#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:50:16 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180216 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/02/7110269.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_7110269
loop_
_publ_author_name
'Nassim Nassirini'
'Saeid Amani'
'Simon J. Teat'
'Olivier Roubeau'
'Patrick Gamez'
_publ_section_title
;
 Enhancement of spin-crossover cooperativity mediated by lone pair-pi
 interactions and halogen bonding
;
_journal_name_full               Chem.Commun.
_journal_page_first              1003
_journal_paper_doi               10.1039/c3cc48334g
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C40 H16 Cl2 F10 Fe N14 O2 S2, 2(C H4 O)'
_chemical_formula_sum            'C42 H24 Cl2 F10 Fe N14 O4 S2'
_chemical_formula_weight         1169.62
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                94.784(4)
_cell_angle_beta                 105.483(3)
_cell_angle_gamma                100.902(3)
_cell_formula_units_Z            1
_cell_length_a                   9.173(2)
_cell_length_b                   11.167(3)
_cell_length_c                   12.759(3)
_cell_measurement_reflns_used    5307
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      3.18
_cell_volume                     1224.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            13341
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        28.950
_diffrn_reflns_theta_max         29.051
_diffrn_reflns_theta_min         3.189
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI US'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0547
_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)+(0.0797P)²+1.0973P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3664
_reflns_number_total             4973
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3cc48334g.txt
_cod_data_source_block           c1_200K
_cod_database_code               7110269
#BEGIN Tags that were not found in dictionaries:
_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   0.922
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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 0.5000 0.5000 0.5000 0.0372(2) Uani 1 2 d S . P . .
Cl1 Cl 0.42981(12) 0.17797(9) 0.92988(9) 0.0619(3) Uani 1 1 d . . . . .
S1 S 0.30283(14) 0.78386(10) 0.26568(10) 0.0658(3) Uani 1 1 d . . . . .
O1 O 0.8299(3) 0.5504(2) 1.0236(2) 0.0506(6) Uani 1 1 d . . . . .
N1 N 0.3903(3) 0.5967(3) 0.3823(2) 0.0474(7) Uani 1 1 d . . . . .
N2 N 0.5315(3) 0.6625(3) 0.6233(2) 0.0462(7) Uani 1 1 d . . . . .
N3 N 0.2780(3) 0.4403(3) 0.5415(2) 0.0426(6) Uani 1 1 d . . . . .
N4 N 0.4096(3) 0.5295(3) 0.7236(2) 0.0401(6) Uani 1 1 d . . . . .
N5 N 0.4224(3) 0.3652(3) 0.8235(2) 0.0433(6) Uani 1 1 d . . . . .
N6 N 0.6226(3) 0.5477(3) 0.8740(2) 0.0422(6) Uani 1 1 d . . . . .
N7 N 0.6378(3) 0.3817(3) 0.9826(2) 0.0465(7) Uani 1 1 d . . . . .
C1 C 0.3540(4) 0.6750(3) 0.3337(3) 0.0426(8) Uani 1 1 d . . . . .
C2 C 0.5852(5) 0.7766(3) 0.6047(4) 0.0607(10) Uani 1 1 d . . . . .
H2A H 0.6256 0.7860 0.5439 0.073 Uiso 1 1 calc R U . . .
C3 C 0.5842(6) 0.8808(4) 0.6701(4) 0.0774(13) Uani 1 1 d . . . . .
H3A H 0.6256 0.9602 0.6556 0.093 Uiso 1 1 calc R U . . .
C4 C 0.5232(6) 0.8686(4) 0.7554(4) 0.0734(13) Uani 1 1 d . . . . .
H4A H 0.5207 0.9395 0.8009 0.088 Uiso 1 1 calc R U . . .
C5 C 0.4643(5) 0.7519(4) 0.7760(3) 0.0576(10) Uani 1 1 d . . . . .
H5A H 0.4205 0.7408 0.8350 0.069 Uiso 1 1 calc R U . . .
C6 C 0.4719(4) 0.6525(3) 0.7073(3) 0.0427(7) Uani 1 1 d . . . . .
C7 C 0.1500(4) 0.3809(4) 0.4642(3) 0.0525(9) Uani 1 1 d . . . . .
H7A H 0.1532 0.3682 0.3904 0.063 Uiso 1 1 calc R U . . .
C8 C 0.0116(4) 0.3365(4) 0.4876(4) 0.0606(10) Uani 1 1 d . . . . .
H8A H -0.0780 0.2934 0.4310 0.073 Uiso 1 1 calc R U . . .
C9 C 0.0075(4) 0.3563(4) 0.5944(4) 0.0611(10) Uani 1 1 d . . . . .
H9A H -0.0849 0.3252 0.6128 0.073 Uiso 1 1 calc R U . . .
C10 C 0.1360(4) 0.4206(4) 0.6739(3) 0.0521(9) Uani 1 1 d . . . . .
H10A H 0.1336 0.4383 0.7475 0.063 Uiso 1 1 calc R U . . .
C11 C 0.2711(4) 0.4598(3) 0.6445(3) 0.0407(7) Uani 1 1 d . . . . .
C12 C 0.4862(4) 0.4787(3) 0.8100(3) 0.0403(7) Uani 1 1 d . . . . .
C13 C 0.5045(4) 0.3251(3) 0.9094(3) 0.0441(8) Uani 1 1 d . . . . .
C14 C 0.6887(4) 0.4920(3) 0.9547(3) 0.0428(7) Uani 1 1 d . . . . .
C15 C 0.9127(4) 0.6508(3) 0.9932(3) 0.0478(8) Uani 1 1 d . . . . .
C16 C 0.9627(4) 0.7602(4) 1.0629(3) 0.0552(9) Uani 1 1 d . . . . .
C17 C 1.0612(5) 0.8576(4) 1.0408(4) 0.0690(13) Uani 1 1 d . . . . .
C18 C 1.1095(5) 0.8453(5) 0.9481(5) 0.0762(14) Uani 1 1 d . . . . .
C19 C 1.0598(5) 0.7391(5) 0.8781(4) 0.0699(12) Uani 1 1 d . . . . .
C20 C 0.9621(4) 0.6403(4) 0.8994(3) 0.0536(9) Uani 1 1 d . . . . .
F1 F 0.9167(3) 0.7702(2) 1.1546(2) 0.0711(7) Uani 1 1 d . . . . .
F2 F 1.1094(4) 0.9632(2) 1.1122(3) 0.0973(10) Uani 1 1 d . . . . .
F3 F 1.2080(4) 0.9414(3) 0.9295(3) 0.1205(14) Uani 1 1 d . . . . .
F4 F 1.1083(3) 0.7276(4) 0.7878(3) 0.1049(11) Uani 1 1 d . . . . .
F5 F 0.9178(3) 0.5355(2) 0.8317(2) 0.0676(6) Uani 1 1 d . . . . .
O1S O 0.820(2) 0.9621(18) 0.3549(16) 0.183(6) Uani 0.430(11) 1 d D U P A 1
C1S C 0.973(3) 1.0037(19) 0.3414(17) 0.157(7) Uani 0.430(11) 1 d D U P A 1
H1S1 H 0.9795 1.0834 0.3141 0.235 Uiso 0.430(11) 1 calc R U P A 1
H1S2 H 0.9911 0.9433 0.2887 0.235 Uiso 0.430(11) 1 calc R U P A 1
H1S3 H 1.0518 1.0124 0.4124 0.235 Uiso 0.430(11) 1 calc R U P A 1
O2S O 0.740(2) 0.8906(17) 0.3868(12) 0.224(6) Uani 0.570(11) 1 d D U P A 2
C2S C 0.772(2) 1.0018(14) 0.4635(15) 0.171(6) Uani 0.570(11) 1 d D U P A 2
H2S1 H 0.8465 0.9944 0.5326 0.257 Uiso 0.570(11) 1 calc R U P A 2
H2S2 H 0.6758 1.0140 0.4775 0.257 Uiso 0.570(11) 1 calc R U P A 2
H2S3 H 0.8163 1.0724 0.4323 0.257 Uiso 0.570(11) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
F F -0.0053 0.0125
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
S S 0.1206 0.1480
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1408 0.1896
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2064 0.9930
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
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
N1 Fe1 N1 180.00(13) . 2_666
N1 Fe1 N2 87.31(12) . .
N1 Fe1 N2 92.69(12) 2_666 .
N1 Fe1 N2 92.69(12) . 2_666
N1 Fe1 N2 87.31(12) 2_666 2_666
N2 Fe1 N2 180.00(16) . 2_666
N1 Fe1 N3 89.77(11) . .
N1 Fe1 N3 90.23(11) 2_666 .
N2 Fe1 N3 83.13(11) . .
N2 Fe1 N3 96.86(11) 2_666 .
N1 Fe1 N3 90.23(11) . 2_666
N1 Fe1 N3 89.77(11) 2_666 2_666
N2 Fe1 N3 96.87(11) . 2_666
N2 Fe1 N3 83.14(11) 2_666 2_666
N3 Fe1 N3 180.0 . 2_666
C14 O1 C15 118.7(3) . .
C1 N1 Fe1 163.3(3) . .
C6 N2 C2 117.1(3) . .
C6 N2 Fe1 121.0(2) . .
C2 N2 Fe1 120.7(3) . .
C7 N3 C11 118.3(3) . .
C7 N3 Fe1 120.6(2) . .
C11 N3 Fe1 121.1(2) . .
C12 N4 C11 121.1(3) . .
C12 N4 C6 120.3(3) . .
C11 N4 C6 118.6(3) . .
C13 N5 C12 113.6(3) . .
C14 N6 C12 112.6(3) . .
C13 N7 C14 109.6(3) . .
N1 C1 S1 179.8(5) . .
N2 C2 C3 122.7(4) . .
N2 C2 H2A 118.6 . .
C3 C2 H2A 118.6 . .
C4 C3 C2 119.1(4) . .
C4 C3 H3A 120.5 . .
C2 C3 H3A 120.5 . .
C3 C4 C5 119.7(4) . .
C3 C4 H4A 120.1 . .
C5 C4 H4A 120.1 . .
C6 C5 C4 117.4(4) . .
C6 C5 H5A 121.3 . .
C4 C5 H5A 121.3 . .
N2 C6 C5 123.9(3) . .
N2 C6 N4 116.4(3) . .
C5 C6 N4 119.7(3) . .
N3 C7 C8 122.4(4) . .
N3 C7 H7A 118.8 . .
C8 C7 H7A 118.8 . .
C9 C8 C7 118.4(4) . .
C9 C8 H8A 120.8 . .
C7 C8 H8A 120.8 . .
C10 C9 C8 119.9(4) . .
C10 C9 H9A 120.0 . .
C8 C9 H9A 120.0 . .
C9 C10 C11 118.3(4) . .
C9 C10 H10A 120.9 . .
C11 C10 H10A 120.9 . .
N3 C11 C10 122.7(3) . .
N3 C11 N4 116.1(3) . .
C10 C11 N4 121.1(3) . .
N5 C12 N6 125.2(3) . .
N5 C12 N4 118.3(3) . .
N6 C12 N4 116.5(3) . .
N5 C13 N7 129.2(3) . .
N5 C13 Cl1 115.8(3) . .
N7 C13 Cl1 115.0(3) . .
N6 C14 N7 129.7(3) . .
N6 C14 O1 118.5(3) . .
N7 C14 O1 111.7(3) . .
C16 C15 O1 119.3(3) . .
C16 C15 C20 119.0(4) . .
O1 C15 C20 121.3(3) . .
F1 C16 C15 119.1(4) . .
F1 C16 C17 120.4(4) . .
C15 C16 C17 120.4(4) . .
F2 C17 C18 121.6(4) . .
F2 C17 C16 118.7(5) . .
C18 C17 C16 119.8(4) . .
C19 C18 F3 121.0(5) . .
C19 C18 C17 120.5(4) . .
F3 C18 C17 118.5(5) . .
F4 C19 C18 120.1(4) . .
F4 C19 C20 119.4(5) . .
C18 C19 C20 120.5(5) . .
F5 C20 C19 119.9(4) . .
F5 C20 C15 120.4(3) . .
C19 C20 C15 119.8(4) . .
O1S C1S H1S1 109.5 . .
O1S C1S H1S2 109.5 . .
H1S1 C1S H1S2 109.5 . .
O1S C1S H1S3 109.5 . .
H1S1 C1S H1S3 109.5 . .
H1S2 C1S H1S3 109.5 . .
O2S C2S H2S1 109.5 . .
O2S C2S H2S2 109.5 . .
H2S1 C2S H2S2 109.5 . .
O2S C2S H2S3 109.5 . .
H2S1 C2S H2S3 109.5 . .
H2S2 C2S H2S3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.076(3) .
Fe1 N1 2.076(3) 2_666
Fe1 N2 2.221(3) .
Fe1 N2 2.221(3) 2_666
Fe1 N3 2.235(3) .
Fe1 N3 2.235(3) 2_666
Cl1 C13 1.726(4) .
S1 C1 1.620(4) .
O1 C14 1.361(4) .
O1 C15 1.377(4) .
N1 C1 1.163(4) .
N2 C6 1.330(4) .
N2 C2 1.342(5) .
N3 C7 1.330(5) .
N3 C11 1.334(4) .
N4 C12 1.368(4) .
N4 C11 1.431(4) .
N4 C6 1.439(4) .
N5 C13 1.318(4) .
N5 C12 1.338(4) .
N6 C14 1.315(4) .
N6 C12 1.346(4) .
N7 C13 1.330(5) .
N7 C14 1.344(4) .
C2 C3 1.377(6) .
C2 H2A 0.9500 .
C3 C4 1.356(7) .
C3 H3A 0.9500 .
C4 C5 1.387(6) .
C4 H4A 0.9500 .
C5 C6 1.379(5) .
C5 H5A 0.9500 .
C7 C8 1.391(5) .
C7 H7A 0.9500 .
C8 C9 1.375(6) .
C8 H8A 0.9500 .
C9 C10 1.361(6) .
C9 H9A 0.9500 .
C10 C11 1.392(5) .
C10 H10A 0.9500 .
C15 C16 1.373(6) .
C15 C20 1.391(5) .
C16 F1 1.348(5) .
C16 C17 1.375(6) .
C17 F2 1.351(5) .
C17 C18 1.375(7) .
C18 C19 1.347(7) .
C18 F3 1.348(5) .
C19 F4 1.346(6) .
C19 C20 1.379(6) .
C20 F5 1.321(5) .
O1S C1S 1.451(17) .
C1S H1S1 0.9800 .
C1S H1S2 0.9800 .
C1S H1S3 0.9800 .
O2S C2S 1.447(15) .
C2S H2S1 0.9800 .
C2S H2S2 0.9800 .
C2S H2S3 0.9800 .
