#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:16:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180032 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/26/7032607.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_7032607
loop_
_publ_author_name
'Luo, Yang-Hui'
'Yang, Li-Jing'
'Liu, Qing-Ling'
'Ling, Yang'
'Wang, Wei'
'Sun, Bai-Wang'
_publ_section_title
;
 Lattice water molecules tuned spin-crossover for an iron(ii) complex with
 thermal hysteresis.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16937
_journal_page_last               16942
_journal_paper_doi               10.1039/c4dt02587c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'2(C36 H36 Fe N6), C Cl N O2 S, 2(C N S), 6(O)'
_chemical_formula_sum            'C75 H72 Cl Fe2 N15 O8 S3'
_chemical_formula_weight         1554.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.551(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5927(6)
_cell_length_b                   27.0994(14)
_cell_length_c                   14.2354(8)
_cell_measurement_reflns_used    6694
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      28.3520
_cell_measurement_theta_min      3.5130
_cell_volume                     3988.7(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19641
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.4368
_exptl_crystal_size_mid          0.3266
_exptl_crystal_size_min          0.1454
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4373
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0639P)²+9.5629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                3577
_reflns_number_total             4373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02587c2.cif
_cod_data_source_block           x-2
_cod_depositor_comments
'Adding full bibliography for 7032606--7032608.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7032607
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.346619(18) 0.2500 0.02827(18) Uani 1 2 d S . .
N1 N 0.6397(2) 0.34424(8) 0.36578(16) 0.0316(5) Uani 1 1 d . . .
N2 N 0.4298(2) 0.29526(8) 0.32020(16) 0.0312(5) Uani 1 1 d . . .
N3 N 0.4261(2) 0.40174(8) 0.31015(16) 0.0321(5) Uani 1 1 d . . .
C1 C 0.3553(3) 0.21914(11) 0.4304(2) 0.0422(7) Uani 1 1 d . . .
C2 C 0.4604(3) 0.44723(10) 0.2864(2) 0.0345(6) Uani 1 1 d . . .
C3 C 0.5000(3) 0.28456(10) 0.40951(19) 0.0335(6) Uani 1 1 d . . .
C4 C 0.8051(3) 0.34494(11) 0.5485(2) 0.0434(7) Uani 1 1 d . . .
C5 C 0.2831(3) 0.23116(11) 0.3403(2) 0.0457(7) Uani 1 1 d . . .
H5 H 0.2070 0.2135 0.3146 0.055 Uiso 1 1 calc R . .
C6 C 0.7478(3) 0.37163(11) 0.3845(2) 0.0381(6) Uani 1 1 d . . .
H6 H 0.7674 0.3911 0.3348 0.046 Uiso 1 1 calc R . .
C7 C 0.4247(3) 0.48956(11) 0.3283(2) 0.0478(8) Uani 1 1 d . . .
H7 H 0.4510 0.5207 0.3104 0.057 Uiso 1 1 calc R . .
C8 C 0.8313(3) 0.37250(12) 0.4733(2) 0.0451(7) Uani 1 1 d . . .
H8 H 0.9065 0.3919 0.4828 0.054 Uiso 1 1 calc R . .
C9 C 0.4647(3) 0.24727(11) 0.4651(2) 0.0412(7) Uani 1 1 d . . .
H9 H 0.5153 0.2410 0.5268 0.049 Uiso 1 1 calc R . .
C10 C 0.6957(3) 0.31521(12) 0.5284(2) 0.0440(7) Uani 1 1 d . . .
H10 H 0.6755 0.2950 0.5768 0.053 Uiso 1 1 calc R . .
C11 C 0.6166(3) 0.31517(10) 0.4376(2) 0.0346(6) Uani 1 1 d . . .
C12 C 0.3495(3) 0.48596(12) 0.3971(3) 0.0504(8) Uani 1 1 d . . .
C13 C 0.3216(3) 0.26883(11) 0.2879(2) 0.0401(7) Uani 1 1 d . . .
H13 H 0.2702 0.2764 0.2271 0.048 Uiso 1 1 calc R . .
C14 C 0.3525(3) 0.39887(12) 0.3755(2) 0.0467(8) Uani 1 1 d . . .
H14 H 0.3262 0.3675 0.3921 0.056 Uiso 1 1 calc R . .
C15 C 0.3168(4) 0.17724(13) 0.4868(3) 0.0582(9) Uani 1 1 d . . .
H15A H 0.3467 0.1837 0.5551 0.087 Uiso 1 1 calc R . .
H15B H 0.3553 0.1469 0.4702 0.087 Uiso 1 1 calc R . .
H15C H 0.2233 0.1740 0.4718 0.087 Uiso 1 1 calc R . .
C16 C 0.3138(4) 0.43944(13) 0.4195(3) 0.0550(9) Uani 1 1 d . . .
H16 H 0.2625 0.4354 0.4652 0.066 Uiso 1 1 calc R . .
C17 C 0.8886(4) 0.34776(15) 0.6484(3) 0.0612(10) Uani 1 1 d . . .
H17A H 0.9122 0.3147 0.6719 0.092 Uiso 1 1 calc R . .
H17B H 0.8411 0.3639 0.6908 0.092 Uiso 1 1 calc R . .
H17C H 0.9662 0.3665 0.6470 0.092 Uiso 1 1 calc R . .
C18 C 0.3082(5) 0.53135(15) 0.4431(3) 0.0757(13) Uani 1 1 d . . .
H18A H 0.2180 0.5383 0.4150 0.114 Uiso 1 1 calc R . .
H18B H 0.3609 0.5591 0.4322 0.114 Uiso 1 1 calc R . .
H18C H 0.3188 0.5259 0.5117 0.114 Uiso 1 1 calc R . .
S1 S 0.5000 0.18578(16) 0.7500 0.1328(11) Uani 1 2 d SU . .
C19 C 0.5000 0.1269(6) 0.7500 0.122(4) Uani 1 2 d SU . .
N4 N 0.5000 0.0843(7) 0.7500 0.222(7) Uani 1 2 d SU . .
C20 C -0.211(2) 0.0898(9) 0.185(2) 0.124(6) Uani 0.25 1 d PDU A 1
S2 S -0.3522(15) 0.0609(5) 0.1343(10) 0.200(5) Uani 0.25 1 d PDU A 1
N5 N -0.122(3) 0.1138(11) 0.225(4) 0.145(9) Uani 0.25 1 d PDU A 1
Cl1 Cl 0.0000 0.13156(12) 0.2500 0.1005(15) Uani 0.50 2 d SPDU . 2
O1 O 0.0184(15) 0.1551(5) 0.1726(9) 0.218(6) Uani 0.50 1 d PDU B 2
O2 O -0.1016(11) 0.1033(6) 0.2012(16) 0.185(7) Uani 0.50 1 d PDU C 2
O1W O 0.514(4) -0.0135(9) 0.728(4) 0.343(18) Uani 0.50 1 d PU . .
O2W O 0.522(2) 0.0173(9) 0.5641(15) 0.316(11) Uani 0.50 1 d PU . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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
N2 Fe1 N2 89.07(13) . 2_655
N2 Fe1 N1 96.01(9) . 2_655
N2 Fe1 N1 81.28(9) 2_655 2_655
N2 Fe1 N1 81.28(9) . .
N2 Fe1 N1 96.01(9) 2_655 .
N1 Fe1 N1 176.24(13) 2_655 .
N2 Fe1 N3 174.96(9) . 2_655
N2 Fe1 N3 94.96(9) 2_655 2_655
N1 Fe1 N3 87.60(9) 2_655 2_655
N1 Fe1 N3 95.26(9) . 2_655
N2 Fe1 N3 94.96(9) . .
N2 Fe1 N3 174.96(9) 2_655 .
N1 Fe1 N3 95.26(9) 2_655 .
N1 Fe1 N3 87.60(9) . .
N3 Fe1 N3 81.17(13) 2_655 .
C6 N1 C11 117.3(2) . .
C6 N1 Fe1 127.2(2) . .
C11 N1 Fe1 115.23(19) . .
C13 N2 C3 117.3(2) . .
C13 N2 Fe1 126.59(19) . .
C3 N2 Fe1 116.07(18) . .
C14 N3 C2 117.2(2) . .
C14 N3 Fe1 127.2(2) . .
C2 N3 Fe1 115.47(18) . .
C5 C1 C9 116.9(3) . .
C5 C1 C15 121.1(3) . .
C9 C1 C15 122.0(3) . .
N3 C2 C7 122.4(3) . .
N3 C2 C2 113.82(15) . 2_655
C7 C2 C2 123.82(18) . 2_655
N2 C3 C9 122.0(3) . .
N2 C3 C11 113.1(2) . .
C9 C3 C11 124.9(3) . .
C8 C4 C10 116.9(3) . .
C8 C4 C17 121.9(3) . .
C10 C4 C17 121.1(3) . .
C13 C5 C1 120.5(3) . .
C13 C5 H5 119.8 . .
C1 C5 H5 119.8 . .
N1 C6 C8 122.8(3) . .
N1 C6 H6 118.6 . .
C8 C6 H6 118.6 . .
C2 C7 C12 119.8(3) . .
C2 C7 H7 120.1 . .
C12 C7 H7 120.1 . .
C6 C8 C4 120.3(3) . .
C6 C8 H8 119.8 . .
C4 C8 H8 119.8 . .
C1 C9 C3 120.4(3) . .
C1 C9 H9 119.8 . .
C3 C9 H9 119.8 . .
C11 C10 C4 120.2(3) . .
C11 C10 H10 119.9 . .
C4 C10 H10 119.9 . .
N1 C11 C10 122.3(3) . .
N1 C11 C3 113.7(2) . .
C10 C11 C3 124.0(3) . .
C16 C12 C7 117.1(3) . .
C16 C12 C18 122.0(3) . .
C7 C12 C18 120.9(3) . .
N2 C13 C5 122.7(3) . .
N2 C13 H13 118.6 . .
C5 C13 H13 118.6 . .
N3 C14 C16 123.2(3) . .
N3 C14 H14 118.4 . .
C16 C14 H14 118.4 . .
C1 C15 H15A 109.5 . .
C1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 C12 120.3(3) . .
C14 C16 H16 119.8 . .
C12 C16 H16 119.8 . .
C4 C17 H17A 109.5 . .
C4 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C4 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C12 C18 H18A 109.5 . .
C12 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C12 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N4 C19 S1 180.000(2) . .
N5 C20 S2 172(3) . .
O1 Cl1 O1 122.3(14) 2 .
O1 Cl1 O2 116.6(11) 2 .
O1 Cl1 O2 95.1(13) . .
O1 Cl1 O2 95.1(13) 2 2
O1 Cl1 O2 116.6(11) . 2
O2 Cl1 O2 112.5(15) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.953(2) .
Fe1 N2 1.953(2) 2_655
Fe1 N1 1.962(2) 2_655
Fe1 N1 1.962(2) .
Fe1 N3 1.967(2) 2_655
Fe1 N3 1.967(2) .
N1 C6 1.342(4) .
N1 C11 1.355(4) .
N2 C13 1.344(4) .
N2 C3 1.357(4) .
N3 C14 1.339(4) .
N3 C2 1.349(3) .
C1 C5 1.382(5) .
C1 C9 1.385(4) .
C1 C15 1.498(4) .
C2 C7 1.383(4) .
C2 C2 1.467(5) 2_655
C3 C9 1.384(4) .
C3 C11 1.470(4) .
C4 C8 1.382(5) .
C4 C10 1.389(5) .
C4 C17 1.505(4) .
C5 C13 1.378(4) .
C5 H5 0.9400 .
C6 C8 1.377(4) .
C6 H6 0.9400 .
C7 C12 1.394(5) .
C7 H7 0.9400 .
C8 H8 0.9400 .
C9 H9 0.9400 .
C10 C11 1.379(4) .
C10 H10 0.9400 .
C12 C16 1.373(5) .
C12 C18 1.502(4) .
C13 H13 0.9400 .
C14 C16 1.372(4) .
C14 H14 0.9400 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 H15C 0.9700 .
C16 H16 0.9400 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 H17C 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 H18C 0.9700 .
S1 C19 1.595(15) .
C19 N4 1.154(17) .
C20 N5 1.180(11) .
C20 S2 1.708(10) .
Cl1 O1 1.324(9) 2
Cl1 O1 1.324(9) .
Cl1 O2 1.380(10) .
Cl1 O2 1.380(10) 2
O1W O1W 0.76(11) 2_656
