# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Len Barbour' _publ_contact_author_address ; ; _publ_contact_author_email ljb@sun.ac.za loop_ _publ_author_name L.Barbour T.Jacobs # Attachment '- CoCl2 MeOH 100K.CIF' data_CoCl2_MeOH _database_code_depnum_ccdc_archive 'CCDC 892651' #TrackingRef '- CoCl2 MeOH 100K.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 Cl4 Co2 N8, 2(C H4 O)' _chemical_formula_sum 'C46 H52 Cl4 Co2 N8 O2' _chemical_formula_weight 1008.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.232(2) _cell_length_b 15.471(2) _cell_length_c 9.4730(11) _cell_angle_alpha 90.00 _cell_angle_beta 114.150(2) _cell_angle_gamma 90.00 _cell_volume 2304.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 729 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 20.23 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7536 _exptl_absorpt_correction_T_max 0.8980 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7310 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.35 _reflns_number_total 2774 _reflns_number_gt 2072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood & Barbour, 2003) ; _computing_publication_material ; X-Seed (Atwood & Barbour, 2003; Barbour, 2001) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+3.5943P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2774 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl2 Cl 0.13008(11) 0.0000 0.9916(2) 0.0256(4) Uani 1 2 d S . . Cl3 Cl 0.34413(14) 0.0000 1.3445(2) 0.0342(5) Uani 1 2 d S . . Co1 Co 0.27408(6) 0.0000 1.08151(10) 0.0161(3) Uani 1 2 d S . . N4 N 0.3138(2) 0.1095(2) 1.0198(4) 0.0160(8) Uani 1 1 d . . . C5 C 0.3841(3) 0.1565(3) 1.1162(6) 0.0241(11) Uani 1 1 d . . . H5 H 0.4218 0.1399 1.2178 0.029 Uiso 1 1 calc R . . C6 C 0.3907(3) 0.2288(3) 1.0439(6) 0.0244(11) Uani 1 1 d . . . H6 H 0.4332 0.2722 1.0837 0.029 Uiso 1 1 calc R . . N7 N 0.3237(2) 0.2277(2) 0.9005(4) 0.0170(8) Uani 1 1 d . . . C8 C 0.2790(3) 0.1549(3) 0.8899(5) 0.0166(9) Uani 1 1 d . . . C9 C 0.2029(3) 0.1298(3) 0.7519(5) 0.0244(11) Uani 1 1 d . . . H9A H 0.2198 0.1126 0.6689 0.037 Uiso 1 1 calc R . . H9B H 0.1637 0.1790 0.7173 0.037 Uiso 1 1 calc R . . H9C H 0.1746 0.0812 0.7777 0.037 Uiso 1 1 calc R . . C10 C 0.3072(3) 0.2961(3) 0.7844(6) 0.0222(11) Uani 1 1 d . . . H10A H 0.3133 0.3530 0.8356 0.027 Uiso 1 1 calc R . . H10B H 0.2478 0.2911 0.7066 0.027 Uiso 1 1 calc R . . C11 C 0.3664(3) 0.2928(3) 0.7025(5) 0.0162(10) Uani 1 1 d . . . C12 C 0.4134(3) 0.3649(3) 0.7009(5) 0.0165(10) Uani 1 1 d . . . H12 H 0.4098 0.4157 0.7542 0.020 Uiso 1 1 calc R . . C13 C 0.4656(3) 0.3637(3) 0.6220(5) 0.0154(9) Uani 1 1 d . . . H13 H 0.4971 0.4139 0.6212 0.018 Uiso 1 1 calc R . . C14 C 0.4727(3) 0.2905(3) 0.5444(5) 0.0140(9) Uani 1 1 d . . . C15 C 0.4270(3) 0.2171(3) 0.5500(5) 0.0150(9) Uani 1 1 d . . . H15 H 0.4323 0.1655 0.5001 0.018 Uiso 1 1 calc R . . C16 C 0.3743(3) 0.2182(3) 0.6267(5) 0.0179(10) Uani 1 1 d . . . H16 H 0.3432 0.1678 0.6281 0.021 Uiso 1 1 calc R . . C17 C 0.4215(5) 0.0000 0.7891(10) 0.042(2) Uani 1 2 d S . . H17A H 0.4587 0.0231 0.7429 0.062 Uiso 0.50 1 calc PR . . H17B H 0.4387 -0.0592 0.8247 0.062 Uiso 0.50 1 calc PR . . H17C H 0.4259 0.0361 0.8770 0.062 Uiso 0.50 1 calc PR . . O18 O 0.3351(3) 0.0000 0.6756(6) 0.0399(14) Uani 1 2 d S . . H18 H 0.3346 0.0000 0.5866 0.048 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.0250(9) 0.0246(9) 0.0329(10) 0.000 0.0178(8) 0.000 Cl3 0.0603(13) 0.0216(9) 0.0166(9) 0.000 0.0115(9) 0.000 Co1 0.0214(5) 0.0132(4) 0.0158(5) 0.000 0.0097(4) 0.000 N4 0.021(2) 0.0164(18) 0.0120(18) 0.0000(15) 0.0079(16) 0.0007(16) C5 0.021(3) 0.031(3) 0.018(2) -0.004(2) 0.007(2) -0.007(2) C6 0.031(3) 0.024(3) 0.024(3) -0.009(2) 0.017(2) -0.012(2) N7 0.022(2) 0.0144(18) 0.022(2) 0.0016(15) 0.0166(18) -0.0003(15) C8 0.019(2) 0.014(2) 0.023(2) 0.0025(18) 0.015(2) 0.0060(18) C9 0.020(3) 0.025(3) 0.025(3) 0.007(2) 0.006(2) -0.001(2) C10 0.029(3) 0.014(2) 0.029(3) 0.0023(19) 0.016(2) 0.001(2) C11 0.021(2) 0.013(2) 0.018(2) 0.0043(18) 0.012(2) 0.0050(18) C12 0.023(2) 0.010(2) 0.022(2) -0.0020(17) 0.015(2) 0.0034(18) C13 0.015(2) 0.013(2) 0.019(2) 0.0032(17) 0.0078(19) 0.0014(17) C14 0.017(2) 0.015(2) 0.010(2) 0.0037(17) 0.0057(18) 0.0041(17) C15 0.022(2) 0.012(2) 0.013(2) -0.0002(17) 0.009(2) 0.0027(18) C16 0.019(2) 0.014(2) 0.022(3) 0.0030(18) 0.010(2) -0.0009(18) C17 0.036(5) 0.034(5) 0.057(6) 0.000 0.021(5) 0.000 O18 0.039(3) 0.042(3) 0.041(3) 0.000 0.018(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl2 Co1 2.2701(19) . ? Cl3 Co1 2.2811(19) . ? Co1 N4 2.001(4) . ? Co1 N4 2.001(4) 6 ? N4 C8 1.328(5) . ? N4 C5 1.387(6) . ? C5 C6 1.341(7) . ? C5 H5 0.9500 . ? C6 N7 1.376(6) . ? C6 H6 0.9500 . ? N7 C8 1.345(6) . ? N7 C10 1.469(6) . ? C8 C9 1.476(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.513(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.383(6) . ? C11 C16 1.395(6) . ? C12 C13 1.386(6) . ? C12 H12 0.9500 . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.395(6) . ? C14 C14 1.497(8) 2_656 ? C15 C16 1.375(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O18 1.436(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O18 H18 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N4 115.6(2) . 6 ? N4 Co1 Cl2 110.03(11) . . ? N4 Co1 Cl2 110.03(11) 6 . ? N4 Co1 Cl3 103.15(11) . . ? N4 Co1 Cl3 103.15(11) 6 . ? Cl2 Co1 Cl3 114.74(8) . . ? C8 N4 C5 105.9(4) . . ? C8 N4 Co1 129.7(3) . . ? C5 N4 Co1 124.2(3) . . ? C6 C5 N4 109.6(4) . . ? C6 C5 H5 125.2 . . ? N4 C5 H5 125.2 . . ? C5 C6 N7 106.3(4) . . ? C5 C6 H6 126.8 . . ? N7 C6 H6 126.8 . . ? C8 N7 C6 108.0(4) . . ? C8 N7 C10 128.2(4) . . ? C6 N7 C10 123.8(4) . . ? N4 C8 N7 110.2(4) . . ? N4 C8 C9 125.6(4) . . ? N7 C8 C9 124.1(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N7 C10 C11 113.3(4) . . ? N7 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N7 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 118.7(4) . . ? C12 C11 C10 119.9(4) . . ? C16 C11 C10 121.4(4) . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 121.1(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 118.2(4) . . ? C13 C14 C14 120.7(3) . 2_656 ? C15 C14 C14 121.0(3) . 2_656 ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 120.5(4) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? O18 C17 H17A 109.5 . . ? O18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 O18 H18 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O18 H18 Cl3 0.84 2.36 3.203(6) 175.8 1_554 _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.667 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.120 # Attachment '- CoCl2 empty 100K.cif' data_CoCl2_empty _database_code_depnum_ccdc_archive 'CCDC 892652' #TrackingRef '- CoCl2 empty 100K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 Cl4 Co2 N8' _chemical_formula_sum 'C44 H44 Cl4 Co2 N8' _chemical_formula_weight 944.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.020(4) _cell_length_b 14.595(3) _cell_length_c 17.102(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.62(3) _cell_angle_gamma 90.00 _cell_volume 4386.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 764 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 20.96 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7452 _exptl_absorpt_correction_T_max 0.8940 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13411 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.1597 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.36 _reflns_number_total 5107 _reflns_number_gt 3069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood & Barbour, 2003) ; _computing_publication_material ; X-Seed (Atwood & Barbour, 2003; Barbour, 2001) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^+29.6084P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5107 _refine_ls_number_parameters 264 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1992 _refine_ls_R_factor_gt 0.1308 _refine_ls_wR_factor_ref 0.2617 _refine_ls_wR_factor_gt 0.2320 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl2 Cl 0.36765(12) 0.50840(15) 0.52958(17) 0.0363(6) Uani 1 1 d . . . Cl3 Cl 0.17674(13) 0.49395(14) 0.32936(14) 0.0311(5) Uani 1 1 d . . . Co1 Co 0.24219(6) 0.49232(7) 0.47957(8) 0.0198(3) Uani 1 1 d . . . N4A N 0.2130(4) 0.3778(5) 0.5210(5) 0.0241(16) Uani 1 1 d . . . N4B N 0.2098(4) 0.6012(5) 0.5248(5) 0.0251(17) Uani 1 1 d . . . C5A C 0.1633(4) 0.3109(5) 0.4636(5) 0.0192(17) Uani 1 1 d . . . H5A H 0.1374 0.3138 0.4004 0.023 Uiso 1 1 calc R . . C5B C 0.2569(5) 0.6706(6) 0.5786(5) 0.0206(18) Uani 1 1 d . . . H5B H 0.3109 0.6689 0.6107 0.025 Uiso 1 1 calc R . . C6A C 0.1586(4) 0.2429(5) 0.5125(5) 0.0184(17) Uani 1 1 d U . . H6A H 0.1291 0.1887 0.4908 0.022 Uiso 1 1 calc R . . C6B C 0.2122(5) 0.7412(6) 0.5775(6) 0.025(2) Uani 1 1 d . . . H6B H 0.2291 0.7978 0.6081 0.030 Uiso 1 1 calc R . . N7A N 0.2051(3) 0.2659(4) 0.6015(5) 0.0179(15) Uani 1 1 d . . . N7B N 0.1373(4) 0.7151(5) 0.5232(4) 0.0217(15) Uani 1 1 d . . . C8A C 0.2364(4) 0.3485(5) 0.6024(6) 0.0205(18) Uani 1 1 d . . . C8B C 0.1384(5) 0.6304(5) 0.4926(5) 0.0195(18) Uani 1 1 d . . . C9A C 0.2907(5) 0.3969(6) 0.6839(6) 0.032(2) Uani 1 1 d . . . H9A1 H 0.3137 0.4479 0.6679 0.047 Uiso 1 1 calc R . . H9A2 H 0.3306 0.3544 0.7231 0.047 Uiso 1 1 calc R . . H9A3 H 0.2639 0.4207 0.7148 0.047 Uiso 1 1 calc R . . C9B C 0.0688(4) 0.5739(6) 0.4389(6) 0.026(2) Uani 1 1 d . . . H9B1 H 0.0793 0.5294 0.4032 0.039 Uiso 1 1 calc R . . H9B2 H 0.0268 0.6139 0.3993 0.039 Uiso 1 1 calc R . . H9B3 H 0.0547 0.5413 0.4789 0.039 Uiso 1 1 calc R . . C10A C 0.2160(5) 0.2061(5) 0.6744(6) 0.0213(18) Uani 1 1 d . . . H10A H 0.2620 0.2257 0.7291 0.026 Uiso 1 1 calc R . . H10B H 0.2245 0.1427 0.6605 0.026 Uiso 1 1 calc R . . C10B C 0.0723(5) 0.7717(5) 0.5061(5) 0.0229(19) Uani 1 1 d . . . H10C H 0.0273 0.7492 0.4519 0.028 Uiso 1 1 calc R . . H10D H 0.0824 0.8354 0.4947 0.028 Uiso 1 1 calc R . . C11A C 0.1481(5) 0.2071(6) 0.6915(5) 0.0216(18) Uani 1 1 d . . . C11B C 0.0553(4) 0.7712(5) 0.5819(5) 0.0186(18) Uani 1 1 d . . . C12A C 0.1066(4) 0.1270(5) 0.6818(5) 0.0186(17) Uani 1 1 d . . . H12A H 0.1176 0.0730 0.6591 0.022 Uiso 1 1 calc R . . C12B C 0.0658(4) 0.6957(6) 0.6342(5) 0.0216(18) Uani 1 1 d . . . H12B H 0.0883 0.6424 0.6248 0.026 Uiso 1 1 calc R . . C13A C 0.0497(4) 0.1267(5) 0.7055(5) 0.0139(16) Uani 1 1 d . . . H13A H 0.0223 0.0716 0.6992 0.017 Uiso 1 1 calc R . . C13B C 0.0446(4) 0.6945(5) 0.7004(5) 0.0196(18) Uani 1 1 d . . . H13B H 0.0529 0.6411 0.7357 0.024 Uiso 1 1 calc R . . C14A C 0.0312(4) 0.2039(5) 0.7381(5) 0.0121(15) Uani 1 1 d U . . C14B C 0.0113(4) 0.7710(6) 0.7151(5) 0.0199(18) Uani 1 1 d . . . C15A C 0.0730(4) 0.2840(5) 0.7456(5) 0.0155(16) Uani 1 1 d . . . H15A H 0.0612 0.3388 0.7663 0.019 Uiso 1 1 calc R . . C15B C 0.0038(4) 0.8487(5) 0.6646(5) 0.0198(18) Uani 1 1 d . . . H15B H -0.0162 0.9030 0.6761 0.024 Uiso 1 1 calc R . . C16A C 0.1302(4) 0.2845(5) 0.7235(5) 0.0206(18) Uani 1 1 d . . . H16A H 0.1581 0.3393 0.7305 0.025 Uiso 1 1 calc R . . C16B C 0.0242(4) 0.8500(5) 0.5990(5) 0.0190(17) Uani 1 1 d . . . H16B H 0.0174 0.9041 0.5651 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.0215(11) 0.0225(12) 0.0628(17) 0.0052(11) 0.0184(11) -0.0012(9) Cl3 0.0394(13) 0.0224(11) 0.0294(12) 0.0017(9) 0.0149(10) 0.0065(10) Co1 0.0192(6) 0.0108(6) 0.0290(6) 0.0038(5) 0.0113(5) 0.0020(5) N4A 0.019(4) 0.023(4) 0.031(4) 0.003(3) 0.013(3) 0.006(3) N4B 0.023(4) 0.022(4) 0.022(4) 0.003(3) 0.004(3) 0.002(3) C5A 0.017(4) 0.020(4) 0.019(4) -0.005(3) 0.008(4) 0.000(3) C5B 0.016(4) 0.030(5) 0.023(5) 0.006(4) 0.015(4) 0.007(4) C6A 0.017(2) 0.018(2) 0.018(2) -0.0017(17) 0.0065(17) -0.0016(17) C6B 0.033(5) 0.026(5) 0.028(5) -0.001(4) 0.024(5) 0.002(4) N7A 0.012(3) 0.015(4) 0.031(4) -0.003(3) 0.013(3) 0.002(3) N7B 0.023(4) 0.023(4) 0.019(4) 0.004(3) 0.011(3) 0.000(3) C8A 0.017(4) 0.021(4) 0.034(5) 0.005(4) 0.021(4) 0.006(3) C8B 0.026(5) 0.021(4) 0.012(4) 0.008(3) 0.009(4) 0.010(3) C9A 0.017(4) 0.036(5) 0.031(5) -0.005(4) 0.003(4) -0.012(4) C9B 0.018(4) 0.023(5) 0.033(5) 0.001(4) 0.008(4) 0.004(3) C10A 0.022(4) 0.017(4) 0.030(5) 0.004(3) 0.017(4) 0.001(3) C10B 0.030(5) 0.018(4) 0.022(5) 0.005(4) 0.013(4) 0.007(4) C11A 0.021(4) 0.024(5) 0.018(4) 0.008(3) 0.008(4) 0.009(4) C11B 0.010(4) 0.015(4) 0.026(5) -0.002(3) 0.005(4) 0.001(3) C12A 0.015(4) 0.009(4) 0.026(5) -0.001(3) 0.005(4) -0.001(3) C12B 0.019(4) 0.019(4) 0.023(5) -0.001(3) 0.007(4) 0.004(3) C13A 0.006(3) 0.011(4) 0.024(4) -0.003(3) 0.006(3) 0.000(3) C13B 0.016(4) 0.016(4) 0.014(4) 0.004(3) -0.002(3) 0.004(3) C14A 0.011(2) 0.012(2) 0.012(2) 0.0020(16) 0.0044(16) 0.0007(16) C14B 0.012(4) 0.028(5) 0.012(4) -0.008(3) 0.000(3) -0.005(3) C15A 0.011(4) 0.016(4) 0.016(4) 0.002(3) 0.004(3) 0.008(3) C15B 0.013(4) 0.017(4) 0.023(5) -0.001(3) 0.003(4) 0.001(3) C16A 0.019(4) 0.013(4) 0.028(5) 0.000(3) 0.009(4) -0.005(3) C16B 0.017(4) 0.015(4) 0.020(4) 0.007(3) 0.005(4) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl2 Co1 2.244(2) . ? Cl3 Co1 2.256(3) . ? Co1 N4B 2.006(7) . ? Co1 N4A 2.008(7) . ? N4A C8A 1.310(10) . ? N4A C5A 1.404(10) . ? N4B C8B 1.332(10) . ? N4B C5B 1.390(11) . ? C5A C6A 1.331(11) . ? C5A H5A 0.9500 . ? C5B C6B 1.359(11) . ? C5B H5B 0.9500 . ? C6A N7A 1.392(10) . ? C6A H6A 0.9500 . ? C6B N7B 1.386(11) . ? C6B H6B 0.9500 . ? N7A C8A 1.356(10) . ? N7A C10A 1.449(10) . ? N7B C8B 1.345(10) . ? N7B C10B 1.448(10) . ? C8A C9A 1.473(11) . ? C8B C9B 1.497(11) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10A C11A 1.521(11) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C10B C11B 1.489(11) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11A C16A 1.377(11) . ? C11A C12A 1.397(11) . ? C11B C12B 1.372(11) . ? C11B C16B 1.403(10) . ? C12A C13A 1.379(11) . ? C12A H12A 0.9500 . ? C12B C13B 1.385(11) . ? C12B H12B 0.9500 . ? C13A C14A 1.386(10) . ? C13A H13A 0.9500 . ? C13B C14B 1.385(11) . ? C13B H13B 0.9500 . ? C14A C15A 1.406(10) . ? C14A C14A 1.487(14) 2_556 ? C14B C15B 1.390(11) . ? C14B C14B 1.465(16) 2_556 ? C15A C16A 1.366(11) . ? C15A H15A 0.9500 . ? C15B C16B 1.365(11) . ? C15B H15B 0.9500 . ? C16A H16A 0.9500 . ? C16B H16B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4B Co1 N4A 108.7(3) . . ? N4B Co1 Cl2 106.2(2) . . ? N4A Co1 Cl2 114.5(2) . . ? N4B Co1 Cl3 108.2(2) . . ? N4A Co1 Cl3 107.6(2) . . ? Cl2 Co1 Cl3 111.49(11) . . ? C8A N4A C5A 106.8(7) . . ? C8A N4A Co1 129.1(6) . . ? C5A N4A Co1 124.1(6) . . ? C8B N4B C5B 107.1(7) . . ? C8B N4B Co1 125.1(6) . . ? C5B N4B Co1 126.2(5) . . ? C6A C5A N4A 108.6(7) . . ? C6A C5A H5A 125.7 . . ? N4A C5A H5A 125.7 . . ? C6B C5B N4B 108.0(7) . . ? C6B C5B H5B 126.0 . . ? N4B C5B H5B 126.0 . . ? C5A C6A N7A 107.2(7) . . ? C5A C6A H6A 126.4 . . ? N7A C6A H6A 126.4 . . ? C5B C6B N7B 107.1(8) . . ? C5B C6B H6B 126.4 . . ? N7B C6B H6B 126.4 . . ? C8A N7A C6A 106.9(7) . . ? C8A N7A C10A 130.3(7) . . ? C6A N7A C10A 122.8(7) . . ? C8B N7B C6B 107.5(7) . . ? C8B N7B C10B 128.7(7) . . ? C6B N7B C10B 123.8(7) . . ? N4A C8A N7A 110.5(7) . . ? N4A C8A C9A 125.1(8) . . ? N7A C8A C9A 124.4(8) . . ? N4B C8B N7B 110.3(7) . . ? N4B C8B C9B 125.2(7) . . ? N7B C8B C9B 124.2(7) . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C8B C9B H9B1 109.5 . . ? C8B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C8B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? N7A C10A C11A 112.3(6) . . ? N7A C10A H10A 109.1 . . ? C11A C10A H10A 109.1 . . ? N7A C10A H10B 109.1 . . ? C11A C10A H10B 109.1 . . ? H10A C10A H10B 107.9 . . ? N7B C10B C11B 112.3(7) . . ? N7B C10B H10C 109.1 . . ? C11B C10B H10C 109.1 . . ? N7B C10B H10D 109.1 . . ? C11B C10B H10D 109.1 . . ? H10C C10B H10D 107.9 . . ? C16A C11A C12A 118.7(8) . . ? C16A C11A C10A 120.7(7) . . ? C12A C11A C10A 120.3(7) . . ? C12B C11B C16B 117.8(8) . . ? C12B C11B C10B 123.0(7) . . ? C16B C11B C10B 119.2(7) . . ? C13A C12A C11A 119.7(7) . . ? C13A C12A H12A 120.1 . . ? C11A C12A H12A 120.1 . . ? C11B C12B C13B 122.2(8) . . ? C11B C12B H12B 118.9 . . ? C13B C12B H12B 118.9 . . ? C12A C13A C14A 122.2(7) . . ? C12A C13A H13A 118.9 . . ? C14A C13A H13A 118.9 . . ? C14B C13B C12B 120.1(7) . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13A C14A C15A 116.8(7) . . ? C13A C14A C14A 122.1(5) . 2_556 ? C15A C14A C14A 121.1(5) . 2_556 ? C13B C14B C15B 117.6(8) . . ? C13B C14B C14B 120.8(6) . 2_556 ? C15B C14B C14B 121.5(5) . 2_556 ? C16A C15A C14A 121.4(7) . . ? C16A C15A H15A 119.3 . . ? C14A C15A H15A 119.3 . . ? C16B C15B C14B 122.4(8) . . ? C16B C15B H15B 118.8 . . ? C14B C15B H15B 118.8 . . ? C15A C16A C11A 121.2(8) . . ? C15A C16A H16A 119.4 . . ? C11A C16A H16A 119.4 . . ? C15B C16B C11B 119.9(7) . . ? C15B C16B H16B 120.1 . . ? C11B C16B H16B 120.1 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.069 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.147 # Attachment '- ZnCl2 MeOH 100K.CIF' data_ZnCl2_MeOH _database_code_depnum_ccdc_archive 'CCDC 892653' #TrackingRef '- ZnCl2 MeOH 100K.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 Cl4 N8 Zn2, 2(C H4 O)' _chemical_formula_sum 'C46 H52 Cl4 N8 O2 Zn2' _chemical_formula_weight 1021.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 17.36(2) _cell_length_b 15.483(20) _cell_length_c 9.440(12) _cell_angle_alpha 90.00 _cell_angle_beta 113.97(2) _cell_angle_gamma 90.00 _cell_volume 2318(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 654 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 19.27 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7021 _exptl_absorpt_correction_T_max 0.8479 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7139 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.1528 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.21 _reflns_number_total 2778 _reflns_number_gt 1809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood & Barbour, 2003) ; _computing_publication_material ; X-Seed (Atwood & Barbour, 2003; Barbour, 2001) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+3.3583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2778 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl2 Cl 0.12851(14) 0.0000 0.4888(3) 0.0316(5) Uani 1 2 d S . . Cl3 Cl 0.33950(17) 0.0000 0.8465(3) 0.0393(6) Uani 1 2 d S . . Zn1 Zn 0.27122(6) 0.0000 0.58223(11) 0.0205(3) Uani 1 2 d S . . N4 N 0.3133(3) 0.1076(3) 0.5207(5) 0.0211(10) Uani 1 1 d . . . C5 C 0.3849(4) 0.1530(4) 0.6173(7) 0.0305(15) Uani 1 1 d . . . H5 H 0.4229 0.1353 0.7178 0.037 Uiso 1 1 calc R . . C6 C 0.3916(4) 0.2257(4) 0.5455(8) 0.0310(15) Uani 1 1 d . . . H6 H 0.4343 0.2685 0.5860 0.037 Uiso 1 1 calc R . . N7 N 0.3246(3) 0.2265(3) 0.4012(6) 0.0221(11) Uani 1 1 d . . . C8 C 0.2790(3) 0.1547(4) 0.3893(7) 0.0211(12) Uani 1 1 d . . . C9 C 0.2023(4) 0.1303(4) 0.2510(7) 0.0300(15) Uani 1 1 d . . . H9A H 0.1606 0.1769 0.2263 0.045 Uiso 1 1 calc R . . H9B H 0.1784 0.0772 0.2728 0.045 Uiso 1 1 calc R . . H9C H 0.2172 0.1208 0.1626 0.045 Uiso 1 1 calc R . . C10 C 0.3088(4) 0.2957(4) 0.2867(7) 0.0247(14) Uani 1 1 d . . . H10A H 0.3154 0.3521 0.3395 0.030 Uiso 1 1 calc R . . H10B H 0.2498 0.2914 0.2091 0.030 Uiso 1 1 calc R . . C11 C 0.3675(4) 0.2926(4) 0.2035(7) 0.0232(13) Uani 1 1 d . . . C12 C 0.4142(4) 0.3646(3) 0.2027(7) 0.0211(13) Uani 1 1 d . . . H12 H 0.4111 0.4152 0.2573 0.025 Uiso 1 1 calc R . . C13 C 0.4657(3) 0.3631(3) 0.1218(7) 0.0226(13) Uani 1 1 d . . . H13 H 0.4969 0.4133 0.1202 0.027 Uiso 1 1 calc R . . C14 C 0.4723(3) 0.2899(3) 0.0438(7) 0.0190(12) Uani 1 1 d . . . C15 C 0.4273(4) 0.2168(3) 0.0511(6) 0.0197(12) Uani 1 1 d . . . H15 H 0.4334 0.1652 0.0022 0.024 Uiso 1 1 calc R . . C16 C 0.3745(4) 0.2169(4) 0.1264(7) 0.0232(13) Uani 1 1 d . . . H16 H 0.3431 0.1667 0.1267 0.028 Uiso 1 1 calc R . . C17 C 0.4208(6) 0.0000 0.2945(13) 0.045(3) Uani 1 2 d S . . H17A H 0.4353 0.0575 0.3414 0.068 Uiso 0.50 1 calc PR . . H17B H 0.4585 -0.0148 0.2439 0.068 Uiso 0.50 1 calc PR . . H17C H 0.4272 -0.0427 0.3752 0.068 Uiso 0.50 1 calc PR . . O18 O 0.3334(4) 0.0000 0.1792(9) 0.0495(19) Uani 1 2 d S . . H18 H 0.3316 -0.0181 0.0941 0.059 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.0315(12) 0.0293(12) 0.0385(13) 0.000 0.0188(10) 0.000 Cl3 0.0665(17) 0.0266(12) 0.0212(12) 0.000 0.0139(11) 0.000 Zn1 0.0266(5) 0.0173(5) 0.0194(5) 0.000 0.0112(4) 0.000 N4 0.022(3) 0.024(2) 0.021(3) -0.003(2) 0.012(2) -0.001(2) C5 0.030(3) 0.037(4) 0.022(3) 0.003(3) 0.008(3) -0.006(3) C6 0.034(4) 0.034(4) 0.029(4) -0.009(3) 0.017(3) -0.012(3) N7 0.026(3) 0.021(2) 0.026(3) 0.000(2) 0.016(2) -0.001(2) C8 0.021(3) 0.017(3) 0.025(3) 0.005(2) 0.009(2) 0.009(2) C9 0.027(3) 0.032(4) 0.029(4) 0.006(3) 0.009(3) -0.003(3) C10 0.029(3) 0.020(3) 0.033(4) 0.005(3) 0.020(3) 0.004(3) C11 0.029(3) 0.020(3) 0.026(3) 0.004(3) 0.017(3) 0.005(3) C12 0.029(3) 0.014(3) 0.024(3) 0.000(2) 0.014(3) 0.004(2) C13 0.021(3) 0.018(3) 0.030(3) 0.003(3) 0.012(3) 0.001(2) C14 0.023(3) 0.022(3) 0.016(3) 0.001(2) 0.012(2) -0.003(2) C15 0.036(3) 0.013(3) 0.015(3) 0.002(2) 0.015(3) 0.003(2) C16 0.028(3) 0.022(3) 0.023(3) 0.005(2) 0.014(3) -0.001(2) C17 0.033(6) 0.046(6) 0.054(7) 0.000 0.014(5) 0.000 O18 0.053(5) 0.053(5) 0.046(5) 0.000 0.023(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl2 Zn1 2.267(4) . ? Cl3 Zn1 2.286(4) . ? Zn1 N4 1.999(5) . ? Zn1 N4 1.999(5) 6 ? N4 C8 1.351(7) . ? N4 C5 1.396(8) . ? C5 C6 1.343(9) . ? C5 H5 0.9500 . ? C6 N7 1.386(8) . ? C6 H6 0.9500 . ? N7 C8 1.343(7) . ? N7 C10 1.466(7) . ? C8 C9 1.486(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.518(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.380(8) . ? C11 C16 1.411(8) . ? C12 C13 1.393(8) . ? C12 H12 0.9500 . ? C13 C14 1.381(8) . ? C13 H13 0.9500 . ? C14 C15 1.393(7) . ? C14 C14 1.501(10) 2_655 ? C15 C16 1.369(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O18 1.465(12) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O18 H18 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn1 N4 113.0(3) . 6 ? N4 Zn1 Cl2 110.97(14) . . ? N4 Zn1 Cl2 110.97(14) 6 . ? N4 Zn1 Cl3 103.20(15) . . ? N4 Zn1 Cl3 103.20(15) 6 . ? Cl2 Zn1 Cl3 115.14(10) . . ? C8 N4 C5 105.8(5) . . ? C8 N4 Zn1 129.8(4) . . ? C5 N4 Zn1 124.3(4) . . ? C6 C5 N4 109.2(6) . . ? C6 C5 H5 125.4 . . ? N4 C5 H5 125.4 . . ? C5 C6 N7 107.0(5) . . ? C5 C6 H6 126.5 . . ? N7 C6 H6 126.5 . . ? C8 N7 C6 107.8(5) . . ? C8 N7 C10 128.0(5) . . ? C6 N7 C10 124.2(5) . . ? N7 C8 N4 110.2(5) . . ? N7 C8 C9 124.8(5) . . ? N4 C8 C9 125.0(5) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N7 C10 C11 113.3(5) . . ? N7 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N7 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 119.6(5) . . ? C12 C11 C10 119.7(5) . . ? C16 C11 C10 120.6(5) . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 121.2(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 118.1(5) . . ? C13 C14 C14 120.3(4) . 2_655 ? C15 C14 C14 121.6(4) . 2_655 ? C16 C15 C14 122.1(5) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C11 119.0(5) . . ? C15 C16 H16 120.5 . . ? C11 C16 H16 120.5 . . ? O18 C17 H17A 109.5 . . ? O18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 O18 H18 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O18 H18 Cl3 0.84 2.41 3.186(9) 153.2 1_554 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.803 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.140 # Attachment '- ZnCl2 empty 100K.CIF' data_ZnCl2_empty _database_code_depnum_ccdc_archive 'CCDC 892654' #TrackingRef '- ZnCl2 empty 100K.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 Cl4 N8 Zn2' _chemical_formula_sum 'C44 H44 Cl4 N8 Zn2' _chemical_formula_weight 957.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.010(5) _cell_length_b 14.658(3) _cell_length_c 17.146(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.325(3) _cell_angle_gamma 90.00 _cell_volume 4426.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1381 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 22.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7351 _exptl_absorpt_correction_T_max 0.7813 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12944 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.1393 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5067 _reflns_number_gt 2502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood & Barbour, 2003) ; _computing_publication_material ; X-Seed (Atwood & Barbour, 2003; Barbour, 2001) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5067 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1793 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl3 Cl 0.32179(11) 0.50454(11) 0.67098(11) 0.0352(4) Uani 1 1 d . . . Zn1 Zn 0.25618(4) 0.50673(5) 0.52121(5) 0.0247(2) Uani 1 1 d . . . Cl2 Cl 0.13086(10) 0.49401(11) 0.46998(13) 0.0394(5) Uani 1 1 d . . . N4A N 0.2891(3) 0.3994(4) 0.4745(4) 0.0273(13) Uani 1 1 d . . . N4B N 0.2871(3) 0.6203(3) 0.4806(4) 0.0264(13) Uani 1 1 d . . . C5A C 0.2423(4) 0.3291(5) 0.4202(4) 0.0292(16) Uani 1 1 d . . . H5A H 0.1884 0.3306 0.3878 0.035 Uiso 1 1 calc R . . C5B C 0.3372(4) 0.6855(4) 0.5368(4) 0.0262(15) Uani 1 1 d . . . H5B H 0.3644 0.6811 0.5996 0.031 Uiso 1 1 calc R . . C6A C 0.2865(4) 0.2597(4) 0.4217(4) 0.0310(17) Uani 1 1 d . . . H6A H 0.2699 0.2035 0.3909 0.037 Uiso 1 1 calc R . . C6B C 0.3412(4) 0.7548(4) 0.4895(4) 0.0262(15) Uani 1 1 d . . . H6B H 0.3702 0.8089 0.5120 0.031 Uiso 1 1 calc R . . N7A N 0.3603(3) 0.2852(4) 0.4764(3) 0.0262(13) Uani 1 1 d . . . N7B N 0.2952(3) 0.7336(3) 0.4010(4) 0.0231(12) Uani 1 1 d . . . C8A C 0.3602(4) 0.3699(4) 0.5060(4) 0.0293(16) Uani 1 1 d . . . C8B C 0.2635(4) 0.6517(4) 0.3987(4) 0.0242(15) Uani 1 1 d . . . C9A C 0.4285(4) 0.4250(4) 0.5604(4) 0.0330(17) Uani 1 1 d . . . H9A1 H 0.4211 0.4590 0.6049 0.050 Uiso 1 1 calc R . . H9A2 H 0.4372 0.4679 0.5223 0.050 Uiso 1 1 calc R . . H9A3 H 0.4726 0.3847 0.5901 0.050 Uiso 1 1 calc R . . C9B C 0.2093(4) 0.6039(5) 0.3175(4) 0.0353(17) Uani 1 1 d . . . H9B1 H 0.1863 0.5529 0.3333 0.053 Uiso 1 1 calc R . . H9B2 H 0.2360 0.5807 0.2863 0.053 Uiso 1 1 calc R . . H9B3 H 0.1694 0.6464 0.2790 0.053 Uiso 1 1 calc R . . C10A C 0.4257(4) 0.2290(4) 0.4939(4) 0.0281(16) Uani 1 1 d . . . H10A H 0.4160 0.1657 0.5061 0.034 Uiso 1 1 calc R . . H10B H 0.4705 0.2521 0.5475 0.034 Uiso 1 1 calc R . . C10B C 0.2848(4) 0.7927(4) 0.3281(4) 0.0275(15) Uani 1 1 d . . . H10C H 0.2759 0.8558 0.3415 0.033 Uiso 1 1 calc R . . H10D H 0.2390 0.7729 0.2738 0.033 Uiso 1 1 calc R . . C11A C 0.4435(4) 0.2280(4) 0.4177(4) 0.0238(14) Uani 1 1 d . . . C11B C 0.3513(4) 0.7926(4) 0.3103(4) 0.0237(14) Uani 1 1 d . . . C12A C 0.4734(4) 0.1504(4) 0.3999(4) 0.0254(15) Uani 1 1 d . . . H12A H 0.4784 0.0959 0.4322 0.031 Uiso 1 1 calc R . . C12B C 0.3707(4) 0.7155(4) 0.2787(4) 0.0243(15) Uani 1 1 d . . . H12B H 0.3440 0.6602 0.2733 0.029 Uiso 1 1 calc R . . C13A C 0.4961(4) 0.1518(4) 0.3354(4) 0.0247(15) Uani 1 1 d . . . H13A H 0.5178 0.0985 0.3252 0.030 Uiso 1 1 calc R . . C13B C 0.4275(3) 0.7165(4) 0.2549(4) 0.0222(14) Uani 1 1 d . . . H13B H 0.4385 0.6624 0.2326 0.027 Uiso 1 1 calc R . . C14A C 0.4878(4) 0.2296(4) 0.2849(4) 0.0211(14) Uani 1 1 d . . . C14B C 0.4696(3) 0.7962(4) 0.2630(4) 0.0178(13) Uani 1 1 d . . . C15A C 0.4552(4) 0.3069(4) 0.3006(4) 0.0235(14) Uani 1 1 d . . . H15A H 0.4480 0.3605 0.2664 0.028 Uiso 1 1 calc R . . C15B C 0.4514(4) 0.8732(4) 0.2958(4) 0.0209(14) Uani 1 1 d . . . H15B H 0.4790 0.9279 0.3025 0.025 Uiso 1 1 calc R . . C16A C 0.4332(4) 0.3057(4) 0.3655(4) 0.0282(16) Uani 1 1 d . . . H16A H 0.4107 0.3586 0.3751 0.034 Uiso 1 1 calc R . . C16B C 0.3933(3) 0.8727(4) 0.3196(4) 0.0227(14) Uani 1 1 d . . . H16B H 0.3822 0.9266 0.3420 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl3 0.0493(11) 0.0287(9) 0.0286(9) 0.0043(8) 0.0193(9) 0.0089(8) Zn1 0.0271(4) 0.0204(4) 0.0310(4) 0.0026(3) 0.0173(4) 0.0013(3) Cl2 0.0291(9) 0.0289(9) 0.0621(13) 0.0033(9) 0.0234(9) -0.0003(8) N4A 0.034(4) 0.024(3) 0.028(3) -0.001(2) 0.019(3) -0.002(3) N4B 0.025(3) 0.025(3) 0.037(3) 0.005(3) 0.020(3) 0.005(2) C5A 0.030(4) 0.035(4) 0.027(4) 0.001(3) 0.017(3) -0.003(3) C5B 0.033(4) 0.026(3) 0.019(4) -0.002(3) 0.012(3) -0.002(3) C6A 0.047(5) 0.028(4) 0.023(4) 0.002(3) 0.021(4) -0.002(3) C6B 0.022(4) 0.032(4) 0.027(4) -0.012(3) 0.014(3) -0.009(3) N7A 0.035(4) 0.027(3) 0.021(3) 0.004(2) 0.016(3) 0.004(3) N7B 0.026(3) 0.021(3) 0.033(3) -0.003(2) 0.022(3) 0.000(2) C8A 0.041(5) 0.029(4) 0.020(4) 0.009(3) 0.016(4) 0.009(3) C8B 0.024(4) 0.023(3) 0.032(4) 0.001(3) 0.019(3) -0.001(3) C9A 0.028(4) 0.035(4) 0.033(4) 0.007(3) 0.012(4) 0.006(3) C9B 0.027(4) 0.043(4) 0.033(4) -0.006(3) 0.012(4) -0.005(3) C10A 0.031(4) 0.030(4) 0.029(4) 0.008(3) 0.020(3) 0.010(3) C10B 0.032(4) 0.024(3) 0.034(4) 0.004(3) 0.022(4) 0.006(3) C11A 0.023(4) 0.028(3) 0.021(4) -0.001(3) 0.012(3) 0.004(3) C11B 0.024(4) 0.022(3) 0.030(4) 0.005(3) 0.018(3) 0.004(3) C12A 0.027(4) 0.024(3) 0.027(4) 0.007(3) 0.014(3) 0.002(3) C12B 0.029(4) 0.014(3) 0.033(4) 0.002(3) 0.017(3) 0.000(3) C13A 0.023(4) 0.024(3) 0.026(4) -0.007(3) 0.010(3) -0.001(3) C13B 0.025(4) 0.018(3) 0.024(4) -0.007(3) 0.012(3) 0.001(3) C14A 0.020(3) 0.025(3) 0.017(3) -0.005(3) 0.007(3) -0.003(3) C14B 0.025(4) 0.018(3) 0.013(3) 0.005(2) 0.011(3) 0.003(3) C15A 0.025(4) 0.021(3) 0.022(4) 0.004(3) 0.009(3) 0.007(3) C15B 0.027(4) 0.015(3) 0.024(4) 0.000(3) 0.014(3) -0.005(3) C16A 0.035(4) 0.024(3) 0.029(4) 0.004(3) 0.018(3) 0.008(3) C16B 0.025(4) 0.022(3) 0.021(3) 0.002(3) 0.011(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl3 Zn1 2.2628(19) . ? Zn1 N4B 2.012(5) . ? Zn1 N4A 2.012(5) . ? Zn1 Cl2 2.237(2) . ? N4A C8A 1.333(8) . ? N4A C5A 1.406(8) . ? N4B C8B 1.332(8) . ? N4B C5B 1.390(8) . ? C5A C6A 1.340(9) . ? C5A H5A 0.9500 . ? C5B C6B 1.326(9) . ? C5B H5B 0.9500 . ? C6A N7A 1.374(9) . ? C6A H6A 0.9500 . ? C6B N7B 1.386(8) . ? C6B H6B 0.9500 . ? N7A C8A 1.342(8) . ? N7A C10A 1.452(8) . ? N7B C8B 1.351(7) . ? N7B C10B 1.452(8) . ? C8A C9A 1.476(9) . ? C8B C9B 1.473(9) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10A C11A 1.508(8) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C10B C11B 1.501(8) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11A C12A 1.386(8) . ? C11A C16A 1.403(8) . ? C11B C12B 1.386(8) . ? C11B C16B 1.408(8) . ? C12A C13A 1.379(8) . ? C12A H12A 0.9500 . ? C12B C13B 1.378(8) . ? C12B H12B 0.9500 . ? C13A C14A 1.394(8) . ? C13A H13A 0.9500 . ? C13B C14B 1.408(8) . ? C13B H13B 0.9500 . ? C14A C15A 1.396(8) . ? C14A C14A 1.490(12) 2_655 ? C14B C15B 1.385(8) . ? C14B C14B 1.483(11) 2_655 ? C15A C16A 1.376(8) . ? C15A H15A 0.9500 . ? C15B C16B 1.401(8) . ? C15B H15B 0.9500 . ? C16A H16A 0.9500 . ? C16B H16B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4B Zn1 N4A 107.3(2) . . ? N4B Zn1 Cl2 113.84(16) . . ? N4A Zn1 Cl2 107.22(17) . . ? N4B Zn1 Cl3 107.26(17) . . ? N4A Zn1 Cl3 108.52(16) . . ? Cl2 Zn1 Cl3 112.52(8) . . ? C8A N4A C5A 106.1(5) . . ? C8A N4A Zn1 125.5(5) . . ? C5A N4A Zn1 126.6(4) . . ? C8B N4B C5B 105.8(5) . . ? C8B N4B Zn1 129.5(5) . . ? C5B N4B Zn1 124.6(4) . . ? C6A C5A N4A 108.5(6) . . ? C6A C5A H5A 125.7 . . ? N4A C5A H5A 125.7 . . ? C6B C5B N4B 109.5(6) . . ? C6B C5B H5B 125.2 . . ? N4B C5B H5B 125.2 . . ? C5A C6A N7A 107.0(6) . . ? C5A C6A H6A 126.5 . . ? N7A C6A H6A 126.5 . . ? C5B C6B N7B 107.3(6) . . ? C5B C6B H6B 126.3 . . ? N7B C6B H6B 126.3 . . ? C8A N7A C6A 108.4(6) . . ? C8A N7A C10A 127.6(6) . . ? C6A N7A C10A 123.9(6) . . ? C8B N7B C6B 106.8(5) . . ? C8B N7B C10B 129.2(6) . . ? C6B N7B C10B 124.0(5) . . ? N4A C8A N7A 109.9(6) . . ? N4A C8A C9A 124.7(6) . . ? N7A C8A C9A 125.3(6) . . ? N4B C8B N7B 110.5(6) . . ? N4B C8B C9B 124.5(6) . . ? N7B C8B C9B 125.1(6) . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C8B C9B H9B1 109.5 . . ? C8B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C8B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? N7A C10A C11A 112.7(5) . . ? N7A C10A H10A 109.1 . . ? C11A C10A H10A 109.1 . . ? N7A C10A H10B 109.1 . . ? C11A C10A H10B 109.1 . . ? H10A C10A H10B 107.8 . . ? N7B C10B C11B 113.3(5) . . ? N7B C10B H10C 108.9 . . ? C11B C10B H10C 108.9 . . ? N7B C10B H10D 108.9 . . ? C11B C10B H10D 108.9 . . ? H10C C10B H10D 107.7 . . ? C12A C11A C16A 118.3(6) . . ? C12A C11A C10A 120.2(6) . . ? C16A C11A C10A 121.5(5) . . ? C12B C11B C16B 117.5(6) . . ? C12B C11B C10B 121.3(6) . . ? C16B C11B C10B 121.0(6) . . ? C13A C12A C11A 120.3(6) . . ? C13A C12A H12A 119.8 . . ? C11A C12A H12A 119.8 . . ? C13B C12B C11B 122.0(6) . . ? C13B C12B H12B 119.0 . . ? C11B C12B H12B 119.0 . . ? C12A C13A C14A 121.6(6) . . ? C12A C13A H13A 119.2 . . ? C14A C13A H13A 119.2 . . ? C12B C13B C14B 121.2(6) . . ? C12B C13B H13B 119.4 . . ? C14B C13B H13B 119.4 . . ? C13A C14A C15A 118.2(6) . . ? C13A C14A C14A 120.7(4) . 2_655 ? C15A C14A C14A 121.1(4) . 2_655 ? C15B C14B C13B 117.2(5) . . ? C15B C14B C14B 122.3(4) . 2_655 ? C13B C14B C14B 120.5(4) . 2_655 ? C16A C15A C14A 120.3(6) . . ? C16A C15A H15A 119.9 . . ? C14A C15A H15A 119.9 . . ? C14B C15B C16B 121.8(5) . . ? C14B C15B H15B 119.1 . . ? C16B C15B H15B 119.1 . . ? C15A C16A C11A 121.3(6) . . ? C15A C16A H16A 119.3 . . ? C11A C16A H16A 119.3 . . ? C15B C16B C11B 120.3(6) . . ? C15B C16B H16B 119.9 . . ? C11B C16B H16B 119.9 . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.050 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.140