6) 1_555 1_555 no C17 C18 1.377(7) 1_555 1_555 no C18 C19 1.380(7) 1_555 1_555 no C19 C20 1.370(7) 1_555 1_555 no C21 C22 1.494(6) 1_555 1_555 no C22 C23 1.369(6) 1_555 1_555 no C23 C24 1.369(7) 1_555 1_555 no C24 C25 1.368(7) 1_555 1_555 no C25 C26 1.386(6) 1_555 1_555 no B1T C1T 1.655(6) 1_555 1_555 no B1T C7T 1.636(6) 1_555 1_555 no B1T C13T 1.646(6) 1_555 1_555 no B1T C19T 1.653(6) 1_555 1_555 no C1T C2T 1.401(2) 1_555 1_555 no C1T C6T 1.401(2) 1_555 1_555 no C2T C3T 1.387(2) 1_555 1_555 no C3T C4T 1.378(2) 1_555 1_555 no C4T C5T 1.378(2) 1_555 1_555 no C5T C6T 1.387(2) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Co N1 112.1(1) 1_555 1_555 1_555 no Cl Co N2 103.1(1) 1_555 1_555 1_555 no Cl Co N3 95.8(1) 1_555 1_555 1_555 no Cl Co N4 170.3(1) 1_555 1_555 1_555 no N1 Co N2 115.4(2) 1_555 1_555 1_555 no N1 Co N3 113.8(1) 1_555 1_555 1_555 no N1 Co N4 76.3(1) 1_555 1_555 1_555 no N2 Co N3 114.2(2) 1_555 1_555 1_555 no N2 Co N4 76.4(1) 1_555 1_555 1_555 no N3 Co N4 75.9(1) 1_555 1_555 1_555 no C8 O1 C13 118.4(5) 1_555 1_555 1_555 no C11 O2 C14 120.5(6) 1_555 1_555 1_555 no Co N1 C2 115.1(3) 1_555 1_555 1_555 no Co N1 C6 126.5(3) 1_555 1_555 1_555 no C2 N1 C6 118.3(4) 1_555 1_555 1_555 no Co N2 C16 117.1(3) 1_555 1_555 1_555 no Co N2 C20 124.8(3) 1_555 1_555 1_555 no C16 N2 C20 118.2(4) 1_555 1_555 1_555 no Co N3 C22 117.1(3) 1_555 1_555 1_555 no Co N3 C26 125.1(3) 1_555 1_555 1_555 no C22 N3 C26 117.8(4) 1_555 1_555 1_555 no Co N4 C1 108.2(3) 1_555 1_555 1_555 no Co N4 C15 106.6(3) 1_555 1_555 1_555 no Co N4 C21 107.0(3) 1_555 1_555 1_555 no C1 N4 C15 111.8(3) 1_555 1_555 1_555 no C1 N4 C21 110.8(3) 1_555 1_555 1_555 no C15 N4 C21 112.1(4) 1_555 1_555 1_555 no N4 C1 C2 109.3(4) 1_555 1_555 1_555 no N1 C2 C1 117.2(4) 1_555 1_555 1_555 no N1 C2 C3 123.3(5) 1_555 1_555 1_555 no C1 C2 C3 119.6(4) 1_555 1_555 1_555 no C2 C3 C4 118.3(5) 1_555 1_555 1_555 no C3 C4 C5 119.2(5) 1_555 1_555 1_555 no C4 C5 C6 119.6(5) 1_555 1_555 1_555 no N1 C6 C5 121.3(5) 1_555 1_555 1_555 no N1 C6 C7 119.1(5) 1_555 1_555 1_555 no C5 C6 C7 119.5(5) 1_555 1_555 1_555 no C6 C7 C8 119.0(5) 1_555 1_555 1_555 no C6 C7 C12 120.5(5) 1_555 1_555 1_555 no C8 C7 C12 120.4(5) 1_555 1_555 1_555 no O1 C8 C7 115.6(5) 1_555 1_555 1_555 no O1 C8 C9 124.9(6) 1_555 1_555 1_555 no C7 C8 C9 119.5(6) 1_555 1_555 1_555 no C8 C9 C10 120.2(6) 1_555 1_555 1_555 no C9 C10 C11 120.3(6) 1_555 1_555 1_555 no O2 C11 C10 116.3(6) 1_555 1_555 1_555 no O2 C11 C12 122.0(6) 1_555 1_555 1_555 no C10 C11 C12 121.6(6) 1_555 1_555 1_555 no C7 C12 C11 118.0(6) 1_555 1_555 1_555 no N4 C15 C16 109.5(4) 1_555 1_555 1_555 no N2 C16 C15 114.9(4) 1_555 1_555 1_555 no N2 C16 C17 121.6(5) 1_555 1_555 1_555 no C15 C16 C17 123.5(5) 1_555 1_555 1_555 no C16 C17 C18 120.1(5) 1_555 1_555 1_555 no C17 C18 C19 118.5(5) 1_555 1_555 1_555 no C18 C19 C20 119.1(5) 1_555 1_555 1_555 no N2 C20 C19 122.6(5) 1_555 1_555 1_555 no N4 C21 C22 109.4(4) 1_555 1_555 1_555 no N3 C22 C21 114.1(4) 1_555 1_555 1_555 no N3 C22 C23 122.3(5) 1_555 1_555 1_555 no C21 C22 C23 123.5(5) 1_555 1_555 1_555 no C22 C23 C24 119.1(5) 1_555 1_555 1_555 no C23 C24 C25 120.0(5) 1_555 1_555 1_555 no C24 C25 C26 118.4(5) 1_555 1_555 1_555 no N3 C26 C25 122.3(5) 1_555 1_555 1_555 no C1T B1T C7T 108.5(3) 1_555 1_555 1_555 no C1T B1T C13T 110.4(3) 1_555 1_555 1_555 no C1T B1T C19T 110.0(3) 1_555 1_555 1_555 no C7T B1T C13T 108.1(3) 1_555 1_555 1_555 no C7T B1T C19T 109.3(3) 1_555 1_555 1_555 no C13T B1T C19T 110.5(3) 1_555 1_555 1_555 no B1T C1T C2T 122.4(3) 1_555 1_555 1_555 no B1T C1T C6T 123.0(3) 1_555 1_555 1_555 no C2T C1T C6T 114.6(2) 1_555 1_555 1_555 no C1T C2T C3T 123.0(2) 1_555 1_555 1_555 no C2T C3T C4T 120.4(2) 1_555 1_555 1_555 no C3T C4T C5T 118.6(2) 1_555 1_555 1_555 no C4T C5T C6T 120.4(2) 1_555 1_555 1_555 no C1T C6T C5T 123.0(2) 1_555 1_555 1_555 no B1T C7T C8T 122.2(3) 1_555 1_555 1_555 no B1T C7T C12T 122.4(3) 1_555 1_555 1_555 no B1T C13T C14T 123.8(3) 1_555 1_555 1_555 no B1T C13T C18T 121.6(3) 1_555 1_555 1_555 no B1T C19T C20T 124.4(3) 1_555 1_555 1_555 no B1T C19T C24T 121.0(3) 1_555 1_555 1_555 no #===END data_[Ni2Cl2(L)2]Cl2.MeOH _database_code_CSD 190793 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 Cl N4 Ni O2 1+,Cl 1-,2.5(H2 O),0.5(C H4 O)' _chemical_formula_sum 'C26.5 H33 Cl2 N4 Ni O5' _chemical_formula_iupac ? _chemical_formula_weight 617.2 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.830(6) _cell_length_b 12.202(7) _cell_length_c 12.865(8) _cell_angle_alpha 107.78(3) _cell_angle_beta 92.45(4) _cell_angle_gamma 95.74(3) _cell_volume 1458(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 12 _cell_measurement_theta_max 14 _cell_measurement_temperature 294 _exptl_crystal_description parallelipiped _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644.0 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.91 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4527 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 15 # REFINEMENT DATA _refine_special_details ; Thermal motion was refined using two 15-parameter TLX rigid body thermal parameters, one for the hydroquinone, and the other with all remaining ligand atoms except the methyls. Individual anisotropic parameters were used for the metal,chlorines, methyl carbons, waters and solvent atoms. ; _reflns_number_total 4293 _reflns_number_gt 2945 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.063 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2945 _refine_ls_number_parameters 213 _refine_ls_goodness_of_fit_ref 1.90 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.007 _refine_diff_density_max 0.74 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description OW/Cl1 '0.90O+0.10Cl' OW/Cl2 '0.75O+0.25Cl' OW/Cl3 '0.85O+0.15Cl' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Ni 0.42797(6) 0.62218(6) 0.58659(5) 0.0421(2) Uani Ni 1.0 Cl1 0.3442(1) 0.4499(1) 0.4468(1) 0.0466(4) Uani Cl 1.0 O1 0.1858(4) 0.8173(3) 0.4713(3) 0.068(1) Uani O 1.0 O2 0.2025(4) 0.4312(4) 0.1123(3) 0.080(3) Uani O 1.0 N1 0.4782(4) 0.7496(4) 0.5038(3) 0.0480(6) Uani N 1.0 N2 0.2447(4) 0.6814(4) 0.6340(3) 0.0465(7) Uani N 1.0 N3 0.4083(4) 0.5491(4) 0.7136(3) 0.0469(6) Uani N 1.0 N4 0.5102(4) 0.7660(4) 0.7146(3) 0.0487(6) Uani N 1.0 C1 0.6270(5) 0.8228(5) 0.6730(5) 0.0541(6) Uani C 1.0 C2 0.5875(5) 0.8262(5) 0.5596(5) 0.0542(6) Uani C 1.0 C3 0.6594(6) 0.9015(5) 0.5176(6) 0.068(1) Uani C 1.0 C4 0.6226(6) 0.8999(6) 0.4124(6) 0.075(1) Uani C 1.0 C5 0.5093(6) 0.8268(6) 0.3555(5) 0.068(1) Uani C 1.0 C6 0.4362(5) 0.7539(5) 0.4036(5) 0.0550(7) Uani C 1.0 C7 0.3068(5) 0.6843(5) 0.3476(4) 0.049(1) Uani C 1.0 C8 0.1792(5) 0.7189(5) 0.3816(4) 0.054(1) Uani C 1.0 C9 0.0603(6) 0.6575(5) 0.3256(5) 0.064(2) Uani C 1.0 C10 0.0630(6) 0.5612(5) 0.2344(5) 0.063(2) Uani C 1.0 C11 0.1868(6) 0.5271(5) 0.2000(5) 0.059(2) Uani C 1.0 C12 0.3070(6) 0.5898(5) 0.2554(4) 0.055(1) Uani C 1.0 C13 0.0605(7) 0.8636(6) 0.4989(6) 0.083(2) Uani C 1.0 C14 0.0858(8) 0.3686(6) 0.0467(5) 0.090(2) Uani C 1.0 C15 0.4026(5) 0.8438(5) 0.7442(4) 0.0550(9) Uani C 1.0 C16 0.2604(5) 0.7806(5) 0.7179(4) 0.0530(9) Uani C 1.0 C17 0.1505(6) 0.8237(5) 0.7737(5) 0.065(2) Uani C 1.0 C18 0.0216(6) 0.7641(6) 0.7429(5) 0.069(2) Uani C 1.0 C19 0.0057(5) 0.6618(5) 0.6567(5) 0.062(1) Uani C 1.0 C20 0.1202(5) 0.6228(5) 0.6044(4) 0.0515(9) Uani C 1.0 C21 0.5550(5) 0.7250(5) 0.8066(4) 0.0537(6) Uani C 1.0 C22 0.4601(5) 0.6231(5) 0.8118(4) 0.0530(6) Uani C 1.0 C23 0.4354(6) 0.6012(6) 0.9082(5) 0.0657(8) Uani C 1.0 C24 0.3569(6) 0.4998(6) 0.9048(5) 0.072(1) Uani C 1.0 C25 0.3068(6) 0.4227(6) 0.8051(5) 0.0664(9) Uani C 1.0 C26 0.3330(5) 0.4503(5) 0.7109(5) 0.0535(6) Uani C 1.0 Cl2 0.0967(16) 0.1159(9) -0.2398(8) 0.341(7) Uani Cl 0.5 OW/Cl1 0.1492(6) 0.0473(5) 0.0530(4) 0.160(4) Uani OW/Cl1 1.0 OW/Cl2 0.3250(7) 0.1368(4) -0.1079(4) 0.188(4) Uani OW/Cl2 1.0 OW/Cl3 0.3936(6) -0.0832(5) 0.0623(5) 0.182(4) Uani OW/Cl3 1.0 O1Me 0.1763(21) -0.1940(21) 0.1456(20) 0.285(9) Uani O 0.5 C1Me 0.1337(36) -0.0846(23) 0.2114(26) 0.255(9) Uani C 0.5 H1C1 0.7074 0.7781 0.6705 0.055 Uani H 1.0 H2C1 0.6521 0.9038 0.7231 0.064 Uani H 1.0 HC3 0.7376 0.9571 0.5621 0.077 Uani H 1.0 HC4 0.6773 0.9511 0.3778 0.089 Uani H 1.0 HC5 0.4798 0.8263 0.2800 0.078 Uani H 1.0 HC9 -0.0298 0.6823 0.3508 0.085 Uani H 1.0 HC10 -0.0245 0.5170 0.1940 0.079 Uani H 1.0 HC12 0.3966 0.5661 0.2279 0.070 Uani H 1.0 H1C13 0.0780 0.9342 0.5646 0.083 Uani H 1.0 H2C13 0.0205 0.8850 0.4359 0.083 Uani H 1.0 H3C13 -0.0053 0.8043 0.5154 0.083 Uani H 1.0 H1C14 0.1134 0.3022 -0.0129 0.090 Uani H 1.0 H2C14 0.0216 0.3384 0.0926 0.090 Uani H 1.0 H3C14 0.0391 0.4206 0.0137 0.090 Uani H 1.0 H1C15 0.4127 0.9014 0.7031 0.059 Uani H 1.0 H2C15 0.4154 0.8854 0.8247 0.063 Uani H 1.0 HC17 0.1647 0.8976 0.8361 0.075 Uani H 1.0 HC18 -0.0593 0.7942 0.7820 0.081 Uani H 1.0 HC19 -0.0869 0.6167 0.6326 0.070 Uani H 1.0 HC20 0.1089 0.5485 0.5425 0.052 Uani H 1.0 H1C21 0.5560 0.7895 0.8770 0.063 Uani H 1.0 H2C21 0.6494 0.7019 0.7961 0.055 Uani H 1.0 HC23 0.4737 0.6579 0.9799 0.075 Uani H 1.0 HC24 0.3367 0.4825 0.9741 0.087 Uani H 1.0 HC25 0.2521 0.3477 0.8009 0.076 Uani H 1.0 HC26 0.2947 0.3950 0.6386 0.054 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Ni 0.0359(4) 0.0397(4) 0.0440(4) 0.0046(3) -0.0006(3) 0.0039(3) Ni Cl1 0.0357(7) 0.0472(8) 0.0482(8) 0.0050(6) -0.0020(6) 0.0026(6) Cl O1 0.060(2) 0.064(2) 0.072(2) 0.024(1) 0.000(1) 0.005(1) O O2 0.075(3) 0.079(3) 0.068(2) 0.016(2) -0.001(2) -0.004(2) O N1 0.0416(9) 0.043(1) 0.0568(9) 0.0049(7) 0.0003(6) 0.0124(8) N N2 0.0368(9) 0.046(1) 0.052(1) 0.0091(8) 0.0013(7) 0.0063(7) N N3 0.0404(8) 0.0484(9) 0.049(1) 0.0068(7) 0.0003(7) 0.0109(7) N N4 0.0423(9) 0.042(1) 0.0513(9) 0.0039(7) -0.0039(7) 0.0004(8) N C1 0.044(1) 0.043(1) 0.064(1) -0.0019(9) -0.0053(8) 0.0038(9) C C2 0.046(1) 0.043(1) 0.069(1) -0.0002(7) -0.0001(7) 0.0134(8) C C3 0.057(2) 0.053(1) 0.092(2) -0.004(1) 0.004(1) 0.026(1) C C4 0.067(2) 0.068(1) 0.098(2) 0.001(1) 0.010(1) 0.042(2) C C5 0.064(2) 0.072(1) 0.080(1) 0.009(1) 0.007(1) 0.038(1) C C6 0.050(1) 0.056(1) 0.062(1) 0.0087(7) 0.0019(7) 0.022(1) C C7 0.047(2) 0.052(2) 0.051(2) 0.014(2) 0.002(1) 0.020(1) C C8 0.049(2) 0.055(1) 0.058(2) 0.019(1) 0.000(1) 0.016(1) C C9 0.047(2) 0.071(3) 0.069(2) 0.019(1) -0.003(1) 0.013(2) C C10 0.052(2) 0.069(3) 0.064(2) 0.013(1) -0.006(2) 0.014(2) C C11 0.057(2) 0.062(2) 0.055(2) 0.014(1) -0.001(1) 0.012(1) C C12 0.051(1) 0.060(2) 0.053(1) 0.015(1) 0.004(1) 0.015(1) C C13 0.078(5) 0.074(5) 0.095(5) 0.039(4) 0.019(4) 0.014(4) C C14 0.097(5) 0.083(5) 0.066(5) -0.002(4) -0.015(4) -0.002(4) C C15 0.052(1) 0.043(1) 0.058(1) 0.0092(7) -0.0008(9) -0.0024(9) C C16 0.046(1) 0.049(1) 0.056(1) 0.0139(9) 0.0037(8) 0.0025(8) C C17 0.055(1) 0.064(2) 0.066(2) 0.023(1) 0.011(1) 0.003(1) C C18 0.049(1) 0.079(3) 0.075(2) 0.025(2) 0.014(1) 0.012(2) C C19 0.0382(9) 0.073(2) 0.073(2) 0.015(1) 0.0079(9) 0.016(2) C C20 0.0348(9) 0.056(1) 0.060(1) 0.0085(9) 0.0018(7) 0.0107(9) C C21 0.047(1) 0.055(1) 0.048(1) 0.0058(8) -0.0064(8) 0.0010(8) C C22 0.048(1) 0.060(1) 0.046(1) 0.0094(7) -0.0010(7) 0.0097(8) C C23 0.062(2) 0.085(2) 0.050(1) 0.015(1) 0.0024(9) 0.019(1) C C24 0.069(2) 0.094(2) 0.063(1) 0.015(1) 0.009(1) 0.036(2) C C25 0.060(2) 0.075(1) 0.072(1) 0.009(1) 0.009(1) 0.035(1) C C26 0.0466(9) 0.0537(9) 0.061(1) 0.0055(8) 0.0035(7) 0.0199(8) C Cl2 0.592(9) 0.228(9) 0.219(9) 0.206(9) 0.060(9) 0.041(8) Cl OW/Cl1 0.154(6) 0.163(6) 0.112(5) 0.033(4) 0.021(4) -0.036(4) OW/Cl1 OW/Cl2 0.280(8) 0.108(4) 0.147(5) -0.006(4) 0.073(5) -0.004(3) OW/Cl2 OW/Cl3 0.165(6) 0.160(6) 0.147(5) -0.009(4) 0.011(4) -0.054(4) OW/Cl3 O1Me 0.228(9) 0.357(9) 0.372(9) -0.012(9) -0.072(9) 0.290(9) O C1Me 0.306(9) 0.177(9) 0.214(9) -0.147(9) 0.010(9) 0.015(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni Cl1 2.356(1) 1_555 1_555 no Ni Cl1 2.494(1) 1_555 2_666 no Ni N1 2.167(4) 1_555 1_555 no Ni N2 2.056(4) 1_555 1_555 no Ni N3 2.094(4) 1_555 1_555 no Ni N4 2.070(4) 1_555 1_555 no O1 C8 1.382(6) 1_555 1_555 no O1 C13 1.420(7) 1_555 1_555 no O2 C11 1.383(7) 1_555 1_555 no O2 C14 1.400(7) 1_555 1_555 no N1 C2 1.366(6) 1_555 1_555 no N1 C6 1.355(6) 1_555 1_555 no N2 C16 1.343(6) 1_555 1_555 no N2 C20 1.331(6) 1_555 1_555 no N3 C22 1.351(6) 1_555 1_555 no N3 C26 1.341(6) 1_555 1_555 no N4 C1 1.484(6) 1_555 1_555 no N4 C15 1.476(6) 1_555 1_555 no N4 C21 1.486(7) 1_555 1_555 no C1 C2 1.508(7) 1_555 1_555 no C2 C3 1.357(7) 1_555 1_555 no C3 C4 1.380(8) 1_555 1_555 no C4 C5 1.380(8) 1_555 1_555 no C5 C6 1.392(7) 1_555 1_555 no C6 C7 1.480(7) 1_555 1_555 no C7 C8 1.408(7) 1_555 1_555 no C7 C12 1.379(7) 1_555 1_555 no C8 C9 1.367(7) 1_555 1_555 no C9 C10 1.388(8) 1_555 1_555 no C10 C11 1.373(7) 1_555 1_555 no C11 C12 1.379(7) 1_555 1_555 no C15 C16 1.499(7) 1_555 1_555 no C16 C17 1.381(7) 1_555 1_555 no C17 C18 1.375(8) 1_555 1_555 no C18 C19 1.383(8) 1_555 1_555 no C19 C20 1.387(7) 1_555 1_555 no C21 C22 1.499(7) 1_555 1_555 no C22 C23 1.373(7) 1_555 1_555 no C23 C24 1.378(8) 1_555 1_555 no C24 C25 1.374(8) 1_555 1_555 no C25 C26 1.380(7) 1_555 1_555 no O1Me C1Me 1.459(18) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ni Cl1 84.41(4) 1_555 1_555 2_666 no Cl1 Ni N1 105.4(1) 1_555 1_555 1_555 no Cl1 Ni N2 99.3(1) 1_555 1_555 1_555 no Cl1 Ni N3 94.9(1) 1_555 1_555 1_555 no Cl1 Ni N4 175.6(1) 1_555 1_555 1_555 no Cl1 Ni N1 90.8(1) 2_666 1_555 1_555 no Cl1 Ni N2 172.8(1) 2_666 1_555 1_555 no Cl1 Ni N3 90.1(1) 2_666 1_555 1_555 no Cl1 Ni N4 92.6(1) 2_666 1_555 1_555 no N1 Ni N2 94.1(2) 1_555 1_555 1_555 no N1 Ni N3 159.7(2) 1_555 1_555 1_555 no N1 Ni N4 77.7(2) 1_555 1_555 1_555 no N2 Ni N3 83.4(2) 1_555 1_555 1_555 no N2 Ni N4 83.4(2) 1_555 1_555 1_555 no N3 Ni N4 82.0(2) 1_555 1_555 1_555 no Ni Cl1 Ni 95.59(4) 1_555 1_555 2_666 no C8 O1 C13 116.8(4) 1_555 1_555 1_555 no C11 O2 C14 118.8(5) 1_555 1_555 1_555 no Ni N1 C2 109.8(3) 1_555 1_555 1_555 no Ni N1 C6 131.6(4) 1_555 1_555 1_555 no C2 N1 C6 117.7(5) 1_555 1_555 1_555 no Ni N2 C16 113.0(3) 1_555 1_555 1_555 no Ni N2 C20 126.7(4) 1_555 1_555 1_555 no C16 N2 C20 119.2(4) 1_555 1_555 1_555 no Ni N3 C22 112.8(4) 1_555 1_555 1_555 no Ni N3 C26 127.7(4) 1_555 1_555 1_555 no C22 N3 C26 118.5(5) 1_555 1_555 1_555 no Ni N4 C1 106.7(3) 1_555 1_555 1_555 no Ni N4 C15 107.7(3) 1_555 1_555 1_555 no Ni N4 C21 107.7(3) 1_555 1_555 1_555 no C1 N4 C15 110.4(4) 1_555 1_555 1_555 no C1 N4 C21 112.0(4) 1_555 1_555 1_555 no C15 N4 C21 112.0(4) 1_555 1_555 1_555 no N4 C1 C2 109.9(4) 1_555 1_555 1_555 no N1 C2 C1 116.2(5) 1_555 1_555 1_555 no N1 C2 C3 123.4(5) 1_555 1_555 1_555 no C1 C2 C3 120.4(5) 1_555 1_555 1_555 no C2 C3 C4 118.8(6) 1_555 1_555 1_555 no C3 C4 C5 119.1(6) 1_555 1_555 1_555 no C4 C5 C6 119.8(6) 1_555 1_555 1_555 no N1 C6 C5 120.9(5) 1_555 1_555 1_555 no N1 C6 C7 119.1(5) 1_555 1_555 1_555 no C5 C6 C7 119.9(5) 1_555 1_555 1_555 no C6 C7 C8 120.6(5) 1_555 1_555 1_555 no C6 C7 C12 121.3(5) 1_555 1_555 1_555 no C8 C7 C12 117.9(5) 1_555 1_555 1_555 no O1 C8 C7 115.3(5) 1_555 1_555 1_555 no O1 C8 C9 124.6(5) 1_555 1_555 1_555 no C7 C8 C9 120.1(5) 1_555 1_555 1_555 no C8 C9 C10 120.9(5) 1_555 1_555 1_555 no C9 C10 C11 119.5(5) 1_555 1_555 1_555 no O2 C11 C10 124.8(5) 1_555 1_555 1_555 no O2 C11 C12 115.5(5) 1_555 1_555 1_555 no C10 C11 C12 119.8(5) 1_555 1_555 1_555 no C7 C12 C11 121.8(5) 1_555 1_555 1_555 no N4 C15 C16 113.0(4) 1_555 1_555 1_555 no N2 C16 C15 116.2(5) 1_555 1_555 1_555 no N2 C16 C17 121.7(5) 1_555 1_555 1_555 no C15 C16 C17 122.1(5) 1_555 1_555 1_555 no C16 C17 C18 119.4(5) 1_555 1_555 1_555 no C17 C18 C19 118.8(5) 1_555 1_555 1_555 no C18 C19 C20 119.0(5) 1_555 1_555 1_555 no N2 C20 C19 121.9(5) 1_555 1_555 1_555 no N4 C21 C22 111.2(4) 1_555 1_555 1_555 no N3 C22 C21 114.9(5) 1_555 1_555 1_555 no N3 C22 C23 122.1(5) 1_555 1_555 1_555 no C21 C22 C23 122.8(5) 1_555 1_555 1_555 no C22 C23 C24 119.0(6) 1_555 1_555 1_555 no C23 C24 C25 119.3(6) 1_555 1_555 1_555 no C24 C25 C26 119.1(6) 1_555 1_555 1_555 no N3 C26 C25 121.9(5) 1_555 1_555 1_555 no #===END data_[CuCl(L)][PF6] _database_code_CSD 190794 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 Cl Cu N4 O2 1+, F6 P 1-' _chemical_formula_sum 'C26 H26 Cl1 Cu1 F6 N4 O2 P1' _chemical_formula_iupac ? _chemical_formula_weight 670.5 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.032(6) _cell_length_b 11.704(4) _cell_length_c 13.306(6) _cell_angle_alpha 90.74(3) _cell_angle_beta 110.90(3) _cell_angle_gamma 117.83(2) _cell_volume 1385(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 19 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 682.0 _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.87 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5088 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 4858 _reflns_number_gt 3662 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_ref 0.072 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3662 _refine_ls_number_parameters 186 _refine_ls_goodness_of_fit_ref 1.75 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.008 _refine_diff_density_max 1.05 _refine_diff_density_min -0.62 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Cu 0.10381(6) 0.47003(5) 0.42291(4) 0.0379(2) Uani Cu 1.0 Cl 0.1135(1) 0.6616(1) 0.4572(1) 0.0483(3) Uani Cl 1.0 O1 0.2586(4) 0.8109(3) 0.1442(3) 0.068(2) Uani O 1.0 O2 0.6688(4) 0.8930(3) 0.5645(3) 0.0553(8) Uani O 1.0 N1 0.2389(4) 0.5001(3) 0.2998(3) 0.0362(4) Uani N 1.0 N2 -0.0839(4) 0.3901(4) 0.2860(3) 0.0415(5) Uani N 1.0 N3 0.2725(4) 0.5009(3) 0.5617(3) 0.0401(4) Uani N 1.0 N4 0.0806(4) 0.2861(3) 0.3994(3) 0.0390(5) Uani N 1.0 C1 0.1702(5) 0.2856(4) 0.3389(4) 0.0404(7) Uani C 1.0 C2 0.1720(5) 0.3715(4) 0.2553(3) 0.0382(5) Uani C 1.0 C3 0.1124(5) 0.3212(4) 0.1433(4) 0.0450(7) Uani C 1.0 C4 0.1236(5) 0.4117(5) 0.0755(4) 0.0490(8) Uani C 1.0 C5 0.1963(5) 0.5445(5) 0.1206(4) 0.0471(6) Uani C 1.0 C6 0.2583(5) 0.5879(4) 0.2349(4) 0.0410(4) Uani C 1.0 C7 0.3610(5) 0.7291(4) 0.2937(3) 0.037(1) Uani C 1.0 C8 0.3656(5) 0.8375(4) 0.2471(4) 0.047(2) Uani C 1.0 C9 0.4760(5) 0.9656(4) 0.3071(4) 0.049(2) Uani C 1.0 C10 0.5803(5) 0.9887(4) 0.4125(4) 0.044(1) Uani C 1.0 C11 0.5741(5) 0.8833(4) 0.4601(4) 0.0401(7) Uani C 1.0 C12 0.4653(4) 0.7550(4) 0.4000(3) 0.0354(9) Uani C 1.0 C13 0.2561(7) 0.9184(6) 0.0975(5) 0.081(2) Uani C 1.0 C14 0.7961(6) 1.0202(5) 0.6226(4) 0.061(1) Uani C 1.0 C15 -0.0823(5) 0.1922(4) 0.3345(4) 0.0451(6) Uani C 1.0 C16 -0.1524(5) 0.2573(4) 0.2564(4) 0.0463(6) Uani C 1.0 C17 -0.2817(5) 0.1855(5) 0.1617(4) 0.0600(7) Uani C 1.0 C18 -0.3438(6) 0.2528(6) 0.0961(4) 0.0693(9) Uani C 1.0 C19 -0.2738(6) 0.3890(6) 0.1267(4) 0.064(1) Uani C 1.0 C20 -0.1451(5) 0.4533(5) 0.2211(4) 0.0501(8) Uani C 1.0 C21 0.1385(5) 0.2609(4) 0.5112(4) 0.0445(6) Uani C 1.0 C22 0.2683(5) 0.3894(5) 0.5898(4) 0.0449(5) Uani C 1.0 C23 0.3740(6) 0.3937(6) 0.6888(4) 0.0581(8) Uani C 1.0 C24 0.4832(6) 0.5156(7) 0.7587(4) 0.0662(8) Uani C 1.0 C25 0.4903(6) 0.6287(6) 0.7282(4) 0.0610(6) Uani C 1.0 C26 0.3819(5) 0.6182(5) 0.6289(4) 0.0477(4) Uani C 1.0 P1 0.2102(2) 0.1666(2) 0.8885(2) 0.056(2) Uani P 0.76 F1 0.0767(5) 0.0239(3) 0.8644(3) 0.097(2) Uani F 0.76 F2 0.1049(5) 0.2230(5) 0.8795(4) 0.184(2) Uani F 0.76 F3 0.1701(5) 0.1559(4) 0.7630(2) 0.142(3) Uani F 0.76 F4 0.3437(5) 0.3094(4) 0.9125(3) 0.159(3) Uani F 0.76 F5 0.3154(5) 0.1103(6) 0.8974(5) 0.181(4) Uani F 0.76 F6 0.2503(5) 0.1774(4) 1.0140(2) 0.123(2) Uani F 0.76 P1' 0.2191(8) 0.1782(7) 0.8912(6) 0.059(2) Uani P 0.24 F1' 0.1342(15) 0.1346(13) 0.7636(6) 0.115(2) Uani F 0.24 F2' 0.3708(11) 0.2277(21) 0.8810(14) 0.191(6) Uani F 0.24 F3' 0.2022(22) 0.0393(11) 0.8968(11) 0.137(2) Uani F 0.24 F4' 0.3039(15) 0.2219(13) 1.0188(7) 0.110(2) Uani F 0.24 F5' 0.0673(11) 0.1287(20) 0.9014(12) 0.141(3) Uani F 0.24 F6' 0.2360(24) 0.3172(10) 0.8856(13) 0.209(2) Uani F 0.24 H1C1 0.1260 0.1927 0.2998 0.047 Uani H 1.0 H2C1 0.2759 0.3189 0.3931 0.042 Uani H 1.0 HC3 0.0637 0.2245 0.1127 0.052 Uani H 1.0 HC4 0.0788 0.3801 -0.0063 0.058 Uani H 1.0 HC5 0.2047 0.6097 0.0719 0.055 Uani H 1.0 HC9 0.4798 1.0423 0.2733 0.064 Uani H 1.0 HC10 0.6598 1.0813 0.4540 0.052 Uani H 1.0 HC12 0.4623 0.6790 0.4348 0.041 Uani H 1.0 H1C13 0.1721 0.8837 0.0224 0.081 Uani H 1.0 H2C13 0.2407 0.9722 0.1455 0.081 Uani H 1.0 H3C13 0.3538 0.9750 0.0918 0.081 Uani H 1.0 H1C14 0.8556 1.0140 0.6970 0.061 Uani H 1.0 H2C14 0.8604 1.0523 0.5804 0.061 Uani H 1.0 H3C14 0.7616 1.0836 0.6311 0.061 Uani H 1.0 H1C15 -0.1330 0.1628 0.3859 0.048 Uani H 1.0 H2C15 -0.0952 0.1135 0.2914 0.052 Uani H 1.0 HC17 -0.3300 0.0872 0.1404 0.069 Uani H 1.0 HC18 -0.4382 0.2029 0.0275 0.085 Uani H 1.0 HC19 -0.3163 0.4391 0.0807 0.076 Uani H 1.0 HC20 -0.0939 0.5518 0.2431 0.052 Uani H 1.0 H1C21 0.1736 0.1967 0.5076 0.052 Uani H 1.0 H2C21 0.0564 0.2231 0.5378 0.047 Uani H 1.0 HC23 0.3710 0.3106 0.7087 0.067 Uani H 1.0 HC24 0.5571 0.5209 0.8318 0.081 Uani H 1.0 HC25 0.5721 0.7174 0.7766 0.072 Uani H 1.0 HC26 0.3855 0.7007 0.6068 0.049 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Cu 0.0404(3) 0.0278(3) 0.0391(3) 0.0183(2) 0.0085(2) -0.0002(2) Cu Cl 0.0583(7) 0.0293(5) 0.0593(7) 0.0234(5) 0.0245(6) 0.0053(5) Cl O1 0.077(2) 0.044(2) 0.052(3) 0.025(1) 0.002(1) 0.012(1) O O2 0.054(2) 0.038(1) 0.051(1) 0.019(1) 0.004(1) 0.0023(9) O N1 0.0380(6) 0.0302(7) 0.0403(7) 0.0174(5) 0.0157(5) 0.0054(4) N N2 0.0366(8) 0.0428(9) 0.0418(7) 0.0198(6) 0.0132(6) 0.0049(5) N N3 0.0389(6) 0.0397(6) 0.0387(7) 0.0195(5) 0.0135(5) 0.0047(5) N N4 0.0432(8) 0.0288(8) 0.0470(7) 0.0182(6) 0.0207(5) 0.0066(5) N C1 0.0461(9) 0.0301(8) 0.0496(7) 0.0204(8) 0.0228(6) 0.0069(5) C C2 0.0401(7) 0.0312(8) 0.0417(7) 0.0170(6) 0.0167(6) 0.0031(5) C C3 0.046(1) 0.040(1) 0.0432(7) 0.017(1) 0.0184(6) -0.0004(6) C C4 0.050(1) 0.054(1) 0.0404(7) 0.025(1) 0.0186(7) 0.0056(7) C C5 0.054(1) 0.051(1) 0.0450(7) 0.0301(9) 0.0237(8) 0.0150(8) C C6 0.0466(7) 0.0360(7) 0.0459(7) 0.0227(6) 0.0221(7) 0.0111(6) C C7 0.038(1) 0.0309(9) 0.040(2) 0.0154(7) 0.017(1) 0.0071(7) C C8 0.051(1) 0.034(1) 0.046(2) 0.0181(7) 0.014(1) 0.0107(7) C C9 0.051(2) 0.032(1) 0.054(3) 0.0166(8) 0.017(1) 0.0126(8) C C10 0.040(2) 0.030(1) 0.054(2) 0.0140(8) 0.017(1) 0.0072(7) C C11 0.038(1) 0.0312(9) 0.045(1) 0.0150(8) 0.0148(9) 0.0051(7) C C12 0.035(1) 0.030(1) 0.041(1) 0.0150(8) 0.018(1) 0.0071(7) C C13 0.089(4) 0.052(3) 0.068(4) 0.033(3) 0.001(3) 0.021(3) C C14 0.047(3) 0.043(3) 0.058(3) 0.013(2) 0.001(2) -0.002(2) C C15 0.0452(9) 0.0299(8) 0.0543(8) 0.0122(6) 0.0237(6) 0.0007(5) C C16 0.0369(8) 0.0426(9) 0.0462(8) 0.0125(6) 0.0143(6) -0.0024(6) C C17 0.0382(9) 0.064(1) 0.051(1) 0.0106(7) 0.0125(7) -0.0098(9) C C18 0.040(1) 0.097(2) 0.049(1) 0.0251(9) 0.0077(8) -0.002(1) C C19 0.047(1) 0.097(2) 0.0490(9) 0.041(1) 0.0130(8) 0.015(1) C C20 0.0445(9) 0.065(1) 0.0469(8) 0.0335(9) 0.0163(7) 0.0142(7) C C21 0.055(1) 0.0392(7) 0.0537(8) 0.0294(6) 0.0283(6) 0.0172(6) C C22 0.0480(7) 0.0508(7) 0.0439(7) 0.0306(6) 0.0192(5) 0.0148(6) C C23 0.060(1) 0.082(1) 0.0479(8) 0.047(1) 0.0222(6) 0.0249(8) C C24 0.0540(9) 0.101(2) 0.0421(8) 0.042(1) 0.0131(5) 0.0143(8) C C25 0.0444(8) 0.079(1) 0.0409(8) 0.0231(8) 0.0096(6) -0.0024(8) C C26 0.0403(7) 0.0488(7) 0.0411(7) 0.0161(6) 0.0127(5) -0.0023(6) C P1 0.060(1) 0.046(2) 0.047(1) 0.023(1) 0.0109(6) 0.0035(8) P F1 0.093(2) 0.061(3) 0.062(1) 0.002(1) 0.003(1) 0.0131(9) F F2 0.164(4) 0.160(4) 0.205(3) 0.133(4) -0.017(4) -0.059(4) F F3 0.120(3) 0.135(3) 0.051(2) -0.015(3) 0.021(1) 0.012(1) F F4 0.137(3) 0.085(2) 0.085(3) -0.031(2) -0.008(3) 0.022(2) F F5 0.110(2) 0.218(6) 0.198(4) 0.118(4) -0.001(3) -0.054(5) F F6 0.116(3) 0.115(3) 0.047(1) 0.002(2) 0.0152(8) -0.003(1) F P1' 0.063(1) 0.046(2) 0.049(1) 0.022(1) 0.0102(6) 0.0038(8) P F1' 0.106(3) 0.099(2) 0.048(2) -0.001(2) 0.0106(8) 0.0118(8) F F2' 0.071(2) 0.268(7) 0.127(5) 0.004(2) 0.043(2) -0.021(5) F F3' 0.144(3) 0.074(3) 0.135(2) 0.074(2) -0.028(3) -0.008(2) F F4' 0.108(3) 0.090(3) 0.050(1) 0.009(2) 0.004(1) -0.005(1) F F5' 0.083(2) 0.196(5) 0.120(3) 0.057(2) 0.036(2) -0.042(3) F F6' 0.243(6) 0.051(1) 0.174(4) 0.059(2) -0.057(5) -0.003(2) F # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu Cl 2.228(1) 1_555 1_555 no Cu N1 2.509(3) 1_555 1_555 no Cu N2 1.984(3) 1_555 1_555 no Cu N3 1.977(3) 1_555 1_555 no Cu N4 2.051(3) 1_555 1_555 no O1 C8 1.363(5) 1_555 1_555 no O1 C13 1.418(6) 1_555 1_555 no O2 C11 1.372(5) 1_555 1_555 no O2 C14 1.424(5) 1_555 1_555 no N1 C2 1.337(5) 1_555 1_555 no N1 C6 1.341(5) 1_555 1_555 no N2 C16 1.348(6) 1_555 1_555 no N2 C20 1.347(5) 1_555 1_555 no N3 C22 1.347(6) 1_555 1_555 no N3 C26 1.339(5) 1_555 1_555 no N4 C1 1.483(5) 1_555 1_555 no N4 C15 1.486(5) 1_555 1_555 no N4 C21 1.490(5) 1_555 1_555 no C1 C2 1.508(6) 1_555 1_555 no C2 C3 1.384(6) 1_555 1_555 no C3 C4 1.391(6) 1_555 1_555 no C4 C5 1.374(6) 1_555 1_555 no C5 C6 1.397(6) 1_555 1_555 no C6 C7 1.488(6) 1_555 1_555 no C7 C8 1.408(6) 1_555 1_555 no C7 C12 1.385(6) 1_555 1_555 no C8 C9 1.392(6) 1_555 1_555 no C9 C10 1.383(6) 1_555 1_555 no C10 C11 1.379(6) 1_555 1_555 no C11 C12 1.391(5) 1_555 1_555 no C15 C16 1.503(6) 1_555 1_555 no C16 C17 1.378(6) 1_555 1_555 no C17 C18 1.395(8) 1_555 1_555 no C18 C19 1.383(8) 1_555 1_555 no C19 C20 1.366(7) 1_555 1_555 no C21 C22 1.512(6) 1_555 1_555 no C22 C23 1.394(6) 1_555 1_555 no C23 C24 1.383(8) 1_555 1_555 no C24 C25 1.365(8) 1_555 1_555 no C25 C26 1.387(6) 1_555 1_555 no P1 F1 1.554(2) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Cu N1 105.70(8) 1_555 1_555 1_555 no Cl Cu N2 96.1(1) 1_555 1_555 1_555 no Cl Cu N3 97.1(1) 1_555 1_555 1_555 no Cl Cu N4 174.2(1) 1_555 1_555 1_555 no N1 Cu N2 86.5(1) 1_555 1_555 1_555 no N1 Cu N3 96.7(1) 1_555 1_555 1_555 no N1 Cu N4 80.1(1) 1_555 1_555 1_555 no N2 Cu N3 165.0(2) 1_555 1_555 1_555 no N2 Cu N4 83.4(1) 1_555 1_555 1_555 no N3 Cu N4 82.8(1) 1_555 1_555 1_555 no C8 O1 C13 118.6(4) 1_555 1_555 1_555 no C11 O2 C14 117.3(4) 1_555 1_555 1_555 no Cu N1 C2 96.2(3) 1_555 1_555 1_555 no Cu N1 C6 125.5(3) 1_555 1_555 1_555 no C2 N1 C6 119.4(4) 1_555 1_555 1_555 no Cu N2 C16 113.8(3) 1_555 1_555 1_555 no Cu N2 C20 127.6(3) 1_555 1_555 1_555 no C16 N2 C20 118.6(4) 1_555 1_555 1_555 no Cu N3 C22 114.1(3) 1_555 1_555 1_555 no Cu N3 C26 126.4(3) 1_555 1_555 1_555 no C22 N3 C26 119.4(4) 1_555 1_555 1_555 no Cu N4 C1 109.6(2) 1_555 1_555 1_555 no Cu N4 C15 106.3(2) 1_555 1_555 1_555 no Cu N4 C21 106.4(2) 1_555 1_555 1_555 no C1 N4 C15 111.2(3) 1_555 1_555 1_555 no C1 N4 C21 110.4(3) 1_555 1_555 1_555 no C15 N4 C21 112.8(3) 1_555 1_555 1_555 no N4 C1 C2 112.4(3) 1_555 1_555 1_555 no N1 C2 C1 113.8(4) 1_555 1_555 1_555 no N1 C2 C3 123.6(4) 1_555 1_555 1_555 no C1 C2 C3 122.6(4) 1_555 1_555 1_555 no C2 C3 C4 116.7(4) 1_555 1_555 1_555 no C3 C4 C5 120.1(4) 1_555 1_555 1_555 no C4 C5 C6 119.6(4) 1_555 1_555 1_555 no N1 C6 C5 120.3(4) 1_555 1_555 1_555 no N1 C6 C7 115.3(4) 1_555 1_555 1_555 no C5 C6 C7 124.1(4) 1_555 1_555 1_555 no C6 C7 C8 124.8(4) 1_555 1_555 1_555 no C6 C7 C12 117.1(4) 1_555 1_555 1_555 no C8 C7 C12 117.9(4) 1_555 1_555 1_555 no O1 C8 C7 117.4(4) 1_555 1_555 1_555 no O1 C8 C9 123.0(4) 1_555 1_555 1_555 no C7 C8 C9 119.6(4) 1_555 1_555 1_555 no C8 C9 C10 121.3(4) 1_555 1_555 1_555 no C9 C10 C11 119.6(4) 1_555 1_555 1_555 no O2 C11 C10 125.2(4) 1_555 1_555 1_555 no O2 C11 C12 115.4(4) 1_555 1_555 1_555 no C10 C11 C12 119.4(4) 1_555 1_555 1_555 no C7 C12 C11 122.2(4) 1_555 1_555 1_555 no N4 C15 C16 110.5(3) 1_555 1_555 1_555 no N2 C16 C15 116.0(4) 1_555 1_555 1_555 no N2 C16 C17 121.8(5) 1_555 1_555 1_555 no C15 C16 C17 122.1(4) 1_555 1_555 1_555 no C16 C17 C18 118.6(5) 1_555 1_555 1_555 no C17 C18 C19 119.5(5) 1_555 1_555 1_555 no C18 C19 C20 118.4(5) 1_555 1_555 1_555 no N2 C20 C19 123.0(5) 1_555 1_555 1_555 no N4 C21 C22 109.5(3) 1_555 1_555 1_555 no N3 C22 C21 116.1(4) 1_555 1_555 1_555 no N3 C22 C23 121.2(4) 1_555 1_555 1_555 no C21 C22 C23 122.7(4) 1_555 1_555 1_555 no C22 C23 C24 118.5(5) 1_555 1_555 1_555 no C23 C24 C25 120.1(5) 1_555 1_555 1_555 no C24 C25 C26 118.7(5) 1_555 1_555 1_555 no N3 C26 C25 121.9(5) 1_555 1_555 1_555 no F1 P1 F2 90.00 1_555 1_555 1_555 no #===END data_[Cu4(L)4(CO3)2][BF4]4.5.2H2O _database_code_CSD 190795 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C106 H104 Cu4 N16 O14 4+, 4(B F4 1-), 5.2(H2 O)' _chemical_formula_sum 'C106 H114.4 B4 Cu4 F16 N16 O19.2' _chemical_formula_iupac ? _chemical_formula_weight 2521.2 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 17.903(18) _cell_length_b 18.445(15) _cell_length_c 17.806(28) _cell_angle_alpha 90 _cell_angle_beta 91.71(5) _cell_angle_gamma 90 _cell_volume 5877(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 9 _cell_measurement_theta_max 10 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592.0 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5692 _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_theta_max 20 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 22 # REFINEMENT DATA _refine_special_details ; Data were rather poor quality and limited in theta range. The cation was refined using eight refineable planar groups of four types to describe the pyridine and hydroquinone moieties, and single atom positional parameters for the remaining atoms. The tetrafluoroborates were modelled as ideal tetrahedra with a common refineable B-F distance. Thermal motion of the cation was refined using five 15-parameter TLX rigid body thermal parameters, one for each hydroquinone, one for the uncoordinated pyridine, and one each for the remaining ligand atoms associated with each copper. Individual anisotropic parameters were used for the metals, carbonates and waters. Two additional thermal groups were used for the anions. ; _reflns_number_total 5463 _reflns_number_gt 3261 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.060 _refine_ls_wR_factor_ref 0.088 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3261 _refine_ls_number_parameters 307 _refine_ls_goodness_of_fit_ref 1.71 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.83 _refine_diff_density_min -0.63 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy CuA 0.51831(7) 0.57913(6) 0.54318(6) 0.0571(4) Uani Cu 1.0 O1A 0.8879(5) 0.8873(4) 0.5109(5) 0.153(3) Uani O 1.0 O2A 0.9077(7) 0.6722(5) 0.7250(6) 0.245(8) Uani O 1.0 N1A 0.7055(5) 0.7705(4) 0.5751(3) 0.068(2) Uani N 1.0 N2A 0.6010(3) 0.5493(3) 0.6130(3) 0.056(1) Uani N 1.0 N3A 0.4510(4) 0.6343(3) 0.4744(3) 0.056(1) Uani N 1.0 N4A 0.5921(4) 0.6559(4) 0.5137(4) 0.052(1) Uani N 1.0 C1A 0.5826(5) 0.7198(5) 0.5658(5) 0.061(2) Uani C 1.0 C2A 0.6349(6) 0.7825(4) 0.5533(4) 0.068(2) Uani C 1.0 C3A 0.6100(7) 0.8467(5) 0.5237(5) 0.083(2) Uani C 1.0 C4A 0.6605(7) 0.9016(6) 0.5160(5) 0.098(3) Uani C 1.0 C5A 0.7335(8) 0.8923(6) 0.5375(5) 0.096(3) Uani C 1.0 C6A 0.7565(7) 0.8243(6) 0.5680(4) 0.080(2) Uani C 1.0 C7A 0.8335(5) 0.8028(5) 0.5920(5) 0.086(3) Uani C 1.0 C8A 0.8986(5) 0.8340(4) 0.5643(4) 0.119(2) Uani C 1.0 C9A 0.9679(6) 0.8112(5) 0.5903(6) 0.165(3) Uani C 1.0 C10A 0.9733(6) 0.7584(7) 0.6427(7) 0.179(5) Uani C 1.0 C11A 0.9112(7) 0.7261(5) 0.6718(6) 0.166(4) Uani C 1.0 C12A 0.8408(6) 0.7502(5) 0.6445(5) 0.117(3) Uani C 1.0 C13A 0.9477(11) 0.9137(12) 0.4761(13) 0.249(5) Uani C 1.0 C14A 0.9695(14) 0.6506(15) 0.7615(15) 0.331(9) Uani C 1.0 C15A 0.6656(5) 0.6209(5) 0.5223(5) 0.060(2) Uani C 1.0 C16A 0.6678(4) 0.5752(3) 0.5927(3) 0.063(2) Uani C 1.0 C17A 0.7324(4) 0.5604(4) 0.6320(5) 0.080(2) Uani C 1.0 C18A 0.7294(4) 0.5174(4) 0.6947(5) 0.093(2) Uani C 1.0 C19A 0.6615(5) 0.4900(4) 0.7168(4) 0.084(2) Uani C 1.0 C20A 0.5991(4) 0.5071(4) 0.6747(4) 0.065(1) Uani C 1.0 C21A 0.5706(6) 0.6758(5) 0.4353(5) 0.058(2) Uani C 1.0 C22A 0.4873(4) 0.6696(3) 0.4201(4) 0.061(1) Uani C 1.0 C23A 0.4513(5) 0.6980(4) 0.3585(4) 0.078(2) Uani C 1.0 C24A 0.3753(5) 0.6905(4) 0.3511(4) 0.091(2) Uani C 1.0 C25A 0.3366(4) 0.6544(4) 0.4060(5) 0.084(2) Uani C 1.0 C26A 0.3763(4) 0.6273(3) 0.4662(4) 0.066(1) Uani C 1.0 CuB 0.30750(7) 0.51841(6) 0.71794(6) 0.0586(5) Uani Cu 1.0 O1B 0.0986(4) 0.3704(4) 0.6055(4) 0.119(2) Uani O 1.0 O2B 0.3545(5) 0.2454(4) 0.7260(4) 0.113(3) Uani O 1.0 N1B 0.2066(4) 0.4706(4) 0.7719(4) 0.064(1) Uani N 1.0 N2B 0.2378(3) 0.5725(3) 0.6527(3) 0.064(1) Uani N 1.0 N3B 0.3879(3) 0.4932(4) 0.7914(3) 0.064(1) Uani N 1.0 N4B 0.2881(4) 0.6001(4) 0.7935(4) 0.063(1) Uani N 1.0 C1B 0.2370(6) 0.5726(6) 0.8525(5) 0.072(1) Uani C 1.0 C2B 0.1788(4) 0.5220(5) 0.8178(4) 0.071(1) Uani C 1.0 C3B 0.1044(6) 0.5259(6) 0.8339(5) 0.087(1) Uani C 1.0 C4B 0.0569(6) 0.4751(6) 0.8017(5) 0.096(2) Uani C 1.0 C5B 0.0836(6) 0.4234(6) 0.7558(5) 0.090(2) Uani C 1.0 C6B 0.1589(6) 0.4225(5) 0.7419(5) 0.074(1) Uani C 1.0 C7B 0.1963(5) 0.3639(4) 0.6969(4) 0.069(2) Uani C 1.0 C8B 0.1623(4) 0.3355(4) 0.6313(4) 0.089(2) Uani C 1.0 C9B 0.1926(5) 0.2761(5) 0.5965(5) 0.103(2) Uani C 1.0 C10B 0.2553(6) 0.2451(5) 0.6256(6) 0.089(2) Uani C 1.0 C11B 0.2908(6) 0.2709(4) 0.6898(6) 0.084(2) Uani C 1.0 C12B 0.2589(5) 0.3317(4) 0.7247(4) 0.077(2) Uani C 1.0 C13B 0.0614(10) 0.3431(11) 0.5413(9) 0.188(3) Uani C 1.0 C14B 0.3763(9) 0.1746(8) 0.7090(8) 0.133(5) Uani C 1.0 C15B 0.2565(6) 0.6620(5) 0.7508(6) 0.073(2) Uani C 1.0 C16B 0.2204(4) 0.6396(4) 0.6765(4) 0.074(1) Uani C 1.0 C17B 0.1757(5) 0.6854(4) 0.6356(5) 0.098(3) Uani C 1.0 C18B 0.1470(5) 0.6625(5) 0.5674(5) 0.111(3) Uani C 1.0 C19B 0.1639(5) 0.5938(5) 0.5414(4) 0.099(2) Uani C 1.0 C20B 0.2092(4) 0.5509(4) 0.5855(4) 0.076(1) Uani C 1.0 C21B 0.3623(6) 0.6162(6) 0.8280(5) 0.070(2) Uani C 1.0 C22B 0.4074(4) 0.5474(4) 0.8388(4) 0.071(1) Uani C 1.0 C23B 0.4678(5) 0.5432(5) 0.8869(4) 0.090(2) Uani C 1.0 C24B 0.5105(4) 0.4815(5) 0.8873(4) 0.104(2) Uani C 1.0 C25B 0.4918(5) 0.4250(4) 0.8392(5) 0.097(2) Uani C 1.0 C26B 0.4306(4) 0.4329(4) 0.7925(4) 0.076(1) Uani C 1.0 CC 0.4086(6) 0.5166(6) 0.6159(5) 0.051(2) Uani C 1.0 O1C 0.4501(4) 0.4983(3) 0.5603(4) 0.058(2) Uani O 1.0 O2C 0.3578(4) 0.4720(3) 0.6352(3) 0.052(2) Uani O 1.0 O3C 0.4193(4) 0.5768(4) 0.6482(3) 0.064(2) Uani O 1.0 BA 0.3433(3) 0.8460(3) 0.5439(3) 0.124(4) Uani B 1.0 F1A 0.4084(4) 0.8225(5) 0.5213(5) 0.198(5) Uani F 1.0 F2A 0.3366(5) 0.9156(4) 0.5287(5) 0.219(5) Uani F 1.0 F3A 0.2892(4) 0.8099(4) 0.5088(5) 0.195(3) Uani F 1.0 F4A 0.3390(5) 0.8359(5) 0.6169(4) 0.214(6) Uani F 1.0 BB 0.8662(7) 0.1459(9) 0.2040(7) 0.211(9) Uani B 0.63 F1B 0.8523(10) 0.1146(11) 0.1386(9) 0.243(9) Uani F 0.63 F2B 0.8037(10) 0.1721(11) 0.2302(10) 0.242(9) Uani F 0.63 F3B 0.8945(10) 0.0979(13) 0.2517(10) 0.313(9) Uani F 0.63 F4B 0.9144(13) 0.1991(14) 0.1957(12) 0.350(9) Uani F 0.63 BB' 0.8686(14) 0.1721(17) 0.1744(13) 0.232(9) Uani B 0.37 F1B' 0.9079(24) 0.1952(28) 0.2334(19) 0.365(9) Uani F 0.37 F2B' 0.8619(27) 0.2248(22) 0.1247(21) 0.356(9) Uani F 0.37 F3B' 0.9028(18) 0.1166(24) 0.1442(24) 0.307(9) Uani F 0.37 F4B' 0.8018(14) 0.1520(20) 0.1953(18) 0.204(9) Uani F 0.37 OW1 0.4346(5) 0.7219(4) 0.6854(4) 0.110(3) Uani O 1.0 OW2 0.8795(18) 0.3104(16) 0.0525(27) 0.371(9) Uani O 0.63 OW3 0.8498(13) 0.4073(22) -0.0987(26) 0.631(9) Uani O 1.0 H1C1A 0.5910 0.7023 0.6185 0.062 Uani H 1.0 H2C1A 0.5302 0.7379 0.5591 0.065 Uani H 1.0 HC3A 0.5563 0.8533 0.5080 0.089 Uani H 1.0 HC4A 0.6436 0.9491 0.4945 0.118 Uani H 1.0 HC5A 0.7703 0.9325 0.5319 0.111 Uani H 1.0 HC9A 1.0141 0.8336 0.5703 0.220 Uani H 1.0 HC10A 1.0240 0.7424 0.6611 0.234 Uani H 1.0 HC12A 0.7947 0.7276 0.6646 0.138 Uani H 1.0 H1C13A 0.9313 0.9517 0.4392 0.305 Uani H 1.0 H2C13A 0.9834 0.9354 0.5142 0.281 Uani H 1.0 H3C13A 0.9731 0.8735 0.4491 0.270 Uani H 1.0 H1C14A 0.9570 0.6114 0.7978 0.419 Uani H 1.0 H2C14A 1.0059 0.6317 0.7248 0.335 Uani H 1.0 H3C14A 0.9922 0.6926 0.7895 0.342 Uani H 1.0 H1C15A 0.7054 0.6588 0.5261 0.066 Uani H 1.0 H2C15A 0.6743 0.5893 0.4777 0.063 Uani H 1.0 HC17A 0.7811 0.5805 0.6155 0.091 Uani H 1.0 HC18A 0.7762 0.5058 0.7243 0.113 Uani H 1.0 HC19A 0.6584 0.4586 0.7623 0.097 Uani H 1.0 HC20A 0.5499 0.4876 0.6903 0.065 Uani H 1.0 H1C21A 0.5969 0.6426 0.4003 0.062 Uani H 1.0 H2C21A 0.5864 0.7269 0.4259 0.064 Uani H 1.0 HC23A 0.4799 0.7240 0.3192 0.087 Uani H 1.0 HC24A 0.3478 0.7110 0.3062 0.110 Uani H 1.0 HC25A 0.2811 0.6484 0.4015 0.099 Uani H 1.0 HC26A 0.3487 0.6012 0.5061 0.067 Uani H 1.0 H1C1B 0.2113 0.6146 0.8761 0.164 Uani H 1.0 H2C1B 0.2670 0.5458 0.8918 0.178 Uani H 1.0 HC3B 0.0852 0.5644 0.8679 0.088 Uani H 1.0 HC4B 0.0024 0.4764 0.8123 0.087 Uani H 1.0 HC5B 0.0493 0.3865 0.7324 0.095 Uani H 1.0 HC9B 0.1682 0.2561 0.5497 0.138 Uani H 1.0 HC10B 0.2767 0.2020 0.5997 0.102 Uani H 1.0 HC12B 0.2835 0.3516 0.7714 0.094 Uani H 1.0 H1C13B 0.0165 0.3737 0.5292 0.228 Uani H 1.0 H2C13B 0.0958 0.3441 0.4981 0.129 Uani H 1.0 H3C13B 0.0453 0.2921 0.5508 0.142 Uani H 1.0 H1C14B 0.4229 0.1622 0.7385 0.170 Uani H 1.0 H2C14B 0.3357 0.1401 0.7222 0.171 Uani H 1.0 H3C14B 0.3859 0.1709 0.6540 0.156 Uani H 1.0 H1C15B 0.2976 0.6971 0.7409 0.080 Uani H 1.0 H2C15B 0.2179 0.6860 0.7817 0.084 Uani H 1.0 HC17B 0.1639 0.7348 0.6550 0.114 Uani H 1.0 HC18B 0.1140 0.6953 0.5364 0.138 Uani H 1.0 HC19B 0.1435 0.5762 0.4918 0.116 Uani H 1.0 HC20B 0.2216 0.5012 0.5671 0.075 Uani H 1.0 H1C21B 0.3557 0.6398 0.8779 0.082 Uani H 1.0 H2C21B 0.3897 0.6499 0.7944 0.073 Uani H 1.0 HC23B 0.4807 0.5845 0.9214 0.103 Uani H 1.0 HC24B 0.5551 0.4774 0.9222 0.127 Uani H 1.0 HC25B 0.5224 0.3796 0.8387 0.115 Uani H 1.0 HC26B 0.4167 0.3923 0.7576 0.078 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol CuA 0.0626(9) 0.0493(8) 0.0595(8) -0.0089(6) 0.0056(6) 0.0078(6) Cu O1A 0.122(4) 0.152(6) 0.190(7) -0.060(5) 0.063(5) -0.013(4) O O2A 0.296(9) 0.216(9) 0.220(9) 0.078(8) -0.062(8) 0.019(6) O N1A 0.073(4) 0.067(3) 0.065(3) -0.014(3) 0.016(3) -0.016(3) N N2A 0.061(2) 0.045(2) 0.062(2) 0.000(2) 0.001(2) -0.001(1) N N3A 0.063(2) 0.043(2) 0.060(2) 0.001(2) 0.002(2) 0.000(1) N N4A 0.060(2) 0.041(2) 0.056(2) -0.005(2) 0.013(2) -0.004(2) N C1A 0.065(4) 0.053(3) 0.064(4) -0.001(3) 0.013(4) -0.012(3) C C2A 0.077(3) 0.054(3) 0.073(3) -0.007(3) 0.014(3) -0.013(3) C C3A 0.100(4) 0.051(3) 0.098(5) -0.004(3) 0.013(4) -0.010(3) C C4A 0.126(7) 0.055(3) 0.115(6) -0.018(3) 0.016(6) -0.009(3) C C5A 0.119(6) 0.071(3) 0.098(6) -0.035(4) 0.021(5) -0.017(4) C C6A 0.089(4) 0.080(4) 0.073(5) -0.029(4) 0.020(4) -0.020(4) C C7A 0.094(4) 0.075(6) 0.090(6) -0.022(4) 0.017(4) -0.049(4) C C8A 0.090(4) 0.122(5) 0.148(6) -0.033(4) 0.029(4) -0.059(4) C C9A 0.092(4) 0.185(9) 0.219(9) -0.015(4) 0.009(4) -0.095(5) C C10A 0.131(4) 0.192(9) 0.211(9) 0.034(6) -0.040(5) -0.102(6) C C11A 0.177(5) 0.154(6) 0.163(7) 0.039(6) -0.038(6) -0.047(4) C C12A 0.139(4) 0.099(6) 0.112(6) 0.000(4) 0.000(4) -0.031(4) C C13A 0.165(5) 0.269(9) 0.318(9) -0.093(7) 0.115(8) 0.026(9) C C14A 0.380(9) 0.315(9) 0.291(9) 0.147(9) -0.126(9) 0.011(9) C C15A 0.057(2) 0.050(3) 0.073(3) -0.006(2) 0.015(2) -0.010(2) C C16A 0.057(2) 0.054(2) 0.078(2) 0.000(2) 0.001(2) -0.005(2) C C17A 0.063(2) 0.071(4) 0.107(4) 0.004(2) -0.013(2) -0.007(3) C C18A 0.086(2) 0.077(4) 0.112(4) 0.009(3) -0.032(3) 0.002(3) C C19A 0.101(3) 0.064(3) 0.086(3) 0.004(3) -0.026(3) 0.008(2) C C20A 0.082(2) 0.049(2) 0.065(2) 0.000(2) -0.007(2) 0.004(1) C C21A 0.080(2) 0.041(2) 0.054(2) -0.009(2) 0.015(2) -0.003(2) C C22A 0.083(2) 0.044(2) 0.057(2) -0.003(2) 0.001(2) 0.003(2) C C23A 0.114(4) 0.053(3) 0.066(2) -0.003(3) -0.013(3) 0.009(2) C C24A 0.115(4) 0.066(3) 0.089(3) 0.005(3) -0.032(3) 0.011(2) C C25A 0.083(2) 0.068(3) 0.100(3) 0.008(2) -0.025(2) 0.003(2) C C26A 0.064(2) 0.054(2) 0.080(2) 0.004(2) -0.006(2) -0.002(1) C CuB 0.0684(9) 0.0572(8) 0.0508(8) 0.0017(7) 0.0148(6) -0.0047(6) Cu O1B 0.127(4) 0.142(5) 0.089(4) 0.013(3) -0.010(3) -0.051(3) O O2B 0.139(4) 0.107(4) 0.094(4) 0.021(4) 0.018(3) -0.005(4) O N1B 0.073(2) 0.064(2) 0.056(2) -0.009(2) 0.019(2) -0.002(2) N N2B 0.075(2) 0.063(2) 0.055(2) 0.002(1) 0.007(1) 0.004(2) N N3B 0.073(2) 0.066(2) 0.052(2) 0.000(1) 0.007(1) 0.001(1) N N4B 0.074(2) 0.060(2) 0.056(2) -0.004(1) 0.015(1) -0.010(2) N C1B 0.080(2) 0.080(3) 0.056(2) -0.007(2) 0.021(2) -0.014(2) C C2B 0.076(2) 0.078(3) 0.060(2) -0.009(2) 0.024(2) -0.009(2) C C3B 0.079(2) 0.103(4) 0.083(3) -0.012(2) 0.033(2) -0.020(2) C C4B 0.078(2) 0.113(5) 0.099(4) -0.021(2) 0.035(2) -0.022(3) C C5B 0.080(2) 0.096(4) 0.094(4) -0.025(3) 0.029(2) -0.016(3) C C6B 0.078(2) 0.072(2) 0.073(3) -0.017(2) 0.022(2) -0.007(2) C C7B 0.096(4) 0.053(3) 0.060(3) -0.028(3) 0.021(3) -0.001(2) C C8B 0.107(4) 0.085(3) 0.077(3) -0.018(3) 0.012(3) -0.025(2) C C9B 0.113(5) 0.096(4) 0.099(4) -0.019(3) 0.015(3) -0.042(3) C C10B 0.111(5) 0.064(3) 0.094(4) -0.027(3) 0.032(3) -0.017(3) C C11B 0.112(4) 0.063(3) 0.079(3) -0.015(3) 0.028(3) 0.000(2) C C12B 0.103(4) 0.063(3) 0.066(3) -0.018(3) 0.020(3) -0.001(2) C C13B 0.163(7) 0.259(9) 0.139(5) 0.062(6) -0.048(5) -0.124(6) C C14B 0.176(6) 0.109(5) 0.116(7) 0.040(5) 0.040(5) 0.010(4) C C15B 0.084(3) 0.056(2) 0.081(3) 0.002(2) 0.015(2) -0.008(2) C C16B 0.085(2) 0.062(2) 0.077(2) 0.008(2) 0.007(2) 0.005(2) C C17B 0.107(3) 0.078(2) 0.108(4) 0.021(3) -0.002(3) 0.017(2) C C18B 0.118(3) 0.109(3) 0.105(4) 0.024(3) -0.015(3) 0.028(3) C C19B 0.106(3) 0.116(4) 0.074(2) 0.011(3) -0.013(2) 0.017(2) C C20B 0.085(2) 0.086(2) 0.056(2) 0.002(2) 0.000(2) 0.005(2) C C21B 0.079(2) 0.072(2) 0.060(2) -0.009(2) 0.013(1) -0.017(2) C C22B 0.077(2) 0.083(2) 0.054(2) -0.005(2) 0.004(2) -0.007(2) C C23B 0.087(2) 0.117(4) 0.065(2) -0.003(3) -0.007(2) -0.011(2) C C24B 0.095(2) 0.132(5) 0.083(3) 0.010(3) -0.018(2) 0.002(3) C C25B 0.093(2) 0.105(3) 0.092(3) 0.018(2) -0.012(2) 0.010(2) C C26B 0.082(2) 0.074(2) 0.072(2) 0.009(2) 0.002(2) 0.006(2) C CC 0.058(7) 0.048(7) 0.046(6) 0.000(6) 0.005(6) 0.000(6) C O1C 0.067(4) 0.052(4) 0.057(4) -0.007(3) 0.021(4) -0.002(3) O O2C 0.059(4) 0.049(4) 0.048(4) -0.009(4) 0.018(3) -0.002(3) O O3C 0.086(5) 0.045(4) 0.060(4) -0.008(4) 0.019(4) -0.008(4) O BA 0.147(6) 0.110(5) 0.115(5) -0.033(5) -0.001(4) 0.011(5) B F1A 0.167(6) 0.248(9) 0.179(7) 0.008(6) 0.012(5) -0.017(6) F F2A 0.247(9) 0.117(5) 0.292(9) -0.035(5) -0.041(7) 0.046(5) F F3A 0.189(7) 0.170(7) 0.223(7) -0.053(6) -0.044(6) -0.026(5) F F4A 0.218(8) 0.304(9) 0.121(5) -0.014(7) 0.007(5) 0.042(5) F BB 0.115(9) 0.301(9) 0.215(9) 0.025(9) -0.054(9) -0.130(9) B F1B 0.183(9) 0.323(9) 0.220(9) 0.035(9) -0.009(9) -0.162(9) F F2B 0.203(9) 0.261(9) 0.262(9) 0.070(9) -0.006(9) -0.156(9) F F3B 0.134(9) 0.482(9) 0.320(9) 0.078(9) -0.082(9) -0.027(9) F F4B 0.264(9) 0.490(9) 0.292(9) -0.147(9) -0.061(9) -0.112(9) F BB' 0.159(9) 0.307(9) 0.228(9) -0.001(9) -0.046(9) -0.124(9) B F1B' 0.302(9) 0.510(9) 0.279(9) -0.174(9) -0.078(9) -0.137(9) F F2B' 0.368(9) 0.364(9) 0.333(9) -0.045(9) -0.036(9) -0.038(9) F F3B' 0.171(9) 0.443(9) 0.308(9) 0.081(9) 0.035(9) -0.132(9) F F4B' 0.121(9) 0.262(9) 0.227(9) 0.068(9) -0.045(9) -0.125(9) F OW1 0.149(8) 0.078(5) 0.104(6) -0.023(5) 0.034(6) -0.016(5) O OW2 0.307(9) 0.215(9) 0.607(9) -0.054(9) 0.253(9) -0.203(9) O OW3 0.229(9) 0.701(9) 0.967(9) -0.047(9) 0.113(9) -0.537(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CuA N2A 1.982(5) 1_555 1_555 no CuA N3A 1.974(5) 1_555 1_555 no CuA N4A 2.017(7) 1_555 1_555 no CuA O1C 1.957(6) 1_555 1_555 no CuA O1C 2.411(6) 1_555 3_666 no O1A C8A 1.377(9) 1_555 1_555 no O1A C13A 1.344(14) 1_555 1_555 no O2A C11A 1.376(11) 1_555 1_555 no O2A C14A 1.328(15) 1_555 1_555 no N1A C2A 1.331(10) 1_555 1_555 no N1A C6A 1.357(12) 1_555 1_555 no N2A C16A 1.347(5) 1_555 1_555 no N2A C20A 1.348(6) 1_555 1_555 no N3A C22A 1.347(5) 1_555 1_555 no N3A C26A 1.348(6) 1_555 1_555 no N4A C1A 1.512(10) 1_555 1_555 no N4A C15A 1.470(11) 1_555 1_555 no N4A C21A 1.483(11) 1_555 1_555 no C1A C2A 1.509(12) 1_555 1_555 no C2A C3A 1.365(12) 1_555 1_555 no C3A C4A 1.368(14) 1_555 1_555 no C4A C5A 1.362(16) 1_555 1_555 no C5A C6A 1.423(16) 1_555 1_555 no C6A C7A 1.485(14) 1_555 1_555 no C7A C8A 1.402(10) 1_555 1_555 no C7A C12A 1.350(11) 1_555 1_555 no C8A C9A 1.378(9) 1_555 1_555 no C9A C10A 1.350(12) 1_555 1_555 no C10A C11A 1.377(13) 1_555 1_555 no C11A C12A 1.410(12) 1_555 1_555 no C15A C16A 1.510(11) 1_555 1_555 no C16A C17A 1.361(6) 1_555 1_555 no C17A C18A 1.372(7) 1_555 1_555 no C18A C19A 1.384(7) 1_555 1_555 no C19A C20A 1.364(7) 1_555 1_555 no C21A C22A 1.513(11) 1_555 1_555 no C22A C23A 1.361(6) 1_555 1_555 no C23A C24A 1.372(7) 1_555 1_555 no C24A C25A 1.384(7) 1_555 1_555 no C25A C26A 1.364(7) 1_555 1_555 no CuB N1B 2.251(6) 1_555 1_555 no CuB N2B 1.954(5) 1_555 1_555 no CuB N3B 1.973(5) 1_555 1_555 no CuB N4B 2.057(7) 1_555 1_555 no CuB O2C 1.948(5) 1_555 1_555 no O1B C8B 1.377(9) 1_555 1_555 no O1B C13B 1.399(14) 1_555 1_555 no O2B C11B 1.376(11) 1_555 1_555 no O2B C14B 1.399(14) 1_555 1_555 no N1B C2B 1.356(10) 1_555 1_555 no N1B C6B 1.333(11) 1_555 1_555 no N2B C16B 1.347(5) 1_555 1_555 no N2B C20B 1.348(6) 1_555 1_555 no N3B C22B 1.347(5) 1_555 1_555 no N3B C26B 1.348(6) 1_555 1_555 no N4B C1B 1.502(11) 1_555 1_555 no N4B C15B 1.475(12) 1_555 1_555 no N4B C21B 1.476(12) 1_555 1_555 no C1B C2B 1.516(12) 1_555 1_555 no C2B C3B 1.373(12) 1_555 1_555 no C3B C4B 1.379(14) 1_555 1_555 no C4B C5B 1.352(14) 1_555 1_555 no C5B C6B 1.378(13) 1_555 1_555 no C6B C7B 1.512(12) 1_555 1_555 no C7B C8B 1.402(10) 1_555 1_555 no C7B C12B 1.350(11) 1_555 1_555 no C8B C9B 1.378(9) 1_555 1_555 no C9B C10B 1.350(12) 1_555 1_555 no C10B C11B 1.377(13) 1_555 1_555 no C11B C12B 1.410(12) 1_555 1_555 no C15B C16B 1.511(11) 1_555 1_555 no C16B C17B 1.361(6) 1_555 1_555 no C17B C18B 1.372(7) 1_555 1_555 no C18B C19B 1.384(7) 1_555 1_555 no C19B C20B 1.364(7) 1_555 1_555 no C21B C22B 1.514(12) 1_555 1_555 no C22B C23B 1.361(6) 1_555 1_555 no C23B C24B 1.372(7) 1_555 1_555 no C24B C25B 1.384(7) 1_555 1_555 no C25B C26B 1.364(7) 1_555 1_555 no CC O1C 1.301(10) 1_555 1_555 no CC O2C 1.281(10) 1_555 1_555 no CC O3C 1.262(10) 1_555 1_555 no O1C CuA 2.411(6) 1_555 3_666 no BA F1A 1.317(4) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2A CuA N3A 164.2(3) 1_555 1_555 1_555 no N2A CuA N4A 82.8(3) 1_555 1_555 1_555 no N2A CuA O1C 98.5(3) 1_555 1_555 1_555 no N2A CuA O1C 97.3(2) 1_555 1_555 3_666 no N3A CuA N4A 82.4(3) 1_555 1_555 1_555 no N3A CuA O1C 96.8(3) 1_555 1_555 1_555 no N3A CuA O1C 89.0(2) 1_555 1_555 3_666 no N4A CuA O1C 172.8(3) 1_555 1_555 1_555 no N4A CuA O1C 92.7(2) 1_555 1_555 3_666 no O1C CuA O1C 80.2(3) 1_555 1_555 3_666 no C8A O1A C13A 118.7(11) 1_555 1_555 1_555 no C11A O2A C14A 119.9(13) 1_555 1_555 1_555 no C2A N1A C6A 119.1(7) 1_555 1_555 1_555 no CuA N2A C16A 112.7(4) 1_555 1_555 1_555 no CuA N2A C20A 129.4(5) 1_555 1_555 1_555 no C16A N2A C20A 117.8(3) 1_555 1_555 1_555 no CuA N3A C22A 113.3(4) 1_555 1_555 1_555 no CuA N3A C26A 127.1(4) 1_555 1_555 1_555 no C22A N3A C26A 117.8(3) 1_555 1_555 1_555 no CuA N4A C1A 107.5(5) 1_555 1_555 1_555 no CuA N4A C15A 104.8(5) 1_555 1_555 1_555 no CuA N4A C21A 105.4(5) 1_555 1_555 1_555 no C1A N4A C15A 113.2(7) 1_555 1_555 1_555 no C1A N4A C21A 110.8(7) 1_555 1_555 1_555 no C15A N4A C21A 114.4(7) 1_555 1_555 1_555 no N4A C1A C2A 115.2(7) 1_555 1_555 1_555 no N1A C2A C1A 114.6(7) 1_555 1_555 1_555 no N1A C2A C3A 123.7(9) 1_555 1_555 1_555 no C1A C2A C3A 121.6(10) 1_555 1_555 1_555 no C2A C3A C4A 118.1(12) 1_555 1_555 1_555 no C3A C4A C5A 120.7(12) 1_555 1_555 1_555 no C4A C5A C6A 118.9(11) 1_555 1_555 1_555 no N1A C6A C5A 119.5(11) 1_555 1_555 1_555 no N1A C6A C7A 113.5(10) 1_555 1_555 1_555 no C5A C6A C7A 127.0(11) 1_555 1_555 1_555 no C6A C7A C8A 124.2(9) 1_555 1_555 1_555 no C6A C7A C12A 117.4(9) 1_555 1_555 1_555 no C8A C7A C12A 118.4(8) 1_555 1_555 1_555 no O1A C8A C7A 115.9(8) 1_555 1_555 1_555 no O1A C8A C9A 123.7(8) 1_555 1_555 1_555 no C7A C8A C9A 120.4(6) 1_555 1_555 1_555 no C8A C9A C10A 119.9(8) 1_555 1_555 1_555 no C9A C10A C11A 122.0(10) 1_555 1_555 1_555 no O2A C11A C10A 128.8(10) 1_555 1_555 1_555 no O2A C11A C12A 114.0(10) 1_555 1_555 1_555 no C10A C11A C12A 117.3(10) 1_555 1_555 1_555 no C7A C12A C11A 122.1(9) 1_555 1_555 1_555 no N4A C15A C16A 109.5(7) 1_555 1_555 1_555 no N2A C16A C15A 114.7(6) 1_555 1_555 1_555 no N2A C16A C17A 122.6(4) 1_555 1_555 1_555 no C15A C16A C17A 122.7(7) 1_555 1_555 1_555 no C16A C17A C18A 118.8(6) 1_555 1_555 1_555 no C17A C18A C19A 119.8(6) 1_555 1_555 1_555 no C18A C19A C20A 118.1(5) 1_555 1_555 1_555 no N2A C20A C19A 122.8(5) 1_555 1_555 1_555 no N4A C21A C22A 112.0(7) 1_555 1_555 1_555 no N3A C22A C21A 113.7(6) 1_555 1_555 1_555 no N3A C22A C23A 122.6(4) 1_555 1_555 1_555 no C21A C22A C23A 123.7(7) 1_555 1_555 1_555 no C22A C23A C24A 118.8(6) 1_555 1_555 1_555 no C23A C24A C25A 119.8(6) 1_555 1_555 1_555 no C24A C25A C26A 118.1(5) 1_555 1_555 1_555 no N3A C26A C25A 122.8(5) 1_555 1_555 1_555 no N1B CuB N2B 87.0(2) 1_555 1_555 1_555 no N1B CuB N3B 101.7(2) 1_555 1_555 1_555 no N1B CuB N4B 81.6(3) 1_555 1_555 1_555 no N1B CuB O2C 123.1(3) 1_555 1_555 1_555 no N2B CuB N3B 162.9(3) 1_555 1_555 1_555 no N2B CuB N4B 84.2(3) 1_555 1_555 1_555 no N2B CuB O2C 94.3(3) 1_555 1_555 1_555 no N3B CuB N4B 82.7(3) 1_555 1_555 1_555 no N3B CuB O2C 93.1(3) 1_555 1_555 1_555 no N4B CuB O2C 155.2(3) 1_555 1_555 1_555 no C8B O1B C13B 118.3(10) 1_555 1_555 1_555 no C11B O2B C14B 116.8(11) 1_555 1_555 1_555 no CuB N1B C2B 107.3(5) 1_555 1_555 1_555 no CuB N1B C6B 127.0(5) 1_555 1_555 1_555 no C2B N1B C6B 117.7(6) 1_555 1_555 1_555 no CuB N2B C16B 115.5(4) 1_555 1_555 1_555 no CuB N2B C20B 126.6(5) 1_555 1_555 1_555 no C16B N2B C20B 117.8(3) 1_555 1_555 1_555 no CuB N3B C22B 114.3(4) 1_555 1_555 1_555 no CuB N3B C26B 127.3(5) 1_555 1_555 1_555 no C22B N3B C26B 117.8(3) 1_555 1_555 1_555 no CuB N4B C1B 109.2(6) 1_555 1_555 1_555 no CuB N4B C15B 107.4(6) 1_555 1_555 1_555 no CuB N4B C21B 104.6(6) 1_555 1_555 1_555 no C1B N4B C15B 112.9(8) 1_555 1_555 1_555 no C1B N4B C21B 109.7(7) 1_555 1_555 1_555 no C15B N4B C21B 112.7(8) 1_555 1_555 1_555 no N4B C1B C2B 110.4(7) 1_555 1_555 1_555 no N1B C2B C1B 114.6(6) 1_555 1_555 1_555 no N1B C2B C3B 122.6(8) 1_555 1_555 1_555 no C1B C2B C3B 122.8(9) 1_555 1_555 1_555 no C2B C3B C4B 117.8(10) 1_555 1_555 1_555 no C3B C4B C5B 120.4(11) 1_555 1_555 1_555 no C4B C5B C6B 118.8(11) 1_555 1_555 1_555 no N1B C6B C5B 122.6(10) 1_555 1_555 1_555 no N1B C6B C7B 113.6(8) 1_555 1_555 1_555 no C5B C6B C7B 123.7(10) 1_555 1_555 1_555 no C6B C7B C8B 121.3(8) 1_555 1_555 1_555 no C6B C7B C12B 119.8(8) 1_555 1_555 1_555 no C8B C7B C12B 118.4(8) 1_555 1_555 1_555 no O1B C8B C7B 115.9(8) 1_555 1_555 1_555 no O1B C8B C9B 123.7(8) 1_555 1_555 1_555 no C7B C8B C9B 120.4(6) 1_555 1_555 1_555 no C8B C9B C10B 119.9(8) 1_555 1_555 1_555 no C9B C10B C11B 122.0(10) 1_555 1_555 1_555 no O2B C11B C10B 128.8(10) 1_555 1_555 1_555 no O2B C11B C12B 114.0(10) 1_555 1_555 1_555 no C10B C11B C12B 117.3(10) 1_555 1_555 1_555 no C7B C12B C11B 122.1(9) 1_555 1_555 1_555 no N4B C15B C16B 112.8(7) 1_555 1_555 1_555 no N2B C16B C15B 115.5(6) 1_555 1_555 1_555 no N2B C16B C17B 122.6(4) 1_555 1_555 1_555 no C15B C16B C17B 121.9(7) 1_555 1_555 1_555 no C16B C17B C18B 118.8(6) 1_555 1_555 1_555 no C17B C18B C19B 119.8(6) 1_555 1_555 1_555 no C18B C19B C20B 118.1(5) 1_555 1_555 1_555 no N2B C20B C19B 122.8(5) 1_555 1_555 1_555 no N4B C21B C22B 110.8(8) 1_555 1_555 1_555 no N3B C22B C21B 114.5(6) 1_555 1_555 1_555 no N3B C22B C23B 122.6(4) 1_555 1_555 1_555 no C21B C22B C23B 122.6(7) 1_555 1_555 1_555 no C22B C23B C24B 118.8(6) 1_555 1_555 1_555 no C23B C24B C25B 119.8(6) 1_555 1_555 1_555 no C24B C25B C26B 118.1(5) 1_555 1_555 1_555 no N3B C26B C25B 122.8(5) 1_555 1_555 1_555 no O1C CC O2C 117.6(9) 1_555 1_555 1_555 no O1C CC O3C 119.6(9) 1_555 1_555 1_555 no O2C CC O3C 122.9(9) 1_555 1_555 1_555 no CuA O1C CC 107.0(6) 1_555 1_555 1_555 no CuA O1C CuA 99.8(3) 1_555 1_555 3_666 no CC O1C CuA 152.7(6) 1_555 1_555 3_666 no CuB O2C CC 105.6(6) 1_555 1_555 1_555 no F1A BA F2A 109.47(0) 1_555 1_555 1_555 no #===END data_[ZnCl2(L)] _database_code_CSD 190796 # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 Cl2 N4 O2 Zn' _chemical_formula_sum 'C26 H26 Cl2 N4 O2 Zn' _chemical_formula_iupac ? _chemical_formula_weight 562.8 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.049(4) _cell_length_b 11.144(5) _cell_length_c 14.023(5) _cell_angle_alpha 112.54(2) _cell_angle_beta 100.09(2) _cell_angle_gamma 90.97(3) _cell_volume 1280.4(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 20 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580.0 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.84 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4595 _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ; Thermal motion was refined using three 15-parameter TLX rigid body thermal parameters, one for the hydroquinone, one for the uncoordinated pyridine, and the other with all remaining ligand atoms except the methyls. Individual anisotropic parameters were used for the metal, chlorines, and methyl carbons. ; _reflns_number_total 4488 _reflns_number_gt 3610 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.051 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3610 _refine_ls_number_parameters 180 _refine_ls_goodness_of_fit_ref 1.85 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.015 _refine_diff_density_max 0.70 _refine_diff_density_min -0.51 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Zn 0.41777(4) 0.65337(3) 0.22894(3) 0.0396(1) Uani Zn 1.0 Cl1 0.47983(10) 0.66749(9) 0.08599(7) 0.0581(2) Uani Cl 1.0 Cl2 0.42706(10) 0.84363(8) 0.36691(6) 0.0595(2) Uani Cl 1.0 O1 -0.0803(3) 0.0885(3) 0.3989(2) 0.080(3) Uani O 1.0 O2 -0.2869(4) -0.0009(4) -0.0209(3) 0.122(4) Uani O 1.0 N1 0.1507(3) 0.2814(2) 0.2861(2) 0.0402(8) Uani N 1.0 N2 0.1717(3) 0.6211(2) 0.1800(2) 0.0449(4) Uani N 1.0 N3 0.6275(3) 0.5891(3) 0.2957(2) 0.0456(3) Uani N 1.0 N4 0.3604(3) 0.4519(2) 0.2134(2) 0.0412(4) Uani N 1.0 C1 0.3256(3) 0.4649(3) 0.3171(2) 0.0429(9) Uani C 1.0 C2 0.2918(3) 0.3383(3) 0.3283(2) 0.0424(9) Uani C 1.0 C3 0.3995(4) 0.2876(3) 0.3818(3) 0.051(2) Uani C 1.0 C4 0.3604(4) 0.1733(4) 0.3920(3) 0.056(3) Uani C 1.0 C5 0.2154(4) 0.1149(3) 0.3501(3) 0.051(2) Uani C 1.0 C6 0.1133(3) 0.1700(3) 0.2966(2) 0.043(1) Uani C 1.0 C7 -0.0409(3) 0.1081(3) 0.2439(3) 0.047(2) Uani C 1.0 C8 -0.1369(4) 0.0645(4) 0.2947(3) 0.061(2) Uani C 1.0 C9 -0.2786(4) 0.0032(4) 0.2404(4) 0.077(3) Uani C 1.0 C10 -0.3255(4) -0.0159(4) 0.1363(4) 0.084(4) Uani C 1.0 C11 -0.2335(5) 0.0272(4) 0.0855(4) 0.081(3) Uani C 1.0 C12 -0.0930(4) 0.0900(3) 0.1390(3) 0.059(2) Uani C 1.0 C13 -0.1818(6) 0.0810(6) 0.4616(4) 0.108(2) Uani C 1.0 C14 -0.2382(5) 0.0781(5) -0.0651(3) 0.089(1) Uani C 1.0 C15 0.2290(3) 0.3976(3) 0.1262(2) 0.0447(4) Uani C 1.0 C16 0.1144(3) 0.4963(3) 0.1382(2) 0.0471(4) Uani C 1.0 C17 -0.0400(4) 0.4617(4) 0.1061(3) 0.0577(5) Uani C 1.0 C18 -0.1361(4) 0.5573(4) 0.1156(3) 0.0672(6) Uani C 1.0 C19 -0.0786(4) 0.6849(4) 0.1578(3) 0.0648(7) Uani C 1.0 C20 0.0763(4) 0.7139(3) 0.1893(3) 0.0530(6) Uani C 1.0 C21 0.4937(4) 0.3795(3) 0.1901(2) 0.0460(4) Uani C 1.0 C22 0.6317(3) 0.4595(3) 0.2647(3) 0.0490(3) Uani C 1.0 C23 0.7556(4) 0.4051(4) 0.2981(3) 0.0609(6) Uani C 1.0 C24 0.8775(4) 0.4858(4) 0.3667(3) 0.0695(6) Uani C 1.0 C25 0.8736(4) 0.6181(4) 0.4007(3) 0.0649(4) Uani C 1.0 C26 0.7478(3) 0.6657(4) 0.3632(3) 0.0528(4) Uani C 1.0 H1C1 0.2357 0.5158 0.3282 0.045 Uani H 1.0 H2C1 0.4144 0.5143 0.3732 0.049 Uani H 1.0 HC3 0.5035 0.3327 0.4124 0.058 Uani H 1.0 HC4 0.4362 0.1336 0.4292 0.068 Uani H 1.0 HC5 0.1840 0.0333 0.3581 0.057 Uani H 1.0 HC9 -0.3472 -0.0272 0.2770 0.097 Uani H 1.0 HC10 -0.4273 -0.0615 0.0974 0.108 Uani H 1.0 HC12 -0.0275 0.1232 0.1023 0.067 Uani H 1.0 H1C13 -0.1255 0.1006 0.5348 0.108 Uani H 1.0 H2C13 -0.2573 0.1460 0.4635 0.108 Uani H 1.0 H3C13 -0.2350 -0.0088 0.4315 0.108 Uani H 1.0 H1C14 -0.2870 0.0445 -0.1414 0.089 Uani H 1.0 H2C14 -0.2656 0.1687 -0.0283 0.089 Uani H 1.0 H3C14 -0.1262 0.0793 -0.0582 0.089 Uani H 1.0 H1C15 0.1828 0.3164 0.1277 0.049 Uani H 1.0 H2C15 0.2620 0.3766 0.0576 0.046 Uani H 1.0 HC17 -0.0804 0.3679 0.0764 0.063 Uani H 1.0 HC18 -0.2474 0.5339 0.0918 0.080 Uani H 1.0 HC19 -0.1470 0.7562 0.1658 0.076 Uani H 1.0 HC20 0.1183 0.8074 0.2202 0.055 Uani H 1.0 H1C21 0.5039 0.3617 0.1162 0.047 Uani H 1.0 H2C21 0.4815 0.2950 0.1986 0.051 Uani H 1.0 HC23 0.7566 0.3082 0.2728 0.067 Uani H 1.0 HC24 0.9686 0.4481 0.3916 0.083 Uani H 1.0 HC25 0.9604 0.6787 0.4518 0.074 Uani H 1.0 HC26 0.7456 0.7625 0.3873 0.054 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Zn 0.0372(2) 0.0396(2) 0.0455(2) 0.0030(1) 0.0078(1) 0.0208(2) Zn Cl1 0.0620(5) 0.0693(5) 0.0545(5) 0.0106(4) 0.0203(4) 0.0330(4) Cl Cl2 0.0594(5) 0.0543(5) 0.0526(5) 0.0159(4) 0.0046(4) 0.0102(4) Cl O1 0.069(1) 0.109(3) 0.086(5) -0.002(1) 0.027(1) 0.058(3) O O2 0.108(2) 0.145(5) 0.096(6) -0.046(2) -0.036(2) 0.055(3) O N1 0.038(2) 0.0454(9) 0.0435(9) 0.0066(9) 0.012(1) 0.0222(8) N N2 0.0409(7) 0.0513(7) 0.0463(5) 0.0064(4) 0.0071(5) 0.0236(5) N N3 0.0385(6) 0.0534(6) 0.0479(5) 0.0053(5) 0.0093(4) 0.0228(4) N N4 0.0439(6) 0.0403(6) 0.0429(6) 0.0035(4) 0.0102(4) 0.0193(5) N C1 0.040(2) 0.048(1) 0.044(1) 0.0028(8) 0.011(1) 0.0205(8) C C2 0.039(2) 0.0507(8) 0.043(1) 0.0048(6) 0.009(1) 0.0240(7) C C3 0.045(2) 0.066(2) 0.051(2) 0.0051(7) 0.004(1) 0.034(2) C C4 0.054(3) 0.070(3) 0.059(4) 0.010(1) 0.008(1) 0.042(3) C C5 0.056(3) 0.056(2) 0.054(3) 0.0099(9) 0.015(2) 0.034(2) C C6 0.045(2) 0.047(1) 0.047(1) 0.0066(9) 0.015(2) 0.0239(9) C C7 0.043(1) 0.042(2) 0.062(4) 0.007(1) 0.0149(8) 0.024(2) C C8 0.048(1) 0.065(3) 0.084(5) 0.004(1) 0.020(1) 0.043(3) C C9 0.048(1) 0.080(4) 0.121(6) -0.002(2) 0.014(1) 0.061(4) C C10 0.055(1) 0.081(4) 0.122(7) -0.014(2) -0.007(2) 0.057(4) C C11 0.067(1) 0.082(3) 0.088(5) -0.017(1) -0.011(1) 0.041(3) C C12 0.055(1) 0.058(2) 0.064(4) -0.002(1) 0.0052(8) 0.027(2) C C13 0.098(4) 0.147(5) 0.108(4) -0.008(3) 0.051(3) 0.069(4) C C14 0.081(3) 0.118(4) 0.064(3) 0.029(3) 0.004(2) 0.034(3) C C15 0.0479(7) 0.0448(6) 0.0425(6) -0.0028(5) 0.0090(5) 0.0187(5) C C16 0.0409(7) 0.0559(6) 0.0455(6) -0.0009(5) 0.0055(5) 0.0224(4) C C17 0.0419(8) 0.0781(8) 0.0515(8) -0.0054(6) 0.0031(6) 0.0266(6) C C18 0.0404(8) 0.100(1) 0.062(1) 0.0058(6) 0.0032(7) 0.0358(9) C C19 0.0463(8) 0.091(1) 0.064(1) 0.0203(6) 0.0081(7) 0.0382(9) C C20 0.0475(7) 0.0641(8) 0.0541(7) 0.0162(5) 0.0096(6) 0.0302(7) C C21 0.0522(7) 0.0439(6) 0.0481(7) 0.0106(5) 0.0153(5) 0.0221(5) C C22 0.0453(6) 0.0556(6) 0.0524(6) 0.0141(5) 0.0133(4) 0.0261(4) C C23 0.0533(7) 0.0755(8) 0.064(1) 0.0266(7) 0.0168(6) 0.0351(7) C C24 0.0466(7) 0.099(1) 0.070(1) 0.0249(8) 0.0120(6) 0.041(1) C C25 0.0390(7) 0.095(1) 0.0623(9) 0.0075(6) 0.0065(5) 0.0342(9) C C26 0.0386(6) 0.0690(7) 0.0516(7) 0.0007(5) 0.0072(4) 0.0253(6) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn Cl1 2.234(1) 1_555 1_555 no Zn Cl2 2.244(1) 1_555 1_555 no Zn N2 2.193(2) 1_555 1_555 no Zn N3 2.220(2) 1_555 1_555 no Zn N4 2.215(2) 1_555 1_555 no O1 C8 1.379(5) 1_555 1_555 no O1 C13 1.401(5) 1_555 1_555 no O2 C11 1.393(5) 1_555 1_555 no O2 C14 1.362(6) 1_555 1_555 no N1 C2 1.342(4) 1_555 1_555 no N1 C6 1.349(4) 1_555 1_555 no N2 C16 1.338(4) 1_555 1_555 no N2 C20 1.341(4) 1_555 1_555 no N3 C22 1.343(4) 1_555 1_555 no N3 C26 1.341(4) 1_555 1_555 no N4 C1 1.495(4) 1_555 1_555 no N4 C15 1.475(4) 1_555 1_555 no N4 C21 1.477(4) 1_555 1_555 no C1 C2 1.510(4) 1_555 1_555 no C2 C3 1.386(4) 1_555 1_555 no C3 C4 1.381(4) 1_555 1_555 no C4 C5 1.378(5) 1_555 1_555 no C5 C6 1.387(4) 1_555 1_555 no C6 C7 1.478(4) 1_555 1_555 no C7 C8 1.402(4) 1_555 1_555 no C7 C12 1.397(5) 1_555 1_555 no C8 C9 1.386(5) 1_555 1_555 no C9 C10 1.378(6) 1_555 1_555 no C10 C11 1.374(6) 1_555 1_555 no C11 C12 1.380(5) 1_555 1_555 no C15 C16 1.507(4) 1_555 1_555 no C16 C17 1.390(4) 1_555 1_555 no C17 C18 1.368(5) 1_555 1_555 no C18 C19 1.366(6) 1_555 1_555 no C19 C20 1.386(5) 1_555 1_555 no C21 C22 1.496(4) 1_555 1_555 no C22 C23 1.379(4) 1_555 1_555 no C23 C24 1.372(5) 1_555 1_555 no C24 C25 1.369(6) 1_555 1_555 no C25 C26 1.371(5) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Zn Cl2 115.59(4) 1_555 1_555 1_555 no Cl1 Zn N2 100.25(7) 1_555 1_555 1_555 no Cl1 Zn N3 101.09(7) 1_555 1_555 1_555 no Cl1 Zn N4 114.59(7) 1_555 1_555 1_555 no Cl2 Zn N2 97.09(7) 1_555 1_555 1_555 no Cl2 Zn N3 95.79(7) 1_555 1_555 1_555 no Cl2 Zn N4 129.80(7) 1_555 1_555 1_555 no N2 Zn N3 147.22(9) 1_555 1_555 1_555 no N2 Zn N4 75.01(9) 1_555 1_555 1_555 no N3 Zn N4 73.57(9) 1_555 1_555 1_555 no C8 O1 C13 118.1(3) 1_555 1_555 1_555 no C11 O2 C14 119.6(4) 1_555 1_555 1_555 no C2 N1 C6 118.1(2) 1_555 1_555 1_555 no Zn N2 C16 115.5(2) 1_555 1_555 1_555 no Zn N2 C20 126.1(2) 1_555 1_555 1_555 no C16 N2 C20 118.4(3) 1_555 1_555 1_555 no Zn N3 C22 115.5(2) 1_555 1_555 1_555 no Zn N3 C26 126.8(2) 1_555 1_555 1_555 no C22 N3 C26 117.6(3) 1_555 1_555 1_555 no Zn N4 C1 105.7(2) 1_555 1_555 1_555 no Zn N4 C15 106.6(2) 1_555 1_555 1_555 no Zn N4 C21 107.2(2) 1_555 1_555 1_555 no C1 N4 C15 112.7(2) 1_555 1_555 1_555 no C1 N4 C21 112.3(2) 1_555 1_555 1_555 no C15 N4 C21 112.0(2) 1_555 1_555 1_555 no N4 C1 C2 115.7(2) 1_555 1_555 1_555 no N1 C2 C1 115.7(2) 1_555 1_555 1_555 no N1 C2 C3 122.8(3) 1_555 1_555 1_555 no C1 C2 C3 121.4(3) 1_555 1_555 1_555 no C2 C3 C4 118.7(3) 1_555 1_555 1_555 no C3 C4 C5 119.0(3) 1_555 1_555 1_555 no C4 C5 C6 119.5(3) 1_555 1_555 1_555 no N1 C6 C5 121.9(3) 1_555 1_555 1_555 no N1 C6 C7 115.8(3) 1_555 1_555 1_555 no C5 C6 C7 122.3(3) 1_555 1_555 1_555 no C6 C7 C8 122.4(3) 1_555 1_555 1_555 no C6 C7 C12 119.2(3) 1_555 1_555 1_555 no C8 C7 C12 118.4(3) 1_555 1_555 1_555 no O1 C8 C7 115.5(3) 1_555 1_555 1_555 no O1 C8 C9 124.5(3) 1_555 1_555 1_555 no C7 C8 C9 120.0(4) 1_555 1_555 1_555 no C8 C9 C10 120.3(4) 1_555 1_555 1_555 no C9 C10 C11 120.6(4) 1_555 1_555 1_555 no O2 C11 C10 116.9(4) 1_555 1_555 1_555 no O2 C11 C12 123.3(4) 1_555 1_555 1_555 no C10 C11 C12 119.8(4) 1_555 1_555 1_555 no C7 C12 C11 121.0(3) 1_555 1_555 1_555 no N4 C15 C16 109.5(2) 1_555 1_555 1_555 no N2 C16 C15 115.3(3) 1_555 1_555 1_555 no N2 C16 C17 121.7(3) 1_555 1_555 1_555 no C15 C16 C17 123.1(3) 1_555 1_555 1_555 no C16 C17 C18 119.3(3) 1_555 1_555 1_555 no C17 C18 C19 119.3(3) 1_555 1_555 1_555 no C18 C19 C20 118.9(3) 1_555 1_555 1_555 no N2 C20 C19 122.3(3) 1_555 1_555 1_555 no N4 C21 C22 109.3(2) 1_555 1_555 1_555 no N3 C22 C21 115.0(3) 1_555 1_555 1_555 no N3 C22 C23 122.1(3) 1_555 1_555 1_555 no C21 C22 C23 122.9(3) 1_555 1_555 1_555 no C22 C23 C24 119.1(4) 1_555 1_555 1_555 no C23 C24 C25 119.5(3) 1_555 1_555 1_555 no C24 C25 C26 118.4(3) 1_555 1_555 1_555 no N3 C26 C25 123.3(3) 1_555 1_555 1_555 no #===END