#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/10/2221033.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_2221033
loop_
_publ_author_name
'Hwang, In-Chul'
'Kim, Nam-Ho'
'Ha, Kwang'
_publ_section_title
'[μ-N,N,N',N'-Tetrakis(2-pyridylmethyl)hexane-1,6-diamine]bis[dichloridomanganese(II)]'
_journal_coeditor_code           CS2107
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m249
_journal_paper_doi               10.1107/S1600536809003663
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn2 Cl4 (C30 H36 N6)]'
_chemical_formula_moiety         'C30 H36 Cl4 Mn2 N6'
_chemical_formula_sum            'C30 H36 Cl4 Mn2 N6'
_chemical_formula_weight         732.33
_chemical_name_systematic
;[μ-N,N,N',N'-Tetrakis(2-pyridylmethyl)hexane-1,6-
diamine]bis[dichloridomanganese(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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.309(3)
_cell_angle_beta                 88.329(3)
_cell_angle_gamma                66.666(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7149(13)
_cell_length_b                   8.4660(14)
_cell_length_c                   14.263(2)
_cell_measurement_reflns_used    886
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.64
_cell_volume                     849.4(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4845
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0427
_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)+(0.0564P)²+0.3638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                2705
_reflns_number_total             3368
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cs2107.cif
_cod_data_source_block           I
_cod_database_code               2221033
_cod_database_fobs_code          2221033
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_disorder_assembly
_atom_site_disorder_group
Mn Mn1 1.04002(6) 0.18359(5) 0.26548(3) 0.04078(16) Uani d . 1 . .
Cl Cl1 1.23775(14) -0.01680(11) 0.38692(7) 0.0661(3) Uani d . 1 . .
Cl Cl2 1.19512(14) 0.26409(14) 0.13691(7) 0.0677(3) Uani d . 1 . .
N N1 0.9580(4) 0.4267(3) 0.33551(19) 0.0477(6) Uani d . 1 . .
N N2 0.9371(3) 0.0059(3) 0.20318(19) 0.0456(6) Uani d . 1 . .
N N3 0.7153(3) 0.2854(3) 0.29208(17) 0.0410(6) Uani d . 1 . .
C C1 1.0607(6) 0.5221(5) 0.3353(3) 0.0633(10) Uani d . 1 . .
H H1 1.1711 0.4909 0.3008 0.076 Uiso calc R 1 . .
C C2 1.0105(8) 0.6646(5) 0.3840(3) 0.0790(14) Uani d . 1 . .
H H2 1.0868 0.7264 0.3839 0.095 Uiso calc R 1 . .
C C3 0.8461(8) 0.7127(5) 0.4324(3) 0.0820(15) Uani d . 1 . .
H H3 0.8101 0.8069 0.4670 0.098 Uiso calc R 1 . .
C C4 0.7338(7) 0.6216(5) 0.4298(2) 0.0715(12) Uani d . 1 . .
H H4 0.6178 0.6571 0.4595 0.086 Uiso calc R 1 . .
C C5 0.7963(5) 0.4759(4) 0.3822(2) 0.0504(8) Uani d . 1 . .
C C6 0.6920(5) 0.3593(4) 0.3819(2) 0.0532(8) Uani d . 1 . .
H H6A 0.7393 0.2665 0.4332 0.064 Uiso calc R 1 . .
H H6B 0.5589 0.4247 0.3919 0.064 Uiso calc R 1 . .
C C7 1.0319(5) -0.0980(5) 0.1386(3) 0.0601(9) Uani d . 1 . .
H H7 1.1506 -0.1024 0.1210 0.072 Uiso calc R 1 . .
C C8 0.9591(6) -0.1979(5) 0.0977(3) 0.0752(11) Uani d . 1 . .
H H8 1.0272 -0.2683 0.0527 0.090 Uiso calc R 1 . .
C C9 0.7868(6) -0.1926(5) 0.1237(3) 0.0767(12) Uani d . 1 . .
H H9 0.7360 -0.2601 0.0967 0.092 Uiso calc R 1 . .
C C10 0.6872(5) -0.0877(5) 0.1898(3) 0.0634(10) Uani d . 1 . .
H H10 0.5691 -0.0834 0.2086 0.076 Uiso calc R 1 . .
C C11 0.7668(4) 0.0118(4) 0.2281(2) 0.0464(7) Uani d . 1 . .
C C12 0.6656(5) 0.1324(4) 0.2993(2) 0.0527(8) Uani d . 1 . .
H H12A 0.5305 0.1708 0.2896 0.063 Uiso calc R 1 . .
H H12B 0.6977 0.0708 0.3622 0.063 Uiso calc R 1 . .
C C13 0.5988(4) 0.4236(4) 0.2181(2) 0.0469(7) Uani d . 1 . .
H H13A 0.6265 0.5251 0.2209 0.056 Uiso calc R 1 . .
H H13B 0.4667 0.4551 0.2332 0.056 Uiso calc R 1 . .
C C14 0.6265(4) 0.3777(4) 0.1184(2) 0.0465(7) Uani d . 1 . .
H H14A 0.6050 0.2731 0.1151 0.056 Uiso calc R 1 . .
H H14B 0.7557 0.3547 0.1005 0.056 Uiso calc R 1 . .
C C15 0.4928(5) 0.5226(4) 0.0496(2) 0.0497(8) Uani d . 1 . .
H H15A 0.3642 0.5508 0.0705 0.060 Uiso calc R 1 . .
H H15B 0.5200 0.6249 0.0505 0.060 Uiso calc R 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'
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'
N N 0.0061 0.0033 '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
N2 Mn1 N1 . . 145.81(10) ?
N2 Mn1 N3 . . 73.58(9) ?
N1 Mn1 N3 . . 72.37(9) ?
N2 Mn1 Cl2 . . 101.15(8) ?
N1 Mn1 Cl2 . . 97.35(8) ?
N3 Mn1 Cl2 . . 128.09(6) ?
N2 Mn1 Cl1 . . 98.49(7) ?
N1 Mn1 Cl1 . . 98.94(7) ?
N3 Mn1 Cl1 . . 116.01(7) ?
Cl2 Mn1 Cl1 . . 115.84(4) ?
C5 N1 C1 . . 118.3(3) ?
C5 N1 Mn1 . . 116.8(2) ?
C1 N1 Mn1 . . 124.9(3) ?
C11 N2 C7 . . 118.7(3) ?
C11 N2 Mn1 . . 117.6(2) ?
C7 N2 Mn1 . . 123.6(2) ?
C6 N3 C12 . . 112.0(2) ?
C6 N3 C13 . . 108.5(2) ?
C12 N3 C13 . . 111.5(2) ?
C6 N3 Mn1 . . 104.43(18) ?
C12 N3 Mn1 . . 106.39(18) ?
C13 N3 Mn1 . . 113.75(18) ?
N1 C1 C2 . . 122.9(4) ?
N1 C1 H1 . . 118.5 ?
C2 C1 H1 . . 118.5 ?
C3 C2 C1 . . 118.3(4) ?
C3 C2 H2 . . 120.8 ?
C1 C2 H2 . . 120.8 ?
C2 C3 C4 . . 119.8(4) ?
C2 C3 H3 . . 120.1 ?
C4 C3 H3 . . 120.1 ?
C3 C4 C5 . . 118.8(4) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
N1 C5 C4 . . 121.8(4) ?
N1 C5 C6 . . 115.2(3) ?
C4 C5 C6 . . 123.0(4) ?
N3 C6 C5 . . 111.0(3) ?
N3 C6 H6A . . 109.4 ?
C5 C6 H6A . . 109.4 ?
N3 C6 H6B . . 109.4 ?
C5 C6 H6B . . 109.4 ?
H6A C6 H6B . . 108.0 ?
N2 C7 C8 . . 122.0(4) ?
N2 C7 H7 . . 119.0 ?
C8 C7 H7 . . 119.0 ?
C9 C8 C7 . . 119.1(4) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 120.0(4) ?
C8 C9 H9 . . 120.0 ?
C10 C9 H9 . . 120.0 ?
C9 C10 C11 . . 118.4(4) ?
C9 C10 H10 . . 120.8 ?
C11 C10 H10 . . 120.8 ?
N2 C11 C10 . . 121.8(3) ?
N2 C11 C12 . . 116.5(3) ?
C10 C11 C12 . . 121.7(3) ?
N3 C12 C11 . . 111.9(3) ?
N3 C12 H12A . . 109.2 ?
C11 C12 H12A . . 109.2 ?
N3 C12 H12B . . 109.2 ?
C11 C12 H12B . . 109.2 ?
H12A C12 H12B . . 107.9 ?
N3 C13 C14 . . 115.8(3) ?
N3 C13 H13A . . 108.3 ?
C14 C13 H13A . . 108.3 ?
N3 C13 H13B . . 108.3 ?
C14 C13 H13B . . 108.3 ?
H13A C13 H13B . . 107.4 ?
C13 C14 C15 . . 111.5(3) ?
C13 C14 H14A . . 109.3 ?
C15 C14 H14A . . 109.3 ?
C13 C14 H14B . . 109.3 ?
C15 C14 H14B . . 109.3 ?
H14A C14 H14B . . 108.0 ?
C15 C15 C14 2_665 . 113.2(3) ?
C15 C15 H15A 2_665 . 108.9 ?
C14 C15 H15A . . 108.9 ?
C15 C15 H15B 2_665 . 108.9 ?
C14 C15 H15B . . 108.9 ?
H15A C15 H15B . . 107.8 ?
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
Mn1 N2 . 2.232(2) ?
Mn1 N1 . 2.246(3) ?
Mn1 N3 . 2.339(2) ?
Mn1 Cl2 . 2.3422(10) ?
Mn1 Cl1 . 2.3716(9) ?
N1 C5 . 1.334(4) ?
N1 C1 . 1.337(4) ?
N2 C11 . 1.334(4) ?
N2 C7 . 1.340(4) ?
N3 C6 . 1.465(4) ?
N3 C12 . 1.482(4) ?
N3 C13 . 1.492(4) ?
C1 C2 . 1.377(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.362(7) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.372(6) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.386(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.501(5) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.372(5) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.355(6) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.372(6) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.386(5) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.499(5) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C13 C14 . 1.504(4) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 C15 . 1.519(4) ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C15 C15 2_665 1.499(6) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N2 Mn1 N1 C5 . . . . 25.2(3) ?
N3 Mn1 N1 C5 . . . . 19.9(2) ?
Cl2 Mn1 N1 C5 . . . . 147.7(2) ?
Cl1 Mn1 N1 C5 . . . . -94.6(2) ?
N2 Mn1 N1 C1 . . . . -156.3(2) ?
N3 Mn1 N1 C1 . . . . -161.6(3) ?
Cl2 Mn1 N1 C1 . . . . -33.9(3) ?
Cl1 Mn1 N1 C1 . . . . 83.9(3) ?
N1 Mn1 N2 C11 . . . . -20.5(3) ?
N3 Mn1 N2 C11 . . . . -15.3(2) ?
Cl2 Mn1 N2 C11 . . . . -142.0(2) ?
Cl1 Mn1 N2 C11 . . . . 99.5(2) ?
N1 Mn1 N2 C7 . . . . 155.5(2) ?
N3 Mn1 N2 C7 . . . . 160.7(3) ?
Cl2 Mn1 N2 C7 . . . . 34.0(3) ?
Cl1 Mn1 N2 C7 . . . . -84.5(3) ?
N2 Mn1 N3 C6 . . . . 147.77(19) ?
N1 Mn1 N3 C6 . . . . -35.30(18) ?
Cl2 Mn1 N3 C6 . . . . -120.79(17) ?
Cl1 Mn1 N3 C6 . . . . 56.21(19) ?
N2 Mn1 N3 C12 . . . . 29.15(19) ?
N1 Mn1 N3 C12 . . . . -153.9(2) ?
Cl2 Mn1 N3 C12 . . . . 120.59(18) ?
Cl1 Mn1 N3 C12 . . . . -62.4(2) ?
N2 Mn1 N3 C13 . . . . -94.1(2) ?
N1 Mn1 N3 C13 . . . . 82.9(2) ?
Cl2 Mn1 N3 C13 . . . . -2.6(2) ?
Cl1 Mn1 N3 C13 . . . . 174.37(18) ?
C5 N1 C1 C2 . . . . 2.5(5) ?
Mn1 N1 C1 C2 . . . . -176.0(3) ?
N1 C1 C2 C3 . . . . -1.8(5) ?
C1 C2 C3 C4 . . . . -1.4(6) ?
C2 C3 C4 C5 . . . . 3.7(5) ?
C1 N1 C5 C4 . . . . 0.0(4) ?
Mn1 N1 C5 C4 . . . . 178.6(2) ?
C1 N1 C5 C6 . . . . -178.1(3) ?
Mn1 N1 C5 C6 . . . . 0.5(3) ?
C3 C4 C5 N1 . . . . -3.1(5) ?
C3 C4 C5 C6 . . . . 174.9(3) ?
C12 N3 C6 C5 . . . . 162.7(3) ?
C13 N3 C6 C5 . . . . -73.7(3) ?
Mn1 N3 C6 C5 . . . . 47.9(3) ?
N1 C5 C6 N3 . . . . -34.7(4) ?
C4 C5 C6 N3 . . . . 147.2(3) ?
C11 N2 C7 C8 . . . . -0.1(5) ?
Mn1 N2 C7 C8 . . . . -176.0(3) ?
N2 C7 C8 C9 . . . . -0.5(6) ?
C7 C8 C9 C10 . . . . 0.3(7) ?
C8 C9 C10 C11 . . . . 0.4(6) ?
C7 N2 C11 C10 . . . . 0.8(5) ?
Mn1 N2 C11 C10 . . . . 177.0(2) ?
C7 N2 C11 C12 . . . . -178.9(3) ?
Mn1 N2 C11 C12 . . . . -2.7(3) ?
C9 C10 C11 N2 . . . . -0.9(5) ?
C9 C10 C11 C12 . . . . 178.8(3) ?
C6 N3 C12 C11 . . . . -154.0(3) ?
C13 N3 C12 C11 . . . . 84.1(3) ?
Mn1 N3 C12 C11 . . . . -40.4(3) ?
N2 C11 C12 N3 . . . . 30.8(4) ?
C10 C11 C12 N3 . . . . -148.9(3) ?
C6 N3 C13 C14 . . . . 171.8(3) ?
C12 N3 C13 C14 . . . . -64.3(3) ?
Mn1 N3 C13 C14 . . . . 56.0(3) ?
N3 C13 C14 C15 . . . . 176.4(2) ?
C13 C14 C15 C15 . . . 2_665 -176.3(3) ?
