#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:09:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179315 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321273.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_4321273
loop_
_publ_author_name
'Alain Diebold'
'Abdelaziz Elbouadili'
'Karl S. Hagen'
_publ_section_title
;
 Crystal Structures and Solution Behavior of Paramagnetic Divalent
 Transition Metal Complexes (Fe, Co) of the Sterically Encumbered
 Tridentate Macrocycles 1,4,7-R3-1,4,7-Triazacyclononane: Coordination
 Numbers 5 (R = i-Pr) and 6 (R = i-Bu)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3915
_journal_page_last               3923
_journal_paper_doi               10.1021/ic000456h
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         Fe(i-Bu3TACN)(H2O)(SO3CF3)2
_chemical_formula_sum            'C20 H41 F6 Fe N3 O7 S2'
_chemical_formula_weight         669.53
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.990(2)
_cell_length_b                   15.768(2)
_cell_length_c                   17.564(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      10.07
_cell_volume                     6067.3(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4524
_diffrn_reflns_theta_max         56.74
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        17.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.986
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       cut_from_large_crystal
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00048(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         3931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_obs          0.0794
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1247P)²+50.9041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2297
_refine_ls_wR_factor_obs         0.2074
_reflns_number_observed          3059
_reflns_number_total             3933
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000456h_4.cif
_cod_data_source_block           Complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+50.9041P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+50.9041P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321273
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.21589(5) 0.11626(7) -0.12926(6) 0.0335(4) Uani 1 d . .
N1 N 0.1662(3) 0.1527(4) -0.2545(3) 0.0395(15) Uani 1 d . .
N2 N 0.1890(3) -0.0124(4) -0.1785(3) 0.042(2) Uani 1 d . .
N3 N 0.2905(3) 0.0942(4) -0.1825(3) 0.0401(15) Uani 1 d . .
O1 O 0.2437(3) 0.2387(4) -0.0896(4) 0.0516(15) Uani 1 d . .
H1 H 0.2213(49) 0.2789(69) -0.0972(65) 0.080 Uiso 1 d . .
H2 H 0.2780(51) 0.2521(68) -0.0821(66) 0.080 Uiso 1 d . .
O2 O 0.2724(2) 0.0717(3) -0.0135(3) 0.0435(13) Uani 1 d . .
O5 O 0.1405(3) 0.1256(4) -0.0864(4) 0.058(2) Uani 1 d . .
C1 C 0.1203(4) 0.0842(5) -0.2796(5) 0.048(2) Uani 1 d . .
H1A H 0.0991(4) 0.0897(5) -0.3376(5) 0.058 Uiso 1 calc R .
H1B H 0.0895(4) 0.0908(5) -0.2511(5) 0.058 Uiso 1 calc R .
C2 C 0.1483(4) -0.0029(6) -0.2630(5) 0.052(2) Uani 1 d . .
H2A H 0.1153(4) -0.0457(6) -0.2733(5) 0.062 Uiso 1 calc R .
H2B H 0.1724(4) -0.0142(6) -0.3000(5) 0.062 Uiso 1 calc R .
C3 C 0.2489(3) -0.0503(5) -0.1743(5) 0.048(2) Uani 1 d . .
H3A H 0.2422(3) -0.1059(5) -0.2018(5) 0.058 Uiso 1 calc R .
H3B H 0.2723(3) -0.0603(5) -0.1176(5) 0.058 Uiso 1 calc R .
C4 C 0.2857(4) 0.0055(5) -0.2120(5) 0.050(2) Uani 1 d . .
H4A H 0.3273(4) -0.0185(5) -0.2007(5) 0.061 Uiso 1 calc R .
H4B H 0.2666(4) 0.0056(5) -0.2706(5) 0.061 Uiso 1 calc R .
C5 C 0.2764(3) 0.1576(6) -0.2485(4) 0.046(2) Uani 1 d . .
H5A H 0.3036(3) 0.1479(6) -0.2818(4) 0.055 Uiso 1 calc R .
H5B H 0.2847(3) 0.2153(6) -0.2254(4) 0.055 Uiso 1 calc R .
C6 C 0.2100(3) 0.1525(6) -0.3011(4) 0.049(2) Uani 1 d . .
H6A H 0.2011(3) 0.2012(6) -0.3383(4) 0.058 Uiso 1 calc R .
H6B H 0.2042(3) 0.0999(6) -0.3334(4) 0.058 Uiso 1 calc R .
C7 C 0.1367(3) 0.2362(5) -0.2549(5) 0.044(2) Uani 1 d . .
H7A H 0.1685(3) 0.2801(5) -0.2487(5) 0.053 Uiso 1 calc R .
H7B H 0.1231(3) 0.2389(5) -0.2065(5) 0.053 Uiso 1 calc R .
C8 C 0.0820(4) 0.2621(6) -0.3265(5) 0.054(2) Uani 1 d . .
H8A H 0.0489(4) 0.2197(6) -0.3303(5) 0.065 Uiso 1 calc R .
C9 C 0.0934(4) 0.2638(7) -0.4071(5) 0.074(3) Uani 1 d . .
H9A H 0.1083(4) 0.2082(7) -0.4179(5) 0.110 Uiso 1 calc R .
H9B H 0.1241(4) 0.3072(7) -0.4067(5) 0.110 Uiso 1 calc R .
H9C H 0.0553(4) 0.2772(7) -0.4489(5) 0.110 Uiso 1 calc R .
C10 C 0.0587(4) 0.3474(6) -0.3072(7) 0.071(3) Uani 1 d . .
H10A H 0.0518(4) 0.3444(6) -0.2549(7) 0.106 Uiso 1 calc R .
H10B H 0.0203(4) 0.3614(6) -0.3482(7) 0.106 Uiso 1 calc R .
H10C H 0.0891(4) 0.3914(6) -0.3060(7) 0.106 Uiso 1 calc R .
C11 C 0.1575(4) -0.0583(5) -0.1287(5) 0.047(2) Uani 1 d . .
H11A H 0.1178(4) -0.0299(5) -0.1358(5) 0.056 Uiso 1 calc R .
H11B H 0.1819(4) -0.0506(5) -0.0721(5) 0.056 Uiso 1 calc R .
C12 C 0.1452(4) -0.1524(6) -0.1427(5) 0.059(2) Uani 1 d . .
H12A H 0.1461(4) -0.1659(6) -0.1980(5) 0.071 Uiso 1 calc R .
C13 C 0.1935(5) -0.2072(6) -0.0842(6) 0.075(3) Uani 1 d . .
H13A H 0.2340(5) -0.1925(6) -0.0878(6) 0.112 Uiso 1 calc R .
H13B H 0.1852(5) -0.2672(6) -0.0976(6) 0.112 Uiso 1 calc R .
H13C H 0.1924(5) -0.1969(6) -0.0296(6) 0.112 Uiso 1 calc R .
C14 C 0.0825(5) -0.1744(8) -0.1377(7) 0.087(3) Uani 1 d . .
H14A H 0.0753(5) -0.2353(8) -0.1468(7) 0.131 Uiso 1 calc R .
H14B H 0.0516(5) -0.1425(8) -0.1784(7) 0.131 Uiso 1 calc R .
H14C H 0.0800(5) -0.1596(8) -0.0846(7) 0.131 Uiso 1 calc R .
C15 C 0.3510(3) 0.1100(5) -0.1232(4) 0.042(2) Uani 1 d . .
H15A H 0.3569(3) 0.0671(5) -0.0803(4) 0.051 Uiso 1 calc R .
H15B H 0.3492(3) 0.1661(5) -0.0987(4) 0.051 Uiso 1 calc R .
C16 C 0.4086(3) 0.1088(6) -0.1511(5) 0.048(2) Uani 1 d . .
H16A H 0.4012(3) 0.0692(6) -0.1976(5) 0.057 Uiso 1 calc R .
C17 C 0.4617(4) 0.0750(7) -0.0835(6) 0.070(3) Uani 1 d . .
H17A H 0.4512(4) 0.0191(7) -0.0670(6) 0.105 Uiso 1 calc R .
H17B H 0.4704(4) 0.1141(7) -0.0381(6) 0.105 Uiso 1 calc R .
H17C H 0.4978(4) 0.0699(7) -0.1017(6) 0.105 Uiso 1 calc R .
C18 C 0.4248(4) 0.1938(8) -0.1759(7) 0.087(4) Uani 1 d . .
H18A H 0.3906(4) 0.2158(8) -0.2196(7) 0.130 Uiso 1 calc R .
H18B H 0.4610(4) 0.1886(8) -0.1941(7) 0.130 Uiso 1 calc R .
H18C H 0.4336(4) 0.2328(8) -0.1304(7) 0.130 Uiso 1 calc R .
S1 S 0.28616(8) 0.03654(12) 0.06631(10) 0.0392(5) Uani 1 d . .
O3 O 0.2512(3) -0.0368(4) 0.0722(3) 0.057(2) Uani 1 d . .
O4 O 0.2937(3) 0.0985(4) 0.1285(3) 0.055(2) Uani 1 d . .
C19 C 0.3630(4) -0.0042(6) 0.0838(5) 0.053(2) Uani 1 d . .
F1 F 0.4022(2) 0.0559(4) 0.0822(3) 0.078(2) Uani 1 d . .
F2 F 0.3823(2) -0.0424(4) 0.1543(3) 0.082(2) Uani 1 d . .
F3 F 0.3651(3) -0.0607(4) 0.0284(3) 0.076(2) Uani 1 d . .
S2 S 0.10442(11) 0.1670(2) -0.0467(2) 0.0672(8) Uani 1 d . .
O6 O 0.0676(4) 0.2312(5) -0.0761(7) 0.119(4) Uani 1 d . .
O7 O 0.1481(4) 0.1901(9) 0.0359(7) 0.169(6) Uani 1 d . .
C20 C 0.0648(5) 0.0869(8) -0.0133(8) 0.088(4) Uani 1 d . .
F4 F 0.0232(4) 0.0531(6) -0.0836(6) 0.143(3) Uani 1 d . .
F5 F 0.0947(3) 0.0205(5) 0.0186(4) 0.103(2) Uani 1 d . .
F6 F 0.0296(3) 0.1142(5) 0.0269(5) 0.116(3) Uani 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
O1 Fe O5 91.0(2) . . ?
O1 Fe O2 87.2(2) . . ?
O5 Fe O2 90.6(2) . . ?
O1 Fe N3 95.0(2) . . ?
O5 Fe N3 173.7(2) . . ?
O2 Fe N3 91.4(2) . . ?
O1 Fe N2 176.0(2) . . ?
O5 Fe N2 92.4(2) . . ?
O2 Fe N2 95.0(2) . . ?
N3 Fe N2 81.5(2) . . ?
O1 Fe N1 96.0(2) . . ?
O5 Fe N1 96.0(2) . . ?
O2 Fe N1 172.6(2) . . ?
N3 Fe N1 81.6(2) . . ?
N2 Fe N1 81.5(2) . . ?
C6 N1 C7 112.9(6) . . ?
C6 N1 C1 112.1(6) . . ?
C7 N1 C1 111.3(6) . . ?
C6 N1 Fe 108.4(4) . . ?
C7 N1 Fe 109.4(4) . . ?
C1 N1 Fe 102.2(4) . . ?
C3 N2 C11 112.7(6) . . ?
C3 N2 C2 112.3(6) . . ?
C11 N2 C2 111.2(6) . . ?
C3 N2 Fe 101.8(4) . . ?
C11 N2 Fe 110.1(4) . . ?
C2 N2 Fe 108.1(5) . . ?
C4 N3 C15 111.0(6) . . ?
C4 N3 C5 112.7(6) . . ?
C15 N3 C5 111.7(6) . . ?
C4 N3 Fe 108.0(4) . . ?
C15 N3 Fe 111.0(4) . . ?
C5 N3 Fe 102.0(4) . . ?
S1 O2 Fe 157.3(3) . . ?
S2 O5 Fe 153.3(4) . . ?
N1 C1 C2 112.6(6) . . ?
N2 C2 C1 112.5(7) . . ?
N2 C3 C4 112.3(6) . . ?
N3 C4 C3 112.9(6) . . ?
N3 C5 C6 112.1(6) . . ?
N1 C6 C5 112.9(6) . . ?
N1 C7 C8 120.0(7) . . ?
C9 C8 C10 111.3(8) . . ?
C9 C8 C7 116.0(7) . . ?
C10 C8 C7 107.9(7) . . ?
N2 C11 C12 118.8(7) . . ?
C14 C12 C11 110.4(8) . . ?
C14 C12 C13 110.0(8) . . ?
C11 C12 C13 112.5(7) . . ?
N3 C15 C16 119.0(6) . . ?
C18 C16 C17 109.3(8) . . ?
C18 C16 C15 113.3(7) . . ?
C17 C16 C15 108.6(7) . . ?
O3 S1 O4 115.9(3) . . ?
O3 S1 O2 114.6(3) . . ?
O4 S1 O2 114.5(3) . . ?
O3 S1 C19 104.0(4) . . ?
O4 S1 C19 103.0(4) . . ?
O2 S1 C19 102.4(3) . . ?
F1 C19 F2 108.1(7) . . ?
F1 C19 F3 106.9(7) . . ?
F2 C19 F3 107.6(7) . . ?
F1 C19 S1 112.3(6) . . ?
F2 C19 S1 110.5(6) . . ?
F3 C19 S1 111.2(6) . . ?
O6 S2 O5 124.9(5) . . ?
O6 S2 O7 110.2(7) . . ?
O5 S2 O7 105.4(5) . . ?
O6 S2 C20 110.1(5) . . ?
O5 S2 C20 106.0(5) . . ?
O7 S2 C20 96.4(7) . . ?
F5 C20 F6 111.9(10) . . ?
F5 C20 F4 101.8(11) . . ?
F6 C20 F4 103.4(9) . . ?
F5 C20 S2 117.9(8) . . ?
F6 C20 S2 114.5(9) . . ?
F4 C20 S2 105.1(8) . . ?
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
Fe O1 2.086(6) . ?
Fe O5 2.095(5) . ?
Fe O2 2.171(5) . ?
Fe N3 2.217(6) . ?
Fe N2 2.218(7) . ?
Fe N1 2.225(6) . ?
N1 C6 1.477(9) . ?
N1 C7 1.479(10) . ?
N1 C1 1.480(10) . ?
N2 C3 1.482(9) . ?
N2 C11 1.483(10) . ?
N2 C2 1.502(9) . ?
N3 C4 1.483(10) . ?
N3 C15 1.484(9) . ?
N3 C5 1.490(9) . ?
O2 S1 1.450(5) . ?
O5 S2 1.395(6) . ?
C1 C2 1.508(12) . ?
C3 C4 1.507(12) . ?
C5 C6 1.529(10) . ?
C7 C8 1.540(10) . ?
C8 C9 1.518(12) . ?
C8 C10 1.524(13) . ?
C11 C12 1.517(12) . ?
C12 C14 1.510(13) . ?
C12 C13 1.531(13) . ?
C15 C16 1.544(10) . ?
C16 C18 1.492(13) . ?
C16 C17 1.519(11) . ?
S1 O3 1.430(6) . ?
S1 O4 1.437(6) . ?
S1 C19 1.817(9) . ?
C19 F1 1.312(10) . ?
C19 F2 1.328(9) . ?
C19 F3 1.330(10) . ?
S2 O6 1.320(8) . ?
S2 O7 1.538(9) . ?
S2 C20 1.760(11) . ?
C20 F5 1.284(13) . ?
C20 F6 1.297(12) . ?
C20 F4 1.42(2) . ?
