#------------------------------------------------------------------------------
#$Date: 2016-02-19 15:29:56 +0100 (vie 19 de feb de 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/84/2008452.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_2008452
loop_
_publ_author_name
'Qian, Ming'
'Gou, Shao-Hua'
'He, Ling'
'Zhou, Yu-Ming'
'Duan, Chun-Ying'
_publ_section_title
;[Tris(2-pyridyl-κN-methyleneamino-κN-ethyl)amine-κN]manganese(II)
 diperchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              742
_journal_page_last               744
_journal_paper_doi               10.1107/S0108270198017624
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         '[Mn(C24 H27 N7)](ClO4)2'
_chemical_formula_sum            'C24 H27 Cl2 Mn N7 O8'
_chemical_formula_weight         667.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.068(3)
_cell_length_b                   10.068(3)
_cell_length_c                   16.728(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.24
_cell_volume                     1468.5(8)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2960
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        7.59
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.8000
_exptl_absorpt_correction_T_min  0.7612
_exptl_absorpt_correction_type   'empirical psi-scan  (North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.371
_refine_ls_abs_structure_details 'Flack  (1983)'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1232
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.243
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_obs          .0516
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(Fo^2^)+(0.0467P)^2^] where
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.1267
_refine_ls_wR_factor_obs         .1165
_reflns_number_observed          791
_reflns_number_total             1232
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            da1054.cif
_cod_data_source_block           qm2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P31c '
_cod_database_code               2008452
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mn1 .0491(6) .0491(6) .0371(7) .0246(3) .000 .000
N1 .062(4) .062(4) .045(4) .031(2) .000 .000
N2 .057(4) .092(5) .050(3) .039(3) -.001(3) -.020(3)
N3 .047(3) .047(3) .049(3) .023(2) -.005(2) -.002(2)
C1 .072(5) .100(6) .044(3) .043(5) .006(3) -.012(4)
C2 .072(5) .088(5) .047(3) .040(4) .008(3) -.021(4)
C3 .057(5) .094(6) .062(4) .040(5) -.005(3) -.010(4)
C4 .044(4) .054(4) .049(3) .024(3) .002(3) .003(3)
C5 .070(5) .068(5) .067(4) .040(4) -.010(4) -.002(4)
C6 .061(5) .072(5) .055(4) .028(4) -.017(4) -.009(4)
C7 .069(5) .075(5) .048(3) .031(4) -.013(4) -.019(4)
C8 .056(4) .056(4) .057(4) .020(3) -.010(3) -.019(3)
Cl1 .0715(13) .0715(13) .077(2) .0358(7) .000 .000
O12 .177(9) .177(9) .081(9) .088(4) .000 .000
O11 .113(5) .081(4) .179(7) .046(4) -.027(6) -.043(5)
Cl2 .102(2) .102(2) .0416(13) .0509(8) .000 .000
O22 .126(5) .126(5) .043(5) .063(3) .000 .000
O21 .181(8) .149(8) .117(5) .107(7) -.019(6) -.036(5)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Mn1 .6667 .3333 .02401(7) .0451(4) Uani d S 1 . Mn
N1 .6667 .3333 .1753(5) .056(2) Uani d S 1 . N
N2 .4996(7) .4070(7) .0640(3) .066(2) Uani d . 1 . N
N3 .4514(6) .2214(6) -.0639(3) .0482(12) Uani d . 1 . N
C1 .5392(10) .3537(10) .2019(4) .072(2) Uani d . 1 . C
H1B .5585(10) .3924(10) .2557(4) .086 Uiso d R 1 . H
H1C .4461(10) .2563(10) .2021(4) .086 Uiso d R 1 . H
C2 .5195(9) .4647(9) .1481(4) .069(2) Uani d . 1 . C
H2A .4303(9) .4708(9) .1645(4) .083 Uiso calc R 1 . H
H2B .6090(9) .5663(9) .1518(4) .083 Uiso calc R 1 . H
C3 .3587(8) .3273(10) .0338(4) .070(2) Uani d . 1 . C
H3A .2724(8) .3128(10) .0616(4) .084 Uiso calc R 1 . H
C4 .3491(7) .2642(8) -.0463(4) .0494(14) Uani d . 1 . C
C5 .2349(9) .2422(9) -.1005(4) .066(2) Uani d . 1 . C
H5A .1613(9) .2682(9) -.0867(4) .079 Uiso calc R 1 . H
C6 .2318(8) .1816(9) -.1748(4) .065(2) Uani d . 1 . C
H6A .1598(8) .1719(9) -.2126(4) .078 Uiso calc R 1 . H
C7 .3346(9) .1361(9) -.1924(4) .066(2) Uani d . 1 . C
H7A .3315(9) .0903(9) -.2412(4) .079 Uiso calc R 1 . H
C8 .4445(8) .1598(8) -.1354(4) .060(2) Uani d . 1 . C
H8A .5170(8) .1314(8) -.1477(4) .072 Uiso calc R 1 . H
Cl1 .3333 .6667 -.0424(2) .0733(9) Uani d S 1 . Cl
O12 .3333 .6667 .0405(7) .145(6) Uani d S 1 . O
O11 .1873(8) .5497(8) -.0683(5) .125(3) Uani d . 1 . O
Cl2 .0000 .0000 .1187(2) .0818(11) Uani d S 1 . Cl
O22 .0000 .0000 .0354(5) .098(3) Uani d S 1 . O
O21 -.0069(12) .1291(10) .1484(5) .138(3) Uani d . 1 . O
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_
_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 Mn1 N2 2_655 3_665 111.56(14)
N2 Mn1 N2 2_655 . 111.56(14)
N2 Mn1 N2 3_665 . 111.56(14)
N2 Mn1 N3 2_655 2_655 71.8(2)
N2 Mn1 N3 3_665 2_655 86.7(2)
N2 Mn1 N3 . 2_655 157.0(2)
N2 Mn1 N3 2_655 . 86.7(2)
N2 Mn1 N3 3_665 . 157.0(2)
N2 Mn1 N3 . . 71.8(2)
N3 Mn1 N3 2_655 . 86.0(2)
N2 Mn1 N3 2_655 3_665 157.0(2)
N2 Mn1 N3 3_665 3_665 71.8(2)
N2 Mn1 N3 . 3_665 86.7(2)
N3 Mn1 N3 2_655 3_665 86.0(2)
N3 Mn1 N3 . 3_665 86.0(2)
N2 Mn1 N1 2_655 . 72.70(15)
N2 Mn1 N1 3_665 . 72.70(15)
N2 Mn1 N1 . . 72.70(15)
N3 Mn1 N1 2_655 . 128.07(13)
N3 Mn1 N1 . . 128.07(13)
N3 Mn1 N1 3_665 . 128.07(13)
C1 N1 C1 2_655 3_665 111.2(4)
C1 N1 C1 2_655 . 111.2(4)
C1 N1 C1 3_665 . 111.2(4)
C1 N1 Mn1 2_655 . 107.7(4)
C1 N1 Mn1 3_665 . 107.7(4)
C1 N1 Mn1 . . 107.7(4)
C3 N2 C2 . . 119.1(6)
C3 N2 Mn1 . . 115.8(5)
C2 N2 Mn1 . . 115.5(5)
C8 N3 C4 . . 118.7(6)
C8 N3 Mn1 . . 126.6(5)
C4 N3 Mn1 . . 112.2(4)
N1 C1 C2 . . 111.5(6)
N2 C2 C1 . . 108.2(6)
N2 C3 C4 . . 115.3(6)
N3 C4 C5 . . 121.0(6)
N3 C4 C3 . . 116.6(6)
C5 C4 C3 . . 122.3(6)
C6 C5 C4 . . 119.4(7)
C7 C6 C5 . . 119.6(7)
C6 C7 C8 . . 118.0(6)
N3 C8 C7 . . 123.3(7)
O12 Cl1 O11 . 3_565 107.8(4)
O12 Cl1 O11 . . 107.8(4)
O11 Cl1 O11 3_565 . 111.1(4)
O12 Cl1 O11 . 2_665 107.8(4)
O11 Cl1 O11 3_565 2_665 111.1(4)
O11 Cl1 O11 . 2_665 111.1(4)
O22 Cl2 O21 . 3 110.4(3)
O22 Cl2 O21 . 2 110.4(3)
O21 Cl2 O21 3 2 108.5(3)
O22 Cl2 O21 . . 110.4(3)
O21 Cl2 O21 3 . 108.5(3)
O21 Cl2 O21 2 . 108.5(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
Mn1 N2 2_655 2.252(6) ?
Mn1 N2 3_665 2.252(6) ?
Mn1 N2 . 2.252(6) ?
Mn1 N3 2_655 2.385(5) ?
Mn1 N3 . 2.385(5) ?
Mn1 N3 3_665 2.385(5) ?
Mn1 N1 . 2.531(9) ?
N1 C1 2_655 1.467(8) ?
N1 C1 3_665 1.467(8) ?
N1 C1 . 1.467(8) ?
N2 C3 . 1.333(9) ?
N2 C2 . 1.496(8) ?
N3 C8 . 1.332(8) ?
N3 C4 . 1.333(8) ?
C1 C2 . 1.523(11) ?
C3 C4 . 1.465(9) ?
C4 C5 . 1.393(9) ?
C5 C6 . 1.378(10) ?
C6 C7 . 1.357(11) ?
C7 C8 . 1.388(10) ?
Cl1 O12 . 1.388(13) ?
Cl1 O11 3_565 1.416(7) ?
Cl1 O11 . 1.416(7) ?
Cl1 O11 2_665 1.416(7) ?
Cl2 O22 . 1.393(9) ?
Cl2 O21 3 1.426(8) ?
Cl2 O21 2 1.426(8) ?
Cl2 O21 . 1.426(8) ?
