#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/72/2217232.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_2217232
loop_
_publ_author_name
'Shao-Ming Ying'
'Yun Chen'
'Qiu-Yan Luo'
'Ya-Ping Xv'
'Dong-Sheng Liu'
_publ_section_title
;
 Bis(μ-carboxylatoethylphosphonato)bis[aqua(2,2'-bipyridine)manganese(II)]
;
_journal_coeditor_code           OM2188
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m166
_journal_page_last               m166
_journal_paper_doi               10.1107/S1600536807065142
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Mn2 (C5 H5 O5 P1)2 (C8 H8 N2)2 (H2 O)2]'
_chemical_formula_moiety         'C26 H30 Mn2 N4 O12 P2'
_chemical_formula_sum            'C26 H30 Mn2 N4 O12 P2'
_chemical_formula_weight         762.36
_chemical_name_systematic
;
Bis(μ-carboxylatoethylphosphonato)bis[aqua(2,2'-bipyridine)manganese(II)]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7553(13)
_cell_length_b                   18.060(3)
_cell_length_c                   20.682(3)
_cell_measurement_reflns_used    5461
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.46
_cell_volume                     3270.3(9)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and ω 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23111
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        <0.1%
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.7957
_exptl_absorpt_correction_T_min  0.7540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.604
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0301
_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)+(0.0521P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                2893
_reflns_number_total             4057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2188.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3270.3(8)
_cod_database_code               2217232
_cod_database_fobs_code          2217232
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
Mn Mn1 0.67540(3) 0.073021(14) 0.408219(13) 0.02994(10) Uani d . 1
P P1 0.84779(5) 0.19961(2) 0.50438(2) 0.03026(12) Uani d . 1
N N1 0.70029(19) 0.11228(9) 0.30583(8) 0.0409(4) Uani d . 1
N N2 0.5539(2) -0.01013(9) 0.34242(7) 0.0427(4) Uani d . 1
O O1 0.71646(15) 0.22186(7) 0.55235(6) 0.0417(3) Uani d . 1
H H1B 0.6353 0.2240 0.5327 0.062 Uiso calc R 1
O O2 0.78629(14) 0.16537(7) 0.44369(6) 0.0364(3) Uani d . 1
O O3 0.94774(14) 0.26603(7) 0.49251(7) 0.0441(3) Uani d . 1
O O4 1.29300(14) 0.01457(7) 0.51674(6) 0.0378(3) Uani d . 1
O O5 1.11488(16) 0.00513(7) 0.59060(6) 0.0419(3) Uani d . 1
O O6 0.45857(14) 0.10698(7) 0.44337(6) 0.0415(3) Uani d . 1
H H6A 0.4491 0.1514 0.4658 0.050 Uiso calc R 1
H H6B 0.3731 0.0775 0.4363 0.050 Uiso calc R 1
C C1 0.7756(3) 0.17412(12) 0.29085(11) 0.0538(6) Uani d . 1
H H1A 0.8182 0.2023 0.3239 0.065 Uiso calc R 1
C C2 0.7923(3) 0.19769(14) 0.22728(12) 0.0667(7) Uani d . 1
H H2A 0.8457 0.2408 0.2177 0.080 Uiso calc R 1
C C3 0.7284(3) 0.15608(16) 0.17906(12) 0.0703(8) Uani d . 1
H H3A 0.7376 0.1709 0.1362 0.084 Uiso calc R 1
C C4 0.6509(3) 0.09242(14) 0.19413(11) 0.0600(7) Uani d . 1
H H4A 0.6078 0.0636 0.1616 0.072 Uiso calc R 1
C C5 0.6375(2) 0.07146(11) 0.25805(9) 0.0402(5) Uani d . 1
C C6 0.5559(2) 0.00356(11) 0.27852(9) 0.0412(5) Uani d . 1
C C7 0.4850(3) -0.04431(14) 0.23502(10) 0.0582(6) Uani d . 1
H H7A 0.4878 -0.0345 0.1909 0.070 Uiso calc R 1
C C8 0.4116(3) -0.10562(16) 0.25773(12) 0.0758(8) Uani d . 1
H H8A 0.3634 -0.1377 0.2291 0.091 Uiso calc R 1
C C9 0.4089(3) -0.12002(14) 0.32312(12) 0.0773(9) Uani d . 1
H H9A 0.3599 -0.1616 0.3396 0.093 Uiso calc R 1
C C10 0.4818(3) -0.07028(12) 0.36322(11) 0.0632(7) Uani d . 1
H H10A 0.4803 -0.0794 0.4075 0.076 Uiso calc R 1
C C11 1.0934(2) 0.10444(10) 0.51376(9) 0.0380(4) Uani d . 1
H H11A 1.0651 0.0930 0.4695 0.046 Uiso calc R 1
H H11B 1.1671 0.1445 0.5123 0.046 Uiso calc R 1
C C12 1.1699(2) 0.03742(10) 0.54257(9) 0.0314(4) Uani d . 1
C C13 0.9522(2) 0.13154(10) 0.54921(9) 0.0393(4) Uani d . 1
H H13A 0.9828 0.1526 0.5904 0.047 Uiso calc R 1
H H13B 0.8860 0.0897 0.5580 0.047 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'
P P 0.1023 0.0942 '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
O2 Mn1 O6 . . 93.75(5)
O2 Mn1 O4 . 5_756 105.49(5)
O6 Mn1 O4 . 5_756 94.44(5)
O2 Mn1 N1 . . 91.97(6)
O6 Mn1 N1 . . 108.58(6)
O4 Mn1 N1 5_756 . 150.19(5)
O2 Mn1 N2 . . 163.71(5)
O6 Mn1 N2 . . 88.71(6)
O4 Mn1 N2 5_756 . 90.35(6)
N1 Mn1 N2 . . 72.02(6)
O2 Mn1 O5 . 5_756 96.64(5)
O6 Mn1 O5 . 5_756 151.79(5)
O4 Mn1 O5 5_756 5_756 57.51(4)
N1 Mn1 O5 . 5_756 97.21(5)
N2 Mn1 O5 . 5_756 88.57(6)
O2 Mn1 C12 . 5_756 103.54(5)
O6 Mn1 C12 . 5_756 123.35(6)
O4 Mn1 C12 5_756 5_756 29.05(5)
N1 Mn1 C12 . 5_756 123.89(6)
N2 Mn1 C12 . 5_756 88.38(6)
O5 Mn1 C12 5_756 5_756 28.49(5)
O2 P1 O3 . . 113.64(8)
O2 P1 O1 . . 111.80(8)
O3 P1 O1 . . 108.95(8)
O2 P1 C13 . . 109.49(8)
O3 P1 C13 . . 109.55(9)
O1 P1 C13 . . 102.85(8)
C1 N1 C5 . . 119.24(18)
C1 N1 Mn1 . . 122.14(15)
C5 N1 Mn1 . . 118.61(13)
C10 N2 C6 . . 118.37(18)
C10 N2 Mn1 . . 124.41(14)
C6 N2 Mn1 . . 117.22(13)
P1 O1 H1B . . 109.5
P1 O2 Mn1 . . 143.09(8)
C12 O4 Mn1 . 5_756 92.45(11)
C12 O5 Mn1 . 5_756 89.27(11)
Mn1 O6 H6A . . 120.0
Mn1 O6 H6B . . 120.0
H6A O6 H6B . . 120.0
N1 C1 C2 . . 121.9(2)
N1 C1 H1A . . 119.1
C2 C1 H1A . . 119.1
C3 C2 C1 . . 118.6(2)
C3 C2 H2A . . 120.7
C1 C2 H2A . . 120.7
C2 C3 C4 . . 119.8(2)
C2 C3 H3A . . 120.1
C4 C3 H3A . . 120.1
C3 C4 C5 . . 119.3(2)
C3 C4 H4A . . 120.3
C5 C4 H4A . . 120.3
N1 C5 C4 . . 121.1(2)
N1 C5 C6 . . 116.05(16)
C4 C5 C6 . . 122.8(2)
N2 C6 C7 . . 120.96(19)
N2 C6 C5 . . 116.09(17)
C7 C6 C5 . . 122.95(18)
C8 C7 C6 . . 119.4(2)
C8 C7 H7A . . 120.3
C6 C7 H7A . . 120.3
C7 C8 C9 . . 120.0(2)
C7 C8 H8A . . 120.0
C9 C8 H8A . . 120.0
C8 C9 C10 . . 117.4(2)
C8 C9 H9A . . 121.3
C10 C9 H9A . . 121.3
N2 C10 C9 . . 123.9(2)
N2 C10 H10A . . 118.0
C9 C10 H10A . . 118.0
C12 C11 C13 . . 115.46(16)
C12 C11 H11A . . 108.4
C13 C11 H11A . . 108.4
C12 C11 H11B . . 108.4
C13 C11 H11B . . 108.4
H11A C11 H11B . . 107.5
O5 C12 O4 . . 120.64(17)
O5 C12 C11 . . 121.25(16)
O4 C12 C11 . . 118.11(16)
O5 C12 Mn1 . 5_756 62.24(10)
O4 C12 Mn1 . 5_756 58.50(9)
C11 C12 Mn1 . 5_756 175.17(13)
C11 C13 P1 . . 112.77(13)
C11 C13 H13A . . 109.0
P1 C13 H13A . . 109.0
C11 C13 H13B . . 109.0
P1 C13 H13B . . 109.0
H13A C13 H13B . . 107.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O2 . 2.0646(12)
Mn1 O6 . 2.1233(13)
Mn1 O4 5_756 2.2334(13)
Mn1 N1 . 2.2437(16)
Mn1 N2 . 2.2890(16)
Mn1 O5 5_756 2.3161(14)
Mn1 C12 5_756 2.6170(18)
P1 O2 . 1.4993(13)
P1 O3 . 1.5050(13)
P1 O1 . 1.5710(13)
P1 C13 . 1.7909(18)
N1 C1 . 1.334(2)
N1 C5 . 1.350(3)
N2 C10 . 1.328(2)
N2 C6 . 1.345(2)
O1 H1B . 0.8200
O4 C12 . 1.272(2)
O4 Mn1 5_756 2.2334(13)
O5 C12 . 1.248(2)
O5 Mn1 5_756 2.3161(14)
O6 H6A . 0.9300
O6 H6B . 0.9300
C1 C2 . 1.390(3)
C1 H1A . 0.9300
C2 C3 . 1.368(4)
C2 H2A . 0.9300
C3 C4 . 1.371(4)
C3 H3A . 0.9300
C4 C5 . 1.380(3)
C4 H4A . 0.9300
C5 C6 . 1.481(3)
C6 C7 . 1.394(3)
C7 C8 . 1.364(3)
C7 H7A . 0.9300
C8 C9 . 1.377(3)
C8 H8A . 0.9300
C9 C10 . 1.379(3)
C9 H9A . 0.9300
C10 H10A . 0.9300
C11 C12 . 1.506(2)
C11 C13 . 1.518(2)
C11 H11A . 0.9700
C11 H11B . 0.9700
C12 Mn1 5_756 2.6170(18)
C13 H13A . 0.9700
C13 H13B . 0.9700
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
O6 H6B O4 1_455 0.93 2.13 2.6813(18) 116.6
O1 H1B O3 4_456 0.82 1.73 2.5385(19) 167.4
