#------------------------------------------------------------------------------
#$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $
#$Revision: 19 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003075.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2003075
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     1999
_journal_volume     B55
_journal_page_first     186
_journal_page_last     191
loop_
    _publ_author_name
    'D. Ramalakshmi'
    'M. V. Rajasekharan'
_chemical_name_systematic
;
 'Tetrakis(2,2'-bipyridine)bis(mu-oxo)dimanganese(3+)
 hexanitratocerate(3-) pentahydrate'
;
_chemical_formula_sum     'C40 H42 Ce Mn2 N14 O25'
_chemical_formula_structural     '[Mn2O2(bpy)4][Ce(NO3)6].5H2O'
_chemical_formula_analytical     'C40 H42 Ce Mn2 N14 025'
_chemical_formula_iupac     '[Mn2 O2 (C10 H8 N2)4][Ce(N O3)6].5(H2 O)'
_chemical_formula_weight     1368.88
_symmetry_cell_setting     'Monoclinic'
_symmetry_space_group_name_H-M     'C 2/c'
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'
_cell_length_a     12.940(3)
_cell_length_b     18.060(2)
_cell_length_c     22.544(11)
_cell_angle_alpha     90.00
_cell_angle_beta     96.29(2)
_cell_angle_gamma     90.00
_cell_volume     5237.(3)
_cell_formula_units_Z     4
_cell_measurement_temperature     132(2)
_exptl_crystal_description     'rectangular rods'
_exptl_crystal_colour     'dark greenish black'
_exptl_crystal_size_max     0.35
_exptl_crystal_size_mid     0.30
_exptl_crystal_size_min     0.26
_exptl_crystal_density_diffrn     1.736
_exptl_crystal_density_meas     1.75
_exptl_crystal_density_method     'floatation'
_exptl_crystal_F_000     2752
_exptl_absorpt_coefficient_mu     1.429
_exptl_absorpt_correction_type     semiempirical
_exptl_absorpt_correction_T_min     0.257
_exptl_absorpt_correction_T_max     0.327
_diffrn_ambient_temperature     132(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device     'Siemens P4'
_diffrn_measurement_method     '\w-2\q'
_diffrn_reflns_number     6034
_diffrn_reflns_av_R_equivalents     0.0281
_diffrn_reflns_av_sigmaI/netI     0.0344
_diffrn_reflns_theta_min     2.07
_diffrn_reflns_theta_max     27.50
_diffrn_reflns_limit_h_min     -16
_diffrn_reflns_limit_h_max     16
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     23
_diffrn_reflns_limit_l_min     0
_diffrn_reflns_limit_l_max     29
_diffrn_standards_number     3
_diffrn_standards_interval_count     100
_diffrn_standards_decay_%     0
_reflns_number_total     6021
_reflns_number_observed     4877
_reflns_observed_criterion     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0539
_refine_ls_R_factor_obs     0.0358
_refine_ls_wR_factor_all     0.0947
_refine_ls_wR_factor_obs     0.0783
_refine_ls_goodness_of_fit_all     1.105
_refine_ls_goodness_of_fit_obs     1.136
_refine_ls_restrained_S_all     1.224
_refine_ls_restrained_S_obs     1.134
_refine_ls_number_reflns     5645
_refine_ls_number_parameters     409
_refine_ls_number_restraints     12
_refine_ls_hydrogen_treatment
;
 Hydrogen atoms are labelled according to the atom to which they are
 attached. All hydrogens except HW1A, HW1B, HW2A, HW2B, HW3A, HW3B,
 HW4A and HW4B were refined using the riding model (the positional
 parameters of the riding atoms have same e.s.ds as the atom on which
 they ride). Bond length constraints were applied to the hydrogens
 of the water molecules. All hydrogens except HW1A, HW1B, HW2A and
 HW2B were assigned fixed U(iso) values (= 1.5 times the U(iso) of
 the atom to which they are attached).
;
_refine_ls_weighting_scheme
        'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+13.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_shift/esd_max
                           ' -0.157 (for y of HW3A, < 0.03 for all non-H atoms)'
_refine_ls_shift/esd_mean     0.006
_refine_diff_density_max     0.925
_refine_diff_density_min     -0.589
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'Mn' 'Mn' 0.3368 0.7283
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ce' 'Ce' -0.2486 2.6331
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
    Mn 0.10205(3) -0.31120(2) 0.27211(2) 0.01864(8) Uani d . 1 . Mn
    O1 0.0000 -0.37795(13) 0.2500 0.0236(6) Uani d S 1 . O
    O2 0.0000 -0.24494(13) 0.2500 0.0231(6) Uani d S 1 . O
    N1 0.1644(2) -0.29545(12) 0.18985(9) 0.0241(5) Uani d . 1 . N
    N2 0.2151(2) -0.39399(11) 0.27394(9) 0.0218(5) Uani d . 1 . N
    N3 0.2023(2) -0.23294(12) 0.31588(10) 0.0247(5) Uani d . 1 . N
    N4 0.0801(2) -0.32638(12) 0.36371(10) 0.0279(5) Uani d . 1 . N
    C1 0.1366(2) -0.24126(15) 0.15081(12) 0.0288(6) Uani d . 1 . C
    H1 0.0880(2) -0.20516(15) 0.16071(12) 0.043 Uiso calc R 1 . H
    C2 0.1768(2) -0.2361(2) 0.09620(13) 0.0341(7) Uani d . 1 . C
    H2 0.1561(2) -0.1971(2) 0.06921(13) 0.051 Uiso calc R 1 . H
    C3 0.2476(2) -0.2889(2) 0.08194(13) 0.0366(7) Uani d . 1 . C
    H3 0.2761(2) -0.2865(2) 0.04492(13) 0.055 Uiso calc R 1 . H
    C4 0.2766(2) -0.3455(2) 0.12229(12) 0.0306(6) Uani d . 1 . C
    H4 0.3246(2) -0.3824(2) 0.11307(12) 0.046 Uiso calc R 1 . H
    C5 0.3286(2) -0.4612(2) 0.21593(13) 0.0332(7) Uani d . 1 . C
    H5 0.3612(2) -0.4658(2) 0.18037(13) 0.050 Uiso calc R 1 . H
    C6 0.3474(2) -0.5126(2) 0.26134(13) 0.0368(7) Uani d . 1 . C
    H6 0.3924(2) -0.5534(2) 0.25717(13) 0.055 Uiso calc R 1 . H
    C7 0.2997(2) -0.5039(2) 0.31275(12) 0.0326(6) Uani d . 1 . C
    H7 0.3113(2) -0.5388(2) 0.34433(12) 0.049 Uiso calc R 1 . H
    C8 0.2352(2) -0.4442(2) 0.31778(12) 0.0272(6) Uani d . 1 . C
    H8 0.2036(2) -0.4382(2) 0.35358(12) 0.041 Uiso calc R 1 . H
    C9 0.2615(2) -0.40292(14) 0.22310(11) 0.0228(5) Uani d . 1 . C
    C10 0.2340(2) -0.34700(14) 0.17646(11) 0.0233(6) Uani d . 1 . C
    C11 0.2668(2) -0.1883(2) 0.28910(13) 0.0323(7) Uani d . 1 . C
    H11 0.2757(2) -0.1969(2) 0.24840(13) 0.048 Uiso calc R 1 . H
    C12 0.3204(2) -0.1306(2) 0.31851(14) 0.0363(7) Uani d . 1 . C
    H12 0.3658(2) -0.1005(2) 0.29850(14) 0.054 Uiso calc R 1 . H
    C13 0.3070(2) -0.1175(2) 0.37704(14) 0.0339(7) Uani d . 1 . C
    H13 0.3418(2) -0.0773(2) 0.39788(14) 0.051 Uiso calc R 1 . H
    C14 0.2419(2) -0.1634(2) 0.40556(13) 0.0296(6) Uani d . 1 . C
    H14 0.2320(2) -0.1550(2) 0.44615(13) 0.044 Uiso calc R 1 . H
    C15 0.1064(2) -0.2737(2) 0.46118(13) 0.0344(7) Uani d . 1 . C
    H15 0.1368(2) -0.2362(2) 0.48709(13) 0.052 Uiso calc R 1 . H
    C16 0.0441(2) -0.3279(2) 0.48282(15) 0.0407(8) Uani d . 1 . C
    H16 0.0309(2) -0.3278(2) 0.52344(15) 0.061 Uiso calc R 1 . H
    C17 0.0018(2) -0.3818(2) 0.44388(15) 0.0390(7) Uani d . 1 . C
    H17 -0.0400(2) -0.4201(2) 0.45758(15) 0.058 Uiso calc R 1 . H
    C18 0.0210(2) -0.3794(2) 0.38509(14) 0.0341(7) Uani d . 1 . C
    H18 -0.0084(2) -0.4165(2) 0.35858(14) 0.051 Uiso calc R 1 . H
    C19 0.1242(2) -0.27452(14) 0.40150(12) 0.0259(6) Uani d . 1 . C
    C20 0.1917(2) -0.22138(15) 0.37445(12) 0.0247(6) Uani d . 1 . C
    Ce 0.0000 0.0000 0.0000 0.01991(4) Uani d S 1 . Ce
    N5 0.0230(2) 0.07341(12) -0.11877(9) 0.0235(5) Uani d . 1 . N
    O3 0.01358(14) 0.00350(10) -0.11422(8) 0.0265(4) Uani d . 1 . O
    O4 0.03210(15) 0.10318(11) -0.16699(8) 0.0306(5) Uani d . 1 . O
    O5 0.02212(14) 0.11081(10) -0.07128(8) 0.0263(4) Uani d . 1 . O
    N6 -0.2367(2) 0.02987(13) -0.01468(10) 0.0289(5) Uani d . 1 . N
    O6 -0.19677(14) -0.00094(12) 0.03188(8) 0.0325(4) Uani d . 1 . O
    O7 -0.3317(2) 0.03582(15) -0.02636(11) 0.0506(7) Uani d . 1 . O
    O8 -0.17629(14) 0.05590(11) -0.05042(9) 0.0311(5) Uani d . 1 . O
    N7 0.0548(2) 0.14382(13) 0.06822(10) 0.0312(5) Uani d . 1 . N
    O9 -0.03740(15) 0.12916(10) 0.04789(9) 0.0305(4) Uani d . 1 . O
    O10 0.0757(2) 0.19869(13) 0.09999(11) 0.0530(6) Uani d . 1 . O
    O11 0.12523(14) 0.10117(11) 0.05393(9) 0.0322(5) Uani d . 1 . O
    OW1 0.0000 -0.52877(9) 0.2500 0.0433(8) Uani d SD 1 . O
    HW1A 0.0000 -0.47507(10) 0.2500 0.15(3)   Uiso d SD 1 . H
    HW1B 0.0317(5) -0.5428(2) 0.28939(14) 0.05(2)   Uiso d PD 0.50 . H
    OW2 -0.0493(2) 0.26400(14) 0.19167(8) 0.0646(8) Uani d D 1 . O
    HW2A 0.0073(3) 0.2598(5) 0.22342(14) 0.24(4)   Uiso d D 1 . H
    HW2B -0.0247(5) 0.2394(5) 0.1577(2) 0.13(2)   Uiso d D 1 . H
    OW3 -0.4372(2) 0.0877(2) -0.13899(10) 0.0566(14) Uani d PD 0.610(6) . O
    HW3A -0.3956(6) 0.1252(3) -0.1167(2) 0.085 Uiso d PD 0.610(6) . H
    HW3B -0.4166(7) 0.0899(5) -0.17906(15) 0.085 Uiso d PD 0.610(6) . H
    OW4 -0.3942(2) 0.1105(2) -0.15369(14) 0.069(3) Uani d PD 0.390(6) . O
    HW4A -0.4479(3) 0.1469(2) -0.1491(3) 0.104 Uiso d PD 0.390(6) . H
    HW4B -0.3888(9) 0.0815(4) -0.1172(2) 0.104 Uiso d PD 0.390(6) . H
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 0.0181(2) 0.0199(2) 0.0189(2) -0.00037(14) 0.00665(13) -0.00080(14)
    O1 0.0238(12) 0.0177(11) 0.0293(13) 0.000 0.0034(10) 0.000
    O2 0.0249(12) 0.0177(11) 0.0288(13) 0.000 0.0124(10) 0.000
    N1 0.0273(10) 0.0223(10) 0.0232(10) 0.0030(9) 0.0044(9) -0.0024(8)
    N2 0.0178(9) 0.0250(10) 0.0229(10) -0.0003(8) 0.0037(8) -0.0017(8)
    N3 0.0181(9) 0.0243(10) 0.0323(11) -0.0010(8) 0.0059(8) -0.0005(9)
    N4 0.0243(10) 0.0219(10) 0.0395(13) 0.0006(9) 0.0120(9) -0.0026(9)
    C1 0.0310(13) 0.0230(12) 0.0320(14) -0.0004(11) 0.0024(11) -0.0004(11)
    C2 0.039(2) 0.0289(14) 0.0344(15) 0.0005(12) 0.0035(12) 0.0092(12)
    C3 0.042(2) 0.042(2) 0.0280(14) 0.0038(13) 0.0140(12) 0.0069(12)
    C4 0.0295(13) 0.0365(15) 0.0279(13) 0.0043(12) 0.0123(11) 0.0018(12)
    C5 0.0357(14) 0.038(2) 0.0273(13) 0.0136(12) 0.0100(11) 0.0006(12)
    C6 0.0346(14) 0.042(2) 0.0341(14) 0.0178(12) 0.0054(12) 0.0037(12)
    C7 0.0294(12) 0.0387(14) 0.0294(13) 0.0079(13) 0.0017(10) 0.0057(13)
    C8 0.0236(12) 0.0349(14) 0.0234(12) 0.0016(11) 0.0038(10) 0.0017(11)
    C9 0.0217(11) 0.0267(12) 0.0206(12) 0.0014(10) 0.0049(9) -0.0025(10)
    C10 0.0221(11) 0.0238(12) 0.0240(12) -0.0011(10) 0.0031(10) -0.0009(10)
    C11 0.0292(13) 0.0313(14) 0.0378(15) -0.0048(12) 0.0106(11) -0.0037(12)
    C12 0.0306(14) 0.0343(15) 0.045(2) -0.0098(12) 0.0087(13) 0.0011(13)
    C13 0.0272(13) 0.0290(14) 0.044(2) -0.0058(11) -0.0010(12) -0.0056(13)
    C14 0.0254(13) 0.0317(14) 0.0316(14) 0.0030(11) 0.0036(11) -0.0056(12)
    C15 0.0311(14) 0.039(2) 0.0342(15) 0.0070(12) 0.0066(12) 0.0027(13)
    C16 0.0335(15) 0.048(2) 0.043(2) 0.0070(13) 0.0125(13) 0.0127(14)
    C17 0.0316(14) 0.035(2) 0.052(2) 0.0014(12) 0.0160(13) 0.0158(14)
    C18 0.0264(13) 0.0269(13) 0.051(2) -0.0009(11) 0.0123(12) -0.0003(13)
    C19 0.0195(11) 0.0253(12) 0.0335(14) 0.0045(10) 0.0057(10) 0.0010(11)
    C20 0.0174(11) 0.0269(12) 0.0302(13) 0.0033(10) 0.0045(10) -0.0027(11)
    Ce 0.02058(8) 0.01974(8) 0.02078(8) 0.00124(8) 0.00843(6) 0.00004(9)
    N5 0.0218(10) 0.0259(11) 0.0237(10) 0.0000(8) 0.0061(8) 0.0017(9)
    O3 0.0330(9) 0.0226(8) 0.0250(8) -0.0008(8) 0.0081(7) -0.0021(8)
    O4 0.0343(10) 0.0345(10) 0.0237(9) -0.0030(8) 0.0067(8) 0.0058(8)
    O5 0.0331(9) 0.0243(9) 0.0231(9) -0.0006(8) 0.0104(7) -0.0011(7)
    N6 0.0258(11) 0.0326(11) 0.0291(12) 0.0029(9) 0.0064(9) -0.0063(10)
    O6 0.0315(9) 0.0391(10) 0.0289(9) 0.0023(9) 0.0121(7) 0.0020(9)
    O7 0.0228(10) 0.071(2) 0.0588(15) 0.0061(11) 0.0070(10) -0.0042(13)
    O8 0.0291(9) 0.0338(10) 0.0316(10) 0.0049(8) 0.0087(8) 0.0036(8)
    N7 0.0371(12) 0.0275(11) 0.0308(12) -0.0055(10) 0.0123(10) -0.0025(10)
    O9 0.0317(9) 0.0275(9) 0.0346(10) 0.0023(8) 0.0137(8) -0.0029(8)
    O10 0.0661(15) 0.0409(12) 0.0555(14) -0.0157(11) 0.0222(12) -0.0255(11)
    O11 0.0289(9) 0.0347(10) 0.0343(10) -0.0019(8) 0.0086(8) -0.0043(9)
    OW1 0.049(2) 0.0247(14) 0.055(2) 0.000 0.000(2) 0.000
    OW2 0.0578(15) 0.079(2) 0.060(2) -0.0158(14) 0.0187(13) -0.0298(14)
    OW3 0.052(3) 0.064(3) 0.052(3) 0.009(2) -0.007(2) 0.000(2)
    OW4 0.076(5) 0.064(5) 0.061(5) 0.018(4) -0.022(4) -0.021(4)