#------------------------------------------------------------------------------
#$Date: 2016-02-14 05:40:26 +0100 (dom 14 de feb de 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/70/1517059.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_1517059
loop_
_publ_author_name
'Tiffany M. Smith'
'Diona Symester'
'Kathryn Perrin'
'Jose Vargas'
'Michael Tichenor'
'Charles J. O-Connor'
'Jon Zubieta'
_publ_section_title
;
 Hydrothermal syntheses and structural chemistry of Mn(II), Co(II) and
 Ni(II) coordination polymers with xylyl-diphosphonate ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              46
_journal_page_last               59
_journal_volume                  402
_journal_year                    2013
_chemical_formula_moiety         'C18 H18 Mn N2 O6 P2'
_chemical_formula_sum            'C18 H18 Mn N2 O6 P2'
_chemical_formula_weight         475.22
_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
_cell_angle_alpha                96.309(4)
_cell_angle_beta                 91.689(4)
_cell_angle_gamma                94.815(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6596(14)
_cell_length_b                   10.843(2)
_cell_length_c                   11.025(2)
_cell_measurement_reflns_used    4610
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.12
_cell_measurement_theta_min      2.50
_cell_volume                     906.2(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2011)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2011)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16131
_diffrn_reflns_theta_full        32.17
_diffrn_reflns_theta_max         32.17
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         6279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0349
_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)+(0.0380P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                4976
_reflns_number_total             6279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-402-46-59-2.cif
_cod_data_source_block           compound_2
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1517059
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
Mn1 Mn 0.24415(3) 0.97071(2) 0.65269(2) 0.00716(6) Uani 1 1 d .
P1 P 0.34577(5) 0.85176(4) 0.37537(4) 0.00739(8) Uani 1 1 d .
P2 P -0.14046(5) 0.82220(4) 0.54121(4) 0.00756(8) Uani 1 1 d .
O1 O 0.12498(15) 1.11925(10) 0.57744(10) 0.0099(2) Uani 1 1 d .
O2 O 0.52203(15) 1.04345(10) 0.64818(11) 0.0105(2) Uani 1 1 d .
O3 O -0.01560(15) 0.87575(10) 0.64406(10) 0.0099(2) Uani 1 1 d .
O4 O 0.29565(15) 0.84238(10) 0.50428(10) 0.0096(2) Uani 1 1 d .
O5 O 0.17472(15) 0.86340(11) 0.29457(11) 0.0110(2) Uani 1 1 d .
H5' H 0.0924 0.8751 0.3391 0.013 Uiso 1 1 calc R
O6 O -0.33516(14) 0.82096(11) 0.58363(11) 0.0113(2) Uani 1 1 d .
H6' H -0.3624 0.8927 0.5960 0.014 Uiso 1 1 calc R
N1 N 0.22247(17) 1.06624(13) 0.84628(12) 0.0098(3) Uani 1 1 d .
N2 N 0.33561(18) 0.84204(13) 0.78919(12) 0.0097(3) Uani 1 1 d .
C1 C 0.1669(2) 1.17952(16) 0.87024(15) 0.0121(3) Uani 1 1 d .
H1 H 0.1494 1.2260 0.8056 0.015 Uiso 1 1 calc R
C2 C 0.1340(2) 1.23088(16) 0.98695(16) 0.0146(3) Uani 1 1 d .
H2 H 0.0957 1.3103 1.0003 0.018 Uiso 1 1 calc R
C3 C 0.1589(2) 1.16215(17) 1.08324(16) 0.0157(3) Uani 1 1 d .
H3 H 0.1356 1.1938 1.1624 0.019 Uiso 1 1 calc R
C4 C 0.2188(2) 1.04575(16) 1.06026(15) 0.0137(3) Uani 1 1 d .
H4 H 0.2381 0.9983 1.1239 0.016 Uiso 1 1 calc R
C5 C 0.2501(2) 1.00023(15) 0.94053(15) 0.0106(3) Uani 1 1 d .
C6 C 0.3168(2) 0.87651(15) 0.90850(15) 0.0107(3) Uani 1 1 d .
C7 C 0.3602(2) 0.80028(17) 0.99664(16) 0.0159(3) Uani 1 1 d .
H7 H 0.3452 0.8248 1.0789 0.019 Uiso 1 1 calc R
C8 C 0.4258(2) 0.68805(17) 0.96043(16) 0.0178(4) Uani 1 1 d .
H8 H 0.4550 0.6359 1.0180 0.021 Uiso 1 1 calc R
C9 C 0.4478(2) 0.65381(16) 0.83813(16) 0.0147(3) Uani 1 1 d .
H9 H 0.4937 0.5792 0.8118 0.018 Uiso 1 1 calc R
C10 C 0.3998(2) 0.73315(15) 0.75558(15) 0.0116(3) Uani 1 1 d .
H10 H 0.4129 0.7097 0.6729 0.014 Uiso 1 1 calc R
C11 C -0.1206(2) 0.65844(14) 0.50188(15) 0.0102(3) Uani 1 1 d .
H11A H -0.2088 0.6274 0.4385 0.012 Uiso 1 1 calc R
H11B H -0.0069 0.6491 0.4672 0.012 Uiso 1 1 calc R
C12 C -0.1389(2) 0.57703(14) 0.60405(15) 0.0095(3) Uani 1 1 d .
C13 C -0.0158(2) 0.59380(15) 0.70120(16) 0.0118(3) Uani 1 1 d .
H13 H 0.0739 0.6576 0.7045 0.014 Uiso 1 1 calc R
C14 C -0.0258(2) 0.51605(15) 0.79306(16) 0.0135(3) Uani 1 1 d .
H14 H 0.0570 0.5280 0.8576 0.016 Uiso 1 1 calc R
C15 C -0.1591(2) 0.42051(15) 0.78895(15) 0.0117(3) Uani 1 1 d .
H15 H -0.1649 0.3685 0.8506 0.014 Uiso 1 1 calc R
C16 C -0.2843(2) 0.40218(14) 0.69292(14) 0.0092(3) Uani 1 1 d .
C17 C -0.2726(2) 0.48127(14) 0.60158(14) 0.0098(3) Uani 1 1 d .
H17 H -0.3560 0.4699 0.5374 0.012 Uiso 1 1 calc R
C18 C 0.4238(2) 0.70573(14) 0.31441(15) 0.0091(3) Uani 1 1 d .
H18A H 0.4661 0.7137 0.2333 0.011 Uiso 1 1 calc R
H18B H 0.5218 0.6881 0.3656 0.011 Uiso 1 1 calc R
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
O4 Mn1 O1 106.45(5) . .
O4 Mn1 O3 86.06(4) . .
O1 Mn1 O3 86.30(4) . .
O4 Mn1 O2 86.50(4) . .
O1 Mn1 O2 98.81(4) . .
O3 Mn1 O2 171.93(4) . .
O4 Mn1 N1 162.62(5) . .
O1 Mn1 N1 90.92(5) . .
O3 Mn1 N1 94.70(5) . .
O2 Mn1 N1 91.48(5) . .
O4 Mn1 N2 91.44(5) . .
O1 Mn1 N2 161.49(5) . .
O3 Mn1 N2 90.31(5) . .
O2 Mn1 N2 86.75(5) . .
N1 Mn1 N2 71.20(5) . .
O4 P1 O2 117.89(7) . 2_676
O4 P1 O5 108.92(7) . .
O2 P1 O5 107.21(7) 2_676 .
O4 P1 C18 108.62(7) . .
O2 P1 C18 108.82(7) 2_676 .
O5 P1 C18 104.57(7) . .
O3 P2 O1 116.71(7) . 2_576
O3 P2 O6 110.41(7) . .
O1 P2 O6 109.82(7) 2_576 .
O3 P2 C11 111.47(7) . .
O1 P2 C11 105.91(7) 2_576 .
O6 P2 C11 101.36(7) . .
P2 O1 Mn1 134.57(7) 2_576 .
P1 O2 Mn1 148.50(7) 2_676 .
P2 O3 Mn1 133.64(7) . .
P1 O4 Mn1 134.89(7) . .
P1 O5 H5' 109.5 . .
P2 O6 H6' 109.5 . .
C1 N1 C5 118.23(14) . .
C1 N1 Mn1 123.21(11) . .
C5 N1 Mn1 118.21(11) . .
C10 N2 C6 118.80(14) . .
C10 N2 Mn1 123.34(11) . .
C6 N2 Mn1 117.80(11) . .
N1 C1 C2 122.97(16) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C3 C2 C1 118.77(16) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C4 C3 C2 118.97(16) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 119.13(16) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
N1 C5 C4 121.91(16) . .
N1 C5 C6 115.72(14) . .
C4 C5 C6 122.37(15) . .
N2 C6 C7 121.28(16) . .
N2 C6 C5 116.33(14) . .
C7 C6 C5 122.38(15) . .
C8 C7 C6 119.20(16) . .
C8 C7 H7 120.4 . .
C6 C7 H7 120.4 . .
C9 C8 C7 119.42(16) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
C8 C9 C10 118.31(16) . .
C8 C9 H9 120.8 . .
C10 C9 H9 120.8 . .
N2 C10 C9 122.98(16) . .
N2 C10 H10 118.5 . .
C9 C10 H10 118.5 . .
C12 C11 P2 116.66(12) . .
C12 C11 H11A 108.1 . .
P2 C11 H11A 108.1 . .
C12 C11 H11B 108.1 . .
P2 C11 H11B 108.1 . .
H11A C11 H11B 107.3 . .
C13 C12 C17 118.65(15) . .
C13 C12 C11 119.69(14) . .
C17 C12 C11 121.60(14) . .
C14 C13 C12 120.49(15) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C13 C14 C15 120.21(15) . .
C13 C14 H14 119.9 . .
C15 C14 H14 119.9 . .
C14 C15 C16 120.37(15) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C15 C16 C17 118.70(15) . .
C15 C16 C18 120.15(14) . 2_566
C17 C16 C18 121.08(14) . 2_566
C12 C17 C16 121.58(15) . .
C12 C17 H17 119.2 . .
C16 C17 H17 119.2 . .
C16 C18 P1 112.98(11) 2_566 .
C16 C18 H18A 109.0 2_566 .
P1 C18 H18A 109.0 . .
C16 C18 H18B 109.0 2_566 .
P1 C18 H18B 109.0 . .
H18A C18 H18B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.0973(12) .
Mn1 O1 2.1474(11) .
Mn1 O3 2.1566(12) .
Mn1 O2 2.2108(12) .
Mn1 N1 2.2848(14) .
Mn1 N2 2.2947(14) .
P1 O4 1.4950(12) .
P1 O2 1.5071(12) 2_676
P1 O5 1.5842(12) .
P1 C18 1.8067(16) .
P2 O3 1.4952(12) .
P2 O1 1.5190(12) 2_576
P2 O6 1.5755(12) .
P2 C11 1.8012(16) .
O1 P2 1.5190(12) 2_576
O2 P1 1.5071(12) 2_676
O5 H5' 0.8200 .
O6 H6' 0.8200 .
N1 C1 1.335(2) .
N1 C5 1.346(2) .
N2 C10 1.336(2) .
N2 C6 1.343(2) .
C1 C2 1.384(2) .
C1 H1 0.9300 .
C2 C3 1.380(2) .
C2 H2 0.9300 .
C3 C4 1.379(2) .
C3 H3 0.9300 .
C4 C5 1.392(2) .
C4 H4 0.9300 .
C5 C6 1.485(2) .
C6 C7 1.394(2) .
C7 C8 1.379(3) .
C7 H7 0.9300 .
C8 C9 1.378(2) .
C8 H8 0.9300 .
C9 C10 1.382(2) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.508(2) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.392(2) .
C12 C17 1.393(2) .
C13 C14 1.387(2) .
C13 H13 0.9300 .
C14 C15 1.388(2) .
C14 H14 0.9300 .
C15 C16 1.394(2) .
C15 H15 0.9300 .
C16 C17 1.393(2) .
C16 C18 1.510(2) 2_566
C17 H17 0.9300 .
C18 C16 1.510(2) 2_566
C18 H18A 0.9700 .
C18 H18B 0.9700 .
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_4
O4 Mn1 O1 P2 -31.05(10) . 2_576
O3 Mn1 O1 P2 -115.84(10) . 2_576
O2 Mn1 O1 P2 57.88(10) . 2_576
N1 Mn1 O1 P2 149.52(10) . 2_576
N2 Mn1 O1 P2 164.28(11) . 2_576
O4 Mn1 O2 P1 112.26(14) . 2_676
O1 Mn1 O2 P1 6.14(14) . 2_676
O3 Mn1 O2 P1 135.1(3) . 2_676
N1 Mn1 O2 P1 -85.03(14) . 2_676
N2 Mn1 O2 P1 -156.10(14) . 2_676
O1 P2 O3 Mn1 -27.26(12) 2_576 .
O6 P2 O3 Mn1 -153.57(8) . .
C11 P2 O3 Mn1 94.58(10) . .
O4 Mn1 O3 P2 -40.02(10) . .
O1 Mn1 O3 P2 66.78(10) . .
O2 Mn1 O3 P2 -62.8(3) . .
N1 Mn1 O3 P2 157.40(10) . .
N2 Mn1 O3 P2 -131.44(10) . .
O2 P1 O4 Mn1 40.59(12) 2_676 .
O5 P1 O4 Mn1 -81.77(10) . .
C18 P1 O4 Mn1 164.89(9) . .
O1 Mn1 O4 P1 33.36(10) . .
O3 Mn1 O4 P1 118.33(10) . .
O2 Mn1 O4 P1 -64.80(10) . .
N1 Mn1 O4 P1 -148.53(13) . .
N2 Mn1 O4 P1 -151.46(10) . .
O4 Mn1 N1 C1 176.09(14) . .
O1 Mn1 N1 C1 -5.73(13) . .
O3 Mn1 N1 C1 -92.09(13) . .
O2 Mn1 N1 C1 93.11(13) . .
N2 Mn1 N1 C1 179.18(14) . .
O4 Mn1 N1 C5 -10.8(2) . .
O1 Mn1 N1 C5 167.35(12) . .
O3 Mn1 N1 C5 80.98(12) . .
O2 Mn1 N1 C5 -93.81(12) . .
N2 Mn1 N1 C5 -7.74(11) . .
O4 Mn1 N2 C10 2.71(13) . .
O1 Mn1 N2 C10 168.02(13) . .
O3 Mn1 N2 C10 88.78(13) . .
O2 Mn1 N2 C10 -83.70(13) . .
N1 Mn1 N2 C10 -176.37(14) . .
O4 Mn1 N2 C6 -174.63(12) . .
O1 Mn1 N2 C6 -9.3(2) . .
O3 Mn1 N2 C6 -88.56(12) . .
O2 Mn1 N2 C6 98.96(12) . .
N1 Mn1 N2 C6 6.29(11) . .
C5 N1 C1 C2 -1.0(2) . .
Mn1 N1 C1 C2 172.03(13) . .
N1 C1 C2 C3 -0.3(3) . .
C1 C2 C3 C4 1.2(3) . .
C2 C3 C4 C5 -0.9(3) . .
C1 N1 C5 C4 1.4(2) . .
Mn1 N1 C5 C4 -172.04(12) . .
C1 N1 C5 C6 -178.31(14) . .
Mn1 N1 C5 C6 8.27(18) . .
C3 C4 C5 N1 -0.4(3) . .
C3 C4 C5 C6 179.24(15) . .
C10 N2 C6 C7 -1.0(2) . .
Mn1 N2 C6 C7 176.48(13) . .
C10 N2 C6 C5 178.11(14) . .
Mn1 N2 C6 C5 -4.42(18) . .
N1 C5 C6 N2 -2.5(2) . .
C4 C5 C6 N2 177.81(15) . .
N1 C5 C6 C7 176.60(16) . .
C4 C5 C6 C7 -3.1(3) . .
N2 C6 C7 C8 0.8(3) . .
C5 C6 C7 C8 -178.26(16) . .
C6 C7 C8 C9 0.3(3) . .
C7 C8 C9 C10 -1.1(3) . .
C6 N2 C10 C9 0.1(2) . .
Mn1 N2 C10 C9 -177.21(12) . .
C8 C9 C10 N2 1.0(3) . .
O3 P2 C11 C12 54.48(14) . .
O1 P2 C11 C12 -177.62(11) 2_576 .
O6 P2 C11 C12 -62.98(13) . .
P2 C11 C12 C13 -64.51(19) . .
P2 C11 C12 C17 118.18(15) . .
C17 C12 C13 C14 0.4(2) . .
C11 C12 C13 C14 -176.97(15) . .
C12 C13 C14 C15 0.0(3) . .
C13 C14 C15 C16 -0.3(3) . .
C14 C15 C16 C17 0.1(2) . .
C14 C15 C16 C18 176.98(15) . 2_566
C13 C12 C17 C16 -0.6(2) . .
C11 C12 C17 C16 176.75(15) . .
C15 C16 C17 C12 0.3(2) . .
C18 C16 C17 C12 -176.52(14) 2_566 .
O4 P1 C18 C16 63.65(12) . 2_566
O2 P1 C18 C16 -166.83(11) 2_676 2_566
O5 P1 C18 C16 -52.53(13) . 2_566
