#------------------------------------------------------------------------------
#$Date: 2019-11-28 12:40:12 +0100 (jue 28 de nov de 2019) $
#$Revision: 243882 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/24/7702497.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_7702497
loop_
_publ_author_name
'Pascaly, Matthias'
'Duda, Mark'
'Schweppe, Florian'
'Zurlinden, Kristin'
'Müller, Felizitas K.'
'Krebs, Bernt'
_publ_section_title
;
 The systematic influence of tripodal ligands on the catechol cleaving
 activity of iron(III) containing model compounds for catechol
 1,2-dioxygenases †
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              828
_journal_paper_doi               10.1039/b008511l
_journal_year                    2001
_chemical_formula_moiety         '[Fe(bpqa)tcc]ClO4*CH3CH2OH'
_chemical_formula_sum            'C30 H26 Cl5 Fe N4 O7'
_chemical_formula_weight         787.65
_chemical_melting_point          '242 &#x00B0;C'
_chemical_name_systematic
; 
(Tetrachlorocatecholato-O,O')-(bis((2-pyridyl)methyl)
((2-quinolyl)methyl)amine)-iron(III) perchlorate ethanol solvate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.553(2)
_cell_length_b                   17.660(4)
_cell_length_c                   20.095(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3314.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P3'
_diffrn_measurement_method       ω-scan
_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  0.0842
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12000
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0850
_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)+(0.1062P)²+8.0277P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2347
_reflns_number_gt                3801
_reflns_number_total             5824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008511l.txt
_cod_data_source_block           3
_cod_original_cell_volume        3314.5(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7702497
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.08642(10) 0.21728(5) 0.14624(5) 0.0391(3) Uani 1 1 d .
N1 N 0.3090(6) 0.1807(3) 0.1803(3) 0.0440(15) Uani 1 1 d .
N2 N 0.0813(7) 0.0981(3) 0.1214(3) 0.0478(15) Uani 1 1 d .
N3 N 0.0331(6) 0.1743(3) 0.2367(3) 0.0413(13) Uani 1 1 d .
N4 N -0.1377(6) 0.2014(3) 0.1030(3) 0.0423(14) Uani 1 1 d .
O1 O 0.1245(5) 0.2569(2) 0.0612(2) 0.0400(11) Uani 1 1 d .
O2 O 0.1088(5) 0.3198(3) 0.1769(2) 0.0428(11) Uani 1 1 d .
C1 C 0.4081(8) 0.2201(5) 0.2231(4) 0.056(2) Uani 1 1 d .
H1 H 0.3842 0.2669 0.2413 0.067 Uiso 1 1 calc R
C2 C 0.5517(9) 0.1910(6) 0.2413(4) 0.064(2) Uani 1 1 d .
H2 H 0.6241 0.2173 0.2724 0.077 Uiso 1 1 calc R
C3 C 0.5802(9) 0.1260(6) 0.2134(5) 0.072(3) Uani 1 1 d .
H3 H 0.6751 0.1069 0.2251 0.086 Uiso 1 1 calc R
C4 C 0.4797(8) 0.0849(5) 0.1684(5) 0.055(2) Uani 1 1 d .
H4 H 0.5031 0.0388 0.1489 0.066 Uiso 1 1 calc R
C5 C 0.3401(8) 0.1153(4) 0.1529(4) 0.0501(19) Uani 1 1 d .
C6 C 0.2219(8) 0.0819(4) 0.1034(4) 0.055(2) Uani 1 1 d .
H6A H 0.2358 0.0265 0.1018 0.066 Uiso 1 1 calc R
H6B H 0.2220 0.1027 0.0576 0.066 Uiso 1 1 calc R
C7 C 0.0615(9) 0.0534(4) 0.1820(4) 0.055(2) Uani 1 1 d .
H7A H 0.1515 0.0258 0.2005 0.066 Uiso 1 1 calc R
H7B H -0.0143 0.0152 0.1667 0.066 Uiso 1 1 calc R
C8 C 0.0220(7) 0.0991(4) 0.2387(4) 0.0419(16) Uani 1 1 d .
C9 C -0.0218(7) 0.0636(4) 0.2925(4) 0.0489(18) Uani 1 1 d .
H9 H -0.0308 0.0101 0.2930 0.059 Uiso 1 1 calc R
C10 C -0.0517(9) 0.1055(5) 0.3445(4) 0.062(2) Uani 1 1 d .
H10 H -0.0796 0.0813 0.3819 0.075 Uiso 1 1 calc R
C11 C -0.0413(8) 0.1837(5) 0.3427(4) 0.058(2) Uani 1 1 d .
H11 H -0.0622 0.2140 0.3785 0.070 Uiso 1 1 calc R
C12 C 0.0002(7) 0.2164(5) 0.2877(3) 0.0459(17) Uani 1 1 d .
H12 H 0.0059 0.2700 0.2854 0.055 Uiso 1 1 calc R
C13 C -0.0394(10) 0.0869(4) 0.0651(5) 0.064(2) Uani 1 1 d .
H13A H -0.0698 0.0333 0.0646 0.077 Uiso 1 1 calc R
H13B H -0.0082 0.0969 0.0220 0.077 Uiso 1 1 calc R
C14 C -0.1648(8) 0.1362(5) 0.0680(4) 0.0508(19) Uani 1 1 d .
C15 C -0.3013(9) 0.1186(5) 0.0326(5) 0.064(2) Uani 1 1 d .
H15 H -0.3169 0.0724 0.0081 0.077 Uiso 1 1 calc R
C16 C -0.4113(8) 0.1648(5) 0.0321(4) 0.058(2) Uani 1 1 d .
H16 H -0.5043 0.1510 0.0081 0.070 Uiso 1 1 calc R
C17 C -0.3900(8) 0.2352(5) 0.0676(4) 0.056(2) Uani 1 1 d .
C18 C -0.4985(9) 0.2854(5) 0.0715(5) 0.065(2) Uani 1 1 d .
H18 H -0.5930 0.2752 0.0470 0.078 Uiso 1 1 calc R
C19 C -0.4717(8) 0.3499(6) 0.1102(5) 0.071(3) Uani 1 1 d .
H19 H -0.5472 0.3846 0.1113 0.085 Uiso 1 1 calc R
C20 C -0.3337(8) 0.3650(5) 0.1484(5) 0.062(2) Uani 1 1 d .
H20 H -0.3165 0.4089 0.1762 0.074 Uiso 1 1 calc R
C21 C -0.2225(8) 0.3153(4) 0.1452(4) 0.0518(19) Uani 1 1 d .
H21 H -0.1288 0.3254 0.1707 0.062 Uiso 1 1 calc R
C22 C -0.2482(7) 0.2505(4) 0.1043(3) 0.0438(17) Uani 1 1 d .
C23 C 0.1392(6) 0.3311(4) 0.0646(3) 0.0354(14) Uani 1 1 d .
C24 C 0.1675(6) 0.3759(4) 0.0116(4) 0.0421(16) Uani 1 1 d .
C25 C 0.1829(7) 0.4541(4) 0.0204(4) 0.0512(19) Uani 1 1 d .
C26 C 0.1652(7) 0.4885(4) 0.0794(4) 0.0485(19) Uani 1 1 d .
C27 C 0.1357(7) 0.4444(4) 0.1329(4) 0.0451(17) Uani 1 1 d .
C28 C 0.1278(7) 0.3658(4) 0.1274(4) 0.0384(15) Uani 1 1 d .
Cl1 Cl 0.1858(2) 0.33146(13) -0.06265(10) 0.0591(6) Uani 1 1 d .
Cl2 Cl 0.2214(2) 0.50860(14) -0.04591(14) 0.0804(8) Uani 1 1 d .
Cl3 Cl 0.1763(2) 0.58532(11) 0.08847(15) 0.0809(8) Uani 1 1 d .
Cl4 Cl 0.1065(2) 0.48414(12) 0.20705(12) 0.0691(6) Uani 1 1 d .
Cl5 Cl 0.2810(3) 0.09847(13) -0.13206(14) 0.0743(7) Uani 1 1 d .
O3 O 0.2507(8) 0.0355(4) -0.1731(4) 0.106(3) Uani 1 1 d .
O4 O 0.4157(10) 0.1246(6) -0.1336(5) 0.140(4) Uani 1 1 d .
O5 O 0.2634(13) 0.0815(6) -0.0691(4) 0.146(4) Uani 1 1 d .
O6 O 0.1859(18) 0.1567(6) -0.1572(7) 0.217(7) Uani 1 1 d .
O7 O 0.0859(11) -0.0975(4) 0.0995(4) 0.098(3) Uani 1 1 d .
H7 H -0.0182 -0.1228 0.0771 0.25(10) Uiso 1 1 d R
C29 C -0.1989(12) 0.1479(5) -0.1303(5) 0.079(3) Uani 1 1 d .
H29A H -0.2903 0.1315 -0.1190 0.095 Uiso 1 1 calc R
H29B H -0.2102 0.1469 -0.1804 0.095 Uiso 1 1 calc R
C30 C 0.1629(11) 0.7739(5) 0.1043(6) 0.084(3) Uani 1 1 d .
H30A H 0.2363 0.7386 0.1275 0.126 Uiso 1 1 calc R
H30B H 0.1591 0.7725 0.0552 0.126 Uiso 1 1 calc R
H30C H 0.0695 0.7592 0.1132 0.126 Uiso 1 1 calc R
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
O2 Fe1 O1 85.06(19) . .
O2 Fe1 N3 95.3(2) . .
O1 Fe1 N3 177.0(2) . .
O2 Fe1 N4 106.8(2) . .
O1 Fe1 N4 92.6(2) . .
N3 Fe1 N4 84.4(2) . .
O2 Fe1 N2 173.3(2) . .
O1 Fe1 N2 98.4(2) . .
N3 Fe1 N2 81.5(2) . .
N4 Fe1 N2 78.9(2) . .
O2 Fe1 N1 98.2(2) . .
O1 Fe1 N1 91.8(2) . .
N3 Fe1 N1 91.1(2) . .
N4 Fe1 N1 154.9(2) . .
N2 Fe1 N1 76.0(2) . .
C1 N1 C5 121.7(7) . .
C1 N1 Fe1 124.0(5) . .
C5 N1 Fe1 114.3(5) . .
C13 N2 C6 113.2(6) . .
C13 N2 C7 110.3(6) . .
C6 N2 C7 111.8(6) . .
C13 N2 Fe1 106.8(4) . .
C6 N2 Fe1 105.4(5) . .
C7 N2 Fe1 109.1(4) . .
C8 N3 C12 119.4(6) . .
C8 N3 Fe1 114.5(5) . .
C12 N3 Fe1 125.9(5) . .
C14 N4 C22 119.2(6) . .
C14 N4 Fe1 112.8(5) . .
C22 N4 Fe1 127.9(5) . .
C23 O1 Fe1 110.4(4) . .
C28 O2 Fe1 111.2(4) . .
N1 C1 C2 119.1(8) . .
C3 C2 C1 118.0(9) . .
C2 C3 C4 123.7(8) . .
C3 C4 C5 116.1(8) . .
N1 C5 C4 121.3(8) . .
N1 C5 C6 114.9(6) . .
C4 C5 C6 123.7(7) . .
C5 C6 N2 111.3(6) . .
N2 C7 C8 115.2(6) . .
N3 C8 C9 120.7(7) . .
N3 C8 C7 118.5(6) . .
C9 C8 C7 120.8(7) . .
C10 C9 C8 120.1(7) . .
C9 C10 C11 119.6(7) . .
C12 C11 C10 118.2(8) . .
N3 C12 C11 121.9(7) . .
N2 C13 C14 113.8(6) . .
N4 C14 C15 121.1(8) . .
N4 C14 C13 116.8(7) . .
C15 C14 C13 121.9(8) . .
C16 C15 C14 121.7(9) . .
C15 C16 C17 120.1(7) . .
C18 C17 C22 119.5(8) . .
C18 C17 C16 123.9(8) . .
C22 C17 C16 116.4(7) . .
C19 C18 C17 120.9(8) . .
C18 C19 C20 120.5(8) . .
C21 C20 C19 119.7(9) . .
C20 C21 C22 120.1(8) . .
N4 C22 C21 119.2(6) . .
N4 C22 C17 121.4(7) . .
C21 C22 C17 119.3(7) . .
O1 C23 C24 124.0(6) . .
O1 C23 C28 116.4(6) . .
C24 C23 C28 119.6(6) . .
C25 C24 C23 119.7(7) . .
C25 C24 Cl1 122.1(6) . .
C23 C24 Cl1 118.2(5) . .
C26 C25 C24 121.2(7) . .
C26 C25 Cl2 119.9(6) . .
C24 C25 Cl2 118.9(7) . .
C25 C26 C27 119.8(6) . .
C25 C26 Cl3 121.0(6) . .
C27 C26 Cl3 119.2(6) . .
C28 C27 C26 120.5(7) . .
C28 C27 Cl4 117.3(6) . .
C26 C27 Cl4 122.2(6) . .
O2 C28 C27 124.3(7) . .
O2 C28 C23 116.7(6) . .
C27 C28 C23 119.0(7) . .
O5 Cl5 O4 113.5(6) . .
O5 Cl5 O3 109.3(6) . .
O4 Cl5 O3 109.7(6) . .
O5 Cl5 O6 107.8(8) . .
O4 Cl5 O6 106.6(9) . .
O3 Cl5 O6 109.8(8) . .
O7 C29 C30 109.0(9) 3 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O2 1.911(5) .
Fe1 O1 1.950(5) .
Fe1 N3 2.128(5) .
Fe1 N4 2.153(6) .
Fe1 N2 2.160(6) .
Fe1 N1 2.190(6) .
N1 C1 1.334(10) .
N1 C5 1.339(9) .
N2 C13 1.450(10) .
N2 C6 1.491(9) .
N2 C7 1.496(9) .
N3 C8 1.334(9) .
N3 C12 1.354(9) .
N4 C14 1.346(10) .
N4 C22 1.371(9) .
O1 C23 1.320(8) .
O2 C28 1.326(8) .
C1 C2 1.439(11) .
C2 C3 1.331(13) .
C3 C4 1.379(13) .
C4 C5 1.410(10) .
C5 C6 1.463(11) .
C7 C8 1.506(10) .
C8 C9 1.389(10) .
C9 C10 1.358(11) .
C10 C11 1.386(12) .
C11 C12 1.378(10) .
C13 C14 1.491(11) .
C14 C15 1.383(11) .
C15 C16 1.329(12) .
C16 C17 1.425(12) .
C17 C18 1.378(11) .
C17 C22 1.425(10) .
C18 C19 1.374(13) .
C19 C20 1.404(12) .
C20 C21 1.390(10) .
C21 C22 1.400(11) .
C23 C24 1.397(9) .
C23 C28 1.428(9) .
C24 C25 1.396(11) .
C24 Cl1 1.726(8) .
C25 C26 1.374(11) .
C25 Cl2 1.744(8) .
C26 C27 1.404(11) .
C26 Cl3 1.721(7) .
C27 C28 1.393(9) .
C27 Cl4 1.722(8) .
Cl5 O5 1.344(9) .
Cl5 O4 1.374(9) .
Cl5 O3 1.378(7) .
Cl5 O6 1.395(10) .
O7 C29 1.435(12) 3
C29 O7 1.435(12) 3
C29 C30 1.491(12) 3_565
C30 C29 1.491(12) 3_565
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7 O5 1.10 2.43 3.276(16) 133.1 3
O7 H7 O6 1.10 2.57 3.232(19) 118.0 3
