#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/06/2210678.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_2210678
loop_
_publ_author_name
'Jian-Hua Sun'
'Tong-Ming Shang'
_publ_section_title
Poly[di-μ-chloro-bis(1,10-phenanthroline)-μ₄-terephthalato-dimanganese(II)]
_journal_coeditor_code           IS2079
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2775
_journal_page_last               m2777
_journal_paper_doi               10.1107/S1600536806039134
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mn2 (C8 H4 O4) Cl2 (C12 H8 N2)2]'
_chemical_formula_moiety         'C32 H20 Cl2 Mn2 N4 O4'
_chemical_formula_sum            'C32 H20 Cl2 Mn2 N4 O4'
_chemical_formula_weight         705.30
_chemical_name_systematic
Poly[di-μ-chloro-bis(1,10-phenanthroline)-μ₄-terephthalato-dimanganese(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                 133.949(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.997(2)
_cell_length_b                   10.4104(9)
_cell_length_c                   16.2512(18)
_cell_measurement_reflns_used    2178
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.37
_cell_volume                     2801.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  'SHELXTL (Bruker, 2002)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD 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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10077
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.8211
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0447
_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)+(0.0266P)²+8.647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                2409
_reflns_number_total             2553
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            is2079.cif
_cod_data_source_block           I
_cod_original_cell_volume        2801.2(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2210678
_cod_database_fobs_code          2210678
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 -0.00748(3) 0.04700(4) 0.60835(4) 0.02163(14) Uani d . 1
Cl Cl1 -0.07616(5) -0.10466(8) 0.43997(7) 0.0317(2) Uani d . 1
O O1 0.09226(13) -0.0113(2) 0.88284(18) 0.0338(5) Uani d . 1
O O2 0.08527(14) -0.0703(2) 0.74477(18) 0.0394(6) Uani d . 1
N N1 0.05009(15) 0.2404(3) 0.7097(2) 0.0303(6) Uani d . 1
N N2 -0.09630(16) 0.2093(3) 0.4958(2) 0.0306(6) Uani d . 1
C C1 0.1214(2) 0.2564(4) 0.8147(3) 0.0423(9) Uani d . 1
H H1 0.1498 0.1838 0.8592 0.051 Uiso calc R 1
C C2 0.1563(3) 0.3763(4) 0.8622(4) 0.0591(12) Uani d . 1
H H2 0.2065 0.3830 0.9368 0.071 Uiso calc R 1
C C3 0.1163(3) 0.4825(4) 0.7986(5) 0.0674(14) Uani d . 1
H H3 0.1389 0.5632 0.8294 0.081 Uiso calc R 1
C C4 0.0411(3) 0.4716(4) 0.6867(4) 0.0527(11) Uani d . 1
C C5 -0.0056(4) 0.5794(4) 0.6128(6) 0.0759(16) Uani d . 1
H H5 0.0156 0.6618 0.6383 0.091 Uiso calc R 1
C C6 -0.0791(4) 0.5631(4) 0.5078(5) 0.0729(15) Uani d . 1
H H6 -0.1082 0.6347 0.4621 0.088 Uiso calc R 1
C C7 -0.1138(3) 0.4390(4) 0.4646(4) 0.0519(11) Uani d . 1
C C8 -0.1924(3) 0.4162(5) 0.3587(4) 0.0650(14) Uani d . 1
H H8 -0.2249 0.4850 0.3116 0.078 Uiso calc R 1
C C9 -0.2213(3) 0.2947(5) 0.3242(3) 0.0589(12) Uani d . 1
H H9 -0.2739 0.2797 0.2550 0.071 Uiso calc R 1
C C10 -0.1707(2) 0.1929(4) 0.3942(3) 0.0444(9) Uani d . 1
H H10 -0.1900 0.1096 0.3687 0.053 Uiso calc R 1
C C11 -0.0684(2) 0.3299(3) 0.5321(3) 0.0348(8) Uani d . 1
C C12 0.0100(2) 0.3469(3) 0.6456(3) 0.0343(8) Uani d . 1
C C13 0.11480(18) -0.0756(3) 0.8447(3) 0.0250(7) Uani d . 1
C C14 0.18523(17) -0.1663(3) 0.9258(2) 0.0220(6) Uani d . 1
C C15 0.21157(18) -0.1977(3) 1.0300(3) 0.0282(7) Uani d . 1
H H15 0.1860 -0.1627 1.0508 0.034 Uiso calc R 1
C C16 0.27593(18) -0.2812(3) 1.1034(3) 0.0283(7) Uani d . 1
H H16 0.2932 -0.3022 1.1732 0.034 Uiso calc R 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 Mn1 O1 . 2_556 93.98(9) yes
O2 Mn1 N2 . . 165.70(10) yes
O1 Mn1 N2 2_556 . 85.03(9) yes
O2 Mn1 N1 . . 95.37(10) yes
O1 Mn1 N1 2_556 . 107.07(9) yes
N2 Mn1 N1 . . 71.43(10) yes
O2 Mn1 Cl1 . . 101.09(7) yes
O1 Mn1 Cl1 2_556 . 88.94(6) yes
N2 Mn1 Cl1 . . 93.15(7) yes
N1 Mn1 Cl1 . . 156.19(7) yes
O2 Mn1 Cl1 . 5_556 91.77(7) yes
O1 Mn1 Cl1 2_556 5_556 169.82(6) yes
N2 Mn1 Cl1 . 5_556 91.44(7) yes
N1 Mn1 Cl1 . 5_556 80.70(7) yes
Cl1 Mn1 Cl1 . 5_556 81.71(3) yes
Mn1 Cl1 Mn1 . 5_556 98.29(3) yes
C13 O1 Mn1 . 2_556 154.2(2) ?
C13 O2 Mn1 . . 129.4(2) ?
C1 N1 C12 . . 117.6(3) ?
C1 N1 Mn1 . . 127.2(2) ?
C12 N1 Mn1 . . 114.3(2) ?
C10 N2 C11 . . 118.4(3) ?
C10 N2 Mn1 . . 124.6(2) ?
C11 N2 Mn1 . . 116.8(2) ?
N1 C1 C2 . . 123.3(4) ?
N1 C1 H1 . . 118.3 ?
C2 C1 H1 . . 118.3 ?
C3 C2 C1 . . 119.2(4) ?
C3 C2 H2 . . 120.4 ?
C1 C2 H2 . . 120.4 ?
C2 C3 C4 . . 120.1(4) ?
C2 C3 H3 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C3 C4 C12 . . 117.1(4) ?
C3 C4 C5 . . 123.9(4) ?
C12 C4 C5 . . 119.0(4) ?
C6 C5 C4 . . 121.1(4) ?
C6 C5 H5 . . 119.4 ?
C4 C5 H5 . . 119.4 ?
C5 C6 C7 . . 121.6(4) ?
C5 C6 H6 . . 119.2 ?
C7 C6 H6 . . 119.2 ?
C8 C7 C11 . . 116.5(4) ?
C8 C7 C6 . . 124.3(4) ?
C11 C7 C6 . . 119.2(4) ?
C9 C8 C7 . . 120.6(4) ?
C9 C8 H8 . . 119.7 ?
C7 C8 H8 . . 119.7 ?
C8 C9 C10 . . 118.8(4) ?
C8 C9 H9 . . 120.6 ?
C10 C9 H9 . . 120.6 ?
N2 C10 C9 . . 123.0(4) ?
N2 C10 H10 . . 118.5 ?
C9 C10 H10 . . 118.5 ?
N2 C11 C7 . . 122.6(3) ?
N2 C11 C12 . . 118.0(3) ?
C7 C11 C12 . . 119.4(3) ?
N1 C12 C4 . . 122.7(3) ?
N1 C12 C11 . . 117.7(3) ?
C4 C12 C11 . . 119.6(3) ?
O1 C13 O2 . . 125.7(3) ?
O1 C13 C14 . . 117.7(3) ?
O2 C13 C14 . . 116.5(3) ?
C16 C14 C15 7_547 . 119.2(3) ?
C16 C14 C13 7_547 . 120.2(3) ?
C15 C14 C13 . . 120.6(3) ?
C14 C15 C16 . . 120.0(3) ?
C14 C15 H15 . . 120.0 ?
C16 C15 H15 . . 120.0 ?
C14 C16 C15 7_547 . 120.8(3) ?
C14 C16 H16 7_547 . 119.6 ?
C15 C16 H16 . . 119.6 ?
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 Cl1 . 2.5448(9) yes
Mn1 Cl1 5_556 2.6024(9) yes
Mn1 O2 . 2.096(2) yes
Mn1 O1 2_556 2.140(2) yes
Mn1 N2 . 2.277(3) yes
Mn1 N1 . 2.344(3) yes
O1 C13 . 1.244(4) ?
O2 C13 . 1.253(4) ?
N1 C1 . 1.322(4) ?
N1 C12 . 1.353(4) ?
N2 C10 . 1.327(4) ?
N2 C11 . 1.346(4) ?
C1 C2 . 1.391(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.348(7) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.395(7) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.407(5) ?
C4 C5 . 1.436(7) ?
C5 C6 . 1.340(7) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.422(6) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.402(7) ?
C7 C11 . 1.412(5) ?
C8 C9 . 1.356(7) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.390(5) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.438(5) ?
C13 C14 . 1.513(4) ?
C14 C16 7_547 1.383(4) ?
C14 C15 . 1.385(4) ?
C15 C16 . 1.385(4) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
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_site_symmetry_4
_geom_torsion
O2 Mn1 Cl1 Mn1 . 5_556 -90.19(7)
O1 Mn1 Cl1 Mn1 2_556 5_556 175.96(7)
N2 Mn1 Cl1 Mn1 . 5_556 90.99(7)
N1 Mn1 Cl1 Mn1 . 5_556 42.70(17)
Cl1 Mn1 Cl1 Mn1 5_556 5_556 0.0
O1 Mn1 O2 C13 2_556 . -54.8(3)
N2 Mn1 O2 C13 . . 30.7(6)
N1 Mn1 O2 C13 . . 52.7(3)
Cl1 Mn1 O2 C13 . . -144.5(3)
Cl1 Mn1 O2 C13 5_556 . 133.6(3)
O2 Mn1 N1 C1 . . 5.0(3)
O1 Mn1 N1 C1 2_556 . 100.9(3)
N2 Mn1 N1 C1 . . 179.4(3)
Cl1 Mn1 N1 C1 . . -128.7(3)
Cl1 Mn1 N1 C1 5_556 . -85.9(3)
O2 Mn1 N1 C12 . . 174.4(2)
O1 Mn1 N1 C12 2_556 . -89.8(2)
N2 Mn1 N1 C12 . . -11.3(2)
Cl1 Mn1 N1 C12 . . 40.6(3)
Cl1 Mn1 N1 C12 5_556 . 83.4(2)
O2 Mn1 N2 C10 . . -151.2(4)
O1 Mn1 N2 C10 2_556 . -64.5(3)
N1 Mn1 N2 C10 . . -174.4(3)
Cl1 Mn1 N2 C10 . . 24.1(3)
Cl1 Mn1 N2 C10 5_556 . 105.9(3)
O2 Mn1 N2 C11 . . 34.0(5)
O1 Mn1 N2 C11 2_556 . 120.6(2)
N1 Mn1 N2 C11 . . 10.7(2)
Cl1 Mn1 N2 C11 . . -150.7(2)
Cl1 Mn1 N2 C11 5_556 . -68.9(2)
C12 N1 C1 C2 . . 0.7(5)
Mn1 N1 C1 C2 . . 169.8(3)
N1 C1 C2 C3 . . -0.5(6)
C1 C2 C3 C4 . . -0.1(7)
C2 C3 C4 C12 . . 0.5(6)
C3 C4 C5 C6 . . -177.0(5)
C12 C4 C5 C6 . . 2.7(7)
C4 C5 C6 C7 . . -0.5(8)
C5 C6 C7 C8 . . 175.6(5)
C5 C6 C7 C11 . . -2.6(7)
C11 C7 C8 C9 . . -1.0(6)
C6 C7 C8 C9 . . -179.3(4)
C7 C8 C9 C10 . . -2.0(6)
C11 N2 C10 C9 . . -0.4(5)
Mn1 N2 C10 C9 . . -175.2(3)
C8 C9 C10 N2 . . 2.8(6)
C10 N2 C11 C7 . . -2.8(5)
Mn1 N2 C11 C7 . . 172.4(3)
C10 N2 C11 C12 . . 175.5(3)
Mn1 N2 C11 C12 . . -9.3(4)
C8 C7 C11 N2 . . 3.5(5)
C6 C7 C11 N2 . . -178.1(4)
C8 C7 C11 C12 . . -174.8(3)
C6 C7 C11 C12 . . 3.6(5)
C1 N1 C12 C4 . . -0.3(5)
Mn1 N1 C12 C4 . . -170.7(3)
C1 N1 C12 C11 . . -178.7(3)
Mn1 N1 C12 C11 . . 10.9(4)
C3 C4 C12 N1 . . -0.3(6)
C5 C4 C12 N1 . . 180.0(4)
C3 C4 C12 C11 . . 178.1(3)
C5 C4 C12 C11 . . -1.6(5)
N2 C11 C12 N1 . . -1.4(4)
C7 C11 C12 N1 . . 177.0(3)
N2 C11 C12 C4 . . -179.9(3)
C7 C11 C12 C4 . . -1.4(5)
Mn1 O1 C13 O2 2_556 . 64.7(6)
Mn1 O1 C13 C14 2_556 . -116.8(4)
Mn1 O2 C13 O1 . . 1.9(5)
Mn1 O2 C13 C14 . . -176.6(2)
O1 C13 C14 C16 . 7_547 -166.0(3)
O2 C13 C14 C16 . 7_547 12.7(4)
O1 C13 C14 C15 . . 14.1(4)
O2 C13 C14 C15 . . -167.3(3)
C16 C14 C15 C16 7_547 . -0.2(5)
C13 C14 C15 C16 . . 179.7(3)
C14 C15 C16 C14 . 7_547 0.3(5)
