#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/98/2209847.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_2209847
loop_
_publ_author_name
'Guang-Bo Che'
'Chun-Bo Liu'
_publ_section_title
;
 A new dinuclear MnII compound with intermolecular π--π
 interactions
;
_journal_coeditor_code           HB2098
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1728
_journal_page_last               m1730
_journal_paper_doi               10.1107/S1600536806024871
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Mn2 (C7 H3 N O4)2 (C14 H8 N4)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C42 H26 Mn2 N10 O10, 2H2 O'
_chemical_formula_sum            'C42 H30 Mn2 N10 O12'
_chemical_formula_weight         976.64
_chemical_name_systematic
;
bis(μ-pyridine-2,5-dicarboxylato)bis[aqua(pyrazino[2,3-
f][1,10]phenanthroline)manganese(II)] dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.71(3)
_cell_angle_beta                 94.42(3)
_cell_angle_gamma                109.47(3)
_cell_formula_units_Z            1
_cell_length_a                   7.3813(15)
_cell_length_b                   10.044(2)
_cell_length_c                   14.052(3)
_cell_measurement_reflns_used    6037
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     970.6(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.1133
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9612
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.543
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0642
_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)+(0.05P)²+0.1792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2620
_reflns_number_total             4413
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2098.cif
_cod_data_source_block           I
_cod_database_code               2209847
_cod_database_fobs_code          2209847
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C C1 0.1484(6) -0.0429(5) 0.2213(3) 0.0357(10) Uani d . 1
H H1 0.1262 -0.0493 0.1546 0.043 Uiso calc R 1
C C2 0.0527(6) -0.1609(5) 0.2647(3) 0.0382(10) Uani d . 1
H H2 -0.0294 -0.2445 0.2279 0.046 Uiso calc R 1
C C3 0.0820(6) -0.1516(4) 0.3632(3) 0.0350(10) Uani d . 1
H H3 0.0189 -0.2285 0.3944 0.042 Uiso calc R 1
C C4 0.3004(5) 0.0859(4) 0.3667(3) 0.0244(8) Uani d . 1
C C5 0.4400(5) 0.2191(4) 0.4179(3) 0.0266(9) Uani d . 1
C C6 0.6651(6) 0.4382(5) 0.4113(3) 0.0403(11) Uani d . 1
H H6 0.7265 0.5096 0.3754 0.048 Uiso calc R 1
C C7 0.7229(7) 0.4593(5) 0.5103(3) 0.0460(12) Uani d . 1
H H7 0.8224 0.5412 0.5392 0.055 Uiso calc R 1
C C8 0.6294(6) 0.3565(5) 0.5633(3) 0.0418(11) Uani d . 1
H H8 0.6621 0.3692 0.6296 0.050 Uiso calc R 1
C C9 0.4844(6) 0.2322(5) 0.5183(3) 0.0314(9) Uani d . 1
C C10 0.2077(6) -0.0252(4) 0.4158(3) 0.0292(9) Uani d . 1
C C11 0.3794(6) 0.1181(5) 0.5697(3) 0.0313(10) Uani d . 1
C C12 0.2447(6) -0.0071(5) 0.5209(3) 0.0294(9) Uani d . 1
C C13 0.1805(7) -0.0952(6) 0.6617(3) 0.0442(12) Uani d . 1
H H13 0.1129 -0.1659 0.6966 0.053 Uiso calc R 1
C C14 0.3181(7) 0.0289(6) 0.7110(3) 0.0474(13) Uani d . 1
H H14 0.3408 0.0368 0.7777 0.057 Uiso calc R 1
C C15 0.2413(5) 0.2467(4) -0.0069(3) 0.0276(9) Uani d . 1
C C16 0.4009(5) 0.3177(4) -0.0647(3) 0.0260(9) Uani d . 1
C C17 0.5662(6) 0.2821(5) -0.0628(3) 0.0345(10) Uani d . 1
H H17 0.5770 0.2100 -0.0285 0.041 Uiso calc R 1
C C18 0.7151(6) 0.3538(4) -0.1121(3) 0.0326(10) Uani d . 1
H H18 0.8260 0.3294 -0.1127 0.039 Uiso calc R 1
C C19 0.6967(5) 0.4624(4) -0.1604(3) 0.0271(9) Uani d . 1
N N5 0.5366(4) 0.4991(3) -0.1625(2) 0.0254(7) Uani d . 1
C C21 0.8572(5) 0.5515(4) -0.2122(3) 0.0301(9) Uani d . 1
N N1 0.5278(4) 0.3225(4) 0.3657(2) 0.0306(8) Uani d . 1
N N2 0.2688(4) 0.0777(4) 0.2691(2) 0.0275(7) Uani d . 1
N N3 0.1432(5) -0.1153(4) 0.5671(3) 0.0388(9) Uani d . 1
N N4 0.4178(5) 0.1358(4) 0.6673(2) 0.0432(10) Uani d . 1
C C20 0.3913(5) 0.4251(4) -0.1163(3) 0.0252(8) Uani d . 1
H H20 0.2785 0.4473 -0.1194 0.030 Uiso calc R 1
O O1 0.2819(4) 0.1790(3) 0.05948(19) 0.0338(7) Uani d . 1
O O2 0.0819(4) 0.2597(3) -0.0247(2) 0.0410(7) Uani d . 1
O O1W 0.6746(4) 0.2682(4) 0.1776(2) 0.0414(8) Uani d D 1
O O3 0.9978(4) 0.5098(3) -0.2213(2) 0.0446(8) Uani d . 1
O O2W 0.7844(5) 0.0845(4) 0.0618(3) 0.0584(10) Uani d D 1
O O4 0.8387(4) 0.6606(3) -0.2406(2) 0.0376(7) Uani d . 1
Mn Mn1 0.40163(8) 0.27795(7) 0.20439(4) 0.02762(19) Uani d . 1
H HW12 0.779(4) 0.338(3) 0.194(3) 0.041 Uiso d D 1
H HW22 0.884(4) 0.139(3) 0.042(3) 0.041 Uiso d D 1
H HW11 0.688(5) 0.204(3) 0.140(3) 0.041 Uiso d D 1
H HW21 0.744(5) 0.003(2) 0.028(3) 0.041 Uiso d D 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'
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'
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
N2 C1 C2 . . 123.7(4) ?
N2 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C3 C2 C1 . . 118.5(4) ?
C3 C2 H2 . . 120.7 ?
C1 C2 H2 . . 120.7 ?
C2 C3 C10 . . 119.1(4) ?
C2 C3 H3 . . 120.5 ?
C10 C3 H3 . . 120.5 ?
N2 C4 C10 . . 122.3(4) ?
N2 C4 C5 . . 116.6(3) ?
C10 C4 C5 . . 121.1(3) ?
N1 C5 C9 . . 122.4(4) ?
N1 C5 C4 . . 118.2(3) ?
C9 C5 C4 . . 119.3(4) ?
N1 C6 C7 . . 123.8(4) ?
N1 C6 H6 . . 118.1 ?
C7 C6 H6 . . 118.1 ?
C8 C7 C6 . . 118.1(4) ?
C8 C7 H7 . . 121.0 ?
C6 C7 H7 . . 121.0 ?
C7 C8 C9 . . 120.2(4) ?
C7 C8 H8 . . 119.9 ?
C9 C8 H8 . . 119.9 ?
C8 C9 C5 . . 117.5(4) ?
C8 C9 C11 . . 123.4(4) ?
C5 C9 C11 . . 119.1(4) ?
C4 C10 C3 . . 118.7(4) ?
C4 C10 C12 . . 119.2(4) ?
C3 C10 C12 . . 122.1(4) ?
N4 C11 C12 . . 120.7(4) ?
N4 C11 C9 . . 118.2(4) ?
C12 C11 C9 . . 121.1(4) ?
N3 C12 C11 . . 122.4(4) ?
N3 C12 C10 . . 117.7(4) ?
C11 C12 C10 . . 119.9(4) ?
N3 C13 C14 . . 122.0(4) ?
N3 C13 H13 . . 119.0 ?
C14 C13 H13 . . 119.0 ?
N4 C14 C13 . . 123.0(4) ?
N4 C14 H14 . . 118.5 ?
C13 C14 H14 . . 118.5 ?
O2 C15 O1 . . 124.4(3) ?
O2 C15 C16 . . 118.4(3) ?
O1 C15 C16 . . 117.2(3) ?
C20 C16 C17 . . 118.2(3) ?
C20 C16 C15 . . 121.1(3) ?
C17 C16 C15 . . 120.6(3) ?
C18 C17 C16 . . 119.7(4) ?
C18 C17 H17 . . 120.2 ?
C16 C17 H17 . . 120.2 ?
C17 C18 C19 . . 118.8(3) ?
C17 C18 H18 . . 120.6 ?
C19 C18 H18 . . 120.6 ?
N5 C19 C18 . . 122.3(3) ?
N5 C19 C21 . . 115.4(3) ?
C18 C19 C21 . . 122.3(3) ?
C20 N5 C19 . . 117.8(3) ?
C20 N5 Mn1 . 2_665 128.1(2) ?
C19 N5 Mn1 . 2_665 111.1(2) ?
O4 C21 O3 . . 126.1(4) ?
O4 C21 C19 . . 117.1(3) ?
O3 C21 C19 . . 116.8(4) ?
C6 N1 C5 . . 118.0(4) ?
C6 N1 Mn1 . . 127.9(3) ?
C5 N1 Mn1 . . 114.0(3) ?
C1 N2 C4 . . 117.7(3) ?
C1 N2 Mn1 . . 124.9(3) ?
C4 N2 Mn1 . . 117.1(3) ?
C13 N3 C12 . . 115.9(4) ?
C14 N4 C11 . . 116.0(4) ?
N5 C20 C16 . . 123.2(3) ?
N5 C20 H20 . . 118.4 ?
C16 C20 H20 . . 118.4 ?
C15 O1 Mn1 . . 123.5(2) ?
Mn1 O1W HW12 . . 123(2) ?
Mn1 O1W HW11 . . 123(3) ?
HW12 O1W HW11 . . 113(3) ?
HW22 O2W HW21 . . 111(3) ?
C21 O4 Mn1 . 2_665 119.4(2) ?
O1W Mn1 O4 . 2_665 166.72(12) y
O1W Mn1 O1 . . 90.57(11) y
O4 Mn1 O1 2_665 . 96.89(11) y
O1W Mn1 N2 . . 102.65(12) y
O4 Mn1 N2 2_665 . 87.86(11) y
O1 Mn1 N2 . . 93.72(11) y
O1W Mn1 N5 . 2_665 94.60(12) y
O4 Mn1 N5 2_665 2_665 74.22(11) y
O1 Mn1 N5 . 2_665 92.22(11) y
N2 Mn1 N5 . 2_665 161.67(10) y
O1W Mn1 N1 . . 85.04(12) y
O4 Mn1 N1 2_665 . 90.46(11) y
O1 Mn1 N1 . . 164.46(11) y
N2 Mn1 N1 . . 72.82(12) y
N5 Mn1 N1 2_665 . 102.97(12) y
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
C1 N2 . 1.317(5) ?
C1 C2 . 1.389(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.373(6) ?
C2 H2 . 0.9300 ?
C3 C10 . 1.393(6) ?
C3 H3 . 0.9300 ?
C4 N2 . 1.364(5) ?
C4 C10 . 1.380(5) ?
C4 C5 . 1.464(5) ?
C5 N1 . 1.346(5) ?
C5 C9 . 1.407(5) ?
C6 N1 . 1.325(5) ?
C6 C7 . 1.396(6) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.362(6) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.397(6) ?
C8 H8 . 0.9300 ?
C9 C11 . 1.447(6) ?
C10 C12 . 1.463(5) ?
C11 N4 . 1.361(5) ?
C11 C12 . 1.389(6) ?
C12 N3 . 1.356(5) ?
C13 N3 . 1.317(5) ?
C13 C14 . 1.393(7) ?
C13 H13 . 0.9300 ?
C14 N4 . 1.321(6) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.503(5) ?
C16 C20 . 1.377(5) ?
C16 C17 . 1.381(5) ?
C17 C18 . 1.376(5) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.379(5) ?
C18 H18 . 0.9300 ?
C19 N5 . 1.350(4) ?
C19 C21 . 1.513(5) ?
N5 C20 . 1.340(5) ?
N5 Mn1 2_665 2.278(3) n
C20 H20 . 0.9300 ?
O1W HW12 . 0.849(18) ?
O1W HW11 . 0.83(4) ?
O2W HW22 . 0.846(18) ?
O2W HW21 . 0.851(18) ?
O4 Mn1 2_665 2.143(3) n
Mn1 O1W . 2.110(3) y
Mn1 O1 . 2.156(3) y
Mn1 O4 2_665 2.143(3) y
Mn1 N2 . 2.241(3) y
Mn1 N5 2_665 2.278(3) y
Mn1 N1 . 2.324(3) y
C15 O2 . 1.236(4) y
C15 O1 . 1.280(4) y
C21 O4 . 1.248(5) y
C21 O3 . 1.252(4) y
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
O1W HW11 O2W . 0.83(4) 1.89(2) 2.704(4) 166(4)
O1W HW12 O3 2_765 0.849(18) 1.818(19) 2.665(4) 176(4)
O2W HW21 O1 2_655 0.851(18) 2.04(2) 2.874(4) 165(4)
O2W HW22 O2 1_655 0.846(18) 1.93(2) 2.767(4) 170(4)
