#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003488.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_2003488 loop_ _publ_author_name 'Licoccia, S.' 'Paolesse, R.' 'Boschi, T.' 'Bandoli, G.' 'Dolmella, A.' _publ_section_title ; Trichlorotin(II)--(meso-Tetraphenylporphyrinato)rhodium(III), a Porphyrin Derivative with an Rh---Sn Bond ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 833 _journal_page_last 835 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C44 H28 Cl3 N4 Rh1 Sn1' _chemical_formula_sum 'C44 H28 Cl3 N4 Rh Sn' _chemical_formula_weight 940.7 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source IntTabIV _cell_angle_alpha 68.20(2) _cell_angle_beta 68.23(2) _cell_angle_gamma 64.08(2) _cell_formula_units_Z 2 _cell_length_a 12.719(2) _cell_length_b 12.906(2) _cell_length_c 16.930(3) _cell_measurement_reflns_used 50 _cell_measurement_temperature 294 _cell_measurement_theta_max 13 _cell_measurement_theta_min 8 _cell_volume 2247.2(8) _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 8311 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.13 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_type empirical _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.390 _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.37 _refine_diff_density_min -1.08 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.72 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 479 _refine_ls_number_reflns 4754 _refine_ls_R_factor_obs 0.057 _refine_ls_shift/esd_max 0.02 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0016F^2^]' _refine_ls_wR_factor_obs 0.080 _reflns_number_observed 4754 _reflns_number_total 7926 _reflns_observed_criterion F>4\s(F) _[local]_cod_data_source_file na1113.cif _[local]_cod_data_source_block na1113a _[local]_cod_chemical_formula_sum_orig 'C44 H28 Cl3 N4 Rh1 Sn1' _cod_original_cell_volume 2247.5(7) _cod_database_code 2003488 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Sn .2054(1) .1974(1) .2390(1) .041(1) Cl(1) .1036(4) .3935(3) .1775(3) .110(2) Cl(2) .3199(4) .2204(5) .3064(3) .130(3) Cl(3) .3440(4) .1330(4) .1181(3) .127(3) Rh .0825(1) .0739(1) .3355(1) .049(1) N(1) -.0611(6) .2204(6) .3619(4) .038(3) N(2) .0260(6) .0855(6) .2345(4) .040(3) N(3) .2253(6) -.0719(6) .3097(4) .040(3) N(4) .1287(6) .0504(6) .4433(5) .041(3) C(1) -.0801(7) .2770(8) .4232(6) .041(4) C(2) -.1763(8) .3922(8) .4077(6) .050(5) C(3) -.2148(8) .3973(9) .3423(7) .052(5) C(4) -.1432(7) .2921(7) .3114(6) .041(4) C(5) -.1542(7) .2661(8) .2428(6) .044(4) C(6) -.0765(8) .1691(8) .2088(6) .045(4) C(7) -.0869(9) .1424(9) .1365(6) .055(5) C(8) .0079(9) .0477(9) .1199(6) .053(5) C(9) .0809(8) .0097(8) .1792(6) .045(5) C(10) .1901(7) -.0819(8) .1796(6) .044(4) C(11) .2591(7) -.1173(8) .2380(5) .040(4) C(12) .3779(8) -.2086(9) .2358(6) .052(5) C(13) .4143(8) -.2160(9) .3043(7) .053(5) C(14) .3188(7) -.1338(8) .3520(5) .041(4) C(15) .3180(8) -.1200(7) .4296(6) .042(4) C(16) .2248(7) -.0378(7) .4746(5) .038(4) C(17) .2212(8) -.0295(8) .5579(6) .049(5) C(18) .1224(8) .0677(8) .5766(6) .047(5) C(19) .0694(7) .1228(7) .5031(5) .038(4) C(20) -.0242(7) .2321(7) .4908(5) .038(4) C(21) -.2574(9) .3531(8) .2020(7) .052(5) C(22) -.3710(8) .3435(11) .2443(7) .067(6) C(23) -.4701(10) .4270(16) .2071(11) .095(9) C(24) -.4553(13) .5128(12) .1377(11) .082(8) C(25) -.3422(17) .5191(12) .0968(11) .105(11) C(26) -.2446(12) .4407(11) .1300(9) .079(8) C(27) .2368(8) -.1524(8) .1116(6) .046(4) C(28) .1850(10) -.2335(9) .1222(7) .059(6) C(29) .2304(11) -.2973(11) .0588(9) .076(7) C(30) .3223(11) -.2802(13) -.0114(9) .082(8) C(31) .3759(12) -.2001(13) -.0226(8) .085(8) C(32) .3316(10) -.1374(12) .0414(8) .075(7) C(33) .4256(8) -.1942(8) .4672(6) .044(4) C(34) .4595(8) -.3177(9) .4989(7) .054(5) C(35) .5581(9) -.3795(9) .5317(6) .056(5) C(36) .6258(9) -.3265(10) .5343(7) .065(6) C(37) .5923(10) -.2044(11) .5058(8) .071(7) C(38) .4942(9) -.1400(9) .4720(7) .061(6) C(39) -.0576(8) .3055(8) .5530(6) .044(4) C(40) .0301(11) .3373(10) .5592(7) .064(6) C(41) -.0056(17) .4076(11) .6181(10) .089(10) C(42) -.1104(15) .4368(11) .6693(9) .079(8) C(43) -.2003(15) .4048(11) .6654(8) .091(8) C(44) -.1708(9) .3393(8) .6052(6) .054(5) H(2A) -.2060 .4513 .4396 ? H(3A) -.2787 .4621 .3186 ? H(7A) -.1509 .1867 .1069 ? H(8A) .0252 .0093 .0754 ? H(12A) .4224 -.2545 .1929 ? H(13A) .4904 -.2673 .3179 ? H(17A) .2763 -.0826 .5941 ? H(18A) .0949 .0954 .6286 ? H(22A) -.3814 .2806 .2959 ? H(23A) -.5475 .4176 .2339 ? H(24A) -.5247 .5709 .1169 ? H(25A) -.3345 .5820 .0447 ? H(26A) -.1657 .4455 .1003 ? H(28A) .1185 -.2441 .1714 ? H(29A) .1966 -.3542 .0648 ? H(30A) .3527 -.3246 -.0546 ? H(31A) .4422 -.1907 -.0722 ? H(32A) .3667 -.0811 .0346 ? H(34A) .4129 -.3572 .4958 ? H(35A) .5785 -.4641 .5545 ? H(36A) .6959 -.3721 .5573 ? H(37A) .6392 -.1644 .5080 ? H(38A) .4721 -.0551 .4511 ? H(40A) .1109 .3144 .5230 ? H(41A) .0523 .4319 .6234 ? H(42A) -.1311 .4832 .7095 ? H(43A) -.2804 .4283 .7025 ? H(44A) -.2308 .3165 .6013 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl(1) Sn Rh 116.90(10) yes Cl(3) Sn Rh 116.0(2) yes Sn Rh N(2) 91.7(2) yes Sn Rh N(4) 94.4(2) yes N(2) Rh N(3) 89.9(3) yes N(1) Rh N(4) 90.2(3) yes N(2) Rh N(4) 173.8(3) yes Cl(2) Sn Rh 114.80(10) yes Sn Rh N(1) 90.8(2) yes Sn Rh N(3) 89.3(2) yes N(1) Rh N(2) 90.3(3) yes N(3) Rh N(4) 89.6(3) yes N(1) Rh N(3) 179.7(4) yes Cl(1) Sn Cl(2) 101.1(2) no C(1) N(1) C(4) 108.1(7) no C(6) N(2) C(9) 106.7(9) no C(11) N(3) C(14) 106.9(6) no C(16) N(4) C(19) 105.2(8) no C(2) C(1) C(20) 125.1(10) no N(1) C(4) C(3) 107.9(10) no C(4) C(5) C(6) 124.9(8) no N(2) C(6) C(5) 126.0(11) no C(6) C(7) C(8) 106.7(10) no N(2) C(9) C(10) 125.0(10) no C(9) C(10) C(27) 116.9(10) no N(3) C(11) C(12) 108.2(9) no C(12) C(13) C(14) 107.5(8) no C(13) C(14) C(15) 125.2(8) no C(16) C(15) C(33) 116.7(10) no C(15) C(16) C(17) 124.0(8) no N(4) C(19) C(18) 109.3(6) no C(1) C(20) C(19) 124.0(9) no C(5) C(21) C(22) 117.7(8) no C(21) C(22) C(23) 118.3(10) no C(24) C(25) C(26) 121.5(13) no C(10) C(27) C(32) 119.4(12) no C(28) C(29) C(30) 120.6(16) no C(27) C(32) C(31) 120.8(6) no C(34) C(33) C(38) 117.7(9) no C(35) C(36) C(37) 119.3(11) no C(20) C(39) C(40) 119.5(8) no C(39) C(40) C(41) 117.6(12) no C(42) C(43) C(44) 118.6(12) no Cl(1) Sn Cl(3) 102.3(2) no Rh N(1) C(1) 125.3(6) no Rh N(2) C(6) 126.4(7) no Rh N(3) C(11) 126.2(6) no Rh N(4) C(16) 128.0(6) no N(1) C(1) C(2) 107.9(9) no C(1) C(2) C(3) 106.9(10) no N(1) C(4) C(5) 125.9(8) no C(4) C(5) C(21) 116.6(8) no N(2) C(6) C(7) 108.8(8) no C(7) C(8) C(9) 109.6(11) no C(8) C(9) C(10) 126.9(10) no C(11) C(10) C(27) 117.3(7) no C(10) C(11) C(12) 126.3(10) no N(3) C(14) C(13) 109.5(9) no C(14) C(15) C(16) 124.4(8) no N(4) C(16) C(15) 125.0(9) no C(16) C(17) C(18) 106.5(8) no N(4) C(19) C(20) 124.8(8) no C(1) C(20) C(39) 119.9(7) no C(5) C(21) C(26) 122.6(11) no C(22) C(23) C(24) 120.7(13) no C(21) C(26) C(25) 120.1(14) no C(28) C(27) C(32) 120.7(12) no C(29) C(30) C(31) 121.7(15) no C(15) C(33) C(34) 122.8(11) no C(33) C(34) C(35) 119.7(12) no C(36) C(37) C(38) 119.9(15) no C(20) C(39) C(44) 121.4(11) no C(40) C(41) C(42) 124.(2) no C(39) C(44) C(43) 121.0(14) no Cl(2) Sn Cl(3) 103.6(2) no Rh N(1) C(4) 125.6(7) no Rh N(2) C(9) 126.9(5) no Rh N(3) C(14) 126.2(7) no Rh N(4) C(19) 126.8(5) no N(1) C(1) C(20) 126.9(7) no C(2) C(3) C(4) 109.1(8) no C(3) C(4) C(5) 126.1(8) no C(6) C(5) C(21) 118.5(11) no C(5) C(6) C(7) 125.1(8) no N(2) C(9) C(8) 108.1(7) no C(9) C(10) C(11) 125.8(10) no N(3) C(11) C(10) 125.4(7) no C(11) C(12) C(13) 107.9(9) no N(3) C(14) C(15) 125.3(7) no C(14) C(15) C(33) 118.8(7) no N(4) C(16) C(17) 111.0(7) no C(17) C(18) C(19) 107.6(9) no C(18) C(19) C(20) 125.9(9) no C(19) C(20) C(39) 116.0(9) no C(22) C(21) C(26) 119.6(10) no C(23) C(24) C(25) 119.6(14) no C(10) C(27) C(28) 119.9(8) no C(27) C(28) C(29) 118.5(10) no C(30) C(31) C(32) 117.8(12) no C(15) C(33) C(38) 119.5(8) no C(34) C(35) C(36) 122.2(10) no C(33) C(38) C(37) 121.2(11) no C(40) C(39) C(44) 119.1(11) no C(41) C(42) C(43) 119.7(17) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Sn Rh 2.4500(10) yes Sn Cl(2) 2.318(7) yes Rh N(1) 2.028(6) yes Rh N(3) 2.017(6) yes Sn Cl(1) 2.313(3) yes Sn Cl(3) 2.301(4) yes Rh N(2) 2.022(9) yes Rh N(4) 2.000(9) yes N(1) C(1) 1.380(10) no N(2) C(6) 1.380(10) no N(3) C(11) 1.390(10) no N(4) C(16) 1.370(10) no C(1) C(2) 1.460(10) no C(2) C(3) 1.34(2) no C(4) C(5) 1.39(2) no C(5) C(21) 1.510(10) no C(7) C(8) 1.320(10) no C(9) C(10) 1.380(10) no C(10) C(27) 1.52(2) no C(12) C(13) 1.36(2) no C(14) C(15) 1.39(2) no C(15) C(33) 1.500(10) no C(17) C(18) 1.370(10) no C(19) C(20) 1.400(10) no C(21) C(22) 1.390(10) no C(22) C(23) 1.43(2) no C(24) C(25) 1.37(3) no C(27) C(28) 1.39(2) no C(28) C(29) 1.39(2) no C(30) C(31) 1.39(3) no C(33) C(34) 1.400(10) no C(34) C(35) 1.350(10) no C(36) C(37) 1.38(2) no C(39) C(40) 1.39(2) no C(40) C(41) 1.41(2) no C(42) C(43) 1.40(3) no N(1) C(4) 1.380(10) no N(2) C(9) 1.390(10) no N(3) C(14) 1.390(10) no N(4) C(19) 1.410(10) no C(1) C(20) 1.380(10) no C(3) C(4) 1.430(10) no C(5) C(6) 1.380(10) no C(6) C(7) 1.45(2) no C(8) C(9) 1.43(2) no C(10) C(11) 1.380(10) no C(11) C(12) 1.450(10) no C(13) C(14) 1.430(10) no C(15) C(16) 1.390(10) no C(16) C(17) 1.44(2) no C(18) C(19) 1.430(10) no C(20) C(39) 1.500(10) no C(21) C(26) 1.330(10) no C(23) C(24) 1.30(2) no C(25) C(26) 1.37(2) no C(27) C(32) 1.370(10) no C(29) C(30) 1.35(2) no C(31) C(32) 1.40(2) no C(33) C(38) 1.37(2) no C(35) C(36) 1.33(2) no C(37) C(38) 1.36(2) no C(39) C(44) 1.360(10) no C(41) C(42) 1.27(2) no C(43) C(44) 1.40(2) no