#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:06:16 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178934 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116391.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_4116391
loop_
_publ_author_name
'Karsten Meyer'
'Eckhard Bill'
'Bernd Mienert'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
 Photolysis of cis- and trans-[FeIII(cyclam)(N3)2]+ Complexes:
 Spectroscopic Characterization of a Nitridoiron(V) Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4859
_journal_page_last               4876
_journal_paper_doi               10.1021/ja983454t
_journal_volume                  121
_journal_year                    1999
_chemical_formula_structural     '[C10 H24 Fe N10]+, (PF6)-'
_chemical_formula_sum            'C10 H24 F6 Fe N10 P'
_chemical_formula_weight         485.21
_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                 102.95(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.858(1)
_cell_length_b                   13.323(2)
_cell_length_c                   9.335(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      9.5
_cell_volume                     952.4(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       2θ/ω-scan
_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2058
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.3965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0995
_refine_ls_wR_factor_obs         0.0858
_reflns_number_observed          1398
_reflns_number_total             1941
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983454t_1.cif
_cod_data_source_block           (1b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.3965P] 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^)+(0.0000P)^2^+0.3965P] 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               4116391
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
Fe Fe 0.0000 0.5000 0.5000 0.0261(2) Uani 1 d S
N1 N 0.1590(3) 0.4070(2) 0.4229(3) 0.0381(6) Uani 1 d .
H1 H 0.2694(3) 0.4306(2) 0.4572(3) 0.046 Uiso 1 calc R
N2 N 0.0420(3) 0.4368(2) 0.6989(2) 0.0385(6) Uani 1 d .
H2 H 0.1447(3) 0.4633(2) 0.7496(2) 0.046 Uiso 1 calc R
N3 N 0.1883(3) 0.5915(2) 0.5815(3) 0.0363(5) Uani 1 d .
N4 N 0.3176(3) 0.6090(2) 0.5418(3) 0.0434(6) Uani 1 d .
N5 N 0.4453(4) 0.6295(3) 0.5092(4) 0.0875(12) Uani 1 d .
C1 C 0.1215(4) 0.4176(3) 0.2613(4) 0.0513(8) Uani 1 d .
H1A H 0.0185(4) 0.3790(3) 0.2168(4) 0.062 Uiso 1 calc R
H1B H 0.2191(4) 0.3928(3) 0.2237(4) 0.062 Uiso 1 calc R
C2 C 0.1602(4) 0.3007(2) 0.4701(4) 0.0500(8) Uani 1 d .
H2A H 0.2449(4) 0.2637(2) 0.4296(4) 0.060 Uiso 1 calc R
H2B H 0.0462(4) 0.2714(2) 0.4312(4) 0.060 Uiso 1 calc R
C3 C 0.2046(4) 0.2903(2) 0.6343(4) 0.0568(9) Uani 1 d .
H3A H 0.3115(4) 0.3271(2) 0.6730(4) 0.068 Uiso 1 calc R
H3B H 0.2274(4) 0.2200(2) 0.6587(4) 0.068 Uiso 1 calc R
C4 C 0.0661(5) 0.3269(2) 0.7102(4) 0.0541(9) Uani 1 d .
H4A H -0.0436(5) 0.2942(2) 0.6670(4) 0.065 Uiso 1 calc R
H4B H 0.0983(5) 0.3081(2) 0.8132(4) 0.065 Uiso 1 calc R
C5 C -0.0917(4) 0.4736(3) 0.7752(3) 0.0512(8) Uani 1 d .
H5A H -0.0517(4) 0.4650(3) 0.8806(3) 0.061 Uiso 1 calc R
H5B H -0.1995(4) 0.4363(3) 0.7429(3) 0.061 Uiso 1 calc R
P1 P 0.0000 0.0000 0.5000 0.0360(2) Uani 1 d S
F1 F 0.1936(2) 0.0441(2) 0.5392(2) 0.0664(6) Uani 1 d .
F2 F 0.0780(3) -0.1046(2) 0.4722(4) 0.0997(10) Uani 1 d .
F3 F -0.0148(3) 0.0284(3) 0.3353(3) 0.1021(10) 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'
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
N3 Fe N3 180.0 3_566 .
N3 Fe N2 87.00(10) 3_566 3_566
N3 Fe N2 93.00(10) . 3_566
N3 Fe N2 93.00(10) 3_566 .
N3 Fe N2 87.00(10) . .
N2 Fe N2 180.0 3_566 .
N3 Fe N1 92.70(10) 3_566 3_566
N3 Fe N1 87.30(10) . 3_566
N2 Fe N1 94.95(10) 3_566 3_566
N2 Fe N1 85.05(10) . 3_566
N3 Fe N1 87.30(10) 3_566 .
N3 Fe N1 92.70(10) . .
N2 Fe N1 85.05(10) 3_566 .
N2 Fe N1 94.95(10) . .
N1 Fe N1 180.0 3_566 .
C1 N1 C2 112.4(2) . .
C1 N1 Fe 108.0(2) . .
C2 N1 Fe 116.6(2) . .
C4 N2 C5 112.8(3) . .
C4 N2 Fe 118.5(2) . .
C5 N2 Fe 108.7(2) . .
N4 N3 Fe 129.5(2) . .
N5 N4 N3 176.4(3) . .
N1 C1 C5 108.1(2) . 3_566
N1 C2 C3 112.1(3) . .
C2 C3 C4 115.1(3) . .
N2 C4 C3 112.5(3) . .
N2 C5 C1 107.7(2) . 3_566
F3 P1 F3 180.0 . 3_556
F3 P1 F2 90.1(2) . 3_556
F3 P1 F2 89.9(2) 3_556 3_556
F3 P1 F2 89.9(2) . .
F3 P1 F2 90.1(2) 3_556 .
F2 P1 F2 180.0 3_556 .
F3 P1 F1 90.37(13) . 3_556
F3 P1 F1 89.63(13) 3_556 3_556
F2 P1 F1 88.68(12) 3_556 3_556
F2 P1 F1 91.32(12) . 3_556
F3 P1 F1 89.63(13) . .
F3 P1 F1 90.37(13) 3_556 .
F2 P1 F1 91.32(12) 3_556 .
F2 P1 F1 88.68(12) . .
F1 P1 F1 180.0 3_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N3 1.937(2) 3_566
Fe N3 1.937(2) .
Fe N2 1.998(2) 3_566
Fe N2 1.998(2) .
Fe N1 2.004(2) 3_566
Fe N1 2.004(2) .
N1 C1 1.478(4) .
N1 C2 1.483(4) .
N2 C4 1.476(4) .
N2 C5 1.480(4) .
N3 N4 1.180(3) .
N4 N5 1.145(4) .
C1 C5 1.495(5) 3_566
C2 C3 1.500(5) .
C3 C4 1.507(5) .
C5 C1 1.495(5) 3_566
P1 F3 1.562(2) .
P1 F3 1.562(2) 3_556
P1 F2 1.568(2) 3_556
P1 F2 1.568(2) .
P1 F1 1.594(2) 3_556
P1 F1 1.594(2) .
