#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/18/7001818.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7001818
loop_
_publ_author_name
'Liu, Gao-Feng'
'Dürr, Katharina'
'Puchta, Ralph'
'Heinemann, Frank W.'
'van Eldik, Rudi'
'Ivanović-Burmazović, Ivana'
_publ_section_title
;
 Chelate electronic properties control the redox behaviour and
 superoxide reactivity of seven-coordinate manganese(II) complexes
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              6292
_journal_page_last               6295
_journal_paper_doi               10.1039/b906100m
_journal_year                    2009
_chemical_formula_moiety         'C19 H23 Mn N7 O2, 2(Cl O4)'
_chemical_formula_sum            'C19 H23 Cl2 Mn N7 O10'
_chemical_formula_weight         635.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.613(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9947(6)
_cell_length_b                   31.380(4)
_cell_length_c                   7.9492(6)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     2599.1(4)
_computing_cell_refinement       'EVALCCD (Bruker-Nonius, 2002)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Bruker-Nonius, 2002)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
φ- and ω-rotations with 2.0 ° and 40 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            31490
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0331
_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)+(0.0346P)²+3.0702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                2482
_reflns_number_total             3105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906100m.txt
_cod_data_source_block           ii0301
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7001818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 1.0000 0.138676(12) 0.2500 0.00904(11) Uani 1 2 d S . .
N1 N 1.0000 0.06496(7) 0.2500 0.0124(5) Uani 1 2 d S . .
N2 N 0.79425(14) 0.11025(5) 0.13769(19) 0.0108(3) Uani 1 1 d . . .
N3 N 0.69640(15) 0.13858(5) 0.0832(2) 0.0128(3) Uani 1 1 d . . .
H3N H 0.623(2) 0.1312(7) 0.040(3) 0.015 Uiso 1 1 d . . .
N4 N 0.84339(14) 0.19033(5) 0.2279(2) 0.0116(3) Uani 1 1 d . . .
O1 O 1.01808(14) 0.14486(5) 0.53460(18) 0.0163(3) Uani 1 1 d . . .
H1A H 1.067(2) 0.1299(7) 0.616(3) 0.020 Uiso 1 1 d . . .
H1B H 0.953(2) 0.1430(7) 0.553(3) 0.020 Uiso 1 1 d . . .
C3 C 1.0000 -0.02280(10) 0.2500 0.0439(11) Uani 1 2 d S . .
H3 H 1.0000 -0.0542(13) 0.2500 0.053 Uiso 1 2 d S . .
C4 C 0.8863(2) -0.00085(7) 0.1766(4) 0.0303(6) Uani 1 1 d . . .
H4 H 0.812(3) -0.0146(8) 0.124(3) 0.036 Uiso 1 1 d . . .
C5 C 0.88920(17) 0.04338(6) 0.1789(3) 0.0152(4) Uani 1 1 d . . .
C6 C 0.77287(17) 0.06997(6) 0.1086(2) 0.0127(4) Uani 1 1 d . . .
C7 C 0.72095(17) 0.18003(6) 0.1434(2) 0.0115(4) Uani 1 1 d . . .
C8 C 0.6186(2) 0.20876(6) 0.1171(3) 0.0166(4) Uani 1 1 d . . .
H8 H 0.536(2) 0.1997(7) 0.056(3) 0.020 Uiso 1 1 d . . .
C9 C 0.6463(2) 0.24930(6) 0.1841(3) 0.0195(4) Uani 1 1 d . . .
H9 H 0.584(2) 0.2691(7) 0.169(3) 0.023 Uiso 1 1 d . . .
C10 C 0.7723(2) 0.26042(7) 0.2778(3) 0.0191(4) Uani 1 1 d . . .
H10 H 0.794(2) 0.2871(7) 0.325(3) 0.023 Uiso 1 1 d . . .
C11 C 0.86588(19) 0.23018(6) 0.2964(3) 0.0156(4) Uani 1 1 d . . .
H11 H 0.953(2) 0.2364(7) 0.359(3) 0.019 Uiso 1 1 d . . .
C13 C 0.64338(19) 0.05141(7) 0.0160(3) 0.0196(4) Uani 1 1 d . . .
H13A H 0.602(2) 0.0657(8) -0.092(3) 0.029 Uiso 1 1 d . . .
H13B H 0.649(2) 0.0221(8) -0.005(3) 0.029 Uiso 1 1 d . . .
H13C H 0.586(2) 0.0557(8) 0.082(3) 0.029 Uiso 1 1 d . . .
Cl1 Cl 0.69552(4) 0.111538(14) -0.42303(6) 0.01169(11) Uani 1 1 d . . .
O11 O 0.65709(14) 0.07866(5) -0.55430(18) 0.0238(3) Uani 1 1 d . . .
O12 O 0.58622(13) 0.12833(5) -0.38235(19) 0.0219(3) Uani 1 1 d . . .
O13 O 0.78657(13) 0.09422(4) -0.26279(18) 0.0211(3) Uani 1 1 d . . .
O14 O 0.75783(14) 0.14595(4) -0.4853(2) 0.0235(3) Uani 1 1 d . . .
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.065
-1 0 0 0.110
0 1 0 0.135
0 -1 0 0.110
0 0 1 0.155
0 0 -1 0.120
-2 -3 0 0.085
3 -4 0 0.022
0 -3 -1 0.082
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 169.95(8) . 2_755 ?
O1 Mn1 N1 95.02(4) . . ?
O1 Mn1 N1 95.02(4) 2_755 . ?
O1 Mn1 N2 100.64(5) . . ?
O1 Mn1 N2 83.25(5) 2_755 . ?
N1 Mn1 N2 67.47(4) . . ?
O1 Mn1 N2 83.25(5) . 2_755 ?
O1 Mn1 N2 100.64(5) 2_755 2_755 ?
N1 Mn1 N2 67.47(4) . 2_755 ?
N2 Mn1 N2 134.95(7) . 2_755 ?
O1 Mn1 N4 92.22(5) . 2_755 ?
O1 Mn1 N4 80.76(5) 2_755 2_755 ?
N1 Mn1 N4 134.07(4) . 2_755 ?
N2 Mn1 N4 154.10(5) . 2_755 ?
N2 Mn1 N4 68.49(5) 2_755 2_755 ?
O1 Mn1 N4 80.76(5) . . ?
O1 Mn1 N4 92.22(5) 2_755 . ?
N1 Mn1 N4 134.07(4) . . ?
N2 Mn1 N4 68.49(5) . . ?
N2 Mn1 N4 154.10(5) 2_755 . ?
N4 Mn1 N4 91.85(7) 2_755 . ?
C5 N1 C5 119.8(2) . 2_755 ?
C5 N1 Mn1 120.11(11) . . ?
C5 N1 Mn1 120.11(11) 2_755 . ?
C6 N2 N3 120.23(15) . . ?
C6 N2 Mn1 122.82(12) . . ?
N3 N2 Mn1 116.50(11) . . ?
N2 N3 C7 117.32(15) . . ?
N2 N3 H3N 122.2(16) . . ?
C7 N3 H3N 118.6(15) . . ?
C7 N4 C11 116.75(16) . . ?
C7 N4 Mn1 118.07(12) . . ?
C11 N4 Mn1 125.17(13) . . ?
Mn1 O1 H1A 124.2(15) . . ?
Mn1 O1 H1B 113.6(17) . . ?
H1A O1 H1B 102(2) . . ?
C4 C3 C4 120.2(3) 2_755 . ?
C4 C3 H3 119.88(15) 2_755 . ?
C4 C3 H3 119.88(15) . . ?
C3 C4 C5 118.6(2) . . ?
C3 C4 H4 121.5(16) . . ?
C5 C4 H4 119.9(16) . . ?
N1 C5 C4 121.39(18) . . ?
N1 C5 C6 115.53(16) . . ?
C4 C5 C6 123.07(17) . . ?
N2 C6 C5 113.45(16) . . ?
N2 C6 C13 123.97(17) . . ?
C5 C6 C13 122.57(16) . . ?
N4 C7 N3 117.07(16) . . ?
N4 C7 C8 123.33(17) . . ?
N3 C7 C8 119.59(17) . . ?
C9 C8 C7 117.91(19) . . ?
C9 C8 H8 123.2(14) . . ?
C7 C8 H8 118.9(14) . . ?
C8 C9 C10 119.94(19) . . ?
C8 C9 H9 121.3(14) . . ?
C10 C9 H9 118.7(14) . . ?
C11 C10 C9 117.91(19) . . ?
C11 C10 H10 120.0(14) . . ?
C9 C10 H10 122.1(14) . . ?
N4 C11 C10 124.09(18) . . ?
N4 C11 H11 115.1(13) . . ?
C10 C11 H11 120.8(13) . . ?
C6 C13 H13A 111.5(14) . . ?
C6 C13 H13B 111.4(15) . . ?
H13A C13 H13B 110(2) . . ?
C6 C13 H13C 111.7(14) . . ?
H13A C13 H13C 103(2) . . ?
H13B C13 H13C 109(2) . . ?
O11 Cl1 O12 110.72(9) . . ?
O11 Cl1 O14 110.49(9) . . ?
O12 Cl1 O14 108.88(9) . . ?
O11 Cl1 O13 109.29(9) . . ?
O12 Cl1 O13 109.34(9) . . ?
O14 Cl1 O13 108.07(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.2155(14) . ?
Mn1 O1 2.2155(14) 2_755 ?
Mn1 N1 2.313(2) . ?
Mn1 N2 2.3282(15) . ?
Mn1 N2 2.3282(15) 2_755 ?
Mn1 N4 2.3302(15) 2_755 ?
Mn1 N4 2.3302(15) . ?
N1 C5 1.350(2) . ?
N1 C5 1.350(2) 2_755 ?
N2 C6 1.293(2) . ?
N2 N3 1.356(2) . ?
N3 C7 1.382(2) . ?
N3 H3N 0.80(2) . ?
N4 C7 1.338(2) . ?
N4 C11 1.355(2) . ?
O1 H1A 0.84(2) . ?
O1 H1B 0.77(2) . ?
C3 C4 1.383(3) 2_755 ?
C3 C4 1.383(3) . ?
C3 H3 0.98(4) . ?
C4 C5 1.388(3) . ?
C4 H4 0.90(3) . ?
C5 C6 1.479(3) . ?
C6 C13 1.496(3) . ?
C7 C8 1.405(3) . ?
C8 C9 1.375(3) . ?
C8 H8 0.92(2) . ?
C9 C10 1.392(3) . ?
C9 H9 0.90(2) . ?
C10 C11 1.373(3) . ?
C10 H10 0.92(2) . ?
C11 H11 0.95(2) . ?
C13 H13A 0.94(2) . ?
C13 H13B 0.94(2) . ?
C13 H13C 0.96(2) . ?
Cl1 O11 1.4319(14) . ?
Cl1 O12 1.4403(14) . ?
Cl1 O14 1.4479(14) . ?
Cl1 O13 1.4512(14) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O13 0.84(2) 2.00(2) 2.818(2) 164(2) 2_755
O1 H1B O14 0.77(2) 2.08(2) 2.815(2) 160(2) 1_556
N3 H3N O12 0.80(2) 2.24(2) 3.023(2) 164(2) 2_654
