#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/35/2213526.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_2213526
loop_
_publ_author_name
'Yu-Li Shen'
'Sheng-Li Sun'
'Wen-Dong Song'
_publ_section_title
μ-Aqua-bis(μ-4-chlorobenzoato)bis[(4-chlorobenzoato)(1,10-phenanthroline)manganese(II)]
_journal_coeditor_code           RZ2129
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1309
_journal_page_last               m1311
_journal_paper_doi               10.1107/S1600536807017801
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Mn2 (C7 H4 Cl O2)4 (C12 H8 N2)2 (H2 O)]'
_chemical_formula_moiety         'C52 H34 Cl4 Mn2 N4 O9'
_chemical_formula_sum            'C52 H34 Cl4 Mn2 N4 O9'
_chemical_formula_weight         1110.51
_chemical_name_systematic
;
μ-Aqua-bis(μ-4-chlorobenzoato)bis[(4-chlorobenzoato)(1,10-
phenanthroline)manganese(II)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.0120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4037(4)
_cell_length_b                   15.5866(3)
_cell_length_c                   15.5960(3)
_cell_measurement_reflns_used    2567
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.12
_cell_volume                     4875.96(16)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16907
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.8695
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0448
_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)+(0.049P)²+3.6113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                3220
_reflns_number_total             4789
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rz2129.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2213526
_cod_database_fobs_code          2213526
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'
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
Mn Mn1 0.95729(2) 0.14240(3) 0.61870(3) 0.04110(15) Uani d . 1
Cl Cl1 1.09812(10) 0.46735(12) 0.30516(12) 0.1513(7) Uani d . 1
Cl Cl2 1.23754(9) -0.29182(9) 0.85550(12) 0.1410(7) Uani d . 1
O O1 1.01247(11) 0.20592(14) 0.56182(17) 0.0590(6) Uani d . 1
O O1W 1.0000 0.23392(18) 0.7500 0.0459(7) Uani d S 1
H H1W 1.0169 0.2680 0.7269 0.069 Uiso d R 1
O O2 1.03880(12) 0.32596(15) 0.65308(17) 0.0658(6) Uani d . 1
O O3 1.02047(10) 0.03192(13) 0.66629(15) 0.0522(5) Uani d . 1
N N1 0.88572(12) 0.06835(16) 0.47941(17) 0.0472(6) Uani d . 1
N N2 0.86796(12) 0.23075(17) 0.52395(18) 0.0493(6) Uani d . 1
C C1 0.89484(17) -0.0113(2) 0.4579(2) 0.0569(8) Uani d . 1
H H1 0.9358 -0.0375 0.4994 0.068 Uiso calc R 1
C C2 0.8458(2) -0.0575(3) 0.3758(3) 0.0725(11) Uani d . 1
H H2 0.8538 -0.1131 0.3630 0.087 Uiso calc R 1
C C3 0.7862(2) -0.0189(3) 0.3155(3) 0.0807(13) Uani d . 1
H H3 0.7530 -0.0485 0.2607 0.097 Uiso calc R 1
C C4 0.77390(17) 0.0654(3) 0.3347(2) 0.0649(10) Uani d . 1
C C5 0.71301(19) 0.1104(4) 0.2739(3) 0.0842(13) Uani d . 1
H H5 0.6782 0.0829 0.2187 0.101 Uiso calc R 1
C C6 0.70494(18) 0.1905(4) 0.2942(3) 0.0831(13) Uani d . 1
H H6 0.6645 0.2178 0.2528 0.100 Uiso calc R 1
C C7 0.75674(16) 0.2363(3) 0.3783(2) 0.0637(10) Uani d . 1
C C8 0.75078(18) 0.3214(3) 0.4032(3) 0.0732(11) Uani d . 1
H H8 0.7116 0.3519 0.3636 0.088 Uiso calc R 1
C C9 0.80229(18) 0.3585(3) 0.4850(3) 0.0705(10) Uani d . 1
H H9 0.7989 0.4149 0.5013 0.085 Uiso calc R 1
C C10 0.86019(17) 0.3121(2) 0.5445(3) 0.0585(9) Uani d . 1
H H10 0.8950 0.3384 0.6008 0.070 Uiso calc R 1
C C11 0.81723(14) 0.1926(2) 0.4411(2) 0.0497(8) Uani d . 1
C C12 0.82598(15) 0.1063(2) 0.4187(2) 0.0501(8) Uani d . 1
C C13 1.03232(14) 0.2832(2) 0.5810(2) 0.0492(8) Uani d . 1
C C14 1.04923(15) 0.3275(2) 0.5114(2) 0.0519(8) Uani d . 1
C C15 1.0576(2) 0.2830(3) 0.4425(3) 0.0745(11) Uani d . 1
H H15 1.0527 0.2237 0.4381 0.089 Uiso calc R 1
C C16 1.0735(2) 0.3265(3) 0.3790(3) 0.0977(15) Uani d . 1
H H16 1.0795 0.2963 0.3328 0.117 Uiso calc R 1
C C17 1.0799(2) 0.4125(3) 0.3853(3) 0.0873(13) Uani d . 1
C C18 1.0718(2) 0.4579(3) 0.4534(3) 0.0842(12) Uani d . 1
H H18 1.0760 0.5173 0.4568 0.101 Uiso calc R 1
C C19 1.05719(17) 0.4147(2) 0.5169(3) 0.0654(10) Uani d . 1
H H19 1.0527 0.4453 0.5642 0.079 Uiso calc R 1
C C20 1.07326(14) 0.0284(2) 0.7503(2) 0.0445(7) Uani d . 1
C C21 1.11302(15) -0.05360(19) 0.7768(2) 0.0460(7) Uani d . 1
C C22 1.09239(18) -0.1213(2) 0.7109(3) 0.0574(9) Uani d . 1
H H22 1.0527 -0.1174 0.6496 0.069 Uiso calc R 1
C C23 1.1304(2) -0.1947(2) 0.7354(3) 0.0768(12) Uani d . 1
H H23 1.1163 -0.2409 0.6915 0.092 Uiso calc R 1
C C24 1.1897(2) -0.1988(3) 0.8260(4) 0.0839(13) Uani d . 1
C C25 1.2111(2) -0.1322(3) 0.8921(3) 0.0850(13) Uani d . 1
H H25 1.2512 -0.1356 0.9527 0.102 Uiso calc R 1
C C26 1.17241(17) -0.0603(2) 0.8678(3) 0.0644(9) Uani d . 1
H H26 1.1861 -0.0150 0.9130 0.077 Uiso calc R 1
O O4 1.09546(10) 0.08829(13) 0.81304(16) 0.0529(5) Uani 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'
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'
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'
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
O3 Mn1 O1 . . 93.40(8) y
O3 Mn1 O4 . 2_756 89.04(8) y
O1 Mn1 O4 . 2_756 174.36(9) y
O3 Mn1 N1 . . 87.70(9) y
O1 Mn1 N1 . . 98.28(9) y
O4 Mn1 N1 2_756 . 86.90(8) y
O3 Mn1 O1W . . 106.84(7) y
O1 Mn1 O1W . . 90.22(7) y
O4 Mn1 O1W 2_756 . 84.19(7) y
N1 Mn1 O1W . . 162.76(7) y
O3 Mn1 N2 . . 160.80(9) y
O1 Mn1 N2 . . 89.97(9) y
O4 Mn1 N2 2_756 . 89.38(8) y
N1 Mn1 N2 . . 73.11(9) y
O1W Mn1 N2 . . 92.03(8) y
C13 O1 Mn1 . . 124.4(2) ?
Mn1 O1W Mn1 . 2_756 101.82(11) ?
Mn1 O1W H1W . . 95.5 ?
Mn1 O1W H1W 2_756 . 134.1 ?
C20 O3 Mn1 . . 122.0(2) ?
C1 N1 C12 . . 118.2(3) ?
C1 N1 Mn1 . . 125.6(2) ?
C12 N1 Mn1 . . 115.8(2) ?
C10 N2 C11 . . 118.7(3) ?
C10 N2 Mn1 . . 127.1(2) ?
C11 N2 Mn1 . . 114.1(2) ?
N1 C1 C2 . . 123.2(3) ?
N1 C1 H1 . . 118.4 ?
C2 C1 H1 . . 118.4 ?
C3 C2 C1 . . 118.2(4) ?
C3 C2 H2 . . 120.9 ?
C1 C2 H2 . . 120.9 ?
C2 C3 C4 . . 121.0(3) ?
C2 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
C12 C4 C3 . . 116.6(3) ?
C12 C4 C5 . . 119.3(4) ?
C3 C4 C5 . . 124.1(4) ?
C6 C5 C4 . . 121.4(4) ?
C6 C5 H5 . . 119.3 ?
C4 C5 H5 . . 119.3 ?
C5 C6 C7 . . 122.0(4) ?
C5 C6 H6 . . 119.0 ?
C7 C6 H6 . . 119.0 ?
C8 C7 C11 . . 117.9(3) ?
C8 C7 C6 . . 124.3(4) ?
C11 C7 C6 . . 117.8(4) ?
C9 C8 C7 . . 119.7(3) ?
C9 C8 H8 . . 120.1 ?
C7 C8 H8 . . 120.1 ?
C8 C9 C10 . . 119.8(4) ?
C8 C9 H9 . . 120.1 ?
C10 C9 H9 . . 120.1 ?
N2 C10 C9 . . 122.6(3) ?
N2 C10 H10 . . 118.7 ?
C9 C10 H10 . . 118.7 ?
N2 C11 C7 . . 121.4(3) ?
N2 C11 C12 . . 118.5(3) ?
C7 C11 C12 . . 120.1(3) ?
N1 C12 C4 . . 122.8(3) ?
N1 C12 C11 . . 117.8(3) ?
C4 C12 C11 . . 119.4(3) ?
O2 C13 O1 . . 125.4(3) ?
O2 C13 C14 . . 116.8(3) ?
O1 C13 C14 . . 117.8(3) ?
C19 C14 C15 . . 118.7(3) ?
C19 C14 C13 . . 119.3(3) ?
C15 C14 C13 . . 122.0(3) ?
C14 C15 C16 . . 120.3(4) ?
C14 C15 H15 . . 119.8 ?
C16 C15 H15 . . 119.8 ?
C17 C16 C15 . . 119.5(4) ?
C17 C16 H16 . . 120.3 ?
C15 C16 H16 . . 120.3 ?
C16 C17 C18 . . 121.0(4) ?
C16 C17 Cl1 . . 119.8(4) ?
C18 C17 Cl1 . . 119.1(4) ?
C17 C18 C19 . . 119.3(4) ?
C17 C18 H18 . . 120.3 ?
C19 C18 H18 . . 120.3 ?
C14 C19 C18 . . 121.1(4) ?
C14 C19 H19 . . 119.4 ?
C18 C19 H19 . . 119.4 ?
O4 C20 O3 . . 124.7(3) ?
O4 C20 C21 . . 117.9(3) ?
O3 C20 C21 . . 117.4(3) ?
C22 C21 C26 . . 119.2(3) ?
C22 C21 C20 . . 121.0(3) ?
C26 C21 C20 . . 119.7(3) ?
C21 C22 C23 . . 120.1(3) ?
C21 C22 H22 . . 119.9 ?
C23 C22 H22 . . 119.9 ?
C22 C23 C24 . . 119.2(4) ?
C22 C23 H23 . . 120.4 ?
C24 C23 H23 . . 120.4 ?
C25 C24 C23 . . 121.5(4) ?
C25 C24 Cl2 . . 120.0(4) ?
C23 C24 Cl2 . . 118.6(4) ?
C24 C25 C26 . . 118.9(4) ?
C24 C25 H25 . . 120.6 ?
C26 C25 H25 . . 120.6 ?
C25 C26 C21 . . 121.1(4) ?
C25 C26 H26 . . 119.5 ?
C21 C26 H26 . . 119.5 ?
C20 O4 Mn1 . 2_756 124.00(18) ?
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 O3 . 2.138(2) y
Mn1 O1 . 2.148(2) y
Mn1 O4 2_756 2.173(2) y
Mn1 N1 . 2.260(2) y
Mn1 O1W . 2.2624(18) y
Mn1 N2 . 2.295(2) y
Cl1 C17 . 1.739(4) ?
Cl2 C24 . 1.742(4) ?
O1 C13 . 1.270(4) ?
O1W Mn1 2_756 2.2623(18) ?
O1W H1W . 0.8456 ?
O2 C13 . 1.247(4) ?
O3 C20 . 1.256(3) ?
N1 C1 . 1.331(4) ?
N1 C12 . 1.355(4) ?
N2 C10 . 1.343(4) ?
N2 C11 . 1.360(4) ?
C1 C2 . 1.400(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.356(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.410(6) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.401(4) ?
C4 C5 . 1.424(6) ?
C5 C6 . 1.326(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.435(5) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.409(5) ?
C7 C11 . 1.413(4) ?
C8 C9 . 1.353(5) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.387(5) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.431(5) ?
C13 C14 . 1.502(4) ?
C14 C19 . 1.369(5) ?
C14 C15 . 1.375(5) ?
C15 C16 . 1.400(5) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.346(6) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.369(6) ?
C18 C19 . 1.377(5) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
C20 O4 . 1.256(3) ?
C20 C21 . 1.507(4) ?
C21 C22 . 1.375(4) ?
C21 C26 . 1.387(4) ?
C22 C23 . 1.378(5) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.381(6) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.364(6) ?
C25 C26 . 1.365(5) ?
C25 H25 . 0.9300 ?
C26 H26 . 0.9300 ?
O4 Mn1 2_756 2.173(2) ?
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 H1W O2 . 0.85 1.74 2.565(3) 166.5
C1 H1 O3 . 0.93 2.56 3.133(3) 120.1
C8 H8 O4 8_455 0.93 2.58 3.450(5) 155.5
