#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/52/2105294.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_2105294 loop_ _publ_author_name 'Lamberts, Kevin' 'Englert, Ulli' _publ_section_title ; Structures from MnX~2~ and proline: isomorphous racemic compounds and a series of chiral non-isomorphous chain polymers ; _journal_coeditor_code GP5056 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 610 _journal_page_last 618 _journal_paper_doi 10.1107/S0108768112043996 _journal_volume 68 _journal_year 2012 _chemical_formula_moiety 'C5 H15 I Mn N O5, I' _chemical_formula_sum 'C5 H15 I2 Mn N O5' _chemical_formula_weight 477.92 _chemical_name_systematic ; ? ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.1264(18) _cell_length_b 11.867(3) _cell_length_c 13.727(3) _cell_measurement_reflns_used 1755 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.51 _cell_measurement_theta_min 2.27 _cell_volume 1323.8(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 goniometer with SMART APEX CCD detector' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator 'multi layer optics' _diffrn_radiation_source microsource _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15709 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.27 _exptl_absorpt_coefficient_mu 5.659 _exptl_absorpt_correction_T_max 0.6602 _exptl_absorpt_correction_T_min 0.5046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 892 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.133 _refine_diff_density_min -1.086 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 2690 _refine_ls_number_restraints 21 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.0778 _reflns_number_gt 2412 _reflns_number_total 2690 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 1c in P2(1)2(1)2(1) CELL 0.71073 8.1264 11.8671 13.7270 90.000 90.000 90.000 ZERR 4.00 0.0018 0.0025 0.0029 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N MN I O UNIT 20 60 4 4 8 20 TEMP -173.000 L.S. 9 ACTA BOND BOND $H FMAP 2 SIZE .14 .08 .08 PLAN -20 DELU 0.001 C1 > N1 DFIX 0.85 O3 H6A O3 H6B O4 H7A O4 H7B O5 H8A O5 H8B DFIX 0.92 H1A N1 H1B N1 WGHT 0.030000 FVAR 0.21603 MN1 4 0.469466 0.164295 0.579961 11.00000 0.01264 0.01044 = 0.01741 0.00094 -0.00098 0.00056 I1 5 0.476166 -0.035177 0.693187 11.00000 0.01794 0.01302 = 0.02237 0.00490 -0.00119 0.00080 O1 6 0.483335 0.331696 0.512118 11.00000 0.01413 0.00961 = 0.02367 0.00571 -0.00243 0.00224 O2 6 0.752719 0.367479 0.502469 11.00000 0.01262 0.01487 = 0.02166 -0.00075 -0.00056 0.00177 C1 1 0.603479 0.391103 0.489198 11.00000 0.01407 0.00667 = 0.00802 -0.00355 0.00268 -0.00080 C2 1 0.569188 0.504200 0.440022 11.00000 0.01539 0.01023 = 0.01863 0.00158 -0.00149 -0.00025 AFIX 13 H2 2 0.625587 0.507482 0.375337 11.00000 -1.20000 AFIX 0 C3 1 0.617724 0.607003 0.502052 11.00000 0.02144 0.00543 = 0.02958 0.00026 -0.00653 0.00348 AFIX 23 H3A 2 0.698991 0.585552 0.552480 11.00000 -1.20000 H3B 2 0.665702 0.666982 0.460748 11.00000 -1.20000 AFIX 0 C4 1 0.458604 0.646629 0.548579 11.00000 0.02661 0.00969 = 0.02711 -0.00168 -0.00263 0.00396 AFIX 23 H4A 2 0.465208 0.727141 0.567060 11.00000 -1.20000 H4B 2 0.431826 0.601414 0.607078 11.00000 -1.20000 AFIX 0 C5 1 0.332603 0.628240 0.468564 11.00000 0.02051 0.00833 = 0.03073 0.00400 -0.00303 0.00380 AFIX 23 H5A 2 0.219637 0.624176 0.495335 11.00000 -1.20000 H5B 2 0.337740 0.688800 0.419055 11.00000 -1.20000 AFIX 0 N1 3 0.385359 0.517221 0.426897 11.00000 0.01509 0.01194 = 0.01978 0.00199 0.00139 0.00055 H1A 2 0.359212 0.514140 0.361742 11.00000 -1.20000 H1B 2 0.331314 0.459499 0.458171 11.00000 -1.20000 O3 6 0.618724 0.102768 0.457312 11.00000 0.02112 0.01191 = 0.02153 -0.00336 0.00122 -0.00491 H6A 2 0.572506 0.056205 0.420225 11.00000 -1.20000 H6B 2 0.661782 0.147834 0.417115 11.00000 -1.20000 O4 6 0.689258 0.218581 0.649883 11.00000 0.02108 0.01841 = 0.02234 0.00829 -0.00494 -0.00247 H7A 2 0.733333 0.270487 0.618611 11.00000 -1.20000 H7B 2 0.740747 0.197473 0.699734 11.00000 -1.20000 O5 6 0.299950 0.260124 0.679082 11.00000 0.02081 0.00903 = 0.01717 0.00083 0.00447 -0.00200 H8A 2 0.316634 0.311915 0.720118 11.00000 -1.20000 H8B 2 0.236073 0.226143 0.717030 11.00000 -1.20000 I2 5 1.011858 0.619331 0.693425 11.00000 0.01651 0.01847 = 0.01675 -0.00242 -0.00094 0.00217 HKLF 4 REM 1c in P2(1)2(1)2(1) REM R1 = 0.0334 for 2412 Fo > 4sig(Fo) and 0.0402 for all 2690 data REM 145 parameters refined using 19 restraints END WGHT 0.0311 0.0000 REM Highest difference peak 1.133, deepest hole -1.086, 1-sigma level 0.188 Q1 1 0.5972 0.3804 0.1979 11.00000 0.05 1.13 Q2 1 0.4984 -0.0378 0.6237 11.00000 0.05 1.13 Q3 1 0.3836 0.3813 0.2182 11.00000 0.05 1.12 Q4 1 0.5821 -0.0323 0.6761 11.00000 0.05 1.05 Q5 1 0.4751 0.3947 0.1231 11.00000 0.05 1.03 Q6 1 0.5243 0.3724 0.2576 11.00000 0.05 0.99 Q7 1 0.3891 0.3739 0.1692 11.00000 0.05 0.91 Q8 1 0.3790 -0.0431 0.7165 11.00000 0.05 0.88 Q9 1 0.4569 -0.0252 0.7620 11.00000 0.05 0.88 Q10 1 0.3756 -0.0295 0.6614 11.00000 0.05 0.80 ; _cod_data_source_file gp5056.cif _cod_data_source_block 1c _cod_database_code 2105294 _cod_database_fobs_code 2105294 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_type_symbol _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_symmetry_multiplicity Mn Mn1 0.46947(13) 0.16430(8) 0.57996(7) 0.0135(2) Uani d . 1 1 I I1 0.47616(5) -0.03518(3) 0.69319(3) 0.01778(12) Uani d . 1 1 O O1 0.4834(6) 0.3317(3) 0.5121(3) 0.0158(10) Uani d . 1 1 O O2 0.7527(6) 0.3675(4) 0.5025(3) 0.0164(11) Uani d . 1 1 C C1 0.6035(8) 0.3912(6) 0.4892(4) 0.0095(12) Uani d U 1 1 C C2 0.5693(8) 0.5042(5) 0.4401(5) 0.0147(12) Uani d U 1 1 H H2 0.6258 0.5075 0.3754 0.018 Uiso calc R 1 1 C C3 0.6178(9) 0.6069(6) 0.5021(5) 0.0187(13) Uani d U 1 1 H H3A 0.6990 0.5854 0.5525 0.022 Uiso calc R 1 1 H H3B 0.6658 0.6669 0.4608 0.022 Uiso calc R 1 1 C C4 0.4586(9) 0.6466(6) 0.5486(5) 0.0212(14) Uani d U 1 1 H H4A 0.4653 0.7271 0.5671 0.025 Uiso calc R 1 1 H H4B 0.4318 0.6014 0.6070 0.025 Uiso calc R 1 1 C C5 0.3327(9) 0.6283(6) 0.4685(6) 0.0198(14) Uani d U 1 1 H H5A 0.2197 0.6242 0.4953 0.024 Uiso calc R 1 1 H H5B 0.3378 0.6889 0.4191 0.024 Uiso calc R 1 1 N N1 0.3856(7) 0.5171(5) 0.4267(4) 0.0156(11) Uani d DU 1 1 H H1A 0.348(8) 0.517(7) 0.363(2) 0.019 Uiso d D 1 1 H H1B 0.331(8) 0.465(5) 0.463(4) 0.019 Uiso d D 1 1 O O3 0.6187(6) 0.1028(4) 0.4573(4) 0.0183(11) Uani d D 1 1 H H6A 0.572(8) 0.056(5) 0.420(4) 0.022 Uiso d D 1 1 H H6B 0.661(9) 0.148(5) 0.417(4) 0.022 Uiso d D 1 1 O O4 0.6893(7) 0.2186(5) 0.6499(4) 0.0206(12) Uani d D 1 1 H H7A 0.733(9) 0.270(5) 0.618(5) 0.025 Uiso d D 1 1 H H7B 0.740(8) 0.198(6) 0.700(3) 0.025 Uiso d D 1 1 O O5 0.2999(6) 0.2602(4) 0.6791(4) 0.0156(10) Uani d D 1 1 H H8A 0.317(9) 0.312(4) 0.720(4) 0.019 Uiso d D 1 1 H H8B 0.236(7) 0.226(6) 0.717(4) 0.019 Uiso d D 1 1 I I2 1.01186(5) 0.61933(3) 0.69342(3) 0.01725(12) Uani d . 1 1 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 Mn1 0.0126(5) 0.0105(5) 0.0174(5) 0.0006(4) -0.0010(4) 0.0009(4) I1 0.0179(2) 0.0130(2) 0.0224(2) 0.00079(17) -0.0012(2) 0.00490(18) O1 0.014(2) 0.010(2) 0.024(2) 0.002(2) -0.002(2) 0.0058(18) O2 0.013(2) 0.015(3) 0.022(3) 0.002(2) -0.001(2) -0.001(2) C1 0.014(3) 0.007(2) 0.008(3) -0.001(2) 0.002(2) -0.004(2) C2 0.015(2) 0.011(2) 0.018(3) 0.000(2) -0.002(3) 0.0017(17) C3 0.021(2) 0.005(2) 0.029(4) 0.003(2) -0.006(2) 0.001(3) C4 0.026(3) 0.010(3) 0.027(4) 0.004(3) -0.003(2) -0.002(2) C5 0.021(3) 0.008(3) 0.031(4) 0.004(2) -0.003(3) 0.004(3) N1 0.015(2) 0.012(3) 0.020(3) 0.0007(19) 0.001(2) 0.002(2) O3 0.021(3) 0.012(3) 0.022(3) -0.005(2) 0.001(2) -0.003(2) O4 0.021(3) 0.018(3) 0.022(3) -0.002(2) -0.005(2) 0.008(2) O5 0.021(3) 0.009(3) 0.017(3) -0.002(2) 0.004(2) 0.001(2) I2 0.0165(2) 0.0185(2) 0.0167(2) 0.00217(18) -0.0009(2) -0.00241(18) 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' Mn Mn 0.3368 0.7283 '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' O O 0.0106 0.0060 '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 O2 Mn1 O4 4_456 . 171.42(19) O2 Mn1 O1 4_456 . 88.70(18) O4 Mn1 O1 . . 82.79(18) O2 Mn1 O3 4_456 . 89.47(19) O4 Mn1 O3 . . 89.0(2) O1 Mn1 O3 . . 86.97(18) O2 Mn1 O5 4_456 . 84.48(18) O4 Mn1 O5 . . 95.1(2) O1 Mn1 O5 . . 80.24(17) O3 Mn1 O5 . . 165.95(19) O2 Mn1 I1 4_456 . 99.19(13) O4 Mn1 I1 . . 89.38(14) O1 Mn1 I1 . . 170.89(12) O3 Mn1 I1 . . 97.59(14) O5 Mn1 I1 . . 95.90(13) C1 O1 Mn1 . . 131.3(4) C1 O2 Mn1 . 4_556 139.5(4) O1 C1 O2 . . 126.3(6) O1 C1 C2 . . 117.9(6) O2 C1 C2 . . 115.8(6) N1 C2 C1 . . 108.8(5) N1 C2 C3 . . 103.9(6) C1 C2 C3 . . 113.9(5) N1 C2 H2 . . 110.0 C1 C2 H2 . . 110.0 C3 C2 H2 . . 110.0 C4 C3 C2 . . 105.1(6) C4 C3 H3A . . 110.7 C2 C3 H3A . . 110.7 C4 C3 H3B . . 110.7 C2 C3 H3B . . 110.7 H3A C3 H3B . . 108.8 C3 C4 C5 . . 103.1(6) C3 C4 H4A . . 111.2 C5 C4 H4A . . 111.2 C3 C4 H4B . . 111.2 C5 C4 H4B . . 111.2 H4A C4 H4B . . 109.1 N1 C5 C4 . . 102.1(5) N1 C5 H5A . . 111.3 C4 C5 H5A . . 111.3 N1 C5 H5B . . 111.3 C4 C5 H5B . . 111.3 H5A C5 H5B . . 109.2 C5 N1 C2 . . 109.0(6) C5 N1 H1A . . 105(5) C2 N1 H1A . . 116(5) C5 N1 H1B . . 104(5) C2 N1 H1B . . 110(5) H1A N1 H1B . . 111(7) Mn1 O3 H6A . . 116(5) Mn1 O3 H6B . . 121(5) H6A O3 H6B . . 102(7) Mn1 O4 H7A . . 110(6) Mn1 O4 H7B . . 134(5) H7A O4 H7B . . 116(8) Mn1 O5 H8A . . 132(5) Mn1 O5 H8B . . 120(5) H8A O5 H8B . . 92(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 O2 4_456 2.127(5) Mn1 O4 . 2.128(6) Mn1 O1 . 2.197(4) Mn1 O3 . 2.200(5) Mn1 O5 . 2.246(5) Mn1 I1 . 2.8323(11) O1 C1 . 1.245(7) O2 C1 . 1.258(8) O2 Mn1 4_556 2.127(5) C1 C2 . 1.527(9) C2 N1 . 1.512(9) C2 C3 . 1.538(9) C2 H2 . 1.0000 C3 C4 . 1.517(10) C3 H3A . 0.9900 C3 H3B . 0.9900 C4 C5 . 1.517(10) C4 H4A . 0.9900 C4 H4B . 0.9900 C5 N1 . 1.502(9) C5 H5A . 0.9900 C5 H5B . 0.9900 N1 H1A . 0.92(2) N1 H1B . 0.91(2) O3 H6A . 0.84(2) O3 H6B . 0.84(2) O4 H7A . 0.83(2) O4 H7B . 0.84(2) O5 H8A . 0.84(2) O5 H8B . 0.84(2)