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#$Date: 2019-11-23 06:41:17 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232342 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/74/4347499.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_4347499
loop_
_publ_author_name
'Stock, Philipp'
'Deck, Eva'
'Hohnstein, Silvia'
'Korzekwa, Jana'
'Meyer, Karsten'
'Heinemann, Frank W.'
'Breher, Frank'
'Hörner, Gerald'
_publ_section_title
;
 Molecular Spin Crossover in Slow Motion: Light-Induced Spin-State
 Transitions in Trigonal Prismatic Iron(II) Complexes.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5254
_journal_page_last               5265
_journal_paper_doi               10.1021/acs.inorgchem.6b00238
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H27 Fe N12 P S, 2(B F4)'
_chemical_formula_sum            'C18 H27 B2 F8 Fe N12 P S'
_chemical_formula_weight         704.01
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.0780(14)
_cell_length_b                   10.0780(14)
_cell_length_c                   16.090(3)
_cell_measurement_reflns_used    15949
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.990
_cell_measurement_theta_min      2.334
_cell_volume                     1415.3(4)
_computing_cell_refinement       'Stoe X-Area 1.66'
_computing_data_collection       'Stoe X-Area 1.66'
_computing_data_reduction        'Stoe X-Area 1.66'
_computing_molecular_graphics    'Ortep 32'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15949
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.990
_diffrn_reflns_theta_min         2.334
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 846 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1871
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0822P)²+0.8634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1837
_reflns_number_total             1871
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00238_si_002.cif
_cod_data_source_block           compound_2OTf2
_cod_original_cell_volume        1415.3(5)
_cod_database_code               4347499
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.929
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, 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_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
Fe1 Fe 0.6667 0.3333 0.62740(4) 0.02879(17) Uani 1 3 d S T P . .
S1 S 0.6667 0.3333 0.96232(9) 0.0378(4) Uani 1 3 d S T P . .
P1 P 0.6667 0.3333 0.84401(9) 0.0296(3) Uani 1 3 d S T P . .
N1 N 0.5158(3) 0.1763(3) 0.80498(18) 0.0359(7) Uani 1 1 d . . . . .
N4 N 0.2496(3) -0.0334(3) 0.5498(2) 0.0363(6) Uani 1 1 d . . . . .
N3 N 0.4745(3) 0.1771(3) 0.55614(19) 0.0369(6) Uani 1 1 d . . . . .
C11 C 0.3639(3) 0.0627(3) 0.5995(2) 0.0331(7) Uani 1 1 d . . . . .
C13 C 0.4283(4) 0.1512(4) 0.4747(2) 0.0397(7) Uani 1 1 d . . . . .
H13 H 0.4843 0.2139 0.4290 0.048 Uiso 1 1 calc R U . . .
C12 C 0.2893(4) 0.0210(4) 0.4700(2) 0.0406(8) Uani 1 1 d . . . . .
H12 H 0.2310 -0.0236 0.4211 0.049 Uiso 1 1 calc R U . . .
C14 C 0.1090(4) -0.1734(5) 0.5748(3) 0.0536(11) Uani 1 1 d . . . . .
H14A H 0.1319 -0.2559 0.5843 0.080 Uiso 1 1 calc R U . . .
H14B H 0.0321 -0.2037 0.5308 0.080 Uiso 1 1 calc R U . . .
H14C H 0.0692 -0.1538 0.6262 0.080 Uiso 1 1 calc R U . . .
C1 C 0.4160(4) 0.0414(4) 0.8533(2) 0.0415(9) Uani 1 1 d . . . . .
H1A H 0.3102 0.0204 0.8488 0.062 Uiso 1 1 calc R U . . .
H1B H 0.4480 0.0589 0.9116 0.062 Uiso 1 1 calc R U . . .
H1C H 0.4221 -0.0465 0.8320 0.062 Uiso 1 1 calc R U . . .
C10 C 0.3740(4) 0.0556(4) 0.6884(2) 0.0351(8) Uani 1 1 d . . . . .
H10 H 0.2997 -0.0271 0.7207 0.042 Uiso 1 1 calc R U . . .
N2 N 0.4924(3) 0.1709(3) 0.72018(17) 0.0321(6) Uani 1 1 d . . . . .
B1 B 0.3363(9) -0.3235(9) 0.7372(5) 0.0510(19) Uani 0.3333 1 d D U P A -1
F1 F 0.4707(7) -0.1938(7) 0.7352(7) 0.129(3) Uani 0.3333 1 d D U P A -1
F2 F 0.3335(10) -0.4224(8) 0.6847(4) 0.105(2) Uani 0.3333 1 d D U P A -1
F3 F 0.3254(10) -0.3752(11) 0.8157(3) 0.123(4) Uani 0.3333 1 d D U P A -1
F4 F 0.2227(6) -0.2943(7) 0.7305(7) 0.109(3) Uani 0.3333 1 d D U P A -1
B2 B 0.0012(9) 0.0150(8) 0.7887(5) 0.0490(18) Uani 0.3333 1 d D U P B -1
F5 F 0.0066(12) -0.0260(9) 0.8677(4) 0.138(3) Uani 0.3333 1 d D U P B -1
F6 F 0.1230(7) 0.1523(6) 0.7781(5) 0.066(2) Uani 0.3333 1 d D U P B -1
F7 F -0.1265(5) 0.0209(7) 0.7814(6) 0.069(2) Uani 0.3333 1 d D U P B -1
F8 F 0.0006(10) -0.0857(7) 0.7374(5) 0.211(3) Uani 0.3333 1 d D U P B -1
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
N3 Fe1 N3 93.52(11) . 2_655
N3 Fe1 N3 93.52(11) . 3_665
N3 Fe1 N3 93.52(11) 2_655 3_665
N3 Fe1 N2 137.24(11) . 2_655
N3 Fe1 N2 74.28(10) 2_655 2_655
N3 Fe1 N2 127.39(12) 3_665 2_655
N3 Fe1 N2 127.39(12) . 3_665
N3 Fe1 N2 137.24(12) 2_655 3_665
N3 Fe1 N2 74.28(10) 3_665 3_665
N2 Fe1 N2 81.19(10) 2_655 3_665
N3 Fe1 N2 74.28(10) . .
N3 Fe1 N2 127.39(12) 2_655 .
N3 Fe1 N2 137.24(11) 3_665 .
N2 Fe1 N2 81.19(10) 2_655 .
N2 Fe1 N2 81.19(10) 3_665 .
N1 P1 N1 106.81(12) 2_655 .
N1 P1 N1 106.81(12) 2_655 3_665
N1 P1 N1 106.81(12) . 3_665
N1 P1 S1 112.02(11) 2_655 .
N1 P1 S1 112.02(11) . .
N1 P1 S1 112.02(11) 3_665 .
N2 N1 C1 117.9(2) . .
N2 N1 P1 117.65(19) . .
C1 N1 P1 124.2(2) . .
C11 N4 C12 107.2(2) . .
C11 N4 C14 126.8(3) . .
C12 N4 C14 126.0(3) . .
C11 N3 C13 106.1(3) . .
C11 N3 Fe1 114.7(2) . .
C13 N3 Fe1 139.1(2) . .
N3 C11 N4 111.0(3) . .
N3 C11 C10 121.0(3) . .
N4 C11 C10 128.0(3) . .
C12 C13 N3 108.9(3) . .
C12 C13 H13 125.5 . .
N3 C13 H13 125.5 . .
C13 C12 N4 106.7(3) . .
C13 C12 H12 126.7 . .
N4 C12 H12 126.7 . .
N4 C14 H14A 109.5 . .
N4 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N4 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N2 C10 C11 114.1(3) . .
N2 C10 H10 123.0 . .
C11 C10 H10 123.0 . .
C10 N2 N1 119.5(2) . .
C10 N2 Fe1 115.2(2) . .
N1 N2 Fe1 124.61(17) . .
F2 B1 F4 115.4(8) . .
F2 B1 F1 111.1(8) . .
F4 B1 F1 110.4(8) . .
F2 B1 F3 110.3(8) . .
F4 B1 F3 104.5(8) . .
F1 B1 F3 104.3(8) . .
F8 B2 F7 110.6(8) . .
F8 B2 F6 111.9(8) . .
F7 B2 F6 110.8(7) . .
F8 B2 F5 110.1(8) . .
F7 B2 F5 106.7(8) . .
F6 B2 F5 106.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N3 2.120(3) .
Fe1 N3 2.120(3) 2_655
Fe1 N3 2.120(3) 3_665
Fe1 N2 2.262(2) 2_655
Fe1 N2 2.262(2) 3_665
Fe1 N2 2.262(2) .
S1 P1 1.904(2) .
P1 N1 1.675(3) 2_655
P1 N1 1.675(3) .
P1 N1 1.675(3) 3_665
N1 N2 1.381(4) .
N1 C1 1.448(4) .
N4 C11 1.337(4) .
N4 C12 1.374(5) .
N4 C14 1.470(4) .
N3 C11 1.332(4) .
N3 C13 1.371(5) .
C11 C10 1.438(5) .
C13 C12 1.361(4) .
C13 H13 0.9500 .
C12 H12 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C10 N2 1.284(4) .
C10 H10 0.9500 .
B1 F2 1.296(9) .
B1 F4 1.321(10) .
B1 F1 1.332(8) .
B1 F3 1.349(9) .
B2 F8 1.306(9) .
B2 F7 1.323(10) .
B2 F6 1.324(8) .
B2 F5 1.347(9) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N1 P1 N1 N2 -64.6(2) 2_655
N1 P1 N1 N2 49.4(3) 3_665
S1 P1 N1 N2 172.4(2) .
N1 P1 N1 C1 110.2(4) 2_655
N1 P1 N1 C1 -135.8(4) 3_665
S1 P1 N1 C1 -12.8(4) .
C13 N3 C11 N4 -0.6(4) .
Fe1 N3 C11 N4 -177.8(2) .
C13 N3 C11 C10 -178.8(3) .
Fe1 N3 C11 C10 3.9(4) .
C12 N4 C11 N3 0.7(4) .
C14 N4 C11 N3 179.4(4) .
C12 N4 C11 C10 178.8(4) .
C14 N4 C11 C10 -2.6(6) .
C11 N3 C13 C12 0.3(4) .
Fe1 N3 C13 C12 176.4(3) .
N3 C13 C12 N4 0.1(4) .
C11 N4 C12 C13 -0.5(4) .
C14 N4 C12 C13 -179.2(4) .
N3 C11 C10 N2 3.3(5) .
N4 C11 C10 N2 -174.6(4) .
C11 C10 N2 N1 -179.2(3) .
C11 C10 N2 Fe1 -8.4(4) .
C1 N1 N2 C10 8.0(5) .
P1 N1 N2 C10 -176.8(3) .
C1 N1 N2 Fe1 -161.9(3) .
P1 N1 N2 Fe1 13.3(4) .
