#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:16:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180032 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/26/7032608.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_7032608
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                 102.761(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4193(6)
_cell_length_b                   26.9922(11)
_cell_length_c                   14.3238(8)
_cell_measurement_reflns_used    6362
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.6060
_cell_measurement_theta_min      3.1580
_cell_volume                     3928.9(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      130(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0333
_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            19178
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.314
_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         1.030
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4292
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+26.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                3539
_reflns_number_total             4292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02587c2.cif
_cod_data_source_block           x-3
_cod_depositor_comments
'Adding full bibliography for 7032606--7032608.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7032608
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 0.34662(2) 0.2500 0.0267(2) Uani 1 2 d S . .
N1 N 0.6415(3) 0.34438(10) 0.3658(2) 0.0285(6) Uani 1 1 d . . .
N2 N 0.4274(3) 0.29487(10) 0.3193(2) 0.0278(6) Uani 1 1 d . . .
N3 N 0.4246(3) 0.40202(10) 0.3096(2) 0.0287(6) Uani 1 1 d . . .
C1 C 0.3506(4) 0.21894(13) 0.4281(3) 0.0363(9) Uani 1 1 d . . .
C2 C 0.4601(3) 0.44773(12) 0.2863(2) 0.0276(7) Uani 1 1 d . . .
C3 C 0.4980(4) 0.28427(12) 0.4078(3) 0.0304(8) Uani 1 1 d . . .
C4 C 0.8088(4) 0.34494(14) 0.5487(3) 0.0378(9) Uani 1 1 d . . .
C5 C 0.2775(4) 0.23074(14) 0.3384(3) 0.0382(9) Uani 1 1 d . . .
H5 H 0.1993 0.2128 0.3121 0.046 Uiso 1 1 calc R . .
C6 C 0.7516(4) 0.37177(13) 0.3851(3) 0.0332(8) Uani 1 1 d . . .
H6 H 0.7724 0.3913 0.3354 0.040 Uiso 1 1 calc R . .
C7 C 0.4244(4) 0.49016(13) 0.3290(3) 0.0347(8) Uani 1 1 d . . .
H7 H 0.4520 0.5217 0.3115 0.042 Uiso 1 1 calc R . .
C8 C 0.8355(4) 0.37278(14) 0.4734(3) 0.0387(9) Uani 1 1 d . . .
H8 H 0.9126 0.3926 0.4833 0.046 Uiso 1 1 calc R . .
C9 C 0.4620(4) 0.24684(13) 0.4638(3) 0.0345(8) Uani 1 1 d . . .
H9 H 0.5135 0.2405 0.5262 0.041 Uiso 1 1 calc R . .
C10 C 0.6974(4) 0.31508(14) 0.5280(3) 0.0378(9) Uani 1 1 d . . .
H10 H 0.6764 0.2946 0.5765 0.045 Uiso 1 1 calc R . .
C11 C 0.6173(4) 0.31510(12) 0.4374(3) 0.0306(8) Uani 1 1 d . . .
C12 C 0.3486(4) 0.48670(14) 0.3971(3) 0.0380(9) Uani 1 1 d . . .
C13 C 0.3180(4) 0.26865(13) 0.2864(3) 0.0343(8) Uani 1 1 d . . .
H13 H 0.2659 0.2763 0.2249 0.041 Uiso 1 1 calc R . .
C14 C 0.3497(4) 0.39906(14) 0.3744(3) 0.0415(10) Uani 1 1 d . . .
H14 H 0.3222 0.3672 0.3905 0.050 Uiso 1 1 calc R . .
C15 C 0.3111(5) 0.17666(14) 0.4845(3) 0.0459(10) Uani 1 1 d . . .
H15A H 0.3471 0.1821 0.5529 0.069 Uiso 1 1 calc R . .
H15B H 0.3455 0.1455 0.4647 0.069 Uiso 1 1 calc R . .
H15C H 0.2149 0.1749 0.4725 0.069 Uiso 1 1 calc R . .
C16 C 0.3110(4) 0.43969(14) 0.4186(3) 0.0439(10) Uani 1 1 d . . .
H16 H 0.2580 0.4355 0.4642 0.053 Uiso 1 1 calc R . .
C17 C 0.8926(5) 0.34792(17) 0.6486(3) 0.0497(11) Uani 1 1 d . . .
H17A H 0.9185 0.3145 0.6720 0.075 Uiso 1 1 calc R . .
H17B H 0.8423 0.3636 0.6909 0.075 Uiso 1 1 calc R . .
H17C H 0.9715 0.3676 0.6481 0.075 Uiso 1 1 calc R . .
C18 C 0.3075(5) 0.53231(16) 0.4429(4) 0.0532(12) Uani 1 1 d . . .
H18A H 0.2166 0.5407 0.4119 0.080 Uiso 1 1 calc R . .
H18B H 0.3656 0.5599 0.4356 0.080 Uiso 1 1 calc R . .
H18C H 0.3135 0.5261 0.5111 0.080 Uiso 1 1 calc R . .
S1 S 0.5000 0.17995(11) 0.7500 0.0825(7) Uani 1 2 d SU . .
C19 C 0.5000 0.1209(5) 0.7500 0.101(3) Uani 1 2 d SU . .
N4 N 0.5000 0.0776(6) 0.7500 0.177(5) Uani 1 2 d SU . .
C20 C -0.199(2) 0.0941(10) 0.191(3) 0.115(7) Uani 0.25 1 d PDU A 1
S2 S -0.3406(17) 0.0654(5) 0.1379(11) 0.185(5) Uani 0.25 1 d PDU A 1
N5 N -0.102(4) 0.113(2) 0.233(4) 0.151(10) Uani 0.25 1 d PDU A 1
Cl1 Cl 0.0000 0.13099(11) 0.2500 0.0724(15) Uani 0.50 2 d SPDU . 2
O1 O 0.0208(14) 0.1570(5) 0.1755(8) 0.180(6) Uani 0.50 1 d PDU B 2
O2 O -0.1063(14) 0.1027(6) 0.1976(14) 0.192(7) Uani 0.50 1 d PDU C 2
O1W O 0.500(6) -0.0172(7) 0.772(4) 0.253(14) Uani 0.50 1 d PU . .
O2W O 0.5434(19) 0.0123(8) 0.5734(14) 0.241(9) 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 89.05(16) 2_655 .
N2 Fe1 N1 81.49(12) 2_655 2_655
N2 Fe1 N1 95.97(12) . 2_655
N2 Fe1 N1 95.97(12) 2_655 .
N2 Fe1 N1 81.49(12) . .
N1 Fe1 N1 176.46(16) 2_655 .
N2 Fe1 N3 175.15(12) 2_655 .
N2 Fe1 N3 94.94(11) . .
N1 Fe1 N3 95.32(12) 2_655 .
N1 Fe1 N3 87.38(12) . .
N2 Fe1 N3 94.94(11) 2_655 2_655
N2 Fe1 N3 175.15(12) . 2_655
N1 Fe1 N3 87.38(12) 2_655 2_655
N1 Fe1 N3 95.32(12) . 2_655
N3 Fe1 N3 81.22(16) . 2_655
C6 N1 C11 117.1(3) . .
C6 N1 Fe1 127.3(3) . .
C11 N1 Fe1 115.2(2) . .
C13 N2 C3 117.7(3) . .
C13 N2 Fe1 126.5(2) . .
C3 N2 Fe1 115.8(2) . .
C14 N3 C2 117.3(3) . .
C14 N3 Fe1 127.2(2) . .
C2 N3 Fe1 115.4(2) . .
C5 C1 C9 117.7(3) . .
C5 C1 C15 121.0(4) . .
C9 C1 C15 121.4(4) . .
N3 C2 C7 122.1(3) . .
N3 C2 C2 113.83(18) . 2_655
C7 C2 C2 124.1(2) . 2_655
N2 C3 C9 122.4(3) . .
N2 C3 C11 113.6(3) . .
C9 C3 C11 124.0(3) . .
C10 C4 C8 116.6(4) . .
C10 C4 C17 121.0(4) . .
C8 C4 C17 122.3(4) . .
C1 C5 C13 120.0(4) . .
C1 C5 H5 120.0 . .
C13 C5 H5 120.0 . .
N1 C6 C8 123.0(4) . .
N1 C6 H6 118.5 . .
C8 C6 H6 118.5 . .
C2 C7 C12 120.2(3) . .
C2 C7 H7 119.9 . .
C12 C7 H7 119.9 . .
C6 C8 C4 120.6(4) . .
C6 C8 H8 119.7 . .
C4 C8 H8 119.7 . .
C1 C9 C3 119.5(4) . .
C1 C9 H9 120.2 . .
C3 C9 H9 120.2 . .
C11 C10 C4 120.2(4) . .
C11 C10 H10 119.9 . .
C4 C10 H10 119.9 . .
N1 C11 C10 122.3(3) . .
N1 C11 C3 113.2(3) . .
C10 C11 C3 124.5(3) . .
C16 C12 C7 116.9(3) . .
C16 C12 C18 122.2(3) . .
C7 C12 C18 120.9(4) . .
N2 C13 C5 122.7(4) . .
N2 C13 H13 118.7 . .
C5 C13 H13 118.7 . .
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(1) . .
N5 C20 S2 176(4) . .
O1 Cl1 O1 116.6(13) 2 .
O1 Cl1 O2 117.5(11) 2 .
O1 Cl1 O2 96.0(11) . .
O1 Cl1 O2 96.0(11) 2 2
O1 Cl1 O2 117.5(11) . 2
O2 Cl1 O2 114.8(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 1.959(3) 2_655
Fe1 N2 1.959(3) .
Fe1 N1 1.961(3) 2_655
Fe1 N1 1.961(3) .
Fe1 N3 1.969(3) .
Fe1 N3 1.969(3) 2_655
N1 C6 1.342(5) .
N1 C11 1.362(4) .
N2 C13 1.336(5) .
N2 C3 1.349(5) .
N3 C14 1.340(4) .
N3 C2 1.351(4) .
C1 C5 1.379(6) .
C1 C9 1.383(6) .
C1 C15 1.507(5) .
C2 C7 1.387(5) .
C2 C2 1.468(6) 2_655
C3 C9 1.393(5) .
C3 C11 1.478(5) .
C4 C10 1.390(6) .
C4 C8 1.393(6) .
C4 C17 1.505(6) .
C5 C13 1.385(5) .
C5 H5 0.9500 .
C6 C8 1.369(6) .
C6 H6 0.9500 .
C7 C12 1.388(5) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 H9 0.9500 .
C10 C11 1.379(5) .
C10 H10 0.9500 .
C12 C16 1.383(5) .
C12 C18 1.501(5) .
C13 H13 0.9500 .
C14 C16 1.370(5) .
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16 0.9500 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
S1 C19 1.595(13) .
C19 N4 1.168(15) .
C20 N5 1.168(11) .
C20 S2 1.693(11) .
Cl1 O1 1.335(10) 2
Cl1 O1 1.335(10) .
Cl1 O2 1.416(10) .
Cl1 O2 1.416(10) 2
O1W O1W 0.63(10) 2_656
