#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006507.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_2006507
loop_
_publ_author_name
'Baumeister, Ute'
'Hartung, Helmut'
_publ_section_title
;Bis(μ-bicyclo[2.2.1]hept-5-ene-2-exo,3-exo-dicarboxylato-κ²O,O':κ²O'',O''')bis[aqua(2,2'-bipyridine-N,N')manganese(II)]
 Monohydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1246
_journal_page_last               1248
_journal_paper_doi               10.1107/S0108270197004757
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Mn (C10 H8 N2) (H2 O) (C9 H8 O4)]2 , H2 O'
_chemical_formula_structural
'((Mn (C10 H8 N2) (H2 O))2 (C9 H8 O4)2) (H2 O)'
_chemical_formula_sum            'C38 H38 Mn2 N4 O11'
_chemical_formula_weight         836.60
_chemical_melting_point          'decomposition > 90_C'
_chemical_name_systematic
;
 Bis(μ-bicyclo[2.2.1]hept-5-ene-2-exo,3-exo-dicarboxylato-
 κ²O,O':κ²O'',O''')bis[aqua(2,2'-bipyridine-N,N')manganese(II)]
 Monohydrate
;
_chemical_temperature_decomposition_gt 363.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                109.050(10)
_cell_angle_beta                 92.000(10)
_cell_angle_gamma                110.640(10)
_cell_formula_units_Z            1
_cell_length_a                   9.534(2)
_cell_length_b                   10.486(2)
_cell_length_c                   10.486(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      10.0
_cell_volume                     913.9(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1991a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1991b)'
_computing_molecular_graphics    'XP/PC (Siemens, 1990)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe STADI4'
_diffrn_measurement_method       'ω/2theta 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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10617
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        4.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .271
_refine_diff_density_min         -.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.006
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    'constr except H1W1, H1W2 refxyz'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_obs          .0316
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0451P)²+0.0847P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0840
_refine_ls_wR_factor_obs         .0768
_reflns_number_observed          3866
_reflns_number_total             5315
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1202.cif
_cod_data_source_block           k208
_cod_depositor_comments
;
'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value had been given
as 'decomposition > 90_C'. The value 'decomposition > 90_C' was changed
to '363.15' - it was converted from degrees Celsius(C) to Kelvins(K).

Adriana Da\<skevi\<c, 2011-06-07
;
_cod_database_code               2006507
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 .08874(2) .21811(2) .19923(2) .03194(7) Uani d . 1 . Mn
N1 .03695(13) .41647(13) .23519(12) .0332(2) Uani d . 1 . N
N2 .21299(14) .38021(14) .41066(12) .0367(3) Uani d . 1 . N
O1 .11249(12) .20675(12) -.03065(12) .0414(2) Uani d . 1 . O
O2 .31358(13) .29905(14) .12662(11) .0474(3) Uani d . 1 . O
O3 .17817(13) -.06597(12) -.10595(12) .0434(3) Uani d . 1 . O
O4 .07752(13) -.09850(13) -.30949(12) .0519(3) Uani d . 1 . O
O1W .1549(2) .02984(14) .16840(13) .0456(3) Uani d . 1 . O
H1W1 .186(3) .012(2) .099(2) .055 Uiso d . 1 . H
H1W2 .082(3) -.041(2) .156(2) .055 Uiso d . 1 . H
O2W .0936(5) .0272(5) .4871(5) .124(2) Uani d P .50 . O
H2W1 .0554(5) -.0431(5) .5118(5) .148 Uiso d PR .50 . H
H2W2 .0305(5) .0181(5) .4222(5) .148 Uiso d PR .50 . H
C1 .2539(2) .25141(14) .00347(15) .0323(3) Uani d . 1 . C
C2 .1843(2) -.03001(15) -.2086(2) .0361(3) Uani d . 1 . C
C3 .3202(2) .0953(2) -.2180(2) .0383(3) Uani d . 1 . C
H3 .3050(2) .1008(2) -.3087(2) .046 Uiso calc R 1 . H
C4 .3542(2) .25023(15) -.10661(14) .0313(3) Uani d . 1 . C
H4 .3428(2) .31471(15) -.15245(14) .038 Uiso calc R 1 . H
C5 .5251(2) .3026(2) -.0480(2) .0389(3) Uani d . 1 . C
H5 .5632(2) .3867(2) .0384(2) .047 Uiso calc R 1 . H
C6 .6127(2) .3180(2) -.1636(2) .0549(5) Uani d . 1 . C
H6 .6747(2) .4050(2) -.1719(2) .066 Uiso calc R 1 . H
C7 .5844(2) .1851(2) -.2499(2) .0688(6) Uani d . 1 . C
H7 .6245(2) .1610(2) -.3298(2) .083 Uiso calc R 1 . H
C8 .4756(2) .0786(2) -.1963(2) .0556(5) Uani d . 1 . C
H8 .4720(2) -.0216(2) -.2318(2) .067 Uiso calc R 1 . H
C9 .5292(2) .1604(2) -.0425(2) .0500(4) Uani d . 1 . C
H9A .4585(2) .1197(2) .0116(2) .060 Uiso calc R 1 . H
H9B .6306(2) .1691(2) -.0123(2) .060 Uiso calc R 1 . H
C10 -.0513(2) .4276(2) .1409(2) .0408(3) Uani d . 1 . C
H10 -.0949(2) .3483(2) .0591(2) .049 Uiso calc R 1 . H
C11 -.0804(2) .5512(2) .1597(2) .0498(4) Uani d . 1 . C
H11 -.1411(2) .5562(2) .0915(2) .060 Uiso calc R 1 . H
C12 -.0180(2) .6672(2) .2812(2) .0546(5) Uani d . 1 . C
H12 -.0365(2) .7519(2) .2965(2) .066 Uiso calc R 1 . H
C13 .0719(2) .6577(2) .3802(2) .0476(4) Uani d . 1 . C
H13 .1133(2) .7350(2) .4636(2) .057 Uiso calc R 1 . H
C14 .0999(2) .53043(15) .35373(15) .0341(3) Uani d . 1 . C
C15 .2005(2) .5105(2) .45050(14) .0362(3) Uani d . 1 . C
C16 .2787(2) .6209(2) .5758(2) .0536(5) Uani d . 1 . C
H16 .2675(2) .7100(2) .6025(2) .064 Uiso calc R 1 . H
C17 .3722(2) .5958(3) .6588(2) .0639(6) Uani d . 1 . C
H17 .4267(2) .6688(3) .7417(2) .077 Uiso calc R 1 . H
C18 .3849(2) .4632(3) .6191(2) .0605(5) Uani d . 1 . C
H18 .4476(2) .4444(3) .6744(2) .073 Uiso calc R 1 . H
C19 .3023(2) .3571(2) .4944(2) .0491(4) Uani d . 1 . C
H19 .3094(2) .2661(2) .4681(2) .059 Uiso calc 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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn .3368 .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
_geom_angle_publ_flag
O1W Mn1 N1 . . 176.51(5) yes
O1W Mn1 O4 . 2 80.22(5) yes
N1 Mn1 O4 . 2 101.92(5) yes
O1W Mn1 N2 . . 105.12(5) yes
N1 Mn1 N2 . . 72.42(5) yes
O4 Mn1 N2 2 . 85.88(5) yes
O1W Mn1 O2 . . 80.05(5) yes
N1 Mn1 O2 . . 97.21(5) yes
O4 Mn1 O2 2 . 156.07(5) yes
N2 Mn1 O2 . . 86.34(5) yes
O1W Mn1 O1 . . 91.83(5) yes
N1 Mn1 O1 . . 88.37(4) yes
O4 Mn1 O1 2 . 138.42(4) yes
N2 Mn1 O1 . . 135.21(4) yes
O2 Mn1 O1 . . 55.68(4) yes
O1W Mn1 O3 . 2 93.86(5) yes
N1 Mn1 O3 . 2 89.63(4) yes
O4 Mn1 O3 2 2 55.17(4) yes
N2 Mn1 O3 . 2 133.07(4) yes
O2 Mn1 O3 . 2 139.79(4) yes
O1 Mn1 O3 . 2 85.16(4) yes
C10 N1 C14 . . 118.98(13) ?
C10 N1 Mn1 . . 121.99(10) ?
C14 N1 Mn1 . . 119.00(10) ?
C19 N2 C15 . . 118.41(14) ?
C19 N2 Mn1 . . 124.56(12) ?
C15 N2 Mn1 . . 116.95(10) ?
C1 O1 Mn1 . . 88.08(9) ?
C1 O2 Mn1 . . 94.09(9) ?
C2 O3 Mn1 . 2 87.35(9) ?
C2 O4 Mn1 . 2 95.27(10) ?
O2 C1 O1 . . 120.93(14) ?
O2 C1 C4 . . 119.69(13) ?
O1 C1 C4 . . 119.37(13) ?
O3 C2 O4 . . 120.61(14) ?
O3 C2 C3 . . 121.82(13) ?
O4 C2 C3 . . 117.56(14) ?
C2 C3 C8 . . 113.52(14) ?
C2 C3 C4 . . 116.02(12) ?
C8 C3 C4 . . 101.33(12) ?
C1 C4 C5 . . 112.83(12) ?
C1 C4 C3 . . 115.02(11) ?
C5 C4 C3 . . 102.64(12) ?
C6 C5 C9 . . 100.81(14) ?
C6 C5 C4 . . 106.97(14) ?
C9 C5 C4 . . 100.07(11) ?
C7 C6 C5 . . 107.1(2) ?
C6 C7 C8 . . 107.9(2) ?
C7 C8 C9 . . 100.29(15) ?
C7 C8 C3 . . 104.7(2) ?
C9 C8 C3 . . 102.02(13) ?
C5 C9 C8 . . 93.52(14) ?
N1 C10 C11 . . 122.7(2) ?
C12 C11 C10 . . 118.6(2) ?
C11 C12 C13 . . 119.8(2) ?
C12 C13 C14 . . 118.9(2) ?
N1 C14 C13 . . 121.01(15) ?
N1 C14 C15 . . 115.35(13) ?
C13 C14 C15 . . 123.63(14) ?
N2 C15 C16 . . 121.6(2) ?
N2 C15 C14 . . 116.20(12) ?
C16 C15 C14 . . 122.2(2) ?
C17 C16 C15 . . 119.0(2) ?
C18 C17 C16 . . 119.7(2) ?
C17 C18 C19 . . 118.6(2) ?
N2 C19 C18 . . 122.7(2) ?
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 O1W . 2.2081(13) yes
Mn1 N1 . 2.2221(13) yes
Mn1 O4 2 2.2573(13) yes
Mn1 N2 . 2.2682(13) yes
Mn1 O2 . 2.2690(12) yes
Mn1 O1 . 2.3971(13) yes
Mn1 O3 2 2.4338(13) yes
N1 C10 . 1.336(2) ?
N1 C14 . 1.344(2) ?
N2 C19 . 1.337(2) ?
N2 C15 . 1.342(2) ?
O1 C1 . 1.256(2) yes
O2 C1 . 1.252(2) yes
O3 C2 . 1.249(2) yes
O3 Mn1 2 2.4338(13) ?
O4 C2 . 1.259(2) yes
O4 Mn1 2 2.2573(13) ?
O2W O2W 2_556 1.732(10) ?
C1 C4 . 1.524(2) ?
C2 C3 . 1.519(2) ?
C3 C8 . 1.569(2) ?
C3 C4 . 1.572(2) ?
C4 C5 . 1.553(2) ?
C5 C6 . 1.515(2) ?
C5 C9 . 1.526(2) ?
C6 C7 . 1.315(3) yes
C7 C8 . 1.508(3) ?
C8 C9 . 1.526(3) ?
C10 C11 . 1.373(2) ?
C11 C12 . 1.372(3) ?
C12 C13 . 1.374(3) ?
C13 C14 . 1.395(2) ?
C14 C15 . 1.484(2) ?
C15 C16 . 1.397(2) ?
C16 C17 . 1.372(3) ?
C17 C18 . 1.366(3) ?
C18 C19 . 1.389(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2W H2W1 O4 1_556 0.828 2.160 2.833(4) 139 yes
O2W H2W2 O4 2 0.850 2.084 2.871(5) 154 yes
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
O1W Mn1 N1 C10 . 133.4(8)
O4 Mn1 N1 C10 2 -99.23(12)
N2 Mn1 N1 C10 . 179.04(12)
O2 Mn1 N1 C10 . 95.22(12)
O1 Mn1 N1 C10 . 40.12(12)
O3 Mn1 N1 C10 2 -45.04(12)
O1W Mn1 N1 C14 . -44.6(8)
O4 Mn1 N1 C14 2 82.79(11)
N2 Mn1 N1 C14 . 1.07(10)
O2 Mn1 N1 C14 . -82.75(11)
O1 Mn1 N1 C14 . -137.85(10)
O3 Mn1 N1 C14 2 136.98(10)
O1W Mn1 N2 C19 . -1.57(13)
N1 Mn1 N2 C19 . -178.99(13)
O4 Mn1 N2 C19 2 77.13(13)
O2 Mn1 N2 C19 . -80.23(13)
O1 Mn1 N2 C19 . -110.18(13)
O3 Mn1 N2 C19 2 108.79(13)
O1W Mn1 N2 C15 . 175.20(10)
N1 Mn1 N2 C15 . -2.21(10)
O4 Mn1 N2 C15 2 -106.10(11)
O2 Mn1 N2 C15 . 96.55(11)
O1 Mn1 N2 C15 . 66.60(12)
O3 Mn1 N2 C15 2 -74.44(12)
O1W Mn1 O1 C1 . -70.41(9)
N1 Mn1 O1 C1 . 106.10(8)
O4 Mn1 O1 C1 2 -147.68(9)
N2 Mn1 O1 C1 . 43.33(11)
O2 Mn1 O1 C1 . 6.23(8)
O3 Mn1 O1 C1 2 -164.13(8)
O1W Mn1 O2 C1 . 92.89(10)
N1 Mn1 O2 C1 . -89.30(10)
O4 Mn1 O2 C1 2 127.72(11)
N2 Mn1 O2 C1 . -161.05(10)
O1 Mn1 O2 C1 . -6.26(8)
O3 Mn1 O2 C1 2 8.73(13)
Mn1 O2 C1 O1 . 11.55(15)
Mn1 O2 C1 C4 . -169.65(11)
Mn1 O1 C1 O2 . -10.91(14)
Mn1 O1 C1 C4 . 170.30(11)
Mn1 O3 C2 O4 2 -12.27(15)
Mn1 O3 C2 C3 2 168.61(13)
Mn1 O4 C2 O3 2 13.3(2)
Mn1 O4 C2 C3 2 -167.56(11)
O3 C2 C3 C8 . 55.5(2)
O4 C2 C3 C8 . -123.6(2)
O3 C2 C3 C4 . -61.3(2)
O4 C2 C3 C4 . 119.5(2)
O2 C1 C4 C5 . 3.6(2)
O1 C1 C4 C5 . -177.58(12)
O2 C1 C4 C3 . 120.90(15)
O1 C1 C4 C3 . -60.3(2)
C2 C3 C4 C1 . 5.0(2)
C8 C3 C4 C1 . -118.38(14)
C2 C3 C4 C5 . 127.96(14)
C8 C3 C4 C5 . 4.54(14)
C1 C4 C5 C6 . -171.50(13)
C3 C4 C5 C6 . 64.12(15)
C1 C4 C5 C9 . 83.82(15)
C3 C4 C5 C9 . -40.56(15)
C9 C5 C6 C7 . 32.3(2)
C4 C5 C6 C7 . -71.8(2)
C5 C6 C7 C8 . 1.2(2)
C6 C7 C8 C9 . -34.3(2)
C6 C7 C8 C3 . 71.1(2)
C2 C3 C8 C7 . 163.75(14)
C4 C3 C8 C7 . -71.1(2)
C2 C3 C8 C9 . -92.1(2)
C4 C3 C8 C9 . 33.0(2)
C6 C5 C9 C8 . -49.65(14)
C4 C5 C9 C8 . 59.97(14)
C7 C8 C9 C5 . 50.1(2)
C3 C8 C9 C5 . -57.46(15)
C14 N1 C10 C11 . 0.2(2)
Mn1 N1 C10 C11 . -177.80(12)
N1 C10 C11 C12 . -1.0(3)
C10 C11 C12 C13 . 0.3(3)
C11 C12 C13 C14 . 1.1(3)
C10 N1 C14 C13 . 1.3(2)
Mn1 N1 C14 C13 . 179.38(11)
C10 N1 C14 C15 . -177.96(13)
Mn1 N1 C14 C15 . 0.1(2)
C12 C13 C14 N1 . -2.0(2)
C12 C13 C14 C15 . 177.25(15)
C19 N2 C15 C16 . 0.3(2)
Mn1 N2 C15 C16 . -176.68(12)
C19 N2 C15 C14 . 180.00(13)
Mn1 N2 C15 C14 . 3.0(2)
N1 C14 C15 N2 . -2.1(2)
C13 C14 C15 N2 . 178.65(14)
N1 C14 C15 C16 . 177.63(14)
C13 C14 C15 C16 . -1.6(2)
N2 C15 C16 C17 . 1.1(3)
C14 C15 C16 C17 . -178.6(2)
C15 C16 C17 C18 . -1.3(3)
C16 C17 C18 C19 . 0.2(3)
C15 N2 C19 C18 . -1.4(2)
Mn1 N2 C19 C18 . 175.30(13)
C17 C18 C19 N2 . 1.2(3)
