#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/51/2215141.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_2215141
loop_
_publ_author_name
'Hwang, In-Chul'
'Ha, Kwang'
_publ_section_title
;catena-Poly[[manganese(II)-μ-[N,N,N',N'-tetrakis(2-pyridylmethyl)hexane-1,6-diamine]]
 bis(perchlorate) acetone disolvate dihydrate]
;
_journal_coeditor_code           HG2266
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2302
_journal_page_last               m2302
_journal_paper_doi               10.1107/S1600536807038603
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Mn (C30 H36 N6)] (Cl O4)2, 2C3 H6 O, 2H2 O'
_chemical_formula_moiety
'C30 H36 Mn N6 2+, 2(Cl O4 -), 2(C3 H6 O), 2(H2 O)'
_chemical_formula_sum            'C36 H52 Cl2 Mn N6 O12'
_chemical_formula_weight         886.68
_chemical_name_systematic
;
catena-Poly[[manganese(II)-μ-[N,N,N',N'-tetrakis(2-pyridylmethyl)hexane-
1,6-diamine]] diperchlorate acetone disolvate dihydrate]
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.782(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7266(16)
_cell_length_b                   14.5252(12)
_cell_length_c                   15.2375(13)
_cell_measurement_reflns_used    2085
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      20.981
_cell_measurement_theta_min      2.171
_cell_volume                     4130.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16555
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.489
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0729
_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)+(0.132P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2271
_reflns_number_gt                2171
_reflns_number_total             4248
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg2266.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2215141
_cod_database_fobs_code          2215141
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_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
Mn Mn 0.0000 0.26386(6) 0.2500 0.0436(3) Uani d S 1
N N1 0.0765(2) 0.2265(2) 0.1478(2) 0.0488(10) Uani d . 1
N N2 0.0500(2) 0.3736(2) 0.3356(3) 0.0509(10) Uani d . 1
N N3 0.1019(2) 0.1940(3) 0.3248(2) 0.0523(10) Uani d . 1
C C1 0.0736(3) 0.2587(3) 0.0651(3) 0.0508(12) Uani d . 1
H H1 0.0380 0.3022 0.0478 0.061 Uiso calc R 1
C C2 0.1189(3) 0.2322(4) 0.0046(3) 0.0588(13) Uani d . 1
H H2 0.1138 0.2562 -0.0529 0.071 Uiso calc R 1
C C3 0.1713(3) 0.1710(4) 0.0281(3) 0.0688(15) Uani d . 1
H H3 0.2030 0.1514 -0.0128 0.083 Uiso calc R 1
C C4 0.1773(3) 0.1378(4) 0.1134(4) 0.0661(15) Uani d . 1
H H4 0.2139 0.0961 0.1318 0.079 Uiso calc R 1
C C5 0.1285(3) 0.1670(3) 0.1715(3) 0.0547(13) Uani d . 1
C C6 0.1313(3) 0.1281(3) 0.2638(3) 0.0637(15) Uani d . 1
H H6A 0.1037 0.0707 0.2633 0.076 Uiso calc R 1
H H6B 0.1811 0.1138 0.2843 0.076 Uiso calc R 1
C C7 0.0191(3) 0.4531(3) 0.3588(3) 0.0620(14) Uani d . 1
H H7 -0.0277 0.4657 0.3345 0.074 Uiso calc R 1
C C8 0.0512(4) 0.5154(4) 0.4146(4) 0.0718(16) Uani d . 1
H H8 0.0276 0.5700 0.4285 0.086 Uiso calc R 1
C C9 0.1186(4) 0.4969(4) 0.4502(4) 0.087(2) Uani d . 1
H H9 0.1423 0.5393 0.4891 0.104 Uiso calc R 1
C C10 0.1522(3) 0.4176(5) 0.4301(4) 0.0754(17) Uani d . 1
H H10 0.1986 0.4045 0.4556 0.090 Uiso calc R 1
C C11 0.1176(3) 0.3571(3) 0.3721(3) 0.0551(13) Uani d . 1
C C12 0.1520(3) 0.2711(4) 0.3387(4) 0.0605(13) Uani d . 1
H H12A 0.1722 0.2853 0.2829 0.073 Uiso calc R 1
H H12B 0.1915 0.2525 0.3811 0.073 Uiso calc R 1
C C13 0.0935(3) 0.1483(4) 0.4109(3) 0.0632(14) Uani d . 1
H H13A 0.1411 0.1307 0.4369 0.076 Uiso calc R 1
H H13B 0.0741 0.1936 0.4503 0.076 Uiso calc R 1
C C14 0.0467(3) 0.0653(3) 0.4084(3) 0.0650(15) Uani d . 1
H H14A 0.0723 0.0132 0.3846 0.078 Uiso calc R 1
H H14B 0.0036 0.0768 0.3690 0.078 Uiso calc R 1
C C15 0.0251(3) 0.0406(3) 0.4997(4) 0.0738(17) Uani d . 1
H H15A 0.0685 0.0267 0.5380 0.089 Uiso calc R 1
H H15B 0.0020 0.0941 0.5244 0.089 Uiso calc R 1
Cl Cl 0.23323(9) 0.43776(12) 0.17809(10) 0.0844(6) Uani d . 1
O O1 0.2592(2) 0.4928(3) 0.1128(3) 0.1020(15) Uani d . 1
O O2 0.2566(4) 0.4597(4) 0.2616(3) 0.150(3) Uani d . 1
O O3 0.1583(3) 0.4373(6) 0.1717(5) 0.193(4) Uani d . 1
O O4 0.2472(4) 0.3424(4) 0.1612(4) 0.154(2) Uani d . 1
O O1S 0.4558(3) 0.2153(4) 0.3938(5) 0.139(2) Uiso d . 1
C C1S 0.4137(6) 0.2292(8) 0.3337(8) 0.150(4) Uiso d . 1
C C2S 0.3836(7) 0.1745(10) 0.2604(9) 0.231(6) Uiso d . 1
H H2S1 0.3393 0.2025 0.2358 0.346 Uiso calc R 1
H H2S2 0.3738 0.1128 0.2807 0.346 Uiso calc R 1
H H2S3 0.4174 0.1714 0.2156 0.346 Uiso calc R 1
C C3S 0.3406(7) 0.2371(9) 0.3732(9) 0.302(10) Uiso d . 1
H H3S1 0.3151 0.2906 0.3488 0.453 Uiso calc R 1
H H3S2 0.3482 0.2436 0.4367 0.453 Uiso calc R 1
H H3S3 0.3125 0.1822 0.3591 0.453 Uiso calc R 1
O O1W 0.4390(7) 0.3332(9) 0.2678(9) 0.416(9) Uiso d 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'
O O 0.0106 0.0060 '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
N2 Mn N2 . 2 88.1(2)
N2 Mn N1 . 2 91.59(13)
N2 Mn N1 2 2 108.42(14)
N2 Mn N1 . . 108.42(14)
N2 Mn N1 2 . 91.59(13)
N1 Mn N1 2 . 152.33(19)
N2 Mn N3 . . 74.99(14)
N2 Mn N3 2 . 151.06(14)
N1 Mn N3 2 . 95.57(14)
N1 Mn N3 . . 72.42(13)
N2 Mn N3 . 2 151.06(14)
N2 Mn N3 2 2 74.98(14)
N1 Mn N3 2 2 72.42(13)
N1 Mn N3 . 2 95.57(14)
N3 Mn N3 . 2 129.2(2)
C5 N1 C1 . . 116.9(4)
C5 N1 Mn . . 117.4(3)
C1 N1 Mn . . 125.7(3)
C7 N2 C11 . . 116.6(4)
C7 N2 Mn . . 126.8(4)
C11 N2 Mn . . 116.6(3)
C12 N3 C6 . . 108.7(4)
C12 N3 C13 . . 109.1(4)
C6 N3 C13 . . 109.8(4)
C12 N3 Mn . . 102.8(3)
C6 N3 Mn . . 107.7(3)
C13 N3 Mn . . 118.3(3)
N1 C1 C2 . . 124.1(5)
N1 C1 H1 . . 118.0
C2 C1 H1 . . 118.0
C3 C2 C1 . . 119.2(5)
C3 C2 H2 . . 120.4
C1 C2 H2 . . 120.4
C2 C3 C4 . . 118.7(5)
C2 C3 H3 . . 120.7
C4 C3 H3 . . 120.7
C3 C4 C5 . . 119.1(5)
C3 C4 H4 . . 120.5
C5 C4 H4 . . 120.5
N1 C5 C4 . . 122.1(5)
N1 C5 C6 . . 117.6(4)
C4 C5 C6 . . 120.3(5)
N3 C6 C5 . . 111.0(4)
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
C8 C7 N2 . . 124.1(6)
C8 C7 H7 . . 118.0
N2 C7 H7 . . 118.0
C7 C8 C9 . . 117.9(6)
C7 C8 H8 . . 121.0
C9 C8 H8 . . 121.0
C8 C9 C10 . . 120.7(6)
C8 C9 H9 . . 119.7
C10 C9 H9 . . 119.7
C9 C10 C11 . . 119.0(6)
C9 C10 H10 . . 120.5
C11 C10 H10 . . 120.5
N2 C11 C10 . . 121.7(5)
N2 C11 C12 . . 114.5(4)
C10 C11 C12 . . 123.7(5)
N3 C12 C11 . . 113.2(4)
N3 C12 H12A . . 108.9
C11 C12 H12A . . 108.9
N3 C12 H12B . . 108.9
C11 C12 H12B . . 108.9
H12A C12 H12B . . 107.7
C14 C13 N3 . . 116.3(4)
C14 C13 H13A . . 108.2
N3 C13 H13A . . 108.2
C14 C13 H13B . . 108.2
N3 C13 H13B . . 108.2
H13A C13 H13B . . 107.4
C13 C14 C15 . . 111.6(5)
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 5_556 . 113.7(6)
C15 C15 H15A 5_556 . 108.8
C14 C15 H15A . . 108.8
C15 C15 H15B 5_556 . 108.8
C14 C15 H15B . . 108.8
H15A C15 H15B . . 107.7
O2 Cl O1 . . 115.6(3)
O2 Cl O3 . . 108.1(5)
O1 Cl O3 . . 111.1(4)
O2 Cl O4 . . 110.3(4)
O1 Cl O4 . . 110.2(3)
O3 Cl O4 . . 100.4(5)
O1S C1S C2S . . 134.4(12)
O1S C1S C3S . . 105.5(11)
C2S C1S C3S . . 92.3(9)
C1S C2S H2S1 . . 109.5
C1S C2S H2S2 . . 109.5
H2S1 C2S H2S2 . . 109.5
C1S C2S H2S3 . . 109.5
H2S1 C2S H2S3 . . 109.5
H2S2 C2S H2S3 . . 109.5
C1S C3S H3S1 . . 109.5
C1S C3S H3S2 . . 109.5
H3S1 C3S H3S2 . . 109.5
C1S C3S H3S3 . . 109.5
H3S1 C3S H3S3 . . 109.5
H3S2 C3S H3S3 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn N2 . 2.217(4)
Mn N2 2 2.217(4)
Mn N1 2 2.267(4)
Mn N1 . 2.267(4)
Mn N3 . 2.369(4)
Mn N3 2 2.369(4)
N1 C5 . 1.331(6)
N1 C1 . 1.341(6)
N2 C7 . 1.352(6)
N2 C11 . 1.360(6)
N3 C12 . 1.465(6)
N3 C6 . 1.472(6)
N3 C13 . 1.490(6)
C1 C2 . 1.360(7)
C1 H1 . 0.9400
C2 C3 . 1.350(7)
C2 H2 . 0.9400
C3 C4 . 1.382(7)
C3 H3 . 0.9400
C4 C5 . 1.390(6)
C4 H4 . 0.9400
C5 C6 . 1.513(7)
C6 H6A . 0.9800
C6 H6B . 0.9800
C7 C8 . 1.349(7)
C7 H7 . 0.9400
C8 C9 . 1.359(8)
C8 H8 . 0.9400
C9 C10 . 1.359(9)
C9 H9 . 0.9400
C10 C11 . 1.370(7)
C10 H10 . 0.9400
C11 C12 . 1.514(7)
C12 H12A . 0.9800
C12 H12B . 0.9800
C13 C14 . 1.489(7)
C13 H13A . 0.9800
C13 H13B . 0.9800
C14 C15 . 1.524(7)
C14 H14A . 0.9800
C14 H14B . 0.9800
C15 C15 5_556 1.509(11)
C15 H15A . 0.9800
C15 H15B . 0.9800
Cl O2 . 1.349(5)
Cl O1 . 1.395(4)
Cl O3 . 1.399(6)
Cl O4 . 1.437(6)
O1S C1S . 1.175(11)
C1S C2S . 1.446(15)
C1S C3S . 1.546(15)
C2S H2S1 . 0.9700
C2S H2S2 . 0.9700
C2S H2S3 . 0.9700
C3S H3S1 . 0.9700
C3S H3S2 . 0.9700
C3S H3S3 . 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_4
_geom_torsion
N2 Mn N1 C5 . . 83.1(4)
N2 Mn N1 C5 2 . 171.6(3)
N1 Mn N1 C5 2 . -51.2(3)
N3 Mn N1 C5 . . 16.1(3)
N3 Mn N1 C5 2 . -113.4(3)
N2 Mn N1 C1 . . -97.5(4)
N2 Mn N1 C1 2 . -9.0(4)
N1 Mn N1 C1 2 . 128.2(4)
N3 Mn N1 C1 . . -164.4(4)
N3 Mn N1 C1 2 . 66.1(4)
N2 Mn N2 C7 2 . 40.4(3)
N1 Mn N2 C7 2 . -67.9(4)
N1 Mn N2 C7 . . 131.5(4)
N3 Mn N2 C7 . . -163.3(4)
N3 Mn N2 C7 2 . -13.0(5)
N2 Mn N2 C11 2 . -143.1(4)
N1 Mn N2 C11 2 . 108.5(3)
N1 Mn N2 C11 . . -52.1(3)
N3 Mn N2 C11 . . 13.1(3)
N3 Mn N2 C11 2 . 163.5(3)
N2 Mn N3 C12 . . -30.5(3)
N2 Mn N3 C12 2 . 25.7(4)
N1 Mn N3 C12 2 . -120.7(3)
N1 Mn N3 C12 . . 84.8(3)
N3 Mn N3 C12 2 . 167.5(3)
N2 Mn N3 C6 . . -145.2(3)
N2 Mn N3 C6 2 . -89.0(4)
N1 Mn N3 C6 2 . 124.7(3)
N1 Mn N3 C6 . . -29.8(3)
N3 Mn N3 C6 2 . 52.8(3)
N2 Mn N3 C13 . . 89.7(3)
N2 Mn N3 C13 2 . 145.9(3)
N1 Mn N3 C13 2 . -0.5(4)
N1 Mn N3 C13 . . -155.0(4)
N3 Mn N3 C13 2 . -72.3(3)
C5 N1 C1 C2 . . 1.9(7)
Mn N1 C1 C2 . . -177.6(4)
N1 C1 C2 C3 . . -1.2(8)
C1 C2 C3 C4 . . -0.5(8)
C2 C3 C4 C5 . . 1.3(8)
C1 N1 C5 C4 . . -1.0(7)
Mn N1 C5 C4 . . 178.5(4)
C1 N1 C5 C6 . . -178.4(4)
Mn N1 C5 C6 . . 1.1(6)
C3 C4 C5 N1 . . -0.6(8)
C3 C4 C5 C6 . . 176.8(5)
C12 N3 C6 C5 . . -70.6(5)
C13 N3 C6 C5 . . 170.2(4)
Mn N3 C6 C5 . . 40.1(5)
N1 C5 C6 N3 . . -29.4(7)
C4 C5 C6 N3 . . 153.2(5)
C11 N2 C7 C8 . . 0.3(7)
Mn N2 C7 C8 . . 176.7(4)
N2 C7 C8 C9 . . -0.4(8)
C7 C8 C9 C10 . . -0.3(9)
C8 C9 C10 C11 . . 1.1(9)
C7 N2 C11 C10 . . 0.6(7)
Mn N2 C11 C10 . . -176.2(4)
C7 N2 C11 C12 . . -175.4(4)
Mn N2 C11 C12 . . 7.8(5)
C9 C10 C11 N2 . . -1.2(8)
C9 C10 C11 C12 . . 174.4(5)
C6 N3 C12 C11 . . 159.4(4)
C13 N3 C12 C11 . . -80.9(5)
Mn N3 C12 C11 . . 45.5(4)
N2 C11 C12 N3 . . -38.9(6)
C10 C11 C12 N3 . . 145.2(5)
C12 N3 C13 C14 . . -177.3(4)
C6 N3 C13 C14 . . -58.3(6)
Mn N3 C13 C14 . . 65.8(5)
N3 C13 C14 C15 . . -164.0(4)
C13 C14 C15 C15 . 5_556 177.3(6)
