#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/56/7035692.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_7035692
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 Fe7 Ho N6 O42 P6, H4 O2'
_chemical_formula_sum            'C30 H46 Fe7 Ho N6 O44 P6'
_chemical_formula_weight         1936.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_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                   15.2935(4)
_cell_length_b                   15.2935(4)
_cell_length_c                   22.7749(12)
_cell_measurement_reflns_used    2596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.36
_cell_volume                     4613.2(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega 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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8237
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.7872
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2877
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.481
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0470
_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)+(0.0691P)²+144.6606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                1770
_reflns_number_total             2021
_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               7035692
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
Ho1 Ho 0.0000 1.0000 0.5000 0.0105(2) Uani 1 6 d S
Fe1 Fe 0.23263(8) 0.79057(8) 0.42216(5) 0.0236(3) Uani 1 1 d .
Fe2 Fe 0.0000 1.0000 0.29856(15) 0.0136(6) Uani 0.50 3 d SP
P1 P 0.09014(13) 0.88029(13) 0.39182(7) 0.0167(4) Uani 1 1 d .
C1 C 0.0208(5) 0.7433(5) 0.3882(3) 0.0196(14) Uani 1 1 d .
H1A H -0.0495 0.7186 0.3977 0.024 Uiso 1 1 calc R
H1B H 0.0240 0.7219 0.3485 0.024 Uiso 1 1 calc R
C2 C 0.0332(6) 0.7049(6) 0.4905(3) 0.0252(16) Uani 1 1 d .
H2A H -0.0068 0.7381 0.4904 0.030 Uiso 1 1 calc R
H2B H -0.0095 0.6367 0.5049 0.030 Uiso 1 1 calc R
C3 C 0.1184(6) 0.7591(6) 0.5321(3) 0.0262(16) Uani 1 1 d .
C4 C 0.0353(6) 0.5946(6) 0.4127(4) 0.0270(16) Uani 1 1 d .
H4A H 0.0223 0.5857 0.3708 0.032 Uiso 1 1 calc R
H4B H -0.0263 0.5473 0.4329 0.032 Uiso 1 1 calc R
C5 C 0.1185(5) 0.5711(5) 0.4280(3) 0.0227(15) Uani 1 1 d .
N1 N 0.0628(5) 0.6994(5) 0.4292(3) 0.0232(13) Uani 1 1 d .
O1 O 0.2007(4) 0.9071(4) 0.4020(2) 0.0210(10) Uani 1 1 d .
O2 O 0.0519(4) 0.9158(4) 0.4419(2) 0.0231(11) Uani 1 1 d .
O3 O 0.0769(4) 0.9149(4) 0.3317(2) 0.0283(12) Uani 1 1 d .
O4 O 0.2082(4) 0.7975(4) 0.5172(3) 0.0329(13) Uani 1 1 d .
O5 O 0.0949(4) 0.7648(5) 0.5866(2) 0.0358(14) Uani 1 1 d .
H5 H 0.0333 0.7335 0.5903 0.054 Uiso 1 1 calc R
O6 O 0.2060(4) 0.6427(4) 0.4386(2) 0.0287(12) Uani 1 1 d .
O7 O 0.0953(4) 0.4803(4) 0.4256(2) 0.0307(12) Uani 1 1 d .
O8 O 0.0000 1.0000 0.954(8) 0.6(2) Uani 1 3 d S
H8A H -0.0100 1.0063 0.9902 0.954 Uiso 0.33 1 d PR
H8B H 0.0129 0.9529 0.9504 0.954 Uiso 0.33 1 d PR
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'
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'
Ho Ho -0.2175 4.6783 '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 Ho1 O2 180.000(1) 12_666 3_465
O2 Ho1 O2 88.91(19) 12_666 11_456
O2 Ho1 O2 91.09(19) 3_465 11_456
O2 Ho1 O2 91.09(19) 12_666 .
O2 Ho1 O2 88.91(19) 3_465 .
O2 Ho1 O2 91.09(19) 11_456 .
O2 Ho1 O2 88.91(19) 12_666 10_576
O2 Ho1 O2 91.09(19) 3_465 10_576
O2 Ho1 O2 88.91(19) 11_456 10_576
O2 Ho1 O2 180.0(2) . 10_576
O2 Ho1 O2 91.09(19) 12_666 2_675
O2 Ho1 O2 88.91(19) 3_465 2_675
O2 Ho1 O2 180.0(2) 11_456 2_675
O2 Ho1 O2 88.91(19) . 2_675
O2 Ho1 O2 91.09(19) 10_576 2_675
O7 Fe1 O1 86.3(2) 3_565 .
O7 Fe1 O6 114.9(2) 3_565 .
O1 Fe1 O6 158.8(2) . .
O7 Fe1 O3 89.6(2) 3_565 16_565
O1 Fe1 O3 100.00(19) . 16_565
O6 Fe1 O3 80.6(2) . 16_565
O7 Fe1 O4 93.9(2) 3_565 .
O1 Fe1 O4 93.2(2) . .
O6 Fe1 O4 86.1(2) . .
O3 Fe1 O4 166.5(2) 16_565 .
O7 Fe1 N1 165.0(2) 3_565 .
O1 Fe1 N1 81.8(2) . .
O6 Fe1 N1 77.3(2) . .
O3 Fe1 N1 101.3(2) 16_565 .
O4 Fe1 N1 77.9(2) . .
O3 Fe2 O3 109.56(15) 2_675 .
O3 Fe2 O3 109.56(15) 2_675 3_465
O3 Fe2 O3 109.56(15) . 3_465
O2 P1 O3 114.5(3) . .
O2 P1 O1 111.2(3) . .
O3 P1 O1 111.2(3) . .
O2 P1 C1 110.1(3) . .
O3 P1 C1 105.0(3) . .
O1 P1 C1 104.0(3) . .
N1 C1 P1 111.2(5) . .
N1 C1 H1A 109.4 . .
P1 C1 H1A 109.4 . .
N1 C1 H1B 109.4 . .
P1 C1 H1B 109.4 . .
H1A C1 H1B 108.0 . .
C3 C2 N1 115.1(6) . .
C3 C2 H2A 108.5 . .
N1 C2 H2A 108.5 . .
C3 C2 H2B 108.5 . .
N1 C2 H2B 108.5 . .
H2A C2 H2B 107.5 . .
O4 C3 O5 120.3(7) . .
O4 C3 C2 123.1(7) . .
O5 C3 C2 116.6(6) . .
N1 C4 C5 112.1(6) . .
N1 C4 H4A 109.2 . .
C5 C4 H4A 109.2 . .
N1 C4 H4B 109.2 . .
C5 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
O7 C5 O6 124.2(7) . .
O7 C5 C4 116.4(6) . .
O6 C5 C4 119.2(6) . .
C1 N1 C2 110.9(6) . .
C1 N1 C4 112.2(6) . .
C2 N1 C4 111.7(6) . .
C1 N1 Fe1 107.6(4) . .
C2 N1 Fe1 108.7(4) . .
C4 N1 Fe1 105.4(4) . .
P1 O1 Fe1 119.4(3) . .
P1 O2 Ho1 165.1(3) . .
P1 O3 Fe1 131.7(3) . 16_565
P1 O3 Fe2 134.1(3) . .
Fe1 O3 Fe2 93.4(2) 16_565 .
C3 O4 Fe1 114.7(5) . .
C3 O5 H5 109.5 . .
C5 O6 Fe1 116.6(5) . .
C5 O7 Fe1 119.8(5) . 2_665
H8A O8 H8B 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O2 2.250(5) 12_666
Ho1 O2 2.250(5) 3_465
Ho1 O2 2.250(5) 11_456
Ho1 O2 2.250(4) .
Ho1 O2 2.250(4) 10_576
Ho1 O2 2.250(5) 2_675
Fe1 O7 2.101(5) 3_565
Fe1 O1 2.120(5) .
Fe1 O6 2.121(5) .
Fe1 O3 2.155(5) 16_565
Fe1 O4 2.209(6) .
Fe1 N1 2.258(6) .
Fe2 O3 2.275(5) 2_675
Fe2 O3 2.275(5) .
Fe2 O3 2.275(5) 3_465
P1 O2 1.502(5) .
P1 O3 1.517(5) .
P1 O1 1.545(5) .
P1 C1 1.817(7) .
C1 N1 1.471(9) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.483(11) .
C2 N1 1.483(9) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 O4 1.240(9) .
C3 O5 1.308(9) .
C4 N1 1.488(9) .
C4 C5 1.526(10) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 O7 1.251(9) .
C5 O6 1.258(9) .
O3 Fe1 2.155(5) 16_565
O5 H5 0.8200 .
O7 Fe1 2.101(5) 2_665
O8 H8A 0.8464 .
O8 H8B 0.8413 .
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
O8 H8A O8 0.85 1.28 2.1(3) 155.4 10_577
O5 H5 O1 0.82 1.77 2.559(7) 161.4 11_456
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
O2 P1 C1 N1 -83.2(5) . .
O3 P1 C1 N1 153.1(5) . .
O1 P1 C1 N1 36.1(5) . .
N1 C2 C3 O4 0.1(11) . .
N1 C2 C3 O5 -179.6(7) . .
N1 C4 C5 O7 167.5(6) . .
N1 C4 C5 O6 -16.8(10) . .
P1 C1 N1 C2 75.4(6) . .
P1 C1 N1 C4 -158.8(5) . .
P1 C1 N1 Fe1 -43.4(5) . .
C3 C2 N1 C1 -123.0(7) . .
C3 C2 N1 C4 111.1(7) . .
C3 C2 N1 Fe1 -4.8(8) . .
C5 C4 N1 C1 146.5(6) . .
C5 C4 N1 C2 -88.2(7) . .
C5 C4 N1 Fe1 29.8(7) . .
O7 Fe1 N1 C1 68.0(10) 3_565 .
O1 Fe1 N1 C1 30.4(4) . .
O6 Fe1 N1 C1 -145.8(5) . .
O3 Fe1 N1 C1 -68.2(4) 16_565 .
O4 Fe1 N1 C1 125.5(4) . .
O7 Fe1 N1 C2 -52.2(11) 3_565 .
O1 Fe1 N1 C2 -89.8(5) . .
O6 Fe1 N1 C2 94.0(5) . .
O3 Fe1 N1 C2 171.6(4) 16_565 .
O4 Fe1 N1 C2 5.3(4) . .
O7 Fe1 N1 C4 -172.2(8) 3_565 .
O1 Fe1 N1 C4 150.3(5) . .
O6 Fe1 N1 C4 -25.9(4) . .
O3 Fe1 N1 C4 51.6(5) 16_565 .
O4 Fe1 N1 C4 -114.6(5) . .
O2 P1 O1 Fe1 108.4(3) . .
O3 P1 O1 Fe1 -122.6(3) . .
C1 P1 O1 Fe1 -10.1(4) . .
O7 Fe1 O1 P1 -180.0(3) 3_565 .
O6 Fe1 O1 P1 1.2(7) . .
O3 Fe1 O1 P1 91.1(3) 16_565 .
O4 Fe1 O1 P1 -86.3(3) . .
N1 Fe1 O1 P1 -9.0(3) . .
O3 P1 O2 Ho1 -22.2(14) . .
O1 P1 O2 Ho1 105.0(13) . .
C1 P1 O2 Ho1 -140.2(12) . .
O2 Ho1 O2 P1 -112.2(12) 12_666 .
O2 Ho1 O2 P1 67.8(12) 3_465 .
O2 Ho1 O2 P1 158.9(12) 11_456 .
O2 Ho1 O2 P1 -157(100) 10_576 .
O2 Ho1 O2 P1 -21.1(12) 2_675 .
O2 P1 O3 Fe1 -172.3(4) . 16_565
O1 P1 O3 Fe1 60.6(5) . 16_565
C1 P1 O3 Fe1 -51.4(5) . 16_565
O2 P1 O3 Fe2 -5.8(6) . .
O1 P1 O3 Fe2 -133.0(4) . .
C1 P1 O3 Fe2 115.1(4) . .
O3 Fe2 O3 P1 67.8(4) 2_675 .
O3 Fe2 O3 P1 -52.4(5) 3_465 .
O3 Fe2 O3 Fe1 -122.3(3) 2_675 16_565
O3 Fe2 O3 Fe1 117.5(3) 3_465 16_565
O5 C3 O4 Fe1 -175.3(6) . .
C2 C3 O4 Fe1 5.0(10) . .
O7 Fe1 O4 C3 161.6(6) 3_565 .
O1 Fe1 O4 C3 75.1(6) . .
O6 Fe1 O4 C3 -83.6(6) . .
O3 Fe1 O4 C3 -93.6(10) 16_565 .
N1 Fe1 O4 C3 -5.8(5) . .
O7 C5 O6 Fe1 167.1(6) . .
C4 C5 O6 Fe1 -8.2(9) . .
O7 Fe1 O6 C5 -169.3(5) 3_565 .
O1 Fe1 O6 C5 9.4(9) . .
O3 Fe1 O6 C5 -84.1(5) 16_565 .
O4 Fe1 O6 C5 98.2(5) . .
N1 Fe1 O6 C5 19.8(5) . .
O6 C5 O7 Fe1 -12.6(10) . 2_665
C4 C5 O7 Fe1 162.9(5) . 2_665
