#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/00/2210050.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2210050
loop_
_publ_author_name
'Zhi-Xin Miao'
'Min Shao'
'Hong-Jiang Liu'
'Ming-Xing Li'
_publ_section_title
;
 Diazidobis(1,10-phenanthroline)iron(II)
;
_journal_coeditor_code           AT2068
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2170
_journal_page_last               m2172
_journal_paper_doi               10.1107/S1600536806029679
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe (N3)2 (C12 H8 N2)2]'
_chemical_formula_moiety         'C24 H16 Fe N10'
_chemical_formula_sum            'C24 H16 Fe N10'
_chemical_formula_weight         500.32
_chemical_name_systematic
;
Diazidobis(1,10-phenanthroline)iron(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.3440(10)
_cell_angle_beta                 81.8440(10)
_cell_angle_gamma                73.4510(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1824(2)
_cell_length_b                   11.1341(2)
_cell_length_c                   12.6788(2)
_cell_measurement_reflns_used    6359
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.825
_cell_measurement_theta_min      2.610
_cell_volume                     1092.56(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'APEX2 (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12819
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.8682
_exptl_absorpt_correction_T_min  0.8114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0699P)²+0.6391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                3348
_reflns_number_total             3845
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2068.cif
_cod_data_source_block           I
_cod_database_code               2210050
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.2267(4) 0.3987(3) 0.6472(3) 0.0511(8) Uani d . 1
H H1 0.2026 0.3755 0.5842 0.061 Uiso calc R 1
C C2 0.3218(4) 0.4853(3) 0.6405(3) 0.0648(10) Uani d . 1
H H2 0.3609 0.5188 0.5743 0.078 Uiso calc R 1
C C3 0.3571(4) 0.5209(3) 0.7329(4) 0.0657(10) Uani d . 1
H H3 0.4223 0.5777 0.7296 0.079 Uiso calc R 1
C C4 0.2950(4) 0.4716(3) 0.8327(3) 0.0504(8) Uani d . 1
C C5 0.2024(3) 0.3836(3) 0.8311(2) 0.0395(6) Uani d . 1
C C6 0.3191(4) 0.5062(3) 0.9338(4) 0.0650(10) Uani d . 1
H H6 0.3799 0.5651 0.9346 0.078 Uiso calc R 1
C C7 0.2575(4) 0.4571(3) 1.0265(3) 0.0604(9) Uani d . 1
H H7 0.2753 0.4823 1.0903 0.072 Uiso calc R 1
C C8 0.1639(4) 0.3655(3) 1.0288(2) 0.0474(7) Uani d . 1
C C9 0.1355(3) 0.3297(2) 0.9314(2) 0.0381(6) Uani d . 1
C C10 0.0972(4) 0.3086(3) 1.1239(2) 0.0562(9) Uani d . 1
H H10 0.1130 0.3296 1.1899 0.067 Uiso calc R 1
C C11 0.0102(5) 0.2234(3) 1.1185(3) 0.0585(9) Uani d . 1
H H11 -0.0329 0.1844 1.1808 0.070 Uiso calc R 1
C C12 -0.0144(4) 0.1946(3) 1.0193(2) 0.0499(7) Uani d . 1
H H12 -0.0753 0.1362 1.0168 0.060 Uiso calc R 1
C C13 0.3202(4) -0.0168(3) 0.8367(2) 0.0485(7) Uani d . 1
H H13 0.2911 0.0164 0.9030 0.058 Uiso calc R 1
C C14 0.4548(4) -0.1255(3) 0.8261(3) 0.0574(8) Uani d . 1
H H14 0.5145 -0.1630 0.8839 0.069 Uiso calc R 1
C C15 0.4981(4) -0.1764(3) 0.7304(3) 0.0550(8) Uani d . 1
H H15 0.5868 -0.2498 0.7224 0.066 Uiso calc R 1
C C16 0.4079(4) -0.1177(3) 0.6433(3) 0.0444(7) Uani d . 1
C C17 0.4464(4) -0.1634(3) 0.5387(3) 0.0548(8) Uani d . 1
H H17 0.5322 -0.2377 0.5273 0.066 Uiso calc R 1
C C18 0.3610(4) -0.1011(3) 0.4566(3) 0.0552(8) Uani d . 1
H H18 0.3891 -0.1329 0.3897 0.066 Uiso calc R 1
C C19 0.2284(4) 0.0125(3) 0.4707(2) 0.0434(7) Uani d . 1
C C20 0.1368(4) 0.0826(3) 0.3879(2) 0.0506(8) Uani d . 1
H H20 0.1605 0.0549 0.3195 0.061 Uiso calc R 1
C C21 0.0139(4) 0.1906(3) 0.4081(2) 0.0504(8) Uani d . 1
H H21 -0.0458 0.2382 0.3534 0.060 Uiso calc R 1
C C22 -0.0224(4) 0.2299(3) 0.5108(2) 0.0451(7) Uani d . 1
H H22 -0.1075 0.3041 0.5234 0.054 Uiso calc R 1
C C23 0.1845(3) 0.0590(2) 0.5725(2) 0.0354(6) Uani d . 1
C C24 0.2763(3) -0.0078(2) 0.6605(2) 0.0365(6) Uani d . 1
Fe Fe1 -0.00792(5) 0.21421(4) 0.76483(3) 0.04126(17) Uani d . 1
N N1 0.1689(3) 0.3477(2) 0.73963(18) 0.0399(5) Uani d . 1
N N2 0.0454(3) 0.2467(2) 0.92752(17) 0.0402(5) Uani d . 1
N N3 0.2311(3) 0.0420(2) 0.75716(18) 0.0394(5) Uani d . 1
N N4 0.0593(3) 0.1660(2) 0.59186(17) 0.0379(5) Uani d . 1
N N5 -0.2140(4) 0.3797(3) 0.7317(3) 0.0636(8) Uani d . 1
N N6 -0.2158(3) 0.4722(2) 0.6788(2) 0.0472(6) Uani d . 1
N N7 -0.2211(5) 0.5652(3) 0.6282(3) 0.0904(12) Uani d . 1
N N8 -0.1758(4) 0.0941(2) 0.8295(2) 0.0530(7) Uani d . 1
N N9 -0.3039(5) 0.1248(3) 0.8590(3) 0.0658(8) Uani d . 1
N N10 -0.4527(6) 0.1556(6) 0.8979(5) 0.149(2) Uani d . 1
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'
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_publ_flag
N1 C1 C2 122.8(3) ?
N1 C1 H1 118.6 ?
C2 C1 H1 118.6 ?
C3 C2 C1 119.1(3) ?
C3 C2 H2 120.4 ?
C1 C2 H2 120.4 ?
C2 C3 C4 120.1(3) ?
C2 C3 H3 120.0 ?
C4 C3 H3 120.0 ?
C5 C4 C3 116.5(3) ?
C5 C4 C6 119.1(3) ?
C3 C4 C6 124.4(3) ?
N1 C5 C4 123.3(3) ?
N1 C5 C9 117.8(2) ?
C4 C5 C9 118.9(3) ?
C7 C6 C4 122.3(3) ?
C7 C6 H6 118.9 ?
C4 C6 H6 118.9 ?
C6 C7 C8 120.6(3) ?
C6 C7 H7 119.7 ?
C8 C7 H7 119.7 ?
C10 C8 C9 117.5(3) ?
C10 C8 C7 123.5(3) ?
C9 C8 C7 119.0(3) ?
N2 C9 C8 122.2(3) ?
N2 C9 C5 117.7(2) ?
C8 C9 C5 120.1(3) ?
C11 C10 C8 119.6(3) ?
C11 C10 H10 120.2 ?
C8 C10 H10 120.2 ?
C10 C11 C12 119.4(3) ?
C10 C11 H11 120.3 ?
C12 C11 H11 120.3 ?
N2 C12 C11 123.0(3) ?
N2 C12 H12 118.5 ?
C11 C12 H12 118.5 ?
N3 C13 C14 123.4(3) ?
N3 C13 H13 118.3 ?
C14 C13 H13 118.3 ?
C15 C14 C13 119.3(3) ?
C15 C14 H14 120.4 ?
C13 C14 H14 120.4 ?
C14 C15 C16 119.7(3) ?
C14 C15 H15 120.2 ?
C16 C15 H15 120.2 ?
C24 C16 C15 117.3(3) ?
C24 C16 C17 119.0(3) ?
C15 C16 C17 123.6(3) ?
C18 C17 C16 121.5(3) ?
C18 C17 H17 119.3 ?
C16 C17 H17 119.3 ?
C17 C18 C19 121.0(3) ?
C17 C18 H18 119.5 ?
C19 C18 H18 119.5 ?
C20 C19 C23 117.1(3) ?
C20 C19 C18 123.6(3) ?
C23 C19 C18 119.2(3) ?
C21 C20 C19 119.7(3) ?
C21 C20 H20 120.1 ?
C19 C20 H20 120.1 ?
C20 C21 C22 119.7(3) ?
C20 C21 H21 120.2 ?
C22 C21 H21 120.2 ?
N4 C22 C21 122.8(3) ?
N4 C22 H22 118.6 ?
C21 C22 H22 118.6 ?
N4 C23 C19 122.5(3) ?
N4 C23 C24 117.8(2) ?
C19 C23 C24 119.7(3) ?
N3 C24 C16 122.9(3) ?
N3 C24 C23 117.6(2) ?
C16 C24 C23 119.5(2) ?
N5 Fe1 N8 95.38(12) y
N5 Fe1 N2 101.59(11) y
N8 Fe1 N2 93.88(10) y
N5 Fe1 N4 94.66(10) y
N8 Fe1 N4 102.20(9) y
N2 Fe1 N4 155.95(9) y
N5 Fe1 N3 166.42(10) y
N8 Fe1 N3 91.33(10) y
N2 Fe1 N3 89.70(8) ?
N4 Fe1 N3 72.34(8) y
N5 Fe1 N1 86.26(10) y
N8 Fe1 N1 166.15(9) y
N2 Fe1 N1 72.34(8) y
N4 Fe1 N1 91.35(8) y
N3 Fe1 N1 90.05(8) y
C1 N1 C5 118.2(3) ?
C1 N1 Fe1 126.9(2) ?
C5 N1 Fe1 114.61(18) ?
C12 N2 C9 118.4(2) ?
C12 N2 Fe1 124.3(2) ?
C9 N2 Fe1 117.23(18) ?
C13 N3 C24 117.4(2) ?
C13 N3 Fe1 127.6(2) ?
C24 N3 Fe1 114.87(17) ?
C22 N4 C23 118.2(2) ?
C22 N4 Fe1 124.96(19) ?
C23 N4 Fe1 116.66(17) ?
N6 N5 Fe1 131.8(2) y
N7 N6 N5 178.2(3) y
N9 N8 Fe1 126.0(3) y
N8 N9 N10 176.5(5) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.327(4) ?
C1 C2 1.391(5) ?
C1 H1 0.9300 ?
C2 C3 1.372(6) ?
C2 H2 0.9300 ?
C3 C4 1.406(5) ?
C3 H3 0.9300 ?
C4 C5 1.402(4) ?
C4 C6 1.435(5) ?
C5 N1 1.357(4) ?
C5 C9 1.445(4) ?
C6 C7 1.333(5) ?
C6 H6 0.9300 ?
C7 C8 1.435(5) ?
C7 H7 0.9300 ?
C8 C9 1.409(4) ?
C8 C10 1.409(5) ?
C9 N2 1.345(4) ?
C10 C11 1.351(5) ?
C10 H10 0.9300 ?
C11 C12 1.388(4) ?
C11 H11 0.9300 ?
C12 N2 1.332(4) ?
C12 H12 0.9300 ?
C13 N3 1.327(4) ?
C13 C14 1.390(4) ?
C13 H13 0.9300 ?
C14 C15 1.357(5) ?
C14 H14 0.9300 ?
C15 C16 1.407(4) ?
C15 H15 0.9300 ?
C16 C24 1.396(4) ?
C16 C17 1.437(5) ?
C17 C18 1.347(5) ?
C17 H17 0.9300 ?
C18 C19 1.423(5) ?
C18 H18 0.9300 ?
C19 C20 1.405(4) ?
C19 C23 1.407(4) ?
C20 C21 1.353(5) ?
C20 H20 0.9300 ?
C21 C22 1.387(4) ?
C21 H21 0.9300 ?
C22 N4 1.328(4) ?
C22 H22 0.9300 ?
C23 N4 1.353(3) ?
C23 C24 1.445(4) ?
C24 N3 1.364(3) ?
Fe1 N5 2.160(3) y
Fe1 N8 2.195(3) y
Fe1 N2 2.257(2) y
Fe1 N4 2.272(2) y
Fe1 N3 2.316(2) y
Fe1 N1 2.321(2) y
N5 N6 1.160(4) y
N6 N7 1.147(4) y
N8 N9 1.034(4) y
N9 N10 1.214(6) y
