#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005471.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_7005471
loop_
_publ_author_name
'Dillinger, Sandra A. T.'
'Schmalle, Helmut W.'
'Fox, Thomas'
'Berke, Heinz'
_publ_section_title
;
 Developing iron nitrosyl complexes as NO donor prodrugs.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3562
_journal_page_last               3571
_journal_paper_doi               10.1039/b702461d
_journal_year                    2007
_chemical_formula_moiety         'C6 H16 Fe N2 O6 P2'
_chemical_formula_sum            'C6 H16 Fe N2 O6 P2'
_chemical_formula_weight         330.00
_chemical_name_systematic
;
Dinitrosyl-(1,2-bis(hydroxymethylphosphino)ethane)iron(II)
;
_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                95.919(15)
_cell_angle_beta                 106.994(15)
_cell_angle_gamma                109.827(14)
_cell_formula_units_Z            2
_cell_length_a                   7.6992(10)
_cell_length_b                   8.5741(11)
_cell_length_c                   11.2515(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.85
_cell_volume                     651.11(18)
_computing_cell_refinement       'Stoe IPDS software'
_computing_data_collection       'Stoe IPDS software'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    'PLATON, PLUTON (Spek, 1990, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_measurement_method       'φ rotation scan'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13195
_diffrn_reflns_theta_full        30.39
_diffrn_reflns_theta_max         30.39
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ' image'
_diffrn_standards_interval_time  4.40
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.7201
_exptl_absorpt_correction_T_min  0.6009
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Coppens et al. 1965'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0506P)²+0.0611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                3022
_reflns_number_total             3544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702461d.txt
_cod_data_source_block           4
_cod_database_code               7005471
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.15588(3) 0.75961(3) 0.40203(2) 0.01298(7) Uani 1 d . . .
P1 P 0.18729(5) 0.91923(5) 0.25741(4) 0.01357(9) Uani 1 d . . .
P2 P -0.14151(5) 0.60141(5) 0.26103(4) 0.01309(9) Uani 1 d . . .
N1 N 0.1458(2) 0.87262(17) 0.52665(14) 0.0190(3) Uani 1 d . . .
O1 O 0.1409(2) 0.94500(19) 0.62114(15) 0.0321(3) Uani 1 d . . .
N2 N 0.26553(19) 0.62287(17) 0.41146(13) 0.0165(3) Uani 1 d . . .
O2 O 0.3260(2) 0.51375(18) 0.42513(15) 0.0297(3) Uani 1 d . . .
C1 C -0.0556(2) 0.85527(19) 0.13046(16) 0.0169(3) Uani 1 d . . .
H1A H -0.1313 0.9168 0.1564 0.020 Uiso 1 calc R . .
H1B H -0.0375 0.8849 0.0510 0.020 Uiso 1 calc R . .
C2 C -0.1695(2) 0.66227(19) 0.10687(16) 0.0170(3) Uani 1 d . . .
H2A H -0.1176 0.6004 0.0563 0.020 Uiso 1 calc R . .
H2B H -0.3108 0.6318 0.0582 0.020 Uiso 1 calc R . .
C3 C 0.3510(2) 0.9122(2) 0.16699(18) 0.0207(3) Uani 1 d . . .
H3A H 0.3515 0.9943 0.1112 0.025 Uiso 1 calc R . .
H3B H 0.4872 0.9472 0.2274 0.025 Uiso 1 calc R . .
O3 O 0.2903(2) 0.74676(17) 0.09088(13) 0.0262(3) Uani 1 d . . .
H3 H 0.3397 0.6888 0.1349 0.039 Uiso 1 calc R . .
C4 C 0.2687(2) 1.15128(19) 0.31135(17) 0.0188(3) Uani 1 d . . .
H4A H 0.2022 1.1740 0.3703 0.023 Uiso 1 calc R . .
H4B H 0.4123 1.2007 0.3592 0.023 Uiso 1 calc R . .
O4 O 0.22705(18) 1.23332(14) 0.20824(13) 0.0193(2) Uani 1 d . . .
H4 H 0.137(4) 1.254(3) 0.203(3) 0.034(7) Uiso 1 d . . .
C5 C -0.3479(2) 0.6245(2) 0.30140(17) 0.0184(3) Uani 1 d . . .
H5A H -0.3604 0.5714 0.3742 0.022 Uiso 1 calc R . .
H5B H -0.3184 0.7470 0.3287 0.022 Uiso 1 calc R . .
O5 O -0.53160(16) 0.54812(16) 0.19692(13) 0.0195(2) Uani 1 d . . .
H5 H -0.586(4) 0.469(4) 0.210(3) 0.041(8) Uiso 1 d . . .
C6 C -0.2183(3) 0.3676(2) 0.22179(18) 0.0209(3) Uani 1 d . . .
H6A H -0.2080 0.3251 0.3011 0.025 Uiso 1 calc R . .
H6B H -0.3580 0.3148 0.1647 0.025 Uiso 1 calc R . .
O6 O -0.1008(2) 0.31782(17) 0.16125(13) 0.0256(3) Uani 1 d . . .
H6 H -0.1524 0.3022 0.0819 0.038 Uiso 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'
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'
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
N2 Fe1 N1 124.28(7) . . yes
N2 Fe1 P2 101.74(5) . . yes
N1 Fe1 P2 112.17(5) . . yes
N2 Fe1 P1 116.96(5) . . yes
N1 Fe1 P1 108.63(5) . . yes
P2 Fe1 P1 85.80(2) . . yes
C4 P1 C3 100.31(8) . . yes
C4 P1 C1 104.09(7) . . yes
C3 P1 C1 103.04(8) . . yes
C4 P1 Fe1 117.87(6) . . yes
C3 P1 Fe1 120.43(6) . . yes
C1 P1 Fe1 109.05(5) . . yes
C2 P2 C5 103.90(8) . . yes
C2 P2 C6 104.61(8) . . yes
C5 P2 C6 102.24(8) . . yes
C2 P2 Fe1 110.48(5) . . yes
C5 P2 Fe1 115.14(6) . . yes
C6 P2 Fe1 118.92(6) . . yes
O1 N1 Fe1 175.11(13) . . yes
O2 N2 Fe1 171.14(14) . . yes
C2 C1 P1 109.38(10) . . yes
C2 C1 H1A 109.8 . . yes
P1 C1 H1A 109.8 . . yes
C2 C1 H1B 109.8 . . yes
P1 C1 H1B 109.8 . . yes
H1A C1 H1B 108.2 . . yes
C1 C2 P2 109.07(11) . . yes
C1 C2 H2A 109.9 . . yes
P2 C2 H2A 109.9 . . yes
C1 C2 H2B 109.9 . . yes
P2 C2 H2B 109.9 . . yes
H2A C2 H2B 108.3 . . yes
O3 C3 P1 112.00(12) . . yes
O3 C3 H3A 109.2 . . yes
P1 C3 H3A 109.2 . . yes
O3 C3 H3B 109.2 . . yes
P1 C3 H3B 109.2 . . yes
H3A C3 H3B 107.9 . . yes
C3 O3 H3 109.5 . . yes
O4 C4 P1 112.85(11) . . yes
O4 C4 H4A 109.0 . . yes
P1 C4 H4A 109.0 . . yes
O4 C4 H4B 109.0 . . yes
P1 C4 H4B 109.0 . . yes
H4A C4 H4B 107.8 . . yes
C4 O4 H4 111(2) . . yes
O5 C5 P2 112.81(12) . . yes
O5 C5 H5A 109.0 . . yes
P2 C5 H5A 109.0 . . yes
O5 C5 H5B 109.0 . . yes
P2 C5 H5B 109.0 . . yes
H5A C5 H5B 107.8 . . yes
C5 O5 H5 106(2) . . yes
O6 C6 P2 112.07(12) . . yes
O6 C6 H6A 109.2 . . yes
P2 C6 H6A 109.2 . . yes
O6 C6 H6B 109.2 . . yes
P2 C6 H6B 109.2 . . yes
H6A C6 H6B 107.9 . . yes
C6 O6 H6 109.5 . . yes
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
Fe1 N2 1.6563(13) . yes
Fe1 N1 1.6567(16) . yes
Fe1 P2 2.2193(7) . yes
Fe1 P1 2.2459(6) . yes
P1 C4 1.8446(16) . yes
P1 C3 1.8481(18) . yes
P1 C1 1.8493(16) . yes
P2 C2 1.8363(17) . yes
P2 C5 1.8404(17) . yes
P2 C6 1.8503(16) . yes
N1 O1 1.192(2) . yes
N2 O2 1.1827(18) . yes
C1 C2 1.538(2) . yes
C1 H1A 0.9900 . yes
C1 H1B 0.9900 . yes
C2 H2A 0.9900 . yes
C2 H2B 0.9900 . yes
C3 O3 1.425(2) . yes
C3 H3A 0.9900 . yes
C3 H3B 0.9900 . yes
O3 H3 0.8400 . yes
C4 O4 1.431(2) . yes
C4 H4A 0.9900 . yes
C4 H4B 0.9900 . yes
O4 H4 0.76(3) . yes
C5 O5 1.433(2) . yes
C5 H5A 0.9900 . yes
C5 H5B 0.9900 . yes
O5 H5 0.72(3) . yes
C6 O6 1.424(2) . yes
C6 H6A 0.9900 . yes
C6 H6B 0.9900 . yes
O6 H6 0.8400 . yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Fe1 P1 C4 -129.46(8) . . . . yes
N1 Fe1 P1 C4 17.50(8) . . . . yes
P2 Fe1 P1 C4 129.50(6) . . . . yes
N2 Fe1 P1 C3 -6.42(9) . . . . yes
N1 Fe1 P1 C3 140.55(9) . . . . yes
P2 Fe1 P1 C3 -107.45(7) . . . . yes
N2 Fe1 P1 C1 112.25(8) . . . . yes
N1 Fe1 P1 C1 -100.79(8) . . . . yes
P2 Fe1 P1 C1 11.21(6) . . . . yes
N2 Fe1 P2 C2 -106.19(8) . . . . yes
N1 Fe1 P2 C2 118.92(8) . . . . yes
P1 Fe1 P2 C2 10.50(6) . . . . yes
N2 Fe1 P2 C5 136.52(8) . . . . yes
N1 Fe1 P2 C5 1.63(8) . . . . yes
P1 Fe1 P2 C5 -106.79(6) . . . . yes
N2 Fe1 P2 C6 14.74(9) . . . . yes
N1 Fe1 P2 C6 -120.15(9) . . . . yes
P1 Fe1 P2 C6 131.42(7) . . . . yes
C4 P1 C1 C2 -161.90(12) . . . . yes
C3 P1 C1 C2 93.77(13) . . . . yes
Fe1 P1 C1 C2 -35.28(13) . . . . yes
P1 C1 C2 P2 43.54(14) . . . . yes
C5 P2 C2 C1 89.26(12) . . . . yes
C6 P2 C2 C1 -163.87(11) . . . . yes
Fe1 P2 C2 C1 -34.76(12) . . . . yes
C4 P1 C3 O3 -167.20(12) . . . . yes
C1 P1 C3 O3 -59.98(13) . . . . yes
Fe1 P1 C3 O3 61.66(14) . . . . yes
C3 P1 C4 O4 65.10(13) . . . . yes
C1 P1 C4 O4 -41.28(14) . . . . yes
Fe1 P1 C4 O4 -162.17(9) . . . . yes
C2 P2 C5 O5 47.01(13) . . . . yes
C6 P2 C5 O5 -61.63(13) . . . . yes
Fe1 P2 C5 O5 167.96(9) . . . . yes
C2 P2 C6 O6 59.34(14) . . . . yes
C5 P2 C6 O6 167.43(12) . . . . yes
Fe1 P2 C6 O6 -64.52(14) . . . . yes
