#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:09:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179315 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321270.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_4321270
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-Pr3TACN)(SO3CF3)2
_chemical_formula_sum            'C17 H33 F6 Fe N3 O6 S2'
_chemical_formula_weight         609.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.37(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.895(1)
_cell_length_b                   14.669(1)
_cell_length_c                   16.617(1)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.40
_cell_measurement_theta_min      5.16
_cell_volume                     2603.6(3)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5815
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        5.31
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale_green
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .35
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.071
_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_all   1.015
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0396P)²+4.6462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1111
_refine_ls_wR_factor_obs         0.1035
_reflns_number_observed          3826
_reflns_number_total             4585
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000456h_1.cif
_cod_data_source_block           Complex2
_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^)+(0.0396P)^2^+4.6462P] 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^)+(0.0396P)^2^+4.6462P] 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               4321270
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.25034(4) 0.26713(3) 0.84249(2) 0.02262(14) Uani 1 d . .
N1 N 0.4242(2) 0.3407(2) 0.89868(15) 0.0283(6) Uani 1 d . .
N2 N 0.2803(2) 0.2042(2) 0.9632(2) 0.0271(6) Uani 1 d . .
N3 N 0.1590(2) 0.3735(2) 0.89737(15) 0.0270(6) Uani 1 d . .
C1 C 0.4667(3) 0.3068(2) 0.9848(2) 0.0333(7) Uani 1 d . .
H1A H 0.4382(3) 0.3498(2) 1.0232(2) 0.040 Uiso 1 calc R .
H1B H 0.5594(3) 0.3054(2) 0.9980(2) 0.040 Uiso 1 calc R .
C2 C 0.4172(3) 0.2125(2) 0.9974(2) 0.0324(7) Uani 1 d . .
H2A H 0.4630(3) 0.1670(2) 0.9706(2) 0.039 Uiso 1 calc R .
H2B H 0.4330(3) 0.1987(2) 1.0569(2) 0.039 Uiso 1 calc R .
C3 C 0.2096(3) 0.2607(2) 1.0135(2) 0.0318(7) Uani 1 d . .
H3A H 0.2692(3) 0.2997(2) 1.0511(2) 0.038 Uiso 1 calc R .
H3B H 0.1684(3) 0.2198(2) 1.0476(2) 0.038 Uiso 1 calc R .
C4 C 0.1102(3) 0.3211(2) 0.9613(2) 0.0305(7) Uani 1 d . .
H4A H 0.0397(3) 0.2824(2) 0.9341(2) 0.037 Uiso 1 calc R .
H4B H 0.0775(3) 0.3644(2) 0.9976(2) 0.037 Uiso 1 calc R .
C5 C 0.2564(3) 0.4412(2) 0.9342(2) 0.0317(7) Uani 1 d . .
H5A H 0.2784(3) 0.4311(2) 0.9942(2) 0.038 Uiso 1 calc R .
H5B H 0.2211(3) 0.5034(2) 0.9248(2) 0.038 Uiso 1 calc R .
C6 C 0.3750(3) 0.4350(2) 0.8987(2) 0.0329(7) Uani 1 d . .
H6A H 0.3569(3) 0.4583(2) 0.8417(2) 0.039 Uiso 1 calc R .
H6B H 0.4402(3) 0.4745(2) 0.9311(2) 0.039 Uiso 1 calc R .
C7 C 0.5281(3) 0.3362(2) 0.8506(2) 0.0344(8) Uani 1 d . .
H7A H 0.4911(3) 0.3550(2) 0.7931(2) 0.041 Uiso 1 calc R .
C8 C 0.6374(3) 0.4012(3) 0.8816(2) 0.0476(10) Uani 1 d . .
H8A H 0.6054(3) 0.4633(3) 0.8841(2) 0.071 Uiso 1 calc R .
H8B H 0.6963(3) 0.3995(3) 0.8441(2) 0.071 Uiso 1 calc R .
H8C H 0.6803(3) 0.3822(3) 0.9365(2) 0.071 Uiso 1 calc R .
C9 C 0.5757(3) 0.2395(3) 0.8463(2) 0.0445(9) Uani 1 d . .
H9A H 0.5049(3) 0.1987(3) 0.8264(2) 0.067 Uiso 1 calc R .
H9B H 0.6184(3) 0.2200(3) 0.9011(2) 0.067 Uiso 1 calc R .
H9C H 0.6344(3) 0.2372(3) 0.8086(2) 0.067 Uiso 1 calc R .
C10 C 0.2372(3) 0.1067(2) 0.9594(2) 0.0363(8) Uani 1 d . .
H10A H 0.1437(3) 0.1073(2) 0.9442(2) 0.044 Uiso 1 calc R .
C11 C 0.2729(4) 0.0562(3) 1.0409(3) 0.0559(11) Uani 1 d . .
H11A H 0.2417(4) 0.0901(3) 1.0836(3) 0.084 Uiso 1 calc R .
H11B H 0.3642(4) 0.0510(3) 1.0560(3) 0.084 Uiso 1 calc R .
H11C H 0.2356(4) -0.0048(3) 1.0355(3) 0.084 Uiso 1 calc R .
C12 C 0.2845(4) 0.0554(2) 0.8924(2) 0.0473(9) Uani 1 d . .
H12A H 0.2609(4) 0.0885(2) 0.8404(2) 0.071 Uiso 1 calc R .
H12B H 0.2472(4) -0.0057(2) 0.8865(2) 0.071 Uiso 1 calc R .
H12C H 0.3758(4) 0.0501(2) 0.9070(2) 0.071 Uiso 1 calc R .
C13 C 0.0504(3) 0.4171(2) 0.8395(2) 0.0324(7) Uani 1 d . .
H13A H -0.0093(3) 0.3671(2) 0.8175(2) 0.039 Uiso 1 calc R .
C14 C -0.0221(4) 0.4862(3) 0.8805(2) 0.0432(9) Uani 1 d . .
H14A H -0.0496(4) 0.4575(3) 0.9271(2) 0.065 Uiso 1 calc R .
H14B H -0.0954(4) 0.5072(3) 0.8407(2) 0.065 Uiso 1 calc R .
H14C H 0.0321(4) 0.5383(3) 0.8998(2) 0.065 Uiso 1 calc R .
C15 C 0.0945(4) 0.4595(2) 0.7667(2) 0.0394(8) Uani 1 d . .
H15A H 0.1407(4) 0.4141(2) 0.7413(2) 0.059 Uiso 1 calc R .
H15B H 0.1492(4) 0.5115(2) 0.7854(2) 0.059 Uiso 1 calc R .
H15C H 0.0218(4) 0.4804(2) 0.7263(2) 0.059 Uiso 1 calc R .
C16 C -0.1130(3) 0.1050(3) 0.8038(2) 0.0431(9) Uani 1 d . .
S1 S -0.04080(9) 0.18013(7) 0.73995(5) 0.0408(2) Uani 1 d . .
O1 O 0.0780(2) 0.2006(2) 0.79501(14) 0.0350(5) Uani 1 d . .
O2 O -0.1256(3) 0.2562(2) 0.7252(2) 0.0752(11) Uani 1 d . .
O3 O -0.0315(3) 0.1278(2) 0.6707(2) 0.0680(10) Uani 1 d . .
F1 F -0.0463(3) 0.0294(2) 0.8205(2) 0.0753(8) Uani 1 d . .
F2 F -0.1224(3) 0.1430(2) 0.87308(15) 0.0757(9) Uani 1 d . .
F3 F -0.2260(2) 0.0794(2) 0.7662(2) 0.0674(7) Uani 1 d . .
C17 C 0.4052(4) 0.2807(3) 0.6109(2) 0.0417(9) Uani 1 d . .
S2 S 0.26433(7) 0.24623(5) 0.64590(4) 0.0281(2) Uani 1 d . .
O4 O 0.3052(2) 0.2549(2) 0.73499(14) 0.0460(7) Uani 1 d . .
O5 O 0.2460(3) 0.1545(2) 0.6187(2) 0.0459(6) Uani 1 d . .
O6 O 0.1732(2) 0.3113(2) 0.6107(2) 0.0443(6) Uani 1 d . .
F4 F 0.4376(3) 0.3648(2) 0.6318(2) 0.0696(7) Uani 1 d . .
F5 F 0.3867(3) 0.2747(2) 0.53001(14) 0.0734(8) Uani 1 d . .
F6 F 0.5012(2) 0.2276(2) 0.64168(15) 0.0599(7) 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 0.0033 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O4 Fe O1 91.43(9) . . ?
O4 Fe N3 133.55(11) . . ?
O1 Fe N3 92.40(10) . . ?
O4 Fe N2 140.28(11) . . ?
O1 Fe N2 96.24(9) . . ?
N3 Fe N2 85.11(10) . . ?
O4 Fe N1 92.22(10) . . ?
O1 Fe N1 176.09(9) . . ?
N3 Fe N1 84.06(10) . . ?
N2 Fe N1 81.82(10) . . ?
C6 N1 C1 110.7(3) . . ?
C6 N1 C7 110.5(2) . . ?
C1 N1 C7 111.6(2) . . ?
C6 N1 Fe 100.1(2) . . ?
C1 N1 Fe 108.5(2) . . ?
C7 N1 Fe 115.0(2) . . ?
C2 N2 C3 109.2(2) . . ?
C2 N2 C10 112.0(3) . . ?
C3 N2 C10 111.1(2) . . ?
C2 N2 Fe 105.9(2) . . ?
C3 N2 Fe 106.3(2) . . ?
C10 N2 Fe 112.1(2) . . ?
C4 N3 C5 112.0(2) . . ?
C4 N3 C13 109.1(2) . . ?
C5 N3 C13 112.6(2) . . ?
C4 N3 Fe 100.8(2) . . ?
C5 N3 Fe 107.8(2) . . ?
C13 N3 Fe 114.0(2) . . ?
N1 C1 C2 112.6(3) . . ?
N2 C2 C1 112.3(3) . . ?
N2 C3 C4 112.8(2) . . ?
N3 C4 C3 113.1(3) . . ?
N3 C5 C6 112.9(2) . . ?
N1 C6 C5 112.9(3) . . ?
N1 C7 C9 111.4(3) . . ?
N1 C7 C8 114.1(3) . . ?
C9 C7 C8 110.3(3) . . ?
N2 C10 C12 110.8(3) . . ?
N2 C10 C11 113.7(3) . . ?
C12 C10 C11 110.3(3) . . ?
N3 C13 C15 110.4(3) . . ?
N3 C13 C14 114.0(3) . . ?
C15 C13 C14 110.8(3) . . ?
F2 C16 F3 108.2(3) . . ?
F2 C16 F1 108.0(3) . . ?
F3 C16 F1 106.5(3) . . ?
F2 C16 S1 112.0(3) . . ?
F3 C16 S1 111.5(3) . . ?
F1 C16 S1 110.4(3) . . ?
O3 S1 O2 115.6(2) . . ?
O3 S1 O1 115.3(2) . . ?
O2 S1 O1 114.0(2) . . ?
O3 S1 C16 104.9(2) . . ?
O2 S1 C16 103.5(2) . . ?
O1 S1 C16 101.1(2) . . ?
S1 O1 Fe 159.3(2) . . ?
F4 C17 F5 108.1(3) . . ?
F4 C17 F6 107.5(3) . . ?
F5 C17 F6 107.7(3) . . ?
F4 C17 S2 112.2(3) . . ?
F5 C17 S2 109.8(3) . . ?
F6 C17 S2 111.5(3) . . ?
O6 S2 O5 117.6(2) . . ?
O6 S2 O4 114.0(2) . . ?
O5 S2 O4 113.6(2) . . ?
O6 S2 C17 104.3(2) . . ?
O5 S2 C17 103.7(2) . . ?
O4 S2 C17 101.0(2) . . ?
S2 O4 Fe 145.6(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
Fe O4 2.000(2) . ?
Fe O1 2.125(2) . ?
Fe N3 2.149(3) . ?
Fe N2 2.173(2) . ?
Fe N1 2.220(3) . ?
N1 C6 1.483(4) . ?
N1 C1 1.500(4) . ?
N1 C7 1.510(4) . ?
N2 C2 1.492(4) . ?
N2 C3 1.495(4) . ?
N2 C10 1.504(4) . ?
N3 C4 1.491(4) . ?
N3 C5 1.493(4) . ?
N3 C13 1.511(4) . ?
C1 C2 1.514(5) . ?
C3 C4 1.530(5) . ?
C5 C6 1.526(5) . ?
C7 C9 1.517(5) . ?
C7 C8 1.533(5) . ?
C10 C12 1.515(5) . ?
C10 C11 1.526(5) . ?
C13 C15 1.521(5) . ?
C13 C14 1.525(5) . ?
C16 F2 1.302(4) . ?
C16 F3 1.320(4) . ?
C16 F1 1.325(5) . ?
C16 S1 1.813(4) . ?
S1 O3 1.404(3) . ?
S1 O2 1.438(3) . ?
S1 O1 1.462(2) . ?
C17 F4 1.310(5) . ?
C17 F5 1.322(4) . ?
C17 F6 1.324(4) . ?
C17 S2 1.817(4) . ?
S2 O6 1.418(3) . ?
S2 O5 1.420(3) . ?
S2 O4 1.465(2) . ?
