#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:49:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179709 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/12/7001235.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_7001235
loop_
_publ_author_name
'Redrup, Kate V.'
'Weller, Mark T.'
_publ_section_title
;
 Synthesis and crystal structures of iron hydrogen phosphates
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3786
_journal_page_last               3792
_journal_paper_doi               10.1039/b902519g
_journal_year                    2009
_chemical_formula_sum            'C H Fe N0 O P'
_chemical_formula_weight         115.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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                64.649(2)
_cell_angle_beta                 70.328(2)
_cell_angle_gamma                69.541(2)
_cell_formula_units_Z            5
_cell_length_a                   7.1290(3)
_cell_length_b                   8.8372(3)
_cell_length_c                   9.4621(3)
_cell_measurement_temperature    293(2)
_cell_volume                     492.27(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5764
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    4.007
_exptl_absorpt_correction_T_max  0.8248
_exptl_absorpt_correction_T_min  0.5013
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          3.817
_refine_ls_shift/su_mean         0.082
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0068P)²+1.3200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                2072
_reflns_number_total             2240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B902519G.txt
_cod_data_source_block           2007kvb0051
_cod_database_code               7001235
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
O1 O 0.1587(3) 0.7611(2) 0.1124(2) 0.0067(4) Uani 1 1 d . . .
O2 O 0.2635(3) 1.0414(2) -0.1422(2) 0.0086(4) Uani 1 1 d . . .
O3 O 0.4053(3) 0.8730(3) 0.2391(2) 0.0099(4) Uani 1 1 d . . .
O4 O 0.0557(3) 1.0867(2) 0.1467(2) 0.0080(4) Uani 1 1 d . . .
O5 O -0.1056(3) 0.5858(3) 0.2502(2) 0.0093(4) Uani 1 1 d . . .
O6 O 0.0260(3) 0.6819(2) 0.4099(2) 0.0079(4) Uani 1 1 d . . .
O7 O 0.4353(3) 0.1257(2) 0.2857(2) 0.0069(4) Uani 1 1 d . . .
O8 O -0.2815(3) 1.2970(2) 0.2146(2) 0.0083(4) Uani 1 1 d . . .
O9 O 0.0146(3) 0.2589(2) 0.3105(2) 0.0076(4) Uani 1 1 d . . .
O10 O 0.1671(3) -0.0173(2) 0.5720(2) 0.0073(4) Uani 1 1 d . . .
O11 O 0.4048(3) 0.1884(2) 0.5636(2) 0.0073(4) Uani 1 1 d . . .
O12 O 0.2540(3) 0.4537(2) 0.2942(2) 0.0066(4) Uani 1 1 d . . .
N1 N 0.3811(5) 1.3349(4) -0.0311(3) 0.0141(5) Uani 1 1 d . . .
N2 N 0.5000 0.5000 0.5000 0.0195(10) Uani 1 2 d S . .
H1 H -0.084(5) 0.500(5) 0.267(4) 0.008(9) Uiso 1 1 d . . .
H2 H 0.514(8) 1.299(6) -0.064(6) 0.050 Uiso 1 1 d . . .
H3 H 0.340(7) 1.297(6) 0.079(6) 0.045 Uiso 1 1 d . . .
H4 H 0.310(7) 0.929(6) 0.220(5) 0.029(12) Uiso 1 1 d . . .
H5 H -0.366(7) 1.261(5) 0.229(5) 0.030(12) Uiso 1 1 d . . .
H6 H 0.348(7) 1.447(6) -0.075(5) 0.038(12) Uiso 1 1 d . . .
H7 H 0.324(7) 1.294(6) -0.055(5) 0.029(12) Uiso 1 1 d . . .
H9 H 0.52(6) 0.28(5) 0.42(5) 0.9(3) Uiso 1 1 d . . .
H8 H 0.09(7) 0.66(5) 0.42(5) 0.5(4) Uiso 1 1 d . . .
H10 H 0.487(16) 0.437(9) 0.525(10) 0.17(3) Uiso 1 1 d . . .
H11 H 0.57(5) 0.46(6) 0.47(4) 0.27(19) Uiso 1 1 d . . .
Fe1 Fe 0.0000 1.0000 0.0000 0.00514(13) Uani 1 2 d S . .
Fe2 Fe 0.20344(6) 0.21676(5) 0.44977(4) 0.00526(11) Uani 1 1 d . . .
P3 P -0.08951(10) 1.15543(8) 0.27900(8) 0.00546(15) Uani 1 1 d . . .
P4 P 0.45262(10) 1.05503(9) -0.27791(8) 0.00549(15) Uani 1 1 d . . .
P5 P 0.08655(10) 0.62240(8) 0.26849(8) 0.00571(15) Uani 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'
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'
N N 0.0061 0.0033 '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
P5 O1 Fe1 129.39(11) . . ?
P4 O2 Fe1 164.83(13) . . ?
P3 O4 Fe1 131.08(12) . . ?
P5 O6 Fe2 144.42(13) . 2_566 ?
P4 O7 Fe2 134.33(11) 2_665 . ?
P3 O9 Fe2 138.45(12) 1_545 . ?
P3 O10 Fe2 153.25(12) 2_566 . ?
P4 O11 Fe2 130.28(12) 1_546 . ?
P5 O12 Fe2 124.21(11) . . ?
O2 Fe1 O2 180.0 . 2_575 ?
O2 Fe1 O1 86.76(8) . . ?
O2 Fe1 O1 93.24(8) 2_575 . ?
O2 Fe1 O1 93.24(8) . 2_575 ?
O2 Fe1 O1 86.76(8) 2_575 2_575 ?
O1 Fe1 O1 180.00(11) . 2_575 ?
O2 Fe1 O4 87.32(8) . . ?
O2 Fe1 O4 92.68(8) 2_575 . ?
O1 Fe1 O4 88.87(7) . . ?
O1 Fe1 O4 91.13(7) 2_575 . ?
O2 Fe1 O4 92.68(8) . 2_575 ?
O2 Fe1 O4 87.32(8) 2_575 2_575 ?
O1 Fe1 O4 91.13(7) . 2_575 ?
O1 Fe1 O4 88.87(7) 2_575 2_575 ?
O4 Fe1 O4 180.0 . 2_575 ?
O6 Fe2 O10 94.19(8) 2_566 . ?
O6 Fe2 O11 93.47(8) 2_566 . ?
O10 Fe2 O11 93.53(8) . . ?
O6 Fe2 O9 90.26(8) 2_566 . ?
O10 Fe2 O9 90.93(8) . . ?
O11 Fe2 O9 173.97(8) . . ?
O6 Fe2 O7 175.16(8) 2_566 . ?
O10 Fe2 O7 88.93(8) . . ?
O11 Fe2 O7 90.03(8) . . ?
O9 Fe2 O7 85.98(7) . . ?
O6 Fe2 O12 92.23(8) 2_566 . ?
O10 Fe2 O12 172.23(8) . . ?
O11 Fe2 O12 90.45(8) . . ?
O9 Fe2 O12 84.66(7) . . ?
O7 Fe2 O12 84.39(7) . . ?
O10 P3 O9 113.28(11) 2_566 1_565 ?
O10 P3 O4 113.26(11) 2_566 . ?
O9 P3 O4 109.04(11) 1_565 . ?
O10 P3 O8 108.30(11) 2_566 . ?
O9 P3 O8 102.73(11) 1_565 . ?
O4 P3 O8 109.66(11) . . ?
O2 P4 O11 112.77(11) . 1_564 ?
O2 P4 O7 108.95(11) . 2_665 ?
O11 P4 O7 113.51(10) 1_564 2_665 ?
O2 P4 O3 107.38(11) . 2_675 ?
O11 P4 O3 104.13(11) 1_564 2_675 ?
O7 P4 O3 109.83(11) 2_665 2_675 ?
O6 P5 O1 110.95(11) . . ?
O6 P5 O12 110.78(11) . . ?
O1 P5 O12 110.29(10) . . ?
O6 P5 O5 110.07(11) . . ?
O1 P5 O5 107.40(11) . . ?
O12 P5 O5 107.23(11) . . ?
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
O1 P5 1.5257(19) . ?
O1 Fe1 2.0211(18) . ?
O2 P4 1.5153(19) . ?
O2 Fe1 1.9573(19) . ?
O3 P4 1.571(2) 2_675 ?
O4 P3 1.5316(19) . ?
O4 Fe1 2.0412(18) . ?
O5 P5 1.590(2) . ?
O6 P5 1.5194(19) . ?
O6 Fe2 1.9423(19) 2_566 ?
O7 P4 1.5374(19) 2_665 ?
O7 Fe2 2.0496(18) . ?
O8 P3 1.588(2) . ?
O9 P3 1.5274(19) 1_545 ?
O9 Fe2 2.0276(19) . ?
O10 P3 1.5021(19) 2_566 ?
O10 Fe2 1.9515(18) . ?
O11 P4 1.5176(19) 1_546 ?
O11 Fe2 1.9600(19) . ?
O12 P5 1.5321(19) . ?
O12 Fe2 2.0524(18) . ?
Fe1 O2 1.9573(19) 2_575 ?
Fe1 O1 2.0211(18) 2_575 ?
Fe1 O4 2.0412(18) 2_575 ?
Fe2 O6 1.9423(19) 2_566 ?
P3 O10 1.5021(19) 2_566 ?
P3 O9 1.5274(19) 1_565 ?
P4 O11 1.5176(19) 1_564 ?
P4 O7 1.5374(19) 2_665 ?
P4 O3 1.571(2) 2_675 ?
