#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:16:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180032 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/26/7032606.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_7032606
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
'4(C36 H36 Fe N6), 4(Cl O4), 3(C N S), 12(O), Cl'
_chemical_formula_sum            'C147 H144 Cl5 Fe4 N27 O28 S3'
_chemical_formula_weight         3233.72
_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                 102.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.771(2)
_cell_length_b                   27.332(8)
_cell_length_c                   14.263(3)
_cell_measurement_reflns_used    6362
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.6060
_cell_measurement_theta_min      3.1580
_cell_volume                     4098.0(17)
_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      300(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1436
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17634
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3620
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0889
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0893P)²+17.8097P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2421
_reflns_number_gt                2091
_reflns_number_total             3620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02587c2.cif
_cod_data_source_block           x-1
_cod_depositor_comments
'Adding full bibliography for 7032606--7032608.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7032606
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 0.34707(4) 0.2500 0.0374(4) Uani 1 2 d S . .
N1 N 0.6375(5) 0.34457(18) 0.3657(3) 0.0416(12) Uani 1 1 d . . .
N2 N 0.4299(5) 0.29601(17) 0.3202(4) 0.0418(13) Uani 1 1 d . . .
N3 N 0.4280(5) 0.40185(18) 0.3106(3) 0.0434(13) Uani 1 1 d . . .
C1 C 0.3575(7) 0.2207(2) 0.4297(5) 0.0548(18) Uani 1 1 d . . .
C2 C 0.4626(6) 0.4475(2) 0.2864(4) 0.0445(15) Uani 1 1 d . . .
C3 C 0.4997(6) 0.2850(2) 0.4089(4) 0.0419(15) Uani 1 1 d . . .
C4 C 0.8015(7) 0.3438(3) 0.5485(5) 0.0561(18) Uani 1 1 d . . .
C5 C 0.2849(7) 0.2326(2) 0.3404(6) 0.0597(19) Uani 1 1 d . . .
H5 H 0.2105 0.2155 0.3155 0.072 Uiso 1 1 calc R . .
C6 C 0.7438(6) 0.3714(2) 0.3849(5) 0.0509(17) Uani 1 1 d . . .
H6 H 0.7627 0.3908 0.3363 0.061 Uiso 1 1 calc R . .
C7 C 0.4256(7) 0.4893(3) 0.3273(5) 0.064(2) Uani 1 1 d . . .
H7 H 0.4495 0.5198 0.3085 0.076 Uiso 1 1 calc R . .
C8 C 0.8269(7) 0.3716(3) 0.4736(5) 0.0559(18) Uani 1 1 d . . .
H8 H 0.9004 0.3905 0.4831 0.067 Uiso 1 1 calc R . .
C9 C 0.4639(7) 0.2479(2) 0.4643(5) 0.0528(18) Uani 1 1 d . . .
H9 H 0.5128 0.2415 0.5253 0.063 Uiso 1 1 calc R . .
C10 C 0.6933(7) 0.3148(3) 0.5282(5) 0.0544(18) Uani 1 1 d . . .
H10 H 0.6735 0.2949 0.5759 0.065 Uiso 1 1 calc R . .
C11 C 0.6148(6) 0.3152(2) 0.4375(4) 0.0433(15) Uani 1 1 d . . .
C12 C 0.3511(8) 0.4859(3) 0.3980(5) 0.069(2) Uani 1 1 d . . .
C13 C 0.3233(7) 0.2702(2) 0.2882(5) 0.0509(17) Uani 1 1 d . . .
H13 H 0.2730 0.2778 0.2283 0.061 Uiso 1 1 calc R . .
C14 C 0.3553(7) 0.3992(3) 0.3765(5) 0.059(2) Uani 1 1 d . . .
H14 H 0.3297 0.3685 0.3932 0.070 Uiso 1 1 calc R . .
C15 C 0.3197(9) 0.1775(3) 0.4863(6) 0.082(3) Uani 1 1 d . . .
H15A H 0.3663 0.1791 0.5518 0.123 Uiso 1 1 calc R . .
H15B H 0.3392 0.1473 0.4580 0.123 Uiso 1 1 calc R . .
H15C H 0.2302 0.1789 0.4844 0.123 Uiso 1 1 calc R . .
C16 C 0.3173(8) 0.4396(3) 0.4200(6) 0.071(2) Uani 1 1 d . . .
H16 H 0.2677 0.4356 0.4653 0.085 Uiso 1 1 calc R . .
C17 C 0.8837(8) 0.3464(3) 0.6485(5) 0.080(2) Uani 1 1 d . . .
H17A H 0.9124 0.3141 0.6693 0.121 Uiso 1 1 calc R . .
H17B H 0.8352 0.3597 0.6915 0.121 Uiso 1 1 calc R . .
H17C H 0.9558 0.3670 0.6483 0.121 Uiso 1 1 calc R . .
C18 C 0.3121(10) 0.5306(3) 0.4439(7) 0.098(3) Uani 1 1 d . . .
H18A H 0.2309 0.5416 0.4080 0.146 Uiso 1 1 calc R . .
H18B H 0.3742 0.5559 0.4448 0.146 Uiso 1 1 calc R . .
H18C H 0.3060 0.5232 0.5085 0.146 Uiso 1 1 calc R . .
Cl1 Cl 0.0000 0.13156(13) 0.2500 0.1204(16) Uani 1 2 d SDU . .
O1 O -0.1106(9) 0.1052(3) 0.2171(11) 0.240(6) Uani 1 1 d DU . .
O2 O 0.0163(13) 0.1685(5) 0.1835(9) 0.274(7) Uani 1 1 d DU . .
S1 S 0.5000 0.1840(7) 0.7500 0.192(6) Uani 0.75 2 d SPDU A 1
N4 N 0.5000 0.0786(8) 0.7500 0.224(10) Uani 0.75 2 d SPDU A 1
C19 C 0.5000 0.1204(7) 0.7500 0.120(7) Uani 0.75 2 d SPDU A 1
Cl2 Cl 0.5000 0.1734(11) 0.7500 0.109(8) Uani 0.25 2 d SPDU . 2
O3 O 0.599(3) 0.1393(12) 0.793(2) 0.155(10) Uani 0.25 1 d PDU B 2
O4 O 0.471(3) 0.2019(13) 0.8285(17) 0.171(11) Uani 0.25 1 d PDU C 2
O1W O 0.3508(16) 0.0598(7) 0.3663(12) 0.155(6) Uani 0.50 1 d PU . .
O2W O 0.512(3) 0.0201(14) 0.554(3) 0.169(9) Uani 0.25 1 d PU . .
O3W O 0.5000 -0.0107(12) 0.7500 0.201(9) Uani 0.50 2 d SPU . .
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
N1 Fe1 N1 176.0(3) 2_655 .
N1 Fe1 N2 95.8(2) 2_655 .
N1 Fe1 N2 81.4(2) . .
N1 Fe1 N2 81.4(2) 2_655 2_655
N1 Fe1 N2 95.8(2) . 2_655
N2 Fe1 N2 89.3(3) . 2_655
N1 Fe1 N3 87.4(2) 2_655 2_655
N1 Fe1 N3 95.6(2) . 2_655
N2 Fe1 N3 175.1(2) . 2_655
N2 Fe1 N3 94.85(19) 2_655 2_655
N1 Fe1 N3 95.6(2) 2_655 .
N1 Fe1 N3 87.4(2) . .
N2 Fe1 N3 94.85(19) . .
N2 Fe1 N3 175.1(2) 2_655 .
N3 Fe1 N3 81.1(3) 2_655 .
C6 N1 C11 117.0(5) . .
C6 N1 Fe1 127.5(4) . .
C11 N1 Fe1 115.2(4) . .
C13 N2 C3 117.4(5) . .
C13 N2 Fe1 126.7(4) . .
C3 N2 Fe1 115.9(4) . .
C14 N3 C2 117.2(5) . .
C14 N3 Fe1 127.4(4) . .
C2 N3 Fe1 115.3(4) . .
C9 C1 C5 117.9(6) . .
C9 C1 C15 121.8(7) . .
C5 C1 C15 120.3(7) . .
N3 C2 C7 121.9(6) . .
N3 C2 C2 114.0(3) . 2_655
C7 C2 C2 124.1(4) . 2_655
N2 C3 C9 121.7(6) . .
N2 C3 C11 113.3(5) . .
C9 C3 C11 125.0(6) . .
C8 C4 C10 116.8(6) . .
C8 C4 C17 122.0(7) . .
C10 C4 C17 121.1(7) . .
C1 C5 C13 119.7(7) . .
C1 C5 H5 120.1 . .
C13 C5 H5 120.1 . .
N1 C6 C8 123.0(6) . .
N1 C6 H6 118.5 . .
C8 C6 H6 118.5 . .
C2 C7 C12 120.3(7) . .
C2 C7 H7 119.8 . .
C12 C7 H7 119.8 . .
C6 C8 C4 120.4(7) . .
C6 C8 H8 119.8 . .
C4 C8 H8 119.8 . .
C1 C9 C3 120.4(7) . .
C1 C9 H9 119.8 . .
C3 C9 H9 119.8 . .
C11 C10 C4 120.3(6) . .
C11 C10 H10 119.9 . .
C4 C10 H10 119.9 . .
N1 C11 C10 122.3(6) . .
N1 C11 C3 113.6(5) . .
C10 C11 C3 124.1(6) . .
C16 C12 C7 116.3(6) . .
C16 C12 C18 122.7(7) . .
C7 C12 C18 121.0(7) . .
N2 C13 C5 122.8(7) . .
N2 C13 H13 118.6 . .
C5 C13 H13 118.6 . .
N3 C14 C16 123.1(6) . .
N3 C14 H14 118.5 . .
C16 C14 H14 118.5 . .
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 121.2(7) . .
C14 C16 H16 119.4 . .
C12 C16 H16 119.4 . .
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 . .
O1 Cl1 O1 117.2(9) . 2
O1 Cl1 O2 111.9(8) . 2
O1 Cl1 O2 111.4(8) 2 2
O1 Cl1 O2 111.4(8) . .
O1 Cl1 O2 111.9(8) 2 .
O2 Cl1 O2 89.5(13) 2 .
N4 C19 S1 180.000(2) . .
O3 Cl2 O3 100(4) 2_656 .
O3 Cl2 O4 114(2) 2_656 .
O3 Cl2 O4 106.4(11) . .
O3 Cl2 O4 106.4(11) 2_656 2_656
O3 Cl2 O4 114(2) . 2_656
O4 Cl2 O4 115(3) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.964(5) 2_655
Fe1 N1 1.964(5) .
Fe1 N2 1.962(5) .
Fe1 N2 1.962(5) 2_655
Fe1 N3 1.971(5) 2_655
Fe1 N3 1.971(5) .
N1 C6 1.336(8) .
N1 C11 1.365(7) .
N2 C13 1.340(8) .
N2 C3 1.358(7) .
N3 C14 1.350(7) .
N3 C2 1.368(7) .
C1 C9 1.364(10) .
C1 C5 1.380(10) .
C1 C15 1.536(9) .
C2 C7 1.380(8) .
C2 C2 1.447(11) 2_655
C3 C9 1.390(8) .
C3 C11 1.471(9) .
C4 C8 1.385(9) .
C4 C10 1.387(10) .
C4 C17 1.507(9) .
C5 C13 1.383(9) .
C5 H5 0.9300 .
C6 C8 1.381(9) .
C6 H6 0.9300 .
C7 C12 1.421(10) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C11 1.383(9) .
C10 H10 0.9300 .
C12 C16 1.371(10) .
C12 C18 1.491(10) .
C13 H13 0.9300 .
C14 C16 1.374(9) .
C14 H14 0.9300 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16 0.9300 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
Cl1 O1 1.384(7) .
Cl1 O1 1.384(7) 2
Cl1 O2 1.423(8) 2
Cl1 O2 1.423(8) .
S1 C19 1.736(10) .
N4 C19 1.142(10) .
Cl2 O3 1.448(10) 2_656
Cl2 O3 1.448(10) .
Cl2 O4 1.454(10) .
Cl2 O4 1.454(10) 2_656
