#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/52/2105297.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_2105297 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 'C10 H22 I2 Mn N2 O6' _chemical_formula_sum 'C10 H22 I2 Mn N2 O6' _chemical_formula_weight 575.04 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 104.454(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.6640(10) _cell_length_b 9.4026(10) _cell_length_c 10.0228(11) _cell_measurement_reflns_used 1525 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.43 _cell_measurement_theta_min 3.02 _cell_volume 881.91(16) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.970 _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 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 13020 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 30.56 _diffrn_reflns_theta_min 3.02 _exptl_absorpt_coefficient_mu 4.273 _exptl_absorpt_correction_T_max 0.6997 _exptl_absorpt_correction_T_min 0.6997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 550 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.876 _refine_diff_density_min -0.683 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 2622 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0314 _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.0606 _reflns_number_gt 2151 _reflns_number_total 2622 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 2c in P2(1)/c CELL 0.71073 9.6640 9.4026 10.0228 90.000 104.454 90.000 ZERR 2.00 0.0010 0.0010 0.0011 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O MN I UNIT 20 44 4 12 2 4 TEMP -173.000 L.S. 9 ACTA 50 SIZE .09 .09 .09 BOND BOND $H FMAP 2 PLAN -10 WGHT 0.020000 DFIX 0.92 H1A N1 H1B N1 FVAR 0.15898 MN1 5 0.000000 0.500000 0.500000 10.50000 0.01696 0.01106 = 0.00931 -0.00015 0.00221 -0.00288 I1 6 0.232273 0.312294 0.456185 11.00000 0.01753 0.01175 = 0.01573 0.00082 0.00119 0.00074 SADI H1O O3 H2O O3 O3 4 0.047157 0.449650 0.716941 11.00000 0.02162 0.01210 = 0.01062 -0.00021 -0.00018 0.00104 H1O 2 0.083485 0.379386 0.751384 11.00000 0.03497 H2O 2 0.076285 0.508575 0.771487 11.00000 0.04011 O1 4 0.141465 0.677868 0.561764 11.00000 0.02062 0.01005 = 0.01700 0.00242 0.00200 -0.00269 O2 4 0.113992 0.824944 0.381167 11.00000 0.03079 0.01618 = 0.01167 0.00169 0.00346 0.00264 C1 1 0.151500 0.796881 0.506852 11.00000 0.01497 0.01467 = 0.01648 -0.00158 0.00749 -0.00071 C2 1 0.223106 0.916208 0.599763 11.00000 0.01535 0.01334 = 0.01426 0.00092 0.00399 0.00142 AFIX 13 H2 2 0.166855 1.005832 0.574950 11.00000 -1.20000 AFIX 0 C3 1 0.376507 0.939366 0.586623 11.00000 0.01974 0.01770 = 0.01965 0.00063 0.00815 -0.00025 AFIX 23 H3A 2 0.412039 0.853926 0.547938 11.00000 -1.20000 H3B 2 0.381184 1.021769 0.526417 11.00000 -1.20000 AFIX 0 C4 1 0.463612 0.967205 0.733106 11.00000 0.01859 0.02889 = 0.02204 0.00064 0.00380 -0.00491 AFIX 23 H4A 2 0.455722 1.067700 0.759741 11.00000 -1.20000 H4B 2 0.565595 0.943291 0.743998 11.00000 -1.20000 AFIX 0 C5 1 0.394211 0.867609 0.817322 11.00000 0.01654 0.02525 = 0.01715 0.00153 0.00231 0.00117 AFIX 23 H5A 2 0.426331 0.768275 0.811893 11.00000 -1.20000 H5B 2 0.415926 0.897218 0.915143 11.00000 -1.20000 AFIX 0 N1 3 0.239046 0.883252 0.749883 11.00000 0.01591 0.01545 = 0.01464 -0.00201 0.00621 -0.00049 H1A 2 0.200646 0.955625 0.790945 11.00000 -1.20000 H1B 2 0.191502 0.800417 0.758840 11.00000 -1.20000 HKLF 4 REM 2c in P2(1)/c REM R1 = 0.0314 for 2151 Fo > 4sig(Fo) and 0.0436 for all 2622 data REM 105 parameters refined using 1 restraints END WGHT 0.0227 0.0000 REM Highest difference peak 0.876, deepest hole -0.680, 1-sigma level 0.165 Q1 1 -0.1633 0.6321 0.5659 11.00000 0.05 0.88 Q2 1 0.2932 0.3731 0.4999 11.00000 0.05 0.78 Q3 1 0.1794 0.2332 0.4326 11.00000 0.05 0.73 Q4 1 0.2566 0.2723 0.5443 11.00000 0.05 0.73 Q5 1 0.2963 0.2462 0.4619 11.00000 0.05 0.71 Q6 1 0.2485 0.2946 0.3751 11.00000 0.05 0.69 Q7 1 0.2032 0.8744 0.6625 11.00000 0.05 0.61 Q8 1 0.4262 0.9303 0.7799 11.00000 0.05 0.60 Q9 1 0.3522 0.1851 0.4176 11.00000 0.05 0.58 Q10 1 0.4211 0.8507 1.0100 11.00000 0.05 0.57 ; _cod_data_source_file gp5056.cif _cod_data_source_block 2c _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2105297 _cod_database_fobs_code 2105297 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.0000 0.5000 0.5000 0.01263(15) Uani d S 1 2 I I1 0.23227(2) 0.31229(2) 0.45619(2) 0.01552(7) Uani d . 1 1 O O3 0.0472(3) 0.4497(3) 0.7170(2) 0.0155(5) Uani d D 1 1 H H1O 0.083(4) 0.379(4) 0.751(4) 0.035(13) Uiso d D 1 1 H H2O 0.077(5) 0.509(4) 0.771(4) 0.039(14) Uiso d D 1 1 O O1 0.1415(2) 0.6779(2) 0.5618(2) 0.0164(5) Uani d . 1 1 O O2 0.1140(3) 0.8249(2) 0.3812(2) 0.0199(5) Uani d . 1 1 C C1 0.1515(3) 0.7969(3) 0.5069(3) 0.0147(6) Uani d . 1 1 C C2 0.2231(3) 0.9162(3) 0.5998(3) 0.0143(6) Uani d . 1 1 H H2 0.1668 1.0058 0.5749 0.017 Uiso calc R 1 1 C C3 0.3765(3) 0.9394(4) 0.5866(3) 0.0184(7) Uani d . 1 1 H H3A 0.4121 0.8540 0.5479 0.022 Uiso calc R 1 1 H H3B 0.3812 1.0218 0.5264 0.022 Uiso calc R 1 1 C C4 0.4636(4) 0.9672(4) 0.7331(4) 0.0235(8) Uani d . 1 1 H H4A 0.4557 1.0677 0.7597 0.028 Uiso calc R 1 1 H H4B 0.5656 0.9433 0.7439 0.028 Uiso calc R 1 1 C C5 0.3942(3) 0.8676(4) 0.8174(4) 0.0200(7) Uani d . 1 1 H H5A 0.4264 0.7683 0.8119 0.024 Uiso calc R 1 1 H H5B 0.4160 0.8972 0.9152 0.024 Uiso calc R 1 1 N N1 0.2390(3) 0.8832(3) 0.7499(3) 0.0149(6) Uani d D 1 1 H H1A 0.206(3) 0.958(3) 0.792(3) 0.018 Uiso d D 1 1 H H1B 0.188(3) 0.802(3) 0.752(4) 0.018 Uiso d 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 0.0170(4) 0.0111(3) 0.0093(3) -0.0029(3) 0.0022(3) -0.0002(3) I1 0.01752(11) 0.01175(11) 0.01572(11) 0.00074(8) 0.00119(8) 0.00082(8) O3 0.0216(13) 0.0121(12) 0.0106(12) 0.0010(10) -0.0002(10) -0.0002(10) O1 0.0206(12) 0.0101(11) 0.0170(12) -0.0027(9) 0.0019(10) 0.0024(9) O2 0.0308(14) 0.0162(12) 0.0117(11) 0.0026(10) 0.0035(10) 0.0017(9) C1 0.0149(16) 0.0147(16) 0.0164(16) -0.0007(13) 0.0075(13) -0.0015(13) C2 0.0153(16) 0.0133(16) 0.0143(15) 0.0014(12) 0.0040(13) 0.0009(12) C3 0.0198(17) 0.0176(17) 0.0197(17) -0.0003(14) 0.0082(14) 0.0006(14) C4 0.0186(18) 0.029(2) 0.0222(19) -0.0049(15) 0.0039(15) 0.0006(15) C5 0.0165(17) 0.0252(18) 0.0172(16) 0.0011(14) 0.0023(13) 0.0016(15) N1 0.0160(14) 0.0153(14) 0.0146(13) -0.0010(11) 0.0059(11) -0.0025(11) 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' O O 0.0106 0.0060 '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' 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 O1 Mn1 O1 3_566 . 180.00(10) O1 Mn1 O3 3_566 3_566 85.49(9) O1 Mn1 O3 . 3_566 94.51(9) O1 Mn1 O3 3_566 . 94.51(9) O1 Mn1 O3 . . 85.50(9) O3 Mn1 O3 3_566 . 180.00(13) O1 Mn1 I1 3_566 3_566 93.15(6) O1 Mn1 I1 . 3_566 86.85(6) O3 Mn1 I1 3_566 3_566 92.36(7) O3 Mn1 I1 . 3_566 87.64(7) O1 Mn1 I1 3_566 . 86.85(6) O1 Mn1 I1 . . 93.15(6) O3 Mn1 I1 3_566 . 87.64(7) O3 Mn1 I1 . . 92.36(7) I1 Mn1 I1 3_566 . 180.0 Mn1 O3 H1O . . 126(3) Mn1 O3 H2O . . 120(3) H1O O3 H2O . . 104(4) C1 O1 Mn1 . . 132.6(2) O2 C1 O1 . . 126.3(3) O2 C1 C2 . . 116.0(3) O1 C1 C2 . . 117.6(3) N1 C2 C1 . . 112.3(3) N1 C2 C3 . . 104.8(2) C1 C2 C3 . . 110.8(3) N1 C2 H2 . . 109.6 C1 C2 H2 . . 109.6 C3 C2 H2 . . 109.6 C4 C3 C2 . . 104.8(3) C4 C3 H3A . . 110.8 C2 C3 H3A . . 110.8 C4 C3 H3B . . 110.8 C2 C3 H3B . . 110.8 H3A C3 H3B . . 108.9 C3 C4 C5 . . 102.4(3) C3 C4 H4A . . 111.3 C5 C4 H4A . . 111.3 C3 C4 H4B . . 111.3 C5 C4 H4B . . 111.3 H4A C4 H4B . . 109.2 N1 C5 C4 . . 102.7(3) N1 C5 H5A . . 111.2 C4 C5 H5A . . 111.2 N1 C5 H5B . . 111.2 C4 C5 H5B . . 111.2 H5A C5 H5B . . 109.1 C5 N1 C2 . . 108.3(2) C5 N1 H1A . . 107(2) C2 N1 H1A . . 110(2) C5 N1 H1B . . 113(2) C2 N1 H1B . . 106(2) H1A N1 H1B . . 113(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 O1 3_566 2.151(2) Mn1 O1 . 2.151(2) Mn1 O3 3_566 2.160(2) Mn1 O3 . 2.160(2) Mn1 I1 3_566 2.9729(3) Mn1 I1 . 2.9730(3) O3 H1O . 0.79(3) O3 H2O . 0.78(3) O1 C1 . 1.261(3) O2 C1 . 1.249(4) C1 C2 . 1.511(4) C2 N1 . 1.507(4) C2 C3 . 1.536(4) C2 H2 . 1.0000 C3 C4 . 1.521(5) C3 H3A . 0.9900 C3 H3B . 0.9900 C4 C5 . 1.524(5) C4 H4A . 0.9900 C4 H4B . 0.9900 C5 N1 . 1.491(4) C5 H5A . 0.9900 C5 H5B . 0.9900 N1 H1A . 0.921(18) N1 H1B . 0.910(18)