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#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$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 MnX₂ 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 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/[σ²(Fo²)+(0.0200P)²+3.0000P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            gp5056.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105296
_cod_database_fobs_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_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)
