#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:12:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178889 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/18/4111870.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_4111870
loop_
_publ_author_name
'John F. Berry'
'Eckhard Bill'
'Eberhard Bothe'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_contact_author_address
;  Max-Planck-Institut fuer Bianorganische Chemie,
   Stiftstrasse 34-36,
   D-45470 Muelheim an der Ruhr, Germany
;
_publ_contact_author_email       wieghardt@mpi-muelheim.mpg-de
_publ_contact_author_fax         '49 (0)208 306-3952'
_publ_contact_author_name        'Karl Wieghardt'
_publ_contact_author_phone       '49 (0)208 306-3609'
_publ_section_title
;
 Octahedral Non-Heme Non-Oxo Fe(IV) Species Stabilized by a Redox-Innocent
 N-Methylated Cyclam-Acetate Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11550
_journal_page_last               11551
_journal_paper_doi               10.1021/ja052673t
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         '[C15 H31 Fe N7 O2]+,(P F6)-'
_chemical_formula_sum            'C15 H31 F6 Fe N7 O2 P'
_chemical_formula_weight         542.29
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.192(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9387(3)
_cell_length_b                   8.7443(2)
_cell_length_c                   12.2164(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1055.50(5)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27202
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0228P)²+1.4833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                3189
_reflns_number_total             3345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja052673tsi20050425_112135.cif
_cod_data_source_block           ST5018
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+1.4833P] 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^)+(0.0228P)^2^+1.4833P] 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               4111870
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.01321(9) Uani 1 d S . .
N1 N 0.40216(15) 0.16431(18) -0.10998(14) 0.0225(3) Uani 1 d . . .
C2 C 0.5052(2) 0.1933(2) -0.18819(18) 0.0284(4) Uani 1 d . . .
H2A H 0.4820 0.2882 -0.2302 0.034 Uiso 1 calc R . .
H2B H 0.5050 0.1076 -0.2412 0.034 Uiso 1 calc R . .
C3 C 0.64571(19) 0.2090(2) -0.12509(18) 0.0259(4) Uani 1 d . . .
H3A H 0.7125 0.2349 -0.1768 0.031 Uiso 1 calc R . .
H3B H 0.6454 0.2925 -0.0704 0.031 Uiso 1 calc R . .
N4 N 0.68465(15) 0.06179(18) -0.06776(13) 0.0197(3) Uani 1 d . . .
C5 C 0.79670(18) 0.0883(2) 0.02279(18) 0.0251(4) Uani 1 d . . .
H5A H 0.7705 0.1733 0.0696 0.030 Uiso 1 calc R . .
H5B H 0.8788 0.1204 -0.0104 0.030 Uiso 1 calc R . .
C6 C 0.83139(19) -0.0516(2) 0.09570(19) 0.0287(4) Uani 1 d . . .
H6A H 0.9165 -0.0298 0.1430 0.034 Uiso 1 calc R . .
H6B H 0.8494 -0.1385 0.0474 0.034 Uiso 1 calc R . .
C7 C 0.7250(2) -0.1023(3) 0.16994(19) 0.0336(5) Uani 1 d . . .
H7A H 0.7653 -0.1817 0.2212 0.040 Uiso 1 calc R . .
H7B H 0.7017 -0.0137 0.2147 0.040 Uiso 1 calc R . .
C12 C 0.7344(2) -0.0437(3) -0.14964(17) 0.0285(4) Uani 1 d . . .
H12A H 0.7606 -0.1412 -0.1140 0.043 Uiso 1 calc R . .
H12B H 0.8129 0.0019 -0.1793 0.043 Uiso 1 calc R . .
H12C H 0.6624 -0.0613 -0.2097 0.043 Uiso 1 calc R . .
C8 C 0.3867(4) 0.3063(5) -0.0298(3) 0.0206(6) Uani 0.50 d P A 1
H8A H 0.4144 0.4004 -0.0665 0.025 Uiso 0.50 calc PR A 1
H8B H 0.2900 0.3174 -0.0188 0.025 Uiso 0.50 calc PR A 1
C9 C 0.4699(4) 0.2938(4) 0.0838(3) 0.0226(5) Uani 0.50 d P A 1
O10 O 0.53484(14) 0.16144(16) 0.10989(12) 0.0192(3) Uani 0.50 d P A 1
O11 O 0.4739(5) 0.4023(6) 0.1484(3) 0.0316(7) Uani 0.50 d P A 1
C13 C 0.3622(4) 0.3127(5) -0.0776(3) 0.0206(6) Uani 0.50 d P A 2
H13A H 0.4396 0.3643 -0.0369 0.031 Uiso 0.50 calc PR A 2
H13B H 0.2889 0.3032 -0.0305 0.031 Uiso 0.50 calc PR A 2
H13C H 0.3307 0.3725 -0.1433 0.031 Uiso 0.50 calc PR A 2
N21 N 0.53484(14) 0.16144(16) 0.10989(12) 0.0192(3) Uani 0.50 d P . 2
N22 N 0.5047(3) -0.2754(4) -0.1512(3) 0.0226(5) Uani 0.50 d P . 2
N23 N 0.5457(6) -0.3859(7) -0.1884(4) 0.0316(7) Uani 0.50 d P B 2
P30 P 0.5000 0.0000 0.5000 0.01889(13) Uani 1 d S . .
F31 F 0.46868(14) 0.11584(14) 0.39886(11) 0.0318(3) Uani 1 d . . .
F32 F 0.58118(13) 0.13319(14) 0.56961(10) 0.0291(3) Uani 1 d . . .
F33 F 0.36358(12) 0.05154(15) 0.54839(12) 0.0317(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 0.0033 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'
P P 0.1023 0.0942 '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
N21 Fe1 O10 0.00(12) 3_655 3_655
N21 Fe1 O10 180.0 3_655 .
O10 Fe1 O10 180.0 3_655 .
N21 Fe1 N1 91.09(6) 3_655 .
O10 Fe1 N1 91.09(6) 3_655 .
O10 Fe1 N1 88.92(6) . .
N21 Fe1 N1 88.91(6) 3_655 3_655
O10 Fe1 N1 88.91(6) 3_655 3_655
O10 Fe1 N1 91.08(6) . 3_655
N1 Fe1 N1 180.0 . 3_655
N21 Fe1 N4 89.29(6) 3_655 3_655
O10 Fe1 N4 89.29(6) 3_655 3_655
O10 Fe1 N4 90.71(6) . 3_655
N1 Fe1 N4 93.53(6) . 3_655
N1 Fe1 N4 86.47(6) 3_655 3_655
N21 Fe1 N4 90.71(6) 3_655 .
O10 Fe1 N4 90.71(6) 3_655 .
O10 Fe1 N4 89.29(6) . .
N1 Fe1 N4 86.47(6) . .
N1 Fe1 N4 93.53(6) 3_655 .
N4 Fe1 N4 180.0 3_655 .
C13 N1 C7 102.7(2) . 3_655
C13 N1 C2 104.7(2) . .
C7 N1 C2 110.49(17) 3_655 .
C13 N1 C8 22.35(18) . .
C7 N1 C8 116.8(2) 3_655 .
C2 N1 C8 112.1(2) . .
C13 N1 Fe1 124.1(2) . .
C7 N1 Fe1 111.67(12) 3_655 .
C2 N1 Fe1 102.70(11) . .
C8 N1 Fe1 101.84(17) . .
N1 C2 C3 110.16(17) . .
N4 C3 C2 109.61(15) . .
C12 N4 C3 107.89(15) . .
C12 N4 C5 108.56(15) . .
C3 N4 C5 110.25(15) . .
C12 N4 Fe1 117.46(12) . .
C3 N4 Fe1 101.94(10) . .
C5 N4 Fe1 110.45(11) . .
N4 C5 C6 114.10(15) . .
C5 C6 C7 116.71(16) . .
N1 C7 C6 114.63(18) 3_655 .
C9 C8 N1 114.7(3) . .
O11 C9 O10 121.9(4) . .
O11 C9 C8 119.9(4) . .
O10 C9 C8 118.1(3) . .
C9 O10 Fe1 114.41(19) . .
N23 N22 N21 177.9(4) . 3_655
F33 P30 F33 180.0 . 3_656
F33 P30 F31 90.28(7) . .
F33 P30 F31 89.72(7) 3_656 .
F33 P30 F31 89.72(7) . 3_656
F33 P30 F31 90.29(7) 3_656 3_656
F31 P30 F31 180.0 . 3_656
F33 P30 F32 90.15(6) . 3_656
F33 P30 F32 89.85(6) 3_656 3_656
F31 P30 F32 90.31(7) . 3_656
F31 P30 F32 89.69(7) 3_656 3_656
F33 P30 F32 89.85(6) . .
F33 P30 F32 90.14(6) 3_656 .
F31 P30 F32 89.69(7) . .
F31 P30 F32 90.31(7) 3_656 .
F32 P30 F32 180.0 3_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N21 1.9530(13) 3_655
Fe1 O10 1.9530(13) 3_655
Fe1 O10 1.9531(13) .
Fe1 N1 2.1291(16) .
Fe1 N1 2.1291(16) 3_655
Fe1 N4 2.1617(14) 3_655
Fe1 N4 2.1617(14) .
N1 C13 1.425(4) .
N1 C7 1.493(3) 3_655
N1 C2 1.496(2) .
N1 C8 1.599(4) .
C2 C3 1.527(3) .
C3 N4 1.496(2) .
N4 C12 1.484(2) .
N4 C5 1.501(2) .
C5 C6 1.530(3) .
C6 C7 1.531(3) .
C7 N1 1.493(3) 3_655
C8 C9 1.541(6) .
C9 O11 1.233(6) .
C9 O10 1.346(4) .
N22 N23 1.160(7) .
N22 N21 1.202(3) 3_655
P30 F33 1.6012(12) .
P30 F33 1.6012(12) 3_656
P30 F31 1.6021(12) .
P30 F31 1.6021(12) 3_656
P30 F32 1.6070(11) 3_656
P30 F32 1.6071(11) .
