# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_FeSe-en
_database_code_depnum_ccdc_archive 'CCDC 1553156'
_audit_update_record             
;
2017-08-01 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
_chemical_name_systematic        Fe0.85Se(C2H8N2)0.3
_chemical_formula_structural     Fe0.85Se(C2H8N2)0.3
_chemical_formula_sum            'Fe0.85 Se C0.6 H2.4 N0.6'
_cell_length_a                   3.9037(5)
_cell_length_b                   21.528(2)
_cell_length_c                   3.8585(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.34(2)
_cell_angle_gamma                90
_cell_volume                     324.17(8)
_cell_formula_units_Z            4
_chemical_formula_weight         144.46
_shelx_F_squared_multiplier      1
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C12/c1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, y, -z+1/2 '
'x, -y, z+1/2 '
'-x, -y, -z '
'x+1/2, y+1/2, z '
'-x+1/2, y+1/2, -z+1/2 '
'x+1/2, -y+1/2, z+1/2 '
'-x+1/2, -y+1/2, -z '

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'Ge111 monochromator'
_diffrn_measurement_device_type  'STOE STADI P'
_cell_measurement_temperature    293
_diffrn_ambient_temperature      293
_pd_proc_ls_prof_R_factor        3.239
_pd_proc_ls_prof_wR_factor       4.294
_pd_proc_ls_prof_wR_expected     3.890
_refine_ls_goodness_of_fit_all   1.104

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Se1 Se 4 0 0.1832(3) 0.25 1 0.96(19)
Fe1 Fe 4 0 0.2499(6) 0.75 0.85 0.96(19)
C1 C 8 0.19533 0.0035 0.0236 0.3333333 3
N1 N 8 0.3404 0.02628 0.69974 0.3333333 3
H1 H 8 0.25169 0.03627 0.23167 0.3333333 5
H2 H 8 0.30791 0.95879 0.0891 0.3333333 5
H5 H 8 0.47118 0.06683 0.76133 0.3333333 5
H6 H 8 0.52387 0.99422 0.62774 0.3333333 5




loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 Fe1 2.405
Se1 Fe1 2.426
Fe1 Fe1 2.712
Fe1 Fe1 2.776


loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Fe1 Se1 Fe1 107.2
Fe1 Se1 Fe1 68.3
Fe1 Se1 Fe1 68.3
Fe1 Se1 Fe1 70.2
Fe1 Se1 Fe1 106.7
Fe1 Se1 Fe1 70.2
Se1 Fe1 Fe1 56.2
Se1 Fe1 Fe1 124.9
Se1 Fe1 Se1 111.69
Se1 Fe1 Fe1 55.3
Se1 Fe1 Se1 111.69
Se1 Fe1 Se1 109.84
Se1 Fe1 Fe1 55.3
Se1 Fe1 Fe1 123.9
Se1 Fe1 Se1 109.84
Se1 Fe1 Fe1 123.9
Se1 Fe1 Fe1 125.3
Se1 Fe1 Fe1 124.4
Fe1 Fe1 Fe1 89.33
Se1 Fe1 Fe1 124.4
Fe1 Fe1 Fe1 90.67
Fe1 Fe1 Fe1 179.8
Se1 Fe1 Fe1 125.3
Fe1 Fe1 Fe1 179.8
Fe1 Fe1 Fe1 90.67
Se1 Fe1 Fe1 54.6
Se1 Fe1 Fe1 124.9
Se1 Fe1 Fe1 56.2
Se1 Fe1 Fe1 55.5
Se1 Fe1 Fe1 54.6
Se1 Fe1 Se1 107.2
Se1 Fe1 Se1 106.7
Se1 Fe1 Fe1 55.5
Fe1 Fe1 Fe1 89.33
N1 N1 C1 132.21
N1 N1 C1 97.62
C1 N1 C1 97.46
C1 N1 H2 76.00
H1 N1 H2 126.00
C1 N1 H5 106.00
H5 N1 H6 99.00
N1 N1 H5 58.00
H2 N1 H5 78.00
C1 N1 H1 50.00
H1 N1 H5 156.00
H2 N1 H5 78.00
C1 N1 H6 107.00
H6 N1 H6 54.00
N1 N1 H6 54.00
H5 N1 H6 96.00
C1 N1 H6 78.00
H1 N1 H6 64.00
H2 N1 H6 109.00
C1 N1 H6 57.00
C1 N1 H5 114.00
C1 N1 H1 60.00
C1 N1 H2 141.00
H5 N1 H5 11.00
C1 N1 H5 153.00
H1 N1 H6 57.00
H2 N1 H6 162.00
N1 N1 H5 50.00
N1 N1 H1 102.00
N1 N1 H2 116.00
C1 N1 H5 149.00
H1 N1 H5 152.00
N1 N1 H6 51.00
H5 N1 H6 96.00
C1 N1 H6 104.00
H5 N1 H6 106.00
N1 C1 C1 109.44
N1 C1 N1 121.65
N1 C1 C1 121.19
H1 C1 H2 109.00
N1 C1 H1 110.00
H1 C1 H6 106.00
N1 C1 H2 109.00
H2 C1 H6 68.00
C1 C1 H2 110.00
N1 C1 H2 29.00
H2 C1 H6 65.00
N1 C1 H6 46.00
N1 C1 H6 82.00
C1 C1 H6 143.00
N1 C1 H6 76.00
H6 C1 H6 46.00
C1 C1 H6 169.00
N1 C1 H6 49.00
C1 C1 H1 109.00
N1 C1 H1 80.00
H1 C1 H6 65.00
####################################################################### 
# 
# 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_Fe3Se4en3
_database_code_depnum_ccdc_archive 'CCDC 1813199'

_audit_update_record             
;
2017-12-22 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_formula_sum            'C6 H24 Fe3 N6 Se4'
_chemical_formula_weight         663.7

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   9.104(4)
_cell_length_b                   10.398(4)
_cell_length_c                   11.675(5)
_cell_angle_alpha                109.880(13)
_cell_angle_beta                 96.370(15)
_cell_angle_gamma                114.093(14)
_cell_volume                     907.8(7)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    409
_cell_measurement_theta_min      4.740
_cell_measurement_theta_max      35.508
_cell_measurement_temperature    293

_exptl_crystal_density_diffrn    2.428
_exptl_crystal_F_000             632

_exptl_absorpt_coefficient_mu    10.379
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8176

#=======================================================================

# 7. EXPERIMENTAL DATA

_diffrn_ambient_temperature      293
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CCD'

_diffrn_reflns_number            37683
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_full        28.51
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_diffrn_radiation_probe          x-ray

#=======================================================================

# 8. REFINEMENT DATA

_reflns_number_total             3280
_reflns_number_gt                2424
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_gt          0.0655
_refine_ls_R_factor_all          0.0651
_refine_ls_wR_factor_ref         0.0724
_refine_ls_goodness_of_fit_ref   1.56
_refine_ls_goodness_of_fit_gt    1.66
_refine_ls_number_reflns         3280
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_number_constraints    102
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0499
_refine_ls_shift/su_mean         0.0013
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     none

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Se -0.0929 2.2259 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.13526(8) 0.74158(7) 0.33777(6) Uani 0.0249(3) 2 1 d . . .
Se2 Se 0.76829(8) 0.35087(7) 0.18216(6) Uani 0.0284(3) 2 1 d . . .
Se3 Se 0.87130(8) 0.59483(7) 0.98113(6) Uani 0.0257(3) 2 1 d . . .
Se4 Se 0.85343(8) 0.57306(8) 0.54767(6) Uani 0.0282(3) 2 1 d . . .
Fe1 Fe 0.98106(10) 0.52543(9) 0.12988(8) Uani 0.0198(4) 2 1 d . . .
Fe2 Fe 0.97611(11) 0.52367(9) 0.38322(8) Uani 0.0209(4) 2 1 d . . .
Fe3 Fe 0.66239(11) 0.88136(10) 0.24881(8) Uani 0.0267(4) 2 1 d . . .
N1 N 0.6610(3) 0.10858(14) 0.3256(3) Uani 0.030(3) 2 1 d . . .
N2 N 0.41219(18) 0.8168(2) 0.1413(3) Uani 0.033(3) 2 1 d . . .
N3 N 0.5870(5) 0.8456(2) 0.4131(2) Uani 0.030(3) 2 1 d . . .
N4 N 0.6037(6) 0.63463(13) 0.19656(14) Uani 0.049(4) 2 1 d . . .
N5 N 0.7703(4) 0.9194(2) 0.09406(15) Uani 0.040(3) 2 1 d . . .
N6 N 0.93694(14) 0.9979(4) 0.34486(15) Uani 0.038(3) 2 1 d . . .
C1 C 0.4897(9) 0.0816(5) 0.2853(6) Uani 0.038(4) 2 1 d . . .
C2 C 0.4062(5) 0.9597(7) 0.1500(6) Uani 0.035(4) 2 1 d . . .
C3 C 0.6015(8) 0.7120(8) 0.4181(6) Uani 0.043(4) 2 1 d . . .
C4 C 0.5258(9) 0.5829(5) 0.2884(6) Uani 0.043(4) 2 1 d . . .
C5 C 0.9439(9) 0.0506(8) 0.1552(5) Uani 0.044(4) 2 1 d . . .
C6 C 0.0332(5) 0.0185(8) 0.2511(6) Uani 0.043(4) 2 1 d . . .
H1n1 H 0.711662 0.176956 0.423205 Uiso 0.0363 2 1 d . . .
H2n1 H 0.733733 0.165473 0.278053 Uiso 0.0363 2 1 d . . .
H1n2 H 0.367751 0.736909 0.046421 Uiso 0.04 2 1 d . . .
H2n2 H 0.337443 0.768982 0.192376 Uiso 0.04 2 1 d . . .
H1n3 H 0.655531 0.941941 0.500158 Uiso 0.036 2 1 d . . .
H2n3 H 0.461276 0.819483 0.394196 Uiso 0.036 2 1 d . . .
H1n4 H 0.512961 0.580973 0.109347 Uiso 0.0593 2 1 d . . .
H2n4 H 0.698706 0.604534 0.185081 Uiso 0.0593 2 1 d . . .
H1n5 H 0.69875 0.948888 0.042567 Uiso 0.0476 2 1 d . . .
H2n5 H 0.773238 0.82126 0.033008 Uiso 0.0476 2 1 d . . .
H1n6 H 0.965726 0.933208 0.385647 Uiso 0.0453 2 1 d . . .
H2n6 H 0.96936 0.106329 0.415612 Uiso 0.0453 2 1 d . . .
H1c1 H 0.492512 0.189555 0.291245 Uiso 0.0451 2 1 d . . .
H2c1 H 0.419493 0.041444 0.346932 Uiso 0.0451 2 1 d . . .
H1c2 H 0.275584 0.933932 0.121519 Uiso 0.0416 2 1 d . . .
H2c2 H 0.472478 0.00239 0.08776 Uiso 0.0416 2 1 d . . .
H1c3 H 0.534642 0.674665 0.482229 Uiso 0.0515 2 1 d . . .
H2c3 H 0.73376 0.745087 0.451608 Uiso 0.0515 2 1 d . . .
H1c4 H 0.544052 0.486078 0.289816 Uiso 0.0512 2 1 d . . .
H2c4 H 0.391059 0.542488 0.258467 Uiso 0.0512 2 1 d . . .
H1c5 H 0.939579 0.158306 0.20412 Uiso 0.053 2 1 d . . .
H2c5 H 0.009513 0.058085 0.083134 Uiso 0.053 2 1 d . . .
H1c6 H 0.041162 0.912857 0.201805 Uiso 0.0522 2 1 d . . .
H2c6 H 0.159459 0.116181 0.30098 Uiso 0.0522 2 1 d . . .


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Se1 Fe1 . 1_455 2.423(3) ?
Se1 Fe2 . 1_455 2.413(2) ?
Se2 Fe1 . . 2.359(2) ?
Se2 Fe2 . . 2.385(3) ?
Se3 Fe1 . 1_556 2.3645(18) ?
Se3 Fe1 . 2_766 2.3889(17) ?
Se4 Fe2 . . 2.3391(19) ?
Se4 Fe2 . 2_766 2.3705(18) ?
Fe3 N2 . . 2.182(3) ?
N1 C1 . . 1.457(8) ?
N2 C2 . . 1.478(9) ?
N3 C3 . . 1.467(10) ?
N4 C4 . . 1.481(8) ?
N5 C5 . 1_565 1.482(7) ?
N6 C6 . 1_665 1.494(7) ?
C1 C2 . 1_545 1.505(8) ?
C1 H1c1 . . 1.09 ?
C1 H2c1 . . 1.09 ?
C2 H1c2 . . 1.09 ?
C2 H2c2 . 1_565 1.09 ?
C3 C4 . . 1.483(8) ?
C3 H1c3 . . 1.09 ?
C3 H2c3 . . 1.09 ?
C4 H1c4 . . 1.09 ?
C4 H2c4 . . 1.09 ?
C5 C6 . 1_655 1.517(12) ?
C5 H1c5 . . 1.09 ?
C5 H2c5 . 1_655 1.09 ?
C6 H1c6 . 1_545 1.09 ?
C6 H2c6 . . 1.09 ?

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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Fe1 Se1 Fe2 1_455 . 1_455 75.76(6) ?
Fe1 Se2 Fe2 . . . 77.49(5) ?
Fe1 Se3 Fe1 1_556 . 2_766 77.67(5) ?
Fe2 Se4 Fe2 . . 2_766 77.51(5) ?
Se1 Fe1 Se2 1_655 . . 100.50(6) ?
Se1 Fe1 Se3 1_655 . 1_554 112.82(6) ?
Se1 Fe1 Se3 1_655 . 2_766 118.06(6) ?
Se2 Fe1 Se3 . . 1_554 112.46(5) ?
Se2 Fe1 Se3 . . 2_766 111.09(6) ?
Se3 Fe1 Se3 1_554 . 2_766 102.33(5) ?
Se1 Fe2 Se2 1_655 . . 100.04(6) ?
Se1 Fe2 Se4 1_655 . . 116.35(5) ?
Se1 Fe2 Se4 1_655 . 2_766 111.97(5) ?
Se2 Fe2 Se4 . . . 111.49(6) ?
Se2 Fe2 Se4 . . 2_766 115.10(6) ?
Se4 Fe2 Se4 . . 2_766 102.49(5) ?
Fe3 N2 C2 . . . 108.85(17) ?
N1 C1 C2 . . 1_545 109.2(5) ?
N1 C1 H1c1 . . . 109.47 ?
N1 C1 H2c1 . . . 109.47 ?
C2 C1 H1c1 1_545 . . 109.47 ?
C2 C1 H2c1 1_545 . . 109.47 ?
H1c1 C1 H2c1 . . . 109.7 ?
N2 C2 C1 . . 1_565 109.1(6) ?
N2 C2 H1c2 . . . 109.47 ?
N2 C2 H2c2 . . 1_565 109.47 ?
C1 C2 H1c2 1_565 . . 109.47 ?
C1 C2 H2c2 1_565 . 1_565 109.47 ?
H1c2 C2 H2c2 . . 1_565 109.8 ?
N3 C3 C4 . . . 108.9(6) ?
N3 C3 H1c3 . . . 109.47 ?
N3 C3 H2c3 . . . 109.47 ?
C4 C3 H1c3 . . . 109.47 ?
C4 C3 H2c3 . . . 109.47 ?
H1c3 C3 H2c3 . . . 109.99 ?
N4 C4 C3 . . . 110.7(4) ?
N4 C4 H1c4 . . . 109.47 ?
N4 C4 H2c4 . . . 109.47 ?
C3 C4 H1c4 . . . 109.47 ?
C3 C4 H2c4 . . . 109.47 ?
H1c4 C4 H2c4 . . . 108.19 ?
N5 C5 C6 1_545 . 1_655 107.9(6) ?
N5 C5 H1c5 1_545 . . 109.47 ?
N5 C5 H2c5 1_545 . 1_655 109.47 ?
C6 C5 H1c5 1_655 . . 109.47 ?
C6 C5 H2c5 1_655 . 1_655 109.47 ?
H1c5 C5 H2c5 . . 1_655 110.98 ?
N6 C6 C5 1_445 . 1_455 109.4(5) ?
N6 C6 H1c6 1_445 . 1_545 109.47 ?
N6 C6 H2c6 1_445 . . 109.47 ?
C5 C6 H1c6 1_455 . 1_545 109.47 ?
C5 C6 H2c6 1_455 . . 109.47 ?
H1c6 C6 H2c6 1_545 . . 109.51 ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1n1 Se1 . . 2_666 1.04 2.65 3.630(5) 157.22 ?
N1 H2n1 Se2 . . . 1.04 2.47 3.366(4) 143.34 ?
N2 H1n2 Se2 . . 2_665 1.04 2.49 3.436(5) 151.68 ?
N2 H2n2 Se1 . . . 1.04 2.64 3.623(4) 158.41 ?
N3 H1n3 Se1 . . 2_676 1.04 2.81 3.780(5) 155.73 ?
N3 H2n3 Se1 . . . 1.04 2.67 3.712(6) 177.71 ?
N4 H2n4 Se2 . . . 1.04 2.94 3.782(5) 138.09 ?
N4 H2n4 Se3 . . 1_554 1.04 2.99 3.729(5) 128.58 ?
N5 H2n5 Se3 . . 1_554 1.04 2.75 3.708(4) 152.85 ?
N6 H1n6 Se1 . . 1_655 1.04 2.93 3.766(5) 137.35 ?
N6 H2n6 Se4 1_545 . 2_766 1.04 2.90 3.719(6) 136.45 ?
C3 H2c3 Se4 . . . 1.09 2.89 3.614(9) 124.31 ?
C4 H2c4 Se3 . . 2_666 1.09 2.93 3.802(8) 137.13 ?
C5 H1c5 Se4 . . 2_766 1.09 2.96 3.769(7) 131.61 ?



































# publcif Fe3Se4en3 _publcif_info_exptl_table_extra_item loop start
loop_
_publcif_info_exptl_table_extra_item
?

# publcif Fe3Se4en3 _publcif_info_exptl_table_extra_item loop end

# publcif Fe3Se4en3 _publcif_info_exptl_table_header_item loop start
loop_
_publcif_info_exptl_table_header_item
?
####################################################################### 
# 
# 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_Fe10Se12en7
_database_code_depnum_ccdc_archive 'CCDC 1813200'

_audit_update_record             
;
2017-12-22 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_formula_sum            'C14 H56 Fe10 N14 Se12'
_chemical_formula_weight         1926.7

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2

_cell_length_a                   9.323(2)
_cell_length_b                   12.273(2)
_cell_length_c                   20.821(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2382.4(8)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    2137
_cell_measurement_theta_min      4.787
_cell_measurement_theta_max      53.211
_cell_measurement_temperature    120

_exptl_crystal_density_diffrn    2.6858
_exptl_crystal_F_000             1812

_exptl_absorpt_coefficient_mu    12.146
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6955

#=======================================================================

# 7. EXPERIMENTAL DATA

_diffrn_ambient_temperature      120
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CCD'

_diffrn_reflns_number            42237
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_full        28.64
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27

_diffrn_radiation_probe          x-ray

#=======================================================================

# 8. REFINEMENT DATA

_reflns_number_total             4294
_reflns_number_gt                3334
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_gt          0.0663
_refine_ls_R_factor_all          0.0518
_refine_ls_wR_factor_ref         0.0708
_refine_ls_goodness_of_fit_ref   1.69
_refine_ls_goodness_of_fit_gt    1.81
_refine_ls_number_reflns         4294
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_number_constraints    119
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0495
_refine_ls_shift/su_mean         0.0015
_refine_diff_density_max         0.98
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     none

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Se -0.0929 2.2259 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.77140(6) 0.93036(5) 0.12391(3) Uani 0.02419(19) 4 1 d . . .
Se2 Se 0.85492(6) 0.40006(5) 0.03729(3) Uani 0.02412(19) 4 1 d . . .
Se3 Se 0.11796(6) 0.88151(4) 0.03094(3) Uani 0.01944(18) 4 1 d . . .
Se4 Se 0.76490(6) 0.69621(5) 0.99923(3) Uani 0.02219(18) 4 1 d . . .
Se5 Se 0.99674(7) 0.64847(5) 0.14486(3) Uani 0.0288(2) 4 1 d . . .
Se6 Se 0.93985(7) 0.85096(5) 0.86411(3) Uani 0.0260(2) 4 1 d . . .
Fe1 Fe 0.90711(9) 0.79092(6) 0.07937(4) Uani 0.0198(3) 4 1 d . . .
Fe2 Fe 0.94844(9) 0.58040(6) 0.04005(4) Uani 0.0199(3) 4 1 d . . .
Fe3 Fe 0.95131(9) 0.02130(6) 0.06705(4) Uani 0.0197(3) 4 1 d . . .
Fe4 Fe 0.99098(9) 0.75666(6) 0.95840(4) Uani 0.0193(3) 4 1 d . . .
Fe5 Fe 0.45243(9) 0.42641(7) 0.18158(4) Uani 0.0261(3) 4 1 d . . .
N1 N 0.4521(6) 0.60599(9) 0.19970(17) Uani 0.043(2) 4 1 d . . .
N2 N 0.4758(3) 0.4916(2) 0.08256(9) Uani 0.0344(19) 4 1 d . . .
N3 N 0.3853(2) 0.3987(3) 0.28151(6) Uani 0.0311(18) 4 1 d . . .
N4 N 0.21578(13) 0.4177(3) 0.16990(10) Uani 0.0306(18) 4 1 d . . .
N5 N 0.4870(3) 0.24995(11) 0.1676(2) Uani 0.051(2) 4 1 d . . .
N6 N 0.68602(15) 0.4163(2) 0.20335(19) Uani 0.041(2) 4 1 d . . .
N7 N 0.4303(6) 0.06143(16) 0.0768(2) Uani 0.069(3) 4 1 d . . .
C1 C 0.5133(7) 0.6590(5) 0.1416(3) Uani 0.043(3) 4 1 d . . .
C2 C 0.4422(6) 0.6097(5) 0.08454(19) Uani 0.039(2) 4 1 d . . .
C3 C 0.2348(8) 0.3792(9) 0.2812(2) Uani 0.150(7) 4 1 d . . .
C4 C 0.1513(4) 0.4124(6) 0.2330(3) Uani 0.061(3) 4 1 d . . .
C5 C 0.6462(7) 0.2344(4) 0.1631(3) Uani 0.045(3) 4 1 d . . .
C6 C 0.7244(5) 0.3022(6) 0.2091(3) Uani 0.050(3) 4 1 d . . .
C7 C 0.4977(7) 0.0560(5) 0.0156(3) Uani 0.049(3) 4 1 d . . .
H1n1 H 0.510766 0.629146 0.23993 Uiso 0.0512 4 1 d . . .
H2n1 H 0.345824 0.629951 0.205316 Uiso 0.0512 4 1 d . . .
H1n2 H 0.415562 0.454569 0.046631 Uiso 0.0413 4 1 d . . .
H2n2 H 0.58438 0.481009 0.073014 Uiso 0.0413 4 1 d . . .
H1n3 H 0.436756 0.33644 0.306372 Uiso 0.0374 4 1 d . . .
H2n3 H 0.406264 0.472794 0.30385 Uiso 0.0374 4 1 d . . .
H1n4 H 0.172051 0.482695 0.144506 Uiso 0.0368 4 1 d . . .
H2n4 H 0.195726 0.345503 0.14536 Uiso 0.0368 4 1 d . . .
H1n5 H 0.440502 0.235022 0.123091 Uiso 0.0612 4 1 d . . .
H2n5 H 0.445073 0.196092 0.201339 Uiso 0.0612 4 1 d . . .
H1n6 H 0.702192 0.455067 0.247175 Uiso 0.049 4 1 d . . .
H2n6 H 0.74966 0.452857 0.168435 Uiso 0.049 4 1 d . . .
H1n7 H 0.503517 0.089391 0.110717 Uiso 0.0833 4 1 d . . .
H2n7 H 0.343562 0.114577 0.074623 Uiso 0.0833 4 1 d . . .
H1c1 H 0.628282 0.643295 0.139485 Uiso 0.0519 4 1 d . . .
H2c1 H 0.490702 0.746111 0.143017 Uiso 0.0519 4 1 d . . .
H1c2 H 0.326484 0.620857 0.088239 Uiso 0.0472 4 1 d . . .
H2c2 H 0.482091 0.648682 0.041016 Uiso 0.0472 4 1 d . . .
H1c3 H 0.21437 0.293373 0.290961 Uiso 0.1795 4 1 d . . .
H2c3 H 0.188844 0.405985 0.326726 Uiso 0.1795 4 1 d . . .
H1c4 H 0.104481 0.491252 0.244894 Uiso 0.0737 4 1 d . . .
H2c4 H 0.055269 0.361928 0.231049 Uiso 0.0737 4 1 d . . .
H1c5 H 0.672258 0.148938 0.171287 Uiso 0.0546 4 1 d . . .
H2c5 H 0.681859 0.253446 0.114514 Uiso 0.0546 4 1 d . . .
H1c6 H 0.701903 0.274205 0.257757 Uiso 0.06 4 1 d . . .
H2c6 H 0.839392 0.292721 0.201409 Uiso 0.06 4 1 d . . .
H1c7 H 0.606155 0.088585 0.019117 Uiso 0.0585 4 1 d . . .
H2c7 H 0.44655 0.113715 0.983101 Uiso 0.0585 4 1 d . . .


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Se1 Fe1 . . 2.3214(11) ?
Se1 Fe3 . 1_565 2.3368(11) ?
Se2 Fe2 . . 2.3796(13) ?
Se2 Fe2 . 3_765 2.4519(12) ?
Se2 Fe4 . 3_766 2.4025(12) ?
Se3 Fe1 . 1_455 2.4734(12) ?
Se3 Fe3 . 1_465 2.4337(11) ?
Se3 Fe3 . 3_665 2.4500(11) ?
Se3 Fe4 . 1_454 2.4558(11) ?
Se4 Fe1 . 1_556 2.4276(11) ?
Se4 Fe2 . 1_556 2.3814(12) ?
Se4 Fe4 . . 2.3908(13) ?
Se5 Fe1 . . 2.3694(11) ?
Se5 Fe2 . . 2.3797(12) ?
Se6 Fe3 . 3_766 2.3542(11) ?
Se6 Fe4 . . 2.3282(11) ?
Fe1 Fe2 . . 2.7378(15) ?
Fe1 Fe4 . 1_554 2.6707(14) ?
Fe2 Fe2 . 3_765 2.7569(13) ?
Fe5 N3 . . 2.1991(18) ?
N1 C1 . . 1.487(7) ?
N2 C2 . . 1.484(7) ?
N3 C3 . . 1.424(8) ?
N4 C4 . . 1.446(6) ?
N5 C5 . . 1.500(7) ?
N6 C6 . . 1.451(7) ?
N7 C7 . . 1.422(8) ?
C1 C2 . . 1.489(8) ?
C1 H1c1 . . 1.09 ?
C1 H2c1 . . 1.09 ?
C2 H1c2 . . 1.09 ?
C2 H2c2 . . 1.09 ?
C3 C4 . . 1.334(9) ?
C3 H1c3 . . 1.09 ?
C3 H2c3 . . 1.09 ?
C4 H1c4 . . 1.09 ?
C4 H2c4 . . 1.09 ?
C5 C6 . . 1.464(8) ?
C5 H1c5 . . 1.09 ?
C5 H2c5 . . 1.09 ?
C6 H1c6 . . 1.09 ?
C6 H2c6 . . 1.09 ?
C7 C7 . 3_655 1.522(9) ?
C7 H1c7 . . 1.09 ?
C7 H2c7 . 1_554 1.09 ?

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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Fe1 Se1 Fe3 . . 1_565 76.03(3) ?
Fe2 Se2 Fe2 . . 3_765 69.57(3) ?
Fe2 Se2 Fe4 . . 3_766 121.64(4) ?
Fe2 Se2 Fe4 3_765 . 3_766 69.86(3) ?
Fe1 Se3 Fe3 1_455 . 1_465 71.55(3) ?
Fe1 Se3 Fe3 1_455 . 3_665 110.42(3) ?
Fe1 Se3 Fe4 1_455 . 1_454 65.61(3) ?
Fe3 Se3 Fe3 1_465 . 3_665 75.27(3) ?
Fe3 Se3 Fe4 1_465 . 1_454 108.79(4) ?
Fe3 Se3 Fe4 3_665 . 1_454 70.40(3) ?
Fe1 Se4 Fe2 1_556 . 1_556 69.39(3) ?
Fe1 Se4 Fe4 1_556 . . 67.32(3) ?
Fe2 Se4 Fe4 1_556 . . 71.26(3) ?
Fe1 Se5 Fe2 . . . 70.41(3) ?
Fe3 Se6 Fe4 3_766 . . 74.30(3) ?
Se1 Fe1 Se3 . . 1_655 105.35(4) ?
Se1 Fe1 Se4 . . 1_554 109.26(4) ?
Se1 Fe1 Se5 . . . 120.42(4) ?
Se1 Fe1 Fe2 . . . 153.11(4) ?
Se1 Fe1 Fe4 . . 1_554 130.72(4) ?
Se3 Fe1 Se4 1_655 . 1_554 111.66(4) ?
Se3 Fe1 Se5 1_655 . . 106.62(4) ?
Se3 Fe1 Fe2 1_655 . . 100.98(4) ?
Se3 Fe1 Fe4 1_655 . 1_554 56.88(3) ?
Se4 Fe1 Se5 1_554 . . 103.58(4) ?
Se4 Fe1 Fe2 1_554 . . 54.51(3) ?
Se4 Fe1 Fe4 1_554 . 1_554 55.68(3) ?
Se5 Fe1 Fe2 . . . 54.97(3) ?
Se5 Fe1 Fe4 . . 1_554 108.86(4) ?
Fe2 Fe1 Fe4 . . 1_554 61.84(3) ?
Se2 Fe2 Se2 . . 3_765 110.43(4) ?
Se2 Fe2 Se4 . . 1_554 106.46(4) ?
Se2 Fe2 Se5 . . . 114.71(4) ?
Se2 Fe2 Fe1 . . . 146.46(4) ?
Se2 Fe2 Fe2 . . 3_765 56.45(3) ?
Se2 Fe2 Se4 3_765 . 1_554 104.15(4) ?
Se2 Fe2 Se5 3_765 . . 115.24(4) ?
Se2 Fe2 Fe1 3_765 . . 102.08(3) ?
Se2 Fe2 Fe2 3_765 . 3_765 53.98(3) ?
Se4 Fe2 Se5 1_554 . . 104.69(4) ?
Se4 Fe2 Fe1 1_554 . . 56.10(3) ?
Se4 Fe2 Fe2 1_554 . 3_765 117.51(4) ?
Se5 Fe2 Fe1 . . . 54.62(3) ?
Se5 Fe2 Fe2 . . 3_765 137.74(4) ?
Fe1 Fe2 Fe2 . . 3_765 154.90(4) ?
Se1 Fe3 Se3 1_545 . 1_645 106.14(4) ?
Se1 Fe3 Se3 1_545 . 3_665 117.72(4) ?
Se1 Fe3 Se6 1_545 . 3_766 108.61(4) ?
Se3 Fe3 Se3 1_645 . 3_665 104.73(3) ?
Se3 Fe3 Se6 1_645 . 3_766 112.48(4) ?
Se3 Fe3 Se6 3_665 . 3_766 107.24(4) ?
Se2 Fe4 Se3 3_766 . 1_656 100.85(4) ?
Se2 Fe4 Se4 3_766 . . 105.40(4) ?
Se2 Fe4 Se6 3_766 . . 123.50(4) ?
Se2 Fe4 Fe1 3_766 . 1_556 105.42(3) ?
Se3 Fe4 Se4 1_656 . . 113.57(4) ?
Se3 Fe4 Se6 1_656 . . 107.89(4) ?
Se3 Fe4 Fe1 1_656 . 1_556 57.51(3) ?
Se4 Fe4 Se6 . . . 105.88(4) ?
Se4 Fe4 Fe1 . . 1_556 57.00(3) ?
Se6 Fe4 Fe1 . . 1_556 131.07(4) ?
Fe5 N3 C3 . . . 107.6(2) ?
N1 C1 C2 . . . 107.5(5) ?
N1 C1 H1c1 . . . 109.47 ?
N1 C1 H2c1 . . . 109.47 ?
C2 C1 H1c1 . . . 109.47 ?
C2 C1 H2c1 . . . 109.47 ?
H1c1 C1 H2c1 . . . 111.4 ?
N2 C2 C1 . . . 109.0(4) ?
N2 C2 H1c2 . . . 109.47 ?
N2 C2 H2c2 . . . 109.47 ?
C1 C2 H1c2 . . . 109.47 ?
C1 C2 H2c2 . . . 109.47 ?
H1c2 C2 H2c2 . . . 109.98 ?
N3 C3 C4 . . . 121.8(6) ?
N3 C3 H1c3 . . . 109.47 ?
N3 C3 H2c3 . . . 109.47 ?
C4 C3 H1c3 . . . 109.47 ?
C4 C3 H2c3 . . . 109.47 ?
H1c3 C3 H2c3 . . . 93.5 ?
N4 C4 C3 . . . 117.1(4) ?
N4 C4 H1c4 . . . 109.47 ?
N4 C4 H2c4 . . . 109.47 ?
C3 C4 H1c4 . . . 109.47 ?
C3 C4 H2c4 . . . 109.47 ?
H1c4 C4 H2c4 . . . 100.59 ?
N5 C5 C6 . . . 112.3(4) ?
N5 C5 H1c5 . . . 109.47 ?
N5 C5 H2c5 . . . 109.47 ?
C6 C5 H1c5 . . . 109.47 ?
C6 C5 H2c5 . . . 109.47 ?
H1c5 C5 H2c5 . . . 106.48 ?
N6 C6 C5 . . . 111.8(4) ?
N6 C6 H1c6 . . . 109.47 ?
N6 C6 H2c6 . . . 109.47 ?
C5 C6 H1c6 . . . 109.47 ?
C5 C6 H2c6 . . . 109.47 ?
H1c6 C6 H2c6 . . . 107 ?
N7 C7 C7 . . 3_655 116.0(5) ?
N7 C7 H1c7 . . . 109.47 ?
N7 C7 H2c7 . . 1_554 109.47 ?
C7 C7 H1c7 3_655 . . 109.47 ?
C7 C7 H2c7 3_655 . 1_554 109.47 ?
H1c7 C7 H2c7 . . 1_554 102.04 ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1n1 Se6 . . 4_464 1.04 2.68 3.466(4) 132.23 ?
N2 H1n2 Se4 . . 3_666 1.04 2.68 3.640(3) 153.91 ?
N2 H2n2 Se2 . . . 1.04 2.81 3.827(3) 165.55 ?
N3 H1n3 Se5 . . 2_645 1.04 2.60 3.604(4) 163.29 ?
N3 H2n3 Se6 . . 4_464 1.04 2.52 3.558(4) 175.26 ?
N4 H1n4 Se5 . . 1_455 1.04 2.61 3.530(3) 147.33 ?
N4 H2n4 Se6 . . 3_666 1.04 2.73 3.672(4) 150.65 ?
N6 H1n6 Se1 . . 2_645 1.04 2.71 3.623(4) 146.13 ?
N6 H2n6 Se2 . . . 1.04 2.97 3.804(4) 137.41 ?
N7 H2n7 Se4 . . 3_666 1.04 2.96 3.830(4) 141.25 ?
N7 H2n7 Se6 . . 3_666 1.04 2.96 3.818(6) 139.78 ?
C2 H2c2 Se4 . . 1_554 1.09 2.84 3.652(6) 131.48 ?
C5 H2c5 Se2 . . . 1.09 2.90 3.845(6) 144.74 ?
C7 H1c7 Se3 . . 3_665 1.09 2.80 3.791(7) 151.16 ?












# publcif Fe10Se12en7 _publcif_info_exptl_table_extra_item loop start
loop_
_publcif_info_exptl_table_extra_item
?

# publcif Fe10Se12en7 _publcif_info_exptl_table_extra_item loop end

# publcif Fe10Se12en7 _publcif_info_exptl_table_header_item loop start
loop_
_publcif_info_exptl_table_header_item
?
