#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200723.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_2200723 loop_ _publ_author_name 'Anzellotti, Atilio' 'Brice\~no, Alexander' _publ_section_title ; Hexakis(acetonitrile)ruthenium(II) tetrachlorozincate 2.55-hydrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m538 _journal_page_last m540 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ru (C2 H3 N)6] [Zn Cl4], 2.55H2 O1' _chemical_formula_moiety 'C12 H18 N6 Ru 2+, Zn Cl4 2-, 2.55H2 O' _chemical_formula_sum 'C12 H23.1 Cl4 N6 O2.55 Ru Zn' _chemical_formula_weight 600.50 _chemical_melting_point 156 _chemical_name_systematic ; ? ; _space_group_IT_number 148 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 6 _cell_length_a 11.7436(17) _cell_length_b 11.7436(17) _cell_length_c 30.932(8) _cell_measurement_reflns_used 20 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 36.67 _cell_measurement_theta_min 26.46 _cell_volume 3694.4(12) _computing_cell_refinement ; MSC/AFC Difractometer Control Software ; _computing_data_collection ; MSC/AFC Difractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1992) ; _computing_molecular_graphics SHELXL97 _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .0227 _diffrn_reflns_av_sigmaI/netI .0448 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1601 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.98 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_T_max .751 _exptl_absorpt_correction_T_min .650 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 1797 _exptl_crystal_size_max .32 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .14 _refine_diff_density_max 2.930 _refine_diff_density_min -.500 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 83 _refine_ls_number_reflns 1461 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all .0893 _refine_ls_R_factor_gt .0583 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1002P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1567 _reflns_number_gt 1033 _reflns_number_total 1461 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob6083.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'R -3' _[local]_cod_chemical_formula_sum_orig 'C12 H23.10 Cl4 N6 O2.55 Ru Zn' _cod_database_code 2200723 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Ru1 .3333 .6667 .57326(3) .0365(3) Uani d S 1 Ru Zn1 .6667 .3333 .60244(4) .0457(4) Uani d S 1 Zn N1 .3262(5) .5233(5) .53491(17) .0412(12) Uani d . 1 N N2 .1881(6) .5260(6) .61031(17) .0444(13) Uani d . 1 N C1 .3214(7) .4479(7) .5119(2) .0454(16) Uani d . 1 C C2 .3143(8) .3485(8) .4820(3) .066(2) Uani d . 1 C H2A .3954 .3832 .4662 .099 Uiso d R 1 H H2B .2431 .3244 .4621 .099 Uiso d R 1 H H2C .2998 .2723 .4980 .099 Uiso d R 1 H C3 .1033(7) .4437(7) .6284(2) .0495(17) Uani d . 1 C C4 -.0066(8) .3371(8) .6516(3) .075(3) Uani d . 1 C H4A -.0305 .2549 .6378 .112 Uiso d R 1 H H4B -.0803 .3512 .6513 .112 Uiso d R 1 H H4C .0190 .3352 .6810 .112 Uiso d R 1 H Cl1 .6667 .3333 .67656(11) .0739(11) Uani d S 1 Cl Cl2 .48714(19) .3411(2) .58055(6) .0616(6) Uani d . 1 Cl O1W .1600(16) .1896(16) .5761(5) .143(9) Uiso d P .57(2) O O2W .0000 .0000 .574(4) .240 Uiso d SP .29(4) O O3W .0000 .0000 .512(2) .24(3) Uiso d SP .55(4) O 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 Ru1 .0373(4) .0373(4) .0348(5) .0186(2) .000 .000 Zn1 .0467(6) .0467(6) .0437(8) .0234(3) .000 .000 N1 .037(3) .043(3) .044(3) .020(3) .002(2) .001(3) N2 .049(3) .049(3) .038(3) .027(3) -.004(3) -.004(3) C1 .045(4) .054(4) .038(3) .025(4) -.003(3) -.004(3) C2 .087(6) .065(5) .064(5) .051(5) -.012(5) -.022(4) C3 .049(4) .055(5) .041(4) .023(4) .004(3) .009(3) C4 .058(5) .069(6) .088(6) .024(4) .016(4) .030(5) Cl1 .0883(17) .0883(17) .0452(19) .0442(9) .000 .000 Cl2 .0564(12) .0786(14) .0590(12) .0406(11) -.0056(9) -.0022(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 .8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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 Ru1 N1 3_565 2_665 89.2(2) no N1 Ru1 N1 3_565 . 89.2(2) y N1 Ru1 N1 2_665 . 89.2(2) no N1 Ru1 N2 3_565 3_565 89.2(2) no N1 Ru1 N2 2_665 3_565 90.3(2) no N1 Ru1 N2 . 3_565 178.3(2) no N1 Ru1 N2 3_565 . 90.3(2) y N1 Ru1 N2 2_665 . 178.3(2) y N1 Ru1 N2 . . 89.2(2) y N2 Ru1 N2 3_565 . 91.3(2) y N1 Ru1 N2 3_565 2_665 178.3(2) no N1 Ru1 N2 2_665 2_665 89.2(2) no N1 Ru1 N2 . 2_665 90.3(2) no N2 Ru1 N2 3_565 2_665 91.3(2) no N2 Ru1 N2 . 2_665 91.3(2) no C1 N1 Ru1 . . 176.1(6) y C3 N2 Ru1 . . 175.3(6) y N1 C1 C2 . . 179.5(9) y N2 C3 C4 . . 179.8(11) y Cl2 Zn1 Cl2 2_655 3_665 111.42(6) no Cl2 Zn1 Cl2 2_655 . 111.42(6) y Cl2 Zn1 Cl2 3_665 . 111.42(6) no Cl2 Zn1 Cl1 2_655 . 107.44(6) no Cl2 Zn1 Cl1 3_665 . 107.44(6) no Cl2 Zn1 Cl1 . . 107.44(6) y 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 Ru1 N1 3_565 2.026(6) no Ru1 N1 2_665 2.026(6) no Ru1 N1 . 2.026(6) y Ru1 N2 3_565 2.033(6) no Ru1 N2 . 2.033(6) y Ru1 N2 2_665 2.033(6) no N1 C1 . 1.116(8) no N2 C3 . 1.129(9) no C1 C2 . 1.459(9) no C3 C4 . 1.461(10) no Cl2 Zn1 . 2.2590(19) y Zn1 Cl2 2_655 2.2590(19) no Zn1 Cl2 3_665 2.2590(19) no Zn1 Cl1 . 2.293(4) y