# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1252 data_global #======================================================= #SUBMISSION DETAILS _publ_contact_author ; Prof.N.Ray Chaudhuri, Department of Inorganic Chememistry Indian Association for the Cultivation of Science Jadavpur Calcutta 700 032 INDIA ; _publ_contact_author_phone '91 33 4733073' _publ_contact_author_fax '91 33 4732805' _publ_contact_author_email icnrc@iacs.ernet.in _publ_requested_journal 'test' _publ_contact_letter ; ; #========================================================= data_n6cub _audit_creation_method 'SHELXL' _chemical_formula_structural '[Cd3{NH2-(CH2)2-NH-(CH2)2-NH2}2\m-(NCS)6]n nH2O' _chemical_formula_analytical 'C14 H28 Cd3 N12 O S6' _chemical_formula_sum 'C14 H28 Cd3 N12 O S6' _chemical_formula_weight 910.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P A -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' ' -x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' ' x+1/2, y, -z+1/2' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-z, -x, -y' '-z+1/2, x+1/2, y' 'z+1/2, x, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z, -x' 'y, -z+1/2, x+1/2' '-y+1/2, z+1/2, x' 'y+1/2, z, -x+1/2' _cell_length_a 14.871(4) _cell_length_b 14.871(4) _cell_length_c 14.871(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3288.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 7.00 _cell_measurement_theta_max 13.03 _exptl_crystal_description Diamond-shaped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 1.842 _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'floatation in benzene-carbontetrachloride mixture' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.333 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet R3m/V diffractometer' _diffrn_measurement_method \w-2\q _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_decay_% none _diffrn_reflns_number 2260 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 22.50 _reflns_number_total 725 _reflns_number_observed 608 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SHELXTL-PLUS90 (Sheldrick,1990)' _computing_cell_refinement 'SHELXTL-PLUS90 (Sheldrick,1990)' _computing_data_reduction 'SHELXTL-PLUS90 (Sheldrick,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (L.Zsolnai, 1994)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+5.0570P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy-atom _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 725 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all 0.0923 _refine_ls_wR_factor_obs 0.0874 _refine_ls_hydrogen_treatment undef _refine_ls_goodness_of_fit_all 1.132 _refine_ls_goodness_of_fit_obs 1.182 _refine_ls_restrained_S_all 1.132 _refine_ls_restrained_S_obs 1.182 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.18953(3) 0.18953(3) 0.18953(3) 0.0630(4) Uani 0.333 P S . N1 N 0.0883(4) 0.0879(4) 0.2451(4) 0.076(2) Uani 1 d . . C1 C 0.0394(5) 0.0383(5) 0.2771(4) 0.054(2) Uani 1 d . . N2 N 0.2882(5) 0.1213(7) 0.3028(5) 0.068(2) Uani 0.667 d P . N3 N 0.2099(11) 0.2894(13) 0.3071(12) 0.064(4) Uani 0.333 d P . C2 C 0.3411(11) 0.1906(11) 0.3447(13) 0.113(6) Uani 0.667 d P . C3 C 0.2637(9) 0.2508(9) 0.3789(7) 0.084(4) Uani 0.667 d P . Cd2 Cd 0.5000 0.5000 0.5000 0.0482(4) Uani 0.167 P S . S S 0.32347(11) 0.46917(13) 0.53356(13) 0.0675(6) Uani 1 P . . OW O 0.0000 0.0000 0.0000 0.403(37) Uani 0.167 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 Cd1 0.0630(4) 0.0630(4) 0.0630(4) -0.0105(2) -0.0105(2) -0.0105(2) N1 0.089(4) 0.078(4) 0.061(4) 0.011(3) 0.015(3) -0.005(4) C1 0.061(4) 0.055(4) 0.046(4) 0.000(3) -0.003(3) 0.014(3) N2 0.062(5) 0.085(7) 0.058(5) 0.000(5) -0.008(4) 0.002(5) N3 0.056(12) 0.066(12) 0.069(12) -0.012(10) 0.006(9) 0.007(9) C2 0.121(13) 0.097(11) 0.122(13) -0.038(9) -0.060(10) 0.037(9) C3 0.093(9) 0.117(10) 0.042(6) -0.002(6) -0.010(6) -0.016(8) Cd2 0.0482(4) 0.0482(4) 0.0482(4) -0.0008(3) -0.0008(3) -0.0008(3) S 0.0519(10) 0.0768(12) 0.0740(12) 0.0195(9) -0.0024(9) -0.0062(9) OW 0.403(37) 0.403(37) 0.403(37) -0.143(22) -0.143(22) -0.143(22) 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 Cd1 N1 2.287(6) . yes Cd1 N1 2.287(6) 9 no Cd1 N1 2.287(6) 5 no Cd1 N3 2.31(2) . yes Cd1 N3 2.31(2) 9 no Cd1 N3 2.31(2) 5 no Cd1 N2 2.453(8) . yes Cd1 N2 2.453(8) 9 no Cd1 N2 2.453(8) 5 no N1 C1 1.140(8) . yes C1 S 1.646(8) 24_565 yes N2 N3 1.36(2) 5 no N2 C2 1.44(2) . no N3 N2 1.36(2) 9 no N3 C3 1.45(2) . no C2 C3 1.54(2) . no C3 N3 1.60(2) 5 no Cd2 S 2.711(2) 21_666 no Cd2 S 2.711(2) 17_666 no Cd2 S 2.711(2) 13_666 no Cd2 S 2.711(2) . yes Cd2 S 2.711(2) 5 yes Cd2 S 2.711(2) 9 yes S C1 1.646(8) 19_566 yes 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 Cd1 N1 92.4(2) . 9 yes N1 Cd1 N1 92.4(2) . 5 no N1 Cd1 N1 92.4(2) 9 5 no N1 Cd1 N3 103.7(5) . . yes N1 Cd1 N3 110.6(5) 9 . no N1 Cd1 N3 103.7(5) 9 9 no N1 Cd1 N3 110.6(5) 5 9 no N1 Cd1 N3 110.6(5) . 5 no N1 Cd1 N3 103.7(5) 5 5 no N1 Cd1 N2 82.7(3) . . yes N1 Cd1 N2 175.1(3) 9 . no N1 Cd1 N2 88.0(3) 5 . no N3 Cd1 N2 70.6(5) . . yes N3 Cd1 N2 80.7(5) 9 . no N1 Cd1 N2 88.0(3) . 9 no N1 Cd1 N2 82.7(3) 9 9 no N1 Cd1 N2 175.1(3) 5 9 no N3 Cd1 N2 70.6(5) 9 9 no N3 Cd1 N2 80.7(5) 5 9 no N2 Cd1 N2 96.9(3) . 9 no N1 Cd1 N2 175.1(3) . 5 no N1 Cd1 N2 88.0(3) 9 5 no N1 Cd1 N2 82.7(3) 5 5 no N3 Cd1 N2 80.7(5) . 5 no N3 Cd1 N2 70.6(5) 5 5 no N2 Cd1 N2 96.9(3) . 5 no N2 Cd1 N2 96.9(3) 9 5 no C1 N1 Cd1 176.6(6) . . yes N1 C1 S 179.8(5) . 24_565 yes C2 N2 Cd1 109.1(9) . . no C3 N3 C3 114.6(15) . 9 no C3 N3 Cd1 112.0(11) . . no C3 N3 Cd1 106.2(10) 9 . no N2 C2 C3 98.7(11) . . no N2 C2 C3 105.1(12) . 5 no N3 C3 C2 113.4(14) . . no N3 C3 C2 105.6(11) 5 9 no S Cd2 S 92.62(6) 21_666 17_666 yes S Cd2 S 92.62(6) 21_666 13_666 no S Cd2 S 92.62(6) 17_666 13_666 no S Cd2 S 87.38(6) 21_666 . yes S Cd2 S 87.39(6) 17_666 . no S Cd2 S 180.0 13_666 . no S Cd2 S 87.39(6) 21_666 5 no S Cd2 S 180.0 17_666 5 yes S Cd2 S 87.38(6) 13_666 5 no S Cd2 S 92.61(6) . 5 no S Cd2 S 180.0 21_666 9 no S Cd2 S 87.39(6) 17_666 9 no S Cd2 S 87.39(6) 13_666 9 no S Cd2 S 92.61(6) . 9 no S Cd2 S 92.61(6) 5 9 no C1 S Cd2 100.3(2) 19_566 . no _refine_diff_density_max 0.516 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.089 #=======================================================================