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#$Date: 2016-03-22 11:44:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178913 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/42/4114282.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_4114282
loop_
_publ_author_name
'Trevor W. Hayton'
'W. Stephen McNeil'
'Brian O. Patrick'
'Peter Legzdins'
_publ_section_title
;
 Toward Binary Nitrosyls: Distinctly Bent Fe-N-O Linkages in
 Base-Stabilized Fe(NO)3+ Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12935
_journal_page_last               12944
_journal_paper_doi               10.1021/ja036887r
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'Cl Fe N3 O3'
_chemical_formula_weight         181.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           186
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   7.1701(15)
_cell_length_b                   7.1701(15)
_cell_length_c                   6.0403(12)
_cell_measurement_reflns_used    1854
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.3
_cell_volume                     268.93(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2302
_diffrn_reflns_theta_full        27.72
_diffrn_reflns_theta_max         27.72
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    3.216
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.239
_exptl_crystal_description       needle
_exptl_crystal_F_000             176
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         231
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0158P)²+0.6061P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                231
_reflns_number_total             231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036887rsi20030624_074545.cif
_cod_data_source_block           pl266
_cod_database_code               4114282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z+1/2'
'-x, -x+y, z+1/2'
'x-y, -y, 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
Fe1 Fe 0.6667 0.3333 0.28987(9) 0.0146(3) Uani 1 6 d S
Cl1 Cl 0.6667 0.3333 0.6626(3) 0.0222(4) Uani 1 6 d S
O1 O 0.8637(3) 0.7274(6) 0.0581(8) 0.0323(8) Uani 1 2 d S
N1 N 0.7935(3) 0.5869(6) 0.1828(7) 0.0212(8) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0148(3) 0.0148(3) 0.0142(5) 0.000 0.000 0.00742(17)
Cl1 0.0269(7) 0.0269(7) 0.0129(9) 0.000 0.000 0.0135(4)
O1 0.0329(15) 0.0223(17) 0.0382(16) 0.0073(18) 0.0036(9) 0.0111(9)
N1 0.0232(14) 0.019(2) 0.0201(17) -0.0014(16) -0.0007(8) 0.0094(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Cl Cl 0.1484 0.1585 '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
N1 Fe1 N1 106.47(16) 4_665 3_655
N1 Fe1 N1 106.47(16) 4_665 .
N1 Fe1 N1 106.47(16) 3_655 .
N1 Fe1 Cl1 112.33(15) 4_665 .
N1 Fe1 Cl1 112.33(15) 3_655 .
N1 Fe1 Cl1 112.33(15) . .
O1 N1 Fe1 161.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.702(4) 4_665
Fe1 N1 1.702(4) 3_655
Fe1 N1 1.702(4) .
Fe1 Cl1 2.252(2) .
O1 N1 1.152(5) .
