#------------------------------------------------------------------------------
#$Date: 2015-08-05 20:36:09 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152794 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/34/4343422.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_4343422
loop_
_publ_author_name
'Fliedel, Christophe'
'Rosa, Vitor'
'Falceto, Andrés'
'Rosa, Patrick'
'Alvarez, Santiago'
'Braunstein, Pierre'
_publ_section_title
;
 Unsymmetrical Chelation of N-Thioether-Functionalized
 Bis(diphenylphosphino)amine-Type Ligands and Substituent Effects on the
 Nuclearity of Iron(II) Complexes: Structures, Magnetism, and Bonding.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6547
_journal_page_last               6559
_journal_paper_doi               10.1021/acs.inorgchem.5b00834
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C62 H54 Cl4 Fe2 N2 P4 S2'
_chemical_formula_sum            'C62 H54 Cl4 Fe2 N2 P4 S2'
_chemical_formula_weight         1268.57
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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                92.167(3)
_cell_angle_beta                 101.448(2)
_cell_angle_gamma                94.786(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6991(5)
_cell_length_b                   11.8203(6)
_cell_length_c                   12.0953(4)
_cell_measurement_reflns_used    3398
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_cell_volume                     1491.67(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9480
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0491
_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)+(0.0646P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                4274
_reflns_number_total             6539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00834_si_002.cif
_cod_data_source_block           Vitor50
_cod_depositor_comments
'Adding full bibliography for 4343421--4343423.cif.'
_cod_database_code               4343422
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 0.58386(4) 0.37735(4) 0.52291(4) 0.02975(15) Uani 1 1 d .
P1 P 0.57864(8) 0.19823(8) 0.66256(7) 0.0324(2) Uani 1 1 d .
P2 P 0.72939(7) 0.40822(7) 0.70906(6) 0.0285(2) Uani 1 1 d .
Cl1 Cl 0.37503(7) 0.41992(7) 0.52624(7) 0.0353(2) Uani 1 1 d .
Cl2 Cl 0.65069(9) 0.29082(8) 0.38210(7) 0.0502(3) Uani 1 1 d .
N1 N 0.6957(2) 0.2792(2) 0.75865(19) 0.0270(6) Uani 1 1 d .
S1 S 0.99427(8) 0.14107(8) 1.19885(7) 0.0423(2) Uani 1 1 d U
C1 C 0.7620(3) 0.2420(3) 0.8653(2) 0.0276(7) Uani 1 1 d .
C2 C 0.7222(3) 0.2676(3) 0.9635(2) 0.0337(8) Uani 1 1 d .
H2 H 0.6491 0.3058 0.9603 0.040 Uiso 1 1 calc R
C3 C 0.7882(3) 0.2378(3) 1.0675(3) 0.0374(8) Uani 1 1 d .
H3 H 0.7588 0.2554 1.1329 0.045 Uiso 1 1 calc R
C4 C 0.8982(3) 0.1819(3) 1.0737(2) 0.0324(8) Uani 1 1 d .
C5 C 0.9371(3) 0.1533(3) 0.9736(3) 0.0407(9) Uani 1 1 d .
H5 H 1.0090 0.1135 0.9763 0.049 Uiso 1 1 calc R
C6 C 0.8701(3) 0.1835(3) 0.8701(3) 0.0382(8) Uani 1 1 d .
H6 H 0.8975 0.1645 0.8040 0.046 Uiso 1 1 calc R
C7 C 0.9145(4) 0.1910(5) 1.3044(3) 0.0812(15) Uani 1 1 d U
H7A H 0.9200 0.2726 1.3072 0.122 Uiso 1 1 calc R
H7B H 0.9543 0.1661 1.3765 0.122 Uiso 1 1 calc R
H7C H 0.8261 0.1613 1.2865 0.122 Uiso 1 1 calc R
C8 C 0.6544(3) 0.0734(3) 0.6291(3) 0.0373(8) Uani 1 1 d .
C9 C 0.7659(4) 0.0913(4) 0.5896(3) 0.0532(10) Uani 1 1 d .
H9 H 0.8038 0.1648 0.5878 0.064 Uiso 1 1 calc R
C10 C 0.8227(4) -0.0023(4) 0.5516(3) 0.0661(13) Uani 1 1 d .
H10 H 0.8967 0.0103 0.5228 0.079 Uiso 1 1 calc R
C11 C 0.7706(4) -0.1114(4) 0.5563(3) 0.0600(12) Uani 1 1 d .
H11 H 0.8093 -0.1728 0.5320 0.072 Uiso 1 1 calc R
C12 C 0.6623(4) -0.1283(4) 0.5967(4) 0.0676(13) Uani 1 1 d .
H12 H 0.6278 -0.2022 0.6025 0.081 Uiso 1 1 calc R
C13 C 0.6013(4) -0.0377(3) 0.6297(3) 0.0540(10) Uani 1 1 d .
H13 H 0.5237 -0.0515 0.6527 0.065 Uiso 1 1 calc R
C14 C 0.4621(3) 0.1486(3) 0.7441(3) 0.0375(8) Uani 1 1 d .
C15 C 0.3479(3) 0.1968(3) 0.7286(3) 0.0458(9) Uani 1 1 d .
H15 H 0.3333 0.2528 0.6768 0.055 Uiso 1 1 calc R
C16 C 0.2536(4) 0.1642(4) 0.7881(3) 0.0550(10) Uani 1 1 d .
H16 H 0.1777 0.1992 0.7767 0.066 Uiso 1 1 calc R
C17 C 0.2720(4) 0.0811(4) 0.8632(3) 0.0569(11) Uani 1 1 d .
H17 H 0.2078 0.0577 0.9014 0.068 Uiso 1 1 calc R
C18 C 0.3859(4) 0.0320(4) 0.8821(3) 0.0594(12) Uani 1 1 d .
H18 H 0.3985 -0.0246 0.9335 0.071 Uiso 1 1 calc R
C19 C 0.4829(4) 0.0663(3) 0.8249(3) 0.0506(10) Uani 1 1 d .
H19 H 0.5608 0.0348 0.8402 0.061 Uiso 1 1 calc R
C20 C 0.9021(3) 0.4301(3) 0.7261(3) 0.0328(7) Uani 1 1 d .
C21 C 0.9534(3) 0.4190(3) 0.6309(3) 0.0412(9) Uani 1 1 d .
H21 H 0.8993 0.4029 0.5608 0.049 Uiso 1 1 calc R
C22 C 1.0849(3) 0.4317(4) 0.6384(3) 0.0537(11) Uani 1 1 d .
H22 H 1.1187 0.4238 0.5737 0.064 Uiso 1 1 calc R
C23 C 1.1646(3) 0.4558(3) 0.7411(3) 0.0531(10) Uani 1 1 d .
H23 H 1.2526 0.4673 0.7456 0.064 Uiso 1 1 calc R
C24 C 1.1159(3) 0.4634(3) 0.8383(3) 0.0505(10) Uani 1 1 d .
H24 H 1.1710 0.4765 0.9083 0.061 Uiso 1 1 calc R
C25 C 0.9848(3) 0.4513(3) 0.8311(3) 0.0441(9) Uani 1 1 d .
H25 H 0.9516 0.4574 0.8963 0.053 Uiso 1 1 calc R
C26 C 0.6854(3) 0.5159(3) 0.8018(2) 0.0309(7) Uani 1 1 d .
C27 C 0.5682(3) 0.4993(3) 0.8339(3) 0.0361(8) Uani 1 1 d .
H27 H 0.5200 0.4293 0.8177 0.043 Uiso 1 1 calc R
C28 C 0.5226(3) 0.5853(3) 0.8894(3) 0.0427(9) Uani 1 1 d .
H28 H 0.4441 0.5724 0.9109 0.051 Uiso 1 1 calc R
C29 C 0.5904(4) 0.6893(4) 0.9135(3) 0.0540(10) Uani 1 1 d .
H29 H 0.5589 0.7466 0.9520 0.065 Uiso 1 1 calc R
C30 C 0.7059(4) 0.7088(4) 0.8801(4) 0.0645(12) Uani 1 1 d .
H30 H 0.7523 0.7797 0.8952 0.077 Uiso 1 1 calc R
C31 C 0.7529(4) 0.6221(3) 0.8237(3) 0.0517(10) Uani 1 1 d .
H31 H 0.8304 0.6357 0.8006 0.062 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
Fe Fe 0.3463 0.8444 '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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
Cl2 Fe1 Cl1 127.04(4) . .
Cl2 Fe1 P2 119.14(4) . .
Cl1 Fe1 P2 113.07(3) . .
Cl2 Fe1 Cl1 98.91(3) . 2_666
Cl1 Fe1 Cl1 86.41(3) . 2_666
P2 Fe1 Cl1 92.89(3) . 2_666
Cl2 Fe1 P1 99.00(3) . .
Cl1 Fe1 P1 94.83(3) . .
P2 Fe1 P1 64.98(3) . .
Cl1 Fe1 P1 156.47(3) 2_666 .
N1 P1 C14 104.52(13) . .
N1 P1 C8 104.56(13) . .
C14 P1 C8 105.36(17) . .
N1 P1 Fe1 86.60(8) . .
C14 P1 Fe1 131.28(12) . .
C8 P1 Fe1 117.61(11) . .
N1 P2 C20 106.87(14) . .
N1 P2 C26 107.91(13) . .
C20 P2 C26 106.03(15) . .
N1 P2 Fe1 97.40(8) . .
C20 P2 Fe1 122.94(11) . .
C26 P2 Fe1 114.32(10) . .
Fe1 Cl1 Fe1 93.59(3) . 2_666
C1 N1 P2 123.57(19) . .
C1 N1 P1 125.4(2) . .
P2 N1 P1 110.96(13) . .
C4 S1 C7 102.37(18) . .
C2 C1 C6 119.1(3) . .
C2 C1 N1 120.6(3) . .
C6 C1 N1 120.2(3) . .
C1 C2 C3 121.6(3) . .
C1 C2 H2 119.2 . .
C3 C2 H2 119.2 . .
C4 C3 C2 119.9(3) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C5 118.6(3) . .
C3 C4 S1 125.4(2) . .
C5 C4 S1 116.0(3) . .
C6 C5 C4 120.9(3) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C1 C6 C5 119.9(3) . .
C1 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
S1 C7 H7A 109.5 . .
S1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
S1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 C13 118.1(4) . .
C9 C8 P1 117.0(3) . .
C13 C8 P1 124.6(3) . .
C8 C9 C10 119.7(4) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C11 C10 C9 121.2(4) . .
C11 C10 H10 119.4 . .
C9 C10 H10 119.4 . .
C12 C11 C10 118.7(4) . .
C12 C11 H11 120.6 . .
C10 C11 H11 120.6 . .
C11 C12 C13 121.3(4) . .
C11 C12 H12 119.4 . .
C13 C12 H12 119.4 . .
C12 C13 C8 120.9(4) . .
C12 C13 H13 119.5 . .
C8 C13 H13 119.5 . .
C15 C14 C19 117.8(3) . .
C15 C14 P1 118.1(3) . .
C19 C14 P1 124.0(3) . .
C14 C15 C16 121.8(4) . .
C14 C15 H15 119.1 . .
C16 C15 H15 119.1 . .
C17 C16 C15 120.2(4) . .
C17 C16 H16 119.9 . .
C15 C16 H16 119.9 . .
C16 C17 C18 119.6(4) . .
C16 C17 H17 120.2 . .
C18 C17 H17 120.2 . .
C17 C18 C19 120.6(4) . .
C17 C18 H18 119.7 . .
C19 C18 H18 119.7 . .
C18 C19 C14 119.8(4) . .
C18 C19 H19 120.1 . .
C14 C19 H19 120.1 . .
C21 C20 C25 118.9(3) . .
C21 C20 P2 117.8(2) . .
C25 C20 P2 123.2(2) . .
C20 C21 C22 120.8(3) . .
C20 C21 H21 119.6 . .
C22 C21 H21 119.6 . .
C23 C22 C21 119.8(3) . .
C23 C22 H22 120.1 . .
C21 C22 H22 120.1 . .
C22 C23 C24 120.7(3) . .
C22 C23 H23 119.7 . .
C24 C23 H23 119.7 . .
C23 C24 C25 119.6(3) . .
C23 C24 H24 120.2 . .
C25 C24 H24 120.2 . .
C24 C25 C20 120.2(3) . .
C24 C25 H25 119.9 . .
C20 C25 H25 119.9 . .
C31 C26 C27 118.4(3) . .
C31 C26 P2 121.8(3) . .
C27 C26 P2 118.7(2) . .
C28 C27 C26 120.5(3) . .
C28 C27 H27 119.7 . .
C26 C27 H27 119.7 . .
C29 C28 C27 121.2(3) . .
C29 C28 H28 119.4 . .
C27 C28 H28 119.4 . .
C28 C29 C30 119.4(4) . .
C28 C29 H29 120.3 . .
C30 C29 H29 120.3 . .
C29 C30 C31 119.8(4) . .
C29 C30 H30 120.1 . .
C31 C30 H30 120.1 . .
C26 C31 C30 120.6(3) . .
C26 C31 H31 119.7 . .
C30 C31 H31 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl2 2.2208(10) .
Fe1 Cl1 2.3386(9) .
Fe1 P2 2.4654(9) .
Fe1 Cl1 2.5150(9) 2_666
Fe1 P1 2.7616(10) .
P1 N1 1.724(2) .
P1 C14 1.811(3) .
P1 C8 1.812(4) .
P2 N1 1.697(2) .
P2 C20 1.813(3) .
P2 C26 1.817(3) .
Cl1 Fe1 2.5150(9) 2_666
N1 C1 1.447(4) .
S1 C4 1.761(3) .
S1 C7 1.780(4) .
C1 C2 1.370(4) .
C1 C6 1.389(4) .
C2 C3 1.389(4) .
C2 H2 0.9300 .
C3 C4 1.388(4) .
C3 H3 0.9300 .
C4 C5 1.395(4) .
C5 C6 1.390(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.375(5) .
C8 C13 1.387(5) .
C9 C10 1.410(6) .
C9 H9 0.9300 .
C10 C11 1.369(6) .
C10 H10 0.9300 .
C11 C12 1.348(6) .
C11 H11 0.9300 .
C12 C13 1.386(6) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C15 1.374(5) .
C14 C19 1.404(5) .
C15 C16 1.389(5) .
C15 H15 0.9300 .
C16 C17 1.363(5) .
C16 H16 0.9300 .
C17 C18 1.375(6) .
C17 H17 0.9300 .
C18 C19 1.399(5) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 C21 1.377(4) .
C20 C25 1.397(4) .
C21 C22 1.387(5) .
C21 H21 0.9300 .
C22 C23 1.365(5) .
C22 H22 0.9300 .
C23 C24 1.380(5) .
C23 H23 0.9300 .
C24 C25 1.383(5) .
C24 H24 0.9300 .
C25 H25 0.9300 .
C26 C31 1.384(5) .
C26 C27 1.386(4) .
C27 C28 1.371(5) .
C27 H27 0.9300 .
C28 C29 1.366(5) .
C28 H28 0.9300 .
C29 C30 1.378(5) .
C29 H29 0.9300 .
C30 C31 1.392(5) .
C30 H30 0.9300 .
C31 H31 0.9300 .
