#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:56:23 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180281 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/67/7116768.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_7116768
loop_
_publ_author_name
'Joshua T. Greenfield'
'Chongin Pak'
'Saeed Kamali'
'Kathleen Lee'
'Kirill Kovnir'
_publ_section_title
;
 Control over connectivity and magnetism of tetrahedral FeSe2 chains
 through coordination Fe-amine complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              5355
_journal_paper_doi               10.1039/C4cc08608B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C6 H18 Fe3 N4 Se4'
_chemical_formula_weight         629.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           manual
_audit_update_record
;
2014-10-17 deposited with the CCDC.
2014-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.652(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0393(16)
_cell_length_b                   10.6303(19)
_cell_length_c                   16.641(3)
_cell_measurement_temperature    90(2)
_cell_volume                     1560.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5391
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    12.067
_exptl_absorpt_correction_T_max  0.8888
_exptl_absorpt_correction_T_min  0.1455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0361
_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)+(0.0342P)²+0.4104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                4286
_reflns_number_total             5391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08608b2.cif
_cod_data_source_block           added_by_encifer_1
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7116768
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Se1 Se 0.62839(5) 0.17891(4) 0.15460(3) 0.01174(9) Uani 1 1 d .
Se2 Se 0.36046(5) 0.46833(4) 0.15146(3) 0.01076(9) Uani 1 1 d .
Se3 Se 0.56931(5) 0.34921(4) 0.36083(3) 0.00959(8) Uani 1 1 d .
Se4 Se 0.26881(5) 0.13606(4) 0.23142(3) 0.00980(9) Uani 1 1 d .
Fe1 Fe 0.45944(7) 0.28628(5) 0.22138(4) 0.00965(12) Uani 1 1 d .
Fe2 Fe 0.49585(7) 0.03186(5) 0.21771(4) 0.00931(12) Uani 1 1 d .
Fe3 Fe 0.29990(7) 0.28146(5) 0.36516(4) 0.00946(12) Uani 1 1 d .
N1 N 0.0813(4) 0.2247(3) 0.4029(2) 0.0112(7) Uani 1 1 d .
N2 N 0.3596(4) 0.1103(3) 0.4352(2) 0.0115(7) Uani 1 1 d .
H2NB H 0.4334 0.0686 0.4153 0.014 Uiso 1 1 calc R
H2NA H 0.3996 0.1308 0.4893 0.014 Uiso 1 1 calc R
N3 N 0.3097(4) 0.3987(3) 0.4746(2) 0.0135(7) Uani 1 1 d .
H3NA H 0.3856 0.3698 0.5167 0.016 Uiso 1 1 calc R
H3NB H 0.3326 0.4801 0.4630 0.016 Uiso 1 1 calc R
N4 N 0.1281(4) 0.4014(3) 0.2897(2) 0.0126(7) Uani 1 1 d .
H4NA H 0.1176 0.4743 0.3177 0.015 Uiso 1 1 calc R
H4NB H 0.1572 0.4227 0.2418 0.015 Uiso 1 1 calc R
C1 C 0.2277(5) 0.0248(4) 0.4313(3) 0.0156(9) Uani 1 1 d .
H1B H 0.2263 -0.0045 0.4875 0.019 Uiso 1 1 calc R
H1A H 0.2401 -0.0499 0.3978 0.019 Uiso 1 1 calc R
C2 C 0.0772(5) 0.0878(4) 0.3942(3) 0.0196(10) Uani 1 1 d .
H2B H 0.0477 0.0663 0.3350 0.024 Uiso 1 1 calc R
H2A H -0.0015 0.0538 0.4213 0.024 Uiso 1 1 calc R
C3 C 0.1644(5) 0.3966(4) 0.5010(3) 0.0172(9) Uani 1 1 d .
H3B H 0.0930 0.4572 0.4679 0.021 Uiso 1 1 calc R
H3A H 0.1809 0.4216 0.5596 0.021 Uiso 1 1 calc R
C4 C 0.0984(6) 0.2658(5) 0.4898(3) 0.0201(10) Uani 1 1 d .
H4A H 0.1658 0.2066 0.5267 0.024 Uiso 1 1 calc R
H4B H -0.0018 0.2650 0.5047 0.024 Uiso 1 1 calc R
C5 C -0.0173(5) 0.3334(4) 0.2701(3) 0.0134(8) Uani 1 1 d .
H5A H -0.0107 0.2622 0.2327 0.016 Uiso 1 1 calc R
H5B H -0.0990 0.3904 0.2421 0.016 Uiso 1 1 calc R
C6 C -0.0529(5) 0.2847(5) 0.3497(3) 0.0182(10) Uani 1 1 d .
H6B H -0.0872 0.3554 0.3798 0.022 Uiso 1 1 calc R
H6A H -0.1365 0.2227 0.3366 0.022 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
Fe2 Se1 Fe1 70.55(3) . .
Fe1 Se2 Fe2 72.89(3) . 2_655
Fe2 Se3 Fe1 72.10(3) 2_655 .
Fe2 Se3 Fe3 97.16(2) 2_655 .
Fe1 Se3 Fe3 75.80(2) . .
Fe1 Se4 Fe2 69.76(3) . .
Fe1 Se4 Fe3 74.04(2) . .
Fe2 Se4 Fe3 114.34(3) . .
Se2 Fe1 Se1 112.45(3) . .
Se2 Fe1 Se4 112.75(3) . .
Se1 Fe1 Se4 105.10(3) . .
Se2 Fe1 Se3 106.38(3) . .
Se1 Fe1 Se3 114.41(3) . .
Se4 Fe1 Se3 105.69(3) . .
Se2 Fe1 Fe2 147.83(3) . .
Se1 Fe1 Fe2 54.43(2) . .
Se4 Fe1 Fe2 55.20(2) . .
Se3 Fe1 Fe2 105.70(3) . .
Se2 Fe1 Fe2 54.26(2) . 2_655
Se1 Fe1 Fe2 124.24(3) . 2_655
Se4 Fe1 Fe2 130.50(3) . 2_655
Se3 Fe1 Fe2 52.828(19) . 2_655
Fe2 Fe1 Fe2 157.68(3) . 2_655
Se3 Fe2 Se1 113.09(3) 2_645 .
Se3 Fe2 Se2 107.21(3) 2_645 2_645
Se1 Fe2 Se2 111.61(3) . 2_645
Se3 Fe2 Se4 108.76(3) 2_645 .
Se1 Fe2 Se4 105.49(3) . .
Se2 Fe2 Se4 110.69(3) 2_645 .
Se3 Fe2 Fe1 144.86(3) 2_645 .
Se1 Fe2 Fe1 55.02(2) . .
Se2 Fe2 Fe1 107.81(3) 2_645 .
Se4 Fe2 Fe1 55.04(2) . .
Se3 Fe2 Fe1 55.07(2) 2_645 2_645
Se1 Fe2 Fe1 137.27(3) . 2_645
Se2 Fe2 Fe1 52.85(2) 2_645 2_645
Se4 Fe2 Fe1 117.22(3) . 2_645
Fe1 Fe2 Fe1 157.82(2) . 2_645
N2 Fe3 N4 149.71(14) . .
N2 Fe3 N3 94.05(14) . .
N4 Fe3 N3 92.31(14) . .
N2 Fe3 N1 76.01(13) . .
N4 Fe3 N1 76.31(13) . .
N3 Fe3 N1 78.56(13) . .
N2 Fe3 Se3 97.19(10) . .
N4 Fe3 Se3 112.42(10) . .
N3 Fe3 Se3 89.87(10) . .
N1 Fe3 Se3 165.98(9) . .
N2 Fe3 Se4 86.02(10) . .
N4 Fe3 Se4 85.80(10) . .
N3 Fe3 Se4 176.28(10) . .
N1 Fe3 Se4 97.87(9) . .
Se3 Fe3 Se4 93.82(2) . .
C2 N1 C6 111.7(4) . .
C2 N1 C4 112.6(4) . .
C6 N1 C4 110.6(3) . .
C2 N1 Fe3 103.9(3) . .
C6 N1 Fe3 111.5(3) . .
C4 N1 Fe3 106.2(3) . .
C1 N2 Fe3 112.7(3) . .
C3 N3 Fe3 111.3(3) . .
C5 N4 Fe3 109.2(3) . .
N2 C1 C2 112.7(3) . .
N1 C2 C1 113.4(4) . .
N3 C3 C4 109.3(4) . .
N1 C4 C3 110.2(4) . .
N4 C5 C6 108.9(4) . .
N1 C6 C5 111.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 Fe2 2.3523(8) .
Se1 Fe1 2.3693(8) .
Se2 Fe1 2.3332(8) .
Se2 Fe2 2.3758(8) 2_655
Se3 Fe2 2.3425(8) 2_655
Se3 Fe1 2.4102(8) .
Se3 Fe3 2.5556(8) .
Se4 Fe1 2.3819(8) .
Se4 Fe2 2.3866(8) .
Se4 Fe3 2.6733(8) .
Fe1 Fe2 2.7268(9) .
Fe1 Fe2 2.7976(9) 2_655
Fe2 Se3 2.3426(8) 2_645
Fe2 Se2 2.3758(8) 2_645
Fe2 Fe1 2.7976(9) 2_645
Fe3 N2 2.164(4) .
Fe3 N4 2.182(4) .
Fe3 N3 2.192(4) .
Fe3 N1 2.282(4) .
N1 C2 1.462(6) .
N1 C6 1.480(6) .
N1 C4 1.485(6) .
N2 C1 1.489(6) .
N3 C3 1.474(6) .
N4 C5 1.473(5) .
C1 C2 1.520(6) .
C3 C4 1.509(7) .
C5 C6 1.522(6) .
