# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ai-Hua Yuan' _publ_contact_author_email zhmiao119@sina.com _publ_section_title ; Ligand-concentration-dependent self-organization of Hoffman- and PtS-type frameworks from one-pot crystallization ; loop_ _publ_author_name 'Xin Chen' 'Hu Zhou' 'Ying-Ying Chen' 'Ai-Hua Yuan' # Attachment '- C1CE05699A_ccdc_823867_823869_cif.txt' data_1 #TrackingRef '- C1CE05699A_ccdc_823867_823869_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 823867' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 N7 Ni O3 Zn, H1.20 O0.60, 2(H O0.50), 2(H0.40 O0.20)' _chemical_formula_sum 'C15 H16 N7 Ni O5 Zn' _chemical_formula_weight 498.43 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/m ' _symmetry_space_group_name_Hall '-P 2yb ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.3620(18) _cell_length_b 12.946(2) _cell_length_c 13.6280(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.312(3) _cell_angle_gamma 90.00 _cell_volume 1298.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 898 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 22.32 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8014 _exptl_absorpt_correction_T_max 0.8449 _exptl_absorpt_process_details 'SADABS; Bruker, 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'f/ and w/ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10031 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2662 _reflns_number_gt 1651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXTL _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^)+(0.05P)^2^+0.55P] 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 2662 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1 C 0.1723(6) 0.9218(4) -0.0464(4) 0.0405(12) Uani 1 1 d . . . C2 C 0.8005(6) 0.9083(4) -0.0378(4) 0.0413(12) Uani 1 1 d . . . C3 C 0.4694(6) 0.6582(4) 0.1233(3) 0.0424(12) Uani 1 1 d . . . H3 H 0.4789 0.5956 0.0903 0.051 Uiso 1 1 calc R . . C4 C 0.4483(6) 0.6586(4) 0.2253(3) 0.0431(12) Uani 1 1 d . . . H4 H 0.4364 0.5965 0.2588 0.052 Uiso 1 1 calc R . . C5 C 0.4453(9) 0.7500 0.2761(5) 0.0441(17) Uani 1 2 d S . . C6 C 0.4242(11) 0.7500 0.3850(6) 0.0497(18) Uani 1 2 d S . . C7 C 0.5407(10) 0.7500 0.5513(5) 0.0468(18) Uani 1 2 d S . . C8 C 0.5310(6) 0.6575(4) 0.5998(4) 0.0435(12) Uani 1 1 d . . . H8 H 0.5413 0.5952 0.5663 0.052 Uiso 1 1 calc R . . C9 C 0.5052(6) 0.6593(4) 0.7010(4) 0.0454(12) Uani 1 1 d . . . H9 H 0.4953 0.5973 0.7349 0.055 Uiso 1 1 calc R . . N1 N 0.6945(5) 0.8602(3) -0.0765(3) 0.0453(10) Uani 1 1 d . . . N2 N 0.2897(5) 0.8664(3) -0.0777(3) 0.0455(10) Uani 1 1 d . . . N3 N 0.4762(8) 0.7500 0.0710(5) 0.0481(15) Uani 1 2 d S . . N4 N 0.5603(8) 0.7500 0.4410(4) 0.0462(15) Uani 1 2 d S . . N5 N 0.4943(8) 0.7500 0.7511(4) 0.0434(14) Uani 1 2 d S . . Ni1 Ni 1.0000 1.0000 0.0000 0.0430(3) Uani 1 2 d S . . O1 O 0.2688(7) 0.7500 0.4226(4) 0.0490(12) Uani 1 2 d S . . O1W O 0.8999(4) 1.0919(3) -0.1144(3) 0.0487(9) Uani 1 1 d . . . H1X H 0.9756 1.0864 -0.1612 0.058 Uiso 1 1 d R . . H1Y H 0.9069 1.1540 -0.0944 0.058 Uiso 1 1 d R . . O2W O 0.1471(8) 0.2315(13) 0.8306(5) 0.046(4) Uani 0.50 1 d P . . H2X H 0.1043 0.2681 0.7843 0.056 Uiso 0.50 1 d PR . . H2Y H 0.1727 0.2700 0.8792 0.056 Uiso 0.50 1 d PR . . O3W O 0.0379(10) 0.7500 0.7238(6) 0.049(2) Uani 0.60 2 d SP . . H3X H 0.0293 0.8099 0.6987 0.058 Uiso 0.30 1 d PR . . H3Y H -0.0330 0.7088 0.6940 0.058 Uiso 0.30 1 d PR . . O4W O 0.916(2) 0.4959(14) 0.6618(12) 0.053(4) Uani 0.20 1 d P . . H4X H 0.9978 0.5410 0.6515 0.063 Uiso 0.20 1 d PR . . H4Y H 0.9105 0.4548 0.6132 0.063 Uiso 0.20 1 d PR . . Zn1 Zn 0.49976(10) 0.7500 -0.08624(7) 0.0400(2) Uani 1 2 d S . . 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 C1 0.037(2) 0.034(3) 0.049(3) -0.022(2) -0.014(2) -0.0027(19) C2 0.031(2) 0.042(3) 0.051(3) -0.028(2) 0.008(2) -0.003(2) C3 0.045(3) 0.044(3) 0.037(3) -0.013(2) -0.018(2) 0.018(2) C4 0.048(3) 0.047(3) 0.035(3) 0.013(2) 0.014(2) 0.018(2) C5 0.041(4) 0.050(4) 0.042(4) 0.000 0.021(3) 0.000 C6 0.058(4) 0.043(4) 0.048(5) 0.000 -0.007(4) 0.000 C7 0.056(4) 0.043(4) 0.041(4) 0.000 -0.017(3) 0.000 C8 0.042(3) 0.045(3) 0.044(3) 0.009(2) 0.013(2) -0.018(2) C9 0.043(3) 0.050(3) 0.043(3) -0.015(2) -0.003(2) -0.005(2) N1 0.037(2) 0.041(2) 0.057(3) -0.015(2) -0.0186(19) 0.0066(18) N2 0.039(2) 0.057(3) 0.041(2) -0.014(2) 0.0101(18) 0.002(2) N3 0.041(3) 0.055(4) 0.048(4) 0.000 -0.014(3) 0.000 N4 0.045(3) 0.054(4) 0.040(4) 0.000 0.007(3) 0.000 N5 0.043(3) 0.051(4) 0.036(3) 0.000 -0.012(3) 0.000 Ni1 0.0397(5) 0.0453(5) 0.0434(5) -0.0145(4) -0.0143(4) -0.0145(4) O1 0.056(3) 0.039(3) 0.053(3) 0.000 0.019(2) 0.000 O1W 0.0464(19) 0.052(2) 0.047(2) -0.0088(18) -0.0124(16) 0.0054(16) O2W 0.054(3) 0.040(12) 0.047(3) 0.003(4) 0.015(3) -0.001(3) O3W 0.041(4) 0.057(5) 0.047(5) 0.000 -0.014(4) 0.000 O4W 0.066(11) 0.054(10) 0.038(10) -0.005(9) -0.003(8) -0.010(9) Zn1 0.0300(4) 0.0446(5) 0.0459(5) 0.000 0.0113(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 C1 N2 1.209(6) . ? C1 Ni1 1.752(5) 1_455 ? C2 N1 1.122(6) . ? C2 Ni1 1.948(5) . ? C3 N3 1.387(6) . ? C3 C4 1.402(7) . ? C3 H3 0.9300 . ? C4 C5 1.371(6) . ? C4 H4 0.9300 . ? C5 C4 1.371(6) 4_575 ? C5 C6 1.496(11) . ? C6 N4 1.245(9) . ? C6 O1 1.265(9) . ? C7 C8 1.371(6) 4_575 ? C7 C8 1.371(6) . ? C7 N4 1.513(9) . ? C8 C9 1.396(7) . ? C8 H8 0.9300 . ? C9 N5 1.361(6) . ? C9 H9 0.9300 . ? N1 Zn1 2.024(4) . ? N2 Zn1 2.164(4) . ? N3 C3 1.387(6) 4_575 ? N3 Zn1 2.154(6) . ? N5 C9 1.361(6) 4_575 ? N5 Zn1 2.216(6) 1_556 ? Ni1 C1 1.752(5) 3_675 ? Ni1 C1 1.752(5) 1_655 ? Ni1 C2 1.948(5) 3_775 ? Ni1 O1W 2.083(3) 3_775 ? Ni1 O1W 2.083(3) . ? O1W H1X 0.8596 . ? O1W H1Y 0.8496 . ? O2W H2X 0.8447 . ? O2W H2Y 0.8466 . ? O3W H3X 0.8494 . ? O3W H3Y 0.8442 . ? O4W H4X 0.8522 . ? O4W H4Y 0.8493 . ? Zn1 N1 2.024(4) 4_575 ? Zn1 N2 2.164(4) 4_575 ? Zn1 N5 2.216(6) 1_554 ? 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 N2 C1 Ni1 178.8(5) . 1_455 ? N1 C2 Ni1 167.3(5) . . ? N3 C3 C4 120.8(5) . . ? N3 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.5(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C4 119.3(7) . 4_575 ? C4 C5 C6 120.3(3) . . ? C4 C5 C6 120.3(3) 4_575 . ? N4 C6 O1 118.3(7) . . ? N4 C6 C5 120.5(7) . . ? O1 C6 C5 121.2(7) . . ? C8 C7 C8 121.8(7) 4_575 . ? C8 C7 N4 119.1(3) 4_575 . ? C8 C7 N4 119.1(3) . . ? C7 C8 C9 118.1(5) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N5 C9 C8 121.4(5) . . ? N5 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C2 N1 Zn1 155.1(5) . . ? C1 N2 Zn1 161.8(4) . . ? C3 N3 C3 117.9(6) 4_575 . ? C3 N3 Zn1 121.1(3) 4_575 . ? C3 N3 Zn1 121.1(3) . . ? C6 N4 C7 121.0(6) . . ? C9 N5 C9 119.1(6) . 4_575 ? C9 N5 Zn1 120.1(3) . 1_556 ? C9 N5 Zn1 120.1(3) 4_575 1_556 ? C1 Ni1 C1 180 3_675 1_655 ? C1 Ni1 C2 95.74(19) 3_675 3_775 ? C1 Ni1 C2 84.26(19) 1_655 3_775 ? C1 Ni1 C2 84.26(19) 3_675 . ? C1 Ni1 C2 95.74(19) 1_655 . ? C2 Ni1 C2 180 3_775 . ? C1 Ni1 O1W 107.83(19) 3_675 3_775 ? C1 Ni1 O1W 72.17(19) 1_655 3_775 ? C2 Ni1 O1W 84.18(19) 3_775 3_775 ? C2 Ni1 O1W 95.82(19) . 3_775 ? C1 Ni1 O1W 72.17(19) 3_675 . ? C1 Ni1 O1W 107.83(19) 1_655 . ? C2 Ni1 O1W 95.82(19) 3_775 . ? C2 Ni1 O1W 84.18(19) . . ? O1W Ni1 O1W 180 3_775 . ? Ni1 O1W H1X 106.5 . . ? Ni1 O1W H1Y 106.4 . . ? H1X O1W H1Y 106.4 . . ? H2X O2W H2Y 109.0 . . ? H3X O3W H3Y 110.0 . . ? H4X O4W H4Y 108.9 . . ? N1 Zn1 N1 89.6(2) . 4_575 ? N1 Zn1 N3 90.45(17) . . ? N1 Zn1 N3 90.45(17) 4_575 . ? N1 Zn1 N2 173.12(17) . 4_575 ? N1 Zn1 N2 90.68(15) 4_575 4_575 ? N3 Zn1 N2 82.68(16) . 4_575 ? N1 Zn1 N2 90.68(15) . . ? N1 Zn1 N2 173.12(17) 4_575 . ? N3 Zn1 N2 82.68(16) . . ? N2 Zn1 N2 88.2(2) 4_575 . ? N1 Zn1 N5 93.56(17) . 1_554 ? N1 Zn1 N5 93.56(16) 4_575 1_554 ? N3 Zn1 N5 174.4(2) . 1_554 ? N2 Zn1 N5 93.29(15) 4_575 1_554 ? N2 Zn1 N5 93.29(15) . 1_554 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C5 -4.0(8) . . . . ? C3 C4 C5 C4 5.2(10) . . . 4_575 ? C3 C4 C5 C6 -179.5(6) . . . . ? C4 C5 C6 N4 92.4(6) . . . . ? C4 C5 C6 N4 -92.4(6) 4_575 . . . ? C4 C5 C6 O1 -87.6(6) . . . . ? C4 C5 C6 O1 87.6(6) 4_575 . . . ? C8 C7 C8 C9 1.9(10) 4_575 . . . ? N4 C7 C8 C9 -177.4(5) . . . . ? C7 C8 C9 N5 -1.6(8) . . . . ? Ni1 C2 N1 Zn1 166.5(13) . . . . ? C4 C3 N3 C3 2.7(9) . . . 4_575 ? C4 C3 N3 Zn1 -178.0(3) . . . . ? O1 C6 N4 C7 0.000(2) . . . . ? C5 C6 N4 C7 180 . . . . ? C8 C7 N4 C6 -89.7(6) 4_575 . . . ? C8 C7 N4 C6 89.7(6) . . . . ? C8 C9 N5 C9 1.3(9) . . . 4_575 ? C8 C9 N5 Zn1 -169.7(3) . . . 1_556 ? N1 C2 Ni1 C1 113.4(19) . . . 3_675 ? N1 C2 Ni1 C1 -66.6(19) . . . 1_655 ? N1 C2 Ni1 O1W -139.2(19) . . . 3_775 ? N1 C2 Ni1 O1W 40.8(19) . . . . ? C2 N1 Zn1 N1 -73.9(9) . . . 4_575 ? C2 N1 Zn1 N3 16.5(9) . . . . ? C2 N1 Zn1 N2 99.2(9) . . . . ? C2 N1 Zn1 N5 -167.5(9) . . . 1_554 ? C3 N3 Zn1 N1 44.9(5) 4_575 . . . ? C3 N3 Zn1 N1 -134.4(5) . . . . ? C3 N3 Zn1 N1 134.4(5) 4_575 . . 4_575 ? C3 N3 Zn1 N1 -44.9(5) . . . 4_575 ? C3 N3 Zn1 N2 -134.9(5) 4_575 . . 4_575 ? C3 N3 Zn1 N2 45.8(4) . . . 4_575 ? C3 N3 Zn1 N2 -45.8(4) 4_575 . . . ? C3 N3 Zn1 N2 134.9(5) . . . . ? C1 N2 Zn1 N1 -100.9(12) . . . . ? C1 N2 Zn1 N3 -10.5(12) . . . . ? C1 N2 Zn1 N2 72.4(12) . . . 4_575 ? C1 N2 Zn1 N5 165.5(12) . . . 1_554 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.463 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.081 # Attachment '2.CIF' data_2 #TrackingRef '- C1CE05699A_ccdc_823867_823869_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 823868' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 N4 Ni Zn' _chemical_formula_sum 'C4 N4 Ni Zn' _chemical_formula_weight 228.16 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' Ni Ni 0.3393 1.1124 '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 Tetragonal _symmetry_space_group_name_H-M P42/mmc _symmetry_space_group_name_Hall '-P 4c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x, -y, -z' '-x, y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x, y, z' 'x, -y, z' '-y, -x, z-1/2' 'y, x, z-1/2' _cell_length_a 7.4474(12) _cell_length_b 7.4474(12) _cell_length_c 13.050(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 723.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2337 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 220 _exptl_absorpt_coefficient_mu 2.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 0.592 _exptl_absorpt_process_details 'SADABS; Bruker, 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 Smart Apex CCD' _diffrn_measurement_method 'f/ and w/ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5329 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 436 _reflns_number_gt 391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXTL _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^)+(0.0332P)^2^+0.0982P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 436 _refine_ls_number_parameters 18 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Zn1 Zn 0.0000 0.0000 0.2500 0.0442(2) Uani 1 8 d S . . Ni1 Ni 0.5000 0.0000 0.0000 0.0525(2) Uani 1 8 d S . . N1 N 0.2112(3) 0.0000 0.16015(14) 0.0621(5) Uani 1 2 d S . . C1 C 0.3228(3) 0.0000 0.10002(16) 0.0566(6) Uani 1 2 d S . . 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 Zn1 0.0545(3) 0.0545(3) 0.0238(3) 0.000 0.000 0.000 Ni1 0.0443(3) 0.0820(5) 0.0311(3) 0.000 0.000 0.000 N1 0.0562(12) 0.0901(15) 0.0400(9) 0.000 0.0059(10) 0.000 C1 0.0512(13) 0.0811(16) 0.0374(11) 0.000 -0.0040(10) 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 Zn1 N1 1.9618(19) 12_556 ? Zn1 N1 1.9618(19) 3 ? Zn1 N1 1.9618(19) 10_556 ? Zn1 N1 1.9618(19) . ? Ni1 C1 1.856(2) 11 ? Ni1 C1 1.856(2) 3_655 ? Ni1 C1 1.856(2) 9_655 ? Ni1 C1 1.856(2) . ? N1 C1 1.143(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 110.93(6) 12_556 3 ? N1 Zn1 N1 106.58(11) 12_556 10_556 ? N1 Zn1 N1 110.93(6) 3 10_556 ? N1 Zn1 N1 110.93(6) 12_556 . ? N1 Zn1 N1 106.58(11) 3 . ? N1 Zn1 N1 110.93(6) 10_556 . ? C1 Ni1 C1 180 11 3_655 ? C1 Ni1 C1 90.62(13) 11 9_655 ? C1 Ni1 C1 89.38(13) 3_655 9_655 ? C1 Ni1 C1 89.38(13) 11 . ? C1 Ni1 C1 90.62(13) 3_655 . ? C1 Ni1 C1 180 9_655 . ? C1 N1 Zn1 173.36(19) . . ? N1 C1 Ni1 178.7(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.414 _refine_diff_density_min -0.128 _refine_diff_density_rms 0.055 # Attachment '3.CIF' data_3 #TrackingRef '- C1CE05699A_ccdc_823867_823869_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 823869' #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 N4 Ni Zn, 2(C2 H3 N)' _chemical_formula_sum 'C8 H6 N6 Ni Zn' _chemical_formula_weight 310.27 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' Ni Ni 0.3393 1.1124 '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 12.6429(19) _cell_length_b 7.9421(12) _cell_length_c 12.4142(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.785(2) _cell_angle_gamma 90.00 _cell_volume 1228.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1754 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 3.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.483 _exptl_absorpt_process_details 'SADABS; Bruker, 2004' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 Smart Apex CCD' _diffrn_measurement_method 'f/ and w/ scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4634 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1208 _reflns_number_gt 1021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material SHELXTL _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^)+(0.0259P)^2^+1.2395P] 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 1208 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0563 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Zn1 Zn 0.0000 0.12315(5) 0.2500 0.01428(12) Uani 1 2 d S . . Ni1 Ni -0.2500 -0.2500 0.0000 0.01570(13) Uani 1 2 d S . . N1 N -0.09686(16) -0.0296(3) 0.15003(17) 0.0214(5) Uani 1 1 d . . . N2 N 0.09895(17) 0.2221(3) 0.16178(17) 0.0186(5) Uani 1 1 d . . . N3 N -0.3659(2) 0.0838(4) -0.0802(3) 0.0562(8) Uani 1 1 d . . . C1 C -0.15540(19) -0.1150(3) 0.09398(19) 0.0177(5) Uani 1 1 d . . . C2 C -0.3421(2) -0.2656(3) 0.1021(2) 0.0166(5) Uani 1 1 d . . . C3 C -0.3746(3) 0.1916(5) 0.1151(3) 0.0619(11) Uani 1 1 d . . . H3A H -0.4468 0.2237 0.1199 0.093 Uiso 1 1 calc R . . H3B H -0.3279 0.2868 0.1320 0.093 Uiso 1 1 calc R . . H3C H -0.3520 0.1027 0.1663 0.093 Uiso 1 1 calc R . . C4 C -0.3699(3) 0.1332(4) 0.0047(3) 0.0433(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0115(2) 0.0194(2) 0.0131(2) 0.000 0.00513(15) 0.000 Ni1 0.0127(2) 0.0225(3) 0.0132(2) -0.00239(17) 0.00584(18) -0.00482(18) N1 0.0185(11) 0.0253(13) 0.0216(11) -0.0030(9) 0.0070(9) -0.0022(10) N2 0.0171(11) 0.0215(11) 0.0182(11) 0.0005(9) 0.0060(9) -0.0013(9) N3 0.0469(19) 0.058(2) 0.060(2) 0.0112(17) -0.0004(16) 0.0030(16) C1 0.0148(12) 0.0234(14) 0.0165(12) 0.0018(11) 0.0076(10) 0.0008(11) C2 0.0142(13) 0.0179(13) 0.0168(12) -0.0004(9) 0.0003(11) -0.0025(10) C3 0.049(2) 0.054(2) 0.086(3) -0.019(2) 0.019(2) 0.010(2) C4 0.0249(17) 0.0342(19) 0.069(3) 0.0075(18) 0.0016(17) 0.0091(14) _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 Zn1 N2 1.962(2) 2 ? Zn1 N2 1.962(2) . ? Zn1 N1 1.999(2) . ? Zn1 N1 1.999(2) 2 ? Ni1 C1 1.862(3) . ? Ni1 C1 1.862(3) 7_445 ? Ni1 C2 1.865(3) . ? Ni1 C2 1.865(3) 7_445 ? N1 C1 1.148(3) . ? N2 C2 1.141(3) 3 ? N3 C4 1.134(4) . ? C2 N2 1.141(3) 3_445 ? C3 C4 1.458(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? 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 N2 Zn1 N2 132.74(13) 2 . ? N2 Zn1 N1 102.03(8) 2 . ? N2 Zn1 N1 106.15(8) . . ? N2 Zn1 N1 106.15(8) 2 2 ? N2 Zn1 N1 102.03(8) . 2 ? N1 Zn1 N1 105.26(12) . 2 ? C1 Ni1 C1 180 . 7_445 ? C1 Ni1 C2 91.22(10) . . ? C1 Ni1 C2 88.78(10) 7_445 . ? C1 Ni1 C2 88.78(10) . 7_445 ? C1 Ni1 C2 91.22(10) 7_445 7_445 ? C2 Ni1 C2 180 . 7_445 ? C1 N1 Zn1 177.7(2) . . ? C2 N2 Zn1 161.0(2) 3 . ? N1 C1 Ni1 178.5(2) . . ? N2 C2 Ni1 177.6(2) 3_445 . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C3 178.3(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.324 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.073