#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018721.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_2018721
loop_
_publ_author_name
'Lennartson, Anders'
'McKenzie, Christine J.'
_publ_section_title
;
 Oxidation of a dinuclear manganese(II) complex to an oxide-bridged
 dimanganese(IV) complex
;
_journal_coeditor_code           QS3017
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m347
_journal_page_last               m352
_journal_paper_doi               10.1107/S0108270112043296
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Mn2 (C15 H16 N3 O2)2 (H2 O)2] (C F3 O3 S)2, 2H2 O'
_chemical_formula_moiety
'C30 H36 Mn2 N6 O6 2+, 2(C F3 O3 S -), 2(H2 O)'
_chemical_formula_sum            'C32 H40 F6 Mn2 N6 O14 S2'
_chemical_formula_weight         1020.70
_chemical_name_systematic
;
bis{μ-3-[bis(pyridin-2-ylmethyl)amino]propionato}bis[aquamanganese(II)]
bis(trifluoromethandsulfonate) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.599(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9179(5)
_cell_length_b                   21.7212(16)
_cell_length_c                   12.2638(10)
_cell_measurement_reflns_used    5179
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.82
_cell_volume                     2041.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker--Nonius X8 APEXII CCD'
_diffrn_measurement_method       'thin-slice ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29597
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         3.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.7908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.341
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0343
_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/[σ²(Fo²)+(0.0291P)²+0.7004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                3184
_reflns_number_total             4696
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3017.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018721
_cod_database_fobs_code          2018721
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
C C1 0.6935(2) 0.06429(9) 0.45627(17) 0.0136(4) Uani d . 1 1
C C2 0.6966(2) 0.13147(9) 0.42674(18) 0.0156(5) Uani d . 1 1
H H2A 0.7586 0.1361 0.3683 0.019 Uiso calc R 1 1
H H2B 0.7613 0.1538 0.4926 0.019 Uiso calc R 1 1
C C3 0.5173(2) 0.16022(9) 0.38627(17) 0.0154(5) Uani d . 1 1
H H3A 0.5307 0.2027 0.3655 0.018 Uiso calc R 1 1
H H3B 0.4536 0.1387 0.3192 0.018 Uiso calc R 1 1
C C4 0.5039(3) 0.19149(9) 0.57475(17) 0.0160(5) Uani d . 1 1
H H4A 0.4180 0.2124 0.6056 0.019 Uiso calc R 1 1
H H4B 0.5796 0.2226 0.5556 0.019 Uiso calc R 1 1
C C5 0.6112(2) 0.14963(9) 0.66334(17) 0.0144(5) Uani d . 1 1
C C6 0.7596(3) 0.17055(10) 0.74051(18) 0.0196(5) Uani d . 1 1
H H6 0.8028 0.2097 0.7332 0.024 Uiso calc R 1 1
C C7 0.8423(3) 0.13312(10) 0.82773(19) 0.0241(5) Uani d . 1 1
H H7 0.9415 0.1466 0.8804 0.029 Uiso calc R 1 1
C C8 0.7758(3) 0.07500(10) 0.83614(19) 0.0230(5) Uani d . 1 1
H H8 0.8270 0.0492 0.8958 0.028 Uiso calc R 1 1
C C9 0.6317(3) 0.05615(10) 0.75394(17) 0.0191(5) Uani d . 1 1
H H9 0.5894 0.0165 0.7582 0.023 Uiso calc R 1 1
C C10 0.2421(2) 0.18744(9) 0.42243(18) 0.0176(5) Uani d . 1 1
H H10A 0.2594 0.2264 0.3882 0.021 Uiso calc R 1 1
H H10B 0.1848 0.1958 0.4821 0.021 Uiso calc R 1 1
C C11 0.1272(2) 0.14717(9) 0.33573(18) 0.0165(5) Uani d . 1 1
C C12 0.0047(3) 0.17189(10) 0.24521(18) 0.0216(5) Uani d . 1 1
H H12 -0.0032 0.2143 0.2349 0.026 Uiso calc R 1 1
C C13 -0.1055(3) 0.13332(11) 0.17038(19) 0.0255(5) Uani d . 1 1
H H13 -0.1879 0.1492 0.1089 0.031 Uiso calc R 1 1
C C14 -0.0911(3) 0.07051(10) 0.18860(19) 0.0228(5) Uani d . 1 1
H H14 -0.1635 0.0433 0.1397 0.027 Uiso calc R 1 1
C C15 0.0332(3) 0.04905(10) 0.28101(18) 0.0198(5) Uani d . 1 1
H H15 0.0420 0.0068 0.2934 0.024 Uiso calc R 1 1
C C16 0.3595(3) 0.10044(11) 1.0197(2) 0.0287(6) Uani d . 1 1
N N1 0.41334(19) 0.15861(7) 0.47129(14) 0.0130(4) Uani d . 1 1
N N2 0.5498(2) 0.09236(7) 0.66820(14) 0.0143(4) Uani d . 1 1
N N3 0.1415(2) 0.08613(8) 0.35358(14) 0.0152(4) Uani d . 1 1
O O1 0.55054(16) 0.03474(6) 0.42178(12) 0.0162(3) Uani d . 1 1
O O2 0.82717(17) 0.03757(6) 0.51188(12) 0.0199(3) Uani d . 1 1
O O3 0.15174(17) 0.08339(6) 0.60611(12) 0.0193(3) Uani d . 1 1
H H1W 0.1521 0.1200 0.6389 0.029 Uiso d R 1 1
H H2W 0.0565 0.0739 0.5752 0.029 Uiso d R 1 1
O O4 0.17489(18) 0.19971(7) 0.69684(12) 0.0247(4) Uani d . 1 1
H H3W 0.1975 0.2011 0.7675 0.037 Uiso d R 1 1
H H4W 0.1107 0.2256 0.6790 0.037 Uiso d R 1 1
O O5 0.23022(18) 0.20226(7) 0.93272(12) 0.0255(4) Uani d . 1 1
O O6 0.54039(19) 0.18538(7) 0.95694(14) 0.0300(4) Uani d . 1 1
O O7 0.4254(2) 0.20506(7) 1.11884(13) 0.0339(4) Uani d . 1 1
Mn Mn1 0.34090(4) 0.058037(14) 0.51424(3) 0.01289(9) Uani d . 1 1
S S1 0.39402(6) 0.18248(2) 1.00521(5) 0.01773(13) Uani d . 1 1
F F1 0.3244(2) 0.07258(7) 0.92048(15) 0.0560(5) Uani d . 1 1
F F2 0.22492(18) 0.08939(6) 1.06360(14) 0.0462(4) Uani d . 1 1
F F3 0.49740(19) 0.07349(7) 1.08566(16) 0.0645(6) Uani 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
O2 C1 O1 . . 120.39(18) ?
O2 C1 C2 . . 121.25(18) ?
O1 C1 C2 . . 118.35(17) ?
C1 C2 C3 . . 114.03(16) ?
C1 C2 H2A . . 108.7 ?
C3 C2 H2A . . 108.7 ?
C1 C2 H2B . . 108.7 ?
C3 C2 H2B . . 108.7 ?
H2A C2 H2B . . 107.6 ?
N1 C3 C2 . . 113.60(16) ?
N1 C3 H3A . . 108.8 ?
C2 C3 H3A . . 108.8 ?
N1 C3 H3B . . 108.8 ?
C2 C3 H3B . . 108.8 ?
H3A C3 H3B . . 107.7 ?
N1 C4 C5 . . 113.09(16) ?
N1 C4 H4A . . 109.0 ?
C5 C4 H4A . . 109.0 ?
N1 C4 H4B . . 109.0 ?
C5 C4 H4B . . 109.0 ?
H4A C4 H4B . . 107.8 ?
N2 C5 C6 . . 121.83(19) ?
N2 C5 C4 . . 116.58(16) ?
C6 C5 C4 . . 121.46(18) ?
C7 C6 C5 . . 119.6(2) ?
C7 C6 H6 . . 120.2 ?
C5 C6 H6 . . 120.2 ?
C6 C7 C8 . . 118.96(19) ?
C6 C7 H7 . . 120.5 ?
C8 C7 H7 . . 120.5 ?
C9 C8 C7 . . 118.5(2) ?
C9 C8 H8 . . 120.8 ?
C7 C8 H8 . . 120.8 ?
N2 C9 C8 . . 123.0(2) ?
N2 C9 H9 . . 118.5 ?
C8 C9 H9 . . 118.5 ?
N1 C10 C11 . . 111.85(16) ?
N1 C10 H10A . . 109.2 ?
C11 C10 H10A . . 109.2 ?
N1 C10 H10B . . 109.2 ?
C11 C10 H10B . . 109.2 ?
H10A C10 H10B . . 107.9 ?
N3 C11 C12 . . 121.74(19) ?
N3 C11 C10 . . 116.77(17) ?
C12 C11 C10 . . 121.38(19) ?
C13 C12 C11 . . 119.7(2) ?
C13 C12 H12 . . 120.1 ?
C11 C12 H12 . . 120.1 ?
C12 C13 C14 . . 118.6(2) ?
C12 C13 H13 . . 120.7 ?
C14 C13 H13 . . 120.7 ?
C15 C14 C13 . . 118.6(2) ?
C15 C14 H14 . . 120.7 ?
C13 C14 H14 . . 120.7 ?
N3 C15 C14 . . 123.2(2) ?
N3 C15 H15 . . 118.4 ?
C14 C15 H15 . . 118.4 ?
F3 C16 F1 . . 108.0(2) ?
F3 C16 F2 . . 107.2(2) ?
F1 C16 F2 . . 106.59(19) ?
F3 C16 S1 . . 111.88(16) ?
F1 C16 S1 . . 111.07(17) ?
F2 C16 S1 . . 111.83(16) ?
C4 N1 C10 . . 109.97(15) ?
C4 N1 C3 . . 110.96(15) ?
C10 N1 C3 . . 108.70(15) ?
C4 N1 Mn1 . . 110.50(12) ?
C10 N1 Mn1 . . 103.52(11) ?
C3 N1 Mn1 . . 112.92(11) ?
C9 N2 C5 . . 117.99(17) ?
C9 N2 Mn1 . . 123.98(13) ?
C5 N2 Mn1 . . 117.25(13) ?
C15 N3 C11 . . 118.16(18) ?
C15 N3 Mn1 . . 127.07(14) ?
C11 N3 Mn1 . . 114.65(13) ?
C1 O1 Mn1 . 3_656 96.08(12) ?
C1 O1 Mn1 . . 114.66(12) ?
Mn1 O1 Mn1 3_656 . 106.60(6) ?
C1 O2 Mn1 . 3_656 87.98(11) ?
Mn1 O3 H1W . . 122.6 ?
Mn1 O3 H2W . . 113.0 ?
H1W O3 H2W . . 110.3 ?
H3W O4 H4W . . 103.1 ?
O3 Mn1 O1 . 3_656 107.47(5) y
O3 Mn1 N3 . . 87.84(6) y
O1 Mn1 N3 3_656 . 131.45(6) y
O3 Mn1 O1 . . 177.18(5) y
O1 Mn1 O1 3_656 . 73.40(6) y
N3 Mn1 O1 . . 93.55(5) y
O3 Mn1 N2 . . 86.50(6) y
O1 Mn1 N2 3_656 . 82.62(5) y
N3 Mn1 N2 . . 145.37(6) y
O1 Mn1 N2 . . 90.97(5) y
O3 Mn1 N1 . . 96.91(5) y
O1 Mn1 N1 3_656 . 144.66(5) y
N3 Mn1 N1 . . 73.27(6) y
O1 Mn1 N1 . . 81.16(5) y
N2 Mn1 N1 . . 73.56(6) y
O3 Mn1 O2 . 3_656 81.88(5) y
O1 Mn1 O2 3_656 3_656 55.45(5) ?
N3 Mn1 O2 . 3_656 83.01(5) y
O1 Mn1 O2 . 3_656 100.72(5) y
N2 Mn1 O2 . 3_656 129.70(6) y
N1 Mn1 O2 . 3_656 156.28(5) y
O6 S1 O7 . . 115.23(10) ?
O6 S1 O5 . . 115.42(10) ?
O7 S1 O5 . . 113.87(10) ?
O6 S1 C16 . . 103.97(10) ?
O7 S1 C16 . . 103.45(11) ?
O5 S1 C16 . . 102.61(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O2 . 1.249(2) ?
C1 O1 . 1.277(2) ?
C1 C2 . 1.505(3) ?
C2 C3 . 1.515(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 N1 . 1.483(2) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 N1 . 1.475(2) ?
C4 C5 . 1.504(3) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 N2 . 1.342(2) ?
C5 C6 . 1.387(3) ?
C6 C7 . 1.371(3) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.381(3) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.381(3) ?
C8 H8 . 0.9300 ?
C9 N2 . 1.342(3) ?
C9 H9 . 0.9300 ?
C10 N1 . 1.477(2) ?
C10 C11 . 1.495(3) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 N3 . 1.344(3) ?
C11 C12 . 1.385(3) ?
C12 C13 . 1.379(3) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.383(3) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.381(3) ?
C14 H14 . 0.9300 ?
C15 N3 . 1.338(3) ?
C15 H15 . 0.9300 ?
C16 F3 . 1.321(3) ?
C16 F1 . 1.325(3) ?
C16 F2 . 1.331(3) ?
C16 S1 . 1.819(2) ?
N1 Mn1 . 2.3519(16) y
N2 Mn1 . 2.2985(16) y
N3 Mn1 . 2.2758(16) y
O1 Mn1 3_656 2.2529(14) ?
O1 Mn1 . 2.2904(13) y
O2 Mn1 3_656 2.4436(14) y
O3 Mn1 . 2.1603(13) y
O3 H1W . 0.8910 ?
O3 H2W . 0.7819 ?
O4 H3W . 0.8400 ?
O4 H4W . 0.7521 ?
O5 S1 . 1.4407(14) ?
O6 S1 . 1.4294(15) ?
O7 S1 . 1.4387(16) ?
Mn1 O1 3_656 2.2528(14) ?
Mn1 O2 3_656 2.4436(14) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1W O4 1_555 0.891 1.863 2.747 172.26
O3 H2W O2 1_455 0.782 1.952 2.726 170.62
O4 H3W O5 1_555 0.840 1.977 2.815 175.20
O4 H4W O7 4_565 0.752 2.103 2.854 176.20
