#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/69/2206928.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_2206928
loop_
_publ_author_name
'Seewald, Oliver'
'Flörke, Ulrich'
'Henkel, Gerald'
_publ_section_title
Di-μ-bromo-bis{bromo[N-(8-quinolyl)-o-phenylenediamine-κ³N,N',N'']manganese(II)}
_journal_coeditor_code           CV6571
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1948
_journal_page_last               m1950
_journal_paper_doi               10.1107/S1600536805027716
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Mn2 Br4 (C15 H13 N3)2]'
_chemical_formula_moiety         'C30 H26 Br4 Mn2 N6'
_chemical_formula_sum            'C30 H26 Br4 Mn2 N6'
_chemical_formula_weight         900.09
_chemical_name_systematic
;
Di-μ-bromo-bis{bromo[N-(8-quinolyl)-o-phenylenediamine-
κ³N,N',N'']manganese(II)}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.055(2)
_cell_angle_beta                 110.397(2)
_cell_angle_gamma                97.351(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8833(7)
_cell_length_b                   9.8725(8)
_cell_length_c                   9.9162(8)
_cell_measurement_reflns_used    2034
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.5
_cell_volume                     773.45(11)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2002)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10807
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  360
_diffrn_standards_number         2052
_exptl_absorpt_coefficient_mu    6.014
_exptl_absorpt_correction_T_max  0.6447
_exptl_absorpt_correction_T_min  0.3792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0281P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                3167
_reflns_number_total             3837
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv6571.cif
_cod_data_source_block           I
_cod_database_code               2206928
_cod_database_fobs_code          2206928
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_type_symbol
Br1 0.28160(3) 0.01963(3) 0.90887(3) 0.01656(8) Uani d . 1 Br
Br2 0.59253(4) 0.36823(3) 1.17982(3) 0.02113(9) Uani d . 1 Br
Mn1 0.58697(5) 0.16284(5) 0.95876(5) 0.01370(11) Uani d . 1 Mn
N1 0.8275(3) 0.2578(3) 0.9531(3) 0.0144(5) Uani d . 1 N
N2 0.5193(3) 0.2896(3) 0.7812(3) 0.0151(5) Uani d . 1 N
H2 0.4825 0.3682 0.8183 0.018 Uiso calc R 1 H
N3 0.5192(3) 0.0058(3) 0.7201(3) 0.0171(5) Uani d . 1 N
H3B 0.6089 0.0116 0.6938 0.020 Uiso calc R 1 H
H3C 0.4854 -0.0867 0.7189 0.020 Uiso calc R 1 H
C1 0.9749(4) 0.2481(3) 1.0410(4) 0.0199(7) Uani d . 1 C
H1A 0.9813 0.2026 1.1170 0.024 Uiso calc R 1 H
C2 1.1225(4) 0.3014(3) 1.0284(4) 0.0203(7) Uani d . 1 C
H2A 1.2253 0.2935 1.0955 0.024 Uiso calc R 1 H
C3 1.1154(4) 0.3640(3) 0.9190(4) 0.0214(7) Uani d . 1 C
H3A 1.2138 0.4001 0.9084 0.026 Uiso calc R 1 H
C4 0.9613(4) 0.3757(3) 0.8202(3) 0.0171(6) Uani d . 1 C
C5 0.9439(4) 0.4379(3) 0.7020(4) 0.0229(7) Uani d . 1 C
H5A 1.0385 0.4731 0.6853 0.027 Uiso calc R 1 H
C6 0.7920(4) 0.4478(3) 0.6117(4) 0.0242(7) Uani d . 1 C
H6A 0.7813 0.4882 0.5314 0.029 Uiso calc R 1 H
C7 0.6505(4) 0.3985(3) 0.6368(3) 0.0206(7) Uani d . 1 C
H7A 0.5456 0.4069 0.5739 0.025 Uiso calc R 1 H
C8 0.6631(4) 0.3386(3) 0.7508(3) 0.0162(6) Uani d . 1 C
C9 0.8193(4) 0.3236(3) 0.8437(3) 0.0146(6) Uani d . 1 C
C10 0.3854(4) 0.1929(3) 0.6496(3) 0.0158(6) Uani d . 1 C
C11 0.2542(4) 0.2383(3) 0.5623(3) 0.0197(7) Uani d . 1 C
H11A 0.2521 0.3366 0.5861 0.024 Uiso calc R 1 H
C12 0.1252(4) 0.1406(4) 0.4398(4) 0.0241(7) Uani d . 1 C
H12A 0.0356 0.1721 0.3795 0.029 Uiso calc R 1 H
C13 0.1283(4) -0.0022(4) 0.4063(3) 0.0232(7) Uani d . 1 C
H13A 0.0412 -0.0691 0.3220 0.028 Uiso calc R 1 H
C14 0.2580(4) -0.0485(3) 0.4954(3) 0.0205(7) Uani d . 1 C
H14A 0.2583 -0.1472 0.4727 0.025 Uiso calc R 1 H
C15 0.3876(4) 0.0486(3) 0.6176(3) 0.0153(6) Uani d . 1 C
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'
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
_geom_angle_publ_flag
Mn1 Br1 Mn1 2_657 . 89.813(17) y
N1 Mn1 N2 . . 74.48(9) y
N1 Mn1 N3 . . 88.69(9) ?
N2 Mn1 N3 . . 71.32(9) ?
N1 Mn1 Br2 . . 97.31(6) ?
N2 Mn1 Br2 . . 94.96(6) ?
N3 Mn1 Br2 . . 163.06(6) ?
N1 Mn1 Br1 . 2_657 91.66(6) ?
N2 Mn1 Br1 . 2_657 158.02(6) ?
N3 Mn1 Br1 . 2_657 91.77(6) ?
Br2 Mn1 Br1 . 2_657 103.815(19) ?
N1 Mn1 Br1 . . 168.82(6) ?
N2 Mn1 Br1 . . 100.28(6) ?
N3 Mn1 Br1 . . 80.22(6) ?
Br2 Mn1 Br1 . . 92.953(17) ?
Br1 Mn1 Br1 2_657 . 90.187(17) y
C1 N1 C9 . . 117.7(3) ?
C1 N1 Mn1 . . 125.3(2) ?
C9 N1 Mn1 . . 116.86(19) ?
C10 N2 C8 . . 113.0(2) ?
C10 N2 Mn1 . . 105.78(17) ?
C8 N2 Mn1 . . 110.55(18) ?
C10 N2 H2 . . 109.1 ?
C8 N2 H2 . . 109.1 ?
Mn1 N2 H2 . . 109.1 ?
C15 N3 Mn1 . . 106.36(17) ?
C15 N3 H3B . . 110.5 ?
Mn1 N3 H3B . . 110.5 ?
C15 N3 H3C . . 110.5 ?
Mn1 N3 H3C . . 110.5 ?
H3B N3 H3C . . 108.6 ?
N1 C1 C2 . . 123.8(3) ?
N1 C1 H1A . . 118.1 ?
C2 C1 H1A . . 118.1 ?
C3 C2 C1 . . 118.9(3) ?
C3 C2 H2A . . 120.6 ?
C1 C2 H2A . . 120.6 ?
C2 C3 C4 . . 119.9(3) ?
C2 C3 H3A . . 120.0 ?
C4 C3 H3A . . 120.0 ?
C5 C4 C9 . . 119.2(3) ?
C5 C4 C3 . . 123.2(3) ?
C9 C4 C3 . . 117.6(3) ?
C6 C5 C4 . . 120.4(3) ?
C6 C5 H5A . . 119.8 ?
C4 C5 H5A . . 119.8 ?
C5 C6 C7 . . 120.5(3) ?
C5 C6 H6A . . 119.8 ?
C7 C6 H6A . . 119.8 ?
C8 C7 C6 . . 120.6(3) ?
C8 C7 H7A . . 119.7 ?
C6 C7 H7A . . 119.7 ?
C7 C8 C9 . . 119.9(3) ?
C7 C8 N2 . . 121.7(3) ?
C9 C8 N2 . . 118.4(3) ?
N1 C9 C4 . . 122.0(3) ?
N1 C9 C8 . . 118.7(3) ?
C4 C9 C8 . . 119.4(3) ?
C11 C10 C15 . . 120.2(3) ?
C11 C10 N2 . . 122.3(3) ?
C15 C10 N2 . . 117.3(3) ?
C10 C11 C12 . . 120.3(3) ?
C10 C11 H11A . . 119.8 ?
C12 C11 H11A . . 119.8 ?
C13 C12 C11 . . 119.6(3) ?
C13 C12 H12A . . 120.2 ?
C11 C12 H12A . . 120.2 ?
C12 C13 C14 . . 120.3(3) ?
C12 C13 H13A . . 119.9 ?
C14 C13 H13A . . 119.9 ?
C13 C14 C15 . . 120.4(3) ?
C13 C14 H14A . . 119.8 ?
C15 C14 H14A . . 119.8 ?
C14 C15 C10 . . 119.1(3) ?
C14 C15 N3 . . 122.9(3) ?
C10 C15 N3 . . 117.8(3) ?
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
Br1 Mn1 2_657 2.6210(5) y
Br1 Mn1 . 2.7147(6) y
Br2 Mn1 . 2.6096(6) y
Mn1 N1 . 2.245(2) y
Mn1 N2 . 2.340(2) y
Mn1 N3 . 2.340(2) y
Mn1 Br1 2_657 2.6211(5) ?
N1 C1 . 1.326(4) y
N1 C9 . 1.372(4) y
N2 C10 . 1.448(4) y
N2 C8 . 1.460(4) y
N2 H2 . 0.9300 ?
N3 C15 . 1.439(4) y
N3 H3B . 0.9200 ?
N3 H3C . 0.9200 ?
C1 C2 . 1.407(4) ?
C1 H1A . 0.9500 ?
C2 C3 . 1.352(5) ?
C2 H2A . 0.9500 ?
C3 C4 . 1.416(4) ?
C3 H3A . 0.9500 ?
C4 C5 . 1.414(4) ?
C4 C9 . 1.414(4) ?
C5 C6 . 1.365(5) ?
C5 H5A . 0.9500 ?
C6 C7 . 1.413(4) ?
C6 H6A . 0.9500 ?
C7 C8 . 1.368(4) ?
C7 H7A . 0.9500 ?
C8 C9 . 1.421(4) ?
C10 C11 . 1.383(4) ?
C10 C15 . 1.392(4) ?
C11 C12 . 1.391(4) ?
C11 H11A . 0.9500 ?
C12 C13 . 1.379(5) ?
C12 H12A . 0.9500 ?
C13 C14 . 1.387(4) ?
C13 H13A . 0.9500 ?
C14 C15 . 1.390(4) ?
C14 H14A . 0.9500 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
Mn1 Br1 Mn1 N1 2_657 . 99.6(3)
Mn1 Br1 Mn1 N2 2_657 . 160.57(6)
Mn1 Br1 Mn1 N3 2_657 . 91.76(6)
Mn1 Br1 Mn1 Br2 2_657 . -103.843(19)
Mn1 Br1 Mn1 Br1 2_657 2_657 0.0
N2 Mn1 N1 C1 . . 176.4(3)
N3 Mn1 N1 C1 . . -112.6(2)
Br2 Mn1 N1 C1 . . 83.3(2)
Br1 Mn1 N1 C1 2_657 . -20.9(2)
Br1 Mn1 N1 C1 . . -120.3(3)
N2 Mn1 N1 C9 . . -7.71(19)
N3 Mn1 N1 C9 . . 63.3(2)
Br2 Mn1 N1 C9 . . -100.9(2)
Br1 Mn1 N1 C9 2_657 . 154.99(19)
Br1 Mn1 N1 C9 . . 55.6(5)
N1 Mn1 N2 C10 . . 131.21(19)
N3 Mn1 N2 C10 . . 37.26(17)
Br2 Mn1 N2 C10 . . -132.57(17)
Br1 Mn1 N2 C10 2_657 . 78.6(2)
Br1 Mn1 N2 C10 . . -38.65(18)
N1 Mn1 N2 C8 . . 8.54(18)
N3 Mn1 N2 C8 . . -85.41(19)
Br2 Mn1 N2 C8 . . 104.77(17)
Br1 Mn1 N2 C8 2_657 . -44.1(3)
Br1 Mn1 N2 C8 . . -161.32(17)
N1 Mn1 N3 C15 . . -110.51(19)
N2 Mn1 N3 C15 . . -36.46(17)
Br2 Mn1 N3 C15 . . 0.7(4)
Br1 Mn1 N3 C15 2_657 . 157.87(17)
Br1 Mn1 N3 C15 . . 67.98(17)
C9 N1 C1 C2 . . 0.1(5)
Mn1 N1 C1 C2 . . 175.9(2)
N1 C1 C2 C3 . . -1.3(5)
C1 C2 C3 C4 . . 0.3(5)
C2 C3 C4 C5 . . -179.1(3)
C2 C3 C4 C9 . . 1.7(4)
C9 C4 C5 C6 . . 0.1(5)
C3 C4 C5 C6 . . -179.1(3)
C4 C5 C6 C7 . . 1.2(5)
C5 C6 C7 C8 . . -0.7(5)
C6 C7 C8 C9 . . -1.0(5)
C6 C7 C8 N2 . . 178.7(3)
C10 N2 C8 C7 . . 52.8(4)
Mn1 N2 C8 C7 . . 171.1(2)
C10 N2 C8 C9 . . -127.5(3)
Mn1 N2 C8 C9 . . -9.2(3)
C1 N1 C9 C4 . . 2.1(4)
Mn1 N1 C9 C4 . . -174.1(2)
C1 N1 C9 C8 . . -178.3(3)
Mn1 N1 C9 C8 . . 5.5(3)
C5 C4 C9 N1 . . 177.8(3)
C3 C4 C9 N1 . . -3.0(4)
C5 C4 C9 C8 . . -1.8(4)
C3 C4 C9 C8 . . 177.5(3)
C7 C8 C9 N1 . . -177.3(3)
N2 C8 C9 N1 . . 3.0(4)
C7 C8 C9 C4 . . 2.3(4)
N2 C8 C9 C4 . . -177.4(2)
C8 N2 C10 C11 . . -97.4(3)
Mn1 N2 C10 C11 . . 141.5(3)
C8 N2 C10 C15 . . 86.2(3)
Mn1 N2 C10 C15 . . -34.8(3)
C15 C10 C11 C12 . . -1.5(5)
N2 C10 C11 C12 . . -177.7(3)
C10 C11 C12 C13 . . 0.5(5)
C11 C12 C13 C14 . . 0.8(5)
C12 C13 C14 C15 . . -1.1(5)
C13 C14 C15 C10 . . 0.1(4)
C13 C14 C15 N3 . . 175.4(3)
C11 C10 C15 C14 . . 1.2(4)
N2 C10 C15 C14 . . 177.6(3)
C11 C10 C15 N3 . . -174.3(3)
N2 C10 C15 N3 . . 2.1(4)
Mn1 N3 C15 C14 . . -143.5(2)
Mn1 N3 C15 C10 . . 31.9(3)
