#------------------------------------------------------------------------------
#$Date: 2023-12-04 17:48:35 +0200 (Mon, 04 Dec 2023) $
#$Revision: 288000 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/13/7101323.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_7101323
loop_
_publ_author_name
'Groves, John A.'
'Miller, Stuart R.'
'Warrender, Stewart J.'
'Mellot-Draznieks, Caroline'
'Lightfoot, Philip'
'Wright, Paul A.'
_publ_section_title
;
 The first route to large pore metal phosphonates
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   31
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3305
_journal_page_last               3307
_journal_paper_doi               10.1039/b605400e
_journal_year                    2006
_chemical_formula_moiety         '2(C6 H12 Fe N2 O6 P2), O3'
_chemical_formula_sum            'C12 H24 Fe2 N4 O15 P4'
_chemical_formula_weight         699.93
_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                62.781(1)
_cell_angle_beta                 79.029(1)
_cell_angle_gamma                87.088(1)
_cell_formula_units_Z            1
_cell_length_a                   8.3081(7)
_cell_length_b                   9.1647(7)
_cell_length_c                   9.1839(7)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      3.16
_cell_volume                     609.95(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'SRS Daresbury Laboratories'
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_radiation_wavelength     0.69999
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4497
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.536
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   -
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0509
_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)+(0.0596P)²+2.1652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                2128
_reflns_number_total             2473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605400e.txt
_cod_original_sg_symbol_Hall     -p1
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7101323
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
Fe1 Fe 0.75944(7) 0.42363(7) 0.57038(7) 0.00941(19) Uani 1 1 d .
P1 P 0.42074(13) 0.46684(13) 0.75806(13) 0.0098(3) Uani 1 1 d .
P2 P 0.94306(12) 0.74802(13) 0.53460(13) 0.0077(2) Uani 1 1 d .
O1 O 0.5580(4) 0.3523(4) 0.7486(4) 0.0181(7) Uani 1 1 d .
O2 O 0.2973(4) 0.4769(5) 0.6521(4) 0.0307(9) Uani 1 1 d .
O3 O 0.8726(4) 0.5717(4) 0.6214(4) 0.0134(6) Uani 1 1 d .
O4 O 1.1009(3) 0.7673(4) 0.4085(4) 0.0123(6) Uani 1 1 d .
O5 O 0.4814(4) 0.6320(4) 0.7291(4) 0.0204(7) Uani 1 1 d .
O6 O 0.9580(3) 0.8059(3) 0.6610(4) 0.0114(6) Uani 1 1 d .
O7 O 0.8058(11) 0.0393(9) 0.9390(9) 0.0281(17) Uiso 0.50 1 d P
O8 O 0.8903(10) 0.0380(9) 0.9368(9) 0.0252(16) Uiso 0.50 1 d P
O9 O 0.5513(8) 0.0247(8) 0.9837(9) 0.0232(15) Uiso 0.50 1 d P
N1 N 0.1484(4) 0.4086(4) 1.0255(4) 0.0088(7) Uani 1 1 d .
N2 N 0.6373(4) 0.8963(4) 0.4845(4) 0.0097(7) Uani 1 1 d .
C1 C 0.3158(5) 0.3551(5) 0.9757(5) 0.0100(8) Uani 1 1 d .
H1A H 0.3052 0.2403 1.0022 0.012 Uiso 1 1 calc R
H1B H 0.3866 0.3618 1.0453 0.012 Uiso 1 1 calc R
C2 C 0.8041(5) 0.8766(5) 0.3986(5) 0.0096(8) Uani 1 1 d .
H2A H 0.8567 0.9848 0.3290 0.012 Uiso 1 1 calc R
H2B H 0.7893 0.8305 0.3254 0.012 Uiso 1 1 calc R
C3 C 0.0194(5) 0.3696(5) 0.9523(5) 0.0098(8) Uani 1 1 d .
H3A H 0.0187 0.2536 0.9820 0.012 Uiso 1 1 calc R
H3B H 0.0449 0.4311 0.8317 0.012 Uiso 1 1 calc R
C4 C 0.1481(5) 0.5866(5) 0.9836(5) 0.0096(8) Uani 1 1 d .
H4A H 0.1764 0.6527 0.8637 0.012 Uiso 1 1 calc R
H4B H 0.2298 0.6103 1.0333 0.012 Uiso 1 1 calc R
C5 C 0.5223(5) 0.9623(5) 0.3620(5) 0.0104(8) Uani 1 1 d .
H5A H 0.5128 0.8863 0.3171 0.013 Uiso 1 1 calc R
H5B H 0.5670 1.0664 0.2701 0.013 Uiso 1 1 calc R
C6 C 0.6467(5) 1.0137(5) 0.5556(5) 0.0094(8) Uani 1 1 d .
H6A H 0.6936 1.1187 0.4672 0.011 Uiso 1 1 calc R
H6B H 0.7180 0.9714 0.6371 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'
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'
Fe Fe 0.3463 0.8444 '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
O3 Fe1 O2 115.20(15) . 2_666
O3 Fe1 O1 102.10(13) . .
O2 Fe1 O1 111.18(14) 2_666 .
O3 Fe1 O4 109.57(13) . 2_766
O2 Fe1 O4 107.69(15) 2_666 2_766
O1 Fe1 O4 111.06(12) . 2_766
O5 P1 O2 113.8(2) . .
O5 P1 O1 113.78(18) . .
O2 P1 O1 111.6(2) . .
O5 P1 C1 108.34(19) . .
O2 P1 C1 106.40(19) . .
O1 P1 C1 101.87(18) . .
O6 P2 O3 110.50(17) . .
O6 P2 O4 114.99(17) . .
O3 P2 O4 111.07(17) . .
O6 P2 C2 110.26(18) . .
O3 P2 C2 107.68(18) . .
O4 P2 C2 101.80(17) . .
P1 O1 Fe1 123.60(18) . .
P1 O2 Fe1 147.3(2) . 2_666
P2 O3 Fe1 138.86(19) . .
P2 O4 Fe1 121.77(17) . 2_766
C4 N1 C3 110.0(3) . .
C4 N1 C1 112.6(3) . .
C3 N1 C1 112.4(3) . .
C6 N2 C2 110.9(3) . .
C6 N2 C5 108.5(3) . .
C2 N2 C5 109.9(3) . .
N1 C1 P1 118.1(3) . .
N1 C1 H1A 107.8 . .
P1 C1 H1A 107.8 . .
N1 C1 H1B 107.8 . .
P1 C1 H1B 107.8 . .
H1A C1 H1B 107.1 . .
N2 C2 P2 116.1(3) . .
N2 C2 H2A 108.3 . .
P2 C2 H2A 108.3 . .
N2 C2 H2B 108.3 . .
P2 C2 H2B 108.3 . .
H2A C2 H2B 107.4 . .
N1 C3 C4 110.4(3) . 2_567
N1 C3 H3A 109.6 . .
C4 C3 H3A 109.6 2_567 .
N1 C3 H3B 109.6 . .
C4 C3 H3B 109.6 2_567 .
H3A C3 H3B 108.1 . .
N1 C4 C3 110.3(3) . 2_567
N1 C4 H4A 109.6 . .
C3 C4 H4A 109.6 2_567 .
N1 C4 H4B 109.6 . .
C3 C4 H4B 109.6 2_567 .
H4A C4 H4B 108.1 . .
N2 C5 C6 111.2(3) . 2_676
N2 C5 H5A 109.4 . .
C6 C5 H5A 109.4 2_676 .
N2 C5 H5B 109.4 . .
C6 C5 H5B 109.4 2_676 .
H5A C5 H5B 108.0 . .
N2 C6 C5 111.1(3) . 2_676
N2 C6 H6A 109.4 . .
C5 C6 H6A 109.4 2_676 .
N2 C6 H6B 109.4 . .
C5 C6 H6B 109.4 2_676 .
H6A C6 H6B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.956(3) .
Fe1 O2 1.962(3) 2_666
Fe1 O1 2.000(3) .
Fe1 O4 2.004(3) 2_766
P1 O5 1.508(3) .
P1 O2 1.515(3) .
P1 O1 1.527(3) .
P1 C1 1.833(4) .
P2 O6 1.507(3) .
P2 O3 1.526(3) .
P2 O4 1.533(3) .
P2 C2 1.830(4) .
O2 Fe1 1.962(3) 2_666
O4 Fe1 2.004(3) 2_766
O7 O8 0.698(9) .
O9 O9 0.916(12) 2_657
N1 C4 1.495(5) .
N1 C3 1.504(5) .
N1 C1 1.510(5) .
N2 C6 1.503(5) .
N2 C2 1.505(5) .
N2 C5 1.508(5) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.514(5) 2_567
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C3 1.514(5) 2_567
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.519(5) 2_676
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C5 1.519(5) 2_676
C6 H6A 0.9700 .
C6 H6B 0.9700 .
