#------------------------------------------------------------------------------ #$Date: 2014-10-25 18:23:10 +0100 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/52/2105292.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_2105292 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_volume 68 _journal_year 2012 _chemical_formula_moiety 'C5 H9 Cl2 Mn N O2, H2 O' _chemical_formula_sum 'C5 H11 Cl2 Mn N O3' _chemical_formula_weight 258.99 _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 7.0862(6) _cell_length_b 10.0235(8) _cell_length_c 13.2437(11) _cell_measurement_reflns_used 1584 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 21.39 _cell_measurement_theta_min 2.55 _cell_volume 940.68(13) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _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 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11373 _diffrn_reflns_theta_full 27.12 _diffrn_reflns_theta_max 27.12 _diffrn_reflns_theta_min 2.55 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_correction_T_min 0.7731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.524 _refine_diff_density_min -0.328 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 2039 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0319 _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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.0737 _reflns_number_gt 1797 _reflns_number_total 2039 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 1a in P2(1)2(1)2(1) CELL 0.71073 7.0862 10.0235 13.2437 90.000 90.000 90.000 ZERR 4.00 0.0006 0.0008 0.0011 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 O CL MN UNIT 20 44 4 12 8 4 TEMP -173 L.S. 9 ACTA SIZE .14 .06 .05 BOND BOND $H FMAP 2 PLAN -20 DFIX 0.92 H1A N1 H1B N1 WGHT 0.035000 FVAR 0.20556 MN1 6 0.324404 0.247722 0.500344 11.00000 0.01323 0.02118 = 0.01664 0.00303 0.00081 -0.00011 CL1 5 0.574633 0.367058 0.603988 11.00000 0.01576 0.02586 = 0.02170 -0.00411 -0.00144 0.00118 CL2 5 0.575200 0.069940 0.467701 11.00000 0.01602 0.01913 = 0.02185 0.00078 -0.00012 0.00004 O1 4 0.419389 0.357892 0.372307 11.00000 0.01854 0.02676 = 0.02084 0.01063 0.00072 -0.00244 O2 4 0.734629 0.358146 0.367074 11.00000 0.01492 0.02880 = 0.01842 0.00653 0.00096 0.00237 C1 1 0.573331 0.406945 0.349193 11.00000 0.01913 0.02183 = 0.01163 0.00000 -0.00086 -0.00095 C2 1 0.574329 0.540584 0.294586 11.00000 0.01723 0.02931 = 0.02720 0.01082 0.00043 0.00310 AFIX 13 H2 2 0.647777 0.535119 0.230245 11.00000 -1.20000 AFIX 0 C3 1 0.648715 0.651380 0.361790 11.00000 0.03769 0.02568 = 0.05822 0.00622 -0.01390 -0.00744 AFIX 23 H3A 2 0.755215 0.619610 0.403773 11.00000 -1.20000 H3B 2 0.691131 0.728634 0.321119 11.00000 -1.20000 AFIX 0 C4 1 0.480230 0.687970 0.426835 11.00000 0.07813 0.02352 = 0.03737 -0.00444 -0.01320 0.00078 AFIX 23 H4A 2 0.493515 0.779486 0.454036 11.00000 -1.20000 H4B 2 0.466551 0.624857 0.483867 11.00000 -1.20000 AFIX 0 C5 1 0.312323 0.678755 0.356026 11.00000 0.04693 0.02768 = 0.02798 0.00402 0.01194 0.00830 AFIX 23 H5A 2 0.199573 0.645299 0.392182 11.00000 -1.20000 H5B 2 0.282800 0.767119 0.326601 11.00000 -1.20000 AFIX 0 N1 3 0.372529 0.581784 0.274719 11.00000 0.02574 0.02384 = 0.01947 0.00557 -0.00150 0.00507 H1A 2 0.295277 0.508022 0.275410 11.00000 -1.20000 H1B 2 0.363350 0.621529 0.212295 11.00000 -1.20000 O3 4 0.082591 0.403437 0.237999 11.00000 0.03486 0.04804 = 0.03483 0.01783 -0.00061 -0.00192 DFIX 0.85 H1O O3 H2O O3 H1O 2 0.016928 0.377410 0.290559 11.00000 -1.20000 H2O 2 0.005970 0.452612 0.199975 11.00000 -1.20000 HKLF 4 REM 1a in P2(1)2(1)2(1) REM R1 = 0.0319 for 1797 Fo > 4sig(Fo) and 0.0404 for all 2039 data REM 115 parameters refined using 2 restraints END WGHT 0.0312 0.1460 REM Highest difference peak 0.527, deepest hole -0.334, 1-sigma level 0.081 Q1 1 0.1467 0.2425 0.5046 11.00000 0.05 0.53 Q2 1 0.4656 0.1422 0.4730 11.00000 0.05 0.34 Q3 1 0.0006 0.3480 0.5555 11.00000 0.05 0.33 Q4 1 0.2503 0.1321 0.4018 11.00000 0.05 0.32 Q5 1 0.2409 0.1870 0.4741 11.00000 0.05 0.31 Q6 1 0.4234 0.3140 0.5110 11.00000 0.05 0.31 Q7 1 0.1650 0.3559 0.5439 11.00000 0.05 0.30 Q8 1 0.5075 -0.0004 0.4908 11.00000 0.05 0.30 Q9 1 0.4140 0.2374 0.4845 11.00000 0.05 0.30 Q10 1 0.2441 0.3069 0.5067 11.00000 0.05 0.29 ; _[local]_cod_data_source_file gp5056.cif _[local]_cod_data_source_block 1a _cod_database_code 2105292 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 0.32439(6) 0.24773(5) 0.50034(4) 0.01702(13) Uani d . 1 1 Cl Cl1 0.57461(12) 0.36706(8) 0.60399(6) 0.02109(18) Uani d . 1 1 Cl Cl2 0.57519(12) 0.06994(7) 0.46770(5) 0.01899(17) Uani d . 1 1 O O1 0.4195(3) 0.3579(2) 0.37232(15) 0.0220(5) Uani d . 1 1 O O2 0.7347(3) 0.3581(2) 0.36705(16) 0.0207(5) Uani d . 1 1 C C1 0.5733(5) 0.4069(3) 0.3492(2) 0.0176(6) Uani d . 1 1 C C2 0.5742(5) 0.5406(3) 0.2945(2) 0.0249(7) Uani d . 1 1 H H2 0.6477 0.5351 0.2302 0.030 Uiso calc R 1 1 C C3 0.6488(6) 0.6513(4) 0.3617(4) 0.0408(11) Uani d . 1 1 H H3A 0.7552 0.6194 0.4037 0.049 Uiso calc R 1 1 H H3B 0.6914 0.7285 0.3211 0.049 Uiso calc R 1 1 C C4 0.4804(6) 0.6881(4) 0.4268(3) 0.0464(12) Uani d . 1 1 H H4A 0.4938 0.7796 0.4539 0.056 Uiso calc R 1 1 H H4B 0.4667 0.6250 0.4839 0.056 Uiso calc R 1 1 C C5 0.3123(6) 0.6788(4) 0.3561(3) 0.0342(10) Uani d . 1 1 H H5A 0.1997 0.6452 0.3922 0.041 Uiso calc R 1 1 H H5B 0.2826 0.7672 0.3267 0.041 Uiso calc R 1 1 N N1 0.3728(4) 0.5818(3) 0.2746(2) 0.0230(7) Uani d D 1 1 H H1A 0.285(4) 0.516(3) 0.281(3) 0.028 Uiso d D 1 1 H H1B 0.363(5) 0.619(3) 0.2126(17) 0.028 Uiso d D 1 1 O O3 0.0825(4) 0.4035(3) 0.2380(2) 0.0392(7) Uani d D 1 1 H H1O 0.015(5) 0.377(4) 0.290(2) 0.047 Uiso d D 1 1 H H2O 0.006(5) 0.452(4) 0.199(3) 0.047 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 0.0132(2) 0.0212(2) 0.0166(2) -0.00012(18) 0.00084(17) 0.0030(2) Cl1 0.0158(4) 0.0258(4) 0.0217(4) 0.0012(4) -0.0014(4) -0.0042(3) Cl2 0.0160(4) 0.0192(3) 0.0218(4) 0.0001(4) -0.0001(4) 0.0008(3) O1 0.0185(12) 0.0269(12) 0.0207(12) -0.0026(12) 0.0009(12) 0.0105(10) O2 0.0149(12) 0.0285(13) 0.0186(13) 0.0022(11) 0.0011(10) 0.0067(11) C1 0.0194(16) 0.0213(16) 0.0119(14) -0.0011(16) -0.0010(15) -0.0002(12) C2 0.0173(16) 0.0300(18) 0.0274(18) 0.0032(18) 0.0007(17) 0.0114(14) C3 0.038(2) 0.027(2) 0.058(3) -0.0076(18) -0.014(2) 0.007(2) C4 0.078(4) 0.024(2) 0.037(2) 0.001(2) -0.013(2) -0.0044(18) C5 0.047(3) 0.027(2) 0.028(2) 0.0081(19) 0.0118(19) 0.0036(17) N1 0.0246(17) 0.0249(16) 0.0193(15) 0.0049(13) -0.0008(12) 0.0058(13) O3 0.0346(16) 0.0481(17) 0.0349(15) -0.0014(17) -0.0006(15) 0.0179(13) 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 O1 Mn1 O2 . 4_456 177.78(10) O1 Mn1 Cl1 . 4_456 91.29(7) O2 Mn1 Cl1 4_456 4_456 90.87(6) O1 Mn1 Cl1 . . 88.00(7) O2 Mn1 Cl1 4_456 . 89.83(7) Cl1 Mn1 Cl1 4_456 . 179.03(3) O1 Mn1 Cl2 . . 90.39(7) O2 Mn1 Cl2 4_456 . 89.99(7) Cl1 Mn1 Cl2 4_456 . 94.43(3) Cl1 Mn1 Cl2 . . 86.23(3) O1 Mn1 Cl2 . 4_456 88.84(7) O2 Mn1 Cl2 4_456 4_456 90.75(7) Cl1 Mn1 Cl2 4_456 4_456 86.13(3) Cl1 Mn1 Cl2 . 4_456 93.19(3) Cl2 Mn1 Cl2 . 4_456 179.06(3) Mn1 Cl1 Mn1 4_556 . 88.80(2) Mn1 Cl2 Mn1 . 4_556 87.37(2) C1 O1 Mn1 . . 133.0(2) C1 O2 Mn1 . 4_556 127.6(2) O1 C1 O2 . . 126.7(3) O1 C1 C2 . . 118.1(3) O2 C1 C2 . . 115.2(3) N1 C2 C3 . . 103.4(3) N1 C2 C1 . . 108.7(3) C3 C2 C1 . . 111.5(3) N1 C2 H2 . . 111.0 C3 C2 H2 . . 111.0 C1 C2 H2 . . 111.0 C4 C3 C2 . . 103.7(3) 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 C3 C4 C5 . . 104.6(3) C3 C4 H4A . . 110.8 C5 C4 H4A . . 110.8 C3 C4 H4B . . 110.8 C5 C4 H4B . . 110.8 H4A C4 H4B . . 108.9 N1 C5 C4 . . 104.9(3) N1 C5 H5A . . 110.8 C4 C5 H5A . . 110.8 N1 C5 H5B . . 110.8 C4 C5 H5B . . 110.8 H5A C5 H5B . . 108.8 C2 N1 C5 . . 108.6(3) C2 N1 H1A . . 116(3) C5 N1 H1A . . 102(3) C2 N1 H1B . . 110(2) C5 N1 H1B . . 111(2) H1A N1 H1B . . 109(3) H1O O3 H2O . . 106(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 O1 . 2.133(2) Mn1 O2 4_456 2.148(2) Mn1 Cl1 4_456 2.5231(9) Mn1 Cl1 . 2.5414(10) Mn1 Cl2 . 2.5536(9) Mn1 Cl2 4_456 2.5764(9) Cl1 Mn1 4_556 2.5231(9) Cl2 Mn1 4_556 2.5764(9) O1 C1 . 1.234(4) O2 C1 . 1.266(4) O2 Mn1 4_556 2.148(2) C1 C2 . 1.523(4) C2 N1 . 1.509(4) C2 C3 . 1.517(5) C2 H2 . 1.0000 C3 C4 . 1.517(6) C3 H3A . 0.9900 C3 H3B . 0.9900 C4 C5 . 1.518(5) C4 H4A . 0.9900 C4 H4B . 0.9900 C5 N1 . 1.514(5) C5 H5A . 0.9900 C5 H5B . 0.9900 N1 H1A . 0.906(18) N1 H1B . 0.906(18) O3 H1O . 0.878(19) O3 H2O . 0.890(18) _cod_database_fobs_code 2105292 _journal_paper_doi 10.1107/S0108768112043996