#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/18/7011892.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_7011892
loop_
_publ_author_name
'Gott, Andrew L.'
'McGowan, Patrick C.'
'Podesta, Thomas J.'
'Thornton-Pett, Mark'
_publ_section_title
;
 Pendant arm N-monofunctionalised 1,4,7-triazacyclononane complexes of
 Fe(ii) and Ru(ii)
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3619
_journal_paper_doi               10.1039/b205344f
_journal_year                    2002
_chemical_formula_sum            'C12.5 H20 Cl3 Fe N4'
_chemical_formula_weight         388.53
_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                 118.778(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3833(9)
_cell_length_b                   12.7418(5)
_cell_length_c                   14.6966(4)
_cell_measurement_temperature    123(2)
_cell_volume                     3345.6(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17936
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Using multiple and symmetry-related data measurements via the program 
SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0443P)²+0.5440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                2561
_reflns_number_total             3286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205344f.txt
_cod_data_source_block           tjp12
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C12.50 H20 Cl3 Fe N4'
_cod_database_code               7011892
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 0.21542(2) 0.43108(3) 0.19938(3) 0.02098(15) Uani 1 1 d . . .
Cl2 Cl 0.17767(4) 0.58297(5) 0.08254(5) 0.02610(18) Uani 1 1 d . . .
Cl3 Cl 0.32128(4) 0.37848(6) 0.18425(5) 0.0354(2) Uani 1 1 d . . .
N1 N 0.25924(13) 0.5331(2) 0.33913(17) 0.0259(5) Uani 1 1 d . . .
H13 H 0.2728(17) 0.581(2) 0.330(2) 0.020(9) Uiso 1 1 d . . .
N2 N 0.12778(12) 0.33611(17) 0.07731(15) 0.0226(5) Uani 1 1 d . . .
C1 C 0.17250(15) 0.2706(2) 0.31167(19) 0.0268(6) Uani 1 1 d . . .
H1A H 0.1821 0.2254 0.3716 0.032 Uiso 1 1 calc R . .
H1B H 0.1497 0.2269 0.2482 0.032 Uiso 1 1 calc R . .
N3 N 0.24392(13) 0.31563(19) 0.32618(16) 0.0246(5) Uani 1 1 d . . .
H14 H 0.2697(16) 0.268(2) 0.3252(19) 0.022(8) Uiso 1 1 d . . .
N4 N 0.11596(12) 0.44432(16) 0.23064(15) 0.0217(5) Uani 1 1 d . . .
C7 C 0.05811(15) 0.3496(2) 0.06379(18) 0.0214(6) Uani 1 1 d . . .
C2 C 0.20104(16) 0.5687(2) 0.3656(2) 0.0292(6) Uani 1 1 d . . .
H2A H 0.2078 0.6445 0.3826 0.035 Uiso 1 1 calc R . .
H2B H 0.2071 0.5304 0.4278 0.035 Uiso 1 1 calc R . .
C8 C 0.00731(16) 0.2248(2) -0.0744(2) 0.0320(7) Uani 1 1 d . . .
H8 H -0.0337 0.1864 -0.1259 0.038 Uiso 1 1 calc R . .
C3 C 0.28973(16) 0.3639(2) 0.43082(19) 0.0292(6) Uani 1 1 d . . .
H3A H 0.3319 0.3167 0.4742 0.035 Uiso 1 1 calc R . .
H3B H 0.2585 0.3722 0.4651 0.035 Uiso 1 1 calc R . .
C9 C 0.04905(15) 0.4354(2) 0.12801(19) 0.0254(6) Uani 1 1 d . . .
H9A H 0.0401 0.5032 0.0909 0.031 Uiso 1 1 calc R . .
H9B H 0.0049 0.4200 0.1370 0.031 Uiso 1 1 calc R . .
C4 C 0.32020(16) 0.4705(2) 0.42250(19) 0.0307(7) Uani 1 1 d . . .
H4A H 0.3400 0.5081 0.4895 0.037 Uiso 1 1 calc R . .
H4B H 0.3617 0.4610 0.4063 0.037 Uiso 1 1 calc R . .
C10 C 0.07828(16) 0.2121(2) -0.0626(2) 0.0323(7) Uani 1 1 d . . .
H10 H 0.0867 0.1657 -0.1065 0.039 Uiso 1 1 calc R . .
C5 C 0.11872(15) 0.3590(2) 0.30209(19) 0.0259(6) Uani 1 1 d . . .
H5A H 0.0679 0.3295 0.2761 0.031 Uiso 1 1 calc R . .
H5B H 0.1346 0.3891 0.3717 0.031 Uiso 1 1 calc R . .
C11 C 0.13693(16) 0.2681(2) 0.01426(19) 0.0267(6) Uani 1 1 d . . .
H11 H 0.1858 0.2581 0.0229 0.032 Uiso 1 1 calc R . .
C6 C 0.12244(16) 0.5499(2) 0.27600(19) 0.0261(6) Uani 1 1 d . . .
H6A H 0.0856 0.5569 0.3014 0.031 Uiso 1 1 calc R . .
H6B H 0.1108 0.6037 0.2217 0.031 Uiso 1 1 calc R . .
C12 C -0.00302(15) 0.2940(2) -0.01060(19) 0.0268(6) Uani 1 1 d . . .
H12 H -0.0513 0.3037 -0.0172 0.032 Uiso 1 1 calc R . .
Cl4 Cl -0.00260(6) 0.10574(8) 0.14916(7) 0.0633(3) Uani 1 1 d . . .
C13 C 0.0000 0.0275(4) 0.2500 0.0489(13) Uani 1 2 d S . .
H15 H -0.046(2) -0.011(3) 0.224(3) 0.077(13) Uiso 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'
Fe Fe 0.3463 0.8444 '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'
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
N2 Fe1 N3 95.87(8) . . ?
N2 Fe1 N1 152.55(9) . . ?
N3 Fe1 N1 77.63(9) . . ?
N2 Fe1 N4 75.71(8) . . ?
N3 Fe1 N4 77.27(8) . . ?
N1 Fe1 N4 76.84(8) . . ?
N2 Fe1 Cl3 100.80(6) . . ?
N3 Fe1 Cl3 90.53(7) . . ?
N1 Fe1 Cl3 105.85(7) . . ?
N4 Fe1 Cl3 166.76(6) . . ?
N2 Fe1 Cl2 90.30(6) . . ?
N3 Fe1 Cl2 167.81(7) . . ?
N1 Fe1 Cl2 92.08(7) . . ?
N4 Fe1 Cl2 94.17(5) . . ?
Cl3 Fe1 Cl2 98.65(3) . . ?
C2 N1 C4 113.8(2) . . ?
C2 N1 Fe1 113.84(17) . . ?
C4 N1 Fe1 104.59(17) . . ?
C11 N2 C7 117.8(2) . . ?
C11 N2 Fe1 126.27(18) . . ?
C7 N2 Fe1 115.93(16) . . ?
N3 C1 C5 109.8(2) . . ?
C1 N3 C3 113.0(2) . . ?
C1 N3 Fe1 107.07(15) . . ?
C3 N3 Fe1 111.88(16) . . ?
C9 N4 C6 111.7(2) . . ?
C9 N4 C5 111.5(2) . . ?
C6 N4 C5 112.35(19) . . ?
C9 N4 Fe1 105.17(15) . . ?
C6 N4 Fe1 105.18(16) . . ?
C5 N4 Fe1 110.49(15) . . ?
N2 C7 C12 122.2(2) . . ?
N2 C7 C9 115.9(2) . . ?
C12 C7 C9 121.7(2) . . ?
N1 C2 C6 111.4(2) . . ?
C12 C8 C10 119.0(3) . . ?
N3 C3 C4 111.2(2) . . ?
N4 C9 C7 111.3(2) . . ?
N1 C4 C3 109.5(2) . . ?
C8 C10 C11 118.9(3) . . ?
N4 C5 C1 112.5(2) . . ?
N2 C11 C10 122.9(3) . . ?
N4 C6 C2 111.2(2) . . ?
C8 C12 C7 119.3(3) . . ?
Cl4 C13 Cl4 111.2(3) 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 N2 2.188(2) . ?
Fe1 N3 2.221(2) . ?
Fe1 N1 2.223(2) . ?
Fe1 N4 2.290(2) . ?
Fe1 Cl3 2.3699(8) . ?
Fe1 Cl2 2.4525(7) . ?
N1 C2 1.486(4) . ?
N1 C4 1.489(3) . ?
N2 C11 1.345(3) . ?
N2 C7 1.347(3) . ?
C1 N3 1.481(3) . ?
C1 C5 1.530(4) . ?
N3 C3 1.494(3) . ?
N4 C9 1.472(3) . ?
N4 C6 1.479(3) . ?
N4 C5 1.494(3) . ?
C7 C12 1.392(4) . ?
C7 C9 1.513(3) . ?
C2 C6 1.526(4) . ?
C8 C12 1.375(4) . ?
C8 C10 1.381(4) . ?
C3 C4 1.523(4) . ?
C10 C11 1.383(4) . ?
Cl4 C13 1.766(3) . ?
C13 Cl4 1.766(3) 2 ?
