#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:01:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180368 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/37/7203705.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_7203705
loop_
_publ_author_name
'Armentano, Donatella'
'De Munno, Giovanni'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Bis and tris(oxalato)ferrate(iii) complexes as precursors of
 polynuclear compounds
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              57
_journal_paper_doi               10.1039/b417251e
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C40 H30 As Fe N2 O9'
_chemical_formula_weight         813.43
_chemical_name_systematic
;
?
;
_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                103.57(3)
_cell_angle_beta                 99.94(3)
_cell_angle_gamma                105.77(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4991(19)
_cell_length_b                   14.279(3)
_cell_length_c                   14.557(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     1787.2(8)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'R3m/V automatic four-circle diffractometer'
_diffrn_measurement_method       omega/2-theta-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7663
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        2.4
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.7669
_exptl_absorpt_correction_T_min  0.5409
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0688P)²+1.0123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                4854
_reflns_number_total             7058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417251e.txt
_cod_data_source_block           4
_cod_original_cell_volume        1787.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203705
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
Fe1 Fe 0.60832(7) 0.49280(5) 0.28448(4) 0.04906(18) Uani 1 1 d . . .
N1 N 0.8089(4) 0.5478(3) 0.2367(2) 0.0497(8) Uani 1 1 d . . .
N2 N 0.7856(4) 0.5542(2) 0.4179(2) 0.0464(8) Uani 1 1 d . . .
C1 C 0.8181(5) 0.5454(4) 0.1458(3) 0.0577(11) Uani 1 1 d . . .
H1A H 0.7302 0.5166 0.0955 0.069 Uiso 1 1 calc R . .
C2 C 0.9541(6) 0.5844(4) 0.1238(4) 0.0685(13) Uani 1 1 d . . .
H2A H 0.9559 0.5813 0.0595 0.082 Uiso 1 1 calc R . .
C3 C 1.0851(6) 0.6274(4) 0.1957(4) 0.0661(13) Uani 1 1 d . . .
H3A H 1.1765 0.6533 0.1810 0.079 Uiso 1 1 calc R . .
C4 C 1.0799(5) 0.6320(3) 0.2927(3) 0.0552(11) Uani 1 1 d . . .
C5 C 1.2105(5) 0.6765(4) 0.3746(4) 0.0628(12) Uani 1 1 d . . .
H5A H 1.3049 0.7044 0.3644 0.075 Uiso 1 1 calc R . .
C6 C 1.1982(5) 0.6785(4) 0.4652(3) 0.0623(12) Uani 1 1 d . . .
H6A H 1.2845 0.7077 0.5168 0.075 Uiso 1 1 calc R . .
C7 C 1.0549(5) 0.6368(3) 0.4847(3) 0.0490(10) Uani 1 1 d . . .
C8 C 1.0328(5) 0.6387(3) 0.5782(3) 0.0545(11) Uani 1 1 d . . .
H8A H 1.1151 0.6662 0.6326 0.065 Uiso 1 1 calc R . .
C9 C 0.8924(5) 0.6007(4) 0.5889(3) 0.0604(12) Uani 1 1 d . . .
H9A H 0.8776 0.6028 0.6507 0.072 Uiso 1 1 calc R . .
C10 C 0.7691(5) 0.5582(3) 0.5070(3) 0.0530(10) Uani 1 1 d . . .
H10A H 0.6728 0.5320 0.5154 0.064 Uiso 1 1 calc R . .
C11 C 0.9391(5) 0.5906(3) 0.3090(3) 0.0464(9) Uani 1 1 d . . .
C12 C 0.9261(5) 0.5936(3) 0.4065(3) 0.0461(9) Uani 1 1 d . . .
O1 O 0.6383(3) 0.3576(2) 0.2526(2) 0.0566(7) Uani 1 1 d . . .
O2 O 0.4628(3) 0.4242(2) 0.3481(2) 0.0578(7) Uani 1 1 d . . .
C13 C 0.5608(5) 0.2924(4) 0.2876(3) 0.0561(11) Uani 1 1 d . . .
C14 C 0.4545(5) 0.3323(4) 0.3440(3) 0.0592(11) Uani 1 1 d . . .
O3 O 0.3718(4) 0.2777(3) 0.3796(3) 0.0860(11) Uani 1 1 d . . .
O4 O 0.5710(4) 0.2079(3) 0.2808(3) 0.0808(10) Uani 1 1 d . . .
O5 O 0.4755(3) 0.4736(2) 0.1568(2) 0.0604(8) Uani 1 1 d . . .
O6 O 0.5768(4) 0.6270(2) 0.3136(2) 0.0635(8) Uani 1 1 d . . .
C15 C 0.4963(5) 0.6430(4) 0.2423(4) 0.0614(12) Uani 1 1 d . . .
C16 C 0.4241(5) 0.5471(4) 0.1516(3) 0.0625(12) Uani 1 1 d . . .
O7 O 0.4732(4) 0.7223(3) 0.2431(3) 0.0858(11) Uani 1 1 d . . .
O8 O 0.3289(4) 0.5467(3) 0.0836(3) 0.0902(12) Uani 1 1 d . . .
As1 As 0.94878(5) 0.03174(3) 0.20906(3) 0.05228(15) Uani 1 1 d . . .
C17 C 1.1099(5) -0.0242(3) 0.2009(3) 0.0552(11) Uani 1 1 d . . .
C18 C 1.2435(6) 0.0183(5) 0.2706(5) 0.106(2) Uani 1 1 d . . .
H18A H 1.2580 0.0754 0.3222 0.127 Uiso 1 1 calc R . .
C19 C 1.3571(7) -0.0238(5) 0.2638(5) 0.113(3) Uani 1 1 d . . .
H19A H 1.4475 0.0047 0.3121 0.135 Uiso 1 1 calc R . .
C20 C 1.3399(7) -0.1055(4) 0.1887(5) 0.0848(17) Uani 1 1 d . . .
H20A H 1.4171 -0.1335 0.1852 0.102 Uiso 1 1 calc R . .
C21 C 1.2087(7) -0.1457(4) 0.1188(4) 0.0864(17) Uani 1 1 d . . .
H21A H 1.1964 -0.2017 0.0666 0.104 Uiso 1 1 calc R . .
C22 C 1.0919(6) -0.1058(4) 0.1231(4) 0.0720(14) Uani 1 1 d . . .
H22A H 1.0025 -0.1338 0.0738 0.086 Uiso 1 1 calc R . .
C23 C 0.7707(5) -0.0644(4) 0.1163(3) 0.0594(11) Uani 1 1 d . . .
C24 C 0.7166(7) -0.1623(4) 0.1231(4) 0.0880(18) Uani 1 1 d . . .
H24A H 0.7633 -0.1806 0.1744 0.106 Uiso 1 1 calc R . .
C25 C 0.5922(7) -0.2322(5) 0.0526(5) 0.101(2) Uani 1 1 d . . .
H25A H 0.5529 -0.2976 0.0571 0.121 Uiso 1 1 calc R . .
C26 C 0.5266(6) -0.2051(5) -0.0241(4) 0.0893(19) Uani 1 1 d . . .
H26A H 0.4433 -0.2529 -0.0716 0.107 Uiso 1 1 calc R . .
C27 C 0.5808(6) -0.1094(5) -0.0323(4) 0.0806(16) Uani 1 1 d . . .
H27A H 0.5355 -0.0923 -0.0850 0.097 Uiso 1 1 calc R . .
C28 C 0.7033(5) -0.0386(4) 0.0384(3) 0.0667(13) Uani 1 1 d . . .
H28A H 0.7408 0.0269 0.0336 0.080 Uiso 1 1 calc R . .
C29 C 0.9942(5) 0.1567(3) 0.1757(3) 0.0479(9) Uani 1 1 d . . .
C30 C 0.8934(5) 0.2109(3) 0.1813(3) 0.0516(10) Uani 1 1 d . . .
H30A H 0.8054 0.1865 0.2004 0.062 Uiso 1 1 calc R . .
C31 C 0.9248(6) 0.3007(4) 0.1585(3) 0.0592(12) Uani 1 1 d . . .
H31A H 0.8575 0.3373 0.1616 0.071 Uiso 1 1 calc R . .
C32 C 1.0560(6) 0.3373(4) 0.1307(3) 0.0635(12) Uani 1 1 d . . .
H32A H 1.0769 0.3985 0.1155 0.076 Uiso 1 1 calc R . .
C33 C 1.1561(6) 0.2830(4) 0.1256(3) 0.0632(12) Uani 1 1 d . . .
H33A H 1.2445 0.3080 0.1070 0.076 Uiso 1 1 calc R . .
C34 C 1.1256(5) 0.1924(3) 0.1478(3) 0.0575(11) Uani 1 1 d . . .
H34A H 1.1926 0.1555 0.1441 0.069 Uiso 1 1 calc R . .
C35 C 0.9230(6) 0.0597(4) 0.3384(3) 0.0621(12) Uani 1 1 d . . .
C36 C 0.7936(7) 0.0074(6) 0.3590(5) 0.0941(19) Uani 1 1 d . . .
H36A H 0.7149 -0.0422 0.3096 0.113 Uiso 1 1 calc R . .
C37 C 0.7828(10) 0.0308(7) 0.4571(6) 0.116(3) Uani 1 1 d . . .
H37A H 0.6955 -0.0022 0.4727 0.140 Uiso 1 1 calc R . .
C38 C 0.9007(12) 0.1015(7) 0.5280(5) 0.112(3) Uani 1 1 d . . .
H38A H 0.8925 0.1173 0.5921 0.134 Uiso 1 1 calc R . .
C39 C 1.0302(10) 0.1497(5) 0.5077(4) 0.100(2) Uani 1 1 d . . .
H39A H 1.1115 0.1955 0.5579 0.120 Uiso 1 1 calc R . .
C40 C 1.0412(7) 0.1305(4) 0.4126(4) 0.0770(15) Uani 1 1 d . . .
H40A H 1.1286 0.1654 0.3982 0.092 Uiso 1 1 calc R . .
O9 O 0.4299(8) 0.1774(6) 0.5241(5) 0.201(3) 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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
O2 Fe1 O5 101.25(13) . . ?
O2 Fe1 O6 98.88(14) . . ?
O5 Fe1 O6 81.80(13) . . ?
O2 Fe1 O1 81.51(13) . . ?
O5 Fe1 O1 97.18(13) . . ?
O6 Fe1 O1 178.95(12) . . ?
O2 Fe1 N1 163.10(13) . . ?
O5 Fe1 N1 92.16(13) . . ?
O6 Fe1 N1 93.12(14) . . ?
O1 Fe1 N1 86.70(13) . . ?
O2 Fe1 N2 92.18(13) . . ?
O5 Fe1 N2 163.75(13) . . ?
O6 Fe1 N2 87.16(13) . . ?
O1 Fe1 N2 93.80(13) . . ?
N1 Fe1 N2 76.51(13) . . ?
C1 N1 C11 117.7(4) . . ?
C1 N1 Fe1 127.4(3) . . ?
C11 N1 Fe1 114.9(3) . . ?
C10 N2 C12 118.7(3) . . ?
C10 N2 Fe1 126.6(3) . . ?
C12 N2 Fe1 114.7(2) . . ?
N1 C1 C2 122.3(4) . . ?
C3 C2 C1 120.5(4) . . ?
C2 C3 C4 119.0(4) . . ?
C11 C4 C3 117.2(4) . . ?
C11 C4 C5 118.9(4) . . ?
C3 C4 C5 123.8(4) . . ?
C6 C5 C4 121.0(4) . . ?
C5 C6 C7 121.6(4) . . ?
C12 C7 C8 116.7(4) . . ?
C12 C7 C6 118.5(4) . . ?
C8 C7 C6 124.7(4) . . ?
C9 C8 C7 119.9(4) . . ?
C8 C9 C10 120.0(4) . . ?
N2 C10 C9 121.8(4) . . ?
N1 C11 C4 123.4(4) . . ?
N1 C11 C12 116.7(4) . . ?
C4 C11 C12 119.9(4) . . ?
N2 C12 C7 122.8(4) . . ?
N2 C12 C11 117.1(3) . . ?
C7 C12 C11 120.0(4) . . ?
C13 O1 Fe1 115.1(3) . . ?
C14 O2 Fe1 115.8(3) . . ?
O4 C13 O1 124.4(4) . . ?
O4 C13 C14 122.0(4) . . ?
O1 C13 C14 113.6(4) . . ?
O3 C14 O2 125.4(5) . . ?
O3 C14 C13 120.7(5) . . ?
O2 C14 C13 113.9(4) . . ?
C16 O5 Fe1 115.1(3) . . ?
C15 O6 Fe1 115.4(3) . . ?
O7 C15 O6 125.5(5) . . ?
O7 C15 C16 121.5(5) . . ?
O6 C15 C16 113.0(4) . . ?
O8 C16 O5 125.9(5) . . ?
O8 C16 C15 120.2(5) . . ?
O5 C16 C15 113.9(4) . . ?
C35 As1 C23 111.9(2) . . ?
C35 As1 C29 108.20(19) . . ?
C23 As1 C29 108.72(19) . . ?
C35 As1 C17 110.46(19) . . ?
C23 As1 C17 107.4(2) . . ?
C29 As1 C17 110.09(18) . . ?
C18 C17 C22 119.8(5) . . ?
C18 C17 As1 120.5(4) . . ?
C22 C17 As1 119.7(4) . . ?
C17 C18 C19 119.5(5) . . ?
C20 C19 C18 121.4(6) . . ?
C21 C20 C19 118.8(5) . . ?
C20 C21 C22 121.5(5) . . ?
C17 C22 C21 118.9(5) . . ?
C28 C23 C24 120.1(5) . . ?
C28 C23 As1 119.8(4) . . ?
C24 C23 As1 119.9(4) . . ?
C25 C24 C23 119.1(6) . . ?
C26 C25 C24 119.9(6) . . ?
C27 C26 C25 121.4(5) . . ?
C26 C27 C28 119.2(6) . . ?
C27 C28 C23 120.3(5) . . ?
C34 C29 C30 120.9(4) . . ?
C34 C29 As1 120.5(3) . . ?
C30 C29 As1 118.6(3) . . ?
C31 C30 C29 119.3(4) . . ?
C30 C31 C32 120.4(4) . . ?
C33 C32 C31 120.1(4) . . ?
C34 C33 C32 120.2(5) . . ?
C33 C34 C29 119.1(4) . . ?
C36 C35 C40 120.4(5) . . ?
C36 C35 As1 121.4(4) . . ?
C40 C35 As1 118.2(4) . . ?
C35 C36 C37 118.5(7) . . ?
C38 C37 C36 119.5(7) . . ?
C37 C38 C39 121.6(7) . . ?
C38 C39 C40 119.8(7) . . ?
C39 C40 C35 120.1(6) . . ?
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 O2 1.964(3) . ?
Fe1 O5 1.970(3) . ?
Fe1 O6 1.979(3) . ?
Fe1 O1 1.987(3) . ?
Fe1 N1 2.152(3) . ?
Fe1 N2 2.155(3) . ?
N1 C1 1.335(5) . ?
N1 C11 1.359(5) . ?
N2 C10 1.323(5) . ?
N2 C12 1.355(5) . ?
C1 C2 1.384(6) . ?
C2 C3 1.361(7) . ?
C3 C4 1.409(6) . ?
C4 C11 1.393(6) . ?
C4 C5 1.438(6) . ?
C5 C6 1.339(6) . ?
C6 C7 1.435(6) . ?
C7 C12 1.398(6) . ?
C7 C8 1.408(6) . ?
C8 C9 1.347(6) . ?
C9 C10 1.398(6) . ?
C11 C12 1.438(5) . ?
O1 C13 1.284(5) . ?
O2 C14 1.279(6) . ?
C13 O4 1.219(5) . ?
C13 C14 1.548(7) . ?
C14 O3 1.222(6) . ?
O5 C16 1.284(6) . ?
O6 C15 1.284(5) . ?
C15 O7 1.208(5) . ?
C15 C16 1.555(7) . ?
C16 O8 1.218(5) . ?
As1 C35 1.904(5) . ?
As1 C23 1.910(5) . ?
As1 C29 1.915(4) . ?
As1 C17 1.918(4) . ?
C17 C18 1.362(7) . ?
C17 C22 1.369(6) . ?
C18 C19 1.377(7) . ?
C19 C20 1.348(8) . ?
C20 C21 1.348(8) . ?
C21 C22 1.382(7) . ?
C23 C28 1.380(6) . ?
C23 C24 1.386(7) . ?
C24 C25 1.381(8) . ?
C25 C26 1.370(9) . ?
C26 C27 1.364(8) . ?
C27 C28 1.376(7) . ?
C29 C34 1.383(6) . ?
C29 C30 1.386(6) . ?
C30 C31 1.367(6) . ?
C31 C32 1.381(7) . ?
C32 C33 1.381(7) . ?
C33 C34 1.375(6) . ?
C35 C36 1.375(7) . ?
C35 C40 1.379(7) . ?
C36 C37 1.417(9) . ?
C37 C38 1.355(11) . ?
C38 C39 1.355(10) . ?
C39 C40 1.375(8) . ?
