#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/52/2105295.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_2105295 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 Cl2 Mn N2 O6' _chemical_formula_sum 'C10 H22 Cl2 Mn N2 O6' _chemical_formula_weight 392.14 _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 107.704(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.124(3) _cell_length_b 9.034(3) _cell_length_c 10.001(3) _cell_measurement_reflns_used 2761 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.42 _cell_measurement_theta_min 2.34 _cell_volume 785.3(4) _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 0.999 _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 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8789 _diffrn_reflns_theta_full 26.50 _diffrn_reflns_theta_max 26.50 _diffrn_reflns_theta_min 2.34 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_T_max 0.7943 _exptl_absorpt_correction_T_min 0.7134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 406 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.537 _refine_diff_density_min -0.224 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 139 _refine_ls_number_reflns 1630 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0278 _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^)+(0.0370P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.0714 _reflns_number_gt 1445 _reflns_number_total 1630 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 2a in P2(1)/c CELL 0.71073 9.1241 9.0326 10.0012 90.000 107.704 90.000 ZERR 2.00 0.0027 0.0027 0.0030 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL MN UNIT 20 44 4 12 4 2 TEMP -173 L.S. 10 BOND BOND $H FMAP 2 SIZE .3 .2 .2 PLAN -20 ACTA WGHT 0.037000 0.300000 FVAR 0.29605 0.50897 DFIX 0.92 H1A N1 H1B N1 MOLE 1 MN1 6 0.000000 0.500000 0.500000 10.50000 0.01888 0.01153 = 0.01475 -0.00011 0.00278 -0.00210 CL1 5 0.200273 0.332067 0.441301 11.00000 0.02354 0.01446 = 0.01969 -0.00027 0.00328 0.00172 SADI O3 H5A O3 H5B O3 4 0.076125 0.429429 0.717713 11.00000 0.03338 0.01199 = 0.01656 0.00012 0.00199 0.00043 H5A 2 0.099369 0.352060 0.750668 11.00000 0.03356 H5B 2 0.102972 0.488338 0.776048 11.00000 0.04505 O1 4 0.163076 0.681515 0.570407 11.00000 0.02398 0.01314 = 0.02008 0.00117 0.00247 -0.00442 O2 4 0.127455 0.841973 0.393253 11.00000 0.04993 0.01608 = 0.01806 0.00071 0.00706 -0.00095 C1 1 0.164166 0.809029 0.520568 11.00000 0.01807 0.01460 = 0.01942 -0.00105 0.00503 -0.00049 C2 1 0.219206 0.937359 0.621909 11.00000 0.02427 0.01347 = 0.01785 0.00078 0.00164 0.00146 AFIX 13 H2 2 0.136750 1.014566 0.599112 11.00000 -1.20000 AFIX 0 PART 1 C3A 1 0.361017 1.008152 0.627834 21.00000 0.02061 0.02242 = 0.02561 0.00374 0.00642 -0.00178 AFIX 23 H3AA 2 0.367977 1.107411 0.671307 21.00000 -1.20000 H3BA 2 0.372516 1.018199 0.532961 21.00000 -1.20000 AFIX 0 C4A 1 0.482745 0.903113 0.719346 21.00000 0.01379 0.03088 = 0.03219 0.00220 0.00184 -0.00080 AFIX 23 H4AA 2 0.578222 0.957344 0.768515 21.00000 -1.20000 H4BA 2 0.507724 0.823174 0.662128 21.00000 -1.20000 AFIX 0 C5A 1 0.406036 0.840353 0.824211 21.00000 0.02176 0.02662 = 0.02118 0.00297 0.00153 -0.00174 AFIX 23 H5AA 2 0.412504 0.730938 0.827424 21.00000 -1.20000 H5BA 2 0.455584 0.879906 0.919617 21.00000 -1.20000 AFIX 0 PART 2 C3B 1 0.394137 0.976619 0.617718 -21.00000 0.01458 0.02313 = 0.02747 -0.00147 0.00749 -0.00895 AFIX 23 H3AB 2 0.437161 0.894197 0.576183 -21.00000 -1.20000 H3BB 2 0.394540 1.067921 0.563067 -21.00000 -1.20000 AFIX 0 C4B 1 0.484029 0.998211 0.770968 -21.00000 0.02009 0.02880 = 0.02629 0.00047 0.00153 -0.00718 AFIX 23 H4AB 2 0.595346 0.981712 0.787119 -21.00000 -1.20000 H4BB 2 0.468580 1.099119 0.802915 -21.00000 -1.20000 AFIX 0 C5B 1 0.418681 0.883802 0.845048 -21.00000 0.01447 0.02893 = 0.02186 0.00158 -0.00645 -0.00330 AFIX 23 H5AB 2 0.441940 0.908069 0.945892 -21.00000 -1.20000 H5BB 2 0.460602 0.784499 0.835998 -21.00000 -1.20000 AFIX 0 PART 0 N1 3 0.244608 0.889537 0.770409 11.00000 0.02151 0.01781 = 0.01642 -0.00242 0.00453 0.00041 H1A 2 0.227062 0.967068 0.823215 11.00000 -1.20000 H1B 2 0.179106 0.813244 0.773997 11.00000 -1.20000 HKLF 4 REM 2a in P2(1)/c REM R1 = 0.0280 for 1445 Fo > 4sig(Fo) and 0.0330 for all 1630 data REM 133 parameters refined using 1 restraints END WGHT 0.0364 0.3094 REM Highest difference peak 0.535, deepest hole -0.227, 1-sigma level 0.062 Q1 1 -0.0145 0.4988 0.5822 11.00000 0.05 0.53 Q2 1 0.2231 0.3351 0.3568 11.00000 0.05 0.42 Q3 1 -0.1809 0.6783 0.4728 11.00000 0.05 0.41 Q4 1 0.2177 0.9064 0.6863 11.00000 0.05 0.31 Q5 1 0.1854 0.8688 0.5810 11.00000 0.05 0.30 Q6 1 -0.1054 0.5885 0.5270 11.00000 0.05 0.27 Q7 1 0.2139 0.8636 0.4243 11.00000 0.05 0.25 Q8 1 0.2036 1.0240 0.6050 11.00000 0.05 0.24 Q9 1 -0.0780 0.5684 0.3684 11.00000 0.05 0.23 Q10 1 0.1377 0.8199 0.3380 11.00000 0.05 0.22 ; _cod_data_source_file gp5056.cif _cod_data_source_block 2a _cod_original_cell_volume 785.2(4) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2105295 _cod_database_fobs_code 2105295 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 _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn1 0.0000 0.5000 0.5000 0.01557(13) Uani d S 1 2 . . Cl Cl1 0.20028(5) 0.33207(5) 0.44130(5) 0.01996(14) Uani d . 1 1 . . O O3 0.07612(17) 0.42942(16) 0.71773(15) 0.0219(3) Uani d D 1 1 . . H H5A 0.100(3) 0.352(2) 0.750(3) 0.034(7) Uiso d D 1 1 . . H H5B 0.103(3) 0.488(3) 0.776(3) 0.044(9) Uiso d D 1 1 . . O O1 0.16308(15) 0.68153(14) 0.57041(13) 0.0200(3) Uani d . 1 1 . . O O2 0.12745(18) 0.84199(15) 0.39323(14) 0.0288(3) Uani d . 1 1 . . C C1 0.1641(2) 0.8090(2) 0.52060(19) 0.0175(4) Uani d . 1 1 B . C C2 0.2192(2) 0.9373(2) 0.62190(19) 0.0196(4) Uani d . 1 1 . . H H2 0.1368 1.0146 0.5991 0.024 Uiso calc R 1 1 A 1 C C3A 0.3612(13) 1.0081(13) 0.6280(14) 0.0231(19) Uani d P 0.510(8) 1 B 1 H H3AA 0.3682 1.1074 0.6715 0.028 Uiso calc PR 0.510(8) 1 B 1 H H3BA 0.3728 1.0182 0.5332 0.028 Uiso calc PR 0.510(8) 1 B 1 C C4A 0.4827(4) 0.9032(6) 0.7194(5) 0.0268(14) Uani d P 0.510(8) 1 B 1 H H4AA 0.5782 0.9575 0.7684 0.032 Uiso calc PR 0.510(8) 1 B 1 H H4BA 0.5076 0.8233 0.6621 0.032 Uiso calc PR 0.510(8) 1 B 1 C C5A 0.4064(17) 0.8404(12) 0.8244(14) 0.0243(19) Uani d P 0.510(8) 1 B 1 H H5AA 0.4129 0.7309 0.8277 0.029 Uiso calc PR 0.510(8) 1 B 1 H H5BA 0.4559 0.8800 0.9198 0.029 Uiso calc PR 0.510(8) 1 B 1 C C3B 0.3940(13) 0.9766(13) 0.6176(15) 0.0215(19) Uani d P 0.490(8) 1 B 2 H H3AB 0.4370 0.8942 0.5760 0.026 Uiso calc PR 0.490(8) 1 B 2 H H3BB 0.3944 1.0679 0.5629 0.026 Uiso calc PR 0.490(8) 1 B 2 C C4B 0.4841(5) 0.9982(6) 0.7710(5) 0.0262(14) Uani d P 0.490(8) 1 B 2 H H4AB 0.5954 0.9815 0.7871 0.031 Uiso calc PR 0.490(8) 1 B 2 H H4BB 0.4688 1.0992 0.8029 0.031 Uiso calc PR 0.490(8) 1 B 2 C C5B 0.4183(18) 0.8840(12) 0.8449(15) 0.025(2) Uani d P 0.490(8) 1 B 2 H H5AB 0.4415 0.9084 0.9457 0.030 Uiso calc PR 0.490(8) 1 B 2 H H5BB 0.4603 0.7847 0.8359 0.030 Uiso calc PR 0.490(8) 1 B 2 N N1 0.24476(19) 0.88961(19) 0.77046(16) 0.0189(3) Uani d D 1 1 B . H H1A 0.219(2) 0.965(2) 0.818(2) 0.023 Uiso d D 1 1 . . H H1B 0.185(2) 0.812(2) 0.773(2) 0.023 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 0.0189(2) 0.0116(2) 0.0147(2) -0.00210(15) 0.00279(16) -0.00012(15) Cl1 0.0235(3) 0.0145(2) 0.0197(2) 0.00172(17) 0.00328(18) -0.00027(17) O3 0.0335(8) 0.0120(7) 0.0165(7) 0.0004(6) 0.0020(6) 0.0001(6) O1 0.0239(7) 0.0131(7) 0.0201(7) -0.0044(5) 0.0025(5) 0.0012(5) O2 0.0500(10) 0.0160(7) 0.0180(7) -0.0009(7) 0.0070(7) 0.0008(6) C1 0.0181(9) 0.0146(9) 0.0194(9) -0.0005(7) 0.0050(7) -0.0010(7) C2 0.0242(10) 0.0135(9) 0.0180(9) 0.0015(8) 0.0017(8) 0.0008(7) C3A 0.021(5) 0.022(4) 0.025(3) -0.002(3) 0.007(3) 0.004(3) C4A 0.014(2) 0.031(3) 0.032(3) -0.0008(17) 0.0020(17) 0.002(2) C5A 0.022(4) 0.026(5) 0.022(4) -0.001(4) 0.002(3) 0.003(4) C3B 0.015(5) 0.023(5) 0.027(3) -0.009(3) 0.008(3) -0.002(3) C4B 0.020(2) 0.028(3) 0.026(2) -0.0072(18) 0.0017(17) 0.000(2) C5B 0.016(3) 0.029(6) 0.022(4) -0.003(4) -0.006(3) 0.002(4) N1 0.0217(8) 0.0173(8) 0.0169(8) 0.0006(7) 0.0048(7) -0.0024(7) 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' Cl Cl 0.1484 0.1585 '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' 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 O3 Mn1 O3 3_566 . 180.0 O3 Mn1 O1 3_566 . 94.69(5) O3 Mn1 O1 . . 85.31(5) O3 Mn1 O1 3_566 3_566 85.30(5) O3 Mn1 O1 . 3_566 94.69(5) O1 Mn1 O1 . 3_566 180.0 O3 Mn1 Cl1 3_566 3_566 91.31(4) O3 Mn1 Cl1 . 3_566 88.69(4) O1 Mn1 Cl1 . 3_566 86.87(4) O1 Mn1 Cl1 3_566 3_566 93.13(4) O3 Mn1 Cl1 3_566 . 88.69(4) O3 Mn1 Cl1 . . 91.31(4) O1 Mn1 Cl1 . . 93.13(4) O1 Mn1 Cl1 3_566 . 86.87(4) Cl1 Mn1 Cl1 3_566 . 179.9990(10) Mn1 O3 H5A . . 130.8(19) Mn1 O3 H5B . . 120(2) H5A O3 H5B . . 108(3) C1 O1 Mn1 . . 130.38(12) O2 C1 O1 . . 126.18(17) O2 C1 C2 . . 115.41(16) O1 C1 C2 . . 118.39(16) C3A C2 N1 . . 102.8(6) C3A C2 C1 . . 118.7(4) N1 C2 C1 . . 111.24(15) C3A C2 C3B . . 14.6(6) N1 C2 C3B . . 103.2(5) C1 C2 C3B . . 105.8(4) C3A C2 H2 . . 107.9 N1 C2 H2 . . 107.9 C1 C2 H2 . . 107.9 C3B C2 H2 . . 120.7 C2 C3A C4A . . 103.4(8) C2 C3A H3AA . . 111.1 C4A C3A H3AA . . 111.1 C2 C3A H3BA . . 111.1 C4A C3A H3BA . . 111.1 H3AA C3A H3BA . . 109.1 C3A C4A C5A . . 103.9(8) C3A C4A H4AA . . 111.0 C5A C4A H4AA . . 111.0 C3A C4A H4BA . . 111.0 C5A C4A H4BA . . 111.0 H4AA C4A H4BA . . 109.0 N1 C5A C4A . . 104.4(9) N1 C5A H5AA . . 110.9 C4A C5A H5AA . . 110.9 N1 C5A H5BA . . 110.9 C4A C5A H5BA . . 110.9 H5AA C5A H5BA . . 108.9 C4B C3B C2 . . 103.4(7) C4B C3B H3AB . . 111.1 C2 C3B H3AB . . 111.1 C4B C3B H3BB . . 111.1 C2 C3B H3BB . . 111.1 H3AB C3B H3BB . . 109.0 C5B C4B C3B . . 103.6(7) C5B C4B H4AB . . 111.0 C3B C4B H4AB . . 111.0 C5B C4B H4BB . . 111.0 C3B C4B H4BB . . 111.0 H4AB C4B H4BB . . 109.0 C4B C5B N1 . . 104.4(9) C4B C5B H5AB . . 110.9 N1 C5B H5AB . . 110.9 C4B C5B H5BB . . 110.9 N1 C5B H5BB . . 110.9 H5AB C5B H5BB . . 108.9 C5A N1 C2 . . 106.7(6) C5A N1 C5B . . 16.8(5) C2 N1 C5B . . 108.5(6) C5A N1 H1A . . 115.4(15) C2 N1 H1A . . 108.6(14) C5B N1 H1A . . 99.7(15) C5A N1 H1B . . 107.6(15) C2 N1 H1B . . 109.9(14) C5B N1 H1B . . 120.6(15) H1A N1 H1B . . 109(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 O3 3_566 2.1704(15) Mn1 O3 . 2.1704(15) Mn1 O1 . 2.1820(13) Mn1 O1 3_566 2.1820(13) Mn1 Cl1 3_566 2.5763(7) Mn1 Cl1 . 2.5763(7) O3 H5A . 0.774(19) O3 H5B . 0.77(2) O1 C1 . 1.256(2) O2 C1 . 1.251(2) C1 C2 . 1.521(3) C2 C3A . 1.429(13) C2 N1 . 1.496(2) C2 C3B . 1.647(12) C2 H2 . 1.0000 C3A C4A . 1.532(13) C3A H3AA . 0.9900 C3A H3BA . 0.9900 C4A C5A . 1.535(15) C4A H4AA . 0.9900 C4A H4BA . 0.9900 C5A N1 . 1.476(15) C5A H5AA . 0.9900 C5A H5BA . 0.9900 C3B C4B . 1.516(15) C3B H3AB . 0.9900 C3B H3BB . 0.9900 C4B C5B . 1.496(15) C4B H4AB . 0.9900 C4B H4BB . 0.9900 C5B N1 . 1.532(15) C5B H5AB . 0.9900 C5B H5BB . 0.9900 N1 H1A . 0.903(16) N1 H1B . 0.890(16)