#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:18:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179747 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/43/7004340.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7004340
loop_
_publ_author_name
'Murugavel, Ramaswamy'
'Shanmugan, Swaminathan'
_publ_section_title
;
 Assembling metal phosphonates in the presence of monodentate-terminal
 and bidentate-bridging pyridine ligands. Use of non-covalent and
 covalent-coordinate interactions to build polymeric metal--phosphonate
 architectures
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              5358
_journal_page_last               5367
_journal_paper_doi               10.1039/b805848b
_journal_year                    2008
_chemical_formula_moiety         'C18 H32 Mn1 N2 O8 P2'
_chemical_formula_sum            'C18 H32 Mn N2 O8 P2'
_chemical_formula_weight         521.34
_chemical_name_systematic
;
?
;
_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                76.67(2)
_cell_angle_beta                 81.426(19)
_cell_angle_gamma                79.53(2)
_cell_formula_units_Z            1
_cell_length_a                   6.6570(17)
_cell_length_b                   8.896(2)
_cell_length_c                   10.671(2)
_cell_measurement_reflns_used    3818
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4099
_cell_measurement_theta_min      3.3911
_cell_volume                     600.9(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'OXFORD DIFFRACTIOM X CALIBUR-S'
_diffrn_measurement_method       'omega(w)-q scan'
_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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5168
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.9115
_exptl_absorpt_correction_T_min  0.7799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             273
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0314
_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)+(0.0611P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                1694
_reflns_number_total             2101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805848b.txt
_cod_data_source_block           newrm107relable
_cod_database_code               7004340
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C4 C 0.0082(5) 0.5514(4) 0.2745(3) 0.0803(10) Uani 1 1 d . . .
H4A H -0.0293 0.5087 0.2059 0.120 Uiso 1 1 calc R . .
H4B H -0.0604 0.6596 0.2684 0.120 Uiso 1 1 calc R . .
H4C H -0.0349 0.4885 0.3593 0.120 Uiso 1 1 calc R . .
C3 C 0.3032(6) 0.6120(4) 0.3652(3) 0.0806(10) Uani 1 1 d . . .
H3A H 0.2352 0.7204 0.3597 0.121 Uiso 1 1 calc R . .
H3B H 0.4526 0.6088 0.3545 0.121 Uiso 1 1 calc R . .
H3C H 0.2608 0.5488 0.4499 0.121 Uiso 1 1 calc R . .
Mn1 Mn 0.0000 1.0000 0.0000 0.02778(17) Uani 1 2 d S . .
P1 P 0.32367(8) 0.66528(6) 0.10245(5) 0.02933(18) Uani 1 1 d . . .
O2 O 0.5563(2) 0.63903(17) 0.07899(15) 0.0369(4) Uani 1 1 d . . .
O1 O 0.2271(2) 0.83262(16) 0.09771(14) 0.0346(4) Uani 1 1 d . . .
O3 O 0.2316(3) 0.6034(2) -0.00108(17) 0.0375(4) Uani 1 1 d . . .
O111 O -0.1365(3) 0.8054(2) -0.03797(19) 0.0408(4) Uani 1 1 d . . .
N1 N 0.2018(3) 0.9918(2) -0.19312(17) 0.0373(5) Uani 1 1 d . . .
C7 C 0.4377(3) 0.9981(3) -0.4356(2) 0.0373(5) Uani 1 1 d . . .
C1 C 0.2426(4) 0.5471(3) 0.2590(2) 0.0430(6) Uani 1 1 d . . .
C8 C 0.5141(4) 1.0243(3) -0.3310(2) 0.0469(6) Uani 1 1 d . . .
H8 H 0.6510 1.0452 -0.3398 0.056 Uiso 1 1 calc R . .
C6 C 0.2411(4) 0.9615(5) -0.4126(3) 0.0739(10) Uani 1 1 d . . .
H6 H 0.1820 0.9367 -0.4796 0.089 Uiso 1 1 calc R . .
C9 C 0.3937(4) 1.0208(3) -0.2132(2) 0.0465(6) Uani 1 1 d . . .
H9 H 0.4515 1.0400 -0.1433 0.056 Uiso 1 1 calc R . .
C2 C 0.3482(6) 0.3770(3) 0.2683(3) 0.0719(9) Uani 1 1 d . . .
H2A H 0.3090 0.3348 0.1999 0.108 Uiso 1 1 calc R . .
H2B H 0.3052 0.3144 0.3532 0.108 Uiso 1 1 calc R . .
H2C H 0.4976 0.3733 0.2578 0.108 Uiso 1 1 calc R . .
C5 C 0.1301(4) 0.9606(5) -0.2928(3) 0.0736(10) Uani 1 1 d . . .
H5 H -0.0056 0.9362 -0.2805 0.088 Uiso 1 1 calc R . .
H112 H -0.055(6) 0.744(4) -0.029(3) 0.077(13) Uiso 1 1 d . . .
H3 H 0.287(5) 0.537(3) -0.011(3) 0.058(11) Uiso 1 1 d . . .
H111 H -0.240(5) 0.766(4) -0.005(3) 0.078(12) Uiso 1 1 d . . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 Mn1 O1 180.00(7) 2_575 . ?
O1 Mn1 O111 89.49(7) 2_575 2_575 ?
O1 Mn1 O111 90.51(7) . 2_575 ?
O1 Mn1 O111 90.51(7) 2_575 . ?
O1 Mn1 O111 89.49(7) . . ?
O111 Mn1 O111 180.00(9) 2_575 . ?
O1 Mn1 N1 90.48(6) 2_575 . ?
O1 Mn1 N1 89.52(6) . . ?
O111 Mn1 N1 94.00(7) 2_575 . ?
O111 Mn1 N1 86.00(7) . . ?
O1 Mn1 N1 89.52(6) 2_575 2_575 ?
O1 Mn1 N1 90.48(6) . 2_575 ?
O111 Mn1 N1 86.00(7) 2_575 2_575 ?
O111 Mn1 N1 94.00(7) . 2_575 ?
N1 Mn1 N1 180.00(9) . 2_575 ?
O1 P1 O2 114.81(9) . . ?
O1 P1 O3 107.95(9) . . ?
O2 P1 O3 109.85(9) . . ?
O1 P1 C1 109.11(10) . . ?
O2 P1 C1 109.16(11) . . ?
O3 P1 C1 105.55(11) . . ?
O1 P1 H3 126.2(9) . . ?
O2 P1 H3 95.1(9) . . ?
O3 P1 H3 18.9(9) . . ?
C1 P1 H3 100.6(9) . . ?
P1 O1 Mn1 138.50(9) . . ?
P1 O3 H3 110(3) . . ?
Mn1 O111 H112 101(3) . . ?
Mn1 O111 H111 132(2) . . ?
H112 O111 H111 105(3) . . ?
C9 N1 C5 116.1(2) . . ?
C9 N1 Mn1 122.42(15) . . ?
C5 N1 Mn1 121.44(16) . . ?
C8 C7 C6 115.7(2) . . ?
C8 C7 C7 122.3(3) . 2_674 ?
C6 C7 C7 121.9(3) . 2_674 ?
C3 C1 C2 109.3(2) . . ?
C3 C1 C4 110.1(3) . . ?
C2 C1 C4 108.9(3) . . ?
C3 C1 P1 108.83(19) . . ?
C2 C1 P1 109.91(17) . . ?
C4 C1 P1 109.76(19) . . ?
C7 C8 C9 120.7(2) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C5 C6 C7 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
N1 C9 C8 123.2(2) . . ?
N1 C9 H9 118.4 . . ?
C8 C9 H9 118.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C5 C6 123.8(3) . . ?
N1 C5 H5 118.1 . . ?
C6 C5 H5 118.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C4 C1 1.538(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 C1 1.518(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
Mn1 O1 2.1272(16) 2_575 ?
Mn1 O1 2.1272(16) . ?
Mn1 O111 2.2342(18) 2_575 ?
Mn1 O111 2.2342(18) . ?
Mn1 N1 2.2944(18) . ?
Mn1 N1 2.2944(18) 2_575 ?
P1 O1 1.5031(15) . ?
P1 O2 1.5149(16) . ?
P1 O3 1.5828(18) . ?
P1 C1 1.820(2) . ?
P1 H3 1.92(3) . ?
O3 H3 0.66(3) . ?
O111 H112 0.70(3) . ?
O111 H111 0.82(4) . ?
N1 C9 1.326(3) . ?
N1 C5 1.331(3) . ?
C7 C8 1.375(3) . ?
C7 C6 1.379(4) . ?
C7 C7 1.493(4) 2_674 ?
C1 C2 1.536(4) . ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C6 C5 1.377(4) . ?
C6 H6 0.9500 . ?
C9 H9 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C5 H5 0.9500 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 Mn1 126.22(13) . . . . ?
O3 P1 O1 Mn1 3.33(16) . . . . ?
C1 P1 O1 Mn1 -110.90(15) . . . . ?
O1 Mn1 O1 P1 118(100) 2_575 . . . ?
O111 Mn1 O1 P1 -158.22(14) 2_575 . . . ?
O111 Mn1 O1 P1 21.78(14) . . . . ?
N1 Mn1 O1 P1 -64.23(14) . . . . ?
N1 Mn1 O1 P1 115.77(14) 2_575 . . . ?
O1 Mn1 N1 C9 123.75(19) 2_575 . . . ?
O1 Mn1 N1 C9 -56.25(19) . . . . ?
O111 Mn1 N1 C9 34.2(2) 2_575 . . . ?
O111 Mn1 N1 C9 -145.8(2) . . . . ?
N1 Mn1 N1 C9 -174(100) 2_575 . . . ?
O1 Mn1 N1 C5 -54.8(2) 2_575 . . . ?
O1 Mn1 N1 C5 125.2(2) . . . . ?
O111 Mn1 N1 C5 -144.4(2) 2_575 . . . ?
O111 Mn1 N1 C5 35.6(2) . . . . ?
N1 Mn1 N1 C5 8(100) 2_575 . . . ?
O1 P1 C1 C3 -57.5(2) . . . . ?
O2 P1 C1 C3 68.7(2) . . . . ?
O3 P1 C1 C3 -173.3(2) . . . . ?
O1 P1 C1 C2 -177.2(2) . . . . ?
O2 P1 C1 C2 -51.0(2) . . . . ?
O3 P1 C1 C2 67.0(2) . . . . ?
O1 P1 C1 C4 63.0(2) . . . . ?
O2 P1 C1 C4 -170.8(2) . . . . ?
O3 P1 C1 C4 -52.8(2) . . . . ?
C6 C7 C8 C9 -3.0(4) . . . . ?
C7 C7 C8 C9 179.6(3) 2_674 . . . ?
C8 C7 C6 C5 3.2(5) . . . . ?
C7 C7 C6 C5 -179.4(3) 2_674 . . . ?
C5 N1 C9 C8 2.1(4) . . . . ?
Mn1 N1 C9 C8 -176.54(19) . . . . ?
C7 C8 C9 N1 0.3(4) . . . . ?
C9 N1 C5 C6 -1.9(5) . . . . ?
Mn1 N1 C5 C6 176.8(3) . . . . ?
C7 C6 C5 N1 -0.8(6) . . . . ?
