# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Feazpqsal_90K
_database_code_depnum_ccdc_archive 'CCDC 1535601'
_audit_update_record             
;
2017-03-22 deposited with the CCDC.
2017-03-31 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[Fe(azp)(qsal)]0.5MeOH'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28.50 H21 Fe N4 O3.50'
_chemical_formula_iupac          ?
_chemical_formula_weight         531.34

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.211(7)
_cell_length_b                   11.779(11)
_cell_length_c                   11.954(11)
_cell_angle_alpha                95.645(13)
_cell_angle_beta                 100.928(12)
_cell_angle_gamma                97.980(12)
_cell_volume                     1114.9(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1939
_cell_measurement_theta_min      2.5598
_cell_measurement_theta_max      28.0099
_cell_measurement_temperature    90.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.99

_exptl_special_details           
;
;

_diffrn_ambient_temperature      90.(2)

_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            5259
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.948
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             4318
_reflns_number_gt                3399
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.2032
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_number_reflns         4318
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1154P)²+3.0556P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.224
_refine_diff_density_min         -0.863
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 786)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.9184(5) 0.2149(4) 0.7490(4) 0.0282(10) Uani d . . . 1 A 4
C C2 1.0571(5) 0.1597(4) 0.7404(4) 0.0246(9) Uani d . . . 1 A 4
H H2 1.0991 0.1565 0.6716 0.029 Uiso calc U . R 1 A 4
C C3 1.1320(5) 0.1099(4) 0.8325(4) 0.0264(10) Uani d . . . 1 A 4
H H3 1.2264 0.0731 0.8265 0.032 Uiso calc U . R 1 A 4
C C4 1.0727(6) 0.1126(4) 0.9334(4) 0.0326(11) Uani d . . . 1 A 4
H H4 1.1252 0.0773 0.9957 0.039 Uiso calc U . R 1 A 4
C C5 0.9360(6) 0.1672(4) 0.9431(5) 0.0355(12) Uani d . . . 1 A 4
H H5 0.8945 0.1698 1.0121 0.043 Uiso calc U . R 1 A 4
C C6 0.8601(6) 0.2181(4) 0.8511(5) 0.0325(12) Uani d . . . 1 A 4
C C7 0.4229(6) 0.3905(4) 0.8099(4) 0.0241(10) Uani d . . . 1 B 4
C C8 0.2727(5) 0.4324(4) 0.8225(4) 0.0237(9) Uani d . . . 1 B 4
H H8 0.2104 0.4624 0.76 0.028 Uiso calc U . R 1 B 4
C C9 0.2162(5) 0.4304(4) 0.9225(4) 0.0246(10) Uani d . . . 1 B 4
H H9 0.1157 0.4597 0.9286 0.03 Uiso calc U . R 1 B 4
C C10 0.3036(6) 0.3859(4) 1.0164(4) 0.0305(11) Uani d . . . 1 B 4
H H10 0.264 0.3866 1.0862 0.037 Uiso calc U . R 1 B 4
C C11 0.4463(6) 0.3416(4) 1.0067(5) 0.0327(11) Uani d . . . 1 B 4
H H11 0.5055 0.3108 1.0699 0.039 Uiso calc U . R 1 B 4
C C12 0.5063(5) 0.3411(4) 0.9044(5) 0.0285(10) Uani d . . . 1 B 4
C C13 0.8837(5) 0.5508(4) 0.7011(4) 0.0200(9) Uani d . . . 1 C 4
C C14 1.0094(5) 0.6403(4) 0.7667(4) 0.0247(10) Uani d . . . 1 C 4
H H14 1.0389 0.6418 0.8476 0.03 Uiso calc U . R 1 C 4
C C15 1.0892(6) 0.7246(4) 0.7151(4) 0.0270(10) Uani d . . . 1 C 4
H H15 1.1741 0.7827 0.7608 0.032 Uiso calc U . R 1 C 4
C C16 1.0475(6) 0.7261(4) 0.5961(5) 0.0334(11) Uani d . . . 1 C 4
H H16 1.104 0.7842 0.561 0.04 Uiso calc U . R 1 C 4
C C17 0.9238(6) 0.6425(4) 0.5312(4) 0.0293(11) Uani d . . . 1 C 4
H H17 0.8935 0.6443 0.4508 0.035 Uiso calc U . R 1 C 4
C C18 0.8398(5) 0.5534(4) 0.5809(4) 0.0217(9) Uani d . . . 1 C 4
C C19 0.4562(5) 0.1049(4) 0.6630(4) 0.0226(9) Uani d . . . 1 D 4
H H19 0.4994 0.1026 0.7422 0.027 Uiso calc U . R 1 D 4
C C20 0.3377(5) 0.0114(4) 0.6005(4) 0.0254(10) Uani d . . . 1 D 4
H H20 0.3018 -0.0527 0.6373 0.03 Uiso calc U . R 1 D 4
C C21 0.2753(5) 0.0135(4) 0.4871(4) 0.0244(9) Uani d . . . 1 D 4
H H21 0.1944 -0.049 0.4447 0.029 Uiso calc U . R 1 D 4
C C22 0.3303(5) 0.1086(4) 0.4316(4) 0.0223(9) Uani d . . . 1 D 4
C C23 0.2770(5) 0.1190(4) 0.3151(4) 0.0254(10) Uani d . . . 1 D 4
H H23 0.196 0.06 0.2672 0.03 Uiso calc U . R 1 D 4
C C24 0.3410(6) 0.2139(4) 0.2697(4) 0.0261(10) Uani d . . . 1 D 4
H H24 0.3048 0.2189 0.1903 0.031 Uiso calc U . R 1 D 4
C C25 0.4600(6) 0.3047(4) 0.3387(4) 0.0243(9) Uani d . . . 1 D 4
H H25 0.5014 0.3702 0.3059 0.029 Uiso calc U . R 1 D 4
C C26 0.5152(5) 0.2975(4) 0.4536(4) 0.0197(9) Uani d . . . 1 D 4
C C27 0.4495(5) 0.1998(4) 0.5006(4) 0.0189(9) Uani d . . . 1 D 4
C C28 0.7159(5) 0.4690(4) 0.5048(4) 0.0216(9) Uani d . . . 1 C 4
H H28 0.6929 0.4793 0.4258 0.026 Uiso calc U . R 1 C 4
O O4 0.3960(11) 0.9165(8) 0.9315(8) 0.052(2) Uani d . P . 0.5 E -1
Fe Fe1 0.66613(7) 0.33697(5) 0.69009(5) 0.0204(2) Uani d . . . 1 . .
N N1 0.7118(7) 0.2824(4) 0.8361(4) 0.0482(14) Uani d . . . 1 . .
N N2 0.6524(7) 0.2848(5) 0.9186(4) 0.0529(14) Uani d . . . 1 . .
N N3 0.6323(4) 0.3795(3) 0.5353(3) 0.0182(7) Uani d . . . 1 . .
N N4 0.5093(4) 0.1957(3) 0.6154(3) 0.0185(7) Uani d . . . 1 . .
O O1 0.8442(4) 0.2617(3) 0.6596(3) 0.0304(8) Uani d . . . 1 . .
O O2 0.4758(4) 0.3989(3) 0.7140(3) 0.0276(7) Uani d . . . 1 . .
O O3 0.8158(4) 0.4728(3) 0.7570(3) 0.0251(7) Uani d . . . 1 . .
C C29 0.484(3) 1.012(2) 1.018(2) 0.040(4) Uani d . P . 0.5 E -1
H H29A 0.4187 1.0238 1.077 0.06 Uiso calc U P R 0.5 E -1
H H29B 0.4995 1.083 0.981 0.06 Uiso calc U P R 0.5 E -1
H H29C 0.5946 0.9952 1.0527 0.06 Uiso calc U P R 0.5 E -1


_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.334(6) ?
C1 C6 . 1.391(7) ?
C1 C2 . 1.403(6) ?
C2 C3 . 1.380(7) ?
C2 H2 . 0.95 ?
C3 C4 . 1.383(7) ?
C3 H3 . 0.95 ?
C4 C5 . 1.386(8) ?
C4 H4 . 0.95 ?
C5 C6 . 1.390(8) ?
C5 H5 . 0.95 ?
C6 N1 . 1.513(8) ?
C7 O2 . 1.309(5) ?
C7 C8 . 1.418(6) ?
C7 C12 . 1.425(7) ?
C8 C9 . 1.363(6) ?
C8 H8 . 0.95 ?
C9 C10 . 1.402(7) ?
C9 H9 . 0.95 ?
C10 C11 . 1.368(7) ?
C10 H10 . 0.95 ?
C11 C12 . 1.402(7) ?
C11 H11 . 0.95 ?
C12 N2 . 1.440(8) ?
C13 O3 . 1.312(5) ?
C13 C18 . 1.417(6) ?
C13 C14 . 1.421(6) ?
C14 C15 . 1.375(6) ?
C14 H14 . 0.95 ?
C15 C16 . 1.401(7) ?
C15 H15 . 0.95 ?
C16 C17 . 1.369(7) ?
C16 H16 . 0.95 ?
C17 C18 . 1.417(6) ?
C17 H17 . 0.95 ?
C18 C28 . 1.429(6) ?
C19 N4 . 1.320(6) ?
C19 C20 . 1.409(6) ?
C19 H19 . 0.95 ?
C20 C21 . 1.359(7) ?
C20 H20 . 0.95 ?
C21 C22 . 1.421(6) ?
C21 H21 . 0.95 ?
C22 C23 . 1.401(7) ?
C22 C27 . 1.421(6) ?
C23 C24 . 1.373(7) ?
C23 H23 . 0.95 ?
C24 C25 . 1.417(6) ?
C24 H24 . 0.95 ?
C25 C26 . 1.377(6) ?
C25 H25 . 0.95 ?
C26 C27 . 1.414(6) ?
C26 N3 . 1.418(5) ?
C27 N4 . 1.375(6) ?
C28 N3 . 1.298(6) ?
C28 H28 . 0.95 ?
O4 C29 . 1.46(3) ?
Fe1 O2 . 1.871(3) ?
Fe1 O3 . 1.882(3) ?
Fe1 O1 . 1.885(4) ?
Fe1 N1 . 1.908(5) ?
Fe1 N3 . 1.944(4) ?
Fe1 N4 . 1.975(4) ?
N1 N2 . 1.180(7) ?
C29 H29A . 0.98 ?
C29 H29B . 0.98 ?
C29 H29C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 C6 . . 121.5(4) ?
O1 C1 C2 . . 119.7(4) ?
C6 C1 C2 . . 118.8(5) ?
C3 C2 C1 . . 119.6(4) ?
C3 C2 H2 . . 120.2 ?
C1 C2 H2 . . 120.2 ?
C2 C3 C4 . . 121.4(4) ?
C2 C3 H3 . . 119.3 ?
C4 C3 H3 . . 119.3 ?
C3 C4 C5 . . 119.5(5) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
C4 C5 C6 . . 119.6(5) ?
C4 C5 H5 . . 120.2 ?
C6 C5 H5 . . 120.2 ?
C5 C6 C1 . . 121.2(4) ?
C5 C6 N1 . . 131.6(5) ?
C1 C6 N1 . . 107.3(5) ?
O2 C7 C8 . . 118.9(4) ?
O2 C7 C12 . . 124.3(4) ?
C8 C7 C12 . . 116.8(4) ?
C9 C8 C7 . . 121.3(4) ?
C9 C8 H8 . . 119.4 ?
C7 C8 H8 . . 119.4 ?
C8 C9 C10 . . 121.2(4) ?
C8 C9 H9 . . 119.4 ?
C10 C9 H9 . . 119.4 ?
C11 C10 C9 . . 119.3(4) ?
C11 C10 H10 . . 120.3 ?
C9 C10 H10 . . 120.3 ?
C10 C11 C12 . . 120.7(5) ?
C10 C11 H11 . . 119.6 ?
C12 C11 H11 . . 119.6 ?
C11 C12 C7 . . 120.6(4) ?
C11 C12 N2 . . 107.8(5) ?
C7 C12 N2 . . 131.7(5) ?
O3 C13 C18 . . 125.1(4) ?
O3 C13 C14 . . 117.2(4) ?
C18 C13 C14 . . 117.7(4) ?
C15 C14 C13 . . 121.2(4) ?
C15 C14 H14 . . 119.4 ?
C13 C14 H14 . . 119.4 ?
C14 C15 C16 . . 121.0(4) ?
C14 C15 H15 . . 119.5 ?
C16 C15 H15 . . 119.5 ?
C17 C16 C15 . . 118.9(4) ?
C17 C16 H16 . . 120.5 ?
C15 C16 H16 . . 120.5 ?
C16 C17 C18 . . 121.8(4) ?
C16 C17 H17 . . 119.1 ?
C18 C17 H17 . . 119.1 ?
C17 C18 C13 . . 119.3(4) ?
C17 C18 C28 . . 117.0(4) ?
C13 C18 C28 . . 123.6(4) ?
N4 C19 C20 . . 122.2(4) ?
N4 C19 H19 . . 118.9 ?
C20 C19 H19 . . 118.9 ?
C21 C20 C19 . . 119.5(4) ?
C21 C20 H20 . . 120.3 ?
C19 C20 H20 . . 120.3 ?
C20 C21 C22 . . 120.4(4) ?
C20 C21 H21 . . 119.8 ?
C22 C21 H21 . . 119.8 ?
C23 C22 C21 . . 125.2(4) ?
C23 C22 C27 . . 117.9(4) ?
C21 C22 C27 . . 116.8(4) ?
C24 C23 C22 . . 120.4(4) ?
C24 C23 H23 . . 119.8 ?
C22 C23 H23 . . 119.8 ?
C23 C24 C25 . . 121.5(4) ?
C23 C24 H24 . . 119.3 ?
C25 C24 H24 . . 119.3 ?
C26 C25 C24 . . 119.7(4) ?
C26 C25 H25 . . 120.2 ?
C24 C25 H25 . . 120.2 ?
C25 C26 C27 . . 118.9(4) ?
C25 C26 N3 . . 127.5(4) ?
C27 C26 N3 . . 113.6(4) ?
N4 C27 C26 . . 117.0(4) ?
N4 C27 C22 . . 121.5(4) ?
C26 C27 C22 . . 121.5(4) ?
N3 C28 C18 . . 125.0(4) ?
N3 C28 H28 . . 117.5 ?
C18 C28 H28 . . 117.5 ?
O2 Fe1 O3 . . 93.80(15) ?
O2 Fe1 O1 . . 174.62(14) ?
O3 Fe1 O1 . . 91.58(15) ?
O2 Fe1 N1 . . 95.5(2) ?
O3 Fe1 N1 . . 87.33(17) ?
O1 Fe1 N1 . . 84.7(2) ?
O2 Fe1 N3 . . 90.10(15) ?
O3 Fe1 N3 . . 95.00(15) ?
O1 Fe1 N3 . . 89.41(15) ?
N1 Fe1 N3 . . 173.7(2) ?
O2 Fe1 N4 . . 86.46(15) ?
O3 Fe1 N4 . . 178.34(14) ?
O1 Fe1 N4 . . 88.17(15) ?
N1 Fe1 N4 . . 94.28(18) ?
N3 Fe1 N4 . . 83.35(15) ?
N2 N1 C6 . . 110.8(5) ?
N2 N1 Fe1 . . 136.2(6) ?
C6 N1 Fe1 . . 113.1(4) ?
N1 N2 C12 . . 111.8(6) ?
C28 N3 C26 . . 121.5(4) ?
C28 N3 Fe1 . . 124.7(3) ?
C26 N3 Fe1 . . 113.6(3) ?
C19 N4 C27 . . 119.6(4) ?
C19 N4 Fe1 . . 128.0(3) ?
C27 N4 Fe1 . . 112.4(3) ?
C1 O1 Fe1 . . 113.3(3) ?
C7 O2 Fe1 . . 120.4(3) ?
C13 O3 Fe1 . . 125.8(3) ?
O4 C29 H29A . . 109.5 ?
O4 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
O4 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Feazpqsal_273K
_database_code_depnum_ccdc_archive 'CCDC 1535600'
_audit_update_record             
;
2017-03-22 deposited with the CCDC.
2017-03-31 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[Fe(azp)(qsal)2]0.5MeOH'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28.50 H21 Fe N4 O3.50'
_chemical_formula_iupac          ?
_chemical_formula_weight         531.34

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3517(12)
_cell_length_b                   11.4955(17)
_cell_length_c                   12.5888(18)
_cell_angle_alpha                99.329(2)
_cell_angle_beta                 100.429(2)
_cell_angle_gamma                95.311(2)
_cell_volume                     1163.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2591
_cell_measurement_theta_min      2.4995
_cell_measurement_theta_max      27.1049
_cell_measurement_temperature    273.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.99

_exptl_special_details           
;
;

_diffrn_ambient_temperature      273.(2)

_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            6671
_diffrn_reflns_av_R_equivalents  0.0130
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       16

_refine_special_details          
;
;

_reflns_number_total             4981
_reflns_number_gt                4040
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1435
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.049
_refine_ls_number_reflns         4981
_refine_ls_number_parameters     344
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0518P)²+1.9117P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.207
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 786)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.8957(4) 0.2304(3) 0.7646(3) 0.0466(8) Uani d . . . 1 A 4
C C2 1.0353(5) 0.1711(3) 0.7608(4) 0.0559(10) Uani d . . . 1 A 4
H H2 1.0839 0.1668 0.6997 0.067 Uiso calc U . R 1 A 4
C C3 1.0986(6) 0.1204(4) 0.8464(5) 0.0831(17) Uani d . . . 1 A 4
H H3 1.1908 0.0812 0.8437 0.1 Uiso calc U . R 1 A 4
C C4 1.0257(9) 0.1268(5) 0.9395(5) 0.109(3) Uani d . . . 1 A 4
H H4 1.07 0.093 0.9988 0.131 Uiso calc U . R 1 A 4
C C5 0.8867(8) 0.1842(5) 0.9415(4) 0.094(2) Uani d . . . 1 A 4
H H5 0.8374 0.1882 1.0024 0.113 Uiso calc U . R 1 A 4
C C6 0.8225(5) 0.2342(4) 0.8566(3) 0.0577(10) Uani d . . . 1 A 4
C C7 0.3915(4) 0.4204(3) 0.8155(3) 0.0396(7) Uani d . . . 1 B 4
C C8 0.2470(5) 0.4693(3) 0.8276(3) 0.0517(9) Uani d . . . 1 B 4
H H8 0.1967 0.5077 0.7734 0.062 Uiso calc U . R 1 B 4
C C9 0.1787(6) 0.4620(4) 0.9168(4) 0.0728(14) Uani d . . . 1 B 4
H H9 0.0824 0.4954 0.9215 0.087 Uiso calc U . R 1 B 4
C C10 0.2450(8) 0.4084(5) 0.9985(4) 0.0885(19) Uani d . . . 1 B 4
H H10 0.1966 0.4066 1.0592 0.106 Uiso calc U . R 1 B 4
C C11 0.3829(8) 0.3571(4) 0.9914(3) 0.0823(18) Uani d . . . 1 B 4
H H11 0.4292 0.3191 1.0471 0.099 Uiso calc U . R 1 B 4
C C12 0.4578(5) 0.3615(3) 0.8980(4) 0.0545(10) Uani d . . . 1 B 4
C C13 0.8582(4) 0.5879(3) 0.6742(3) 0.0406(7) Uani d . . . 1 C 4
C C14 0.9758(5) 0.6838(3) 0.7318(3) 0.0543(9) Uani d . . . 1 C 4
H H14 0.9971 0.699 0.8082 0.065 Uiso calc U . R 1 C 4
C C15 1.0589(5) 0.7546(3) 0.6775(4) 0.0590(10) Uani d . . . 1 C 4
H H15 1.1367 0.8166 0.7178 0.071 Uiso calc U . R 1 C 4
C C16 1.0301(5) 0.7363(3) 0.5631(3) 0.0546(10) Uani d . . . 1 C 4
H H16 1.0866 0.7858 0.527 0.065 Uiso calc U . R 1 C 4
C C17 0.9169(4) 0.6438(3) 0.5053(3) 0.0467(8) Uani d . . . 1 C 4
H H17 0.8967 0.6308 0.4289 0.056 Uiso calc U . R 1 C 4
C C18 0.8296(4) 0.5676(3) 0.5582(3) 0.0364(7) Uani d . . . 1 C 4
C C19 0.4127(5) 0.1315(3) 0.6389(3) 0.0499(9) Uani d . . . 1 D 4
H H19 0.4334 0.1382 0.7149 0.06 Uiso calc U . R 1 D 4
C C20 0.3075(5) 0.0335(3) 0.5753(3) 0.0571(10) Uani d . . . 1 D 4
H H20 0.2606 -0.0237 0.6088 0.068 Uiso calc U . R 1 D 4
C C21 0.2745(5) 0.0223(3) 0.4646(3) 0.0539(9) Uani d . . . 1 D 4
H H21 0.2045 -0.0425 0.4215 0.065 Uiso calc U . R 1 D 4
C C22 0.3471(4) 0.1099(3) 0.4149(3) 0.0439(8) Uani d . . . 1 D 4
C C23 0.3207(5) 0.1059(3) 0.3009(3) 0.0560(10) Uani d . . . 1 D 4
H H23 0.2518 0.0433 0.2534 0.067 Uiso calc U . R 1 D 4
C C24 0.3962(6) 0.1939(4) 0.2603(3) 0.0610(11) Uani d . . . 1 D 4
H H24 0.3787 0.1904 0.1847 0.073 Uiso calc U . R 1 D 4
C C25 0.5001(5) 0.2903(3) 0.3299(3) 0.0501(9) Uani d . . . 1 D 4
H H25 0.5494 0.3495 0.2997 0.06 Uiso calc U . R 1 D 4
C C26 0.5295(4) 0.2979(3) 0.4415(2) 0.0344(6) Uani d . . . 1 D 4
C C27 0.4525(4) 0.2059(3) 0.4851(3) 0.0357(7) Uani d . . . 1 D 4
C C28 0.7187(4) 0.4713(3) 0.4896(3) 0.0359(7) Uani d . . . 1 C 4
H H28 0.7088 0.4666 0.4142 0.043 Uiso calc U . R 1 C 4
O O4 0.414(3) 0.9089(17) 0.9436(16) 0.305(11) Uani d U P D 0.5 E -1
Fe Fe1 0.64829(6) 0.37048(4) 0.68766(4) 0.03527(15) Uani d . . . 1 . .
N N1 0.6653(5) 0.3060(3) 0.8398(2) 0.0591(9) Uani d . . . 1 . .
N N2 0.6021(8) 0.2989(4) 0.9108(3) 0.119(2) Uani d . . . 1 . .
N N3 0.6301(3) 0.3898(2) 0.5213(2) 0.0334(5) Uani d . . . 1 . .
N N4 0.4837(3) 0.2148(2) 0.5965(2) 0.0380(6) Uani d . . . 1 . .
O O1 0.8334(3) 0.2791(2) 0.6814(2) 0.0564(7) Uani d . . . 1 . .
O O2 0.4563(3) 0.4315(2) 0.7301(2) 0.0458(6) Uani d . . . 1 . .
O O3 0.7788(3) 0.5228(2) 0.72847(19) 0.0510(6) Uani d . . . 1 . .
C C29 0.511(4) 0.997(3) 1.0299(17) 0.155(9) Uani d U P D 0.5 E -1
H H29A 0.464 1.07 1.0326 0.233 Uiso calc U P R 0.5 E -1
H H29B 0.6205 1.0093 1.0164 0.233 Uiso calc U P R 0.5 E -1
H H29C 0.515 0.9704 1.0987 0.233 Uiso calc U P R 0.5 E -1


_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.314(5) ?
C1 C6 . 1.401(5) ?
C1 C2 . 1.408(5) ?
C2 C3 . 1.354(7) ?
C2 H2 . 0.93 ?
C3 C4 . 1.411(9) ?
C3 H3 . 0.93 ?
C4 C5 . 1.390(9) ?
C4 H4 . 0.93 ?
C5 C6 . 1.345(7) ?
C5 H5 . 0.93 ?
C6 N1 . 1.614(6) ?
C7 O2 . 1.307(4) ?
C7 C12 . 1.390(5) ?
C7 C8 . 1.400(5) ?
C8 C9 . 1.358(6) ?
C8 H8 . 0.93 ?
C9 C10 . 1.344(8) ?
C9 H9 . 0.93 ?
C10 C11 . 1.352(8) ?
C10 H10 . 0.93 ?
C11 C12 . 1.434(7) ?
C11 H11 . 0.93 ?
C12 N2 . 1.458(8) ?
C13 O3 . 1.306(4) ?
C13 C14 . 1.410(5) ?
C13 C18 . 1.412(5) ?
C14 C15 . 1.364(5) ?
C14 H14 . 0.93 ?
C15 C16 . 1.394(6) ?
C15 H15 . 0.93 ?
C16 C17 . 1.367(5) ?
C16 H16 . 0.93 ?
C17 C18 . 1.411(4) ?
C17 H17 . 0.93 ?
C18 C28 . 1.428(4) ?
C19 N4 . 1.315(4) ?
C19 C20 . 1.397(5) ?
C19 H19 . 0.93 ?
C20 C21 . 1.353(6) ?
C20 H20 . 0.93 ?
C21 C22 . 1.416(5) ?
C21 H21 . 0.93 ?
C22 C23 . 1.404(5) ?
C22 C27 . 1.413(4) ?
C23 C24 . 1.360(6) ?
C23 H23 . 0.93 ?
C24 C25 . 1.407(5) ?
C24 H24 . 0.93 ?
C25 C26 . 1.369(5) ?
C25 H25 . 0.93 ?
C26 N3 . 1.421(4) ?
C26 C27 . 1.422(4) ?
C27 N4 . 1.364(4) ?
C28 N3 . 1.297(4) ?
C28 H28 . 0.93 ?
O4 C29 . 1.4283(11) ?
Fe1 O3 . 1.916(2) ?
Fe1 O2 . 1.936(2) ?
Fe1 O1 . 1.954(3) ?
Fe1 N3 . 2.122(3) ?
Fe1 N1 . 2.149(3) ?
Fe1 N4 . 2.172(3) ?
N1 N2 . 1.127(5) ?
C29 H29A . 0.96 ?
C29 H29B . 0.96 ?
C29 H29C . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 C6 . . 120.8(4) ?
O1 C1 C2 . . 120.0(4) ?
C6 C1 C2 . . 119.2(4) ?
C3 C2 C1 . . 119.9(5) ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 120.4(5) ?
C2 C3 H3 . . 119.8 ?
C4 C3 H3 . . 119.8 ?
C5 C4 C3 . . 119.1(5) ?
C5 C4 H4 . . 120.4 ?
C3 C4 H4 . . 120.4 ?
C6 C5 C4 . . 120.9(6) ?
C6 C5 H5 . . 119.6 ?
C4 C5 H5 . . 119.6 ?
C5 C6 C1 . . 120.5(5) ?
C5 C6 N1 . . 130.3(5) ?
C1 C6 N1 . . 109.2(4) ?
O2 C7 C12 . . 123.8(3) ?
O2 C7 C8 . . 120.0(3) ?
C12 C7 C8 . . 116.3(3) ?
C9 C8 C7 . . 121.5(4) ?
C9 C8 H8 . . 119.2 ?
C7 C8 H8 . . 119.2 ?
C10 C9 C8 . . 122.5(5) ?
C10 C9 H9 . . 118.7 ?
C8 C9 H9 . . 118.7 ?
C9 C10 C11 . . 119.3(4) ?
C9 C10 H10 . . 120.3 ?
C11 C10 H10 . . 120.3 ?
C10 C11 C12 . . 119.9(5) ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
C7 C12 C11 . . 120.4(4) ?
C7 C12 N2 . . 131.0(4) ?
C11 C12 N2 . . 108.5(4) ?
O3 C13 C14 . . 119.7(3) ?
O3 C13 C18 . . 122.6(3) ?
C14 C13 C18 . . 117.7(3) ?
C15 C14 C13 . . 121.2(4) ?
C15 C14 H14 . . 119.4 ?
C13 C14 H14 . . 119.4 ?
C14 C15 C16 . . 121.6(4) ?
C14 C15 H15 . . 119.2 ?
C16 C15 H15 . . 119.2 ?
C17 C16 C15 . . 118.4(3) ?
C17 C16 H16 . . 120.8 ?
C15 C16 H16 . . 120.8 ?
C16 C17 C18 . . 121.8(3) ?
C16 C17 H17 . . 119.1 ?
C18 C17 H17 . . 119.1 ?
C17 C18 C13 . . 119.3(3) ?
C17 C18 C28 . . 117.0(3) ?
C13 C18 C28 . . 123.7(3) ?
N4 C19 C20 . . 123.2(4) ?
N4 C19 H19 . . 118.4 ?
C20 C19 H19 . . 118.4 ?
C21 C20 C19 . . 119.5(3) ?
C21 C20 H20 . . 120.3 ?
C19 C20 H20 . . 120.3 ?
C20 C21 C22 . . 119.6(3) ?
C20 C21 H21 . . 120.2 ?
C22 C21 H21 . . 120.2 ?
C23 C22 C27 . . 119.0(3) ?
C23 C22 C21 . . 123.7(3) ?
C27 C22 C21 . . 117.3(3) ?
C24 C23 C22 . . 119.7(3) ?
C24 C23 H23 . . 120.2 ?
C22 C23 H23 . . 120.2 ?
C23 C24 C25 . . 121.7(4) ?
C23 C24 H24 . . 119.2 ?
C25 C24 H24 . . 119.2 ?
C26 C25 C24 . . 120.7(3) ?
C26 C25 H25 . . 119.7 ?
C24 C25 H25 . . 119.7 ?
C25 C26 N3 . . 126.8(3) ?
C25 C26 C27 . . 118.3(3) ?
N3 C26 C27 . . 114.9(3) ?
N4 C27 C22 . . 121.8(3) ?
N4 C27 C26 . . 117.5(3) ?
C22 C27 C26 . . 120.7(3) ?
N3 C28 C18 . . 126.9(3) ?
N3 C28 H28 . . 116.5 ?
C18 C28 H28 . . 116.5 ?
O3 Fe1 O2 . . 93.44(11) ?
O3 Fe1 O1 . . 95.47(12) ?
O2 Fe1 O1 . . 161.54(11) ?
O3 Fe1 N3 . . 87.83(10) ?
O2 Fe1 N3 . . 104.82(10) ?
O1 Fe1 N3 . . 91.66(11) ?
O3 Fe1 N1 . . 103.78(11) ?
O2 Fe1 N1 . . 82.49(13) ?
O1 Fe1 N1 . . 79.70(14) ?
N3 Fe1 N1 . . 166.05(11) ?
O3 Fe1 N4 . . 163.49(11) ?
O2 Fe1 N4 . . 86.67(10) ?
O1 Fe1 N4 . . 89.32(11) ?
N3 Fe1 N4 . . 76.22(10) ?
N1 Fe1 N4 . . 92.61(11) ?
N2 N1 C6 . . 107.1(5) ?
N2 N1 Fe1 . . 143.8(5) ?
C6 N1 Fe1 . . 108.9(2) ?
N1 N2 C12 . . 108.9(5) ?
C28 N3 C26 . . 119.5(3) ?
C28 N3 Fe1 . . 123.8(2) ?
C26 N3 Fe1 . . 116.18(19) ?
C19 N4 C27 . . 118.6(3) ?
C19 N4 Fe1 . . 126.1(2) ?
C27 N4 Fe1 . . 115.3(2) ?
C1 O1 Fe1 . . 121.1(2) ?
C7 O2 Fe1 . . 129.9(2) ?
C13 O3 Fe1 . . 132.9(2) ?
O4 C29 H29A . . 109.5 ?
O4 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
O4 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       ', Magnetic properties'
