#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:49:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179865 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/61/7016195.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_7016195
loop_
_publ_author_name
'González-Prieto, Rodrigo'
'Fleury, Benoit'
'Schramm, Frank'
'Zoppellaro, Giorgio'
'Chandrasekar, Rajadurai'
'Fuhr, Olaf'
'Lebedkin, Sergei'
'Kappes, Manfred'
'Ruben, Mario'
_publ_section_title
;
 Tuning the spin-transition properties of pyrene-decorated
 2,6-bispyrazolylpyridine based Fe(ii) complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7564
_journal_page_last               7570
_journal_paper_doi               10.1039/c1dt10420a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C54 H34 Cl2 Fe N10 O8'
_chemical_formula_weight         1077.66
_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                 100.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.180(3)
_cell_length_b                   8.3692(17)
_cell_length_c                   36.505(7)
_cell_measurement_temperature    180(2)
_cell_volume                     4557.3(16)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6333
_diffrn_reflns_theta_full        23.64
_diffrn_reflns_theta_max         23.64
_diffrn_reflns_theta_min         2.73
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.9869
_exptl_absorpt_correction_T_min  0.9123
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0806P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                2169
_reflns_number_total             3259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10420a.txt
_cod_data_source_block           790319
_cod_original_cell_volume        4557.2(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7016195
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 0.0000 0.41926(10) 0.2500 0.0465(3) Uani 1 2 d S . .
N1 N -0.0493(2) 0.5938(4) 0.28433(11) 0.0524(9) Uani 1 1 d . . .
N2 N -0.0373(2) 0.5545(4) 0.32136(11) 0.0506(9) Uani 1 1 d . . .
N3 N 0.0483(2) 0.3525(4) 0.30647(10) 0.0479(9) Uani 1 1 d . . .
N4 N 0.1364(2) 0.1691(4) 0.28432(11) 0.0486(9) Uani 1 1 d . . .
N5 N 0.1092(2) 0.2449(4) 0.25104(11) 0.0505(9) Uani 1 1 d . . .
C1 C -0.0863(3) 0.7384(5) 0.28190(15) 0.0573(12) Uani 1 1 d . . .
H1 H -0.1025 0.7974 0.2594 0.069 Uiso 1 1 calc R . .
C2 C -0.0981(3) 0.7923(6) 0.31719(15) 0.0609(12) Uani 1 1 d . . .
H2 H -0.1238 0.8908 0.3227 0.073 Uiso 1 1 calc R . .
C3 C -0.0655(3) 0.6750(5) 0.34177(14) 0.0561(12) Uani 1 1 d . . .
H3 H -0.0627 0.6765 0.3680 0.067 Uiso 1 1 calc R . .
C4 C 0.0121(3) 0.4160(5) 0.33364(13) 0.0494(10) Uani 1 1 d . . .
C5 C 0.0210(3) 0.3529(5) 0.36898(13) 0.0526(11) Uani 1 1 d . . .
H5 H -0.0072 0.4019 0.3873 0.063 Uiso 1 1 calc R . .
C6 C 0.0725(3) 0.2154(6) 0.37717(13) 0.0533(11) Uani 1 1 d . . .
C7 C 0.1127(3) 0.1472(5) 0.34939(13) 0.0531(11) Uani 1 1 d . . .
H7 H 0.1484 0.0535 0.3540 0.064 Uiso 1 1 calc R . .
C8 C 0.0986(3) 0.2210(5) 0.31495(13) 0.0484(10) Uani 1 1 d . . .
C9 C 0.2013(3) 0.0589(5) 0.28258(14) 0.0525(11) Uani 1 1 d . . .
H9 H 0.2302 -0.0080 0.3022 0.063 Uiso 1 1 calc R . .
C10 C 0.2166(3) 0.0640(5) 0.24670(14) 0.0546(11) Uani 1 1 d . . .
H10 H 0.2587 0.0019 0.2366 0.066 Uiso 1 1 calc R . .
C11 C 0.1579(3) 0.1789(5) 0.22793(14) 0.0522(11) Uani 1 1 d . . .
H11 H 0.1533 0.2062 0.2024 0.063 Uiso 1 1 calc R . .
C12 C 0.0843(3) 0.1368(6) 0.41408(14) 0.0570(12) Uani 1 1 d . . .
C13 C 0.0719(3) -0.0285(6) 0.41457(14) 0.0606(12) Uani 1 1 d . . .
H13 H 0.0581 -0.0857 0.3917 0.073 Uiso 1 1 calc R . .
C14 C 0.0796(3) -0.1099(6) 0.44813(16) 0.0653(13) Uani 1 1 d . . .
H14 H 0.0703 -0.2222 0.4479 0.078 Uiso 1 1 calc R . .
C15 C 0.1008(3) -0.0301(6) 0.48210(14) 0.0597(12) Uani 1 1 d . . .
C16 C 0.1088(3) -0.1122(7) 0.51728(16) 0.0697(14) Uani 1 1 d . . .
H16 H 0.0984 -0.2241 0.5174 0.084 Uiso 1 1 calc R . .
C17 C 0.1307(3) -0.0348(7) 0.54974(16) 0.0696(14) Uani 1 1 d . . .
H17 H 0.1354 -0.0929 0.5724 0.084 Uiso 1 1 calc R . .
C18 C 0.1471(3) 0.1339(6) 0.55109(15) 0.0639(13) Uani 1 1 d . . .
C19 C 0.1710(3) 0.2171(7) 0.58472(15) 0.0682(14) Uani 1 1 d . . .
H19 H 0.1774 0.1610 0.6077 0.082 Uiso 1 1 calc R . .
C20 C 0.1855(3) 0.3813(7) 0.58490(15) 0.0680(14) Uani 1 1 d . . .
H20 H 0.1995 0.4365 0.6080 0.082 Uiso 1 1 calc R . .
C21 C 0.1799(3) 0.4645(7) 0.55209(16) 0.0686(14) Uani 1 1 d . . .
H21 H 0.1915 0.5761 0.5528 0.082 Uiso 1 1 calc R . .
C22 C 0.1571(3) 0.3866(6) 0.51731(14) 0.0594(12) Uani 1 1 d . . .
C23 C 0.1547(3) 0.4654(6) 0.48267(15) 0.0599(12) Uani 1 1 d . . .
H23 H 0.1704 0.5753 0.4827 0.072 Uiso 1 1 calc R . .
C24 C 0.1309(3) 0.3897(6) 0.44974(15) 0.0601(12) Uani 1 1 d . . .
H24 H 0.1292 0.4481 0.4273 0.072 Uiso 1 1 calc R . .
C25 C 0.1080(3) 0.2225(6) 0.44763(14) 0.0580(12) Uani 1 1 d . . .
C26 C 0.1159(3) 0.1373(6) 0.48237(14) 0.0555(11) Uani 1 1 d . . .
C27 C 0.1395(3) 0.2195(6) 0.51677(14) 0.0590(12) Uani 1 1 d . . .
Cl1 Cl 0.20770(7) 0.68114(14) 0.34677(4) 0.0593(3) Uani 1 1 d . . .
O1 O 0.2471(3) 0.5327(4) 0.33933(12) 0.0834(12) Uani 1 1 d . . .
O2 O 0.2755(2) 0.8038(5) 0.35288(12) 0.0823(11) Uani 1 1 d . . .
O3 O 0.1664(3) 0.6644(5) 0.37852(13) 0.0930(13) Uani 1 1 d . . .
O4 O 0.1420(2) 0.7255(5) 0.31509(13) 0.0882(12) Uani 1 1 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'
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'
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
_geom_angle_publ_flag
N3 Fe1 N3 149.58(19) 2 . ?
N3 Fe1 N1 130.42(13) 2 . ?
N3 Fe1 N1 73.05(13) . . ?
N3 Fe1 N1 73.05(13) 2 2 ?
N3 Fe1 N1 130.42(13) . 2 ?
N1 Fe1 N1 94.3(2) . 2 ?
N3 Fe1 N5 88.02(14) 2 . ?
N3 Fe1 N5 71.76(13) . . ?
N1 Fe1 N5 141.54(14) . . ?
N1 Fe1 N5 96.79(13) 2 . ?
N3 Fe1 N5 71.75(13) 2 2 ?
N3 Fe1 N5 88.03(14) . 2 ?
N1 Fe1 N5 96.79(13) . 2 ?
N1 Fe1 N5 141.54(14) 2 2 ?
N5 Fe1 N5 97.02(18) . 2 ?
C1 N1 N2 105.2(4) . . ?
C1 N1 Fe1 140.2(3) . . ?
N2 N1 Fe1 114.5(3) . . ?
C3 N2 N1 111.2(4) . . ?
C3 N2 C4 129.4(4) . . ?
N1 N2 C4 118.5(3) . . ?
C4 N3 C8 116.8(4) . . ?
C4 N3 Fe1 120.1(3) . . ?
C8 N3 Fe1 121.1(3) . . ?
C9 N4 N5 112.1(3) . . ?
C9 N4 C8 130.4(4) . . ?
N5 N4 C8 117.4(3) . . ?
C11 N5 N4 104.9(3) . . ?
C11 N5 Fe1 139.8(3) . . ?
N4 N5 Fe1 115.2(2) . . ?
N1 C1 C2 110.7(4) . . ?
C3 C2 C1 106.3(4) . . ?
C2 C3 N2 106.6(4) . . ?
N3 C4 C5 124.2(4) . . ?
N3 C4 N2 111.1(4) . . ?
C5 C4 N2 124.6(4) . . ?
C4 C5 C6 118.2(4) . . ?
C5 C6 C7 119.0(4) . . ?
C5 C6 C12 122.1(4) . . ?
C7 C6 C12 118.9(4) . . ?
C8 C7 C6 117.5(4) . . ?
N3 C8 C7 124.2(4) . . ?
N3 C8 N4 111.4(4) . . ?
C7 C8 N4 124.3(4) . . ?
N4 C9 C10 106.0(4) . . ?
C9 C10 C11 106.5(4) . . ?
N5 C11 C10 110.5(4) . . ?
C13 C12 C25 120.4(5) . . ?
C13 C12 C6 117.3(4) . . ?
C25 C12 C6 122.3(4) . . ?
C14 C13 C12 120.6(5) . . ?
C13 C14 C15 121.2(5) . . ?
C14 C15 C26 119.3(4) . . ?
C14 C15 C16 122.2(5) . . ?
C26 C15 C16 118.5(5) . . ?
C17 C16 C15 121.7(5) . . ?
C16 C17 C18 121.4(5) . . ?
C19 C18 C27 119.0(5) . . ?
C19 C18 C17 122.4(5) . . ?
C27 C18 C17 118.6(5) . . ?
C20 C19 C18 120.7(5) . . ?
C21 C20 C19 120.8(5) . . ?
C20 C21 C22 121.0(5) . . ?
C21 C22 C23 123.2(5) . . ?
C21 C22 C27 118.7(5) . . ?
C23 C22 C27 118.0(5) . . ?
C24 C23 C22 122.3(5) . . ?
C23 C24 C25 121.8(5) . . ?
C12 C25 C26 118.7(4) . . ?
C12 C25 C24 124.1(4) . . ?
C26 C25 C24 117.0(5) . . ?
C27 C26 C15 119.9(4) . . ?
C27 C26 C25 120.4(4) . . ?
C15 C26 C25 119.7(5) . . ?
C26 C27 C22 120.3(4) . . ?
C26 C27 C18 120.0(5) . . ?
C22 C27 C18 119.7(5) . . ?
O3 Cl1 O1 109.4(2) . . ?
O3 Cl1 O4 109.7(3) . . ?
O1 Cl1 O4 109.1(3) . . ?
O3 Cl1 O2 110.7(3) . . ?
O1 Cl1 O2 109.7(2) . . ?
O4 Cl1 O2 108.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.130(4) 2 ?
Fe1 N3 2.130(4) . ?
Fe1 N1 2.148(4) . ?
Fe1 N1 2.148(4) 2 ?
Fe1 N5 2.203(4) . ?
Fe1 N5 2.203(4) 2 ?
N1 C1 1.330(6) . ?
N1 N2 1.370(5) . ?
N2 C3 1.369(6) . ?
N2 C4 1.408(5) . ?
N3 C4 1.331(5) . ?
N3 C8 1.342(5) . ?
N4 C9 1.360(5) . ?
N4 N5 1.365(5) . ?
N4 C8 1.416(6) . ?
N5 C11 1.340(5) . ?
C1 C2 1.407(7) . ?
C2 C3 1.360(7) . ?
C4 C5 1.377(6) . ?
C5 C6 1.392(6) . ?
C6 C7 1.398(6) . ?
C6 C12 1.480(7) . ?
C7 C8 1.381(6) . ?
C9 C10 1.373(7) . ?
C10 C11 1.400(6) . ?
C12 C13 1.397(7) . ?
C12 C25 1.407(7) . ?
C13 C14 1.387(7) . ?
C14 C15 1.393(7) . ?
C15 C26 1.420(7) . ?
C15 C16 1.441(7) . ?
C16 C17 1.337(8) . ?
C17 C18 1.433(7) . ?
C18 C19 1.400(7) . ?
C18 C27 1.429(7) . ?
C19 C20 1.391(7) . ?
C20 C21 1.374(7) . ?
C21 C22 1.412(7) . ?
C22 C23 1.421(7) . ?
C22 C27 1.424(7) . ?
C23 C24 1.348(7) . ?
C24 C25 1.441(7) . ?
C25 C26 1.440(7) . ?
C26 C27 1.418(7) . ?
Cl1 O3 1.423(4) . ?
Cl1 O1 1.427(3) . ?
Cl1 O4 1.429(4) . ?
Cl1 O2 1.441(4) . ?
