# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1419531'
_audit_update_record             
;
2016-11-17 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Fe(N3)2(4-mpc)]n'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H7 Fe N7 O2'
_chemical_formula_weight         277.05

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.400(2)
_cell_length_b                   8.580(3)
_cell_length_c                   10.802(4)
_cell_angle_alpha                106.749(5)
_cell_angle_beta                 104.441(4)
_cell_angle_gamma                96.194(5)
_cell_volume                     539.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3206
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      27.27

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_F_000             280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.400
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7405
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.060
_diffrn_reflns_theta_max         27.396
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2419
_reflns_number_gt                1932
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0905P)²+1.1828P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2419
_refine_ls_number_parameters     158
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1629
_refine_ls_wR_factor_gt          0.1550
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O -0.0295(5) 0.8795(4) 0.7929(3) 0.0403(8) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 1.0000 1.0000 0.0248(2) Uani 1 2 d S . P . .
Fe2 Fe 0.0000 1.0000 1.0000 0.0257(2) Uani 1 2 d S . P . .
N3 N 0.3104(6) 0.8705(5) 1.1835(4) 0.0378(9) Uani 1 1 d . . . . .
N4 N 0.2577(5) 0.8695(5) 1.0675(4) 0.0334(8) Uani 1 1 d . . . . .
N5 N 0.2816(5) 1.1820(4) 1.0131(4) 0.0309(8) Uani 1 1 d . . . . .
N6 N 0.3413(6) 1.3111(5) 1.1020(4) 0.0422(10) Uani 1 1 d . . . . .
N7 N 0.3997(9) 1.4382(6) 1.1862(7) 0.081(2) Uani 1 1 d . . . . .
N2 N 0.3603(9) 0.8703(7) 1.2930(5) 0.0609(13) Uani 1 1 d . . . . .
O1 O 0.3230(5) 0.8733(4) 0.8000(3) 0.0405(8) Uani 1 1 d . . . . .
C2 C 0.0578(6) 0.7751(5) 0.5887(4) 0.0286(8) Uani 1 1 d . . . . .
C1 C 0.1224(6) 0.8501(5) 0.7411(4) 0.0292(8) Uani 1 1 d . . . . .
C3 C 0.1974(7) 0.6881(6) 0.5283(4) 0.0362(10) Uani 1 1 d . . . . .
H3 H 0.3311 0.6786 0.5814 0.043 Uiso 1 1 calc R U . . .
C7 C -0.1377(7) 0.7908(6) 0.5063(4) 0.0378(10) Uani 1 1 d . . . . .
H7 H -0.2338 0.8486 0.5441 0.045 Uiso 1 1 calc R U . . .
C6 C -0.1885(7) 0.7201(6) 0.3680(5) 0.0408(10) Uani 1 1 d . . . . .
H6 H -0.3173 0.7330 0.3123 0.049 Uiso 1 1 calc R U . . .
C4 C 0.1381(7) 0.6166(6) 0.3911(4) 0.0389(10) Uani 1 1 d . . . . .
H4 H 0.2302 0.5564 0.3511 0.047 Uiso 1 1 calc R U . . .
C5 C -0.1117(9) 0.5560(7) 0.1647(5) 0.0528(14) Uani 1 1 d . . . . .
H5A H -0.1542 0.4379 0.1408 0.079 Uiso 1 1 calc R U . . .
H5B H 0.0129 0.5811 0.1346 0.079 Uiso 1 1 calc R U . . .
H5C H -0.2319 0.5991 0.1224 0.079 Uiso 1 1 calc R U . . .
N1 N -0.0530(6) 0.6328(5) 0.3132(3) 0.0355(8) Uani 1 1 d . . . . .


_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C1 1.251(5) . ?
O2 Fe2 2.127(3) . ?
Fe1 O1 2.071(3) 2_677 ?
Fe1 O1 2.071(3) . ?
Fe1 N4 2.202(4) 2_677 ?
Fe1 N4 2.202(4) . ?
Fe1 N5 2.203(3) . ?
Fe1 N5 2.203(3) 2_677 ?
Fe2 O2 2.127(3) 2_577 ?
Fe2 N4 2.185(4) 2_577 ?
Fe2 N4 2.185(4) . ?
Fe2 N5 2.201(3) 2_577 ?
Fe2 N5 2.201(3) . ?
N3 N2 1.146(6) . ?
N3 N4 1.210(5) . ?
N5 N6 1.187(5) . ?
N6 N7 1.152(6) . ?
O1 C1 1.247(5) . ?
C2 C7 1.388(6) . ?
C2 C3 1.391(6) . ?
C2 C1 1.512(5) . ?
C3 C4 1.365(6) . ?
C7 C6 1.377(6) . ?
C6 N1 1.343(6) . ?
C4 N1 1.346(6) . ?
C5 N1 1.478(6) . ?

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
C1 O2 Fe2 127.5(3) . . ?
O1 Fe1 O1 180.0 2_677 . ?
O1 Fe1 N4 90.22(14) 2_677 2_677 ?
O1 Fe1 N4 89.78(14) . 2_677 ?
O1 Fe1 N4 89.78(14) 2_677 . ?
O1 Fe1 N4 90.22(14) . . ?
N4 Fe1 N4 180.00(18) 2_677 . ?
O1 Fe1 N5 88.89(13) 2_677 . ?
O1 Fe1 N5 91.11(13) . . ?
N4 Fe1 N5 97.59(14) 2_677 . ?
N4 Fe1 N5 82.41(14) . . ?
O1 Fe1 N5 91.11(13) 2_677 2_677 ?
O1 Fe1 N5 88.89(13) . 2_677 ?
N4 Fe1 N5 82.41(14) 2_677 2_677 ?
N4 Fe1 N5 97.59(14) . 2_677 ?
N5 Fe1 N5 180.0 . 2_677 ?
O2 Fe2 O2 180.00(8) 2_577 . ?
O2 Fe2 N4 92.14(13) 2_577 2_577 ?
O2 Fe2 N4 87.86(13) . 2_577 ?
O2 Fe2 N4 87.86(13) 2_577 . ?
O2 Fe2 N4 92.14(13) . . ?
N4 Fe2 N4 180.0 2_577 . ?
O2 Fe2 N5 89.74(13) 2_577 2_577 ?
O2 Fe2 N5 90.26(13) . 2_577 ?
N4 Fe2 N5 82.85(14) 2_577 2_577 ?
N4 Fe2 N5 97.14(14) . 2_577 ?
O2 Fe2 N5 90.26(13) 2_577 . ?
O2 Fe2 N5 89.74(13) . . ?
N4 Fe2 N5 97.15(14) 2_577 . ?
N4 Fe2 N5 82.86(14) . . ?
N5 Fe2 N5 180.0 2_577 . ?
N2 N3 N4 179.6(5) . . ?
N3 N4 Fe2 120.1(3) . . ?
N3 N4 Fe1 117.9(3) . . ?
Fe2 N4 Fe1 93.66(15) . . ?
N6 N5 Fe2 121.2(3) . . ?
N6 N5 Fe1 119.3(3) . . ?
Fe2 N5 Fe1 93.20(14) . . ?
N7 N6 N5 178.5(6) . . ?
C1 O1 Fe1 130.4(3) . . ?
C7 C2 C3 118.5(4) . . ?
C7 C2 C1 121.9(4) . . ?
C3 C2 C1 119.6(4) . . ?
O1 C1 O2 127.9(4) . . ?
O1 C1 C2 115.2(3) . . ?
O2 C1 C2 116.9(3) . . ?
C4 C3 C2 120.0(4) . . ?
C6 C7 C2 119.5(4) . . ?
N1 C6 C7 120.4(4) . . ?
N1 C4 C3 120.4(4) . . ?
C6 N1 C4 121.1(4) . . ?
C6 N1 C5 119.6(4) . . ?
C4 N1 C5 119.3(4) . . ?

_refine_diff_density_max         1.833
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.119


_vrf_PLAT094_b                   
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 4.54 Report
RESPONSE: the largest Q peak (1.83) which lies beside the metal center 
is a ghost peak.
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
