############################################################# # ***Indian Association for the Cultivation of Science*** # # this structure was solved by Raju Mondal on 2/3/2008 ############################################################# data_08rmd023_0m _publ_contact_author ; Dr. Raju Mondal ; _publ_author_address ; Dr. Raju Mondal Department of Inorganic Chemistry Indian Association for the Cultivation of Science Raja S. C. Mullick Road Jadavpur Kolkata 700 078 India ; _publ_requested_journal 'Crystal Growth & Design' _publ_contact_author_email ; icrm@iacs.res.in ; _publ_author_name ; 'Raju Mondal' 'Dipali Sadhukhan' 'Tanmoy Chatterjee' 'Manas Kumar Bhunia' ; _journal_name_full 'Crystal Growth & Design' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 N10 O6 Zn' _chemical_formula_weight 597.95 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/acd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 13.4139(7) _cell_length_b 13.4139(7) _cell_length_c 31.309(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5633.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8870 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.87 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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-2 CCD area detector' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35322 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0113 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.06 _reflns_number_total 1407 _reflns_number_gt 1197 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0420P)^2^+8.9639P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1407 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.5000 0.2500 0.1250 0.01507(15) Uani 1 4 d S . . N2 N 0.38699(11) 0.27937(12) 0.08600(4) 0.0192(3) Uani 1 1 d . . . C6 C 0.37978(14) 0.35178(14) 0.05650(6) 0.0198(4) Uani 1 1 d . . . N3 N 0.29912(13) 0.23034(14) 0.08482(6) 0.0286(4) Uani 1 1 d . . . C5 C 0.46376(17) 0.42210(18) 0.04867(7) 0.0317(5) Uani 1 1 d . . . C4 C 0.28730(14) 0.34820(14) 0.03653(6) 0.0241(4) Uani 1 1 d . . . C3 C 0.2500 0.4112(2) 0.0000 0.0285(6) Uani 1 2 d S . . C2 C 0.23749(16) 0.26975(17) 0.05576(7) 0.0339(5) Uani 1 1 d . . . C1 C 0.1333(3) 0.2326(3) 0.05010(14) 0.0718(12) Uani 1 1 d . . . N1 N 0.75976(15) 0.00976(15) 0.1250 0.0323(6) Uani 1 2 d S . . O2 O 0.74454(14) 0.08666(12) 0.14529(5) 0.0486(5) Uani 1 1 d . . . O1 O 0.69446(16) -0.05554(16) 0.1250 0.0825(12) Uani 1 2 d S . . H3 H 0.3046(17) 0.4568(18) -0.0101(7) 0.035(7) Uiso 1 1 d . . . H333 H 0.291(2) 0.177(2) 0.0980(9) 0.047(8) Uiso 1 1 d . . . H5C H 0.440(3) 0.488(3) 0.0526(12) 0.093(12) Uiso 1 1 d . . . H5B H 0.517(2) 0.414(2) 0.0680(10) 0.061(9) Uiso 1 1 d . . . H5A H 0.488(3) 0.419(3) 0.0182(12) 0.099(13) Uiso 1 1 d . . . H1C H 0.118(3) 0.182(3) 0.0696(12) 0.081(11) Uiso 1 1 d . . . H1B H 0.143(3) 0.193(3) 0.0227(13) 0.094(13) Uiso 1 1 d . . . H1A H 0.086(4) 0.277(4) 0.0434(15) 0.137(19) Uiso 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 0.01703(18) 0.01703(18) 0.0112(2) 0.000 0.000 0.000 N2 0.0181(8) 0.0218(8) 0.0178(7) 0.0021(6) -0.0025(6) -0.0036(6) C6 0.0225(9) 0.0215(9) 0.0154(8) -0.0003(7) -0.0036(7) -0.0011(7) N3 0.0244(9) 0.0298(10) 0.0317(9) 0.0109(8) -0.0078(7) -0.0104(7) C5 0.0304(11) 0.0333(12) 0.0314(11) 0.0130(9) -0.0113(9) -0.0116(9) C4 0.0253(10) 0.0245(10) 0.0226(9) -0.0004(7) -0.0075(8) -0.0015(8) C3 0.0353(16) 0.0233(14) 0.0267(14) 0.000 -0.0159(12) 0.000 C2 0.0256(11) 0.0397(12) 0.0364(11) 0.0084(9) -0.0125(9) -0.0095(9) C1 0.0393(17) 0.090(3) 0.087(3) 0.047(2) -0.0339(17) -0.0367(17) N1 0.0365(10) 0.0365(10) 0.0237(12) -0.0002(7) 0.0002(7) 0.0125(13) O2 0.0693(12) 0.0352(9) 0.0414(9) -0.0082(7) 0.0066(9) 0.0259(9) O1 0.0986(18) 0.0986(18) 0.0504(17) -0.0281(13) 0.0281(13) -0.065(2) _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 1.9860(15) 20_656 ? Zn1 N2 1.9860(15) . ? Zn1 N2 1.9860(15) 27_565 ? Zn1 N2 1.9860(15) 10_554 ? N2 C6 1.344(2) . ? N2 N3 1.350(2) . ? C6 C4 1.390(3) . ? C6 C5 1.490(3) . ? N3 C2 1.338(3) . ? N3 H333 0.83(3) . ? C5 H5C 0.95(4) . ? C5 H5B 0.95(3) . ? C5 H5A 1.01(4) . ? C4 C2 1.384(3) . ? C4 C3 1.507(2) . ? C3 C4 1.507(2) 5 ? C3 H3 1.01(2) . ? C2 C1 1.494(3) . ? C1 H1C 0.93(4) . ? C1 H1B 1.02(4) . ? C1 H1A 0.90(5) . ? N1 O2 1.229(2) . ? N1 O2 1.229(2) 15_534 ? N1 O1 1.239(4) . ? 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 112.21(4) 20_656 . ? N2 Zn1 N2 104.11(9) 20_656 27_565 ? N2 Zn1 N2 112.21(4) . 27_565 ? N2 Zn1 N2 112.21(4) 20_656 10_554 ? N2 Zn1 N2 104.11(9) . 10_554 ? N2 Zn1 N2 112.21(4) 27_565 10_554 ? C6 N2 N3 105.69(15) . . ? C6 N2 Zn1 128.38(12) . . ? N3 N2 Zn1 125.91(12) . . ? N2 C6 C4 110.39(16) . . ? N2 C6 C5 121.09(17) . . ? C4 C6 C5 128.52(17) . . ? C2 N3 N2 111.44(17) . . ? C2 N3 H333 126.4(19) . . ? N2 N3 H333 121.4(19) . . ? C6 C5 H5C 109(2) . . ? C6 C5 H5B 113.5(19) . . ? H5C C5 H5B 106(3) . . ? C6 C5 H5A 112(2) . . ? H5C C5 H5A 106(3) . . ? H5B C5 H5A 111(3) . . ? C2 C4 C6 105.16(17) . . ? C2 C4 C3 126.57(17) . . ? C6 C4 C3 128.18(17) . . ? C4 C3 C4 111.8(2) 5 . ? C4 C3 H3 110.1(13) 5 . ? C4 C3 H3 109.8(14) . . ? N3 C2 C4 107.32(18) . . ? N3 C2 C1 121.8(2) . . ? C4 C2 C1 130.8(2) . . ? C2 C1 H1C 112(2) . . ? C2 C1 H1B 99(2) . . ? H1C C1 H1B 102(3) . . ? C2 C1 H1A 118(3) . . ? H1C C1 H1A 119(4) . . ? H1B C1 H1A 104(3) . . ? O2 N1 O2 123.1(3) . 15_534 ? O2 N1 O1 118.44(15) . . ? O2 N1 O1 118.44(15) 15_534 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.418 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.053