#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/56/7035690.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_7035690
loop_
_publ_author_name
'Yang, Ting-Hai'
'Silva, Ana Rosa'
'Fu, Lianshe'
'Shi, Fa-Nian'
_publ_section_title
;
 Ionothermal synthesis, crystal structure, topology and catalytic
 properties of heterometallic coordination polymers constructed from
 N-(phosphonomethyl) iminodiacetic acid.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13745
_journal_page_last               13751
_journal_paper_doi               10.1039/c5dt02176f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H42 Eu Fe7 N6 O42 P6, 2(H2 O)'
_chemical_formula_sum            'C30 H46 Eu Fe7 N6 O44 P6'
_chemical_formula_weight         1923.46
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.3720(4)
_cell_length_b                   15.3720(4)
_cell_length_c                   22.8499(17)
_cell_measurement_reflns_used    1346
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.511
_cell_measurement_theta_min      2.349
_cell_volume                     4676.0(4)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9435
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         3.77
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  0.8950
_exptl_absorpt_correction_T_min  0.8049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2864.9
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.189
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0566
_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)+(0.0412P)²+62.4848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                1835
_reflns_number_total             2577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02176f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7035690--7035693.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7035690
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Eu1 Eu 0.6667 0.3333 0.8333 0.01066(19) Uani 1 6 d S
Fe1 Fe 0.89916(7) 0.77569(7) 0.75564(4) 0.0247(3) Uani 1 1 d .
Fe2 Fe 0.6667 0.3333 0.63634(16) 0.0266(8) Uani 0.50 3 d SP
P1 P 0.75666(12) 0.54504(11) 0.72450(7) 0.0179(4) Uani 1 1 d .
N1 N 0.7308(4) 0.6988(4) 0.7627(2) 0.0218(11) Uani 1 1 d .
C1 C 0.6886(5) 0.6134(4) 0.7217(3) 0.0210(13) Uani 1 1 d .
H1A H 0.6914 0.6379 0.6823 0.025 Uiso 1 1 calc R
H1B H 0.6186 0.5682 0.7314 0.025 Uiso 1 1 calc R
C2 C 0.6994(5) 0.6617(5) 0.8234(3) 0.0293(15) Uani 1 1 d .
H2A H 0.6598 0.5889 0.8226 0.035 Uiso 1 1 calc R
H2B H 0.6566 0.6866 0.8379 0.035 Uiso 1 1 calc R
C3 C 0.7843(5) 0.6920(5) 0.8649(3) 0.0289(15) Uani 1 1 d .
C4 C 0.7030(5) 0.7761(5) 0.7463(3) 0.0297(16) Uani 1 1 d .
H4A H 0.6420 0.7621 0.7668 0.036 Uiso 1 1 calc R
H4B H 0.6896 0.7722 0.7046 0.036 Uiso 1 1 calc R
C5 C 0.7868(5) 0.8821(5) 0.7617(3) 0.0253(14) Uani 1 1 d .
O1 O 0.8663(3) 0.6272(3) 0.73566(18) 0.0212(9) Uani 1 1 d .
O2 O 0.7169(3) 0.4705(3) 0.77400(19) 0.0277(10) Uani 1 1 d .
O3 O 0.7440(4) 0.4977(3) 0.66456(19) 0.0307(11) Uani 1 1 d .
O4 O 0.8739(4) 0.7443(4) 0.8507(2) 0.0378(12) Uani 1 1 d .
O5 O 0.7600(4) 0.6613(4) 0.9186(2) 0.0426(13) Uani 1 1 d .
H5 H 0.6987 0.6292 0.9217 0.064 Uiso 1 1 calc R
O6 O 0.8733(4) 0.8968(3) 0.7719(2) 0.0327(11) Uani 1 1 d .
O7 O 0.7635(4) 0.9490(3) 0.7599(2) 0.0348(12) Uani 1 1 d .
O8 O 1.0000 0.0000 0.921(4) 0.66(8) Uani 1 3 d SD
H8A H 1.0182 0.0619 0.9237 0.789 Uiso 0.33 1 d PRD
H8B H 0.9558 -0.0264 0.8938 0.789 Uiso 0.33 1 d PRD
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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
H H 0.0000 0.0000 '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
O2 Eu1 O2 88.57(16) 18_546 17_556
O2 Eu1 O2 180.00(18) 18_546 3_665
O2 Eu1 O2 91.43(16) 17_556 3_665
O2 Eu1 O2 91.43(17) 18_546 2_655
O2 Eu1 O2 179.998(1) 17_556 2_655
O2 Eu1 O2 88.57(16) 3_665 2_655
O2 Eu1 O2 88.57(17) 18_546 16_656
O2 Eu1 O2 88.57(16) 17_556 16_656
O2 Eu1 O2 91.43(16) 3_665 16_656
O2 Eu1 O2 91.43(17) 2_655 16_656
O2 Eu1 O2 91.43(17) 18_546 .
O2 Eu1 O2 91.43(17) 17_556 .
O2 Eu1 O2 88.57(17) 3_665 .
O2 Eu1 O2 88.57(16) 2_655 .
O2 Eu1 O2 179.998(1) 16_656 .
O7 Fe1 O6 114.28(19) 2_765 .
O7 Fe1 O1 87.08(17) 2_765 .
O6 Fe1 O1 158.64(18) . .
O7 Fe1 O3 89.79(19) 2_765 13_666
O6 Fe1 O3 81.37(18) . 13_666
O1 Fe1 O3 99.29(17) . 13_666
O7 Fe1 O4 93.73(19) 2_765 .
O6 Fe1 O4 86.00(19) . .
O1 Fe1 O4 93.15(18) . .
O3 Fe1 O4 167.24(19) 13_666 .
O7 Fe1 N1 165.43(19) 2_765 .
O6 Fe1 N1 77.15(18) . .
O1 Fe1 N1 81.81(17) . .
O3 Fe1 N1 101.24(18) 13_666 .
O4 Fe1 N1 77.58(18) . .
O3 Fe2 O3 112.35(13) 3_665 .
O3 Fe2 O3 112.35(13) 3_665 2_655
O3 Fe2 O3 112.35(12) . 2_655
O2 P1 O3 114.0(3) . .
O2 P1 O1 111.2(3) . .
O3 P1 O1 111.6(3) . .
O2 P1 C1 109.5(3) . .
O3 P1 C1 105.8(3) . .
O1 P1 C1 104.0(3) . .
C1 N1 C2 109.7(5) . .
C1 N1 C4 112.0(5) . .
C2 N1 C4 111.8(5) . .
C1 N1 Fe1 107.5(4) . .
C2 N1 Fe1 109.7(4) . .
C4 N1 Fe1 106.0(4) . .
N1 C1 P1 111.6(4) . .
N1 C1 H1A 109.3 . .
P1 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
P1 C1 H1B 109.3 . .
H1A C1 H1B 108.0 . .
N1 C2 C3 114.1(5) . .
N1 C2 H2A 108.7 . .
C3 C2 H2A 108.7 . .
N1 C2 H2B 108.7 . .
C3 C2 H2B 108.7 . .
H2A C2 H2B 107.6 . .
O4 C3 O5 120.3(6) . .
O4 C3 C2 123.6(6) . .
O5 C3 C2 116.1(6) . .
N1 C4 C5 111.4(5) . .
N1 C4 H4A 109.3 . .
C5 C4 H4A 109.3 . .
N1 C4 H4B 109.3 . .
C5 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
O7 C5 O6 125.0(6) . .
O7 C5 C4 115.8(6) . .
O6 C5 C4 119.1(6) . .
P1 O1 Fe1 119.4(2) . .
P1 O2 Eu1 165.2(3) . .
P1 O3 Fe1 132.6(3) . 13_666
P1 O3 Fe2 131.1(3) . .
Fe1 O3 Fe2 95.56(19) 13_666 .
C3 O4 Fe1 114.4(4) . .
C3 O5 H5 109.5 . .
C5 O6 Fe1 117.2(4) . .
C5 O7 Fe1 119.9(4) . 3_675
H8A O8 H8B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu1 O2 2.292(4) 18_546
Eu1 O2 2.292(4) 17_556
Eu1 O2 2.292(4) 3_665
Eu1 O2 2.292(4) 2_655
Eu1 O2 2.292(4) 16_656
Eu1 O2 2.292(4) .
Fe1 O7 2.102(5) 2_765
Fe1 O6 2.121(5) .
Fe1 O1 2.127(4) .
Fe1 O3 2.141(5) 13_666
Fe1 O4 2.218(5) .
Fe1 N1 2.250(5) .
Fe2 O3 2.283(5) 3_665
Fe2 O3 2.283(5) .
Fe2 O3 2.283(5) 2_655
P1 O2 1.505(4) .
P1 O3 1.517(5) .
P1 O1 1.540(4) .
P1 C1 1.817(6) .
N1 C1 1.473(8) .
N1 C2 1.486(8) .
N1 C4 1.498(8) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.487(9) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 O4 1.240(8) .
C3 O5 1.302(8) .
C4 C5 1.529(9) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 O7 1.247(8) .
C5 O6 1.255(8) .
O3 Fe1 2.141(5) 13_666
O5 H5 0.8200 .
O7 Fe1 2.102(5) 3_675
O8 H8A 0.8500 .
O8 H8B 0.8501 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O1 0.82 1.77 2.569(6) 164.6 18_546
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
O7 Fe1 N1 C1 -71.2(9) 2_765 .
O6 Fe1 N1 C1 145.7(4) . .
O1 Fe1 N1 C1 -30.6(3) . .
O3 Fe1 N1 C1 67.3(4) 13_666 .
O4 Fe1 N1 C1 -125.6(4) . .
O7 Fe1 N1 C2 48.0(9) 2_765 .
O6 Fe1 N1 C2 -95.1(4) . .
O1 Fe1 N1 C2 88.7(4) . .
O3 Fe1 N1 C2 -173.4(4) 13_666 .
O4 Fe1 N1 C2 -6.4(4) . .
O7 Fe1 N1 C4 168.8(7) 2_765 .
O6 Fe1 N1 C4 25.7(4) . .
O1 Fe1 N1 C4 -150.5(4) . .
O3 Fe1 N1 C4 -52.6(4) 13_666 .
O4 Fe1 N1 C4 114.4(4) . .
C2 N1 C1 P1 -76.2(5) . .
C4 N1 C1 P1 159.0(4) . .
Fe1 N1 C1 P1 43.0(4) . .
O2 P1 C1 N1 84.0(5) . .
O3 P1 C1 N1 -152.7(4) . .
O1 P1 C1 N1 -35.0(5) . .
C1 N1 C2 C3 123.5(6) . .
C4 N1 C2 C3 -111.6(6) . .
Fe1 N1 C2 C3 5.6(7) . .
N1 C2 C3 O4 0.4(10) . .
N1 C2 C3 O5 179.8(6) . .
C1 N1 C4 C5 -146.5(5) . .
C2 N1 C4 C5 89.9(6) . .
Fe1 N1 C4 C5 -29.5(6) . .
N1 C4 C5 O7 -167.1(6) . .
N1 C4 C5 O6 16.7(9) . .
O2 P1 O1 Fe1 -109.2(3) . .
O3 P1 O1 Fe1 122.3(3) . .
C1 P1 O1 Fe1 8.6(3) . .
O7 Fe1 O1 P1 -179.3(3) 2_765 .
O6 Fe1 O1 P1 0.0(6) . .
O3 Fe1 O1 P1 -90.0(3) 13_666 .
O4 Fe1 O1 P1 87.1(3) . .
N1 Fe1 O1 P1 10.1(3) . .
O3 P1 O2 Eu1 29.0(13) . .
O1 P1 O2 Eu1 -98.2(12) . .
C1 P1 O2 Eu1 147.4(11) . .
O2 Eu1 O2 P1 -165.3(11) 18_546 .
O2 Eu1 O2 P1 106.1(11) 17_556 .
O2 Eu1 O2 P1 14.7(11) 3_665 .
O2 Eu1 O2 P1 -73.9(11) 2_655 .
O2 Eu1 O2 P1 6(19) 16_656 .
O2 P1 O3 Fe1 171.7(3) . 13_666
O1 P1 O3 Fe1 -61.3(4) . 13_666
C1 P1 O3 Fe1 51.2(4) . 13_666
O2 P1 O3 Fe2 4.3(5) . .
O1 P1 O3 Fe2 131.4(3) . .
C1 P1 O3 Fe2 -116.1(4) . .
O3 Fe2 O3 P1 -71.3(3) 3_665 .
O3 Fe2 O3 P1 56.5(4) 2_655 .
O3 Fe2 O3 Fe1 118.0(3) 3_665 13_666
O3 Fe2 O3 Fe1 -114.1(3) 2_655 13_666
O5 C3 O4 Fe1 174.2(5) . .
C2 C3 O4 Fe1 -6.5(9) . .
O7 Fe1 O4 C3 -161.1(5) 2_765 .
O6 Fe1 O4 C3 84.8(5) . .
O1 Fe1 O4 C3 -73.8(5) . .
O3 Fe1 O4 C3 93.2(9) 13_666 .
N1 Fe1 O4 C3 7.1(5) . .
O7 C5 O6 Fe1 -167.9(5) . .
C4 C5 O6 Fe1 7.9(8) . .
O7 Fe1 O6 C5 170.0(4) 2_765 .
O1 Fe1 O6 C5 -9.3(8) . .
O3 Fe1 O6 C5 84.1(5) 13_666 .
O4 Fe1 O6 C5 -97.7(5) . .
N1 Fe1 O6 C5 -19.6(4) . .
O6 C5 O7 Fe1 13.7(9) . 3_675
C4 C5 O7 Fe1 -162.3(4) . 3_675
