#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007088.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2007088 loop_ _publ_author_name 'Blake, A. J.' 'Li, W.-S.' 'Lippolis, V.' 'Schr\"oder, M.' _publ_section_title ; Bis(acetonitrile-N)(1,4,8,12-tetraazacyclopentadecane)nickel(II) Bis(triiodide) and (1,4,8,12-Tetraazacyclopentadecane)palladium(II) Bis(triiodide) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 299 _journal_page_last 302 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Pd (C11 H26 N4)] (I3)2' _chemical_formula_moiety 'C11 H26 N4 Pd 2+, 2I3 -' _chemical_formula_sum 'C11 H26 I6 N4 Pd' _chemical_formula_weight 1082.2 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL _cell_angle_alpha 99.03(9) _cell_angle_beta 101.14(9) _cell_angle_gamma 107.43(10) _cell_formula_units_Z 1 _cell_length_a 7.787(7) _cell_length_b 9.173(9) _cell_length_c 9.382(6) _cell_measurement_reflns_used 28 _cell_measurement_temperature 150 _cell_measurement_theta_max 16.5 _cell_measurement_theta_min 13.0 _cell_volume 610.6(11) _computing_cell_refinement STADI4 _computing_data_collection 'STADI4 (Stoe & Cie, 1996a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1995)' _computing_publication_material SHELXL96 _computing_structure_refinement 'SHELXL96 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 150 _diffrn_measurement_device ; Stoe Stadi-4 four-circle diffractometer with Oxford Cryosystems open-flow cryostat (Cosier & Glazer, 1986) ; _diffrn_measurement_method \w/\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2146 _diffrn_reflns_theta_max 25.09 _diffrn_reflns_theta_min 2.84 _diffrn_standards_decay_% 4.0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 8.346 _exptl_absorpt_correction_T_max 0.392 _exptl_absorpt_correction_T_min 0.204 _exptl_absorpt_correction_type '\y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.943 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description lath _exptl_crystal_F_000 484 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _refine_diff_density_max '1.51 (0.83\%A from I1)' _refine_diff_density_min '-1.84 (0.84\%A from I1)' _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.154 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_hydrogen_treatment 'H atoms placed using riding model' _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 2146 _refine_ls_number_restraints 11 _refine_ls_restrained_S_all 1.154 _refine_ls_restrained_S_obs 1.143 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_obs 0.0503 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.032P)^2^+11.04P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1133 _refine_ls_wR_factor_obs 0.1044 _reflns_number_observed 1863 _reflns_number_total 2146 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ha1203.cif _[local]_cod_data_source_block 2 _cod_original_cell_volume 610.6(9) _cod_database_code 2007088 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd 0.0372(7) 0.0230(6) 0.0242(6) 0.0048(5) 0.0019(5) 0.0079(5) N1 0.069(8) 0.037(6) 0.038(6) 0.012(5) 0.018(5) 0.009(5) C2 0.097(13) 0.032(7) 0.068(10) 0.008(8) -0.016(9) 0.005(7) C3 0.068(10) 0.072(11) 0.057(9) -0.007(9) -0.006(8) 0.029(8) C4 0.041(7) 0.063(9) 0.054(8) 0.007(6) 0.014(6) 0.040(7) N5 0.064(7) 0.061(7) 0.042(6) 0.021(6) 0.020(6) 0.027(5) I1 0.0656(7) 0.1028(9) 0.0647(6) 0.0569(6) 0.0352(5) 0.0550(6) I2 0.0447(5) 0.0321(4) 0.0333(4) 0.0178(3) 0.0048(3) 0.0074(3) I3 0.0867(7) 0.0459(5) 0.0443(5) 0.0257(5) 0.0127(5) 0.0201(4) loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Pd 0.0000 0.0000 0.5000 0.0300(3) Uani d S 1 . Pd N1 0.1503(16) 0.2170(12) 0.6396(11) 0.049(3) Uani d D 1 . N C2 0.171(2) 0.3538(15) 0.5720(17) 0.075(5) Uani d D 1 . C H2A 0.2440 0.4506 0.6498 0.090 Uiso calc R 1 . H H2B 0.0458 0.3598 0.5335 0.090 Uiso calc R 1 . H C3 0.264(2) 0.3463(18) 0.4474(15) 0.074(5) Uani d D 1 . C H3A 0.3837 0.3309 0.4847 0.089 Uiso calc R 1 . H H3B 0.2926 0.4486 0.4189 0.089 Uiso calc R 1 . H C4 0.1529(18) 0.2180(14) 0.3092(14) 0.052(4) Uani d D 1 . C H4A 0.0271 0.2246 0.2772 0.062 Uiso calc R 1 . H H4B 0.2148 0.2337 0.2273 0.062 Uiso calc R 1 . H N5 0.1363(16) 0.0637(13) 0.3371(11) 0.053(3) Uani d D 1 . N C6 0.138(4) -0.041(3) 0.205(3) 0.067(8) Uiso d PD 0.50 1 C H6A 0.2140 -0.1071 0.2315 0.081 Uiso calc PR 0.50 1 H H6B 0.1902 0.0191 0.1347 0.081 Uiso calc PR 0.50 1 H C7 -0.063(3) -0.141(3) 0.136(3) 0.058(7) Uiso d PD 0.50 1 C H7A -0.0778 -0.1868 0.0292 0.069 Uiso calc PR 0.50 1 H H7B -0.1402 -0.0729 0.1395 0.069 Uiso calc PR 0.50 1 H C8 -0.134(6) -0.273(3) 0.211(3) 0.072(10) Uiso d PD 0.50 1 C H8A -0.2580 -0.3440 0.1494 0.086 Uiso calc PR 0.50 1 H H8B -0.0490 -0.3339 0.2177 0.086 Uiso calc PR 0.50 1 H C6A 0.013(4) -0.060(2) 0.200(2) 0.054(7) Uiso d PD 0.50 2 C H6AA 0.0831 -0.0649 0.1230 0.065 Uiso calc PR 0.50 2 H H6AB -0.0960 -0.0312 0.1598 0.065 Uiso calc PR 0.50 2 H C7A -0.052(5) -0.222(3) 0.239(3) 0.067(9) Uiso d PD 0.50 2 C H7AB -0.1375 -0.3006 0.1487 0.081 Uiso calc PR 0.50 2 H H7AC 0.0564 -0.2547 0.2706 0.081 Uiso calc PR 0.50 2 H I1 0.37944(14) 0.88612(14) 0.64546(11) 0.0642(4) Uani d . 1 . I I2 0.36383(11) 0.74962(8) 0.90959(8) 0.0364(2) Uani d . 1 . I I3 0.33942(15) 0.60015(11) 1.15543(10) 0.0577(3) Uani d . 1 . I 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Pd N1 2_556 . 180.0000(10) ? N1 Pd N5 2_556 . 90.0(4) ? N1 Pd N5 . . 90.0(4) yes N1 Pd N5 2_556 2_556 90.0(4) ? N1 Pd N5 . 2_556 90.0(4) ? N5 Pd N5 . 2_556 180.000(2) ? C8 N1 C2 2_556 . 104.2(14) ? C2 N1 C7A . 2_556 112.8(14) ? C8 N1 Pd 2_556 . 126.2(14) ? C2 N1 Pd . . 116.7(8) ? C7A N1 Pd 2_556 . 103.2(14) ? N1 C2 C3 . . 112.6(13) ? C2 C3 C4 . . 115.2(12) ? N5 C4 C3 . . 111.2(11) ? C4 N5 C6 . . 110.4(16) ? C4 N5 C6A . . 109.2(13) ? C4 N5 Pd . . 116.4(8) ? C6 N5 Pd . . 126.5(14) ? C6A N5 Pd . . 101.7(12) ? N5 C6 C7 . . 105(2) ? C6 C7 C8 . . 114(3) ? N1 C8 C7 2_556 . 113(2) ? N5 C6A C7A . . 111(2) ? N1 C7A C6A 2_556 . 111(2) ? I1 I2 I3 . . 176.85(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd N1 2_556 2.060(11) ? Pd N1 . 2.060(11) yes Pd N5 . 2.084(10) yes Pd N5 2_556 2.084(10) ? N1 C8 2_556 1.454(18) ? N1 C2 . 1.473(13) ? N1 C7A 2_556 1.492(18) ? C2 C3 . 1.494(16) ? C3 C4 . 1.514(15) ? C4 N5 . 1.452(13) ? N5 C6 . 1.453(18) ? N5 C6A . 1.504(17) ? C6 C7 . 1.509(19) ? C7 C8 . 1.515(19) ? C8 N1 2_556 1.454(18) ? C6A C7A . 1.546(19) ? C7A N1 2_556 1.492(18) ? I1 I2 . 2.953(3) yes I2 I3 . 2.871(3) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion C8 N1 C2 C3 2_556 . 157(2) C7A N1 C2 C3 2_556 . -178.4(19) N1 C2 C3 C4 . . 67.9(18) C2 C3 C4 N5 . . -69.1(17) C3 C4 N5 C6 . . -145.2(15) C3 C4 N5 C6A . . 175.9(16) C4 N5 C6 C7 . . -101(2) C6A N5 C6 C7 . . -6(2) N5 C6 C7 C8 . . -79(3) C6 C7 C8 N1 . 2_556 69(4) C4 N5 C6A C7A . . -164.1(18) C6 N5 C6A C7A . . 97(3) N5 C6A C7A N1 . 2_556 57(3)