#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/52/2105293.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_2105293 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 'C7 H17 Br2 Mn N O4' _chemical_formula_sum 'C7 H17 Br2 Mn N O4' _chemical_formula_weight 393.98 _chemical_name_systematic ; ? ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 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 92.172(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.286(2) _cell_length_b 8.256(2) _cell_length_c 9.387(3) _cell_measurement_reflns_used 1044 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 22.27 _cell_measurement_theta_min 2.46 _cell_volume 641.7(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 7642 _diffrn_reflns_theta_full 26.50 _diffrn_reflns_theta_max 26.50 _diffrn_reflns_theta_min 2.17 _exptl_absorpt_coefficient_mu 7.249 _exptl_absorpt_correction_T_max 0.5947 _exptl_absorpt_correction_T_min 0.2450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 386 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.613 _refine_diff_density_min -0.478 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_reflns 2665 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0351 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.0643 _reflns_number_gt 2440 _reflns_number_total 2665 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 1b in P2(1) CELL 0.71073 8.2863 8.2565 9.3866 90.000 92.172 90.000 ZERR 2.00 0.0022 0.0022 0.0025 0.000 0.004 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O MN BR UNIT 14 34 2 8 2 4 TEMP -173 SIZE .27 .08 .08 L.S. 10 BOND BOND $H ACTA FMAP 2 PLAN -20 WGHT 0.000000 FVAR 0.17879 DFIX 0.92 H1A N1 H1B N1 MN1 5 -0.007324 0.823019 0.663401 11.00000 0.01660 0.01081 = 0.01244 -0.00003 0.00008 -0.00036 BR1 6 0.102263 0.848591 0.925786 11.00000 0.02155 0.01455 = 0.01242 -0.00054 -0.00014 -0.00136 BR2 6 -0.263333 0.651858 0.713197 11.00000 0.01816 0.01902 = 0.02237 -0.00300 0.00466 -0.00469 O1 4 -0.088809 0.842659 0.435453 11.00000 0.02133 0.01168 = 0.01617 -0.00172 0.00141 -0.00059 O2 4 -0.119538 1.107695 0.401722 11.00000 0.02309 0.00774 = 0.01579 -0.00062 0.00143 -0.00217 C1 1 -0.120901 0.961645 0.359625 11.00000 0.01172 0.01762 = 0.01446 -0.00003 0.00402 -0.00168 C2 1 -0.174148 0.936065 0.203468 11.00000 0.01859 0.00802 = 0.01374 0.00276 -0.00282 0.00309 AFIX 13 H2 2 -0.101695 0.998693 0.140853 11.00000 -1.20000 AFIX 0 C3 1 -0.349936 0.987981 0.173330 11.00000 0.02013 0.01809 = 0.02395 -0.00233 -0.00529 0.00668 AFIX 23 H3A 2 -0.410307 0.991190 0.262302 11.00000 -1.20000 H3B 2 -0.355322 1.096005 0.127622 11.00000 -1.20000 AFIX 0 C4 1 -0.417280 0.856854 0.072077 11.00000 0.01495 0.01754 = 0.01960 0.00358 -0.00303 0.00334 AFIX 23 H4A 2 -0.536316 0.849533 0.075577 11.00000 -1.20000 H4B 2 -0.387254 0.877819 -0.027328 11.00000 -1.20000 AFIX 0 C5 1 -0.337959 0.706711 0.129555 11.00000 0.01586 0.02093 = 0.03201 0.00067 -0.00353 -0.00626 AFIX 23 H5A 2 -0.340614 0.619385 0.057229 11.00000 -1.20000 H5B 2 -0.391486 0.667944 0.215693 11.00000 -1.20000 AFIX 0 N1 3 -0.168023 0.759076 0.164960 11.00000 0.01597 0.00980 = 0.01469 -0.00297 0.00275 0.00032 H1A 2 -0.104474 0.743822 0.087816 11.00000 -1.20000 H1B 2 -0.125417 0.699769 0.240361 11.00000 -1.20000 SADI O3 H3 O4 H4 O3 4 0.212131 0.957512 0.586770 11.00000 0.01888 0.02080 = 0.02275 0.01052 0.00307 0.00089 H3 2 0.207850 0.997387 0.507851 11.00000 0.03001 C6 1 0.369781 0.885711 0.596843 11.00000 0.01326 0.02539 = 0.02735 0.00233 0.00102 -0.00221 AFIX 137 H7A 2 0.395308 0.854838 0.695960 11.00000 -1.50000 H7B 2 0.449904 0.963969 0.565374 11.00000 -1.50000 H7C 2 0.371840 0.789271 0.536076 11.00000 -1.50000 AFIX 0 O4 4 -0.099124 1.072487 0.680919 11.00000 0.02438 0.01448 = 0.01347 -0.00193 0.00455 0.00420 H4 2 -0.111621 1.085274 0.594387 11.00000 0.02538 C7 1 -0.238407 1.121833 0.755700 11.00000 0.02128 0.02499 = 0.02369 -0.00289 0.00608 0.00235 AFIX 137 H6A 2 -0.332802 1.060460 0.720105 11.00000 -1.50000 H6B 2 -0.257382 1.237785 0.740309 11.00000 -1.50000 H6C 2 -0.220321 1.101011 0.857845 11.00000 -1.50000 HKLF 4 1 1 0 0 0 1 0 0 0 1 0.89 REM 1b in P2(1) REM R1 = 0.0351 for 2440 Fo > 4sig(Fo) and 0.0416 for all 2665 data REM 146 parameters refined using 2 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 0.619, deepest hole -0.479, 1-sigma level 0.108 Q1 1 0.0040 0.8575 0.9540 11.00000 0.05 0.62 Q2 1 -0.1751 0.6661 0.6816 11.00000 0.05 0.52 Q3 1 0.1904 0.8332 0.8951 11.00000 0.05 0.51 Q4 1 0.0042 0.8446 0.7656 11.00000 0.05 0.46 Q5 1 -0.1583 0.8568 0.2015 11.00000 0.05 0.41 Q6 1 -0.2948 1.1133 0.2753 11.00000 0.05 0.41 Q7 1 -0.3659 0.6670 0.7424 11.00000 0.05 0.41 Q8 1 -0.1037 0.8020 0.6865 11.00000 0.05 0.40 Q9 1 0.2780 0.8564 0.9653 11.00000 0.05 0.40 Q10 1 -0.2409 0.6009 0.8257 11.00000 0.05 0.39 Q11 1 0.1160 0.7532 0.9809 11.00000 0.05 0.38 Q12 1 -0.5008 0.9010 -0.1058 11.00000 0.05 0.37 Q13 1 -0.3837 0.6652 0.5306 11.00000 0.05 0.37 Q14 1 0.0059 0.7452 0.7378 11.00000 0.05 0.37 Q15 1 -0.3286 1.1461 0.0426 11.00000 0.05 0.37 Q16 1 -0.1035 0.7976 0.9459 11.00000 0.05 0.36 Q17 1 -0.3101 0.6606 0.9635 11.00000 0.05 0.35 Q18 1 -0.3075 0.9785 0.7818 11.00000 0.05 0.35 Q19 1 0.5257 0.8880 0.7730 11.00000 0.05 0.35 Q20 1 0.4108 0.8205 0.5391 11.00000 0.05 0.35 ; _cod_data_source_file gp5056.cif _cod_data_source_block 1b _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2105293 _cod_database_fobs_code 2105293 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, 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 -0.00733(9) 0.82303(10) 0.66340(8) 0.01330(18) Uani d . 1 1 Br Br1 0.10226(6) 0.84859(6) 0.92578(5) 0.01619(13) Uani d . 1 1 Br Br2 -0.26334(6) 0.65186(7) 0.71320(6) 0.01977(14) Uani d . 1 1 O O1 -0.0888(4) 0.8426(5) 0.4355(3) 0.0164(8) Uani d . 1 1 O O2 -0.1196(4) 1.1077(4) 0.4017(4) 0.0154(8) Uani d . 1 1 C C1 -0.1209(6) 0.9616(7) 0.3596(5) 0.0144(12) Uani d . 1 1 C C2 -0.1742(7) 0.9361(6) 0.2035(5) 0.0136(12) Uani d . 1 1 H H2 -0.1017 0.9986 0.1409 0.016 Uiso calc R 1 1 C C3 -0.3499(7) 0.9880(7) 0.1733(6) 0.0210(13) Uani d . 1 1 H H3A -0.4103 0.9912 0.2623 0.025 Uiso calc R 1 1 H H3B -0.3553 1.0961 0.1277 0.025 Uiso calc R 1 1 C C4 -0.4172(6) 0.8570(7) 0.0721(5) 0.0175(11) Uani d . 1 1 H H4A -0.5362 0.8497 0.0756 0.021 Uiso calc R 1 1 H H4B -0.3872 0.8780 -0.0273 0.021 Uiso calc R 1 1 C C5 -0.3379(7) 0.7068(7) 0.1296(6) 0.0229(14) Uani d . 1 1 H H5A -0.3406 0.6195 0.0572 0.028 Uiso calc R 1 1 H H5B -0.3915 0.6680 0.2157 0.028 Uiso calc R 1 1 N N1 -0.1682(6) 0.7588(5) 0.1651(5) 0.0134(10) Uani d D 1 1 H H1A -0.105(5) 0.756(7) 0.085(4) 0.016 Uiso d D 1 1 H H1B -0.117(5) 0.702(6) 0.238(4) 0.016 Uiso d D 1 1 O O3 0.2121(5) 0.9575(5) 0.5868(4) 0.0207(9) Uani d D 1 1 H H3 0.207(7) 0.997(7) 0.508(5) 0.027(19) Uiso d D 1 1 C C6 0.3698(6) 0.8857(7) 0.5969(6) 0.0220(14) Uani d . 1 1 H H7A 0.3953 0.8549 0.6960 0.033 Uiso calc R 1 1 H H7B 0.4499 0.9639 0.5653 0.033 Uiso calc R 1 1 H H7C 0.3718 0.7892 0.5362 0.033 Uiso calc R 1 1 O O4 -0.0991(5) 1.0725(5) 0.6809(4) 0.0174(9) Uani d D 1 1 H H4 -0.111(7) 1.085(8) 0.595(5) 0.026(19) Uiso d D 1 1 C C7 -0.2383(6) 1.1217(8) 0.7557(6) 0.0230(14) Uani d . 1 1 H H6A -0.3328 1.0606 0.7199 0.035 Uiso calc R 1 1 H H6B -0.2571 1.2378 0.7407 0.035 Uiso calc R 1 1 H H6C -0.2204 1.1004 0.8578 0.035 Uiso calc R 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 0.0166(4) 0.0108(5) 0.0124(4) -0.0003(4) 0.0001(3) 0.0000(3) Br1 0.0215(3) 0.0145(3) 0.0124(2) -0.0014(3) -0.0001(2) -0.0005(2) Br2 0.0182(3) 0.0191(3) 0.0224(3) -0.0047(3) 0.0047(2) -0.0030(3) O1 0.0213(19) 0.0117(19) 0.0162(17) -0.0005(19) 0.0013(14) -0.0020(19) O2 0.023(2) 0.008(2) 0.0156(19) -0.0021(16) 0.0014(16) -0.0005(15) C1 0.012(3) 0.018(3) 0.014(3) -0.002(2) 0.004(2) 0.000(2) C2 0.018(3) 0.008(3) 0.014(3) 0.003(2) -0.003(2) 0.003(2) C3 0.020(3) 0.018(3) 0.024(3) 0.007(3) -0.005(2) -0.003(3) C4 0.015(3) 0.018(3) 0.019(3) 0.003(3) -0.003(2) 0.004(3) C5 0.016(3) 0.021(3) 0.032(3) -0.006(2) -0.003(3) 0.001(3) N1 0.016(3) 0.010(2) 0.015(2) 0.0000(19) 0.0022(19) -0.0027(19) O3 0.019(2) 0.021(2) 0.023(2) 0.0008(18) 0.0029(18) 0.0104(19) C6 0.013(3) 0.025(4) 0.028(3) -0.002(2) 0.001(2) 0.002(3) O4 0.024(2) 0.014(2) 0.013(2) 0.0039(17) 0.0045(17) -0.0018(17) C7 0.021(3) 0.024(4) 0.024(3) 0.003(3) 0.006(2) -0.003(3) 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' Br Br -0.2901 2.4595 '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 2_546 . 163.94(14) O2 Mn1 O1 2_546 . 85.49(14) O4 Mn1 O1 . . 84.87(14) O2 Mn1 O3 2_546 . 84.76(14) O4 Mn1 O3 . . 81.34(14) O1 Mn1 O3 . . 82.96(14) O2 Mn1 Br1 2_546 . 100.25(10) O4 Mn1 Br1 . . 87.86(10) O1 Mn1 Br1 . . 170.74(11) O3 Mn1 Br1 . . 90.29(11) O2 Mn1 Br2 2_546 . 90.73(10) O4 Mn1 Br2 . . 102.00(11) O1 Mn1 Br2 . . 89.57(10) O3 Mn1 Br2 . . 171.54(11) Br1 Mn1 Br2 . . 97.56(3) C1 O1 Mn1 . . 131.5(3) C1 O2 Mn1 . 2_556 133.7(3) O1 C1 O2 . . 125.2(5) O1 C1 C2 . . 119.4(5) O2 C1 C2 . . 115.4(5) N1 C2 C1 . . 110.6(4) N1 C2 C3 . . 105.5(4) C1 C2 C3 . . 112.1(4) N1 C2 H2 . . 109.5 C1 C2 H2 . . 109.5 C3 C2 H2 . . 109.5 C4 C3 C2 . . 103.8(4) C4 C3 H3A . . 111.0 C2 C3 H3A . . 111.0 C4 C3 H3B . . 111.0 C2 C3 H3B . . 111.0 H3A C3 H3B . . 109.0 C5 C4 C3 . . 102.6(4) C5 C4 H4A . . 111.3 C3 C4 H4A . . 111.3 C5 C4 H4B . . 111.3 C3 C4 H4B . . 111.3 H4A C4 H4B . . 109.2 C4 C5 N1 . . 103.8(4) C4 C5 H5A . . 111.0 N1 C5 H5A . . 111.0 C4 C5 H5B . . 111.0 N1 C5 H5B . . 111.0 H5A C5 H5B . . 109.0 C5 N1 C2 . . 107.0(4) C5 N1 H1A . . 112(3) C2 N1 H1A . . 104(3) C5 N1 H1B . . 115(3) C2 N1 H1B . . 110(3) H1A N1 H1B . . 109(4) C6 O3 Mn1 . . 121.0(3) C6 O3 H3 . . 104(4) Mn1 O3 H3 . . 118(4) O3 C6 H7A . . 109.5 O3 C6 H7B . . 109.5 H7A C6 H7B . . 109.5 O3 C6 H7C . . 109.5 H7A C6 H7C . . 109.5 H7B C6 H7C . . 109.5 C7 O4 Mn1 . . 126.1(3) C7 O4 H4 . . 112(4) Mn1 O4 H4 . . 94(4) O4 C7 H6A . . 109.5 O4 C7 H6B . . 109.5 H6A C7 H6B . . 109.5 O4 C7 H6C . . 109.5 H6A C7 H6C . . 109.5 H6B C7 H6C . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 O2 2_546 2.165(3) Mn1 O4 . 2.204(4) Mn1 O1 . 2.225(3) Mn1 O3 . 2.270(4) Mn1 Br1 . 2.6011(11) Mn1 Br2 . 2.6060(11) O1 C1 . 1.237(6) O2 C1 . 1.269(6) O2 Mn1 2_556 2.165(3) C1 C2 . 1.529(7) C2 N1 . 1.509(6) C2 C3 . 1.534(7) C2 H2 . 1.0000 C3 C4 . 1.531(8) C3 H3A . 0.9900 C3 H3B . 0.9900 C4 C5 . 1.494(8) C4 H4A . 0.9900 C4 H4B . 0.9900 C5 N1 . 1.496(7) C5 H5A . 0.9900 C5 H5B . 0.9900 N1 H1A . 0.931(19) N1 H1B . 0.924(19) O3 C6 . 1.435(6) O3 H3 . 0.81(4) C6 H7A . 0.9800 C6 H7B . 0.9800 C6 H7C . 0.9800 O4 C7 . 1.432(6) O4 H4 . 0.82(4) C7 H6A . 0.9800 C7 H6B . 0.9800 C7 H6C . 0.9800