#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:05:28 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179523 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/20/4342041.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_4342041
loop_
_publ_author_name
'Iasco, Olga'
'Rivière, Eric'
'Guillot, Régis'
'Buron-Le Cointe, Marylise'
'Meunier, Jean-François'
'Bousseksou, Azzedine'
'Boillot, Marie-Laure'
_publ_section_title
;
 Fe(II)(pap-5NO2)2 and Fe(II)(qsal-5NO2)2 Schiff-Base Spin-Crossover
 Complexes: A Rare Example with Photomagnetism and Room-Temperature
 Bistability.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1791
_journal_page_last               1799
_journal_paper_doi               10.1021/ic5027043
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C32 H20 Fe N6 O6'
_chemical_formula_sum            'C32 H20 Fe N6 O6'
_chemical_formula_weight         640.39
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      54
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2422(13)
_cell_length_b                   10.4155(9)
_cell_length_c                   12.9086(10)
_cell_measurement_reflns_used    2310
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      21.68
_cell_measurement_theta_min      2.73
_cell_volume                     2587.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33767
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.9936
_exptl_absorpt_correction_T_min  0.8761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         1884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0547
_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)+(0.0736P)²+4.4874P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1557
_reflns_number_gt                1295
_reflns_number_total             1884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5027043_si_002.cif
_cod_data_source_block           FeII(qsal-5-NO2)2_100K
_cod_depositor_comments
'Adding full bibliography for 4342039--4342041.cif.'
_cod_database_code               4342041
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
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
Fe Fe 0.5000 0.35275(9) 0.2500 0.0277(3) Uani 1 2 d S
N1 N 0.4336(2) 0.2217(4) 0.2088(3) 0.0302(10) Uani 1 1 d .
C11 C 0.3892(3) 0.5174(5) 0.3883(4) 0.0307(12) Uani 1 1 d .
N2 N 0.5255(2) 0.3495(4) 0.1053(3) 0.0291(10) Uani 1 1 d .
O1 O 0.43285(16) 0.4851(3) 0.2150(2) 0.0305(9) Uani 1 1 d .
C12 C 0.3913(3) 0.5409(5) 0.2781(4) 0.0316(13) Uani 1 1 d .
C5 C 0.4398(3) 0.1880(5) 0.1059(4) 0.0329(13) Uani 1 1 d .
C4 C 0.3991(3) 0.0887(5) 0.0619(5) 0.0396(14) Uani 1 1 d .
C1 C 0.3876(3) 0.1609(5) 0.2645(4) 0.0368(13) Uani 1 1 d .
H1 H 0.3825 0.1842 0.3336 0.044 Uiso 1 1 calc R
C16 C 0.3430(3) 0.5900(5) 0.4492(4) 0.0359(13) Uani 1 1 d .
H16 H 0.3422 0.5776 0.5206 0.043 Uiso 1 1 calc R
C2 C 0.3451(3) 0.0615(5) 0.2253(5) 0.0449(15) Uani 1 1 d .
H2 H 0.3131 0.0213 0.2684 0.054 Uiso 1 1 calc R
O3 O 0.2229(2) 0.8404(5) 0.4353(4) 0.0725(15) Uani 1 1 d .
C10 C 0.5689(3) 0.4256(5) 0.0604(4) 0.0322(12) Uani 1 1 d .
H10 H 0.5730 0.4196 -0.0112 0.039 Uiso 1 1 calc R
C13 C 0.3439(3) 0.6333(5) 0.2386(5) 0.0400(14) Uani 1 1 d .
H13 H 0.3434 0.6489 0.1677 0.048 Uiso 1 1 calc R
C15 C 0.2993(3) 0.6782(5) 0.4058(5) 0.0416(15) Uani 1 1 d .
C9 C 0.4883(2) 0.2553(5) 0.0468(4) 0.0314(12) Uani 1 1 d .
O2 O 0.2541(2) 0.7290(4) 0.5648(3) 0.0643(13) Uani 1 1 d .
C3 C 0.3508(3) 0.0252(5) 0.1267(5) 0.0421(15) Uani 1 1 d .
H3 H 0.3235 -0.0411 0.1008 0.050 Uiso 1 1 calc R
N3 N 0.2552(3) 0.7507(5) 0.4720(4) 0.0497(13) Uani 1 1 d .
C8 C 0.4964(3) 0.2268(6) -0.0561(4) 0.0447(14) Uani 1 1 d .
H8 H 0.5286 0.2708 -0.0964 0.054 Uiso 1 1 calc R
C14 C 0.2993(3) 0.6998(6) 0.3003(4) 0.0436(15) Uani 1 1 d .
H14 H 0.2689 0.7595 0.2715 0.052 Uiso 1 1 calc R
C6 C 0.4075(3) 0.0626(6) -0.0417(5) 0.0495(16) Uani 1 1 d .
H6 H 0.3808 -0.0009 -0.0729 0.059 Uiso 1 1 calc R
C7 C 0.4551(3) 0.1301(6) -0.0991(5) 0.0538(18) Uani 1 1 d .
H7 H 0.4601 0.1108 -0.1690 0.065 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'
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'
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
N2 Fe N2 178.0(3) . 3_655
N2 Fe O1 87.47(15) . .
N2 Fe O1 93.94(16) 3_655 .
N2 Fe O1 93.94(16) . 3_655
N2 Fe O1 87.47(15) 3_655 3_655
O1 Fe O1 89.6(2) . 3_655
N2 Fe N1 94.93(17) . 3_655
N2 Fe N1 83.68(17) 3_655 3_655
O1 Fe N1 177.57(15) . 3_655
O1 Fe N1 89.83(15) 3_655 3_655
N2 Fe N1 83.68(17) . .
N2 Fe N1 94.93(17) 3_655 .
O1 Fe N1 89.83(15) . .
O1 Fe N1 177.57(15) 3_655 .
N1 Fe N1 90.8(2) 3_655 .
C1 N1 C5 117.8(5) . .
C1 N1 Fe 129.5(4) . .
C5 N1 Fe 112.7(3) . .
C16 C11 C10 117.5(5) . 3_655
C16 C11 C12 118.5(5) . .
C10 C11 C12 124.0(5) 3_655 .
C10 N2 C9 120.6(4) . .
C10 N2 Fe 126.1(4) . .
C9 N2 Fe 113.3(3) . .
C12 O1 Fe 126.1(3) . .
O1 C12 C13 118.7(5) . .
O1 C12 C11 124.5(5) . .
C13 C12 C11 116.8(5) . .
N1 C5 C9 117.2(5) . .
N1 C5 C4 121.6(5) . .
C9 C5 C4 121.2(5) . .
C6 C4 C3 124.0(5) . .
C6 C4 C5 118.0(6) . .
C3 C4 C5 117.9(5) . .
N1 C1 C2 123.4(5) . .
C15 C16 C11 121.4(5) . .
C3 C2 C1 120.2(6) . .
N2 C10 C11 125.0(5) . 3_655
C14 C13 C12 122.7(6) . .
C16 C15 C14 121.0(5) . .
C16 C15 N3 118.6(6) . .
C14 C15 N3 120.4(5) . .
C8 C9 C5 119.9(5) . .
C8 C9 N2 127.1(5) . .
C5 C9 N2 113.0(4) . .
C2 C3 C4 119.1(5) . .
O3 N3 O2 121.0(5) . .
O3 N3 C15 118.6(5) . .
O2 N3 C15 120.2(5) . .
C9 C8 C7 118.4(6) . .
C13 C14 C15 119.6(5) . .
C4 C6 C7 120.2(6) . .
C6 C7 C8 122.3(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N2 1.932(4) .
Fe N2 1.932(4) 3_655
Fe O1 1.943(3) .
Fe O1 1.943(3) 3_655
Fe N1 1.944(4) 3_655
Fe N1 1.944(4) .
N1 C1 1.304(6) .
N1 C5 1.379(6) .
C11 C16 1.407(7) .
C11 C10 1.415(7) 3_655
C11 C12 1.445(7) .
N2 C10 1.289(6) .
N2 C9 1.430(6) .
O1 C12 1.281(6) .
C12 C13 1.420(7) .
C5 C9 1.394(7) .
C5 C4 1.416(7) .
C4 C6 1.374(8) .
C4 C3 1.413(8) .
C1 C2 1.413(7) .
C16 C15 1.366(8) .
C2 C3 1.332(8) .
O3 N3 1.218(6) .
C10 C11 1.415(7) 3_655
C13 C14 1.361(8) .
C15 C14 1.381(8) .
C15 N3 1.422(7) .
C9 C8 1.370(7) .
O2 N3 1.220(6) .
C8 C7 1.398(8) .
C6 C7 1.373(8) .
