#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003460.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003460 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 817 _journal_page_last 820 _publ_section_title ; cis,trans-Dibromobis(4-methylpyridine-N)(2,2'-bipyridine -N,N')tungsten(II) ; _chemical_formula_moiety '(C6 H7 N)2, (C10 H8 N2), W 2+, (BR 1-)2' _chemical_formula_sum 'C22 H22 Br2 N4 W' _chemical_formula_weight 686.11 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5690(1) _cell_length_b 17.651(2) _cell_length_c 13.485(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.26(2) _cell_angle_gamma 90.00 _cell_volume 2271.4(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.006 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 12 _exptl_absorpt_coefficient_mu 8.620 _cell_measurement_temperature 293(1) _exptl_crystal_description plate _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _exptl_crystal_colour 'dark red' _chemical_compound_source 'see text' _diffrn_measurement_device 'Enraf Nonius CAD-4 diffractometer' _diffrn_measurement_method 'variable rate \q/2\q scans' _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.100 _exptl_absorpt_correction_T_max 0.596 _diffrn_reflns_number 9921 _reflns_number_total 4973 _reflns_number_observed 3071 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_theta_max 27.11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count 'after 600 reflexions' _diffrn_standards_interval_time 330 _diffrn_standards_decay_% 5.44 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0447 _refine_ls_wR_factor_obs 0.0893 _refine_ls_wR_factor_all 0.1065 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_goodness_of_fit_all 0.988 _refine_ls_number_reflns 4973 _refine_ls_number_parameters 266 _refine_ls_hydrogen_treatment refU _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(Fo^2^) + (0.0528P)^2^ + 0.0000P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.257 _refine_diff_density_max 2.189 _refine_diff_density_min -1.584 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'W' 'W' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.8490 6.87 'Br' 'Br' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.2901 2. _computing_structure_solution ; NRCVAX (Gabe, Le Page, Charland, Lee & White, 1989) and GX (Mallinson & Muir, 1985) ; _computing_molecular_graphics ; ORTEPII (Johnson, 1971) and PLUTON (Spek, 1991) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv W 1 0.24514(3) 0.27437(2) 0.09138(2) 0.03370(11) Br1 1 0.43385(9) 0.18450(7) 0.17461(6) 0.0541(3) Br2 1 0.43587(8) 0.36401(7) 0.03220(6) 0.0553(3) N11 1 0.2485(7) 0.2063(4) -0.0426(5) 0.039(2) C12 1 0.3702(8) 0.1826(6) -0.0799(6) 0.048(2) H12 1 0.4550(8) 0.2003(6) -0.0506(6) 0.055(7) C13 1 0.3719(9) 0.1340(6) -0.1584(6) 0.050(2) H13 1 0.4572(9) 0.1202(6) -0.1819(6) 0.055(7) C14 1 0.2488(9) 0.1049(6) -0.2040(5) 0.050(2) C15 1 0.1274(9) 0.1301(6) -0.1676(6) 0.050(2) H15 1 0.0418(9) 0.1133(6) -0.1965(6) 0.055(7) C16 1 0.1298(8) 0.1795(6) -0.0898(6) 0.048(2) H16 1 0.0447(8) 0.1956(6) -0.0682(6) 0.055(7) C17 1 0.2514(10) 0.0452(6) -0.2854(6) 0.058(3) H171 1 0.2677(71) -0.0038(8) -0.2557(7) 0.088(16) H172 1 0.3251(47) 0.0567(22) -0.3276(31) 0.088(16) H173 1 0.1631(27) 0.0450(27) -0.3242(32) 0.088(16) N21 1 0.2484(6) 0.3420(4) 0.2267(4) 0.036(2) C22 1 0.2561(8) 0.3122(6) 0.3193(5) 0.041(2) H22 1 0.2673(8) 0.2601(6) 0.3256(5) 0.055(7) C23 1 0.2487(9) 0.3534(6) 0.4035(6) 0.045(2) H23 1 0.2518(9) 0.3288(6) 0.4646(6) 0.055(7) C24 1 0.2365(9) 0.4312(7) 0.3998(6) 0.052(2) C25 1 0.2259(10) 0.4635(7) 0.3044(6) 0.060(3) H25 1 0.2157(10) 0.5155(7) 0.2961(6) 0.055(7) C26 1 0.2311(8) 0.4161(6) 0.2230(6) 0.042(2) H26 1 0.2215(8) 0.4384(6) 0.1604(6) 0.055(7) C27 1 0.2251(15) 0.4788(9) 0.4898(8) 0.099(5) H271 1 0.3016(45) 0.5140(28) 0.4958(30) 0.088(16) H272 1 0.2281(74) 0.4469(9) 0.5476(9) 0.088(16) H273 1 0.1381(38) 0.5060(32) 0.4840(25) 0.088(16) N31 1 0.0728(6) 0.2193(4) 0.1435(4) 0.0345(15) C32 1 0.0807(10) 0.1634(6) 0.2112(6) 0.052(2) H32 1 0.1682(10) 0.1431(6) 0.2306(6) 0.055(7) C33 1 -0.0353(10) 0.1347(7) 0.2531(7) 0.067(3) H33 1 -0.0262(10) 0.0947(7) 0.2981(7) 0.055(7) C34 1 -0.1681(10) 0.1668(8) 0.2268(7) 0.065(3) H34 1 -0.2473(10) 0.1488(8) 0.2553(7) 0.055(7) C35 1 -0.1790(9) 0.2230(6) 0.1610(6) 0.045(2) H35 1 -0.2663(9) 0.2440(6) 0.1432(6) 0.055(7) C36 1 -0.0597(8) 0.2510(5) 0.1179(5) 0.036(2) N41 1 0.0748(6) 0.3333(4) 0.0250(4) 0.034(2) C42 1 0.0828(9) 0.3889(6) -0.0443(5) 0.044(2) H42 1 0.1709(9) 0.4031(6) -0.0625(5) 0.055(7) C43 1 -0.0307(9) 0.4245(6) -0.0881(6) 0.055(3) H43 1 -0.0198(9) 0.4629(6) -0.1342(6) 0.055(7) C44 1 -0.1666(10) 0.4029(6) -0.0631(6) 0.051(2) H44 1 -0.2459(10) 0.4266(6) -0.0926(6) 0.055(7) C45 1 -0.1779(8) 0.3473(6) 0.0042(6) 0.047(2) H45 1 -0.2664(8) 0.3327(6) 0.0212(6) 0.055(7) C46 1 -0.0579(7) 0.3106(6) 0.0498(5) 0.036(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 W 0.01715(14) 0.0005(2) -0.00036(9) 0.0478(2) 0.0009(2) 0.0358(2) Br1 0.0300(4) 0.0125(5) -0.0054(3) 0.0706(7) 0.0084(5) 0.0603(5) Br2 0.0271(4) -0.0135(5) 0.0068(3) 0.0797(8) 0.0069(5) 0.0596(5) N11 0.024(3) 0.002(3) 0.001(2) 0.047(5) 0.000(3) 0.045(3) C12 0.025(4) -0.002(5) 0.004(3) 0.062(7) -0.003(5) 0.058(5) C13 0.032(4) 0.006(5) 0.013(3) 0.064(7) -0.002(5) 0.054(5) C14 0.050(5) 0.006(5) 0.006(4) 0.064(7) 0.012(4) 0.037(4) C15 0.031(4) -0.001(5) -0.002(3) 0.069(7) -0.016(5) 0.050(5) C16 0.022(4) 0.007(5) -0.005(3) 0.064(7) -0.007(5) 0.057(5) C17 0.066(7) 0.005(6) 0.009(4) 0.052(7) -0.014(5) 0.057(5) N21 0.021(3) -0.004(3) -0.006(2) 0.048(5) 0.006(3) 0.038(3) C22 0.034(4) 0.011(4) -0.003(3) 0.049(6) 0.005(4) 0.039(4) C23 0.039(5) -0.002(5) -0.002(3) 0.061(7) 0.000(5) 0.034(4) C24 0.048(5) 0.003(5) -0.008(4) 0.064(7) -0.007(5) 0.041(4) C25 0.058(6) -0.001(6) -0.005(4) 0.058(7) 0.000(5) 0.061(6) C26 0.036(5) 0.004(4) 0.001(3) 0.049(6) 0.000(4) 0.041(4) C27 0.126(12) 0.026(10) -0.005(7) 0.095(11) -0.032(7) 0.073(7) N31 0.025(3) -0.004(3) 0.001(2) 0.042(4) -0.003(3) 0.036(3) C32 0.042(5) -0.013(5) -0.006(4) 0.058(7) 0.012(5) 0.055(5) C33 0.051(6) -0.018(6) 0.004(4) 0.080(9) 0.027(6) 0.070(6) C34 0.038(5) -0.010(6) 0.015(4) 0.106(11) -0.001(6) 0.054(5) C35 0.030(4) -0.012(5) 0.014(3) 0.055(6) -0.010(5) 0.050(4) C36 0.021(3) 0.000(4) 0.009(3) 0.047(5) -0.009(3) 0.039(4) N41 0.021(3) -0.001(3) 0.000(2) 0.049(5) -0.002(3) 0.033(3) C42 0.038(5) -0.004(5) 0.004(3) 0.054(6) 0.003(4) 0.040(4) C43 0.046(5) 0.000(5) -0.012(4) 0.060(7) 0.018(5) 0.055(5) C44 0.044(5) 0.016(5) -0.013(4) 0.044(6) -0.003(5) 0.063(5) C45 0.019(4) 0.004(4) -0.005(3) 0.069(7) -0.011(5) 0.053(5) C46 0.019(3) 0.008(4) 0.003(3) 0.050(5) -0.008(4) 0.038(4) _cod_database_code 2003460