#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:00:03 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229236 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045583.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_7045583
loop_
_publ_author_name
'Stahl, J.'
'Shlaen, E.'
'Singer, H.'
'Johrendt, D.'
_publ_section_title
;
 Systematic dimensional reduction of the layered β-FeSe structure by
 solvothermal synthesis.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3264
_journal_page_last               3271
_journal_paper_doi               10.1039/c8dt00025e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C6 H24 Fe3 N6 Se4'
_chemical_formula_weight         663.7
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                109.880(13)
_cell_angle_beta                 96.370(15)
_cell_angle_gamma                114.093(14)
_cell_formula_units_Z            2
_cell_length_a                   9.104(4)
_cell_length_b                   10.398(4)
_cell_length_c                   11.675(5)
_cell_measurement_reflns_used    409
_cell_measurement_temperature    293
_cell_measurement_theta_max      35.508
_cell_measurement_theta_min      4.740
_cell_volume                     907.7(7)
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37683
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    10.379
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.428
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.66
_refine_ls_goodness_of_fit_ref   1.56
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    102
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.0499
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                2424
_reflns_number_total             3280
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            c8dt00025e2.cif
_cod_data_source_block           Fe3Se4en3
_cod_depositor_comments
'Adding full bibliography for 7045582--7045584.cif.'
_cod_original_cell_volume        907.8(7)
_cod_database_code               7045583
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
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
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
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
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_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_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
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
