#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314251.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_4314251
loop_
_publ_author_name
'Sanjit Konar'
'Ennio Zangrando'
'Michael G. B. Drew'
'Talal Mallah'
'Joan Ribas'
'Nirmalendu Ray Chaudhuri'
_publ_section_title
;
 Syntheses, Structural Analyses, and Magneto-Structural Correlations of
 Three Polymeric Fe(II) Complexes with Azide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5966
_journal_page_last               5973
_journal_paper_doi               10.1021/ic034423o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H12 Fe N8'
_chemical_formula_weight         324.15
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.497(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.007(14)
_cell_length_b                   13.789(18)
_cell_length_c                   10.377(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1392(3)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1321
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1321
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.155
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1750P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                990
_reflns_number_total             1321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034423osi20030729_034332.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1750P)^2^] 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^)+(0.1750P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C12 H12 Fe N8 '
_cod_database_code               4314251
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.0000 0.03371(6) 0.2500 0.0322(5) Uani 1 d S . .
N11 N 0.0000 0.1924(4) 0.2500 0.0428(14) Uani 1 d S . .
C12 C 0.0422(7) 0.2440(4) 0.3611(7) 0.0692(17) Uani 1 d DU . .
H12 H 0.0725 0.2103 0.4401 0.083 Uiso 1 calc R . .
C13 C 0.0438(8) 0.3426(5) 0.3662(8) 0.082(2) Uani 1 d DU . .
H13 H 0.0899 0.3712 0.4454 0.099 Uiso 1 calc R . .
C14 C -0.0101(14) 0.3968(7) 0.2757(13) 0.043(3) Uani 0.50 d PDU . .
C17 C -0.0127(11) 0.5057(9) 0.2967(12) 0.048(2) Uani 0.50 d PU . .
H17A H 0.0602 0.5227 0.3728 0.057 Uiso 0.50 calc PR . .
H17B H -0.0994 0.5231 0.3171 0.057 Uiso 0.50 calc PR . .
C18 C 0.0051(12) 0.5656(8) 0.1763(13) 0.052(2) Uani 0.50 d PU . .
H18A H 0.0914 0.5483 0.1552 0.063 Uiso 0.50 calc PR . .
H18B H -0.0685 0.5497 0.1003 0.063 Uiso 0.50 calc PR . .
C19 C 0.0036(12) 0.6706(8) 0.2013(12) 0.054(3) Uani 0.50 d PU . .
C20 C 0.1212(7) 0.7245(5) 0.2757(11) 0.098(2) Uani 1 d U . .
H20 H 0.1991 0.6919 0.3219 0.117 Uiso 1 calc R . .
C21 C 0.1162(5) 0.8228(4) 0.2772(8) 0.0715(19) Uani 1 d U . .
H21 H 0.1991 0.8563 0.2986 0.086 Uiso 1 calc R . .
N22 N 0.0000 0.8747(4) 0.2500 0.0425(14) Uani 1 d S . .
N1 N 0.1493(5) 0.0344(3) 0.1279(4) 0.0470(11) Uani 1 d . . .
N2 N 0.1566(4) 0.0017(3) 0.0266(4) 0.0338(9) Uani 1 d . . .
N3 N 0.1701(5) -0.0316(3) -0.0746(4) 0.0451(11) 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'
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
N1 Fe N1 179.5(2) . 6_556 ?
N1 Fe N3 88.7(2) . 2 ?
N1 Fe N3 91.3(2) 6_556 2 ?
N1 Fe N3 91.3(2) . 5 ?
N1 Fe N3 88.7(2) 6_556 5 ?
N3 Fe N3 178.5(2) 2 5 ?
N1 Fe N11 89.74(12) . . ?
N1 Fe N11 89.74(12) 6_556 . ?
N3 Fe N11 90.75(11) 2 . ?
N3 Fe N11 90.75(11) 5 . ?
N1 Fe N22 90.26(12) . 1_545 ?
N1 Fe N22 90.26(12) 6_556 1_545 ?
N3 Fe N22 89.25(11) 2 1_545 ?
N3 Fe N22 89.24(11) 5 1_545 ?
N11 Fe N22 180.0 . 1_545 ?
C12 N11 C12 115.6(7) 6_556 . ?
C12 N11 Fe 122.2(4) 6_556 . ?
C12 N11 Fe 122.2(4) . . ?
N11 C12 C13 124.4(7) . . ?
N11 C12 H12 117.8 . . ?
C13 C12 H12 117.8 . . ?
C14 C13 C12 125.6(9) . . ?
C14 C13 H13 117.2 . . ?
C12 C13 H13 117.2 . . ?
C14 C14 C13 120(2) 6_556 . ?
C14 C14 C17 98.4(5) 6_556 . ?
C13 C14 C17 120.9(11) . . ?
C14 C14 C13 41.2(19) 6_556 6_556 ?
C13 C14 C13 112.2(8) . 6_556 ?
C17 C14 C13 125.6(9) . 6_556 ?
C14 C14 C17 61.0(5) 6_556 6_556 ?
C13 C14 C17 142.3(12) . 6_556 ?
C17 C14 C17 37.5(8) . 6_556 ?
C13 C14 C17 91.5(8) 6_556 6_556 ?
C14 C17 C18 113.9(8) . . ?
C14 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
C14 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C17 112.1(10) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C19 C19 C20 73.2(13) 6_556 . ?
C19 C19 C18 100.3(6) 6_556 . ?
C20 C19 C18 123.8(10) . . ?
C19 C19 C20 66.3(10) 6_556 6_556 ?
C20 C19 C20 105.1(8) . 6_556 ?
C18 C19 C20 123.5(9) . 6_556 ?
C19 C19 C18 48.2(5) 6_556 6_556 ?
C20 C19 C18 100.8(9) . 6_556 ?
C18 C19 C18 52.1(9) . 6_556 ?
C20 C19 C18 95.6(7) 6_556 6_556 ?
C21 C20 C19 119.4(7) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
N22 C21 C20 124.3(6) . . ?
N22 C21 H21 117.8 . . ?
C20 C21 H21 117.8 . . ?
C21 N22 C21 115.3(6) 6_556 . ?
C21 N22 Fe 122.3(3) 6_556 1_565 ?
C21 N22 Fe 122.3(3) . 1_565 ?
N2 N1 Fe 136.3(4) . . ?
N1 N2 N3 177.2(5) . . ?
N2 N3 Fe 121.2(3) . 5 ?
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 N1 2.173(5) . ?
Fe N1 2.173(5) 6_556 ?
Fe N3 2.183(5) 2 ?
Fe N3 2.183(5) 5 ?
Fe N11 2.188(6) . ?
Fe N22 2.193(7) 1_545 ?
N11 C12 1.336(7) 6_556 ?
N11 C12 1.336(7) . ?
C12 C13 1.360(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.224(13) . ?
C13 H13 0.9300 . ?
C14 C14 0.613(18) 6_556 ?
C14 C17 1.518(17) . ?
C14 C13 1.616(16) 6_556 ?
C14 C17 1.717(17) 6_556 ?
C17 C18 1.542(16) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.471(16) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C19 1.03(2) 6_556 ?
C19 C20 1.452(14) . ?
C19 C20 1.519(13) 6_556 ?
C19 C18 1.941(16) 6_556 ?
C20 C21 1.357(9) . ?
C20 H20 0.9300 . ?
C21 N22 1.339(6) . ?
C21 H21 0.9300 . ?
N22 C21 1.339(6) 6_556 ?
N22 Fe 2.193(7) 1_565 ?
N1 N2 1.162(6) . ?
N2 N3 1.183(6) . ?
N3 Fe 2.183(5) 5 ?
