#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003463.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_2003463 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 820 _journal_page_last 822 _publ_section_title ; Tris(2,2'-bipyridine)manganese(II) Perchlorate Hemihydrate ; _chemical_formula_moiety 'C30 H24 Cl2 Mn1 N6 O8.5' _chemical_formula_sum 'C30 H24 Cl2 Mn N6 O8.5' _[local]_cod_chemical_formula_sum_orig 'C30 H24 Cl2 Mn1 N6 O8.5' _chemical_formula_weight 730.4 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 8.133(2) _cell_length_b 11.056(2) _cell_length_c 18.658(5) _cell_angle_alpha 102.27(2) _cell_angle_beta 91.02(2) _cell_angle_gamma 99.77(2) _cell_volume 1613.1(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 6198 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 0.636 _cell_measurement_temperature 295 _exptl_crystal_description 'needle-like' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.40 _exptl_crystal_size_rad ? _exptl_crystal_colour 'golden yellow' _chemical_compound_source ? _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method '\w' _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.996 _diffrn_reflns_number 6198 _reflns_number_total 5759 _reflns_number_observed 3875 _reflns_observed_criterion F>6\s(F) _diffrn_reflns_av_R_equivalents 0.0142 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0583 _refine_ls_wR_factor_obs 0.0736 _refine_ls_goodness_of_fit_obs 3.02 _refine_ls_number_reflns 3875 _refine_ls_number_parameters 424 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.002F^2^]' _refine_ls_shift/esd_max 0.63 _refine_diff_density_max 0.63 _refine_diff_density_min -0.41 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Mn(1) .0062(1) .2370(1) .7423(1) .055(1) N(11) .1500(5) .0930(3) .6877(2) .060(2) N(12) .1585(4) .1886(3) .8336(2) .058(2) C(10) .1711(6) .0648(5) .6149(3) .068(2) C(11) .2709(7) -.0181(5) .5847(3) .084(3) C(12) .3522(8) -.0746(6) .6295(4) .094(3) C(13) .3303(7) -.0479(5) .7041(3) .081(2) C(14) .2286(6) .0369(4) .7315(3) .057(2) C(15) .2039(5) .0755(4) .8118(3) .057(2) C(16) .2196(7) -.0008(5) .8602(3) .076(2) C(17) .1934(7) .0404(6) .9341(3) .082(3) C(18) .1538(7) .1577(6) .9561(3) .078(2) C(19) .1366(6) .2285(5) .9056(3) .068(2) N(21) -.1445(5) .3495(4) .8202(2) .063(2) N(22) -.2004(5) .0973(4) .7767(2) .062(2) C(20) -.1313(7) .4752(5) .8305(3) .080(2) C(21) -.2425(10) .5386(7) .8721(3) .104(3) C(22) -.3694(10) .4724(9) .9027(4) .115(4) C(23) -.3825(7) .3438(8) .8926(3) .095(3) C(24) -.2695(6) .2856(5) .8510(3) .067(2) C(25) -.2783(6) .1476(5) .8359(3) .067(2) C(26) -.3551(7) .0720(8) .8812(3) .097(3) C(27) -.3587(9) -.0553(8) .8632(4) .117(4) C(28) -.2841(9) -.1049(7) .8019(4) .105(3) C(29) -.2051(7) -.0269(5) .7603(3) .081(2) N(31) -.1295(5) .2783(4) .6477(2) .063(2) N(32) .1719(5) .3920(3) .7074(2) .063(2) C(30) -.2873(7) .2208(5) .6226(3) .073(2) C(31) -.3828(7) .2681(6) .5784(3) .081(3) C(32) -.3190(9) .3796(7) .5603(3) .095(3) C(33) -.1601(8) .4388(5) .5842(3) .084(3) C(34) -.0679(7) .3863(4) .6285(3) .062(2) C(35) .1081(7) .4429(4) .6564(3) .064(2) C(36) .2036(9) .5388(5) .6308(3) .091(3) C(37) .3663(10) .5784(6) .6560(4) .107(3) C(38) .4347(8) .5270(6) .7074(4) .096(3) C(39) .3305(7) .4349(5) .7329(3) .077(2) Cl(1) -.2699(2) .3235(1) 1.0854(1) .080(1) O(11) -.2465(5) .4550(4) 1.0884(3) .107(2) O(12) -.1560(6) .2684(5) 1.0402(3) .138(3) O(13) -.2509(8) .3028(4) 1.1574(2) .142(3) O(14) -.4355(6) .2673(4) 1.0549(3) .124(2) Cl(2) .1999(2) .2256(1) .4378(1) .071(1) O(21) .1924(13) .0886(6) .4356(6) .111(4) O(22) .0525(8) .2288(7) .3926(4) .093(2) O(23) .1899(13) .2876(9) .5135(3) .140(4) O(24) .3475(9) .2734(8) .4055(5) .134(4) O(21') .1678(13) .2532(9) .3665(4) .135(3) O(22') .2448(13) .1083(6) .4306(5) .109(4) O(23') .0640(10) .2482(9) .4818(5) .149(4) O(24') .3431(9) .3237(7) .4702(5) .131(3) O(1w) .0531(23) .2953(17) .2481(10) .254(8) H(10) .1113 .1028 .5835 .100 H(11) .2865 -.0343 .5329 .100 H(12) .4230 -.1329 .6089 .100 H(13) .3839 -.0878 .7366 .100 H(16) .2493 -.0819 .8425 .100 H(17) .2037 -.0120 .9683 .100 H(18) .1384 .1899 1.0071 .100 H(19) .1073 .3102 .9217 .100 H(20) -.0419 .5202 .8083 .100 H(21) -.2274 .6284 .8785 .100 H(22) -.4456 .5178 .9312 .100 H(23) -.4701 .2960 .9142 .100 H(26) -.4055 .1093 .9246 .100 H(27) -.4153 -.1085 .8930 .100 H(28) -.2875 -.1942 .7888 .100 H(29) -.1490 -.0629 .7183 .100 H(30) -.3341 .1450 .6377 .100 H(31) -.4927 .2244 .5601 .100 H(32) -.3849 .4152 .5298 .100 H(33) -.1116 .5165 .5716 .100 H(36) .1555 .5762 .5954 .100 H(37) .4350 .6431 .6374 .100 H(38) .5498 .5537 .7246 .100 H(39) .3748 .3993 .7701 .100 _cod_database_code 2003463