#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007139.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_2007139
loop_
_publ_author_name
'Chang, N.-L.'
'Lynch, V. M.'
'Simonsen, S. H.'
_publ_section_title
;
 Tetrakis[1-(1-phenylcyclohexyl)piperidinium] Tetrachloromanganate(II)
 Dichloride
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              475
_journal_page_last               476
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C17 H26 N)4[Mn Cl4]Cl2'
_chemical_formula_sum            'C68 H104 Cl6 Mn N4'
_chemical_formula_weight         1245.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.7470(10)
_cell_length_b                   15.7470(10)
_cell_length_c                   13.1480(10)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      24.7
_cell_volume                     3260.3(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXL93
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'SHELXL93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       Siemens
_diffrn_measurement_method       '\w scan'
_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  0.046
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12559
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       prism
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.0125(10)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.06
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_obs          0.035
_refine_ls_shift/esd_max         -0.04
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.089
_refine_ls_wR_factor_obs         0.0842
_reflns_number_observed          2777
_reflns_number_total             3237
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    bk1313.cif
_[local]_cod_data_source_block   mnpcp
_[local]_cod_chemical_formula_sum_orig 'C68 H104 Cl6 Mn1 N4'
_cod_database_code               2007139
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, 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
Mn 0.0199(2) 0.0199(2) 0.0216(2) 0.000 0.000 0.000
Cl2 0.0252(2) 0.0356(3) 0.0339(3) 0.0005(2) 0.0070(2) 0.0091(2)
C1 0.0295(10) 0.0250(9) 0.0274(10) -0.0023(8) 0.0028(8) -0.0027(8)
C2 0.0360(12) 0.0249(10) 0.0450(13) 0.0000(9) 0.0078(11) 0.0045(10)
C3 0.0446(14) 0.0275(11) 0.052(2) -0.0054(9) 0.0091(13) 0.0102(12)
C4 0.0352(11) 0.0381(12) 0.0364(12) -0.0043(10) 0.0082(10) 0.0157(11)
C5 0.0235(9) 0.0348(11) 0.0295(10) -0.0017(8) 0.0101(8) 0.0084(9)
C6 0.0189(8) 0.0228(9) 0.0161(7) 0.0002(7) 0.0030(6) 0.0005(7)
C7 0.0236(9) 0.0286(10) 0.0178(8) -0.0005(7) 0.0017(7) -0.0012(7)
C8 0.0338(11) 0.0259(9) 0.0272(10) 0.0014(8) 0.0055(9) -0.0004(8)
C9 0.0372(12) 0.0268(10) 0.0301(10) -0.0040(9) 0.0057(9) 0.0005(9)
C10 0.0313(10) 0.0264(10) 0.0222(9) -0.0028(8) 0.0054(8) 0.0024(8)
C11 0.0205(9) 0.0259(10) 0.0200(8) -0.0007(7) 0.0038(7) 0.0005(7)
C12 0.0223(8) 0.0258(9) 0.0179(8) -0.0002(8) -0.0008(7) 0.0022(7)
C13 0.0227(9) 0.0326(11) 0.0261(10) 0.0007(8) 0.0003(8) 0.0016(8)
C14 0.0235(10) 0.0378(12) 0.0411(13) 0.0002(9) -0.0060(9) 0.0020(11)
C15 0.0332(12) 0.0442(14) 0.0376(13) -0.0057(11) -0.0167(10) 0.0036(11)
C16 0.0434(13) 0.0493(15) 0.0226(10) -0.0078(12) -0.0074(10) 0.0005(10)
C17 0.0291(10) 0.0385(11) 0.0205(8) -0.0036(9) 0.0008(8) 0.0003(8)
Cl1 0.0412(4) 0.0236(3) 0.0203(3) -0.0011(3) 0.000 0.000
N 0.0185(7) 0.0255(8) 0.0199(7) -0.0010(6) 0.0010(6) 0.0022(6)
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_type_symbol
Mn 0 0 0 0.02046(12) Uani d S 1 Mn
Cl2 -0.11804(3) -0.05617(4) 0.08839(5) 0.03157(13) Uani d . 1 Cl
C1 0.34898(15) -0.09177(14) -0.2155(2) 0.0273(4) Uani d . 1 C
H1A 0.39191(15) -0.07645(14) -0.2639(2) 0.080 Uiso d R 1 H
H1B 0.29646(15) -0.09975(14) -0.2513(2) 0.080 Uiso d R 1 H
C2 0.3723(2) -0.17418(15) -0.1616(2) 0.0353(5) Uani d . 1 C
H2A 0.4253(2) -0.16635(15) -0.1267(2) 0.080 Uiso d R 1 H
H2B 0.3794(2) -0.21885(15) -0.2105(2) 0.080 Uiso d R 1 H
C3 0.3048(2) -0.1993(2) -0.0846(2) 0.0415(6) Uani d . 1 C
H3A 0.3213(2) -0.2497(2) -0.0486(2) 0.080 Uiso d R 1 H
H3B 0.2527(2) -0.2107(2) -0.1198(2) 0.080 Uiso d R 1 H
C4 0.2916(2) -0.1269(2) -0.0101(2) 0.0366(5) Uani d . 1 C
H4A 0.2469(2) -0.1412(2) 0.0365(2) 0.080 Uiso d R 1 H
H4B 0.3427(2) -0.1188(2) 0.0285(2) 0.080 Uiso d R 1 H
C5 0.26981(14) -0.04437(15) -0.0645(2) 0.0293(5) Uani d . 1 C
H5A 0.21715(14) -0.05114(15) -0.1004(2) 0.080 Uiso d R 1 H
H5B 0.26298(14) 0.00058(15) -0.0159(2) 0.080 Uiso d R 1 H
C6 0.32578(12) 0.06796(13) -0.19102(14) 0.0193(3) Uani d . 1 C
C7 0.31490(13) 0.13391(13) -0.10540(15) 0.0233(4) Uani d . 1 C
H7A 0.36076(13) 0.12817(13) -0.05779(15) 0.080 Uiso d R 1 H
H7B 0.26265(13) 0.12328(13) -0.07000(15) 0.080 Uiso d R 1 H
C8 0.31498(15) 0.22439(14) -0.1483(2) 0.0290(4) Uani d . 1 C
H8A 0.30769(15) 0.26435(14) -0.0938(2) 0.080 Uiso d R 1 H
H8B 0.26764(15) 0.23033(14) -0.1937(2) 0.080 Uiso d R 1 H
C9 0.3960(2) 0.24432(15) -0.2057(2) 0.0314(5) Uani d . 1 C
H9A 0.3917(2) 0.29963(15) -0.2360(2) 0.080 Uiso d R 1 H
H9B 0.4428(2) 0.24477(15) -0.1591(2) 0.080 Uiso d R 1 H
C10 0.41190(15) 0.17850(14) -0.2887(2) 0.0266(4) Uani d . 1 C
H10A 0.36944(15) 0.18443(14) -0.3406(2) 0.080 Uiso d R 1 H
H10B 0.46630(15) 0.18858(14) -0.3194(2) 0.080 Uiso d R 1 H
C11 0.40945(13) 0.08783(14) -0.2461(2) 0.0221(3) Uani d . 1 C
H11A 0.41635(13) 0.04839(14) -0.3011(2) 0.080 Uiso d R 1 H
H11B 0.45589(13) 0.07989(14) -0.1997(2) 0.080 Uiso d R 1 H
C12 0.24903(13) 0.06421(13) -0.26199(14) 0.0220(4) Uani d . 1 C
C13 0.16673(13) 0.07913(15) -0.2259(2) 0.0271(4) Uani d . 1 C
H13A 0.15850(13) 0.09195(15) -0.1552(2) 0.080 Uiso d R 1 H
C14 0.0971(2) 0.0767(2) -0.2902(2) 0.0342(5) Uani d . 1 C
H14A 0.0412(2) 0.0870(2) -0.2637(2) 0.080 Uiso d R 1 H
C15 0.1082(2) 0.0584(2) -0.3923(2) 0.0383(6) Uani d . 1 C
H15A 0.0602(2) 0.0572(2) -0.4373(2) 0.080 Uiso d R 1 H
C16 0.1888(2) 0.0417(2) -0.4294(2) 0.0384(6) Uani d . 1 C
H16A 0.1963(2) 0.0281(2) -0.5000(2) 0.080 Uiso d R 1 H
C17 0.25884(15) 0.0451(2) -0.3658(2) 0.0294(4) Uani d . 1 C
H17A 0.31442(15) 0.0337(2) -0.3925(2) 0.080 Uiso d R 1 H
Cl1 0 -0.5000 -0.00298(5) 0.02837(14) Uani d S 1 Cl
N 0.33815(10) -0.02079(10) -0.13987(13) 0.0213(3) Uani d . 1 N
H0A 0.38696(10) -0.01815(10) -0.10439(13) 0.080 Uiso d R 1 H
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'
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
Cl2 Mn Cl2 2 4 103.988(14)
Cl2 Mn Cl2 2 . 121.10(3)
Cl2 Mn Cl2 4 . 103.988(14)
Cl2 Mn Cl2 2 3 103.988(14)
Cl2 Mn Cl2 4 3 121.10(3)
Cl2 Mn Cl2 . 3 103.988(14)
N C1 C2 . . 110.6(2)
N C1 H1A . . 109.37(11)
C2 C1 H1A . . 110.69(13)
N C1 H1B . . 108.87(11)
C2 C1 H1B . . 108.92(13)
H1A C1 H1B . . 108.3
C3 C2 C1 . . 111.3(2)
C3 C2 H2A . . 108.9(2)
C1 C2 H2A . . 108.78(13)
C3 C2 H2B . . 109.73(14)
C1 C2 H2B . . 109.90(13)
H2A C2 H2B . . 108.2
C4 C3 C2 . . 109.3(2)
C4 C3 H3A . . 109.83(14)
C2 C3 H3A . . 110.80(14)
C4 C3 H3B . . 109.6(2)
C2 C3 H3B . . 109.0(2)
H3A C3 H3B . . 108.3
C3 C4 C5 . . 111.6(2)
C3 C4 H4A . . 109.69(13)
C5 C4 H4A . . 109.54(12)
C3 C4 H4B . . 109.0(2)
C5 C4 H4B . . 108.92(13)
H4A C4 H4B . . 108.0
N C5 C4 . . 111.0(2)
N C5 H5A . . 108.72(11)
C4 C5 H5A . . 109.33(13)
N C5 H5B . . 109.62(11)
C4 C5 H5B . . 109.95(14)
H5A C5 H5B . . 108.2
C12 C6 C11 . . 113.5(2)
C12 C6 C7 . . 112.6(2)
C11 C6 C7 . . 107.6(2)
C12 C6 N . . 109.1(2)
C11 C6 N . . 106.14(15)
C7 C6 N . . 107.58(15)
C8 C7 C6 . . 111.0(2)
C8 C7 H7A . . 109.07(12)
C6 C7 H7A . . 109.22(10)
C8 C7 H7B . . 109.95(11)
C6 C7 H7B . . 109.39(10)
H7A C7 H7B . . 108.2
C9 C8 C7 . . 112.1(2)
C9 C8 H8A . . 109.68(12)
C7 C8 H8A . . 109.59(11)
C9 C8 H8B . . 108.84(13)
C7 C8 H8B . . 108.59(12)
H8A C8 H8B . . 107.9
C8 C9 C10 . . 110.8(2)
C8 C9 H9A . . 109.64(12)
C10 C9 H9A . . 109.34(12)
C8 C9 H9B . . 109.28(13)
C10 C9 H9B . . 109.61(13)
H9A C9 H9B . . 108.2
C9 C10 C11 . . 111.5(2)
C9 C10 H10A . . 109.14(13)
C11 C10 H10A . . 109.45(12)
C9 C10 H10B . . 109.56(12)
C11 C10 H10B . . 109.25(11)
H10A C10 H10B . . 107.9
C6 C11 C10 . . 112.5(2)
C6 C11 H11A . . 108.71(11)
C10 C11 H11A . . 108.87(11)
C6 C11 H11B . . 109.15(11)
C10 C11 H11B . . 109.51(12)
H11A C11 H11B . . 107.9
C13 C12 C17 . . 117.8(2)
C13 C12 C6 . . 121.2(2)
C17 C12 C6 . . 120.9(2)
C14 C13 C12 . . 121.4(2)
C14 C13 H13A . . 119.34(15)
C12 C13 H13A . . 119.26(12)
C13 C14 C15 . . 119.8(2)
C13 C14 H14A . . 119.99(15)
C15 C14 H14A . . 120.18(15)
C14 C15 C16 . . 119.8(2)
C14 C15 H15A . . 120.12(15)
C16 C15 H15A . . 120.07(14)
C17 C16 C15 . . 120.7(2)
C17 C16 H16A . . 119.64(14)
C15 C16 H16A . . 119.70(14)
C16 C17 C12 . . 120.5(2)
C16 C17 H17A . . 119.84(14)
C12 C17 H17A . . 119.70(13)
C1 N C5 . . 109.4(2)
C1 N C6 . . 113.20(15)
C5 N C6 . . 114.4(2)
C1 N H0A . . 106.25(11)
C5 N H0A . . 106.27(11)
C6 N H0A . . 106.74(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn Cl2 2 2.3639(5)
Mn Cl2 4 2.3639(5)
Mn Cl2 . 2.3639(5)
Mn Cl2 3 2.3639(5)
C1 N . 1.505(3)
C1 C2 . 1.524(3)
C1 H1A . 0.96
C1 H1B . 0.96
C2 C3 . 1.519(4)
C2 H2A . 0.96
C2 H2B . 0.96
C3 C4 . 1.517(4)
C3 H3A . 0.96
C3 H3B . 0.96
C4 C5 . 1.523(3)
C4 H4A . 0.96
C4 H4B . 0.96
C5 N . 1.509(3)
C5 H5A . 0.96
C5 H5B . 0.96
C6 C12 . 1.528(3)
C6 C11 . 1.536(3)
C6 C7 . 1.541(3)
C6 N . 1.563(3)
C7 C8 . 1.532(3)
C7 H7A . 0.96
C7 H7B . 0.96
C8 C9 . 1.515(3)
C8 H8A . 0.96
C8 H8B . 0.96
C9 C10 . 1.526(3)
C9 H9A . 0.96
C9 H9B . 0.96
C10 C11 . 1.534(3)
C10 H10A . 0.96
C10 H10B . 0.96
C11 H11A . 0.96
C11 H11B . 0.96
C12 C13 . 1.400(3)
C12 C17 . 1.406(3)
C13 C14 . 1.386(3)
C13 H13A . 0.96
C14 C15 . 1.384(4)
C14 H14A . 0.96
C15 C16 . 1.385(4)
C15 H15A . 0.96
C16 C17 . 1.385(3)
C16 H16A . 0.96
C17 H17A . 0.96
N H0A . 0.90
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
N C1 C2 C3 58.6(3)
C1 C2 C3 C4 -55.9(3)
C2 C3 C4 C5 55.3(3)
C3 C4 C5 N -57.3(3)
C12 C6 C7 C8 -67.8(2)
C11 C6 C7 C8 58.0(2)
N C6 C7 C8 172.0(2)
C6 C7 C8 C9 -58.4(2)
C7 C8 C9 C10 54.6(3)
C8 C9 C10 C11 -52.8(3)
C12 C6 C11 C10 67.8(2)
C7 C6 C11 C10 -57.5(2)
N C6 C11 C10 -172.4(2)
C9 C10 C11 C6 56.0(2)
C11 C6 C12 C13 -155.4(2)
C7 C6 C12 C13 -32.9(3)
N C6 C12 C13 86.5(2)
C11 C6 C12 C17 25.0(3)
C7 C6 C12 C17 147.5(2)
N C6 C12 C17 -93.1(2)
C17 C12 C13 C14 -1.1(3)
C6 C12 C13 C14 179.3(2)
C12 C13 C14 C15 0.6(4)
C13 C14 C15 C16 0.7(4)
C14 C15 C16 C17 -1.4(4)
C15 C16 C17 C12 0.9(4)
C13 C12 C17 C16 0.4(3)
C6 C12 C17 C16 180.0(2)
C2 C1 N C5 -58.6(2)
C2 C1 N C6 172.5(2)
C4 C5 N C1 58.0(2)
C4 C5 N C6 -173.9(2)
C12 C6 N C1 57.2(2)
C11 C6 N C1 -65.5(2)
C7 C6 N C1 179.6(2)
C12 C6 N C5 -69.0(2)
C11 C6 N C5 168.3(2)
C7 C6 N C5 53.4(2)