#------------------------------------------------------------------------------ #$Date: 2013-01-18 10:50:04 +0000 (Fri, 18 Jan 2013) $ #$Revision: 71144 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/52/2105296.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_2105296 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 'C10 H22 Br2 Mn N2 O6' _chemical_formula_sum 'C10 H22 Br2 Mn N2 O6' _chemical_formula_weight 481.06 _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 106.904(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.3156(12) _cell_length_b 9.1319(12) _cell_length_c 10.0593(13) _cell_measurement_reflns_used 1326 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 22.44 _cell_measurement_theta_min 3.08 _cell_volume 818.76(18) _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 0.933 _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 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 12113 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 30.93 _diffrn_reflns_theta_min 3.08 _exptl_absorpt_coefficient_mu 5.712 _exptl_absorpt_correction_T_max 0.8037 _exptl_absorpt_correction_T_min 0.5019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 478 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.901 _refine_diff_density_min -0.660 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 2421 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0456 _refine_ls_shift/su_max 0.000 _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^+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.0884 _reflns_number_gt 1997 _reflns_number_total 2421 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 2b in P2(1)/c CELL 0.71073 9.3156 9.1319 10.0593 90.000 106.904 90.000 ZERR 2.00 0.0012 0.0012 0.0013 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O MN BR UNIT 20 44 4 12 2 4 TEMP -173.000 L.S. 10 SIZE .04 .08 .14 BOND BOND $H ACTA 50 FMAP 2 PLAN -20 WGHT 0.020000 3.000000 FVAR 0.21168 DFIX 0.92 H1A N1 H1B N1 MOLE 1 MN1 5 0.000000 0.500000 0.500000 10.50000 0.01984 0.01201 = 0.01101 0.00000 0.00316 -0.00330 BR1 6 0.212557 0.319593 0.448674 11.00000 0.02297 0.01310 = 0.01791 -0.00005 0.00207 0.00010 SADI O3 H1O O3 H2O O3 4 0.063266 0.439961 0.717306 11.00000 0.03527 0.01206 = 0.01394 0.00136 0.00101 0.00062 H1O 2 0.102423 0.370667 0.757725 11.00000 0.03069 H2O 2 0.089536 0.502589 0.771159 11.00000 0.07115 O1 4 0.155924 0.679743 0.567485 11.00000 0.02144 0.01373 = 0.02107 0.00300 0.00123 -0.00284 O2 4 0.123765 0.834443 0.389213 11.00000 0.04583 0.01752 = 0.01303 0.00168 0.00612 0.00214 C1 1 0.161299 0.803957 0.515751 11.00000 0.01784 0.01420 = 0.01623 -0.00124 0.00746 0.00143 C2 1 0.227297 0.929459 0.614070 11.00000 0.01923 0.01657 = 0.01427 0.00021 0.00468 -0.00077 AFIX 13 H2 2 0.163013 1.018594 0.587251 11.00000 -1.20000 AFIX 0 C3 1 0.388195 0.963421 0.610889 11.00000 0.02538 0.03003 = 0.02246 0.00146 0.01100 -0.00776 AFIX 23 H3A 2 0.429808 0.880735 0.570212 11.00000 -1.20000 H3B 2 0.390291 1.052800 0.555788 11.00000 -1.20000 AFIX 0 C4 1 0.476389 0.986118 0.762135 11.00000 0.02374 0.03868 = 0.03645 0.00409 0.00651 -0.00812 AFIX 23 H4A 2 0.463499 1.086831 0.793251 11.00000 -1.20000 H4B 2 0.584568 0.966555 0.777747 11.00000 -1.20000 AFIX 0 C5 1 0.406342 0.874143 0.835597 11.00000 0.02471 0.03507 = 0.02053 0.00892 0.00213 -0.00094 AFIX 23 H5A 2 0.442073 0.774001 0.824751 11.00000 -1.20000 H5B 2 0.428439 0.896865 0.935765 11.00000 -1.20000 AFIX 0 N1 3 0.242927 0.890203 0.762163 11.00000 0.02346 0.01774 = 0.01415 -0.00065 0.00790 -0.00139 H1A 2 0.201926 0.962481 0.803461 11.00000 -1.20000 H1B 2 0.193578 0.803812 0.766250 11.00000 -1.20000 HKLF 4 REM 2b in P2(1)/c REM R1 = 0.0457 for 1997 Fo > 4sig(Fo) and 0.0606 for all 2421 data REM 105 parameters refined using 1 restraints END WGHT 0.0237 1.8909 REM Highest difference peak 0.900, deepest hole -0.658, 1-sigma level 0.139 Q1 1 0.4675 0.8893 0.7153 11.00000 0.05 0.90 Q2 1 -0.1255 0.6748 0.5644 11.00000 0.05 0.84 Q3 1 0.3265 0.8190 0.7826 11.00000 0.05 0.66 Q4 1 0.2333 1.0294 0.6611 11.00000 0.05 0.66 Q5 1 0.5805 0.8649 0.6197 11.00000 0.05 0.63 Q6 1 0.3119 0.3220 0.4634 11.00000 0.05 0.62 Q7 1 0.2036 0.8908 0.4191 11.00000 0.05 0.60 Q8 1 -0.1790 0.6247 0.6178 11.00000 0.05 0.60 Q9 1 -0.1612 0.5177 0.6155 11.00000 0.05 0.56 Q10 1 0.1736 0.6811 0.5074 11.00000 0.05 0.54 ; _[local]_cod_data_source_file gp5056.cif _[local]_cod_data_source_block 2b _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2105296 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 0.01456(17) Uani d S 1 2 Br Br1 0.21256(4) 0.31959(4) 0.44867(4) 0.01881(11) Uani d . 1 1 O O3 0.0633(4) 0.4400(3) 0.7173(3) 0.0217(6) Uani d D 1 1 H H1O 0.103(5) 0.371(5) 0.757(5) 0.031(14) Uiso d D 1 1 H H2O 0.090(7) 0.502(6) 0.771(6) 0.07(2) Uiso d D 1 1 O O1 0.1559(3) 0.6797(3) 0.5675(3) 0.0198(6) Uani d . 1 1 O O2 0.1237(4) 0.8344(3) 0.3892(3) 0.0260(7) Uani d . 1 1 C C1 0.1613(4) 0.8040(4) 0.5158(4) 0.0155(7) Uani d . 1 1 C C2 0.2273(4) 0.9295(4) 0.6141(4) 0.0167(7) Uani d . 1 1 H H2 0.1630 1.0186 0.5873 0.020 Uiso calc R 1 1 C C3 0.3882(5) 0.9634(5) 0.6109(4) 0.0251(9) Uani d . 1 1 H H3A 0.4298 0.8807 0.5702 0.030 Uiso calc R 1 1 H H3B 0.3903 1.0528 0.5558 0.030 Uiso calc R 1 1 C C4 0.4764(5) 0.9861(6) 0.7621(5) 0.0334(11) Uani d . 1 1 H H4A 0.5846 0.9666 0.7778 0.040 Uiso calc R 1 1 H H4B 0.4635 1.0869 0.7933 0.040 Uiso calc R 1 1 C C5 0.4064(5) 0.8742(5) 0.8356(4) 0.0277(9) Uani d . 1 1 H H5A 0.4422 0.7740 0.8248 0.033 Uiso calc R 1 1 H H5B 0.4284 0.8969 0.9357 0.033 Uiso calc R 1 1 N N1 0.2429(4) 0.8901(4) 0.7621(3) 0.0179(7) Uani d D 1 1 H H1A 0.212(5) 0.970(3) 0.802(4) 0.022 Uiso d D 1 1 H H1B 0.188(4) 0.810(3) 0.770(5) 0.022 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 0.0198(4) 0.0120(4) 0.0110(4) -0.0033(3) 0.0032(3) 0.0000(3) Br1 0.0230(2) 0.01310(17) 0.01790(18) 0.00011(15) 0.00207(14) -0.00006(15) O3 0.0352(18) 0.0120(13) 0.0140(14) 0.0007(12) 0.0010(12) 0.0013(11) O1 0.0215(14) 0.0137(12) 0.0210(13) -0.0028(11) 0.0013(11) 0.0030(11) O2 0.0458(19) 0.0175(14) 0.0130(13) 0.0022(13) 0.0061(12) 0.0017(11) C1 0.0178(18) 0.0142(17) 0.0162(17) 0.0014(14) 0.0075(14) -0.0012(13) C2 0.0192(19) 0.0165(17) 0.0142(17) -0.0008(14) 0.0047(14) 0.0002(14) C3 0.025(2) 0.030(2) 0.022(2) -0.0077(18) 0.0110(17) 0.0015(17) C4 0.024(2) 0.039(3) 0.036(3) -0.008(2) 0.0065(19) 0.004(2) C5 0.025(2) 0.035(2) 0.021(2) -0.0010(19) 0.0021(17) 0.0088(18) N1 0.0236(18) 0.0176(16) 0.0142(15) -0.0018(13) 0.0079(13) -0.0006(12) 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 O3 Mn1 O3 . 3_566 180.0 O3 Mn1 O1 . 3_566 94.90(11) O3 Mn1 O1 3_566 3_566 85.10(11) O3 Mn1 O1 . . 85.09(11) O3 Mn1 O1 3_566 . 94.90(11) O1 Mn1 O1 3_566 . 180.0 O3 Mn1 Br1 . 3_566 87.79(8) O3 Mn1 Br1 3_566 3_566 92.21(8) O1 Mn1 Br1 3_566 3_566 93.40(8) O1 Mn1 Br1 . 3_566 86.60(8) O3 Mn1 Br1 . . 92.21(8) O3 Mn1 Br1 3_566 . 87.79(8) O1 Mn1 Br1 3_566 . 86.60(8) O1 Mn1 Br1 . . 93.40(8) Br1 Mn1 Br1 3_566 . 180.0 Mn1 O3 H1O . . 132(4) Mn1 O3 H2O . . 117(5) H1O O3 H2O . . 103(6) C1 O1 Mn1 . . 131.2(2) O2 C1 O1 . . 126.2(3) O2 C1 C2 . . 115.8(3) O1 C1 C2 . . 117.9(3) N1 C2 C1 . . 111.7(3) N1 C2 C3 . . 104.8(3) C1 C2 C3 . . 110.5(3) N1 C2 H2 . . 109.9 C1 C2 H2 . . 109.9 C3 C2 H2 . . 109.9 C4 C3 C2 . . 104.6(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 C5 C4 C3 . . 102.2(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 N1 C5 C4 . . 102.4(3) 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 . . 107.8(3) C5 N1 H1A . . 106(3) C2 N1 H1A . . 107(3) C5 N1 H1B . . 114(3) C2 N1 H1B . . 113(3) H1A N1 H1B . . 110(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mn1 O3 . 2.162(3) Mn1 O3 3_566 2.162(3) Mn1 O1 3_566 2.166(3) Mn1 O1 . 2.166(3) Mn1 Br1 3_566 2.7379(5) Mn1 Br1 . 2.7379(5) O3 H1O . 0.78(4) O3 H2O . 0.77(4) O1 C1 . 1.255(4) O2 C1 . 1.249(4) C1 C2 . 1.522(5) C2 N1 . 1.498(5) C2 C3 . 1.540(5) C2 H2 . 1.0000 C3 C4 . 1.519(6) C3 H3A . 0.9900 C3 H3B . 0.9900 C4 C5 . 1.516(6) C4 H4A . 0.9900 C4 H4B . 0.9900 C5 N1 . 1.494(5) C5 H5A . 0.9900 C5 H5B . 0.9900 N1 H1A . 0.922(19) N1 H1B . 0.913(19)