#------------------------------------------------------------------------------
#$Date: 2015-06-07 00:57:03 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138517 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/03/7220344.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_7220344
loop_
_publ_author_name
'Wang, Hongfeng'
'Grosjean, Arnaud'
'Sinito, Chiara'
'Kaiba, Abdellah'
'Baldé, Chérif'
'Desplanches, Cédric'
'Létard, Jean-François'
'Guionneau, Philippe'
_publ_section_title
;
 Towards synergy between spin-crossover and metal--ligand bond break in
 molecular crystals: structural investigations of eight seven-coordinated
 Fe(ii) macrocyclic complexes
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4075
_journal_paper_doi               10.1039/C5CE00557D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C18 H25 Fe N7 S2'
_chemical_formula_weight         459.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-03-18 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 85.856(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6865(2)
_cell_length_b                   11.5038(4)
_cell_length_c                   24.0051(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2117.08(11)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17041
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.056
_diffrn_reflns_theta_min         1.964
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.8733
_exptl_absorpt_correction_T_min  0.6059
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6165
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0733P)²+1.6406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4730
_reflns_number_total             6165
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00557d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7220335--7220350.cif.'
_cod_database_code               7220344
_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   0.606
_shelx_estimated_absorpt_t_max   0.873
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe Fe 0.65055(5) 0.22818(4) 0.37122(2) 0.04598(14) Uani 1 1 d . .
S2 S 0.40746(11) 0.11866(9) 0.19391(3) 0.0623(2) Uani 1 1 d . .
S1 S 0.89834(12) 0.32116(10) 0.54695(3) 0.0676(3) Uani 1 1 d . .
N6 N 0.7844(4) 0.2823(3) 0.44128(12) 0.0659(7) Uani 1 1 d . .
C2 C 0.7886(6) -0.1456(3) 0.37341(15) 0.0681(9) Uani 1 1 d . .
C8 C 0.9366(4) 0.0418(3) 0.34113(11) 0.0543(7) Uani 1 1 d . .
N3 N 0.9092(3) 0.1497(3) 0.33692(11) 0.0562(6) Uani 1 1 d . .
N1 N 0.6529(3) 0.0386(2) 0.38846(9) 0.0437(5) Uani 1 1 d . .
N2 N 0.4109(3) 0.1752(3) 0.42961(11) 0.0590(7) Uani 1 1 d . .
C11 C 0.4729(3) 0.1551(3) 0.25472(11) 0.0456(6) Uani 1 1 d . .
N7 N 0.5190(3) 0.1824(3) 0.29777(11) 0.0554(6) Uani 1 1 d . .
C6 C 0.3766(4) 0.0691(4) 0.43751(12) 0.0582(8) Uani 1 1 d . .
C1 C 0.7879(4) -0.0265(3) 0.36843(11) 0.0485(6) Uani 1 1 d . .
C5 C 0.5133(4) -0.0127(3) 0.41416(11) 0.0519(7) Uani 1 1 d . .
C3 C 0.6442(7) -0.1972(4) 0.3987(2) 0.0832(13) Uani 1 1 d . .
C16 C 0.5335(8) 0.4906(5) 0.3740(3) 0.123(2) Uani 1 1 d . .
H16A H 0.6144 0.5096 0.4019 0.148 Uiso 1 1 calc R U
H16B H 0.4454 0.5510 0.3739 0.148 Uiso 1 1 calc R U
N5 N 0.7765(5) 0.3829(3) 0.31741(15) 0.0860(11) Uani 1 1 d D .
N4 N 0.4583(6) 0.3843(4) 0.3846(2) 0.0937(12) Uani 1 1 d D .
C4 C 0.5037(6) -0.1324(4) 0.41947(17) 0.0758(11) Uani 1 1 d . .
C15 C 0.6283(7) 0.4784(4) 0.3169(3) 0.1025(18) Uani 1 1 d . .
H15A H 0.6798 0.5525 0.3055 0.123 Uiso 1 1 calc R U
H15B H 0.5459 0.4569 0.2899 0.123 Uiso 1 1 calc R U
C7 C 0.2146(5) 0.0208(5) 0.46862(16) 0.0834(12) Uani 1 1 d . .
H7A H 0.2461 -0.0180 0.5018 0.125 Uiso 1 1 calc R U
H7B H 0.1593 -0.0334 0.4452 0.125 Uiso 1 1 calc R U
H7C H 0.1354 0.0832 0.4786 0.125 Uiso 1 1 calc R U
C18 C 0.2865(6) 0.2622(5) 0.45225(19) 0.0816(13) Uani 1 1 d . .
C14 C 0.8428(9) 0.3554(6) 0.2643(2) 0.126(3) Uani 1 1 d . .
H14A H 0.8592 0.4259 0.2424 0.151 Uiso 1 1 calc R U
H14B H 0.7609 0.3061 0.2464 0.151 Uiso 1 1 calc R U
C13 C 1.0087(9) 0.2953(5) 0.2664(2) 0.0980(16) Uani 1 1 d . .
H13A H 1.1002 0.3527 0.2595 0.118 Uiso 1 1 calc R U
H13B H 1.0183 0.2412 0.2354 0.118 Uiso 1 1 calc R U
C12 C 1.0479(5) 0.2304(5) 0.3169(2) 0.0919(15) Uani 1 1 d . .
H12A H 1.1549 0.1868 0.3090 0.110 Uiso 1 1 calc R U
H12B H 1.0678 0.2854 0.3464 0.110 Uiso 1 1 calc R U
C9 C 1.1026(5) -0.0216(4) 0.32291(17) 0.0800(12) Uani 1 1 d . .
H9A H 1.1388 -0.0006 0.2851 0.120 Uiso 1 1 calc R U
H9B H 1.0827 -0.1039 0.3250 0.120 Uiso 1 1 calc R U
H9C H 1.1922 -0.0007 0.3469 0.120 Uiso 1 1 calc R U
C17 C 0.3683(8) 0.3776(6) 0.4470(3) 0.1042(18) Uani 1 1 d . .
C10 C 0.8328(4) 0.2995(3) 0.48481(12) 0.0518(7) Uani 1 1 d . .
H3 H 0.406(5) -0.162(4) 0.4327(17) 0.071(11) Uiso 1 1 d . .
H2 H 0.638(7) -0.267(5) 0.404(2) 0.099(16) Uiso 1 1 d . .
H5 H 0.442(6) 0.371(4) 0.4759(18) 0.073(13) Uiso 1 1 d . .
H4 H 0.288(7) 0.433(5) 0.446(2) 0.105(16) Uiso 1 1 d . .
H7 H 0.170(7) 0.264(4) 0.428(2) 0.103(16) Uiso 1 1 d . .
H8 H 0.252(6) 0.250(4) 0.490(2) 0.088(14) Uiso 1 1 d . .
H6 H 0.883(6) -0.192(4) 0.3608(19) 0.089(14) Uiso 1 1 d . .
H501 H 0.843(5) 0.416(4) 0.3419(16) 0.099(16) Uiso 1 1 d D .
H401 H 0.366(5) 0.367(4) 0.3652(19) 0.109(17) Uiso 1 1 d D .
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'
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
N6 Fe N7 176.74(11)
N6 Fe N1 97.43(11)
N7 Fe N1 85.60(10)
N6 Fe N3 86.70(11)
N7 Fe N3 93.21(10)
N1 Fe N3 70.13(9)
N6 Fe N2 90.45(11)
N7 Fe N2 91.77(10)
N1 Fe N2 69.22(10)
N3 Fe N2 138.49(11)
N6 Fe N4 90.19(13)
N7 Fe N4 88.34(13)
N1 Fe N4 138.08(14)
N3 Fe N4 151.72(15)
N2 Fe N4 69.57(15)
N6 Fe N5 90.52(12)
N7 Fe N5 86.27(11)
N1 Fe N5 146.37(13)
N3 Fe N5 77.82(14)
N2 Fe N5 143.65(14)
N4 Fe N5 74.10(17)
C10 N6 Fe 167.0(3)
C3 C2 C1 117.7(4)
N3 C8 C1 115.0(3)
N3 C8 C9 126.5(3)
C1 C8 C9 118.4(3)
C8 N3 C12 121.7(3)
C8 N3 Fe 120.4(2)
C12 N3 Fe 117.5(3)
C5 N1 C1 119.6(3)
C5 N1 Fe 120.2(2)
C1 N1 Fe 119.90(19)
C6 N2 C18 118.9(3)
C6 N2 Fe 119.7(2)
C18 N2 Fe 121.0(3)
N7 C11 S2 179.2(3)
C11 N7 Fe 169.9(2)
N2 C6 C5 114.9(3)
N2 C6 C7 125.9(3)
C5 C6 C7 119.2(4)
N1 C1 C2 122.2(3)
N1 C1 C8 114.2(3)
C2 C1 C8 123.6(3)
N1 C5 C4 121.2(3)
N1 C5 C6 114.5(3)
C4 C5 C6 124.2(3)
C2 C3 C4 121.2(4)
N4 C16 C15 104.8(5)
C14 N5 C15 111.8(5)
C14 N5 Fe 116.3(3)
C15 N5 Fe 105.1(3)
C16 N4 C17 111.4(5)
C16 N4 Fe 114.1(4)
C17 N4 Fe 108.5(3)
C3 C4 C5 118.1(4)
C16 C15 N5 110.9(4)
N2 C18 C17 108.8(4)
N5 C14 C13 110.2(5)
C14 C13 C12 120.1(4)
N3 C12 C13 113.8(4)
C18 C17 N4 106.0(4)
N6 C10 S1 178.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe N6 2.127(3)
Fe N7 2.160(3)
Fe N1 2.220(2)
Fe N3 2.282(3)
Fe N2 2.315(3)
Fe N4 2.333(4)
Fe N5 2.365(3)
S2 C11 1.633(3)
S1 C10 1.628(3)
N6 C10 1.151(4)
C2 C3 1.363(7)
C2 C1 1.376(5)
C8 N3 1.264(5)
C8 C1 1.498(4)
C8 C9 1.507(4)
N3 C12 1.468(5)
N1 C5 1.336(4)
N1 C1 1.341(4)
N2 C6 1.260(5)
N2 C18 1.461(5)
C11 N7 1.160(4)
C6 C5 1.490(5)
C6 C7 1.511(4)
C5 C4 1.385(5)
C3 C4 1.375(7)
C16 N4 1.369(7)
C16 C15 1.512(9)
N5 C14 1.375(7)
N5 C15 1.583(7)
N4 C17 1.606(7)
C18 C17 1.470(8)
C14 C13 1.454(9)
C13 C12 1.473(7)
