#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/36/2213673.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_2213673
loop_
_publ_author_name
'De-Yun Ma'
'Guo-Hua Deng'
_publ_contact_author_address
;
College of Chemistry, South China University of Technology,
Guang Zhou 510640
P.R. China
;
_publ_contact_author_email       ghdeng@126.com
_publ_contact_author_fax         '86 020 87112906'
_publ_contact_author_name        'Guo-Hua Deng'
_publ_contact_author_phone       '86 020 87236747'
_publ_section_title
;catena-Poly[[[aquabis(4-chlorobenzoato-κ²O,O')manganese(II)]-μ-4,4'-bipyridine-κ²N:N']4,4'-bipyridine
 solvate]
;
_journal_coeditor_code           BH2104
_journal_date_accepted           2007-05-24
_journal_date_recd_electronic    2007-05-08
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1772
_journal_page_last               m1772
_journal_paper_category          QM
_journal_paper_doi               10.1107/S1600536807025305
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Mn (C7 H4 Cl O2)2 (C10 H8 N2) (H2 O)], C10 H8 N2'
_chemical_formula_moiety         'C24 H18 Cl2 Mn N2 O5, C10 H8 N2'
_chemical_formula_sum            'C34 H26 Cl2 Mn N4 O5'
_chemical_formula_weight         696.43
_chemical_name_systematic
;
catena-Poly[[[aquabis(4-chlorobenzoato-\
κ²O,O')manganese(II)]-μ-4,4'-bipyridine-\
κ²N:N'] 4,4'-bipyridine solvate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.369(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6900(3)
_cell_length_b                   6.1510(2)
_cell_length_c                   22.5184(6)
_cell_measurement_reflns_used    2376
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.16
_cell_volume                     1581.61(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'φ and ω'
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16828
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_correction_T_min  0.8573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0451P)²+1.3366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                2373
_reflns_number_total             3115
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bh2104.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2213673
_cod_database_fobs_code          2213673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
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 0.7981(2) 0.7343(5) 0.86400(12) 0.0350(6) Uani d . 1
C C2 0.8244(2) 0.8210(5) 0.92758(12) 0.0338(6) Uani d . 1
C C3 0.7973(3) 1.0318(5) 0.93992(14) 0.0508(8) Uani d . 1
H H3 0.7643 1.1241 0.9081 0.061 Uiso calc R 1
C C4 0.8186(3) 1.1078(6) 0.99910(15) 0.0587(9) Uani d . 1
H H4 0.7979 1.2489 1.0073 0.070 Uiso calc R 1
C C5 0.8706(3) 0.9728(6) 1.04552(14) 0.0490(8) Uani d . 1
C C6 0.8995(3) 0.7654(6) 1.03456(14) 0.0604(9) Uani d . 1
H H6 0.9350 0.6756 1.0664 0.072 Uiso calc R 1
C C7 0.8755(3) 0.6890(5) 0.97564(13) 0.0484(8) Uani d . 1
H H7 0.8942 0.5461 0.9681 0.058 Uiso calc R 1
C C8 0.5015(2) 0.7563(5) 0.76962(13) 0.0399(7) Uani d . 1
H H8 0.5481 0.8737 0.7858 0.048 Uiso calc R 1
C C9 0.3844(2) 0.7609(5) 0.77142(13) 0.0401(7) Uani d . 1
H H9 0.3534 0.8803 0.7878 0.048 Uiso calc R 1
C C10 0.3131(2) 0.5870(5) 0.74867(12) 0.0344(6) Uani d . 1
C C11 0.3641(2) 0.4174(5) 0.72347(14) 0.0427(7) Uani d . 1
H H11 0.3195 0.2978 0.7072 0.051 Uiso calc R 1
C C12 0.4821(2) 0.4272(5) 0.72261(14) 0.0419(7) Uani d . 1
H H12 0.5146 0.3127 0.7049 0.050 Uiso calc R 1
C C13 0.4107(5) 0.1163(10) 0.9169(3) 0.142(3) Uani d . 1
H H13 0.3605 -0.0024 0.9138 0.171 Uiso calc R 1
C C14 0.4212(5) 0.2464(10) 0.9674(3) 0.131(3) Uani d . 1
H H14 0.3802 0.2129 0.9973 0.157 Uiso calc R 1
C C15 0.4926(3) 0.4267(6) 0.97334(16) 0.0558(9) Uani d . 1
C C16 0.5512(3) 0.4561(6) 0.92726(16) 0.0666(10) Uani d . 1
H H16 0.6021 0.5732 0.9287 0.080 Uiso calc R 1
C C17 0.5357(4) 0.3148(7) 0.87917(17) 0.0723(11) Uani d . 1
H H17 0.5775 0.3405 0.8491 0.087 Uiso calc R 1
Cl Cl1 0.90101(10) 1.0741(2) 1.11973(4) 0.0800(3) Uani d . 1
Mn Mn1 0.7500 0.58733(9) 0.7500 0.02869(17) Uani d S 1
N N1 0.55156(17) 0.5918(4) 0.74588(10) 0.0339(5) Uani d . 1
N N2 0.4661(3) 0.1464(6) 0.87269(16) 0.0844(11) Uani d . 1
O O1 0.77094(16) 0.8643(3) 0.81989(8) 0.0410(5) Uani d . 1
O O2 0.80153(18) 0.5331(3) 0.85538(9) 0.0449(5) Uani d . 1
O O1W 0.7500 0.2327(5) 0.7500 0.0453(8) Uani d S 1
H H1W 0.739(3) 0.153(5) 0.7201(14) 0.054 Uiso 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'
Cl Cl 0.1484 0.1585 '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
O2 C1 O1 . . 121.0(3) ?
O2 C1 C2 . . 119.5(3) ?
O1 C1 C2 . . 119.5(3) ?
C3 C2 C7 . . 118.3(3) ?
C3 C2 C1 . . 121.3(3) ?
C7 C2 C1 . . 120.3(3) ?
C2 C3 C4 . . 120.7(3) ?
C2 C3 H3 . . 119.6 ?
C4 C3 H3 . . 119.6 ?
C5 C4 C3 . . 119.3(3) ?
C5 C4 H4 . . 120.4 ?
C3 C4 H4 . . 120.4 ?
C6 C5 C4 . . 121.2(3) ?
C6 C5 Cl1 . . 120.2(3) ?
C4 C5 Cl1 . . 118.6(3) ?
C5 C6 C7 . . 119.3(3) ?
C5 C6 H6 . . 120.4 ?
C7 C6 H6 . . 120.4 ?
C6 C7 C2 . . 121.2(3) ?
C6 C7 H7 . . 119.4 ?
C2 C7 H7 . . 119.4 ?
N1 C8 C9 . . 123.4(3) ?
N1 C8 H8 . . 118.3 ?
C9 C8 H8 . . 118.3 ?
C8 C9 C10 . . 119.7(3) ?
C8 C9 H9 . . 120.1 ?
C10 C9 H9 . . 120.1 ?
C11 C10 C9 . . 117.2(2) ?
C11 C10 C10 . 2_556 122.29(19) ?
C9 C10 C10 . 2_556 120.50(19) ?
C10 C11 C12 . . 119.4(3) ?
C10 C11 H11 . . 120.3 ?
C12 C11 H11 . . 120.3 ?
N1 C12 C11 . . 123.5(3) ?
N1 C12 H12 . . 118.2 ?
C11 C12 H12 . . 118.2 ?
N2 C13 C14 . . 125.1(4) ?
N2 C13 H13 . . 117.5 ?
C14 C13 H13 . . 117.5 ?
C13 C14 C15 . . 119.6(4) ?
C13 C14 H14 . . 120.2 ?
C15 C14 H14 . . 120.2 ?
C16 C15 C14 . . 115.0(3) ?
C16 C15 C15 . 3_667 122.8(4) ?
C14 C15 C15 . 3_667 122.1(4) ?
C17 C16 C15 . . 120.7(4) ?
C17 C16 H16 . . 119.6 ?
C15 C16 H16 . . 119.6 ?
N2 C17 C16 . . 124.4(4) ?
N2 C17 H17 . . 117.8 ?
C16 C17 H17 . . 117.8 ?
O1W Mn1 O1 . . 137.89(5) n
O1W Mn1 O1 . 2_656 137.89(5) ?
O1 Mn1 O1 . 2_656 84.22(10) ?
O1W Mn1 N1 . . 90.69(6) n
O1 Mn1 N1 . . 88.70(7) n
O1 Mn1 N1 2_656 . 90.28(7) ?
O1W Mn1 N1 . 2_656 90.69(6) ?
O1 Mn1 N1 . 2_656 90.28(8) n
O1 Mn1 N1 2_656 2_656 88.70(7) ?
N1 Mn1 N1 . 2_656 178.62(12) n
O1W Mn1 O2 . 2_656 81.82(5) ?
O1 Mn1 O2 . 2_656 139.99(7) ?
O1 Mn1 O2 2_656 2_656 56.30(7) n
N1 Mn1 O2 . 2_656 85.56(7) ?
N1 Mn1 O2 2_656 2_656 94.63(7) ?
O1W Mn1 O2 . . 81.82(5) n
O1 Mn1 O2 . . 56.30(7) n
O1 Mn1 O2 2_656 . 139.99(7) n
N1 Mn1 O2 . . 94.63(7) y
N1 Mn1 O2 2_656 . 85.56(7) n
O2 Mn1 O2 2_656 . 163.65(10) n
C12 N1 C8 . . 116.8(2) ?
C12 N1 Mn1 . . 122.04(18) ?
C8 N1 Mn1 . . 121.13(18) ?
C17 N2 C13 . . 115.1(4) ?
C1 O1 Mn1 . . 92.36(17) ?
C1 O2 Mn1 . . 90.38(16) ?
Mn1 O1W H1W . . 127(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
C1 O2 . 1.254(4) ?
C1 O1 . 1.262(3) ?
C1 C2 . 1.497(4) ?
C2 C3 . 1.377(4) ?
C2 C7 . 1.382(4) ?
C3 C4 . 1.383(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.371(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.356(5) ?
C5 Cl1 . 1.747(3) ?
C6 C7 . 1.378(4) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C8 N1 . 1.336(3) ?
C8 C9 . 1.378(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.385(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.382(4) ?
C10 C10 2_556 1.490(5) ?
C11 C12 . 1.385(4) ?
C11 H11 . 0.9300 ?
C12 N1 . 1.333(3) ?
C12 H12 . 0.9300 ?
C13 N2 . 1.311(6) ?
C13 C14 . 1.375(6) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.378(5) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.372(5) ?
C15 C15 3_667 1.482(7) ?
C16 C17 . 1.370(5) ?
C16 H16 . 0.9300 ?
C17 N2 . 1.306(5) ?
C17 H17 . 0.9300 ?
Mn1 O1W . 2.181(3) n
Mn1 O1 . 2.297(2) n
Mn1 O1 2_656 2.297(2) ?
Mn1 N1 . 2.302(2) n
Mn1 N1 2_656 2.302(2) ?
Mn1 O2 2_656 2.344(2) ?
Mn1 O2 . 2.344(2) n
O1W H1W . 0.82(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
O1W H1W O1 2_646 0.82(3) 1.98(3) 2.740(3) 153(3) y
C8 H8 O1 . 0.93 2.55 3.181(3) 125.0 y
