#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:00:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179875 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/71/7017162.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_7017162
loop_
_publ_author_name
'Hall, Nikita A.'
'Duboc, Carole'
'Collomb, Marie-Noëlle'
'Deronzier, Alain'
'Blackman, Allan G.'
_publ_section_title
;
 Factors influencing mononuclear versus multinuclear coordination in a
 series of potentially hexadentate acyclic N(6) ligands: the roles of
 flexibility and chelate ring size.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12075
_journal_page_last               12082
_journal_paper_doi               10.1039/c1dt10627a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C24 H24 Cl2 Fe N6 O8'
_chemical_formula_weight         651.24
_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                 110.802(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5489(14)
_cell_length_b                   13.2220(11)
_cell_length_c                   11.8908(10)
_cell_measurement_reflns_used    3385
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.38
_cell_volume                     2579.2(4)
_computing_cell_refinement       'ApexII and SAINT (Bruker, 2001)'
_computing_data_collection       'ApexII (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Kappa ApexII area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8803
_diffrn_reflns_theta_full        24.12
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.862614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         1982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0359
_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)+(0.0429P)²+4.4916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                1647
_reflns_number_total             1982
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1dt10627a.txt
_cod_data_source_block           nh21
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7017162
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
Fe1 Fe 0.5000 0.22814(4) 0.7500 0.0141(2) Uani 1 2 d S
Cl2 Cl 0.32965(5) 0.16549(6) 0.32145(6) 0.0199(2) Uani 1 1 d .
O3 O 0.29939(13) 0.21952(16) 0.40195(19) 0.0243(5) Uani 1 1 d .
N1 N 0.44359(15) 0.32860(18) 0.6283(2) 0.0179(6) Uani 1 1 d .
O4 O 0.36714(18) 0.2340(2) 0.2647(2) 0.0525(8) Uani 1 1 d .
O2 O 0.26413(14) 0.11421(17) 0.2305(2) 0.0321(6) Uani 1 1 d .
C5 C 0.47402(19) 0.3390(2) 0.5376(3) 0.0194(7) Uani 1 1 d .
O1 O 0.38838(16) 0.0928(2) 0.3902(2) 0.0471(8) Uani 1 1 d .
C2 C 0.3429(2) 0.4533(2) 0.5329(3) 0.0255(8) Uani 1 1 d .
H4A H 0.2984 0.4916 0.5328 0.031 Uiso 1 1 calc R
C1 C 0.37887(19) 0.3859(2) 0.6244(3) 0.0216(7) Uani 1 1 d .
H5 H 0.3579 0.3794 0.6858 0.026 Uiso 1 1 calc R
C3 C 0.3733(2) 0.4638(2) 0.4414(3) 0.0258(8) Uani 1 1 d .
H3 H 0.3498 0.5096 0.3793 0.031 Uiso 1 1 calc R
C4 C 0.4389(2) 0.4060(2) 0.4427(3) 0.0244(8) Uani 1 1 d .
H2 H 0.4595 0.4116 0.3810 0.029 Uiso 1 1 calc R
N2 N 0.56783(15) 0.22352(18) 0.6580(2) 0.0152(6) Uani 1 1 d .
N3 N 0.57377(15) 0.11543(18) 0.8431(2) 0.0164(6) Uani 1 1 d .
H4B H 0.5881 0.1285 0.9231 0.020 Uiso 1 1 calc R
C6 C 0.54542(19) 0.2752(2) 0.5525(3) 0.0177(7) Uani 1 1 d .
C9 C 0.67816(19) 0.1479(2) 0.6179(3) 0.0230(8) Uani 1 1 d .
H9A H 0.7232 0.1051 0.6410 0.028 Uiso 1 1 calc R
C7 C 0.58814(19) 0.2632(2) 0.4757(3) 0.0227(8) Uani 1 1 d .
H7A H 0.5722 0.2974 0.4026 0.027 Uiso 1 1 calc R
C12 C 0.52684(19) 0.0195(2) 0.8156(3) 0.0201(7) Uani 1 1 d .
H25C H 0.4936 0.0135 0.8654 0.024 Uiso 1 1 calc R
H25D H 0.5639 -0.0377 0.8325 0.024 Uiso 1 1 calc R
C8 C 0.6550(2) 0.1995(3) 0.5093(3) 0.0254(8) Uani 1 1 d .
H8A H 0.6847 0.1911 0.4587 0.030 Uiso 1 1 calc R
C11 C 0.64962(18) 0.1142(2) 0.8124(3) 0.0186(7) Uani 1 1 d .
H15C H 0.6679 0.0451 0.8117 0.022 Uiso 1 1 calc R
H15D H 0.6925 0.1514 0.8729 0.022 Uiso 1 1 calc R
C10 C 0.63290(18) 0.1615(2) 0.6913(3) 0.0177(7) 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
N2 Fe1 N2 176.28(15) . 2_656
N2 Fe1 N1 101.19(10) . 2_656
N2 Fe1 N1 81.37(10) 2_656 2_656
N2 Fe1 N1 81.37(10) . .
N2 Fe1 N1 101.19(10) 2_656 .
N1 Fe1 N1 94.40(14) 2_656 .
N2 Fe1 N3 94.11(10) . 2_656
N2 Fe1 N3 83.14(10) 2_656 2_656
N1 Fe1 N3 164.09(10) 2_656 2_656
N1 Fe1 N3 92.17(10) . 2_656
N2 Fe1 N3 83.14(10) . .
N2 Fe1 N3 94.11(10) 2_656 .
N1 Fe1 N3 92.17(10) 2_656 .
N1 Fe1 N3 164.09(10) . .
N3 Fe1 N3 85.29(14) 2_656 .
O4 Cl2 O1 109.71(19) . .
O4 Cl2 O2 108.93(15) . .
O1 Cl2 O2 109.47(15) . .
O4 Cl2 O3 110.00(15) . .
O1 Cl2 O3 108.31(14) . .
O2 Cl2 O3 110.42(13) . .
C1 N1 C5 118.3(3) . .
C1 N1 Fe1 127.2(2) . .
C5 N1 Fe1 114.5(2) . .
N1 C5 C4 121.1(3) . .
N1 C5 C6 113.7(3) . .
C4 C5 C6 125.2(3) . .
C1 C2 C3 119.5(3) . .
C1 C2 H4A 120.2 . .
C3 C2 H4A 120.2 . .
N1 C1 C2 122.3(3) . .
N1 C1 H5 118.9 . .
C2 C1 H5 118.9 . .
C4 C3 C2 119.4(3) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.3(3) . .
C3 C4 H2 120.3 . .
C5 C4 H2 120.3 . .
C10 N2 C6 121.0(3) . .
C10 N2 Fe1 119.6(2) . .
C6 N2 Fe1 119.0(2) . .
C12 N3 C11 114.1(2) . .
C12 N3 Fe1 108.15(17) . .
C11 N3 Fe1 108.94(17) . .
C12 N3 H4B 108.5 . .
C11 N3 H4B 108.5 . .
Fe1 N3 H4B 108.5 . .
N2 C6 C7 120.4(3) . .
N2 C6 C5 110.8(3) . .
C7 C6 C5 128.8(3) . .
C10 C9 C8 118.7(3) . .
C10 C9 H9A 120.7 . .
C8 C9 H9A 120.7 . .
C6 C7 C8 118.9(3) . .
C6 C7 H7A 120.6 . .
C8 C7 H7A 120.6 . .
N3 C12 C12 108.76(19) . 2_656
N3 C12 H25C 109.9 . .
C12 C12 H25C 109.9 2_656 .
N3 C12 H25D 109.9 . .
C12 C12 H25D 109.9 2_656 .
H25C C12 H25D 108.3 . .
C7 C8 C9 120.3(3) . .
C7 C8 H8A 119.8 . .
C9 C8 H8A 119.8 . .
N3 C11 C10 110.0(2) . .
N3 C11 H15C 109.7 . .
C10 C11 H15C 109.7 . .
N3 C11 H15D 109.7 . .
C10 C11 H15D 109.7 . .
H15C C11 H15D 108.2 . .
N2 C10 C9 120.7(3) . .
N2 C10 C11 113.1(3) . .
C9 C10 C11 126.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.883(2) .
Fe1 N2 1.883(2) 2_656
Fe1 N1 1.955(2) 2_656
Fe1 N1 1.955(2) .
Fe1 N3 2.026(2) 2_656
Fe1 N3 2.026(2) .
Cl2 O4 1.423(3) .
Cl2 O1 1.434(2) .
Cl2 O2 1.438(2) .
Cl2 O3 1.439(2) .
N1 C1 1.352(4) .
N1 C5 1.369(4) .
C5 C4 1.394(4) .
C5 C6 1.468(4) .
C2 C1 1.374(4) .
C2 C3 1.379(5) .
C2 H4A 0.9300 .
C1 H5 0.9300 .
C3 C4 1.376(5) .
C3 H3 0.9300 .
C4 H2 0.9300 .
N2 C10 1.346(4) .
N2 C6 1.358(4) .
N3 C12 1.485(4) .
N3 C11 1.500(4) .
N3 H4B 0.9100 .
C6 C7 1.381(4) .
C9 C10 1.384(4) .
C9 C8 1.388(4) .
C9 H9A 0.9300 .
C7 C8 1.384(5) .
C7 H7A 0.9300 .
C12 C12 1.509(6) 2_656
C12 H25C 0.9700 .
C12 H25D 0.9700 .
C8 H8A 0.9300 .
C11 C10 1.500(4) .
C11 H15C 0.9700 .
C11 H15D 0.9700 .
